Intelligent Manufacturing and Mechatronics: Selected Articles from iM3F 2023, 07–08 August, Pekan, Malaysia (Lecture Notes in Networks and Systems, 850) [1st ed. 2024] 9819988187, 9789819988181

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Springer Proceedings in Materials

Radhiyah Abd. Aziz Zulhelmi Ismail A. K. M. Asif Iqbal Irfan Ahmed   Editors

Intelligent Manufacturing and Mechatronics Selected Articles from iM3F 2023, 7–8 August, Pekan, Malaysia

Springer Proceedings in Materials Volume 40

Series Editors Arindam Ghosh, Department of Physics, Indian Institute of Science, Bengaluru, India Daniel Chua, Department of Materials Science and Engineering, National University of Singapore, Singapore, Singapore Flavio Leandro de Souza, Universidade Federal do ABC, Sao Paulo, São Paulo, Brazil Oral Cenk Aktas, Institute of Material Science, Christian-Albrechts-Universität zu Kiel, Kiel, Schleswig-Holstein, Germany Yafang Han, Beijing Institute of Aeronautical Materials, Beijing, Beijing, China Jianghong Gong, School of Materials Science and Engineering, Tsinghua University, Beijing, Beijing, China Mohammad Jawaid , Laboratory of Biocomposite Technology, INTROP, Universiti Putra Malaysia, Serdang, Selangor, Malaysia

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Radhiyah Abd. Aziz · Zulhelmi Ismail · A. K. M. Asif Iqbal · Irfan Ahmed Editors

Intelligent Manufacturing and Mechatronics Selected Articles from iM3F 2023, 7–8 August, Pekan, Malaysia

Editors Radhiyah Abd. Aziz Faculty of Manufacturing and Mechatronic Engineering Technology Universiti Malaysia Pahang Al-Sultan Abdullah Pekan, Pahang, Malaysia A. K. M. Asif Iqbal Department of Mechanical, Materials and Manufacturing Engineering University of Nottingham Ningbo China Ningbo, China

Zulhelmi Ismail Faculty of Manufacturing and Mechatronic Engineering Technology Universiti Malaysia Pahang Al-Sultan Abdullah Pekan, Pahang, Malaysia Irfan Ahmed Department of Physics Government College Balakot Khyber Pakhtunkhwa, Pakistan

ISSN 2662-3161 ISSN 2662-317X (electronic) Springer Proceedings in Materials ISBN 978-981-99-9847-0 ISBN 978-981-99-9848-7 (eBook) https://doi.org/10.1007/978-981-99-9848-7 © The Editor(s) (if applicable) and The Author(s), under exclusive license to Springer Nature Singapore Pte Ltd. 2024 This work is subject to copyright. All rights are solely and exclusively licensed by the Publisher, whether the whole or part of the material is concerned, specifically the rights of translation, reprinting, reuse of illustrations, recitation, broadcasting, reproduction on microfilms or in any other physical way, and transmission or information storage and retrieval, electronic adaptation, computer software, or by similar or dissimilar methodology now known or hereafter developed. The use of general descriptive names, registered names, trademarks, service marks, etc. in this publication does not imply, even in the absence of a specific statement, that such names are exempt from the relevant protective laws and regulations and therefore free for general use. The publisher, the authors, and the editors are safe to assume that the advice and information in this book are believed to be true and accurate at the date of publication. Neither the publisher nor the authors or the editors give a warranty, expressed or implied, with respect to the material contained herein or for any errors or omissions that may have been made. The publisher remains neutral with regard to jurisdictional claims in published maps and institutional affiliations. This Springer imprint is published by the registered company Springer Nature Singapore Pte Ltd. The registered company address is: 152 Beach Road, #21-01/04 Gateway East, Singapore 189721, Singapore Paper in this product is recyclable.

Preface

The fourth edition forum of the Innovative Manufacturing, Mechatronics and Materials Forum 2023 (iM3F 2023) organized by Universiti Malaysia Pahang Al-Sultan Abdullah through its Faculty of Manufacturing and Mechatronic Engineering Technology was held on 7 and 8 August 2023. The main field focuses on Manufacturing, Mechatronics as well as Materials. About 95 submissions were received during iM3F 2023 and were reviewed in a single-blind manner, and 48 papers were advocated by the reviewers to be published in this Springer Proceedings of Materials. The editors would like to express their gratitude to all the authors who submitted their papers. The paper published in this proceeding has been thoroughly reviewed by the appointed technical review committee which consists of various experts in the field of materials and manufacturing engineering. The conference had brought a new outlook on cutting-edge issues shared through keynote speeches by Assoc. Prof. Ir. Dr. Haji Nik Mohd Zuki Nik Mohamed, Prof. Eng Hwa Yap and Prof. Gian Antonio Susto. Finally, the editors hope that readers find this volume informative as we thank Springer Proceedings in Materials for undertaking this volume publication. We also would like to thank the conference organization staff and the international program committees’ members for their hard work. Pekan, Pahang, Malaysia November 2022

Radhiyah Abd. Aziz Zulhelmi Ismail A. K. M. Asif Iqbal Irfan Ahmed

v

Contents

Manufacturing Friction Welding Analysis: The Impact of Coolant Variation on Hardness and Tensile Strength of ST 37 Carbon Steel and SS 304 Stainless Steel . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . Amri Abdulah, Apang Djafar Shieddique, Dede Ardi Rajab, Choirul Anwar, Ridwan Nurhasan, Sukarman Sukarman, and Khoirudin Khoirudin The Implementation of the Single Perturbation Load Approach to Axially-Compressed Stiffened-Stringer Cylinder . . . . . . . . . . . . . . . . . . . Mohd Shahrom Ismail, Farhah Nadhirah Nordin, Chi Hieu Le, Ho Quang Nguyen, and Jamaluddin Mahmud Enhancing the Energy Efficiency of Heat Exchanger by Using Double Helical Coil in Shell and Tube Heat Exchanger: An Experimental Study . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . K. Hasham, M. W. Muhieldeen, S. Manzoor, and S. G. Solanki Effect of Wobbling Loops with Laser Welding Characteristics to the Shear Strength of Cu/Al Lap Joints for Battery Applications . . . . . M. N. Jamaludin, M. M. Quazi, M. F. M. Yusoff, Mohammadamin Ezazi, and Zawani Ismail Power System Generation: Current Trend Towards Sustainable Energy Storage Systems . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . Mohd Najib Razali, Mohd Sabri Mahmud, Syahirah Syazwani Mohd Tarmizi, and Mohd Khairul Nizam Mohd Zuhan An Integrated TOPSIS Model with Exponential Intuitionistic Entropy Measure for Multi-Attribute Decision-Making (MADM) . . . . . . Omar Ayasrah, Faiz Mohd Turan, and Sheikh Muhammad Hafiz Fahami

3

13

25

37

47

59

vii

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Contents

Enhancing MIG Weld Bead Geometry in Hot Rolled Carbon Steel Through Response Surface Methods Optimization . . . . . . . . . . . . . . . . . . . . Junita Mohd Said and Faiz Mohd Turan Current and Future Challenges of Hybrid Electrochemical-Mechanical Machining Process for Microand Nano-Manufacturing . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . Ahmad Shahir Jamaludin, Mohd Nizar Mhd Razali, Nurul Nadia Nor Hamran, Mohd Zairulnizam Mohd Zawawi, and Mohd Amran Md Ali Application of Activity-Based Costing and Time-Driven Activity-Based Costing for Kitchen Cabin . . . . . . . . . . . . . . . . . . . . . . . . . . . Intan Noralisya Mohd Yusoff, Mohd Yazid Abu, Sri Nur Areena Mohd Zaini, Wan Zuki Azman Wan Muhamad, Faizir Ramlie, Nolia Harudin, and Emelia Sari

71

81

91

Optimization of Surface Roughness on Duplex Stainless Steel in Dry Milling . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 103 Nurul Hidayah Razak and Mohammad Rizal Md Ali Ultrasonic Shot Peening Advancements and Their Impact on Alloys Microstructure Behavior: A Concise Review . . . . . . . . . . . . . . . . 113 Aina Najwa Azmi, Muhammad Syamim Mazlan, and Mohamad Rusydi Mohamad Yasin Current Developments and Future Prospects in Vehicle Tire Technologies: A Review . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 125 Ahmad Noor Syukri Zainal Abidin, Ahmad Shahir Jamaludin, Abdul Nasir, Amirul Hakim Sufian, and Ainur Munira Rosli Experimental of Hot Machining for Stainless Steel 316L Cutting Process . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 135 Nur Cholis, M. A. H. Yusoff, Syh K. Lim, and Ahmad R. Yusoff Enhancing Operational Excellence of Wood and Furniture Manufacturing Industry in Malaysia: The Role of Lean Culture as a Generative Mechanism . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 145 Mohamad Zamir Haszainul, Azim Azuan Osman, Khairunnisa Abdul Aziz, Syed Radzi Rahamaddulla, and Ahmad Nazif Noor Kamar The Effects of Nitrogen-Purged Thermal Debinding and Post-sintering Parameters on Metal Injection Moulded Pulverised Aluminium Alloy Swarf Binded with 100 Vol% of Palm Stearin . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 161 Sarah B. Yussoff, N. H. Mohamad Nor, H. Husain, and J. B. Saedon

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ix

Hybrid Machining: A Review on Recent Progress . . . . . . . . . . . . . . . . . . . . 173 N. N. Nor Hamran, J. A. Ghani, R. Ramli, and W. M. F. Wan Mahmood Sustainable Manufacturing Practices in the Sports Industry: A Review of Biodegradable Polymers for Sports Equipment . . . . . . . . . . . 187 Mohd Nizar Mhd Razali, Nurul Hasya Md Kamil, Ainur Munira Rosli, Amirul Hakim Sufian, and Teo Chong Yaw Orthogonal Cutting Performance of Vegetable-Based Lubricants via Minimum Quantity Lubrication Technique on AISI 316L . . . . . . . . . . 199 Amiril Sahab Abdul Sani, Zubaidah Zamri, Shahandzir Baharom, Mugilan Ganesan, and Norfazillah Talib Prediction of Real Contact Area on Curvature Region in Hot Stamping Process of AA7075 Aluminium Sheet . . . . . . . . . . . . . . . . . . . . . . . 211 Muhammad Amir Iqbal Jefry, Mohamad Farid Mohamad Sharif, Wahaizad Safiei, and Suraya Sulaiman Formulation of Grease for Industrial Applications . . . . . . . . . . . . . . . . . . . . 221 Mohd Najib Razali, Nasreldeen Ishag Obi, A. R. Muhammad Haziq, A. Azharul Aiman, M. S. Muhammad Arif Zakaria, and Najmuddin Mohd Ramli Materials Effects of pH on Grain Size and Structure of ZnO Nanoparticle Synthesized via Sol–Gel Method for Enhanced Thermoelectric Materials . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 233 Suraya Sulaiman, Tuan Muhammad Tuan Zahrin, Nadhrah Md Yatim, Mohd Faizul Mohd Sabri, and Mohamad Farid Mohamad Sharif Effect of Different Shape ZnO Nanoparticles on the Thermal Conductivity of ZnO Nanofluids . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 243 Tengku Nur Azza Tengku Ahmad Faizal, Radhiyah Abd Aziz, and Suraya Sulaiman Carbon Nanotube-Reinforced Polymer Composites for Biomedical Applications . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 255 Mohd Nizar Mhd Razali, Nurul Najwa Ruzlan, and Amirul Hakim Sufian Utilization of Coal Bottom Ash as Lightweight Aggregate in Concrete Production: A Review . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 265 Mohammad I. Al Biajawi, Rahimah Embong, Adli Hilmi Azmi, and Norasyikin Ismail Role of Nanomaterials in Improving Pozzolanic Properties of Blended Cement: A Review . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 275 Haneen Abdel-Jabbar, Rahimah Embong, and Mohammad I. AlBiajawi

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A Comparative Study of Conventional and Hybrid Nanofluids Performance in Machining Processes . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 287 Norasilah Karumdin, Ahmad Shahir Jamaludin, Mohamad Rusydi Mohamad Yasin, Nurul Nadia Nor Hamran, and Mohd Amran Md Ali Influences of Various Particle Sizes of Coal Bottom Ash as Supplementary Cementitious Material on the Pozzolanic Properties . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 297 Mohammad I. Al Biajawi, Rahimah Embong, Andri Kusbiantoro, and Haneen Abd Aljabbar Optimizing DC Alloy Properties: Impact of T6 Heat Treatment at High Solution Temperatures on β-AlFeSi Phase Transformation . . . . . 309 Mohamad Rusydi Mohamad Yasin, Muhammad Syamim Mazlan, and Nurul Nadia Nor Hamran Fracture Behaviour of Zirconia-Reinforced Lithium Silicate Glass–Ceramic Composite . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 319 Afifah Z. Juri, Animesh K. Basak, and Ling Yin Characterisation of the Physico-Chemical Properties of Emulsion Polymerised Poly(N-isopropylacrylamide) . . . . . . . . . . . . . . . . . . . . . . . . . . . 327 Ernest Hsin Nam Yong, Kim Yeow Tshai, Ai Bao Chai, Siew Shee Lim, Ing Kong, and Eng Hwa Yap Synergistic Effect of Electrolyte and Electrode in Nickel Cadmium Aging Battery Performances . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 339 Mohd Najib Razali, Mohd Sabri Mahmud, Syahirah Syazwani Mohd Tarmizi, and Mohd Khairul Nizam Mohd Zuhan Behaviour of Palm Oil Fuel Ash (POFA) as Partial Material Replacement in Oil Palm Shell (OPS) Reinforced Concrete Beam . . . . . . 351 Sharifah Syed Mohsin, Mohd Asmawi Md Desa, Khairunisa Muthusamy, Nur Farhayu Ariffin, Fadzil Mat Yahaya, and Saffuan Wan Ahmad Crash Performance of Automotive Bio-Composite Crash Box Using Finite Element Analysis . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 361 S. Y. Soh, C. S. Hassan, M. F. M. Nazer, A. R. Abd Hamid, L. J. Yu, N. F. Abdullah, N. Abdul Aziz, and R. A. Ilyas The Tribological Performance of Nano-Activated Carbon as Solid Additives in Modified Calophyllum Inophyllum Based-Metalworking Fluid . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 375 Zubaidah Zamri, Amiril Sahab Abdul Sani, Radhiyah Abd Aziz, Ainaa Mardhiah Sabri, and Norfazillah Talib

Contents

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Formulation of NSF H2 Food-Grade Grease from Vegetable-Base Oils . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 385 Mohd Najib Razali, Nur Syahirah Juhari, Nur Kholis Zulkifli, Najmuddin Mohd Ramli, and Mohd Khairul Nizam Mohd Zuhan Multiple Exciton Generation in MoS2 Nanostructures: A Density Functional Theory Study . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 397 Nur Hidayati Ain Natasha Makimin, Saifful Kamaluddin Muzakir, Nur Farha Shaafi, Muhammad Zamzuri Abdul Kadir, and Ruziana Mohamed Relationship Between Strength Development and Porosity of Epoxy-Based Mortar . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 407 Nur Farhayu Ariffin, Sharifah Maszura Syed Mohsin, Khairunisa Muthusamy, Fadzil Mat Yahaya, and Saffuan Wan Ahmad Modification of Cement Brick’s Properties Using Recyclable Paper Egg Tray . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 417 S. Surol, M. Y. Chow, A. R. Abd Hamid, D. Syamsunur, J. L. Ng, H. Jusoh, H. K. Lehl, N. F. Abdullah, E. E. Hussin, and N. I. F. Md Noh Performance Test of Emulsifiers for Bitumen Emulsion Mixture . . . . . . . 429 Mohd Najib Razali, Hana Syakirah Md Hadun, Abdurahman Hamid Nour, Najmuddin Mohd Ramli, and Mohd Khairul Nizam Mohd Zuhan Tensile Properties and Potential Applications of Leucaena-Silicone Biocomposite . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 441 Muhammad Hamizan Hidzer, Abdul Hakim Abdullah, Wan Mohd Nazri Wan Abdul Rahman, Fazlina Ahmat Ruslan, and Jamaluddin Mahmud Enhancing Water-Based Mud Properties with Sodium Lignosulfonate Polymer and Silicon Dioxide Nanoparticles: A Study on Interfacial Tension and Aging Behavior . . . . . . . . . . . . . . . . . . . 451 Norida Ridzuan, Chung King Ling, and Ahmad Syahmi Tajarazhar Effect of Heat Treatment on Hardness and Microstructure of Titanium Alloy (Ti6Al4V) via Laser Powder Bed Fusion (LPBF) . . . . . 469 Farhana Mohd Foudzi, Abu Bakar Sulong, Norhamidi Muhamad, Nabilah Afiqah Mohd Radzuan, Intan Fadhlina Mohamed, Fathin Iliana Jamhari, Minhalina Ahmad Buhairi, Ngoi Hui Lin, Lai Yu Hung, Chun Chuan Chia, and Kim Seah Tan

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Contents

Effect of Curing Regimes Towards Carbonation Resistance of Green Lightweight Aggregate Concrete Containing POFA as Partial Cement Replacement . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 479 Nur Azzimah Zamri, Khairunisa Muthusamy, Mohd Hanafi Hashim, Hamizah Mokhtar, and Muhammad Nazrin Akmal Ahmad Zawawi Advancements in 1D Nanostructure-Enhanced Carbon/carbon Composites for Aerospace Structures . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 487 Ahmad Shahir Jamaludin, Ainur Munira Rosli, Mohd Zairulnizam Mohd Zawawi, Ismayuzri Ishak, and Roshaliza Hamidon The Potential of Nanomaterials for Improving Tire Rolling Resistance . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 497 Mohd Nizar Mhd Razali, Ahmad Noor Syukri Zainal Abidin, Mohamad Rusydi Mohamad Yasin, Amirul Hakim Sufian, and Nurul Nadia Nor Hamran Effect of Doping Nickel/Cobalt Ions on Structural, Optical, Morphological and Photocatalytic Efficiency of Zinc Oxide . . . . . . . . . . . . 509 Ain Nor Annisa Hussin, Nurul Fatihah Norapandi, Nurjannah Salim, and Nurul Huda Abu Bakar Properties of Kenaf Fibre Filled with Natural Rubber/ Thermoplastic Polyurethane Composites . . . . . . . . . . . . . . . . . . . . . . . . . . . . 521 Nur Amirah Ayuni Jamaludin, Nurjannah Salim, Nurul Huda Abu Bakar, and Rasidi Roslan State-of-the-Art Developments and Perspectives on Multifunctional Magnetic Soft Composites (MMSCs) . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 533 Ahmad Shahir Jamaludin, Nurul Najwa, Mohd Zairulnizam Mohd Zawawi, Ahmad Rosli Abdul Manaf, and Roshaliza Hamidon

Manufacturing

Friction Welding Analysis: The Impact of Coolant Variation on Hardness and Tensile Strength of ST 37 Carbon Steel and SS 304 Stainless Steel Amri Abdulah , Apang Djafar Shieddique , Dede Ardi Rajab , Choirul Anwar , Ridwan Nurhasan , Sukarman Sukarman , and Khoirudin Khoirudin

Abstract Friction welding is a method of joining solid objects that combines rotation rate and pressure between two workpieces. The variables of rotating speed, friction duration, and pressure play crucial roles in determining the quality and results of the welding process. This research focuses on welding different materials using ST 37 steel and Stainless Steel 304, with parameters set at a pressure of 70 Psi, rotational speed of 2300 rpm, and friction time of 60 s while varying the coolant. The workpiece is quenched with different cooling liquids, namely oil, air, and water, to know its effect on the mechanical properties of welding results, such as the hardness and tensile strength of the material after the welding process. The study found that the cooling fluids used in the friction welding method significantly affect the mechanical properties of the workpiece. The highest hardness result of 82.58 HRB was found in the water-cooling liquid variation at the weld area, while the lowest hardness of 81.27 HRB was found in the oil-cooling liquid variation. Similarly, the watercooling liquid variation had the highest tensile strength of 711.17 N/mm2 , while the oil-cooling liquid variation had the lowest tensile strength of 364.13 N/mm2 . From these results, the best cooling process is using water media for friction welding different materials between ST 37 carbon steel and Stainless Steel 304. Keywords Friction welding · Coolant · ST 37 · SS 304 · Hardness · Tensile

A. Abdulah (B) · A. D. Shieddique · D. A. Rajab · C. Anwar · R. Nurhasan Sekolah Tinggi Teknologi Wastukancana, Purwakarta, Indonesia e-mail: [email protected] S. Sukarman · K. Khoirudin Universitas Buana Perjuangan, Karawang, Indonesia A. Abdulah · S. Sukarman · K. Khoirudin Universitas Sebelas Maret, Surakarta, Indonesia © The Author(s), under exclusive license to Springer Nature Singapore Pte Ltd. 2024 R. Abd. Aziz et al. (eds.), Intelligent Manufacturing and Mechatronics, Springer Proceedings in Materials 40, https://doi.org/10.1007/978-981-99-9848-7_1

3

4

A. Abdulah et al.

1 Introduction For several decades, welding technology has been a widely-used metal joining process in machinery construction and daily life. The material being joined and the intended use determine the various welding methods. Friction stir welding (FSW) is a welding technique that involves the application of compressive force to generate heat from the friction between the two end surfaces of the workpieces. The axial pressure between the rotating and stationary materials produces heat. FSW typically does not require filler, flux, or shielding gas. Extensive research has been conducted on Friction Stir Welding (FSW). It has been found that the effects of component properties on the quality of the joint are significant, as reported by Aritoshi and Okita [6]. The effect of rotation speed on the frictional properties of welded AISI-304L joined to 4340 steel was investigated by Özdemir et al. [8]. The findings revealed that as rotation speed increased, the thickness of the plastic deformed zone at the interface decreased. Ates et al. [3] investigated the friction properties of superalloy MA956 in order to determine the optimum friction pressure. Friction welding is an effective method for joining mild or low-strength alloy steel with austenitic stainless steel, as Ananthapadmanaban et al. [2] reported. Similarly, Satyanarayana et al. [12] reported that the technique produced positive results when performing austenitic-ferritic stainless-steel splicing. Li [5] say that using electric resistance heat-assisted friction welding reduces joining time. Joining high-strength and ultrahigh-strength steels is of particular interest, as demonstrated in the work by Sahin [10]. Additionally, researchers have explored the joining of other types of steel, including hardened processes Rajamani et al. [9] and thermochemically refined steels Mitelea and Craciunescu [7]. These studies significantly contribute to understanding welding technologies and techniques suitable for a wide range of steel materials, each with unique properties and challenges. Carbon steel can be immediately cooled after welding with oil, air, or water to improve its mechanical properties through heat treatment. Oil can be used as a lubricant as well as a cooling medium. However, the specimen’s viscosity and carbon content may result in the formation of carbon membranes. In contrast, air cooling is commonly used in heating processes that require slow cooling, such as normalizing. It is accomplished by slowing the air entering the cooling chamber. When air is used to cool the material, it can form crystals and potentially bond with other elements in the air. The cooling process in the open air also allows for oxygen oxidation. Water, the oldest and cheapest cooling medium, has a very high cooling ability. However, its use comes with a disadvantage: the cooling rate in the martensite formation temperature region is very high, leading to stress caused by transformation and temperature differences. Consequently, cracking during quenching may occur. Despite this drawback, water is commonly employed for cooling steel with lower hardness, such as carbon steel, due to its exceptional cooling capacity. The conventional friction stir welding method, according to DebRoy and Bhadeshia [4]. Remains the ideal solution for implementing industrial applications involving such materials. However, expanding friction stir welding to harder alloys necessitates the development of cost-effective,

Friction Welding Analysis: The Impact of Coolant Variation …

5

wear-resistant, dependable tools with adequate tool life. Akram et al. [1] studied various welds between austenitic stainless steel and ferritic creep-resistant steel. The welds experienced premature failure due to significant differences in their thermal expansion coefficients. The investigation revealed that the underlying cause of the damage mechanism was cavity expansion, resulting from the impact of diffusion creep and the law of power. This study aims to investigate the effect of various cooling media, namely oil, water, and air, on the welding results of carbon steel using the friction stir welding method. The friction stir welding process was conducted with specific input parameters, including a pressure of 70 psi, a speed of 2300 rpm, and a pressing time of 60 s. The outcomes of interest were the welded material’s tensile strength and hardness values. Furthermore, the study involved friction stir welding research using different steel combinations, such as ST 37 Carbon Steel and SS 304 Stainless Steel.

2 Preparation of Material The specimens used in this study are ST 37 Steel and SS 304. Before use, the materials are thoroughly tested for chemical composition to meet the study’s predetermined requirements. The L01557T0028 Spectrometer Test Apparatus was used for the checks. Table 1 listed the chemical composition of ST37 and SUS 304. Table.1 shows that ST37 Steel is a low-carbon steel with soft properties and relatively weak strength compared to medium-carbon steel and high-carbon steel. However, it exhibits excellent ductile and tough properties. Due to these properties, low carbon steel finds application as steel plates or fins in vehicle body materials, bridge construction, bolts, and pipe materials. It has a tensile strength of 37 kg/ mm2 and is named after the DIN standard. On the other hand, the 304 stainless steel sample is an alloy steel containing 16.8% Cr, which imparts corrosion resistance due to the formation of chromium oxide (Cr2 O3 ) film. Stainless steel is known for its resistance to corrosion and oxidation. It is achieved by adding elements such as nickel, manganese, molybdenum, nitrogen, and others to carbon iron alloys, significantly affecting material properties. AISI 304 stainless steel is widely used in various industries, including chemical, petrochemical, food & beverage processing, pharmaceutical, cryogenic, and heat exchangers. The following step is the creation of specimens. ST 37 and 304 Stainless Steel materials are formed into cylindrical shapes with a diameter of 12.5 mm for hardness and tensile tests during the specimen preparation stage. The appearance of the research specimens is depicted in Fig. 1 Material cutting and forming follow the ASTM E8 standard, ensuring consistency and accuracy in the specimen preparation process.

6 Table 1 Chemical composition of ST37 and 304 stainless steel

A. Abdulah et al.

No.

Element

Composition (%) ST37

SS 304

1

Fe

–

72.1

2

C

0.37

0.884

3

Si

0.37

0.449

4

Mn

0.008

1.11

5

P

0.04

0.0379

6

S

0.035

0.0428

7

Cr

–

16.8

8

Mo

–

0.065

9

Ni

–

8

10

Al

–

0.0603

11

Co

–

0.111

12

Cu

–

1.05

13

Nb

–

0.0113

14

Ti

–

< 0.0050

15

V

–

0.0655

16

W

–

0.05

17

Pb

–

< 0.0150

18

Sn

–

< 0.0020

19

B

–

0.003

Fig. 1 Sample for friction stir welding with dissimilar materials

Friction Welding Analysis: The Impact of Coolant Variation …

7

3 Methods Oil, air, and water are the cooling fluid media used as a coolant in the process of joining two different materials through friction stir welding. For cooling with oil and water, the workpiece is dipped in the respective medium after welding, while cooling with air involves storing the workpiece at room temperature until it naturally cools down after welding. The parameters for the friction welding process in all samples are as follows: (a) Machine speed = 2300 Rpm, (b) Friction time = 60 s, and (c) Pressing force = 70 Psi. The friction welding machine used for preparation uses a lathe equipped with a hydraulic press on the other side of the workpiece. Nine samples are prepared, and each test sample has the same size according to ASTM E8 standards. These samples are essential for the research process in the next stage, which involves tensile and hardness testing (Fig. 2).

3.1 Tensile Testing The tensile test followed the ASTM E8 Standard using a 60-ton capacity Hung-ta HT 2101 S tensile testing machine. The tensile test aims to determine a material’s strength by applying a tensile force or stress to it. The real external stress or extension of the test object’s axis is used as the tensile stress during the test. The objective is to steadily increase the material’s elongation until it eventually breaks, thereby determining its tensile value. During the tensile test, a straight tensile load is applied to the material, and the line of force must coincide with the material’s axis line to accurately calculate its tensile strength. However, bending forces may occur if the tensile force is applied at an angle, which could affect the test results.

Fig. 2 Samples after joining using friction stir welding

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3.2 Hardness Testing Hardness testing in this study using the Future Tech Rockwell Hardness Tester Series (LC 200 RB testing) refers to the ASTM E18 test standard. Hardness testing is used to measure a material’s hardness; it is also a significant aspect of assessing the material’s mechanical properties. Hardness testing can be done in three different ways. Rockwell (HR/RHN), Brinell (HB/BHN), and Vickers (HV/VHN). Each of the three hardness testing procedures will leave a mark of emphasis that may be utilized to determine how hard the test material is. The tougher the substance, the smaller the indentation marks discovered on the test material. The hardness of a substance is a measure of its resistance to localized plastic deformation. The hard test is the most useful since it can quickly determine the mechanical properties of a material. Although measurements are only taken at one spot or area, its hardness value is accurate enough to state a material’s strength. As a result, the material is easily characterized as ductile or brittle.

4 Result and Discussion Tensile testing was performed using a 60-tonne capacity Universal Tensile Machine. The tests followed the ASTM E8 standard test piece geometry (see Fig. 1). The measured tensile strength ranged from 364 to 711 N/mm2 , depending on the cooling media used. The fracture occurred in the weld area in sample 1, which underwent tensile testing with oil and air-cooling media. However, for water cooling, the fracture in the test sample occurred in the Heat Affected Zone (HAZ) area on the ST37 side. In Fig. 3 a fracture is shown in the weld area, and this material was cooled using oil after welding. Similarly, in Fig. 4 the fracture occurs in the weld area, and the cooling media used was air. In Fig. 5 fractures occur between the Heat Affected Zone (HAZ) and the base material, and the cooling process after welding utilized water. From the observations of the three pictures and following the results in Table 2, it can be deduced that water’s cooling process resulted in a higher tensile test value compared to oil or air as cooling media. Regarding hardness testing analysis, further details or findings are needed to provide specific conclusions based on the hardness results (Table 3). In this study, hardness testing was performed at various positions on the welded samples, including the base metal (ST37 side), HAZ (ST37 side) on the weld, HAZ (SS304 side), and base metal (SS304 side). The Rockwell hardness tester was utilized, and hardness measurements were conducted following the ASTM E18 standard (Figs. 6 and 7). All samples exhibited a similar hardness profile, with a slight decrease in hardness observed in the HAZ on the ST37 side, which can be attributed to the effect of the base metal. This decrease in hardness is likely due to the recrystallization process occurring in the HAZ (ST37 side). When friction welding austenitic stainless steel,

Friction Welding Analysis: The Impact of Coolant Variation …

9

Fig. 3 Specimen 1 fractured at weld joint (quenching use oil)

Fig. 4 Specimen 2 fractured at the weld joint (quenching use air)

Fig. 5 Specimen 3 broke out of connection (quenching use water) Table 2 Tensile test results Coolant

Spindle speed (Rpm)

Friction time (s)

Pressure (Psi)

Diameter (mm)

Initial area (mm2 )

Maximum Tensile tensile load strength (N) (N/mm2 )

Oil

2300

60

70

12,44

121,54

44,286

364,13

Air

2300

60

70

12,55

123,70

46,942

379,48

Water

2300

60

70

12,48

122,32

86,990

711,17

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Table 3 Hardness test result Test point

Position

Coolant

Major load (Kgf)

Time (s)

1

ST 37

Oil

100

15

93.58

Air

100

15

93.68

Water

100

15

93.72

Oil

100

15

80.42

Air

100

15

81.44

Water

100

15

81.27

Oil

100

15

81.27

Air

100

15

81.42

Water

100

15

82.58

Oil

100

15

81.88

Air

100

15

82.58

Water

100

15

82.86

Oil

150

15

104.91

Air

150

15

104.89

Water

150

15

105.50

2

3

4

5

HAZ ST 37

Welding

HAZ stainless steel

Stainless steel

Hardness value (HRB)

Fig. 6 Check points in hardness testing

a drop in hardness within the joint interface zone is typically observed, which can be attributed to the non-hardenable nature of AISI 304 steel via heat treatment [11]. The friction and oxidation processes during welding are likely responsible for the increase in hardness at the welding contact. Among all samples, the HAZ on the SS304 side recorded the highest hardness values, indicating that the applied forging pressure had the most significant workhardening effect. The presence of chromium and nickel carbide, combined with the HAZ’s thermal history, contributed to the increased hardness on the HAZ (SS304 side) under the same pressure. These factors likely contributed to the higher hardness levels observed in the HAZ on the SS304 side.

Friction Welding Analysis: The Impact of Coolant Variation …

11

Fig. 7 Graph of hardness at weld area and tensile strength of the materials

5 Conclusion The analysis of coolant variations (oil, air, and water) in the friction welding process with different materials, ST37 and SS304, led to distinct hardness values. In the welding area, the hardness values were 81.27 HRB (oil), 81.42 HRB (air), and 82.58 HRB (water). For the ST37 area, the values were 93.58 HRB (oil), 93.68 HRB (air), and 93.72 HRB (water). In the Heat Affected Zone (HAZ) of ST37, the values were 80.42 HRB (oil), 81.27 HRB (water), and 81.44 HRB (air). In the HAZ of Stainless Steel, the values were 81.88 HRB (oil), 82.58 HRB (air), and 82.86 HRB (water). In the Stainless-Steel area with a load of 150 kg, the values were 104.89 HRB (air), 104.91 HRB (oil), and 105.50 HRB (water). Moreover, the tensile test results showed that all specimens’ highest maximum stress value occurred in water coolant variation at 711.17 N/mm2 . In comparison, the lowest stress value was observed in oil coolant variation at 364.13 N/mm2 . The findings demonstrated that water coolant variation generally resulted in higher hardness values and maximum stress in the tensile tests compared to oil and air coolant variations.

References 1. Akram J (2017) Creep behavior of dissimilar metal weld joints between P91 and AISI 304. Mater Sci Eng, A 688:396–406 2. Ananthapadmanaban D (2009) A study of mechanical properties of friction welded mild steel to stainless steel joints. Mater Des 30(7):2642–2646 3. Ates H (2007) Effect of friction pressure on the properties of friction welded MA956 iron-based superalloy. Mater Des 28(3):948–953 4. DebRoy T (2010) Friction stir welding of dissimilar alloys—a perspective. Sci Technol Weld Joining 15(4):266–270

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5. Li W (2009) Y: Characterizations of 21–4N to 4Cr9Si2 stainless steel dissimilar joint bonded by electric-resistance-heat-aided friction welding. Mater Des 30(10):4230–4235 6. Aritoshi M (2003) Friction welding of dissimilar metals. Weld Int 17(4):271–275 7. Mitelea I (2010) Parameter influence on friction welding of dissimilar surface-carburized/ volume-hardened alloyed steels. Mater Des 31(4):2181–2186 8. Özdemir N (2007) Effect of rotational speed on the interface properties of friction-welded AISI 304L to 4340 steel. Mater Des 28(1):301–307 9. Rajamani GP (1992) Parameter optimization and properties of friction welded quenched and tempered steel friction welding of high-strength steel offers a joint with good properties and a minimal HAZ. Welding Res Suppl 225–230 10. Sahin M (2005) Joining with friction welding of high-speed steel and medium-carbon steel. J Mater Process Technol 168(2):202–210 11. Sahin M (2007) Evaluation of the joint-interface properties of austenitic-stainless steels (AISI 304) joined by friction welding. Mater Des 28(7):2244–2250 12. Satyanarayana VV (2005) Dissimilar metal friction welding of austenitic-ferritic stainless steels. J Mater Process Technol 160(2):128–137

The Implementation of the Single Perturbation Load Approach to Axially-Compressed Stiffened-Stringer Cylinder Mohd Shahrom Ismail , Farhah Nadhirah Nordin, Chi Hieu Le, Ho Quang Nguyen, and Jamaluddin Mahmud

Abstract This work study the influence of imperfections on axially compressed stiffened-stringer cylindrical shells for different geometries and materials that include aluminum and Carbon Fibre Reinforced Polymer (CFRP) using the finite element (FE) analysis. The imperfection technique called the single perturbation load approach (SPLA) is adopted. The verification analysis was performed with two cases reported in previous studies. Conversely, the parametric investigation was conducted focusing on the stiffener flange profile that varies its thickness and width. From the verification analyses SPLA demonstrated its attractive ability for designing imperfections in axially compressed aluminum stiffened cylindrical shells with fair agreement acquires. Finally, several design guidelines have been highlighted according to the parametric study and further deduced as imperfection sensitivity, buckling and postbuckling behaviour together with its collapse load and knockdown factor (KDF) of stringer stiffened cylindrical shells under axial compression primarily depend on the properties of shell and stiffeners themselves. Keywords Finite element analysis · Stiffened-stringer cylindrical shell · Knockdown factor · Post-buckling · Composite material · Structural imperfection

M. S. Ismail (B) Jabatan Kejuruteraan Mekanikal, Politeknik Sultan Salahuddin Abdul Aziz Shah, 40150 Shah Alam, Selangor, Malaysia e-mail: [email protected] F. N. Nordin · J. Mahmud School of Mechanical Engineering, College of Engineering, Universiti Teknologi MARA, 40450 Shah Alam, Selangor, Malaysia C. H. Le Faculty of Science and Engineering, University of Greenwich Kent, Gillingham, UK H. Q. Nguyen Institute of Engineering and Technology Thu Dau, Mot University Binh Duong, Thu Dau Mot, Vietnam © The Author(s), under exclusive license to Springer Nature Singapore Pte Ltd. 2024 R. Abd. Aziz et al. (eds.), Intelligent Manufacturing and Mechatronics, Springer Proceedings in Materials 40, https://doi.org/10.1007/978-981-99-9848-7_2

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1 Introduction Stiffened-stringer cylindrical shell structures are a common configuration that has been widely used in many structural applications mainly in the aircraft and aerospace industry. To date, there are demand made by most of the European aircraft industry to reduce the development and operating cost near to 20–50% in future [1]. Nowadays, the prediction of knockdown factor remains highly dependent on the empirical guideline from NASA SP-8007 [2] that uses the conservative lower bound curve. The approach stated in the guideline excessively led to conservative designs on estimating cylinder buckling load as highlighted by researchers [3–6]. The NASA SP8007 [2] also does not consider the full potential of materials on the knockdown factor [7]. In particular, Arbelo et al. [8] reported the use of NASA SP-8007 [2] in the design of the European Ariane-5 rocket launcher. Even though the rocket has an outstanding performance, the structural design seemed to be considered conservative, resulting in high costs in production and operation [6, 8]. The EU project DESICOS was launched in 2012 and is underway to propose a new design guideline for designing imperfections in composite launcher structures [8]. The relatively new method for designing an imperfection on axially compressed shell structures, namely the single perturbation load approach (SPLA) was proposed by Hühne et al. [6]. This method uses the influence of a single laterally applied load to the surface of the model to simulate the worst-case and realistic geometrical imperfection of typical structural models such as cylindrical shells. Most of the stiffened cylindrical shells are analyzed with the linear theory that gives fair agreement with experiment data [9]. However, this is limited by the configuration of closely spaced stringers as described by Krasovsky et al. [10]. Stiffened stringer cylinder shells are distinguished to be less imperfection sensitive compared to unstiffened ones as the imperfection is improved due to increased structural mass/ weight via stiffeners [11]. Moreover, stiffened cylinder’s structural efficiency and its imperfection sensitivity also can be associated with the design of the stiffener profile and its positions (i.e. inside/outside) around the cylinder circumferential [11, 12]. Next, it should be noted that cylinder shells with externally reinforced stiffeners are more imperfection sensitive rather than internal ones [13]. Despite the excellent performance achieved by DESICOS on employed SPLA technique, most of the works are still pre-dominantly focusing on unstiffened cylinders [14–16], conical shells [17] and sandwich structures [18]. Whereas there is still a lack of data and effective guidelines reported for stiffened cylinders through SPLA or any independent or governed institutions. This study is unique in that there have been fewer or no studies on this topic.

The Implementation of the Single Perturbation Load Approach …

15

2 Materials and Methods 2.1 Finite Element Modelling and Material Properties After performing convergence tests, about 12,660 and more than 20,000 four-node doubly curved shell elements with reduced integration and hourglass control were found to be suitable to model the aluminium and composite cylinders. The element characteristics are represented as the S4R type of shell element. All the analyses were carried out using a finite element software package of ABAQUS. The schematic of the axially compressed cylindrical shell is shown in Fig. 1a. As shown in Fig. 1a, displacement and rotation constraints are applied on one end of the cylindrical shell, and the load-controlled displacement ΔU with slow quasi-static compression is applied on the other end to infuse instability of the cylinder. The stiffened cylinder dimensions and geometries used in this study refer to those experiment series conducted by Weller et al. [9] and Abramovich et al. [19]. Similar material of 7075-T6 aluminum alloy is also employed before performing the verification studies. The position of the stringer blade is located outside of the cylinder with R, h and L terms defined as cylinder radius, thickness and length. Further details Fig. 1 a Boundary condition of FE modelling by SPLA b details of L-shape stiffeners profile and its variables

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Table 1 Dimensions and geometrical properties of verified shells Shell

R (mm)

h (mm)

L (mm)

R/h

L/R

d (mm)

c (mm)

Y1A [19]

120.22

0.26

200

462

1.665

1.75

0.9

AS-1L [9]

120.6

0.241

182

500

1.41

0.751

1.06

* Aluminum-alloy

7075-T6 with E = 75 GPa and υ = 0.3

describe d and c as stringer width and height respectively. Overall the details of test articles configurations and material properties are presented in Table 1.

2.2 Stiffeners Profile Configurations: Parametric Flange Studies For parametric studies CFRP composite material is employed from Bisagni et al. [20]. The cylindrical shell is characterized by 36 stringers with an L-shaped stiffeners profile that is equally spaced in the circumferential direction. The employed stiffened cylinder radius and its walled thickness are designed to be 71.5 and 0.25 mm. Indeed, it should point out that the parametric variables are highly focused on the variation of flange configurations with details shown in Fig. 1b. At first, the flange is designed to be 0.5 and 4 mm in thickness and width in that order and set to be the baseline model. Then the flange is varied with dimensions of; thickness 0.75 mm and 1 mm with widths of 5 mm, 6 mm and 6.5 mm respectively. Altogether the CFRP properties with its ply-layups and flange variables were summarized in Table 2. It is worth mentioning that different layup stacking sequences are only applied for the case of varying flange thickness denoted as Tf1 = 0.5 mm, Tf2 = 0.75 mm Table 2 Material layups properties with flange geometric parameters Layups Walled

[45/− 45]

Web height

[0/90/90/0]

Flange

tf1 = [0/90/90/0] tf2 = [0/90/90/0/0/90] tf3 = [0/90/90/0/0/90/90/0/90/0/90/0]

tplies

0.125 mm

CFRP [20]

E11 = 52,000 MPa, E22 = 52,000 MPa, G12 = 2350 MPa, G13 = 2350 MPa, G23 = 2350 MPa, υ12 = 0.302

Fixed parameters

Variables parameters

R (mm)

twall (mm)

L (mm)

hweb (mm)

tweb (mm)

R/twall

tflange (mm)

wflange (mm)

71.5

0.25

100

4

0.5

286

0.5, 0.75, 1

4, 5, 6 6.5

The Implementation of the Single Perturbation Load Approach …

17

and Tf3 = 1 mm. However, for the case of varying the flange width consistent layups of Tf1 = 0.5 mm are used. It is worth pointing out that the stiffener web height is not varied accordingly like their other counterpart as a reason to minimize the presence of local skin buckling. Rationally the presence of local skin buckling is suspected to bring a strong effect on decreasing the stiffened cylinder collapse load.

2.3 Stiffeners Profile Configurations: Parametric Flange Studies According to the procedure outlined by Huhne et al. [6], as illustrated in Fig. 1a, initially a lateral perturbation load P0 is applied at the mid-section of the cylindrical shell skin to produce a single buckle as the worst imperfection mode. After the equilibrium state of the shell is reached, the pre-buckling quasi-static compressive load is applied to the cylindrical shell until it reaches an instability point. The postbuckling state of the cylindrical shell will begin at this instability point. In this study the load is governed in sequential manners firstly lateral perturbation load follows by compressive end-shortening.

3 Results and Discussions Prior to performing response analyses on the cylindrical shells, the sensitivity study was conducted to determine a suitable value for the artificial damping factor. It is known that too small a value of the artificial damping would possibly result in a singularity of the tangent stiffness matrix. Meanwhile, a large artificial damping value would lead to over-damped results. The responses of different artificial damping values are presented in Fig. 2a. It can be observed that the use of the damping factors c = 4e − 8 fails to reach the first local snap-through. This feature is associated with the singularity of the tangent stiffness matrix, resulting in no convergence problem. Meanwhile, a larger artificial damping value c = 4e − 6 seems to produce over-damped results. Thus, the artificial damping value c = 4e − 7 that produces a convergence result is chosen in this study. At least ten lateral perturbation loads, P0 were tested for each stiffened cylinder as illustrated in Fig. 2b. For example, taking a perturbation load P0 of 20 N and 10 N for case Y1A and AS-1L respectively leads to dented imperfection of eight times shell walled thickness. This level of imperfection has been considered to be the worst-case scenario for the stiffened shell. For both cases, the perturbation loads characters and tendency curves was observed to be quite similar. Figures 2c and d show the responses of collapse load and knockdown factor for Y1A and AS-1L models respectively using SPLA. It can be seen that the collapse load and knockdown factor reach their consistency once the perturbation loads P0

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Fig. 2 a Sensitivity studies b perturbation load in function of a/twall for Y1A model c SPLA estimation of collapse loads and d knockdown factors

are accomplished at 9 N and 5 N for Y1A and AS-1L models respectively. Moreover, this load leads to a dented imperfection amplitude, a/twall nearly 0.71–0.76 for both cylinders. Afterwards, a consistent response of collapse load is observed after surpassing the aforementioned perturbation loads and imperfection amplitudes. By comparing with experimental data obtained from Abramovich et al. [19] for the Y1A model, the SPLA overestimated the collapse load using 10%. At the same time, the SPLA underestimated Weller et al. [9] AS-1L model collapse load by 15%. Remarkably leads to estimating collapse load, PCollapse through SPLA to be 36.06 kN and 19.11 kN for Y1A and AS-1L models respectively. The present studies indicate that both stiffened cylindrical shells would undergo approximately half of the linear buckling load Peigen before reaching its structural load-carrying capacity through SPLA. In another way, this trend appeared to be similar to non-linear analysis for a perfect stiffened cylindrical shell evidently illustrated in Fig. 3a. Judging from this trend it is believed that the presence of a stiffened cylinder may present a relatively high structural imperfection comparable to unstiffened ones. The summarised results are presented in Table 3. Figure 3a shows the variation of compressive loads against cylinder endshortening under SPLA for the case of the baseline model. Interestingly it can be seen

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19

Fig. 3 Parametric results of (a) baseline model under SPLA (b) dissolution of local buckling by increasing the flange width with constant SPLA load of 5N (c) variation flange thickness (d) and width together with their collapse loads

Table 3 Summarized results of verification studies Shell

Peigen (kN)

P0 (N)

a/twall

Pcollapse (kN)

Pexperiment (kN)

KDF, ρ

Y1A [19]

60.7

9

0.76

36.06

32

0.59

AS-1L [9]

32.84

5

0.71

19.11

22.27

0.58

that the model exposes the effect of local buckling over the cylinder skin shell before reaching its global instability. On the other hand, the local buckling, Plocal buckling and collapse loads, PCollapse for the baseline model were found to be 31.2 kN and 42.6 kN. The results it illustrated that SPLA exhibits a weak or almost consistent effect on cylinder local buckling despite its great outcome on global buckling. Furthermore, SPLA demonstrated its competency in capturing the real buckling event without having a strong effect on the whole buckling process, especially with the influence of local buckling. Figure 3b clearly shows that the local buckling also increases subsequent to the changes in flange width. Nonetheless, the effect of local buckling is prohibited as

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M. S. Ismail et al.

the flange width is getting wider by over 50% from its original configuration. This circumstance is exemplified through the case of flange widths 6 and 6.5 mm. At the same time, it was found that no effect of local buckling is observed prior to the increment of flange thickness. In addition, further observation shows that most of the case with increasing flange thickness and some of the flange width carries an increasing load even after the shells exhibit their overall buckles. The results for all cases of flange profiles with their collapse loads are depicted in Figs. 3c and d. Overall the results show that the stiffened cylinder collapse loads increase as the corresponding flange thickness and widths increase. In detail by increasing the flange thickness, the consequence results are derived as follows as tflange1 and tflange2 to be 48.26 kN and 55.14 kN of collapse loads accordingly. In the meantime, for the case of increased flange width the collapse load, PCollapse also increases to 45.28 kN, 48.92 kN and 50.95 kN for wflange1 , wflange2 and wflange3 respectively. Among that, the local buckling load, Plocal buckling also found to increase as follows 41.2 kN and 47.7 kN consequently. Interestingly the effect of local buckling is found to become less prominent after the cylinder reaches its local snap-through at 10 N for 6 mm of flange width. In addition, a more noticeable increment of the highest collapse load attains in changes of the flange thickness of 1 mm. Evidently, the parametric results from the present SPLA suggested that the effect of imperfection amplitude and its sensitivity is weaker prior to the increment of the flange profile. This condition can be linked to the fact that the shell is getting stronger and less imperfection sensitive. Indeed, this finding is found to be consistent with what has been described by Shen et al. [21] in their previous study. Throughout the study several factors that regard the whole of the buckling event are described accordingly: • The presence of shell local buckling can be associated with the designed spacing between stiffeners and the stiffeners configuration itself. Yet it is worth noting that the design of the stiffeners area and its spacing between shells deserved careful judgement as it may permit enough space/area for the development of local skin/ area buckling. • The influence of local shell buckling may reduce the overall structural rigidity including its tension-compression, shear as well as compression and shear [10]. Figures 4a and b show the effect of different stacking sequences and stiffener fibre angles on shell collapse load. The results, confirm that there was no appreciable effect of changing the flange stacking sequence on stiffened cylinder collapse load [22]. A comparison results reveals to be almost identical for both stacking sequences to the baseline model. Apparently, changing the stiffener fibre angle presents a greater effect on the structural imperfection amplitude and collapse load accordingly. By comparing the collapse load determined through varying fibre angles with the baseline model, it remarks the difference to be nearly 5%.

The Implementation of the Single Perturbation Load Approach …

21

Fig. 4 Parametric results of a flange laminate stacking sequence b changing stiffener fiber orientation angle

4 Conclusion Imperfection analyses using SPLA on axially compressed aluminum and CFRP stiffened cylindrical shells through the finite element simulations were presented. From the verification analyses SPLA demonstrated its attractive ability for designing imperfections in axially compressed aluminum stiffened cylindrical shells with fair agreement acquired. Moreover, several design guidelines can be highlighted according to the parametric study and summarized as follows: • From the parametric results it illustrated that SPLA exhibits a weak effect on cylinder local buckling despite its great outcome on global buckling. The effect of local buckling is prohibited as the flange width is getting wider by over 50% from its original configuration. At the same time, it was found that no effect of local buckling is observed prior to the increment of flange thickness. • The parametric results from the present SPLA suggested that the effect of imperfection amplitude and its sensitivity is weaker prior to the increment of the flange profile. • Increased flange width is distinguished to be a more efficient way of improving stiffened cylindrical shell collapse load compared to its thickness. • There was no appreciable effect of changing the flange stacking sequence on stiffened cylinder collapse load while changing the stiffener fiber angle presents a greater effect on the structural imperfection amplitude and collapse load. • The stiffened cylinder shell experiences a decrease in knockdown factor by increasing both flange thickness and width. Acknowledgements The authors would like to express sincere gratitude to Politeknik Sultan Salahuddin Abdul Aziz Shah, Universiti Teknologi MARA and thank the Ministry of Higher Education, Malaysia, through the High Impact Research Grant.

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References 1. Degenhardt R, Castro SGP, Arbelo MA, Zimmerman R, Khakimova R, Kling A (2014) Future structural stability design for composite space and airframe structures. Thin-Walled Struct. 81:29–38 2. Weingarten VI, Seide P, Peterson JP (1968) Buckling of thin-walled circular cylinders. NASA SP-8007 Monograph 1(v2) 3. Arbocz J, Starnes JH Jr (2002) Future directions and challenges in shell stability analysis. Thin-Walled Struct. 40(9):729–754 4. Hilburger MW, Nemeth MP, Starnes JH (2006) Shell buckling design criteria based on manufacturing imperfection signatures. AIAA J 44(3):654–663 5. Degenhardt R, Kling A, Bethge A, Orf J, Kärger L, Zimmermann R, Rohwer K, Calvi A (2010) Investigations on imperfection sensitivity and deduction of improved knock-down factors for unstiffened CFRP cylindrical shells. Compos Struct 92(8):1939–1946 6. Hühne C, Rolfes R, Breitbach E, Teßmer J (2008) Robust design of composite cylindrical shells under axial compression—Simulation and validation. Thin-Walled Struct. 46(7–9):947–962 7. Arbelo MA, Zimmermann R, Castro SGP (2013) Comparison of new design guidelines for composite. In Ninth International conference on composite science and technology, vol 1, pp 96–111 8. Arbelo MA, Degenhardt R, Castro SGP, Zimmermann R (2014) Numerical characterization of imperfection sensitive composite structures. Compos Struct 108:295–303 9. Weller T (1971) Experimental studies on buckling of 7075-T6 Aluminium alloy integrally stringer-stiffened shells. Haifa, Israel 10. Krasovsky VL, Kostyrko VV (2007) Experimental studying of buckling of stringer cylindrical shells under axial compression. Thin-Walled Struct. 45(10–11):877–882 11. Hilburger MW (2007) Developing the next generation shell buckling design factors and technologies, pp 1–15 12. Rahimi GH, Zandi M, Rasouli SF (2013) Analysis of the effect of stiffener profile on buckling strength in composite isogrid stiffened shell under axial loading. Aerosp Sci Technol 24(1):198– 203 13. Andrianov IV, Verbonol VM, Awrejcewicz J (2006) Buckling analysis of discretely stringerstiffened cylindrical shells. Int J Mech Sci 48(12):1505–1515 14. Castro SGP, Zimmermann R, Arbelo MA, Khakimova R, Hilburger MW, Degenhardt R (2014) Geometric imperfections and lower-bound methods used to calculate knock-down factors for axially compressed composite cylindrical shells. Thin-Walled Struct. 74:118–132 15. Castro SGP, Zimmermann R, Arbelo MA, Degenhardt R (2013) Exploring the constancy of the global buckling load after a critical geometric imperfection level in thin-walled cylindrical shells for less conservative knock-down factors. Thin-Walled Struct. 72:76–87 16. Castro SGP, Zimmermann R, Arbelo MA, Degenhardt R (2013) The single perturbation load approach compared with linear buckling mode-shaped, geometric dimple and measured imperfections for the buckling of cylindrical shells. Thin Walled Struct 1–14 17. Khakimova R, Warren CJ, Zimmermann R, Castro SGP, Arbelo MA, Degenhardt R (2014) The single perturbation load approach applied to imperfection sensitive conical composite structures. Thin-Walled Struct 84:369–377 18. Orifici AC, Bisagni C (2013) Perturbation-based imperfection analysis for composite cylindrical shells buckling in compression. Compos Struct 106:520–528 19. Abramovich H, Singer J, Weller T (2002) Repeated buckling and its influence on the geometrical imperfections of stiffened cylindrical shells under combined loading. Int J Non Linear Mech 37:577–588 20. Bisagni C (2000) Numerical analysis and experimental correlation of composite shell buckling and post-buckling. Compos Part B Eng 31(8):655–667

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21. Hui-shen S, Pin Z, Chen (1991) Buckling and postbuckling of stiffened cylindrical shells under axial compression. Appl Math Mech 12(12):1195–1207 22. Ismail MS, Purbolaksono J, Andriyana A, Tan CJ, Muhammad N, Liew HL (2015) The use of initial imperfection approach in design process and buckling failure evaluation of axially compressed composite cylindrical shells. Eng Fail Anal 51:20-28

Enhancing the Energy Efficiency of Heat Exchanger by Using Double Helical Coil in Shell and Tube Heat Exchanger: An Experimental Study K. Hasham, M. W. Muhieldeen, S. Manzoor, and S. G. Solanki

Abstract The primary objective of this study is to enhance the energy efficiency of the heat exchanger by utilizing a double-helical coil tube (DHCT). A double helical coil is incorporated into the shell to achieve this goal, as double tube heat exchangers are well-suited for high-temperature and high-pressure applications due to their narrow diameters. Despite being cost-effective, they provide a large surface area for heat transfer. The experimental apparatus was used to calculate the geometric patterns’ impact on the heat transfer rate, employing the NTU (Number of Transfer Units) method. The NTU approach is particularly useful for assessing heat transfer rates in counter-current heat exchangers, especially in cases where there is insufficient data to calculate the log mean temperature difference. In this experiment, double-helical tubes were placed inside the heat exchanger shell to enhance the heat transfer rate. The data was recorded manually and digitally by connecting it to Arduino software using a billboard circuit. The temperature readings were obtained to calculate the heat transfer rates after specific time intervals. The coil’s desired inner and outer diameter set at 0.05 m ≤ Di, 0.08 m ≤ Do, tube and shell water flow rates range between 1 and 4 kg/s. After conducting numerous experiments, the result shows that the heat transfer rate for the double-helical coil tube (DHCT) is much greater than for the single helical tubes. The experiment shows that the effectiveness of the heat transfer rate observed with the double-helical coil was 54.33%, whereas, with a single helical coil heat transfer rate was 48.88%. It is proved by experimentation that a double-helical coil tube (DHCT) heat exchanger enhances the energy efficiency of the heat exchanger. The findings offer valuable insights K. Hasham · M. W. Muhieldeen (B) Mechanical Engineering Department, Faculty of Engineering, Technology and Built Environment, UCSI University, 56000 Kuala Lumpur, Malaysia e-mail: [email protected] K. Hasham Mechanical Engineering Department, Faculty of Engineering, University of Windsor, 401 Sunset Ave, Windsor, Canada S. Manzoor · S. G. Solanki Electrical and Electronics Engineering Department, Faculty of Engineering, Technology and Built Environment, UCSI University, 56000 Kuala Lumpur, Malaysia © The Author(s), under exclusive license to Springer Nature Singapore Pte Ltd. 2024 R. Abd. Aziz et al. (eds.), Intelligent Manufacturing and Mechatronics, Springer Proceedings in Materials 40, https://doi.org/10.1007/978-981-99-9848-7_3

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for heat exchanger design optimization, potentially contributing to eco-friendly and more energy-efficient solutions in various industrial applications. Keywords Heat exchanger · Double helical coiled tube · NTU method · Energy efficiency · Experimental study · Heat transfer enhancements

1 Introduction 1.1 Heat Exchangers A heat exchanger is a component that transfers heat from one medium to another. Several studies are going on to boost the exchanger’s heat transfer efficiency. Heat exchangers are widely used in industries and machines to meet human needs and simplify tasks. In many industrial processes, heat transfer is commonly observed. It can be achieved using three specific methods: convection of solids and convection in liquids such as fluids, gases, and radiation. A heat exchanger is a tool that can be used in both refrigeration and heating processes [1, 2]. Heat exchangers are being used in numerous applications, and one can research in many ways to find different parameters using several transfer units (NTU) methods and log mean temperature differences. Designing a heat exchanger is a tough job and critical due to its manufacturing cost and compactness of size. However, additional research is needed to minimize the design cost and get maximum heat transfer performance [3]. Many types of heat exchangers are present in industries to meet the requirements. The best kind is chosen due to the impact on the workplace environment. The best heat exchanger can be selected based on the optimizing process [4]. There are fundamental qualitative differences between standard heat exchangers to assist you in determining which can be chosen best for application. Shell and tube heat exchanger is the primary heat exchanger, which consists of tubes placed in the shell that can transfer heat between two fluids. One fluid passes through the tube, and the other from the body. However, placing smaller boxes in helical shape can increase heat transfer effectiveness [5, 6]. Plate and frame heat exchangers are often named plate heat exchangers, constructed with several plates held together in a large frame. It has a large surface area of space between plates to increase heat transfer effectiveness. The benefit is maintenance; cleaning and disassembling the faulty components is effortless. The welded design includes good corrosion resistance and higher operating design parameters. Welded units take more effort to clean than gasket plate designs. When properly handled, they are not prone to fouling and can provide long-term serviceability [7, 8]. The third design includes a fully welded plate pack inserted into a casing, distributing stress and eliminating the need for gaskets. Extreme temperatures and pressures are no problem for this form of heat exchanger. It may work with liquids, gases, or a mixture of fluids. Unlike a shell-and-tube design, there is little chance of fouling in a plate-and-shell design. On the other hand, these modules are almost always

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self-cleaning [9]. Over the years, the industry has encountered a recurring issue in conventional shell and tube heat exchangers, namely fouling. This problem arises due to the accumulation of unwanted substances, leading to a gradual decline in thermal efficiency and heat transfer rates. The present experiment incorporates a double helical coil within the shell to address this challenge. Helically coiled exchangers generate significant shear stresses, effectively reducing the propensity for fouling. Consequently, the heat exchanger can operate for longer cycles between scheduled cleaning intervals. Moreover, the reduced likelihood of fouling allows for the utilization of less conservative safety margins during the initial design phase. Exchangers are vital in some of our primary sectors, e.g., petroleum refining, refrigeration, airconditioning, and the food industry [10, 11]. During the heat exchange process, the sum of the internal energy and the product of pressure and volume of the fluid within a system is known as enthalpy. The temperature is directly proportional to the enthalpy of the water. In this experiment, double helical coil and shell inlet water were fed at 61 °C and 29 °C, respectively. The enthalpy of the cold water was increased due to the temperature increase in the shell, and at the same time, the enthalpy of hot water in the helically coiled tubes was decreased since the temperature dropped. In other words, the overall decrease in enthalpy has been achieved due to heat generated in the shell. Heat exchangers can be used in industries for heating or cooling, primarily air conditioners and fridges. Heat exchangers are used even in heating, ventilation, and air conditioning (HVAC) systems. Heat exchangers are used for central heating devices, in which colder air is removed from the building where it is not required and moved outside [12]. This also makes engines more powerful and work efficiently. In power plants or generators, the exhaust gases also produce useless heat into the atmosphere. That is a loss of electricity and one that a heat exchanger will mitigate, but some power would still be lost if not removed. This question can be solved by heat exchangers found within the smokestacks or exhaust tailpipes [13]. They brush past copper fins with water flowing through them as the hot exhaust gases drift upward. The water carries away the heat, which hits back into the plant. Recycling can be done directly, perhaps by heating the cold gases that are blown into the engine or furnace, saving the energy that would otherwise be needed to heat them [13, 14]. The approach used in this experiment is the number of transfer unit systems (NTU) that can be used if outlet and inlet temperatures are known. The number of transfer unit methods (NTU) is used in this experiment since insufficient parameters were known to use the long mean temperature difference method (LMTD) [15, 16]. This project aims to enhance efficiency using double helical coils in shell and tube heat exchangers. The basic purpose of using a double helical coil is to extend the contact surface area between the shell and the tube. This is done to enhance the area available for heat transfer. This study was investigated using double helical coils, proving that it is a more effective method than a helical or single coil in the shell. Conventional heat exchangers have been used for many years to make particular industries efficient and sustainable, but unfortunately, energy is being utilized to transfer heat. Still, it could have been proven more efficient as it could be done with double helical coil shells and tube heat exchangers. The research from precious authors shows that heat transfer can be way more efficient by fabricating heat exchangers with double helical

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coils. The experiment proved that heat can be efficient using a double helical coil in the shell and tube heat exchangers.

2 Methodology This study’s experimental work focused on the heat exchanger’s design to enhance the heat transfer efficiency between the hot and cold fluid. The fabrication process was divided into three stages: making a shell with a Double helical tube inserted, assembling all the equipment listed in Table 1 and connections, and final testing to ensure no leakage. The shell has been placed horizontally on the upper shelf of the metal stand to avoid turbulence, which can affect the accuracy of temperature readings. The vertical position can create turbulence because of the arrangement of the prototype. The turbulence will be less by placing the shell horizontally due to the larger surface area contact with the shell’s support, making it stable when water is fed. In this study, the helical tube was made of a copper pipe, as shown in Fig. 1. The helical tubes have 20 turns for the inner and outer tubes. The shell is made from polyvinyl chloride (PVC), with an inner and outer diameter of 0.1524 m and 0.3429 m, respectively (Fig. 2). An electrical rod has been placed in the hot water tank to heat the liquid. Plumbing fittings above the pump connected two water flow meters to measure the mass Table 1 Design components No.

Components

Quantity

Remark

1

Water centrifugal pump

2

Power: 1HP

2

Water flow meter

2

3

Temperature sensor

4

4

Pipe flow stopper

2

5

PVC pipe (HE shell)

2m

6

Glue

4

7

PVC connecter

4

8

PVC cap (6 Inch)

2

9

Copper pipe (1/4 inch)

15 m/roll

10

Storage tank

2

11

Steel rods (6ft each)

7

The base of the prototype

12

Wood

2

For shelf

13

Pressure gauge (150 bar)

2

14

Copper pipe bender

1

15

Rubber hose pipe

10 m/roll

22 m

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Fig. 1 Double helical coil

Fig. 2 Heat exchanger PVC shell

flow rate of the working fluid. The shell and tube’s close cycle has hot and cold water. The hot water flows through the double-helical coil, and the cold water runs inside the shell. The hot and cold-water temperatures were measured thermometer sensor connected at the exit point of each section. The hot water returns to the hot water storage tank to keep the temperature of water constant in the tank. The cold water follows the same cycle. The outlet and inlet temperatures are recorded using four temperature waterproof sensors placed in the rubber hose pipe. The number of transfer units (NTU) method is used to calculate the heat transfer rate. Figure 3 shows the experimental setup of the double-helical coil heat exchanger.

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Fig. 3 Experimental setup of shell and tube heat exchanger

The temperature readings were acquired following water feeding into the shell and double helical tubes. Temperature sensors were strategically placed at four locations near the entrance and exit points of the shell to capture crucial temperature data. The significance of temperature lies in determining the Reynolds number for both the shell and double helical tube. The average temperature from the shell and helical tubes were utilized independently to calculate the respective Reynolds number and heat transfer coefficients. Due to the temperature dependence of thermal conductivity and heat transfer coefficient, obtaining accurate temperature measurements from each side of the shell was of paramount importance. This ensured precise evaluations of the heat transfer process within the heat exchanger system. The Number of Transfer Units (NTU), a dimensionless parameter reliant on the shell and tubes’ surface areas, was calculated after determining the maximum heat transfer rate. A higher NTU value was observed, signifying significantly enhanced heat transfer rates compared to single and conventional shell and tube heat exchangers. The temperature data collected from the main pipe entrance and exit offers valuable insights into the overall heat transfer performance of the shell and tube heat exchanger. These measurements provide critical information about the temperature changes occurring during the fluid’s passage through the conventional part of the heat exchanger, enabling us to assess its efficiency. Conversely, data from the entrance and exit of the double helical coil allows for a focused analysis of the specific impact of this innovative coil configuration on the heat transfer process. By monitoring the temperature variations within the double helical coil, we can precisely evaluate how much this design modification enhances heat transfer efficiency. By comparing temperature

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differentials between these points, we can quantitatively assess the improvements achieved by implementing the double helical coil.

2.1 The Calculation of the Heat Transfer Coefficients The calculation has been done based on the number of transfer units (NTU) method. The overall heat transfer coefficient has been calculated using Eq. (1): [17]. Uo =   1 hc

1 +

  1 h0

(1)

where k is the thermal conductivity of the fluid, and its SI unit is W/m K D is the inner diameter of the tubes, and it is measured in meters, hc and ho are heat transfer coefficients for cold and hot water, respectively. The unit for heat transfer coefficient is W/m2 K. Both heat transfer coefficient has been calculated depending on the hot and cold temperature of both the inlet and outlet temperatures of the heat exchanger. The Reynolds number plays an important role in estimating trends in the behaviour of a fluid. The Reynolds number is used to figure out whether the fluid flow is laminar or turbulent. It is a vital regulating parameter of all viscous fluids where a pre-calculated number of Reynolds chooses a numerical model. It can be calculated using Eq. (2). ReD =

4m ˙ πDμ

(2)

m˙ = mass flow rate of the fluid (kg s−1 ). µ = Viscosity of the fluid (Pa s). Nusselt number has been calculated based on the following: 4

N u D = 0.023Re D5 Pr 0.4

(3)

The heat transfer rate (q) can be found using temperature and heat capacity rate. The calculation can be done using the following equations. Cc = mc cp,c (J/Kg k)

(4)

Ch = mh cp,h (J/Kg k)

(5)

  qmax = Cmin Th,i − Tc,i (W)

(6)

where capacity rate (Cmin ) should be chosen minimum to find the heat transfer rate.

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m c = mass flow rate of cold fluid. m h = mass flow rate of hot fluid. c p,c = Heat capacity of cold fluid. c p,h = Heat capacity of hot fluid. Th,i = Temperature inlet of hot fluid. Tc,i = Temperature inlet of cold fluid. As for every engineering problem, when measuring and choosing a heat exchanger or evaluating its thermal efficiency, there are various methods to approach a solution. If the chosen heat exchanger is undersized, it cannot meet the planned heat transfer conditions. The heat transfers and higher fluid outlet temperatures contribute to the quality output. A properly designed heat exchanger must have a minimum excess ability to compensate for the fouling during processing. The NTU method is the ratio of the heat exchanger’s ability to transfer heat (UA) to the total heat absorption potential of the fluid. The equation shows to find the number of transfer units. NTU =

U(A1 + A2) Cmin

(7)

U = Overall heat transfer coefficient. A1 = Area of the outer tube. A2 = Area of the inner tube. Cmin = Minimum specific heat. The range of parameters shown in Table 2 was considered for the experiment shown in Fig. 4, and the outcome was taken in the form of heat transfer and a number of transfer units. Several steps were followed during the study to achieve the goal of the fabrication and results. Table 2 Parameters specification Dimension

Tube specifications

Dimension

Inner diameter

0.1524 m

Outer diameter

0.08 m

Thickness

0.05 m

Inner diameter

0.05 m

Material

PVC

Pitch

0.0015 m

Material

Copper

heat transfer rate(W)

Shell specifications

6 4 2 0 q (W) Conventional Pipe

Single Helical Pipe

qmax(W) Double Helical Pipe

Fig. 4 Comparison of heat transfer between conventional heat exchanger and single, double helical coil heat exchanger

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3 Result and Discussion

Percentage %

The experimental results have been compared with the reference model research [18]. The temperature reading was taken, and both readings have minor differences since the reference model was a simulation-based study. This experiment is done to obtain the optimum efficiency of the heat exchanger. At the same time, the model temperature was set initially to enhance the performance of the shell and tube heat exchanger using a simulation model. Figure 4 shows the bar chart of the three heat exchangers’ actual and max heat transfers. Among the three types of heat exchangers, conventional pipe, single helical coil, and double helical coil, the double-helical coil shows the maximum heat transfer followed by single helical and then by conventional heat pipe, which has the minimum heat transfer. As shown in Fig. 4 double helical coil is more efficient than single helical and conventional pipes due to its shape. Due to their compactness and enhanced heat transfer coefficient, double-helical coils have an advantage over straight tubes. The higher heat transfer coefficients are due to the coil’s curvature, which causes centrifugal forces to operate on the moving fluid. The centrifugal force is governed by the coil’s curvature, which plays an important role in making heat transfer efficient. According to the data, Fig. 5 compares the three configurations of heat exchangers. The normal pipe is the least suitable approach for the heat exchanger as it has the least effectiveness at 40.06%. The second heat transfer method through helical shows a significant increase in the effectiveness of 48.88%, which is 8% more than the normal pipe. Upon further experimentation using a different configuration of heat exchangers, a double-helical design was implemented, increasing the effectiveness to 54.23% and a difference of around 8% from its predecessor single helical design. Hence, the double-helical proves to be more efficient and helps increase the heat energy transfer from the working fluid to the assistant fluid. The above results indicate that double-helical was the most designed to be used as a heat exchanger. Figure 6 shows 29 °C is the shell inlet of this study temperature, whereas 26 °C is set for the reference model [18]. Shell outlet is calculated at 41 °C from Arduino UNO, and in the reference model, 35 °C was selected. As can be observed from the graph, all the temperatures calculated for this study are higher than Jamshidi’s [18] 60 40 20 0 conventional Heat Exchanger

Single helical Pipe Double Helical Pipe Heat Exchanger Heat Exchanger

Fig. 5 Comparison of effectiveness between conventional heat exchanger and single, double helical coil heat exchanger

K. Hasham et al.

Temperature° C

34

80 60 40 20 0 shell inlet

Shell outlet

Helical tube inlet Prototype Temperature Reference Temperature

Helical tube outlet

Fig. 6 Graphical comparison of temperature obtained from reference and experiment

model except helical tube inlet temperature, which is 61 °C. For the reference study, it was 66 °C. The last helical outlet tube is considered the major change because it is the only temperature that will be decreased while leaving the system since it will transfer heat to cold water flow. The helical tube outlet for prototype temperature is determined to be 48 °C, and the reference model is 47 °C. All the temperature readings for the prototype is taken from the water temperature sensor using coding and Arduino software. The previous and current heat exchanger research is mostly done on the shell and helical tubes using single helical coil tubes. Based on Jamshidi’s [18] model, the study shows the comparison in the temperature through simulation to enhance the efficiency of shell and tube heat exchangers. The current study used the number of transfer unit method (NTU) to find the heat transfer rate since the temperature was recorded experimentally. Hence, the outcome is more accurate than the reference model. The heat transfer calculated from the working fluid is 2.17 W, and the maximum heat transfer is 4.01 W. Depending on the requirements, the double-helical coil in this study can enhance a large amount of heat transfer. If compared with straight tubes, helical are found to be more efficient. In my study, double helical coils have been used to enhance heat transfer because the centrifugal force produces secondary flow due to the curvature of tubes. The flow is perpendicular to the axial direction, which helps fluid to mix properly and enhances the heat transfer rate. The parameters decided initially in this study also greatly impact the heat transfer rate. The 0.25-inch copper tube heat transfer rate will be more efficient than other diameter sizes, like 0.5 inches. This is because 0.25 inches of double-helical copper pipe will have more surface area than other diameter tubes if compared to a single helical coil. The higher surface area allows fluid to come into contact with another fluid for longer, increasing the heat transfer rate and effectiveness. Although 0.25 inches is the smallest diameter and can only flow a smaller volume, the larger surface area can increase the effectiveness. Thus, 0.25 inches of the double-helical coil has been used. The effectiveness of the heat exchanger is defined as the ratio of the real amount of heat transferred with an infinite area to the maximum possible amount of heat transferable. Calculating the effectiveness of the double coil heat exchanger from the specified temperature in the experiment is measured at 54.23%, indicating that the prototype can transmit heat between two fluids.

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4 Conclusion Numerous ways have been researched to find the best possible heat exchange rate. Comparing the results with an experiment by Jamshidi’s [18] showed that doublehelical coils are more effective than single-coil heat exchangers. The researcher found heat transfer rate in a similar way as done here. The only difference in Jamshidi’s research is Taguchi method is used to find optimum conditions for desired values to experiment. In this experiment, the coil diameter is set at 0.05 m ≤ Di, 0.08m ≤ Do, whereas Jamshidi’s conducted his research with 0.0813 < Dc < 0.116. This study found heat transfer most effective based on the surface area of tubes and mass flow rate, whereas research shows that the smaller diameter of tubes will make heat transfer rate efficient. Using the number of transfer units’ method (NTU) and apparatus set up with single helical and double helical coils showed heat transfer rates of 48.88% and 54.33%, respectively. The experiment showed that double helical coils’ heat exchangers are more efficient and reliable. In conclusion, a round tube that depends on less transfer heat efficiency should be chosen for industrial heat exchanger use.

References 1. Zohuri B (2017) Heat exchanger types and classifications. Compact heat exchangers, pp 19–56 2. Jouhara H (2018) Waste heat recovery technologies and applications. Therm Sci Eng Process 6: 268–289 3. Alimoradi A (2017) Study of thermal effectiveness and its relation with NTU in shell and helically coiled tube heat exchangers. Case Stud Therm Eng 9(1):100–107 4. Teke I (2010) Determining the best type of heat exchangers for heat recovery. Appl Therm Eng 30(6): 577–583 5. Gugulothu R (2017) A review on enhancement of heat transfer techniques. Mater Today Proc 4(2): 1051–1056 6. Elankavi RS (2018) Study of flow and heat transfer analysis in shell and tube heat exchanger using CFD. Int Res J Eng Technol (IRJET) 5(10): 467–473 7. Jamshak SH (2018) Design and analysis of a plate heat exchanger in the view of performance improvement and cost reduction. Int Res J Eng Technol (IRJET) 7(3): 440–446 8. Velazquez MT (2011) The design of heat exchangers. Sci Res 3: 911–920 9. Ogbonnaya SK (2017) Fouling phenomenon and its effect on heat exchanger 10. Bichkar P (2018) Study of shell and tube heat exchanger with the effect of types of baffles. Procedia Manuf 20(2): 195–200 11. Rennie TJ (2005) Experimental studies of a double-pipe helical heat exchanger. Exp Therm Fluid Sci 29(8): 919–924 12. Chunangad KS (2006) Most frequently used heat exchangers from pioneering research to worldwide applications. Heat Transf Eng 27(6): 4–11 13. Mahendran J (2020) Experimental analysis of shell and tube heat exchanger using flower baffle plate configuration. Mater Today Proc 21(1):419–424 14. Kasban H (2021) Efficient evaluation of heat exchangers behavior in nuclear power plants 54(2):126–136 15. Y. Cengel, "Thermodynamics: An Engineering Approach," MC Graw Hill, (2019). 16. Popov D (2019) Cryogenic heat exchangers for process cooling and renewable energy storage. Appl Therm Eng 153:275–290

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17. Incropera FP, DeWitt DP (2017) Principle of heat and mass transfer. Global Edition 18. Jamshidi N (2013) Experimental analysis of heat transfer enhancement in shell and helical tube heat exchangers. Appl Therm Eng 51(1–2): 644–652

Effect of Wobbling Loops with Laser Welding Characteristics to the Shear Strength of Cu/Al Lap Joints for Battery Applications M. N. Jamaludin , M. M. Quazi , M. F. M. Yusoff, Mohammadamin Ezazi, and Zawani Ismail

Abstract Manufacturing, automotive, and aerospace industries choose fibre laser welding. These industries prefer fibre laser welding because the technology requires less space, has low setup and maintenance costs, and produces high-quality welds without surface conditioning. Fibre laser welding produces joints with a small heataffected zone (HAZ), deep penetration, and good seam quality, making them visually appealing and high-grade. Since intermetallic phases formation and joint efficiency pose issues, thus, welding parameter control is essential. In this work, the tensile shear strength testing results were obtained based on the variation in the laser scanning marking loops of Cu/Al joints. Despite obstacles, the work shows that wobbling can weld thin dissimilar Cu/Al alloys. Mark loop configurations affect welded joint properties. Mark loop 6 boosts tensile strength to 25.19 MPa, followed by mark loops 4 and 3 at 15.13 and 13.22 MPa, respectively. After tensile strength testing, optical microscopy image analysis illuminates the morphological characteristics, failure modes, and mechanical properties of Al/Al, Cu/Cu, and Cu/Al joints. The findings of this study can result in improvements in joint design and fabrication procedures, enhancing industry dependability and performance. In conclusion, welding dissimilar metals has a high potential and parameter modifications are crucial for strong joints and optimal mechanical properties. Keywords Laser · Micro-welding · Automotive · Battery applications · Wobbling technology

M. N. Jamaludin · M. M. Quazi (B) · M. F. M. Yusoff · Z. Ismail Faculty of Mechanical and Automotive Engineering Technology, Universiti Malaysia Pahang Al-Sultan Abdullah, 26600 Pekan, Pahang, Malaysia e-mail: [email protected] M. Ezazi Department of Mechanical Engineering, Georgia Southern University, Statesboro, GA 30460, USA © The Author(s), under exclusive license to Springer Nature Singapore Pte Ltd. 2024 R. Abd. Aziz et al. (eds.), Intelligent Manufacturing and Mechatronics, Springer Proceedings in Materials 40, https://doi.org/10.1007/978-981-99-9848-7_4

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1 Introduction The main issues with battery joining are joint reliability and durability, as well as the formation of defects. Various joining techniques exhibit limitations such as distortion, welding cracks, and underfills, as well as the formation of intermetallic compounds that contribute to mechanical property degradation. According to studies, electric vehicles are more environmentally friendly. They produce lower carbon dioxide emissions and pollutants in the air than gasoline or diesel vehicles. This involves their manufacturing and electricity generation to keep going [1]. Based on the International Energy Agency’s (IEA) Global EV Outlook for 2019, there were more than 5.1 million electric vehicles worldwide in 2018, an increase of 2 million from the previous year [2]. Given existing responsibilities and newly announced targets, the IEA anticipates continued growth in EV market share, with a total global stock exceeding 130 million by 2030. This aim is consistent with the Paris Agreement [3]. With such an estimate in hindsight, the rapid production of batteries of extremely high reliability is a dire need. Hence, the reliable and mass production volume of such batteries would require precision manufacturing technology in the form of highly programmable, mobile, and robust fibre lasers that would be able to weld different materials of various shapes and sizes in a single operation. In laser micro-welding, very low power and small spot diameters produce penetration depths of less than one millimetre. The laser scans the micro-weld portion and is monitored by employing a camera or microscope. Researchers have been actively exploring the role of micro-welding in the automotive, electronics and biomedical, fields of engineering, among others. As observed from the available literature, the micro-welding is carried out by employing pulse wave mode lasers to join a wide range of materials. The research studies have dealt with precisely controlling various laser micro-welding parameters such as pulse energy, pulse width, pulse frequency, the angle of incidence, joint type, and defocus distance. The joining of copper and aluminium sheets is important for battery applications. It is known that copper and aluminium are highly reflective materials. When joining from a copper sheet, the keyhole mode of welding is required to overcome copper’s reflectivity and melting threshold. Nevertheless, in the case of dissimilar metals interaction, the resulting intermetallic compounds (IMC) are brittle, resulting in poor performance [4]. The joining of both metals is difficult due to poor weldability caused by differences in chemical, mechanical, and thermal properties of the materials, particularly the vast formation of hard and brittle intermetallic compounds (IMC) at the weld interface [5]. Considering the buyers’ main issue with Evs is their driving range [6], as space and weight in EVs are limited, higher battery energy densities (the amount of energy stored per unit volume or weight) are required [7]. Battery technologies have evolved from lead-acid to nickel-based to lithium-based types in order to obtain a safe, reliable, and user-friendly storage technology with high energy density and fast charging [8]. Lastly, the major technological challenges are increasing energy density, reducing charging times, and increasing end of life (EoL),

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whereas the initial battery cost, on which the price of a BEV is heavily dependent, is the primary financial concern [8]. Experts have been investigating the wobble technique and reported that the weld improved as a result of this method [9]. Kuryntsev and Gilmutdinov et al. [10] reported that steel’s ductility has been improved due to the restriction of phase transition caused by the cooling phase slowing down. They studied various type of alloys in the experiment. Barbieri et al. [11] proved that oscillating the laser beam optimizes the mechanical properties of the weld by covering a larger area along the weld seam. Groups of researchers additionally provided a comparison of oscillation patterns, claiming that it has an important impact on the quality of the weld zone [11–14]. The claim has been verified and backed by experience, which demonstrates that specific patterns are more effective at providing a stronger weld [13]. Al-Cu welding is challenging and required careful selection of parameters or variation in laser process such as continuous wave, pulsed wave or marking loop or wobbling mode with a combination of these. Here in this work, we are going to try marking loop-based laser micro welding. This study provides better understanding of the role of several characteristics such as mark loop, power, speed, frequency, and wobbling diameter, alongside two materials (T2 copper and aluminium 1060 series).

2 Methodology Samples of Cu (99.9%) and Al (99.5%) were procured locally. Thereafter, the samples were cut in sections, grinded and cleaned for micro-welding. As shown Fig. 1 both metals, T2 pure copper sheet, and aluminium sheet 1060 series are very thin, and have thickness which are 0.3 mm, and 0.4 mm, respectively. The whole laser welding process is carried out by using Herolaser ML-MF-A01 IPG Fibre laser machine with 50 μm laser spot diameter. For pulsed wave mode welding, a maximum mean power of 30 W was employed with a pulsed duration of 100 ns. The wavelength of the laser beam has a major impact on the absorption on the base material [15]. To add more, the aforementioned were not measured in the study but, there were few studies about the Cu/Al welding. Kuryntsev et al. [16] studied about laser welding of dissimilar materials methods, microstructure, and properties. They found that, the absorption coefficient of the metal is greatly impacted by the laser’s wavelength; for instance, Al and Cu do not absorb the CO2 laser’s (λ = 10.6 μm) irradiation. Then, Indhu et al. [17] investigated the approaches to measuring absorptivity that is used when using lasers to treat commercial metals like steel, titanium, aluminium, and copper. They investigation included cutting-edge analytical, numerical, and experimental methodologies for evaluating absorptivity with the aim to produce effective laser control systems. As illustrated in Fig. 1 continuous wave mode using the same average power. Using a fibre optic and collimator end, the laser is transported to the laser head. The focusing lens is attached to the laser head and is protected by a protective mirror. The gap between the laser focused spot and the focusing lens is 192 mm. A computer

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Fig. 1 Schematic drawing of the lap joint micro-welding configuration

is installed with its respective software for the welding parameters to be inserted as shown in Fig. 2. After the completion of the welding process, tensile testing using the universal testing machine was conducted for getting information on the joint efficiency. Nunes et al. [18] stated that, despite several studies on the quality of joints, there is a lacking of information on how the samples should be prepared in order to obtain optimized tensile strength values. As shown in Fig. 3b, c for tensile testing the sample was prepared by not using the standard as brought up by Ascari et al. [19] due to the tensile specimens contrasting with the standard specimens in that they have a straight profile and lack the usual “bone-shape.” Because of these qualities, as well as the samples’ relatively low thickness, it was infeasible to utilize an extensometer throughout the tests, hence the stress- strain curve was not recorded.

3 Results and Discussion The experimental outcomes offer important implications that welding of thin dissimilar metals of Cu/Al is possible despite the challenges. The welding process is achieved by using wobbling technique as shown in Table 1. Next, in Fig. 4 It is noticeable that by varying the mark loop while keeping the other parameters constant can produce a strong welded joint. Furthermore, it is also distinguished that adjusting

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Fig. 2 A schematic drawing of micro-welding fibre laser setup

the number of mark loop certainly gave an effect on the welded joint, as it can be seen in Fig. 4f, h, j at the bottom of each aluminium for mark loop 4 has clear and thick wobbling circle, mark loop 5 has narrower pattern compared to other sample, and mark loop 6 seems to have inconsistent wobbling pattern. Moving on, in Fig. 5 it shows that by increasing the number of mark loop to 6 will increase the tensile strength which reaches maximum of 25.19 MPa. This suggests that applying 6-mark loops significantly improves the material’s capacity to endure tensile stresses. The strength values for loop 3 and loop 4 were obtained as 13.22 MPa and 15.13 MPa, respectively. The outcomes strongly show that increasing the number of mark loops increases the tensile strength of the material accordingly. This understanding has important practical consequences since it allows researchers to adjust the number of mark loops in welding to obtain desired levels of tensile strength. Table 2 illustrates the picture of the sample by using optical microscopy from the microscope after undergone tensile strength test. The study utilized a 400 μm scale factor as standard to calibrate optical microscopy measurements from the microscope. In summary, the optical morphologies obtained at different marking loops provide an in-depth insight of the morphological behaviour, failure modes, and mechanical properties of the Cu/Al joints during tensile strength testing. From the table we can see that different number of mark loops gives different types of morphologies after

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Fig. 3 a Sample is prepared before undergoing tensile testing of different mark loops, b, c sample is clamped by a fixture of the tensile test machine, and d the Instron 3400 series testing system Table 1 Micro-laser welding parameter by using wobbling technique

Wobbling diameter (mm)

0.3

0.3

0.3

Mark loop

4

5

6

Speed (mm/s)

1

1

1

Frequency (kHz)

25

25

25

Result

Welded

Welded

Welded

Fig. 4 a–d Optical microscopy images of Cu/Cu, and Al/Al joints from a microscope, and e– i optical microscopy images of Cu/Al joints from a microscope with different mark loops which were 4, 5, 6 while keeping other parameters consistent

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Fig. 5 Tensile strength (MPa) results of mark loops 4, 5, and 6 for Cu/Al micro welded joints. The error bars indicate standard deviations

undergone tensile shear strength tests. For 4 and 5 mark loops it is visible that, on Al and Cu side of the joints the laser wobbling were very clear when compared with 6 mark loops. In addition, it indicates that number of mark loop gives substantial impact on welding joint in terms of shear strength although higher number of mark loops come with higher strength. Heat affected zone (HAZ) also can be seen on top of every Cu/Al joint, showing that, the melting point of the materials was also reached. To reduce the formation of HAZ in the future, further control of the heat flux of the laser is required. To add more, HAZ can be susceptibility to cracking and reduce the corrosion resistance or lower the toughness. Jeyaraj et al. [20] stated that, the temperature produced at the interface has a strong correlation with joint strength. Next, other researcher like Shin et al. [21] obtain the average tensile shear strength of 21.5 and 16.0 MPa, correspondingly. Other than that, Yan et al. [22] acquire 99.8 MPa along with a laser power of 2.45 kW. The findings of this analysis can be used to improve joint design and fabrication processes for future work, resulting in increased reliability and performance in related areas.

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Table 2 Image of optical microscopy of Cu/Al joints by varying the mark loops and keep other parameters like speed, power, frequency, and wobbling diameter constant Parameters

Al side

Cu side

4-mark loops

5-mark loops

6-mark loops

4 Conclusion In conclusion, despite certain obstacles, our investigation reveals that welding thin dissimilar Cu/Al alloys is achievable. The welding process is successfully completed using the wobbling technique. Variation in the mark loop while maintaining other parameters constant has been shown to be crucial in developing strong welding joints. Additionally, varying the number of mark loops has an obvious impact on the features of the welded joints. By increasing the mark loop to 6, the tensile strength increases to 25.19 MPa, followed by mark loop 4 at 15.13 MPa and mark loop 3 at 13.22 MPa. Following that, an optical microscopy image analysis provides beneficial insights into the morphological behavior, failure modes, and mechanical properties of Al/Al, Cu/ Cu, and Cu/Al joints during tensile strength testing. These discoveries can be used to improve future joint design and fabrication procedures, hence increasing reliability and performance in relevant domains. Overall, this study emphasizes the possibility of welding dissimilar metals and the significance of parameter modifications for generating strong joints and maximizing mechanical qualities. Acknowledgements The authors would like to thank the Ministry of Higher Education for providing financial support under Fundamental Research Grant Scheme (FRGS) FRGS/1/2021/ TK0/UMP/02/22 (University reference RDU210127).

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References 1. Sierra Rodriguez A, de Santana T, MacGill I, Ekins-Daukes NJ, Reinders A (2020) A feasibility study of solar PV-powered electric cars using an interdisciplinary modeling approach for the electricity balance, CO2 emissions, and economic aspects: the cases of The Netherlands, Norway, Brazil, and Australia. Prog Photovoltaics Res Appl 28(6):517–532. https://doi.org/ 10.1002/pip.3202 2. Pelaprat JM, Zediker MS, Finuf M (2017) Visible laser welding of electronic packaging, automotive electrics, battery and other components. Google Patents 3. Helm J, Dietz von Bayer I, Olowinsky A, Gillner A (2019) Influence of the surface properties of the connector material on the reliable and reproducible contacting of battery cells with a laser beam welding process. Weld World 63(5):1221–1228 4. Mathivanan K, Plapper P (2019) Laser welding of dissimilar copper and aluminum sheets by shaping the laser pulses. Procedia Manuf 36:154–162. https://doi.org/10.1016/j.promfg.2019. 08.021 5. Kaspar J, Zimmermann M, Ostwaldt A, Goebel G, Standfuß J, Brenner B (2014) Challenges in joining aluminium with copper for applications in electro mobility. Mater Sci Forum 783– 786(May 2022):1747–1752. https://doi.org/10.4028/www.scientific.net/msf.783-786.1747 6. Deloitte, “New market. New entrants. New challenges. Battery Electric Vehicles,” p 5, 2017, [Online]. Available: https://www2.deloitte.com/content/dam/Deloitte/uk/Documents/manufa cturing/deloitte-uk-battery-electric-vehicles.pdf 7. Deng J, Bae C, Denlinger A, Miller T (2020) Electric vehicles batteries: requirements and challenges. Joule 4(3):511–515. https://doi.org/10.1016/j.joule.2020.01.013 8. Roy H et al (2022) Global advancements and current challenges of electric vehicle batteries and their prospects: a comprehensive review. Sustainability 4(24). https://doi.org/10.3390/su1 42416684 9. Shah LH, Khodabakhshi F, Gerlich A (2019) Effect of beam wobbling on laser welding of aluminum and magnesium alloy with nickel interlayer. J Manuf Process 37:212–219. https:// doi.org/10.1016/j.jmapro.2018.11.028 10. Kuryntsev SV, Gilmutdinov AK (2015) The effect of laser beam wobbling mode in welding process for structural steels. Int J Adv Manuf Technol 81(9–12):1683–1691. https://doi.org/ 10.1007/s00170-015-7312-y 11. Barbieri G, Cognini F, Moncada M, Rinaldi A, Lapi G (2017) Welding of automotive aluminum alloys by laser wobbling processing. Mater Sci Forum 879:1057–1062. https://doi.org/10.4028/ www.scientific.net/MSF.879.1057 12. Hagenlocher C, Sommer M, Fetzer F, Weber R, Graf T (2018) Optimization of the solidification conditions by means of beam oscillation during laser beam welding of aluminum. Mater Des 160:1178–1185. https://doi.org/10.1016/j.matdes.2018.11.009 13. Wang Z, Oliveira JP, Zeng Z, Bu X, Peng B, Shao X (2019) Laser beam oscillating welding of 5A06 aluminum alloys: microstructure, porosity and mechanical properties. Opt Laser Technol 111:58–65. https://doi.org/10.1016/j.optlastec.2018.09.036 14. Wang L, Gao M, Zhang C, Zeng X (2016) Effect of beam oscillating pattern on weld characterization of laser welding of AA6061-T6 aluminum alloy. Mater Des 108:707–717. https:// doi.org/10.1016/j.matdes.2016.07.053 15. Lee SJ, Choi KD, Lee SJ, Shin DS, Jung JP (2022) Welding properties of dissimilar Al-Cu thin plate by a single-mode fiber laser. Metals (Basel) 12(11):1–12. https://doi.org/10.3390/met121 11957 16. Kuryntsev S (2022) A review: laser welding of dissimilar materials (Al/Fe, Al/Ti, Al/Cu) & mdash; methods and techniques, microstructure and properties. Materials 15(1). https://doi. org/10.3390/ma15010122 17. Indhu R, Vivek V, Loganathan S, Bharatish A, Soundarapandian S (2018) Overview of laser absorptivity measurement techniques for material processing. Lasers Manuf Mater Process 5(4):458–481. https://doi.org/10.1007/s40516-018-0075-1

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18. Nunes R, Faes K, De Meester S, De Waele W, Kubit A (2022) Influence of welding parameters and surface preparation on thin copper–copper sheets welded by ultrasonic welding process. Int J Adv Manuf Technol 373–388. https://doi.org/10.1007/s00170-022-10164-9 19. Ascari A, Fortunato A, Dimatteo V (2020) Short pulse laser welding of aluminum and copper alloys in dissimilar configuration. J Laser Appl 32(2):022025. https://doi.org/10.2351/7.000 0073 20. Pradeep Kumar J (2018) Effect of temperature distribution in ultrasonically welded joints of copper wire and sheet used for electrical contacts. Materials 11(6). https://doi.org/10.3390/ ma11061010 21. Shin WS et al (2021) Investigation on laser welding of al ribbon to cu sheet: weldability, microstructure, and mechanical and electrical properties. Metals (Basel) 11(5). https://doi.org/ 10.3390/met11050831 22. Yan S, Shi Y (2019) Influence of laser power on microstructure and mechanical property of laser-welded Al/Cu dissimilar lap joints. J Manuf Process 45(7089):312–321. https://doi.org/ 10.1016/j.jmapro.2019.07.009

Power System Generation: Current Trend Towards Sustainable Energy Storage Systems Mohd Najib Razali , Mohd Sabri Mahmud , Syahirah Syazwani Mohd Tarmizi , and Mohd Khairul Nizam Mohd Zuhan

Abstract Nowadays, our country needs to revise the usage of energy resources in every sector. This generally will affect our economy as well as our environment. Renewable energy has been debated to protect our Earth towards a bright future. Many types of renewable energy should be taken into consideration, along with rechargeable energy. Rechargeable energy seems to be a better option to lower carbon emissions. The battery is one of the chemicals that is frequently used in many industries to supply energy in terms of electrical energy. The trend towards sustainable energy storage systems was studied as the prevention of any pollution in this world. Keywords Renewable energy · Rechargeable energy · Battery · Energy storage systems

1 Introduction Climate change mitigation is crucial for limiting adverse environmental effects. The improvement of the energy sector has been pushed into the global agenda to combat climate change owing to the Paris Agreement’s low carbon dioxide (CO2 ) emission allowance [1]. The United Nations Development Programme’s (UNDP) 2030 Agenda for Sustainable Development (SDGs) and Paris Agreement under the United Nations M. N. Razali (B) · M. S. Mahmud Faculty of Chemical and Process Engineering Technology, Universiti Malaysia Pahang Al-Sultan Abdullah, 26300 Kuantan, Pahang, Malaysia e-mail: [email protected] S. S. Mohd Tarmizi MNR Multitech Sdn. Bhd, K02 Ground Floor, Kompleks UMP Holdings, 26300 Gambang, Pahang, Malaysia M. K. N. Mohd Zuhan Pusat Pengajian Diploma Universiti Tun Hussein Onn Malaysia, Hab Pendidikan Tinggi Pagoh, KM1, Jalan Panchor, 84600 Pagoh, Johor, Malaysia © The Author(s), under exclusive license to Springer Nature Singapore Pte Ltd. 2024 R. Abd. Aziz et al. (eds.), Intelligent Manufacturing and Mechatronics, Springer Proceedings in Materials 40, https://doi.org/10.1007/978-981-99-9848-7_5

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Framework Convention on Climate Change (UNFCC) are two notable global initiatives that tackle the conflict between economic growth and environmental responsibility. The former aims to reduce poverty and hunger, as well as foster justice, peace, and human rights, and create economic growth that is environmentally benign, sustainable and brings about prosperity for all people [2]. The concentration of greenhouse gases (GHGs) in the atmosphere and the global mean temperature are both rising substantially. Carbon dioxide (CO2 ) is the most important anthropogenic greenhouse gas because of its plentifulness and capacity to linger in the atmosphere for a long time [3]. Future low-carbon cities will be built due to careful analysis of how urbanization affects CO2 emissions. Urbanization, directly and indirectly, affects the environment by changing lifestyle trends, manufacturing processes, and land-use schemes [4]. With a target of 1.5 °C, the Paris Climate Agreement seeks to maintain global warming considerably less than 2 °C over the period prior to industrialization [5]. It also requests that financial flows be aligned with these global aims. In contrast to the modest improvements anticipated by present plans, ambitious peak temperature targets necessitate dramatic emission cuts until 2030, with the power sector making the most significant contribution to decarbonization [6]. Undoubtedly, the choice, creation, and execution of significant national-level actions will determine how effective the Paris Agreement is. A more in-depth examination of the Paris Agreement reveals that it is a key legal management tool for international efforts to reduce greenhouse gas emissions and adapt to climate change. It establishes a broadly shared objective but depends on national assessments of individual mitigation and adaptation contributions; institutionalized conformity analyse minimal, with just a facilitating violations procedure; and parties’ acts are not subject to any responsibility for harm or loss that is established by the agreement itself [7]. One of the main drivers of the transition away from fossil fuels and toward renewable energy is climate change. If fossil fuels are used after 2050, these predictions will be reduced by 2100. Feedstock consumption, with a smaller level of carbon than burning, contributes to sixty-five percent and 68 percent, respectively, of the total oil and fossil methane gas consumption in 2100 under a 1.5 °Ccarbon budget [8]. An update on the global community’s capacity to accomplish goals is provided in the Sustainable Development Goal (SDG) 7 Report. Regardless of good development in the use of renewable energy, reaching SDG 7 by 2030 is hard and impossible to achieve. Manageable renewable energy sources, such as bioenergy and hydroelectric power, reduce CO2 emissions significantly by meeting more than 16% of global energy consumption and providing huge growth potential [9]. Although the transition from fossil fuels to RE sources is ideal, its integration into the power grid is still hampered by RE’s unpredictable and intermittent characteristics [1]. Even though there are many preventive ways to use renewable energy, the demand is still higher as the driven towards urbanization and area development. Therefore, studying the improvement of RE in the greatest way has become the research’s focus. From a demand standpoint, the increase in energy demand is related to population expansion. The distribution of resources and the long-term viability of the power

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Table 1 Characteristics of rechargeable batteries Rechargeable Voltage (V) Capacity (Ah) Weight energy Number of Efficiency (%) battery types density (Wh/ times recharge kg) cycle SLA

6

1.3

26

500–800

71–93

NiMH

1.2

2.5

100

1000

70–90

NiCd

1.2

1.3

30–50

1000–1500

75–95

Li-ion

3.7

0.75

165

1200

99.6

generation system both provide challenges to the production of energy. Additionally, the globe generates 87 percent of its entire energy supply from the burning of fossil fuels like coal, oil, and natural gas, six percent from nuclear power, and the remaining 26% from renewable sources, including wind, solar power, and hydropower [10]. Due to recent advancements and commitments to renewable and sustainable power production, renewable energy sources (RES) like solar panels, wind, hydroelectricity power, and hydrogen technology have become preferred and essential integration into the electrical power system [11]. Increasing renewable energy is a precondition for achieving a clean and green environment. Consequently, it is necessary to switch to a carbon-free energy system, and it is critical to understand the elements that contribute to energy efficiency [12]. As rechargeable batteries promise to convince the financial, energy, and power requirements for stationary applications, they are playing a bigger role in the development of renewable energy resources. This attempts to timely offer a summary of the approaches put forth thus far to get through the obstacles still standing in the way of the current aqueous battery technologies using concentrated electrolytes [13]. A good rechargeable battery should be small, inexpensive, and quick to charge and discharge. The dominant option for storage classes is the rechargeable battery, which is charged by an internal chemical reaction [14]. Table 1 shows the characteristics of lead-acid (SLA), nickel metal hydride (NiMH), nickel–cadmium (NiCd), and lithium ions (Li-ions).

2 Background of Rechargeable Energy 2.1 Lead-Acid (SLA) Lead-acid batteries (LAB) are widely used in uninterruptible power supplies, electric cars, energy storage, traction and starting lighting, and ignition (SLI) batteries [15]. Gaston Planté devised the lead-acid battery in 1859, and it remains one of the earliest chemical energy storage systems. Many applications have been discovered over the last 160 years, and they are still widely used, for example, as alternative power sources or batteries for vehicles. When a lead-acid battery is discharged, lead (IV)

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oxide and lead (II) sulfate (IV) are created from metallic lead on the negatively charged electrode and the positively charged electrode, respectively. The electrolyte sulfuric (VI) acid is used in both processes [16]. The following is the discharge reaction: Pb + PbO2 + 2H2 SO4 ↔ 2PbSO4 + 2H2 O

(1)

LAB is one of the most frequently utilised and cost-effective electrical energy storage devices, and it is widely employed in most automobiles to power electrical circuits. A fully charged lead acid battery typically has a voltage of roughly 12.6 V. The capacity qualities of lead-acid batteries generally deteriorate over time. This electrochemical system degrades due to either a sluggish or partial discharge, as well as harsh circumstances (temperature fluctuations, vibrations).

2.2 Nickel-Metal Hydride (NiMH) In general, NiMH batteries are more durable and have longer lifetime cycles, nonetheless, their power and density of energy are lesser [17]. The NiMH battery cannot be recharged; the electrode, for example, is built of a porous alloy of rare earth metals made up of 30 percent, which includes the La10.5 Ce4.3 Pr0.5 Nd1.4 Ni60.0 Co12.7 Mn5.9 A14.7 alloy (in which the numbers denote athe atomic percent of the components) [18]. The automotive sector, such as first generation electric and hybrid vehicles, accounts for an estimated 70% of NiMH battery applications. However, NiMH cells are becoming less popular in the rechargeable battery market as lithium-ion batteries (LIB) replace them. Currently, NiMHs and LIBs account for approximately 28 and 37% of the global rechargeable battery market, respectively, and their consumption is expanding as a result of the global proliferation of electronic devices [19]. Ni-MH batteries utilise a hydride-forming alloy to be the negative electrode (H2 O + M + e OH + MH, M: metallic alloy), nickel hydroxide for the positive electrode (Ni(OH)2 + OH NiO(OH) + H2 O + e), and potassium hydroxide (KOH) for the electrolyte [20]. NiMH batteries have around double the volume of NiCd batteries and far higher energy efficiency versus LIB [21]. NiMH batteries might serve as a secondary supply of limited earth elements, as well as cobalt and nickel. NiMH battery recycling will not only offer economic value, but it will also preserve the environment [22].

2.3 Nickel–Cadmium (NiCd) Since they were created at the beginning of the twentieth century, nickel–cadmium batteries have been a preferred battery option for numerous uses, especially where

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51

high levels of current or an excessive amount of cycles are required. Substitutes are nevertheless frequently employed in a variety of uses, such as emergency lights, medical equipment, security systems, and transportable electric appliances. Also, considering various constraints in the use of nickel–cadmium batteries in Europe, manufacturing is not limited; in fact, it is increasing. Alkaline batteries are currently employed in railway transportation, aircraft, electric cars, and other applications. NiCd batteries, which are backup rechargeable batteries, have an anode made of metallic cadmium, a cathode of nickel oxyhydroxide, and an alkaline electrolyte like potassium hydroxide [23]. To improve the conductive qualities of nickel and cadmium hydroxide powders, graphite and reduced iron oxide powder are commonly used. Cadmium is a dangerous heavy metal that exists naturally in nature, although it is widely employed in a variety of industrial areas. For example, manufacturing workers of nickel–cadmium batteries are significantly exposed to cadmium dust and fumes by inhalation [24].

2.4 Lithium-Ion (Li-Ion) When compared to other batteries, lithium-ion batteries have the benefits of having significant particular energy, a substantial amount of energy, longer durability, minimal discharge rate, and a lengthy lifespan. The health hazards of lead and the rise of lithium-ion batteries were both cited as reasons for the downfall of lead-acid batteries [25]. Studies show that Li-ion batteries outperform lead-acid battery technology in terms of power and energy density, maintenance requirements, and number of cycles [26]. LIBs have been studied extensively around the world and have a wide range of practical uses, including electronic devices and electric vehicles [27]. LIBs have long been the favoured green batteries. Lithium-ion batteries have increased in popularity over the past several years across a number of industries due to cost savings and ongoing advancements in manufacturing technology. As seen in Fig. 1, lithium batteries are frequently used in energy storage devices such as power tools, military equipment, and aerospace, as well as water, fire, wind, and solar power plant.

3 Current Trend The energy requirements of the globe might be satisfied by renewable energy sources while also preserving the environment and ensuring the availability of energy. Table 2 categorises the major renewable energy (RES) sources and their various applications. Table 3 represents the projected global landscape for renewable energy sources until 2040 [28]. Unsteady electricity generation is one concern with renewable energy. Therefore, more energy must be saved to make up for variations in the source of power. Given

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Fig. 1 LIB’s application scenario and operating philosophy

Table 2 Main renewable energy resources with usage form Energy resources

Energy conversion and usage option

Hydropower

Power generation

Biomass

Heat and power generation, pyrolysis, gasification, digestion

Geothermal

Urban heating, power generation, hydrothermal, hot rock

Solar

Solar home systems, solar dryers, solar coolers

Direct solar

Photovoltaic, thermal power generation, water heaters

Wind

Power generation, wind generators, windmills

Wave

Numerous designs

Tidal

Barrage, tidal streams

its substantial density of energy, great specific energy, and strong recharge capabilities, the LIB, being an established technology, maybe a contender for future energy storage. Recycle is essential to the long-term viability of batteries and is determined by factors specific to batteries, which include the environmental risks they pose and the worth of the materials they are made of. As an outcome, recycling should be

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Table 3 Global renewable energy landscape by 2040 Year

2001

2010

2020

2030

2040

Total consumption (million tons equivalent)

10,038

10,549

11,425

12,352

13,310

Biomass

1080

1313

1791

2483

3271

Large hydro

22.7

266

309

341

358

Geothermal

43.7

86

186

333

493

Small hydro

9.5

19

49

106

189

Wind

4.7

44

266

542

688

Solar thermal

4.1

15

66

244

480

Photovoltaic

0.1

2

24

221

784

Solar thermal electricity

0.1

0.4

3

16

68

Marine (tidal/wave/ocean)

0.05

0.1

0.4

3

20

Total RES

1365,5

1745,5

2964,4

4289

6351

Renewable energy contribution source (%)

13.6

16.6

23.6

34.7

47.7

considered while establishing battery systems. To create a circular economy, a material needs to have some parts, a secondary process that is less expensive than the first process, a straightforward purifying flowsheet, precious parts, and a mechanism for accumulation and classification. Additionally, it is beneficial if the substance has significant effects on the environment if it is not recycled because this usually makes recycling essential. A recycling process can benefit from pyrometallurgical or thermal processing methods in a number of ways, involving a greater capacity and the consumption of fewer chemicals. Thermal battery recycling mainly involves introducing reducing agents to used battery materials with the goal of producing alloys and metal oxides right away [29]. Figure 2 shows a flowchart that describes the pyrometallurgical recycling of LIB, Ni–Cd, and NiMH batteries. Many waste NiMH batteries will be generated as lithium batteries become more popular, and NiMH batteries become less popular [30]. Since the number of electric vehicles (EVs) is growing quickly and their batteries are so large (the Tesla Model 3 Long Range battery has 4416 cells and weighs 480 kg), a lot of LIB waste is being produced each year and will continue to do so. If this waste is not recycled and used again, it will have a major adverse effect on the environment and hasten the loss of mineral reserves [31]. One of the top goals for electrical grid structures around the world is the desire for alternative energy generating, transport, and storage technologies. Designing rechargeable electrochemical power sources is crucial for the growing alternative energy industry [32]. In practice, batteries are usually kept in storage for a long time until utilized, hence their lifespan is a crucial performance metric that shows how inner adverse reactions affect the battery’s efficiency. The mechanism and corresponding inhibition technique of self-discharge was investigated in order to improve

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Fig. 2 The flow diagram for pyrometallurgical recycling of Li-ion, Ni–Cd, and NiMH batteries

the battery’s shelf life, and it was discovered that the electrolyte composition is a major element influencing the battery’s shelf life. Renewable energy is viewed as one of the preferred options for adoption in electric grid applications because the usage of fossil fuels, the main energy provider, is hurting the environment due to rising carbon dioxide emissions [33]. Other technologies, such as lithium-ion (Li-ion) batteries, are crucial for the global supply of rechargeable devices, including handheld electronics and electric cars. On a broader

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scale, grid-scale energy storage for renewable energy sources like tide and wind power is also vital [34]. To build a sustainable society, carbon peaking and carbon neutrality policies are advocated. In this context, the development of improved energy storage devices has become an essential compensation for intermittent renewable energy [35]. Flexible energy storage devices, one of the most essential elements of nextgeneration power sources, are at the forefront. However, problems exist in almost all of the recently produced hydrogel electrolytes. In this case, a simple and costeffective approach must be devised. Ionic liquids (ILs) have attracted a lot of attention in recent years due to their outstanding temperature stability, outstanding ion conductivity, and capacity to tolerate high voltages without first decomposing. Ionic liquids are unique, adaptable electrolyte media [36]. Only a few polymer electrolytes are now commercially viable; nonetheless, demand for solid-state electrochemical devices with excellent stability and performance is steadily increasing. To widen the alternatives, it is essential to design polymer electrolytes with high ionic conductivity and chemical stability. Those inventions may enlighten the future in terms of securing energy sources. Acknowledgements The authors are grateful for the financial support given by the Universiti Malaysia Pahang Al-Sultan Abdullah (UMPSA) for the Internal Grant—RDU202403 entitled Material Testing and Evaluation Process for Battery Performance and Durability in TNB Distribution. The assistance provided by the Faculty of Chemical and Process Engineering Technology and MNR Multitech Sdn. Bhd. is also acknowledged.

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An Integrated TOPSIS Model with Exponential Intuitionistic Entropy Measure for Multi-Attribute Decision-Making (MADM) Omar Ayasrah , Faiz Mohd Turan , and Sheikh Muhammad Hafiz Fahami

Abstract The determination of attribute weights in solving multi-attribute decisionmaking (MADM) problems is crucial and significantly impacts the results. Many researchers have highlighted the effectiveness of deriving attribute weights objectively based on the assessments provided by decision-makers for MADM problems. One approach involves using entropy measures to determine weights based on the given ratings. This paper introduces a novel intuitionistic fuzzy entropy measure that takes the form of an exponential function. This new entropy measure is combined with the TOPSIS method to propose a new decision-making method for solving MADM problems. The proposed method does not require attribute weights, thereby eliminating the need for their determination. Keywords TOPSIS · Exponential intuitionistic entropy measure · MADM

1 Introduction Multi-attribute decision-making (MADM) constitutes a pivotal process aimed at resolving issues associated with selecting the most appropriate solution or option based on pre-defined criteria [1]. These methods are commonly deployed to determine the optimal choice while taking into account multiple criteria or attributes [2, 3]. The fundamental goal is to furnish decision-makers with an effective and logical approach to thoroughly assess both objective and subjective aspects of the given problem [4–6]. To attain more accurate results and handle imperfect or imprecise data, researchers have increasingly turned to the application of fuzzy set theory and intuitionistic fuzzy set theory [7]. The realm of fuzzy MADM has garnered noteworthy attention as a significant field of research [8]. O. Ayasrah · F. Mohd Turan (B) · S. M. H. Fahami Faculty of Manufacturing and Mechatronic Engineering Technology, Universiti Malaysia Pahang Al-Sultan Abdullah, 26600 Pekan, Pahang, Malaysia e-mail: [email protected] © The Author(s), under exclusive license to Springer Nature Singapore Pte Ltd. 2024 R. Abd. Aziz et al. (eds.), Intelligent Manufacturing and Mechatronics, Springer Proceedings in Materials 40, https://doi.org/10.1007/978-981-99-9848-7_6

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The Technique for Order of Preference by Similarity to Ideal Solution (TOPSIS) is a widely used and dominant method in the field of multi-attribute decision-making (MADM). It is preferred due to its simplicity in understanding and implementation compared to outranking techniques [9]. Zimmer [10] also concluded that TOPSIS is the leading MADM method among others, primarily due to its ease of understanding and implementation. Additionally, combining TOPSIS with intuitionistic fuzzy sets (IFS) can enhance the decision-making process by effectively handling uncertainty, fuzziness, and imprecise information. The resolution of a multi-attribute decision-making (MADM) quandary is derived from the preferences of a collective of decision-makers. Given the inherent uncertainty and imprecision in the available data, Decision Makers (DMs) resort to employing Intuitionistic Fuzzy Networks (IFNs) to articulate their preferences and create a decision matrix [11, 12]. The foundation of fuzzy set theory (FS) was originally put forth by Zadeh [13], which has garnered significant interest across various domains. Expanding on FS, Atanassov [14] introduced Intuitionistic Fuzzy Sets (IFS) as a broader extension of the theory, which has since attracted even more attention since its inception. In the context of multi-attribute decision-making (MADM), a multitude of criteria exist, and their respective weights wield substantial influence in the assessment of various alternatives [15]. The allocation of weights to these criteria significantly shapes the ultimate ranking sequence of alternatives and the overarching aggregation procedure [16]. Two primary categories for criteria weight assignment emerge: subjective methods, which hinge on decision-makers’ opinions and inputs (often accomplished through methods like the Analytic Hierarchy Process or AHP), and objective methods, including the utilization of the Entropy method [17]. As proposed by Hatefi [18], an alternative approach for determining criteria weights has surfaced. This method is grounded in the decision matrix and preference values, diverging from solely relying on direct evaluations furnished by decision-makers. The “Dispersion Logic” incorporated in this approach endows lower weights to criteria showcasing similar values across the alternatives. Entropy serves as a metric for quantifying the level of vagueness present in a fuzzy set [19]. The concept of fuzzy entropy was initially introduced by Zadeh [20], followed by further exploration of its definition by Deluca and Termini [21]. Subsequently, several fuzzy entropy measures were introduced to capture different aspects of vagueness. In particular, the entropy measure for Intuitionistic Fuzzy Sets (IFS) was introduced by Burillo and Bustince [22]. Many of the existing Intuitionistic Fuzzy (IF) entropy techniques have overlooked the influence of the intuitionistic index effect [23]. This paper presents a novel IF entropy measure that takes into account the impact of the hesitancy degree, in addition to membership and non-membership degrees. Subsequently, a new multi-attribute decision-making (MADM) method is proposed based on this new IF entropy measure and the TOPSIS technique. This approach eliminates the need for attribute weighting in the decision-making process [24].

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2 Methodology The adapted methodology for developing a new intuitionistic fuzzy entropy measure and integrating it into an exponential-based function with the TOPSIS technique is illustrated in Fig. 1. The process begins with the development of the new IF-Entropy measure, which undergoes an iterative process until it is mathematically validated against the predefined axioms (refer to Definition 3). The IF-Entropy, serving as a measure of the fuzziness in decision makers’ preferences, eliminates the requirement to determine criteria weights in MADM problems. This simplifies the resolution of MADM problems. Furthermore, the selection of the TOPSIS technique enhances the ease of implementation when addressing multicriteria problems such as selecting the best project, choosing an appropriate plant or distribution centre location, determining the optimal supplier(s), and more. The validation process will involve presenting a mathematical proof for the new IF-Entropy measure. Additionally, secondary examples from previously published Fig. 1 Proposed methodology

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research will be used to compare the results obtained from the new MADM method with the outcomes generated by employing comparable methods. This comparative analysis will further validate the effectiveness and superiority of the proposed approach.

3 Preliminary Results 3.1 A New Intuitionistic Fuzzy Entropy Measure The measure presented by Eq. (1) is an IF entropy. ( | 2 | ) n |μ − ν 2 | 1∑ π − π E(A) = tan n i=1 4 4

(1)

Proof: xi, ( for A 2= {< ) μA (xi), VA (xi)} ∀ xi ∈ X: |ν −μ2 | π 0 ≤ 4 − 4 π ≤ π4 , then: ( ) |ν 2 −μ2 | 0 ≤ tan π4 − 4 π ≤ 1, thus 0 ≤ E(A) ≤ 1. ( ) n ∑ |μ2 −ν 2 | • For E(A) = 0; then, E(A) = n1 tan π4 − 4 π = 0, therefor i=1 ( ) | 2 | | 2 | |μ2 −ν 2 | π 2| | tan 4 − 4 π = 0, thus μ − ν =1 |μ − ν 2 |=1 when μA (×i ) = 1, VA (xi ) = 0 or μA (xi ) = 0, VA (xi ) = 1, so, A is a crisp set. ( ) n ∑ |μ2 −ν 2 | • For E(A) = 1; then, E( A) = n1 tan π4 − 4 π = 1, that mean i=1 ( ) | | |μ2 −ν 2 | tan π4 − 4 π = 1, thus |μ2 − ν 2 |=0 | 2 | |μ − ν 2 |=0 when μA (xi ) = VA (xi ). ( ) n ∑ |ν 2 −μ2 | • For Ac = {< xi, VA (xi ), μA (×i )} ∀ xi ∈ X, E(Ac ) = n1 tan π4 − 4 π = i=1 ( ) n |μ2 −ν 2 | 1 ∑ π E(A) = n tan 4 − 4 π = E(A) i=1 ( ) 2 2 | • For A ⊆ B, we have ƒ(μ, V) = tan π4 − |μ −ν π , , when μ ≤ V the function 4 ( ) 2 2 ν −μ can be rewritten as ƒ(μ, V) = tan π4 − 4 π the derivatives of ƒ(μ, V) to μ and V: ( ) π πμ ν 2 − μ2 ∂f(μ, ν) = sec2 − π ∂μ 2 4 4

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( ) πν ν 2 − μ2 ∂f(μ, ν) 2 π =− sec − π ∂ν 2 4 4 when μ ≤ V, we have ∂f(μ,ν) ≥ 0 and ∂f(μ,ν) ≤ 0, then ƒ(μ, V) is increasing with μ ∂μ ∂ν and decreasing with V. Therefore, when μB ≤ VB and μA ≤ μB , VA ≥ VB , we have ƒ(μA , VA ) ≤ ƒ(μB , VB ).

3.2 The Intuitionistic Fuzzy MADM Method Based on the New iF Entropy Suppose a MADM problem, with given Ai = {A1 , A2 ,…,Am } as a set of m alternatives, to be evaluated by a group of decision makers (DMs) Dk = {D1 , D2 ,…,Dí }, based on a set of attributes Uj = {U1 , U2 ,…,U ) of Dk rating of alternative Ai ( n }. the

according to attribute Uj in IF value aikj = μikj , νikj (i = 1,2,..,m; j = 1,2,..,n; k = 1,2,…,í). Where a given weights for DMs λk = (λ1 , λ2 ,…, λí ). • Step 1: The DMs evaluations as individual assessment matrices to be aggregated by using the IFWA operator (Eq. 2) to build the group assessment matrix (Rmxn ). (

i i ∏ ( )λk ∏ ( k )λk 1 − μikj , vi j I F W A(d1 , d2 . . . ., dl ) = 1 − k=1

) (2)

k=1

where λ= (λ1 , λ2 , λ3 ,….. λi )T is the assigned DMs’ weights vector. ⎤ (μ11 ,ν11 ) (μ12 ,ν12 ) . . . (μ1n ,ν1n ) ⎢ (μ21 ,ν21 ) (μ22 ,ν22 ) . . . (μ2n ,ν2n ) ⎥ ⎥ ⎢ ⎥ ⎢ .. ⎥ ⎢ . Rmxn (ai j ) = ⎢ ... ... ... ⎥ ⎥ ⎢ . . ⎦ ⎣ . ... ... ... (μm1 ,νm1 ) (μm1 ,νm1 ) . . . (μmn ,νmn ) ⎡

(3)

• Step 2: Using Eq. (4) to calculate the entropy exponential matrix (EEMmxn ); I E E( A) = e where; EE(A) ∈ [1,e].

( ( )) 2 2 tan π4 − μ −v π 4

(4)

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⎡

E E 11 (a11 ) E E 11 (a11 ) ⎢ E E 21 (a21 ) E E 22 (a22 ) ⎢ ⎢ .. .. E E Mmxn (E E i j (ai j )) = ⎢ . . ⎢ ⎢ . . .. .. ⎣ E E m1 (am1 ) E E m2 (am2 )

⎤ · · · E E 1n (a1n ) · · · E E 2n (a2n ) ⎥ ⎥ ⎥ .. .. ⎥ . . ⎥ ⎥ .. .. ⎦ . . · · · E E mn (amn )

(5)

• Step 3: Determine the entropy exponential-based separation measures by using Eqs. (6–7); [ | n |∑ [( ( ( )))]2 + + 1 − E E Mmxn ai j di (A , Ai ) = |

(6)

i=1

[ | n |∑ [( ( ))]2 − − d (A , Ai ) = | E E Mmxn ai j i

(7)

i=1

• Step 4: Compute the closeness coefficient for each alternative (Eq. 8); CCi =

di− (A− , Ai ) Ai ) + di+ (A+ , Ai )

di− (A− ,

(8)

• Step 5: Rank alternatives based on closeness coefficient values in descending order.

4 Illustrative Examples In the context of a company seeking to invest in a suitable firm, three distinct alternative firms from various fields are under consideration: A1 (light vehicles), A2 (television), and A3 (nutrition). The assessment of these alternatives is based on three specific criteria: U1 (investment challenges), U2 (growth), and U3 (environmental impact). To make informed decisions, the company has engaged three decisionmakers (DMs): D1 (High-level manager), D2 (Middle manager), and D3 (Low-level manager). For the purpose of this scenario, the weights assigned to the DMs are defined as follows: λ1 = 0.36, λ2 = 0.32, and λ3 = 0.32. Additionally, the weights assigned to the criteria are as follows: w1 = 0.01, w2 = 0.49, and w3 = 0.50. The preferences of each individual DM are outlined in Table 1. Steps 1 and 2 involve the aggregation of individual assessment matrices utilizing the Intuitionistic Fuzzy Weighted Averaging (IFWA) operator. This results in the

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Table 1 The individual decision matrix DMs D1

D2

D3

Alternatives

Attributes U1

U2

U3

A1

(0.8,0)

(0.5,0.3)

(0.5,0.2)

A2

(0.85,0.01)

(0.85,0.15)

(0.8,0.1)

A3

(0.99,0.01)

(0.9,0.05)

(0.85,0.05)

A1

(0.1,0.9)

(0.15,0.7)

(0.2,0.6)

A2

(0.2,0.65)

(0.35,0.6)

(0.3,0.5)

A3

(0.25,0.01)

(0.5,0.4)

(0.4,0.4)

A1

(0.05,0.95)

(0.2,0.75)

(0.15,0.65)

A2

(0.15,0.8)

(0.4,0.6)

(0.3,0.6)

A3

(0.35,0.6)

(0.5,0.4)

(0.35,0.5)

formation of the group assessment matrix, and finally calculate the entropy exponential matrix as depicted in Table 2. In steps 3 to 5, the process entails the computation of separation measures. This involves calculating the Closeness Coefficient (CC) for each alternative. Subsequently, the alternatives are ranked based on these computations as depicted in Table 3. Table 4 displays the ranking of alternatives based on the proposed method, juxtaposed with a comparative analysis of results acquired from other methods. A substantial majority of these methods indicate that alternative A3 is the preferred Table 2 The aggregated assessment matrix and the entropy exponential matrix Aggregated assessment matrix

Attributes U1

U2

U3

A1

(0.467,0)

(0.311,0.527)

(0.311,0.414)

A2

(0.554,0.155)

(0.626,0.364)

(0.554,0.297)

A3

(0.849,0.037)

(0.72,0.189)

(0.626,0.203)

Entropy exponential matrix

U1

U2

U3

A1

2.024

2.115

2.432

A2

1.881

1.93

2.022

A3

1.252

1.538

1.749

Table 3 The preference order of alternatives Alternatives

Attributes

di− (A− , Ai )

di+ (A+ , Ai )

Closeness coefficient

Rank

U1

U2

U3

A1

2.024

2.115

2.432

2.083891

3.805867

0.646184

3

A2

1.881

1.930

2.022

1.63876

3.3692

0.672769

2

A3

1.252

1.538

1.749

0.955957

2.644133

0.734463

1

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Table 4 Preference order comparison of alternatives for various methods Method

Parameter

Preference order 1

2

3

Xu 2010

A3

A1

A2

Yue 2014

A1

A3

A2

Zeng and Su 2011

A3

A2

A1

Chen et al. 2016 Liu et al. 2019

The proposed method

A3

A2

A1

U=−4

A3

A1

A2

U=0

A3

A1

A2

U=4

A1

A3

A2

A3

A2

A1

option among the three alternatives, with over 70% of the outcomes supporting this conclusion.

5 Discussion and Analysis of the Integrated Approach The newly integrated approach capitalizes on the strengths of both the IF-TOPSISEF and variable weight theory methodologies. Through refining these methods to address their limitations, a novel combined approach was formulated, subsequently validated for its efficacy and viability by comparing its outcomes against those of other established methods. This newly developed approach offers several advantages over alternative methods, including the two foundational methods: • It introduces a novel objective technique to determine the weights of decisionmakers (DMs) that vary based on the attributes involved in MCDM problems. • The approach incorporates an intuitionistic fuzzy entropy measure as an exponential-related function to rank alternatives. This measure accounts for the inherent fuzziness in the available information, contributing to the robustness of the method. • The utilization of two aggregation operators (IFWA and IFWG) empowers the approach to conduct sensitivity analysis, allowing the assessment of how alternative rankings might shift when employing different aggregation operators. • The innovative use of an exponential-related function, based on the proposed entropy measure, facilitates the determination of the separation measures of individual alternatives from positive and negative ideal solutions. This capability enables the method to effectively handle both independent and dependent attributes, unlike traditional Euclidean distance measures which assume implicit attribute independence.

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• The method offers diverse rankings of alternatives as potential solutions to the MCDM problem. These rankings vary according to DMs’ weight parameters and the chosen aggregation operator. This sensitivity analysis aspect empowers decision-makers to confidently select the most stable alternative as the MCDM problem solution. • The development of a mathematical model for a mobile application based on the new method allows DMs to virtually provide preferences and work on MCDM problems without the necessity of physical presence. This virtual approach enhances efficiency, particularly in unique contexts like pandemic situations. • The rationale for employing IF entropy in the exponential-related function form is supported by the following points: – The use of an exponential-related function, as demonstrated in the IFTOPSISEF baseline method, simplifies the original IF-TOPSIS approach by converting DMs’ membership, non-membership, and hesitancy degrees into a single value during the MCDM implementation. – The originally employed exponential-related function in the IF-TOPSISEF method was validated against the proposed axioms by the author, although these axioms lack reference in the literature review. – The utilization of IF entropy enhances the validation process’s rationality due to the presence of predefined axioms in the literature for IF entropy, serving as the basis for validation. – Entropy serves as a measure of fuzziness, and the time required to calculate attribute weights also depends on the fuzziness of DMs’ preferences. Hence, IF entropy in exponential-related form can contribute to determining attribute weights while implementing the new MCDM method.

6 Conclusion Entropy, as a measure of the vagueness of a fuzzy set, has been widely utilized in various studies to determine attribute weights and address multi-attribute decisionmaking (MADM) problems. In this paper, we propose a novel approach that combines the TOPSIS method with the newly introduced intuitionistic fuzzy entropy, formulated in an exponential manner, to tackle MADM problems. This novel MCDM approach underscores its broad applicability across various MCDM domains. This is achieved through the introduction of a method that incorporates variable DMs’ weights using an objective technique. Additionally, the approach offers a sensitivity analysis as an integral facet of the MCDM problem solution. Notably, the method’s virtual deployment capability is also highlighted as a significant contribution. This pioneering method obviates the necessity to explicitly ascertain or compute attribute weights. Furthermore, the method’s applicability extends beyond its current context and could be employed in diverse decision-making scenarios. In forthcoming

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research endeavors, the intention is to further refine this method by integrating objective criteria for establishing decision-makers’ weights within an intuitionistic fuzzy framework. Acknowledgements The authors would like to thank the Universiti Malaysia Pahang Al-Sultan Abdullah, Grant No. RDU220342 for providing financial support the facilities.

References 1. Govindan K, Rajendran S, Sarkis J, Murugesan P (2015) Multicriteria decision making approaches for green supplier evaluation and selection: a literature review. J Clean Prod 2015(98):66–83 2. Chin K-S, Fu C, Wang Y (2015) A method of determining attribute weights in evidential rea-soning approach based on incompatibility among attributes. Comput Ind Eng 87:150–162 3. Aikhuele D, Turan F (2017) Extended TOPSIS model for solving multi-attribute decision making problems in engineering. Decis Sci Lett 6(4):365–376 4. Yue C (2017) Entropy-based weights on decision makers in group decision-making setting with hybrid preference representations. Appl Soft Comput 60:737–749 5. Wan S, Wang F, Dong J (2017) Additive consistent interval-valued intuitionistic fuzzy preference relation and likelihood comparison algorithm-based group decision making. Eur J Oper Res 263(2):571–582 6. Turan FM, Omar B (2013) A three-stage methodology for design evaluation in product development. Universiti Tun Hussein Onn Malaysia 7. Liu S, Yu W, Liu L, Hu Y (2019) Variable weights theory and its application to multi-attribute group decision making with intuitionistic fuzzy numbers on determining decision maker’s weights 8. Wan S-P, Dong J-Y (2015) Interval-valued intuitionistic fuzzy mathematical programming method for hybrid multi-criteria group decision making with interval-valued intuitionistic fuzzy truth degrees. Inf Fusion 26:49–65 9. Memaria A, Dargi A, Jokara M, Ahmad R, Rahim ARA (2019) Sustainable supplier selection: a multi-criteria intuitionistic fuzzy TOPSIS method 10. Zimmer K, Frohling M, Schultmann F (2016) Sustainable supplier management–a review of models supporting sustainable supplier selection, monitoring and development. Int J Prod Res 54(5):1412–1442 11. Eslaminasab Z, Hamzehee A (2019) Determining appropriate weight for criteria in multi criteria group decision making problems using an Lp model and similarity measure 12. Aikhuele DO, Turan FBM (2016) Intuitionistic fuzzy-based model for failure detection. Springerplus 5(1):1–15 13. Zadeh LA (1965) Fuzzy sets. Inf Control 8:338–353 14. Atanassov KT (1986) Intuitionistic fuzzy sets. Fuzzy Sets Syst 20:87–96 15. Choo EU, Schoner B, Wedley WC (1999) Interpretation of criteria weights in multicriteria decision making. Comput Ind Eng 37(3):527–541 16. Garg H (2017) Generalized intuitionistic fuzzy entropy-based approach for solving multiattribute decision-making problems with unknown attribute weights 17. Arian H, Ashkan H, Huchang L, Francisco H (2019) An overview of MULTIMOORA for multi-criteria decision-making: theory, developments, applications, and challenges 18. Hatefi M (2019) Indifference threshold-based attribute ratio analysis: a method for assigning the weights to the attributes in multiple attribute decision making 19. Liu M, Ren H (2014) A new intuitionistic fuzzy entropy and application in multi-attribute decision making. Information 5(4):587–601

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20. Zadeh LA (1968) Probability measures of fuzzy events. J Math Anal Appl 23:421–427 21. De Luca A, Termini S (1972) A definition of non-probabilistic entropy in the setting of fuzzy set theory. Inf Control 20:301–312 22. Burillo P, Bustince H (2001) Entropy on intuitionistic fuzzy sets and on interval-valued fuzzy sets. Fuzzy Sets Syst 118:305–316 23. Atanassov KT (1999) Intuitionistic fuzzy sets. Springer, New York, NY, USA 24. Ayasrah O, Turan FM (2021) A review of multi-criteria decision-making methods using application of variable weight theory and IF-TOPSIS-EF. Recent trends in manufacturing and materials towards Industry 4.0: selected articles from iM3F 2020, Malaysia, pp 13–24

Enhancing MIG Weld Bead Geometry in Hot Rolled Carbon Steel Through Response Surface Methods Optimization Junita Mohd Said and Faiz Mohd Turan

Abstract This study is focused on optimizing the geometry of weld beads in Metal Inert Gas (MIG) butt-welding of hot rolled carbon steel. The quality of welding holds significant sway over the integrity of joints, and various parameters during the welding process can influence this quality. With the advent of computerization and automation, innovative statistical techniques for modelling and optimization have arisen, obviating the need for traditional trial-and-error approaches to achieve desired performance and quality. The research employs experimental methodologies, incorporating critical process parameters like welding current, arc voltage, and welding speed. A central composite design utilizing Response Surface Methodology (RSM) is employed as a statistical approach to experimentally analyse the performance of weld bead geometry. This encompasses aspects such as bead height, bead width, and penetration. The ultimate objective is to establish a mathematical relationship between welding process parameters and output variables. The outcomes derived from these models yield precise predictions of weld bead geometry. By utilizing these mathematical models for specific bead geometries, the influence of process parameters can be estimated. It’s evident that variations in parameters have a notable impact on bead height and width, in comparison to the effect on penetration alone. Keywords Failure · Weld bead geometry · RSM · Optimisation

J. M. Said · F. Mohd Turan (B) Faculty of Manufacturing and Mechatronic Engineering Technology, Universiti Malaysia Pahang Al-Sultan Abdullah, 26600 Pekan, Pahang, Malaysia e-mail: [email protected] J. M. Said University Kuala Lumpur Malaysia France Institute (UniKL MFI), 43650 Bandar Baru Bangi, Selangor, Malaysia © The Author(s), under exclusive license to Springer Nature Singapore Pte Ltd. 2024 R. Abd. Aziz et al. (eds.), Intelligent Manufacturing and Mechatronics, Springer Proceedings in Materials 40, https://doi.org/10.1007/978-981-99-9848-7_7

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1 Introduction Welding is a complex process used for joining parts, and the quality of the weld is influenced by various input parameters. Establishing the relationship between welding quality and process parameters is challenging due to the nonlinear nature of the process [1]. Fatigue failures in engineering structures often occur at welded connections, posing a significant threat to structural integrity [2–4]. Welding discontinuities, such as lack of penetration, undercutting, slag inclusion, and gas pores, can adversely affect the quality of the weld joint. The rate of energy input also plays a role in weldment characteristics, impacting welding quality, productivity, and cost [5–8]. Metal Inert Gas (MIG) welding finds extensive application in diverse industries such as manufacturing, oil and gas, and construction, owing to its ease of use and robustness [9–11]. In the MIG welding process, a concentrated fusion zone is established by introducing transient heat between the filler metal and the base metal. Essential variables in this procedure encompass welding speed, current, voltage, distance between the nozzle and the plate, torch angle, and electrode diameter [12]. The advancement of computer and technology has led to the utilization of optimization techniques, such as Design of Experiments (DoE), in the manufacturing domain. These techniques aim to improve performance, quality, and cost efficiency [13]. Extensive research has been conducted to enhance weldment characteristics through theoretical developments, statistical analysis, and experimental investigations [14–17]. Optimizing welding parameters is crucial for achieving optimal welding quality and predicting weld bead geometry, mechanical properties, and Heat Affected Zones (HAZ) [18, 19]. Traditionally, defining suitable weld input parameters for a new welded joint product with specific requirements through trial and error is time-consuming. However, the Response Surface Methods (RSM) technique, a well-known optimization technique, allows for efficient analysis of experiments with minimal effort [20, 21]. RSM combines mathematical and statistical techniques to develop prediction models and optimize the variables influencing the response of interest [22]. These methods enable the prediction of system responses and assist in defining optimal parameter settings with minimized experimental effort [23]. The focus of this article is centered around evaluating the influence of welding parameters on the weld bead of 3 mm thick hot rolled carbon steel plates (JIS G3131). Empirical investigations were conducted using the Central Composite Design (CCD) matrix. The main objective of this study was to optimize the process parameters in order to achieve the maximum aspect ratio of the weld bead while maintaining acceptable dimensions for the weld bead. The boundaries of the welding parameters were also defined. To achieve this, the study employed Response Surface Methodology (RSM) to construct mathematical models that predict the relationship between processing parameters and the configuration of the weld bead. These regression models are valuable tools for determining the optimal welding conditions, thereby providing significant insights for enhancing production practices.

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2 Methodology The welding experimental process was devised employing Response Surface Methodology (RSM) as the statistical Design of Experiments (DoE) approach. The comprehensive sequence of the experimental methodology is depicted in Fig. 1. RSM was chosen due to its proficiency in modelling quadratic correlations and delivering dependable outcomes in identifying optimal welding conditions. RSM has been widely employed in forecasting weld-bead attributes and pinpointing optimal responses across diverse welding processes [24–26]. The primary objective of utilizing the RSM method is to ascertain the optimal operational conditions needed for the experiment. To streamline the analysis, suitable statistical software was employed to generate the design matrix and analyse the experimental data. This software enabled efficient processing and interpretation of the gathered data. Fig. 1 The experimental process flow for the research

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3 Results and Discussion The experimental results from each test material are presented in Table 1, showing the measured responses. The RSM technique was applied to analyse the experimental data and determine the regression models that best fit the data. The significance of the model terms was evaluated based on the associated p-values, with a threshold of 0.05 (α = 0.05, 95% confidence level). Terms with p-values less than 0.05 were considered statistically significant. The stepwise regression method was used to identify and eliminate irrelevant model terms. The variance value and significance of each model term were assessed. The overall model fit was evaluated using the verification coefficient (R2), which ranges from 0 to 1. A higher R2 value indicates a more accurate model. Table 1 Independent process variables and experimental design levels Std

Responses HI (J/cm)

Weld bead geometry WP (cm)

WW (cm)

WH (cm)

1

51.0

0.033

0.088

0.020

2

61.2

0.032

0.092

0.018

3

34.0

0.029

0.070

0.015

4

40.8

0.035

0.078

0.017

5

57.0

0.032

0.088

0.020

6

68.4

0.037

0.091

0.010

7

38.0

0.029

0.076

0.020

8

45.6

0.043

0.085

0.012

9

43.2

0.033

0.081

0.017

10

51.8

0.042

0.076

0.018

11

59.4

0.042

0.093

0.019

12

39.6

0.034

0.086

0.026

13

44.9

0.036

0.075

0.019

14

50.2

0.045

0.086

0.008

15

47.5

0.035

0.086

0.015

16

47.5

0.033

0.082

0.020

17

47.5

0.032

0.082

0.017

18

47.5

0.028

0.088

0.022

19

47.5

0.038

0.081

0.018

20

47.5

0.037

0.079

0.018

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3.1 The Validation Analysis of the RSM Model The analysis of variance tables of reduced quadratic models is presented in Tables 2, 3, and 4 respectively. Results of Heat Input (HI) in Table 2, shows the heat input model is the most significant model associated with the effect of the welding current (C), welding speed (S) and welding voltage (V), the second order effect (S2) and two-level interaction of current and speed (CS), Current and Voltage (CV) and Speed and Voltage (SV). A crucial attribute among welding parameters is Heat Input (HI), as it quantifies the energy transferred per unit length of the weld. Factors like preheated and interpass temperatures influence the cooling rate, which subsequently impacts the mechanical properties and metallurgical structure of both the weld and the Heat Affected Zone (HAZ). Heat Input can be directly computed, as illustrated in Eq. (1) [27–29]: H=

60.E.I S

(1)

where H is the heat input (J/mm); E the voltage (V); I the current (C); and S is the travel speed (mm/min). Table 2 ANOVA table for heat input (HI) reduced quadratic model Source

Sum of squares

df

Mean square

F-Value

Prob > F

Model

11,853,591

9

1,317,066

17,021.24

0.000

C

1,946,892

1

1,660,325

21,457.39

0.000

S

8,944,123

1

8,077,953

104,396.29

0.000

V

737,319

1

618,645

7995.13

0.000

CS

64,800

1

64,800

837.45

0.000

CV

5000

1

5000

64.62

0.000

SV

24,200

1

24,200

312.75

0.000

S2

54,715

1

44,617

576.61

0.000

Residual

387

5

77

Lack of Fit

387

2

193

Pure error

0

3

0

Total

11,853,978

14

Measures R2 = 1; Adjusted R2 = 1; Predicted R2 = 1

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Table 3 ANOVA for weld bead width (WW) reduced quadratic model Source

Sum of squares

df

Mean square

F-Value

Prob > F

Model

6.18176

9

0.68686

88.39

0.000

C

0.73170

1

0.71643

46.30

0.001

S

4.08974

1

3.34341

216.05

0.000

V

0.38328

1

0.15012

9.70

0.000

CS

0.12500

1

0.12500

8.08

0.036

CV

0.00045

1

0.00045

SV

0.00045

1

0.20480

13.23

0.015

S2

0.11447

1

0.29955

19.36

0.007

Residual

0.07738

5

0.01548

Lack of fit

0.00890

2

0.00445

Pure error

0.06848

3

0.02283

Total

6.25913

14

0.000

Measures R2 = 98.76%; Adjusted R2 = 59.64%; Predicted R2 = 91.83%

Table 4 ANOVA for weld bead height (WH) reduced quadratic model Source

Sum of squares

df

Mean square

F-Value

Prob > F

Model

1.03581

9

0.115089

10.47

0.009

C

0.33684

1

0.372057

33.84

0.002

CV

0.36551

1

0.365513

33.25

0.002

SV

0.07801

1

0.078013

7.10

0.045

C2

0.10182

1

0.075724

6.89

0.047

Residual

0.05497

5

0.010994

Lack of Fit

0.01087

2

0.005434

Pure error

0.04410

3

0.014700

Total

1.09077

14

Measures R2 = 94.96%; Adjusted R2 = 85.89%; Predicted R2 = 41.993%

3.2 Interaction Effect of Welding Process Parameter Towards Optimal Parameter The final mathematical expressions in un-coded factor are obtained as Eqs. (2–5) respectively. Furthermore, the manufacturing proposes using the developed model and the point prediction option in the software. These equations have been optimised simultaneously through response optimisation in the software, to measure the satisfaction of parameters level on every response. The targeted value for each response was set, as indicated in the response optimisation plot in Fig. 2. This figure illustrates the 100% acceptability result of optimal value. Three conformation experiments were

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77

conducted at optimum settings to verify the adequacy of the developed models, and to validate the optimal parameter. The test conditions were run at optimised predicted values. The list of detail parameters and responses are tabulated in Table 5. H I = 652.667 + 28.358(C) − 177.217(S) + 255.194(V )+       0.075 C 2 + 7.501 S 2 + 0.528 V 2 − 1.8(SC) − 11(SV ) W W = −98.212 − 0.615(C) − 1.95(S) + 17.31(V )+       0.003 C 2 + 0.019 S 2 − 0.502 V 2 + 0.003(SC)+

(2)

(3)

0.001(C V ) + 0.032(SV ) W H = −55.927 + 0.866(C) − 0.711(S) − 1.75(V )−       0.002 C 2 + 0.004 S 2 + 0.001 V 2 + 0.001(SC)− 0.021(C V ) + 0.019(SV )

(4)

W P = −54.29 + 0.348(C) − 1.202(S) + 5.151(V )−       0.003 C 2 + 0.013 S 2 − 0.197 V 2 + 0.004(SC)+ 0.017(C V ) + 0.008(SV )

(5)

4 Conclusions The comprehensive methodology of the RSM optimization technique for MIG butt welding of hot rolled carbon steel plates (JIS G3131 SPH270C) was thoroughly examined and subjected to statistical analysis. The aim was to assess a combination of optimal parameters against desired outcomes, specifically the penetration and weld bead characteristics of the Heat Affected Zone (HAZ). These attributes hold crucial significance for welded joints, as they contribute to reduced weld metal consumption by achieving greater penetration and smaller bead height and width. The mechanical and metallurgical traits of the welded joint are influenced by HAZ dimensions. Consequently, the study aimed to minimize HAZ width and depth, essential to prevent significant microstructural discrepancies between the HAZ and the parent metal. Mathematical models were derived from experimental data to explore the correlation between process parameter values and weld size responses. The residual plots of these responses indicate the model’s adequacy. Validation experiments corroborated the optimized outcomes, confirming that the optimum parameter values were determined as current 117A, speed 29 cm/min, and voltage 17 V. These results showcased notably improved welding conditions compared to the initial settings.

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Fig. 2 Result of response optimiser for experimental responses

Table 5 Conformation experimental and validation of optimised welding condition for WP, WW, WH responses Exp. No. Value

Responses

Weld bead geometry C (Amp) S (cm/min) V (volts) HI (J/ mm) 17

1 2 3

117

29

4137

WP (mm) WW (mm) WH (mm) 3.39

7.83

1.69

3.40

7.62

1.64

3.42

7.64

1.80

Acknowledgements The authors would like to thank Universiti Kuala Lumpur—Malaysia France Institure and Universiti Malaysia Pahang Al-Sultan Abdullah for providing financial support and the facilities.

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References 1. Gao Z, Shao X, Jiang P, Cao L, Zhou Q, Yue C, Liu Y, Wang C (2016) Parameters optimization of hybrid fiber laser-arc butt welding on 316L stainless steel using Kriging model and GA. Opt Laser Technol 83:153–162 2. Atzori B, Lazzarin P, Meneghetti G, Ricotta M (2009) Fatigue design of complex welded structures. Int J Fatigue 31:59–69 ˇ c 3. Lazi´c V, Aleksandrovi´c S, Nikoli´c R, Proki´c-Cvetkovi´c R, Popovi´c O, Milosavljevi´c D, Cuki´ R (2012) Estimates of weldability and selection of the optimal procedure and technology for welding of high strength steels. Procedia Eng 40:310–315 4. Ramos-Jaime D, Juárez IL, Perez P (2013) Effect of process parameters on robotic GMAW bead area estimation. Procedia Technol 7:398–405 5. Balasubramanian M (2016) Prediction of optimum weld pool geometry of PCTIG welded titanium alloy using statistical design. Eng Sci Technol Int J 19:15–21 6. Sharma C, Dwivedi DK, Kumar P (2012) Effect of welding parameters on microstructure and mechanical properties of friction stir welded joints of AA7039 aluminum alloy. Mater Des 36:379–390 7. Ganjigatti JP, Pratihar DK, Roy Choudhury A (2007) Global versus cluster-wise regression analyses for prediction of bead geometry in MIG welding process. J Mater Process Technol 189:352–366 8. Ibrahim IA, Mohamat SA, Amir A, Ghalib A (2010) Effect of arc voltage, welding current and welding speed on fatigue life, impact energy and bead penetration of AA6061 joints produced by robotic MIG welding. Indian J Sci Technol 3(2) 9. Palani PK, Murugan N (2006) Review selection of parameter of pulsed current gas metal arc welding. J Mater Process Technol 172:1–10 10. Kolahan F, Heidari M (2009) A new approach for predicting and optimizing weld bead geometry in GMAW. World Acad Sci Eng Technol 59 11. Pal A, Handuja S (2014) The analysis of MIG welding parameters for multi response optimization using Taguchi’s orthogonal array and grey relational approach. Int J Adv Res Eng Sci Technol 12. Ais EE (2015) Effect of arc welding current on the mechanical properties of A36 carbon steel weld joints. SSRG Int J Mech Eng 2 13. Ai Y, Jiang P, Shao X, Wang C, Li P, Mi G, Liu Y, Liu W (2016) A defect-responsive optimization method for the fiber laser butt welding of dissimilar materials. Mater Des 90:669–681 14. Eltawahni HA, Olabi AG, Benyounis KY (2010) Effect of process parameters and optimization of CO2 laser cutting of ultra high-performance polyethylene. Mater Des 31:4029–4038 15. Elatharasana G, Kumar VSS (2013) An experimental analysis and optimization of process parameter on friction stir welding of AA 6061–T6 aluminum alloy using RSM. Procedia Eng 64:1227–1234 16. Khan MMA, Romoli L, Fiaschi M, Dini G, Sarri F (2011) Experimental design approach to the process parameter optimization for laser welding of martensitic stainless steels in a constrained overlap configuration. Opt Laser Technol 43:158–172 17. Bidi L, Le Masson P, Cicala E, Primault C (2017) Experimental design method to the weld bead geometry optimization for hybrid laser-MAG welding in a narrow chamfer configuration. Opt Laser Technol 89:114–125 18. UK PK (2015) Influence of process parameter on microstructural characteristics and tensile properties of Friction Welded ASS304L alloy. Appl Mech Mater 766–767 19. Palani PK, Murugan N (2007) Optimization of weld bead geometry for stainless steel claddings deposited by FCAW. J Mater Process Technol 190:291–299 20. Elatharasan G, Kumar VSS (2012) Modelling and optimization of friction stir welding parameters for dissimilar aluminium alloys using RSM. Procedia Eng 38:3477–3481 21. Ruggiero A, Tricarico L, Olabi AG, Benyounis KY (2011) Weld-bead profile and costs optimisation of the CO2 dissimilar laser welding process of low carbon steel and austenitic steel AISI316. Opt Laser Technol 43:82–90

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Current and Future Challenges of Hybrid Electrochemical-Mechanical Machining Process for Microand Nano-Manufacturing Ahmad Shahir Jamaludin , Mohd Nizar Mhd Razali, Nurul Nadia Nor Hamran, Mohd Zairulnizam Mohd Zawawi, and Mohd Amran Md Ali

Abstract As industries like electronics, aerospace, and biomedical engineering evolve, the demand for intricate, precise components has surged. Traditional machining methods often fall short in the realm of micro- and nanomanufacturing, necessitating the development of innovative techniques like the Hybrid Electrochemical-Mechanical Machining (HEMM). HEMM synergistically combines the salient features of electrochemical machining (ECM) and mechanical machining (MM), offering enhanced precision, reduced tool wear, and the ability to fabricate intricate structures. While ECM facilitates material removal via electrochemical dissolution, MM refines structures through mechanical abrasion. This dual-process approach not only offers distinct advantages such as the ability to craft intricate microstructures and micro- and nano-features, but also the fabrication of advanced devices like MEMS and NEMS. Nevertheless, HEMM does pose challenges, including the need for specialized machinery and meticulous process parameter optimization. Electrochemical parameters such as electrolyte selection, voltage, and machining duration, and mechanical parameters including tool selection and feed rate play pivotal roles in achieving the desired outcomes. Through empirical, analytical, and numerical optimization methods, HEMM’s performance can be fine-tuned to meet specific requirements. Its applications span various fields, from microfluidics and micro-optics to aerospace and biomedical devices, underscoring its transformative potential in contemporary manufacturing. This paper presents a holistic exploration of HEMM, aiming to consolidate its paramount role in future manufacturing paradigms.

A. S. Jamaludin (B) · M. N. Mhd Razali · N. N. Nor Hamran · M. Z. Mohd Zawawi Faculty of Manufacturing and Mechatronic Engineering Technology, Universiti Malaysia Pahang Al-Sultan Abdullah, 26600 Pekan, Pahang, Malaysia e-mail: [email protected] M. A. Md Ali Faculty of Manufacturing Engineering, Universiti Teknikal Malaysia Melaka, HangTuah JayaDurian Tunggal, 76100 Melaka, Malaysia © The Author(s), under exclusive license to Springer Nature Singapore Pte Ltd. 2024 R. Abd. Aziz et al. (eds.), Intelligent Manufacturing and Mechatronics, Springer Proceedings in Materials 40, https://doi.org/10.1007/978-981-99-9848-7_8

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Keywords Hybrid electrochemical-mechanical machining · Advanced manufacturing · High precision manufacturing

1 Introduction to Hybrid Electrochemical-Mechanical Machining (HEMM) Process The demand for complex and precise components in industries such as electronics, biomedical engineering, and aerospace has experienced a significant increase as these sectors continue to evolve. However, conventional machining techniques do not adequately meet the rigorous demands of micro- and nano-manufacturing. Introducing the Hybrid Electrochemical-Mechanical Machining (HEMM), a transformative procedure that combines the advantageous features of electrochemical machining (ECM) and mechanical machining (MM) techniques [1–4]. One of the examples is the PEMEC machine in Fig. 1 [1]. The fundamental principle of HEMM involves subjecting a metal workpiece to a dual machining process. Electrochemical Machining (ECM) facilitates material removal via the electrochemical dissolution process, while Mechanical Machining (MM) employs mechanical abrasion. The implementation of a dual strategy in HEMM offers several significant benefits, such as improved accuracy, decreased wear and tear on tools, and the capability to produce complex structures [1–4]. Nevertheless, akin to other methodologies, the HEMM technique is not devoid of its own set of challenges. The successful execution of this task necessitates the utilization of specialized equipment and meticulous oversight of various process parameters [4–10]. The primary objective of this study is to conduct a thorough examination of HEMM, specifically emphasizing its utilization in the realm of micro- and nanomanufacturing. Through an examination of the underlying principles of the subject matter, this exploration offers a deeper understanding of the electrochemical and mechanical components, thereby shedding light on the notable benefits and inherent

Set up Abrasive media size

Electrolyte Flux

Abrasive media movement

Cathode

Workpiece to be polished (anode)

Fig. 1 HEMM in PEMEC, Polissage Electro-Mécano Chimique machine [1]

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constraints associated with it. Furthermore, the discourse encompasses essential components such as process parameters, optimization methodologies, and the wide array of applications of HEMM—encompassing the fabrication of intricate microstructures on metallic surfaces, the etching of micro- and nano-features on ceramics, and the manufacturing of MEMS (Micro-Electro-Mechanical Systems) and NEMS (Nano-Electro-Mechanical Systems) devices [11–20]. The final sections of the paper examine the obstacles and prospective future directions for HEMM in the fields of micro- and nano-manufacturing. Through conducting a comprehensive analysis, our aim is to strengthen the progressive trajectory of HEMM and its crucial role in next-generation manufacturing [21–24].

2 Revolution of Hybrid Electrochemical-Mechanical Machining The Hybrid Electrochemical-Mechanical Machining (HEMM) is an advanced fusion of electrochemical machining (ECM) and mechanical machining (MM), developed to address the intricate demands of the micro and nano-manufacturing sectors. HEMM stands out for its precision, tool longevity, and capability to craft intricate geometric patterns. A deep understanding of its foundational processes is vital [1, 5, 8, 25–30]. Electrochemical machining (ECM), a process rooted in electrochemistry, uses electrodes and electrolytic solutions for material removal. In this system: i. The workpiece, the anode, connects to an electric source’s positive terminal, while a precisely shaped electrode, the cathode, connects to the negative. ii. An electrolytic medium between the electrode and workpiece aids ion movement and electric current flow. iii. Electricity-driven electrochemical reactions dissolve metal ions from the workpiece, creating a cavity mirroring the electrode’s shape, ideal for complex designs [13, 14, 16, 31–35]. Mechanical machining (MM), based on traditional practices, employs physical tools for material shaping. The methodology involves: i. Using tools harder than the workpiece, removing material through shearing, chipping, or grinding. ii. It incorporates various techniques, such as turning, milling, and grinding, each with unique benefits [19–21, 36–40]. HEMM synergistically merges ECM and MM principles. In practice: i. ECM initially sculpts rough contours and significant features, setting the base for later stages. ii. MM then refines and optimizes the structure, achieving unmatched precision and smoothness at the nanometer scale [22, 25, 27, 40–45].

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Table 1 Notable advantage and disadvantage linked to HEMM Advantage Aspect

Explanation

Precision

Unparalleled accuracy due to combined efficacy of electrochemical and mechanical processes, making it vital for industries like aerospace and biomedical [1, 5, 6]

Tool wear

Minimal wear and tear, leading to extended tool lifespan and consistent machining outcomes [7, 10, 15]

Geometriccapabilities

Ability to craft intricate geometries, especially on harder materials, which might be challenging with conventional methods [16, 19, 21]

Material versatility

Enhanced capacity to machine tough materials which are difficult or impossible using conventional methods, promoting innovation in design and application [24, 28, 31]

Disadvantage Equipment requirement Need for specific, often custom machinery resulting in higher initial costs and steeper learning curve [33, 35, 38] Process control

Complexity in management demanding precise calibration of numerous parameters like current density and tool feed rate [39, 42, 45]

Contamination risks

Potential contamination of the workpiece by the electrolyte, risking product quality and necessitating strict monitoring [47, 50–54]

Table 1 presents a systematic analysis of the notable advantage and disadvantage linked to HEMM. The provided table organizes various elements of the HEMM process, thereby providing a comprehensive analysis of the advantages and difficulties associated with each specific characteristic. The advantages column delineates the innovative and distinctive advantages introduced by HEMM, while the disadvantages column underscores the potential obstacles or difficulties that may arise during its implementation. The inclusion of references serves the purpose of enhancing the depth and credibility of the assertions put forth. The presented table functions as a brief reference tool for stakeholders and professionals seeking to comprehend the intricate complexities of HEMM [1, 7, 16, 46–49].

3 Process Parameters and Optimization for Hybrid Electrochemical-Mechanical Machining The effectiveness of HEMM is derived from the precise management and careful optimization of a range of process parameters. A thorough understanding of these parameters, which can be categorized into electrochemical and mechanical domains, is crucial in order to fully exploit the capabilities of HEMM. The ideal values for these parameters depend on the particular operational conditions and the characteristics

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of the material being worked on. This segment will provide a more comprehensive analysis of the complexities surrounding these parameters and the optimization techniques associated with them [12, 15, 17, 18]. Electrochemical Parameters: • Electrolyte Selection and Concentration: The chosen electrolyte is pivotal, with its nature being contingent on the workpiece material and envisaged machining velocity. The electrolyte’s concentration wields profound influence on the machining velocity, the resulting surface’s texture, and the morphology of the resultant machined construct [12, 15]. • Voltage and Current Density: These factors dictate the material’s removal rate. Through judicious modulation of the applied voltage and current density, one can attain predefined surface textures and feature dimensions. This calibration ensures a balance between speed and quality [13, 17]. • Machining Duration: An often-overlooked factor, the time allocated for machining predominantly dictates the depth of the incision and the overarching machining speed, requiring meticulous planning to achieve desired results [13, 18]. Mechanical Parameters: • Tool Selection and Material: The choice of the tool becomes imperative based on the workpiece’s composition, the anticipated feature size, and the sought surface finish. Ideally, the tool’s material exhibits greater hardness than the workpiece, a precaution ensuring efficacious material removal sans excessive tool degradation [20, 22]. • Tool Geometry: This parameter is instrumental in dictating the tool’s longevity, the resultant surface’s texture, and the capability to intricately carve out convoluted features. A confluence of design and material considerations determines optimal tool geometry [5, 23]. • Feed Rate and Spindle Speed: These determinants influence the material’s removal velocity, the subsequent surface’s granularity, and the tool’s operational life. Their calibration necessitates a nuanced understanding of the tool-workpiece interaction dynamics [5, 24].

4 Avant-Garde Applications of Hybrid Electrochemical-Mechanical Machining The field of Hybrid Electrochemical-Mechanical Machining (HEMM) is characterized by its extensive versatility, as it has made notable advancements, particularly in the area of micro- and nano-manufacturing. The distinguishing characteristic of HEMM lies in its adeptness at machining a wide variety of materials, including metals, alloys, ceramics, and composites. This versatility allows it to

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Table 2 Applications and significance of HEMM in various fields Field

Application

Significance

Microfluidics

Fabrication of microfluidic channels and features on substrates for biomedical and chemical analyses

HEMM ensures unmatched precision and surface finish, critical for the reliable functioning of microfluidic devices [19, 20]

MEMS

Production of microsensors, micro-actuators, and microswitches

HEMM’s capability to craft intricate geometries down to nanometers makes it essential for MEMS device production [17, 18]

Micro-optics

Creation of micro-optical HEMM’s precision and nanometer-scale elements like lenses, mirrors, surface finish guarantee optimal performance in and diffractive components micro-optical components [21, 23]

Aerospace and defense

Fabrication of critical components such as turbine blades, fuel injectors, and missile guidance systems

The ability of HEMM to work with challenging materials, like superalloys, ensures components meet rigorous industry standards [9, 11]

Biomedical devices

Crafting of orthopedic implants, dental prostheses, and surgical instruments

HEMM delivers precision and surface finishes that meet biocompatibility requirements, ensuring devices are well-integrated and functional within the body [21, 25]

cater to numerous industries that require high levels of precision [5, 7, 8]. Table 2 summarize the wide range of applications that utilize the capabilities of HEMM. As mentioned, the Hybrid Electrochemical-Mechanical Machining (HEMM) technique combines electrochemical and mechanical methods creatively. The merger improves each technique’s strengths and addresses its weaknesses. Thus, the HEMM has become a leading force in modern manufacturing, driving progress and expanding fabrication capabilities, particularly at micro and nanoscales. HEMM’s ability to manage a wide range of materials and achieve unmatched accuracy could transform industries that require complex and refined outputs. Multiple studies and practical applications demonstrate HEMM’s transformative potential in the ever-changing manufacturing industry [1, 3, 4, 54].

5 Summary and Future Directions of Hybrid Electrochemical-Mechanical Machining (HEMM) The cutting-edge Hybrid Electrochemical-Mechanical Machining (HEMM) method uses electrochemical and mechanical methods to achieve micro and nano-scale manufacturing precision. Despite its promise, HEMM struggles with tool wear, which is exacerbated by the electrochemical and mechanical processes, reducing precision and increasing costs from tool replacements. Pioneering control methods that enable realtime parameter monitoring and adjustments are needed to maintain precise process control due to the intricately linked electrochemical and mechanical operations.

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Creating accurate models that capture HEMM’s core processes’ dynamic relationship is crucial for operational efficiency but complex. HEMM is mostly used in micro and nano-manufacturing, but macro-scale manufacturing is underexplored. HEMM can also damage surface integrity, causing superficial and subsurface flaws, requiring advanced post-processing methods to ensure surface quality. Resilient tools, innovative control systems, and precise modeling are needed to maximize HEMM’s potential in modern manufacturing. Acknowledgements The author acknowledges the University of Malaysia Pahang Al-Sultan Abdullah for their support and financial help under PGRS grant, PGRS220366, confirming the successfulness of the study.

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Application of Activity-Based Costing and Time-Driven Activity-Based Costing for Kitchen Cabin Intan Noralisya Mohd Yusoff, Mohd Yazid Abu, Sri Nur Areena Mohd Zaini, Wan Zuki Azman Wan Muhamad, Faizir Ramlie, Nolia Harudin, and Emelia Sari

Abstract Kitchen cabinets started to have a big historical impact on Malaysia in the nineteenth century. The drawback with traditional costing methods is that they fail to offer enough information that are crucial to customers, such quality and service. Activity-based costing (ABC) was created to address traditional costing’s limitations in complex product environments. However, it is not universally accepted as it overlooks unused capacity for forecasting. This work compares ABC and time-driven ABC (TDABC) to assess cost sustainability in kitchen cabinet production by determining the cost driver rate and analyzing unused capacity of time and cost, respectively. Data from a Johor-based furniture manufacturer was collected. The work successfully compares both methodologies, considering various factors. Ultimately, the forecast cost and capacity utilization in kitchen cabinet production have been determined. By applying ABC method, a single unit of kitchen cabinets is predicted to cost as much as MYR 3426.32. Whereas in TDABC, the unused capacity of time and cost are −5208.80 min and MYR −2838.32, accordingly. It concludes that both have strengths based on industry needs, but proving TDABC’s efficiency is essential as it is simpler, cheaper, and more powerful than ABC. Nonetheless, neither ABC nor TDABC is well-suited for kitchen cabinets manufacturing. The process of building I. N. Mohd Yusoff · M. Y. Abu (B) · S. N. A. Mohd Zaini Faculty of Manufacturing and Mechatronics Engineering Technology, Universiti Malaysia Pahang Al-Sultan Abdullah, 26600 Pekan, Pahang, Malaysia e-mail: [email protected] W. Wan Muhamad Institute of Engineering Mathematics, Universiti Malaysia Perlis, Kampus Pauh Putra, 02600 Arau, Perlis, Malaysia F. Ramlie Razak Faculty of Technology and Informatics, Department of Mechanical Engineering, Universiti Teknologi Malaysia, Jalan Sultan Yahya Petra, 54100 Kuala Lumpur, Malaysia N. Harudin Universiti Tenaga Nasional, 43000 Kajang, Selangor, Malaysia E. Sari Faculty of Industrial Technology, Department of Industrial Engineering, Universitas Trisakti, Kyai Tapa No 1, 11440 West Jakarta, Indonesia © The Author(s), under exclusive license to Springer Nature Singapore Pte Ltd. 2024 R. Abd. Aziz et al. (eds.), Intelligent Manufacturing and Mechatronics, Springer Proceedings in Materials 40, https://doi.org/10.1007/978-981-99-9848-7_9

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kitchen cabinets involves inherent complexity, such as variations in measurements, material availability, and design specifications. Based on the given factors, such as higher uncertainties, biases in assumptions and inaccurate data collection, it will draw limitations in obtaining accurate and reliable data for ABC and TDABC. Keywords Kitchen cabinet · Activity-based costing · Time-driven activity-based costing

1 Introduction The kitchen furniture sector is the largest segment in the German furniture industry, representing 22% of all furniture. Germany is the leading manufacturer of kitchen furniture in Europe, accounting for 27% of the total supply and serving as the largest consumer market. The value of kitchen output in Germany increased by 5.2% in 2007 to e3882 million, with a focus on export markets. Kitchen furniture exports also saw significant growth, increasing by 14% to e1379 million. This sector employs up to 17,000 people across approximately 100 companies. Germany produces kitchens for the low, medium, and upper-middle segments of the market [1]. ABC methodology was developed to enhance the accuracy of product cost data compared to traditional cost systems. It converts overhead expenses into direct costs by using activities as the basis for cost allocation [2]. Other than that, ABC improves the value of cost accounting for strategic decision-making and helps organizations achieve sustainable development and growth in a competitive global and complex business environment [3]. ABC offers various advantages and disadvantages for organizations. It helps reduce costs, identifies non-value-adding activities, provides precise cost estimation based on cause-and-effect relationships, and identifies areas for improvement [4]. However, implementing ABC can be costly [4], it may not be suitable for companies with low overhead [5], and there is a risk of misinterpretation and making incorrect decisions [4]. Overall, ABC has the potential to enhance management and business operations, but careful consideration is required. Whereas, TDABC is a process-based approach to costing that provides comprehensive cost information through process maps [6]. It simplifies costing by eliminating the need for interviews and surveys to allocate resource costs to activities. Instead, TDABC uses time as the primary cost driver, directly allocating resource costs to objects such as transactions, orders, and products. This bypasses the challenging step of allocating costs to activities in traditional ABC, making the costing process more straightforward [7]. Various cost accounting methods, including TDABC, have been studied in production environment [8]. For service companies, costs primarily stem from service provision. To ensure a consistent profit margin, TDABC considers the sales contract. Overall profitability depends on product pricing, which covers production costs, and the gross margin, which covers service provision expenses. This includes

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order-related fees, specialized logistics, administrative costs, and selling expenses [9]. Last but not least, according to [6], TDABC overcomes various difficulties associated with ABC and offers several advantages. It is simpler, cheaper, and more powerful than traditional ABC. TDABC allows for visibility into process efficiency and capacity utilization, facilitates variance analysis for continuous improvement, and provides insights into capacity management. However, TDABC has a few drawbacks, such as the potential inaccuracy of time estimations collected through interviews when direct observation is not possible, and the additional step of involving managers in the process of time estimation, which can be seen as unnecessary.

2 Methodology In this section, it will discuss the methods and steps involved in carrying out this research as shown in Fig. 1. Basically, this research was done to construct a comparison between the ABC and TDABC methods in kitchen cabinet production by determining the cost driver rate and analyzing unused capacity of time and cost, respectively. The company under discussion is based in Johor Bharu, Malaysia. The company is a global manufacturer that specializes in the design, production, and installation of high quality kitchen cabinetry. In this work, ABC implementation involves five steps. Firstly, the project team conducts interviews with departmental staff and supervisors to understand the manufacturing flow and the tasks involved in producing the product. Secondly, interviews with the business owner determine the time spent on these activities. Thirdly, time percentages are used to calculate the overall activity cost. Fourthly, a cost driver is identified to allocate customer service department costs based on factors like orders processed, complaints received, and credit checks completed. Lastly, the information on cost drivers is utilized to estimate and anticipate the cost of the product [7]. Meanwhile for TDABC system application, it comprises of seven steps. First, create a list of operations involved in each product, obtained from sales registration. Second, calculate the cost of resources supplied to the process, including personnel, supervision, occupancy, equipment, and technology. Third, establish the actual capacity of activity consumption for each product, quantifying it in terms of time. Fourth, estimate the demand for resource capacity needed by each cost object to allocate departmental resource costs to products. Fifth, create a time equation to determine the fundamental time required for each action. Sixth, measure the duration of each activity for each product and track used and unused capacity to reduce future resource costs. Finally, utilize a time equation to directly allocate resource costs to operations and financial transactions [10].

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Fig. 1 Flowchart of research methodologies

3 Result and Discussion The cost of capacity is determined by considering the various resources comprehend in the process. Labor cost refers to the operator’s salary, while material cost represents the expense of raw materials used in product manufacturing. Consumable cost includes the expenditure on materials and equipment utilized but not directly included in the final product. Next, Table 1 shows the cost driver rates for kitchen cabinet production using ABC method. The cost driver quantity is the estimated quantity of products produced in all six activities. Cost driver rates are calculated by dividing the assigned cost by the cost driver quantity for each activity. Forecasting product costs is essential for budgeting, pricing decisions, financial planning, and assessing the profitability of a product. Table 2 shows the fabrication of kitchen cabinets has the highest forecast cost, which is MYR2606.40, due to the

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Table 1 Cost driver rates of all activities in ABC Activities

Cost driver

Cost of all Cost driver resources supplied quantity (MYR) (MYR)

Cost driver rate (MYR)

Precision measurement

The number of square feet

160.00

20

8.00 per ft

Live sketching

The quantity of accessory requests from customers

60.00

8

7.50 per request

Full quotation

Number of customer change orders

150.00

2

75.00 per order

Convert sketching into plan

Number of parts

200.00

102

1.96 per parts

Fabrication of kitchen cabinet

The number of square feet

2606.30

20

130.32 per ft

Installation of kitchen cabinet

The number of square feet

250.00

20

12.50 per ft

complexity of the activity and volume of work. The total forecast cost of kitchen cabinets production is the summation of the forecasts from all six activities. Thus, by applying ABC method, a single unit of kitchen cabinets is predicted to cost as much as MYR3426.32. After that, the first step of TDABC implementation, which is to identify the cost of all resources supplied in each sub-activities. Labour cost is the amount of the salary of the operators, while material cost is the cost of the raw materials used in the production of the product. Consumable cost is the cost of materials and equipment used but not incorporated into the product. In this company, it consisted of 13 operators, 3 office staffs and 1 owner. In the meantime, the practical capacity that based on working hours of employees are been determined. The official working time is an average of seven hours a day for 23 days per month. However, not all time paid is available for productive work. Each day, 65 min are granted for employees to take breaks, solve maintenance issue or attend other activities. Meaning that each employee has an acceptable capacity of 8165 min per month. So, the allocated total practical capacity of manpower is 138,805 min per month. As there are 25 designs to be committed each month, one design has consumed 5552.20 min, and each employee need to spend 326.60 min for it. Then, Table 3 shows the capacity cost rate of each sub-activity. Capacity cost rates help determine the cost per unit of capacity or production volume for a resource or facility. The highest rate, MYR7.729, is attributed to installing accessories due to factors such as high fixed costs, inefficiency, and high-quality standards. On the other hand, placing the cabinet has the lowest rate of only MYR0.084 due to factors such

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Table 2 Forecast cost in ABC Activities

Cost driver

Cost driver rate (MYR)

Cost driver quantity (MYR)

Forecast cost (MYR)

Precision measurement

The number of square feet

8.00 per ft

20

160.00

Live sketching

The quantity of accessory requests from customers

7.50 per request

8

60.00

Full quotation

Number of customer change orders

75.00 per order

2

150.00

Convert sketching into plan

Number of parts

1.96 per parts

102

199.92

Fabrication of kitchen cabinet

The number of square feet

130.32 per ft

20

2606.40

Installation of kitchen cabinet

The number of square feet

12.50 per ft

20

250.00

Total

–

–

–

3426.32

as high utilization, efficiency, and economical facilities. Assessing these factors is crucial to meet customer demand and maintaining quality standards. Subsequently, it is essential to generate an equation to calculate the estimated production time. Table 4 shows the predicted duration of each activity, which was determined by watching the operators carry out the assigned activities. The time equation to calculate the total used time in all sub-activities are presented in Eq. (1) as shown below. Time equation for all sub − activities = 198χ1 + 40χ2 + 30χ3 + 30χ4 + 15χ5 + 30χ6 + 5χ7 + 20χ8 + 0χ9 + 45χ10 + 150χ11 + 280χ12 + 45χ13 + 45χ14 + 60χ15 + 60χ16 + 120χ17

(1)

Hence, the actual time allocated in all activities per month was determined by substituting the volume of cost-drivers into Eq. (2) as shown below. The actual time allocated = (198 × 20) + (40 × 50) + (30 × 8) + (30 × 2) + (15 × 8) + (30 × 2) + (5 × 10) + (45 × 2) + (0 × 5)

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Table 3 Capacity cost rate of each sub-activities in TDABC Activities

Sub-activities

Precision measurement

Cost of all resources supplied (MYR)

Practical capacity (min)

Capacity cost rate (MYR)

Find the total 94.00 height, width and depth of each cabinet

186.60

0.536

Find each cabinet’s interior measurements

32.00

70.00

0.429

Check the measurements of any cabinet accessories

34.00

70.00

0.429

.. ..

.. ..

.. ..

.. ..

.. ..

Installation of kitchen cabinet

Transfer the measurement to the back of cabinet and marking

35.00

326.60

0.107

Drilling the hole

80.00

163.30

0.490

Placing the cabinet

55.00

653.20

0.084

Screw the cabinet 80.00 into place

163.30

0.490

+ (45 × 4) + (150 × 2) + (280 × 2) + (45 × 6) + (45 × 20) + (60 × 2) + (60 × 20) + (120 × 2) = 6241.10 minute

(2)

The total time to find the total height, width and depth of each cabinet in a month can be represented by χ1 equals 20 in 198χ1 , so that 198 × 20 = 3960 min. When multiplied unused time which is −3773.40 min by capacity cost rate of MYR 0.536, it can be determined that the total unused cost MYR −2022.54. Table 5 shows the used and unused capacity for both time and cost. Ultimately, as the final step of TDABC which is capacity utilization, an activity is selected to be discussed in this section. For activity 1 which is precision measurement, Fig. 2 illustrates that measuring the total height, width, and depth of each cabinet shows a much higher quantity of unused cost compared to other sub-activities, which is MYR −2022.54. It means that there is a deficit in the resources allocated or required for an activity. This suggests that the activity is operating beyond its available resources or that the actual resource usage is lower than the allocated capacity.

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Table 4 Time equation for all sub-activities in TDABC Activities

Sub-activities

Precision measurement

Find the total height, width and depth of 198χ1 each cabinet

Live sketching Full quotation Convert sketching into plan

Estimated time (min)

Find each cabinet’s interior measurements

40χ2

Check the measurements of any cabinet accessories

30χ3

Make a general sketch of the kitchen

30χ4

Design selection by customer

15χ5

Preparation of the document

30χ6

Provide to the customer

5χ7

Convert hand-drawn into a digital floor plan

20χ8

Show to the customer

0χ9

Fabrication of kitchen cabinet Prepare the materials

45χ10

Cutting pieces

150χ11

Assembling the cabinet base, face panels and door

280χ12

Installing the accessories

45χ13

Installation of kitchen cabinet Transfer the measurement to the back of 45χ14 cabinet and marking Drilling the hole

60χ15

Placing the cabinet

60χ16

Screw the cabinet into place

120χ17

Ultimately, the capacity utilization in all six activities involved in kitchen cabinet production have been determined. The unused capacity of time and cost are − 5208.80 min and MYR −2838.32, accordingly.

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Table 5 Used and unused capacity in TDABC Activities

Sub-activities

Practicalcapacity Used time Unused (min) (min) time (min)

Capacity Unused cost rate cost (MYR) (MYR)

3960

−3773.40 0.536

−2022.54

Find each 70.00 cabinet’s interior measurements

2000

−1930.00 0.429

−827.97

Check the 70.00 measurements of any cabinet accessories

240

−170.00

0.429

−72.93

.. ..

.. ..

.. ...

.. ..

.. ..

.. ..

.. ..

Installation of kitchen cabinet

Transfer the measurement to the back of cabinet and marking

326.60

900

−573.40

0.107

−61.35

Drilling the hole

163.30

120

43.30

0.490

21.22

Placing the cabinet

653.20

1200

−546.80

0.084

−45.93

Screw the cabinet into place

163.30

240

−256.70

0.490

−125.78

5225.40

10,253.40 −5208.80

Precision Find the total measurement height, width and depth of each cabinet

Total

186.60

−2838.32

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Fig. 2 Capacity utilization in precision measurement

4 Conclusion In conclusion, the comparison between ABC and TDABC in the context of a kitchen cabinet manufacturer offers valuable insights for making an informed decision. First of all, both ABC and TDABC aim to enhance cost accuracy compared to traditional costing methods. ABC identifies and allocates costs based on individual activities, while TDABC emphasizes the time required for activities. Second, implementation complexity is an important factor to consider. ABC requires significant effort and resources due to its reliance on detailed activity analysis and cost driver identification. In contrast, TDABC offers a straightforward implementation process as it primarily relies on time estimates for activities. Third, TDABC excels in time-based efficiency. TDABC enables organizations to identify and eliminate non-value-added activities and inefficiencies. ABC, while providing detailed cost information, does not explicitly address time-related inefficiencies. Nevertheless, it can be concluded that neither ABC nor TDABC is well suited for kitchen cabinets manufacturing. The process of building kitchen cabinets involves inherent uncertainties, such as variations in measurements, material availability, and design specifications. Craftsmen with knowledge of traditional techniques have a better understanding of the required materials, labour, and time involved, allowing them to provide more accurate cost estimates.

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Acknowledgements This work was funded by the Ministry of Higher Education under Fundamental Research Grant Scheme (FRGS) No. FRGS/1/2022/TK10/UMP/02/8 (University reference RDU 220108).

References 1. Kitchen cabinets market—Growth, trends, COVID-19 impact, and forecasts (2023– 2028). Retrieved from https://www.mordorintelligence.com/industry-reports/kitchen-cab inets-market. Accessed on 25 June 2023 2. Tsai WH (1996) Activity-based costing model for joint products. Comput Ind Eng 31(3):725– 729 3. Mahal I, Hossain A (2015) Activity-based costing (ABC)–an effective tool for better management. Res J Finan Account 6(4):66–74 4. Shihab WK, Prasad S (2022) Activity based costing system. Int J Scien Res 8(7):18288–18306 5. The disadvantages and advantages of activity-based costing. Retrieved from https://smallbusi ness.chron.com/disadvantages-advantages-activitybased-costing-45096.html. Accessed on 25 June 2023 6. Cidav Z, Mandell D, Pyne J et al (2020) A pragmatic method for costing implementation strategies using time-driven activity-based costing. Implement Sci 15(1):28 7. Kaplan RS, Anderson SR (2007) Time-driven activity-based costing, a simpler and more powerful path to higher profits. Harvard Business School Press 8. Barros RS, Ferreira AMDSC (2017) Time-driven activity-based costing: designing a model in a Portuguese production environment. Qual Res Account Manage 14(1):2–20 9. Pashkevich N, von Schéele F, Haftor DM (2023) Accounting for cognitive tie in activity-based costing: a technology for the management of digital economy. Technol Forecast Soc Change 186 10. Ganorkar AB, Lakhe RR, Agrawal KN (2019) Methodology for application of maynard operation sequence technique (MOST) for time-driven activity-based costing (TDABC). Int J Product Perform Manag 68(1):2–25

Optimization of Surface Roughness on Duplex Stainless Steel in Dry Milling Nurul Hidayah Razak

and Mohammad Rizal Md Ali

Abstract In manufacturing industry, surface roughness is one of the crucial factors affecting the production costs and machining duplex stainless steel becomes difficult due to its mechanical properties. This study was performed on a duplex stainless steel in dry milling operation using carbide tools. Response surface methodology (RSM) is utilised to identify main cutting parameter that affects the quality of surface roughness as well as optimizing the operation. It is found that feed rate, f contributes to the highest factor affecting the quality of surface roughness, Ra followed by the speed of the cutting, VC and depth-of-cut, D OC. An optimum machining parameters speed of cutting of 78.283 mm/min, rate of feed of 0.100 mm/tooth and axial depth of 0.834 mm is identified as the optimum values. Keywords Duplex stainless steel · Coated carbide tool · Response surface method

1 Introduction Duplex Duplex stainless steel alloys belong to iron based hard-to-cut materials categories as stated by Airao et al. [1]. The causes for difficulties in machining of duplex stainless steel alloys are low thermal conductivity, superior in tensile strength, excellent in ductility and high build up edge. This material is machinable but due to its superior mechanical strength, the machinability become more challenging and difficult. This addresses a concern especially when dry milling operation is applied. Selvaraj [2] stated that the process can be enhance if these few rules are followed. First, the cutting edge should sharp-edged because blunt edge will generate superabundance work hardening effect. Light but sufficient cuts should be made to avoid work hardening impact when the material’s surface is being removed. The chip breakers should be performed to make sure the swarf remain clear during the machining process. Lastly, low thermal conductivity of austenitic alloys will lead to heat concentrating N. H. Razak (B) · M. R. Md Ali Universiti Malaysia Pahang Al-Sultan Abdullah, 26600 Pekan, Malaysia e-mail: [email protected] © The Author(s), under exclusive license to Springer Nature Singapore Pte Ltd. 2024 R. Abd. Aziz et al. (eds.), Intelligent Manufacturing and Mechatronics, Springer Proceedings in Materials 40, https://doi.org/10.1007/978-981-99-9848-7_10

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at the cutting edges. The hardness of duplex stainless steel tends to fasten the period of tool wear, thus affects the quality of surface roughness of workpiece machined. The goal of machining is to keep the surface roughness value as low as possible which is accomplished by using the best cutting parameters [3]. A good quality product is obtained when the material, finish and dimension requirement are satisfied, and all of these are dependent on the cutting parameters of the machining process [4]. As we all know, a manufacturing engineer or machine technician are expected to improve machining parameters to achieve required surface roughness. This could only be done time by time to avoid the delay in production line. Thus, this study aims to optimize the surface roughness of a stainless steel (duplex).

2 Methodology In this study, duplex stainless with dimension of 100 × 75 × 40 mm is used as the workpiece. All cutting experiments have been performed on a MAKINO KE55. Figure 1 shows the experimental set up of the milling process. The experiment being set up so the spindle machined through 100 mm in distance of length per 1 pass. The cutter will operate in clockwise direction from the left side to the right side of the work piece. From the figure show below, it is shown that the cutting operation begins at “Milling start” and finish at “Milling finish” label on the figure.

Fig. 1 Experimental set up

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(a)

105

(b)

Fig. 2 a Single flute tool holder Ø16 mm, b flank face of cutting tool (The red dotted lines indicate the cutting edge of the cutting tool)

Coated tungsten carbides with single flute cutting holder were used as the cutting tools during this experiment as detailed in Fig. 2. The roughness value of the workpiece machined was measured using surface roughness tester after completing 1 pass with distance of 100 mm. An average surface roughness (Ra ) on 100 mm surface machined workpiece were measured and used to indicate the value surface roughness. All experiments were conducted in dry milling. Design of experimental (DOE) with box-behnken has been utilized in order to generate the cutting parameter during milling as shown in Table 1.

3 Results and Discussion Table 2 shows ANOVA table where DF indicates the total degree of freedom, Adj SS indicates the adjusted sum of squares, Adj MS indicates the adjust mean squares, F value indicates testing the significant of adding quadratic terms to the quadratic model and P value as the probability if the means of the various populations are equal, of a value of F greater that what you observed. According to the ANOVA table, Table 2, there are two out of three of the machining parameters (factors) that have the significant effect on the flank wear since their P-Value < 0.05. The most significant factor is feed rate, (P-Value = 0.009) followed by cutting speed, (P-Value

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Table 1 Cutting parameter Exp. run

Cutting speed, Vc (m/min)

Feed rate, f (mm/tooth)

Depth-of-cut, DOC (mm)

Spindle speed, RPM (rev/min)

Feed, F (mm/ min)

1

75

0.3

0.8

1500

360

2

75

0.2

0.9

1500

270

3

75

0.1

1

1500

150

4

50

0.3

0.9

1000

270

5

75

0.3

0.9

1500

270

6

50

0.3

0.8

1000

160

7

100

0.2

0.8

2000

320

8

100

0.3

0.9

2000

540

9

100

0.2

1

2000

400

10

100

0.1

0.9

2000

180

11

50

0.1

0.9

1000

90

12

75

0.3

1

1500

450

13

75

0.1

0.8

1500

120

14

75

0.2

0.9

1500

270

15

50

0.2

1

1000

200

= 0.038). Also, it is shown that the interaction between cutting speed and cutting speed has a dominant influence on the output response (surface roughness). Optimizing the surface roughness is the reciprocation connection affected by diverse cuing scopes which was the aim of this research. RSM refers to establish the connection amongst the input and output data (surface quality). As this empirical model is involved with three-level factorial design in which each factor is determined at a “low’, “center” and “higher” setting, therefore, it correspond to the second-order polynomial mathematical model. Through the regression analysis, the coefficient for each variable is known. Equation 1 shows the second order polynomial mathematical model and regression equation. S R = 1.42033 + 0.28350 f + 0.38988D OC − 0.34488VC + 0.00583( f × f ) − 0.63692(D OC × D OC) + 0.20708(VC × VC ) + 0.02875( f × D OC) − 0.28175( f × VC ) − 0.32300(VC × D OC) where;

S R : surface roughness (mm). f : Feed rate (mm/tooth). D OC: Depth of cut (mm).

(1)

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Table 2 ANOVA data Origin

DF

Adj SS

Adj MS

F-value

P-value

Model

9

0.350020

0.038891

0.64

0.735

Linear

3

0.183448

0.061149

1.01

0.462

Cutting speed

1

0.054120

0.054120

0.89

0.038

Feed rate

1

0.050721

0.050721

0.84

0.009 0.306

d.o.c

1

0.078606

0.078606

1.30

Square

3

0.109507

0.036502

0.60

0.641

Cutting speed*cutting speed

1

0.053317

0.053317

0.88

0.031

Feed rate*feed rate

1

0.002417

0.002417

0.04

0.850

d.o.c*d.o.c

1

0.057155

0.057155

0.94

0.376

2-Way Interaction

3

0.057065

0.019022

0.31

0.815

Cutting speed*feed rate

1

0.031862

0.031862

0.53

0.501

Cutting speed*d.o.c

1

0.012882

0.012882

0.21

0.664

Feed rate*d.o.c

1

0.012321

0.012321

0.20

0.671

2.73

0.280

Error

5

0.302954

0.060591

Lack-of-fit

3

0.243441

0.081147

Pure error

2

0.059513

0.029756

14

0.652974

Total

VC : Cutting speed (mm/min). Figure 3 depicted the major effects plot of the independent variables for surface roughness, Ra which included; the speed of the cutting, VC , rate of feed, f and depthof-cut, DOC. Clearly, surface roughness, Ra value become greater as the rate of feed and cutting speed escalate. However, the value of roughness quality reduces as the speed of cutting get larger. Whereas, the other two cutting parameters; feed rate have a directly proportional relationship with surface roughness and depth of cut shows a decreasing line for surface roughness at first but increase drastically when it reaches 1.0 mm of depth. The decreases in feed rate resulted to the decreases in cutting forces. The lower force of cutting contributes to reduced oscillate, thus improve the surface texture. Similarly, when depth-of-cut increases, large force is needed to allow the work piece to undergo shear deformation and it causes an increasing of cutting force, and therefore also increase the surface roughness. Figure 4a, b represent the contour plot and response surface plot respectively, which depicted the interactive influence between depth-of-cut and rate of the feed on surface roughness, when the cutting speed is kept constant at 75 mm/min. Similarly, Fig. 4a reveals that, with an increasing of depth-of-cut, the density of contour lines remains the same at any level of feed rate, which implied that there is insignificant interactive influence between depth-of-cut and rate of the feed on surface roughness. Figure 4b demonstrates that surface roughness increases substantially when both

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Fig. 3 Main effects plot for surface roughness, Ra

depth-of-cut and feed rate are increasing. It could be noted that lower depth-of-cut and rate of the feed results in lower surface quality development. In Fig. 5 below shows the optimum value generated from RSM with the speed of cutting of 78.283 mm/min, rate of feed of 0.100 mm/tooth and axial depth of 0.834 mm. The rate of feed is the prominent factor on surface texture value, then axial depth of cut and the speed of cutting.

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(a)

(b) Fig. 4 a Contour plot and b surface plot of surface roughness

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Fig. 5 Optimum cutting parameters value for surface roughness using RSM

Table 3. Optimum cutting parameters

Cutting speed

78.2828

Feed rate

0.1

Depth of cut

0.834343

4 Conclusion Through this study, it was discovered that the feed rate, followed by the axial depth and the cutting speed, is the cutting parameter with the greatest influence on surface roughness. The higher the value of feed rate the lower the surface quality which means high in surface roughness and may leads to surface defect such as surface flaw and cavities. The RSM model has the capability of relating the above cutting parameters with the response surface roughness successfully. Therefore, it is crucial to optimize the cutting conditions in order to reduce surface roughness during machining. Also, from RSM, the optimum value of cutting parameters to minimize the surface roughness can be obtained which are as tabulated in Table 3 below. Acknowledgements This project is supported by the Research and Innovation Department of Universiti Malaysia Pahang Al-Sultan Abdullah through grant number RDU210369.

References 1. Airao J, Chaudhary B, Bajpai V, Khanna N (2018) An experimental study of surface roughness variation in end milling of super duplex 2507 stainless steel. Mater Today 5(2):3682–3689 2. Selvaraj DP (2017) Optimization of cutting force of duplex stainless steel in dry milling operation. Mater Today Proceed 4(10):11141–11147. https://doi.org/10.1016/j.matpr.2017. 08.078

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3. Zhou K, Zhang J, Xu C, Feng P, Wu Z (2018) Effects of helix angle and multi-mode on the milling stability prediction using full-discretization method. Precis Eng 54(May):39–50. https:// doi.org/10.1016/j.precisioneng.2018.04.016 4. Karthick PA, Kumar SR, Prathap P, Ragul K, Raghul KS (2020) Materials today : proceedings optimization of reaming parameters to improve surface roughness of En1A leaded material with the approach of particle swarm optimization. Mater Today Proceed 1–6.https://doi.org/10.1016/ j.matpr.2020.06.225

Ultrasonic Shot Peening Advancements and Their Impact on Alloys Microstructure Behavior: A Concise Review Aina Najwa Azmi, Muhammad Syamim Mazlan, and Mohamad Rusydi Mohamad Yasin

Abstract The mechanical properties of solid metals and alloys can be enhanced by applying ultrasonic shot peening (USP) because it results in compressive residual stress. USP has huge potential to be utilized in improving the mechanical properties and fatigue life of metallic components, hence it has recently gained much attention as a novel surface treatment technique. Shot peening uses ultrasonic vibrations at high frequencies to drive tiny spheres, or shots, into a workpiece’s surface, where they cause plastic deformation and create a compressive residual stress layer in the microstructure. The present paper provides a comprehensive overview of the principles, mechanisms, and applications of ultrasonic shot peening, highlighting its benefits over conventional shot peening techniques. The paper also discusses the research gaps and the latest advancements in the field. Keywords Ultrasonic shot peening · Alloys · Microstructure behavior

1 Introduction Advanced surface treatment methods, particularly ultrasonic shot peening (USP), have arisen in response to the need for high-performance materials in sectors like aerospace, automotive, and energy [1–3]. USP is a process that improves the mechanical properties of metals by inducing superficial compressive stress using high velocity shot peening media and ultrasonic frequencies [4]. It offers advantages over conventional shot peening methods in terms of process control, efficiency, and environmental impact [1]. However, USP is limited by part shape and sealed chamber [1]. USP has been shown to enhance the compressive residual stress, corrosion resistance and micro hardness of various metallic materials [1–3]. Conventional shot peening techniques may be limited by factors such as shot velocity, coverage, and A. N. Azmi · M. S. Mazlan · M. R. Mohamad Yasin (B) Faculty of Manufacturing and Mechatronic Engineering Technology, Universiti Malaysia Pahang Al-Sultan Abdullah, 26600 Pekan, Pahang, Malaysia e-mail: [email protected] © The Author(s), under exclusive license to Springer Nature Singapore Pte Ltd. 2024 R. Abd. Aziz et al. (eds.), Intelligent Manufacturing and Mechatronics, Springer Proceedings in Materials 40, https://doi.org/10.1007/978-981-99-9848-7_11

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process repeatability, and may cause undesirable roughness or stress on the surface [4, 5]. USP addresses these limitations by utilizing high-frequency ultrasonic vibrations, allowing for greater control over process parameters and resulting in a more uniform treatment [6]. Enhanced resistance to fatigue, stress corrosion cracking, and contact fatigue are among the key benefits that USP can offer, thereby contributing to increased productivity, improved quality, and reduced costs [5]. Studies have investigated the microstructural changes induced by USP in aluminum die casting alloys, showing refined microstructures and improved mechanical properties [6–9]. USP equipment consists of an ultrasonic signal generator, a transducer, a metal rod (horn), and an enclosure to keep the shots between the horn and the workpiece as seen in Fig. 1. Recent success with using USP to create nanostructure grains on metals and alloys has piqued the interest of experts all over the world [9–13]. The effect of USP on the mechanical properties of various materials, including commercially pure aluminum, has been studied previously [7, 14–16]. The findings revealed that using USP enhances both ductility and strength in all experimental alloys. The usage of USP during solidification of Al-Si-Cu alloys at various processing temperatures has been Fig. 1 An overview of the ultrasonic shot peening (USSP) process [8]

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observed. An extended heat treatment can be used to refine and modify the properties of an aluminum alloy [17]. The findings suggest that USP successfully refines the Fe-rich phases [16]. These studies have reported improvements in hardness, fatigue strength, and wear resistance due to the microstructural changes induced by USP. It has been hypothesized that the mechanical properties of Al-Si alloys can be greatly enhanced by adding Mg. Changes in the material’s microstructure during treatment have a significant impact on the material’s mechanical properties. More silicon (Si) is added to Al-Si alloys used in casting automotive components in order to boost the fluidity, feeding properties, and hot tear resistance. Therefore, understanding the relationship between USP parameters and microstructural changes is essential for optimizing the process to achieve the desired mechanical properties.

2 Microstructural Behaviour 2.1 Impact of USP Treatment on TC2 Thin-Sheet Microstructure and Properties: Qingze Xu’s 2021 Analysis In the past year, numerous investigations have been accomplished to examine the impact of microstructure behavior on diverse materials and how it impacts the outcomes of USSP treatment applied to the chosen materials. In their study [2], analyzed how different USP treatments affected the surface roughness, tensile strength, micro-hardness, and microstructure of a 0.5 mm thick sheet of TC2. Figure 2 illustrates the metallographic composition of TC2 alloys prior to and following USP processing. Because TC2 is a titanium alloy with two distinct phases, the dazzling white areas depict the β phase, while the dark grey areas depict the α phase. Post USP treatment, the dispersed β phases on the surface layer exhibit a minor reduction in size, however, no substantial alterations are observed in the α and β phases. Figure 3a displays the results of XRD testing that looked at how USP treatment affected the microstructure of TC2 alloy. Figure 3b indicates that as the intensity of shot peening Almen increased, the diffraction peaks were wider, as assessed by their full width at half maximum (FWHM). Bragg diffraction peaks have broadened, which is a cause of the increase in micro-strain. The microstructure of TC2 alloy is altered primarily by β phase refinement, dislocation development and slip, and the appearance of mechanical twinning as a result of USP treatment. Since the grain size of the samples was greater than 100 nm before and after the USP treatment, the widening of the diffraction peaks was unaffected. The microstructure of the TC2 alloy changed very slightly after USP treatment, however, this was barely perceptible. Although USP treatment did slow the formation of the diffraction peaks, the grain size of the specimens was always larger than 100 nm. Intense plastic deformation at the surface led to an increase in microstrain, which widened the Bragg diffraction peaks. As the Almen intensity of the

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Fig. 2 The influence of USP on the TC2 alloy microstructure: a Initial b 0.189 mmA c 0.277 mmA, and d 0.360 mmA [2]

Fig. 3 The influence of USP on the TC2 alloy XRD patterns: a XRD patterns; and b partial enlarged views from 38 to 41, 52.8 to 54, and 70 to 72 [2]

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shot peening grew, mechanical twinning, dislocation entanglements, and dislocation barriers all led to the creation of complex duplex and triplex structures. These factors may have a substantial role in the widening of the diffraction peaks.

2.2 Microstructure Evolution in SLM TC4 Titanium Alloy: Zhang’s 2021 Research Ultrasonic shot peening (USP) process has been utilized to enhance the properties of a titanium alloy called Tie6Ale4V (TC4) that was fabricated using selective laser melting (SLM), as reported in [3]. The methods employed to analyses the material’s microstructure following treatment included optical and scanning electron microscopy, hardness testing and X-ray diffractions. After USP treatment, compressive residual stress and a significant increase in microhardness were detected. The researcher [3] produced a TC4 plate with measurements of 100 × 100 × 5 mm3 by selective laser melting TC4 alloy powder. To create completely dense TC4 products and lower internal residual stress, certain selective laser melting (SLM) parameters were applied. The implementation of ultrasonic shot peening involved the use of an instrument capable of inducing microstructure evolution, including grain refinement, surface layer plastic deformation and work hardening. In order to test this approach, 500 pieces of 2.5 mm zirconia balls were utilised as shots. USP treatments of 480, 960, and 1920s were applied to SLM TC4 samples, with corresponding Almen intensities of 015, 0.20, and 0.22 mmA. The microstructure and macrophoto of SLM TC4 alloy are shown in Fig. 4. The scanning path results in an uneven top surface on the SLM TC4 plate shown in Fig. 4a. Figure 4b illustrates the microstructure of the XY plane, which has a checkerboard pattern that lowers internal stress and prevents components from breaking. Figure 4b through d illustrate the microstructure of the SLM TC4 specimens. Due to the SLM process’s rapid cooling characteristics, which prevent the b phase from converting into an α phase, fully acicular martensite develops in the XY plane. Scanning electron microscopy (SEM) images recorded in the XZ plane also reveal the presence of the acicular martensite microstructure seen in the XY plane. Because of the SLM’s epitaxial growth behavior, these characteristics are visible in the XZ view (Fig. 4c). In the study, residual stress patterns in SLM-TC4 samples treated for varied amounts of time are examined, as shown in Fig. 5. According to research made by [3] findings, the samples’ initial residual stress was close to 100 MPa. The research demonstrated that the primary residual stress in the samples subjected to USP was compressive residual stress (CRS). This stress peaked at the subsurface, then progressively diminished with increasing depth, before finally reaching a stable state. The maximum CRS values for samples processed for 480, 960, and 1920 s were 653, 741, and 875 MPa, respectively. As USP therapy was continued into the 1920s, the CRS depth grew from 170 to 227 mm. Moreover, the maximum depth of CRS also increased with longer USP durations. The compressive residual stress

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Fig. 4 a The SLM TC4 alloy’s macrophoto and microstructure. b The SLM TC4 plate. c The SLM Ti-6Al-4 V alloy in various orientations as seen by OM micrographs. d The SEM micrograph of the XZ plane [3]

Fig. 5 The depth distribution of residual stress for various USP durations a the residual stress fields for the SLM TC4 treated by USP. b The surface CRS, maximum CRS, maximum CRS location, and CRS depth [3]

and the overall thickness of the CRS layer after USP were both enhanced by a longer treatment period Multiple high-velocity blows experienced during the USP process caused surface plastic deformation of SLM TC alloy. This layer of plastic deformation was biased towards expansion, but it was limited by the surrounding

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elastic materials, causing compressive residual stress to accumulate. With increasing USP time, the top surface underwent more plastic deformation, leading to a thicker plastic layer and increased interaction between the plastic and elastic components, all of which contributed to an increase in compressive residual stress. To sum up, the residual compressive stress layer and the amount of compressive residual stress can both be increased by prolonging the USP treatment. The SLM TC alloy’s surface is plastically deformed by the USP method, which involves highvelocity impacts. Compressive residual stresses develop in the surface layer as the plastically deformed layer expands within the confines of the surrounding elastic materials. As USP time passes, more plastic deformation accumulates on the surface, resulting in a deeper plastic layer and higher interaction between the plastic and elastic components, resulting in a larger compressive residual stress.

2.3 The Influence of Ultrasonic Shot Peening Parameters on the Fatigue Characteristics of Aluminum Alloy AA7475-T7351: An Investigation of the Microstructure-Fatigue Relationship The results presented here provide conclusive evidence that Ultrasonic Shot Peening treatment significantly increases fatigue life [18]. As a result, optimising process parameters becomes a tough and time-consuming operation. Laser peening [19–21] and ultrasonic peening [22, 23] are two cutting-edge methods developed to overcome these issues. The purpose of these enhancements is to lessen the surface’s roughness and increase the area of the residual stress field’s compression. Aluminum alloys experience work hardening and surface roughness after being shot peened. Work hardening concurrently decreases resistance to fatigue fracture propagation while boosting resistance against crack initiation due to material embrittlement. The choice of shot bead material also assumes a pivotal role in aluminum alloy shot peening. For instance, Luo et al. [24] observed a mere 7% increase in fatigue life when employing steel beads, which generate a roughened peened surface. Conversely, Sharp et al. [25] effectively minimized surface roughness and increased fatigue strength using lighter materials like glass and ceramic beads. The aluminum alloy’s microstructure, which consists of elongated grains that run parallel to the direction of rolling, is seen in Fig. 6a. The focus of Fig. 6b, c is on the surface area that was shot peened using the SB170 and SB110 steel beads, respectively. Steel beads caused a deeper surface layer that was about 100 μm deep and a more extensive damaged region. This increased damage can be attributed to the higher mass of the steel beads in comparison to glass beads. The roughness levels of SB110 and GB35 beads are equivalent to and less severe than those of SB170, as shown in Fig. 6c, d. In comparison to the layer that was shot peened and plastically deformed, these beads likewise exhibit a comparatively low number of shallow surface flaws. When compared to other shot peening series, Fig. 6e shows that

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Fig. 6 Microstructures of: a As-cast aluminum alloy; b USP by SB170; c USP by SB110, d USP by GB35; e USP by GB8 [26]

GB8 beads greatly reduce both the plastic deformation layer and surface roughness. Surface imperfections are absent from the GB8 specimens, nevertheless, as seen in Fig. 6d. These observations highlight the significant influence of shot peening parameters, such as bead diameter and material, on the microstructure and surface characteristics of the aluminum alloy. Scanning electron microscopy (SEM) surface fracture investigation was carried out only on specimens of fatigue tensile that showed both surface and interior crack start. Figure 7 present SEM images of fractured specimens, illustrating surface crack initiation. Figure 7a depicts a macrograph of the SB110_2 tensile specimen fracture surface, and Fig. 7b is showing a more detailed illustration of the crack start site. Figure 7c also displays a macrograph of the broken surface of the untreated Al3 tensile specimen. Although shot peening’s compressive residual stresses in the S110 series are inadequate to totally prevent surface crack initiation, they do have a favorable impact on the series’ fatigue life by lengthening the time before crack initiation happens.

3 Research Gap The results of the reviewed studies indicate that USP can effectively improve the mechanical properties of aluminum die casting alloys by inducing compressive residual stresses, refining the microstructure, and enhancing the surface roughness. The effects of USP on the mechanical properties of these materials can be influenced by various process parameters, such as peening intensity, shot size, and exposure time. By optimizing these parameters, it is possible to enhance the mechanical performance of aluminum die casting components [27–33]. In conclusion, this review paper has

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Fig. 7 Initiation of a surface fracture in the SB110_2 tensile specimen is shown by means of SEM pictures. Δσ = 340 MPa: a A macrograph of the fracture surface; b a closer look at the crack initiation zone; and c SEM pictures of a surface crack in an untreated Al_3 tensile specimen. Δσ = 340 MPa [26]

provided a comprehensive analysis of the effects of ultrasonic shot peening (USP) parameters on the mechanical properties of aluminum die casting alloys. The results of this investigation suggest that USP can effectively improve the mechanical characteristics of aluminum die casting alloys by inducing compressive residual stresses, refining the microstructure, and enhancing the surface roughness. By optimizing the USP process parameters, it is possible to improve the mechanical performance of aluminum die casting components. Acknowledgements The author wishes to express gratitude to the Ministry of Higher Education for their generous support of this study through the Fundamental Research Grant Scheme (FRGS), under the grant number FRGS/1/2022/TK0/UMP/02/67. Additionally, heartfelt thanks are extended to the University of Malaysia Pahang Al-Sultan Abdullah for their invaluable support and financial assistance under the grant RDU Number RDU220138.

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Current Developments and Future Prospects in Vehicle Tire Technologies: A Review Ahmad Noor Syukri Zainal Abidin, Ahmad Shahir Jamaludin, Abdul Nasir, Amirul Hakim Sufian, and Ainur Munira Rosli

Abstract This review discusses vehicle tire technology advancements and their transformative effects on vehicle dynamics. Recent advances in material science, design, and manufacturing have transformed the tire industry. The introduction of “smart tires,” which have sensors for continuous monitoring, is a major development. These tires analyze pressure, temperature, and tread depth to improve safety and fuel efficiency. Nanogenerators in tires demonstrate the automotive industry’s move toward independence. Decision trees and analytical tools have been used to refine the process using retreading techniques, which are environmentally friendly and economically beneficial. The industry is focusing more on integrating intelligent tires with autonomous vehicles. Tire data combined with autonomous driving algorithms could set new safety and efficiency standards. Despite these advances, there is still room for innovation, particularly in commercializing energy harvesters for Tire Pressure Monitoring Systems (TPMS) and developing tire wear monitoring methods. Intelligent tires are increasingly important for vehicle performance and safety as autonomous vehicles become more common. This review discusses tire technologies’ current state, future prospects, and future direction, positioning them as drivers of safer, more sustainable transportation. Keywords Vehicle tire technologies · Intelligent tires · Vehicle dynamics · Electric vehicles · Autonomous vehicles

A. N. S. Zainal Abidin · A. S. Jamaludin (B) · A. H. Sufian · A. M. Rosli Faculty of Manufacturing and Mechatronic Engineering Technology, Universiti Malaysia Pahang Al-Sultan Abdullah, 26600 Pekan, Pahang, Malaysia e-mail: [email protected] A. Nasir Faculty of Electrical and Electronic Engineering Technology, Universiti Malaysia Pahang Al-Sultan Abdullah, 26600 Pekan, Pahang, Malaysia A. N. S. Zainal Abidin Malaysian Institute of Road Safety Research, Taman Kajang Sentral, 43200 Kajang, Selangor, Malaysia © The Author(s), under exclusive license to Springer Nature Singapore Pte Ltd. 2024 R. Abd. Aziz et al. (eds.), Intelligent Manufacturing and Mechatronics, Springer Proceedings in Materials 40, https://doi.org/10.1007/978-981-99-9848-7_12

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1 Introduction on Vehicle Tire Technologies The field of automotive research and development has consistently prioritized the advancement of vehicle tire technologies. Tires are commonly acknowledged as the fundamental element of vehicular performance, as they establish the primary connection between a vehicle and the road surface. In doing so, they exert a significant influence on crucial aspects such as handling, safety, and fuel efficiency [1–9]. Throughout history, the development of tire technologies has been driven by a persistent quest to enhance various facets of vehicular performance [10–19]. The pursuit of excellence has led to the development of various innovations in the automotive industry. One such innovation is the intelligent tire, which incorporates energy harvesters to enhance the safety of autonomous vehicles [1, 20–29]. Additionally, tire condition monitoring systems have been introduced, which not only provide opportunities for improved energy harvesting mechanisms and circuits but also contribute to overall advancements in this field [3, 30–45]. Furthermore, advanced designs and materials have been employed to optimize the reduction of springback in sheet metal bending processes, thereby enhancing the efficiency of the final product [4, 46–53]. In recent years, there has been a notable emergence of intelligent tires, which are equipped with embedded sensors and utilize advanced materials [1, 2, 53–56]. The aforementioned components work together to continuously monitor the conditions of the tires, thereby providing real-time feedback to the control systems of the vehicle [3, 5]. The ability to interact in real-time enables rapid adjustment to various road conditions and driving behaviors, thereby greatly enhancing both the safety and performance of vehicles. In addition, it is worth noting that tire technologies have played a crucial role in improving the stability dynamics of distributed drive electric vehicles as they progress with the advancements in electric and autonomous driving capabilities. This improvement is achieved through mechanisms such as adaptive direct yaw moment control [1]. In the realm of autonomous vehicles, the significance of precise tire performance and condition data has become of utmost importance. This data equips vehicles with the essential information required to make decisions that prioritize both safety and efficiency [3, 9]. In accordance with the prevailing global trend towards sustainability, there is a noticeable transition occurring towards transportation solutions that are more environmentally friendly and technologically advanced. The aforementioned factor has prompted the advancement of tire designs that prioritize energy efficiency by minimizing rolling resistance, thereby improving fuel efficiency [38]. Furthermore, there is a growing interest in the field of self-healing tires, which utilize specific materials and technologies to autonomously mend minor damages. Furthermore, the emphasis on environmentally friendly alternatives underscores the economic and ecological benefits of tire retreading, thereby underscoring the significance of selecting efficient retreading technologies in order to attain sustainability and profitability [21]. This review aims to explore recent advancements in tire technologies, with a specific focus on their implications for the automotive industry and their potential to revolutionize transportation in the future.

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2 Tire Technologies and Their Impact on Vehicle Dynamics In recent years, the tire industry has experienced significant changes as a result of advancements in materials, design, and innovative manufacturing processes [7, 11]. Significantly, the development of intelligent or “smart tires” has facilitated the advent of an era characterized by improved vehicle dynamics and safety. The tires are equipped with sensors that offer immediate data on crucial parameters, including tire pressure, temperature, and tread depth [1, 3]. The depicted continuous monitoring, as shown in Fig. 1, provides drivers with a detailed understanding of tire conditions, facilitating improvements in vehicle safety and optimization of fuel efficiency [3]. One significant focus of tire technology advancement pertains to the minimization of rolling resistance, enhancement of traction, and extension of tire longevity [7]. The incorporation of nanogenerators into tires represents a significant advancement, owing to their capacity for electricity generation. The self-sustaining nature of this capability eliminates the necessity for reliance on external energy sources, thereby establishing the groundwork for autonomous systems that monitor the condition of tires [1, 3]. The field has also adopted tire retreading techniques, which involve revitalizing used tires in order to prolong their operational longevity. The utilization of decision trees and other analytical methodologies has enhanced the retreading process, resulting in increased levels of efficiency and accuracy [21]. Fig. 1 Application of smart tire, real time data measurement [3]

Application

Advantage

FUSION

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The significance of tire technologies in influencing vehicle dynamics is emphasized by numerous studies. This phenomenon governs the manner in which vehicles react to different external stimuli and driving circumstances [1]. There is currently an increased focus on the development of energy-harvesting systems. The strain-based energy harvester presents a potential solution for supplying power to tire sensors [1]. The integration of nonlinear systems with efficient interface circuits has the potential to revolutionize the industry as it moves towards the commercialization of Tire Pressure Monitoring Systems (TPMS) energy harvesters [3]. Furthermore, the utilization of sophisticated algorithms, such as the deep learning-based real-time road surface classification, has the potential to enhance both the safety and performance metrics of vehicles [9]. The utilization of machine learning in predicting tire slip angles is a promising area of research that has the potential to revolutionize vehicle safety and control protocols [50]. An increasing amount of academic literature emphasizes the environmental and economic advantages associated with tire retreading, providing a strong argument for the wider adoption of sustainable retreading methods. These methodologies provide transportation entities with assurance of economic viability, while also promoting environmental conservation [11]. The tire industry, through its continuous research endeavors, is on the verge of significant advancements that have the potential to redefine safety, efficiency, and ecological sustainability in the realm of vehicles. The integration of sensor technology and material science has given rise to the development of “smart tires,” which are considered to be at the forefront of tire technology. These tires are equipped with nanogenerators that utilize piezoelectric, electromagnetic, and triboelectric phenomena, providing valuable insights beyond basic tire conditions. Tire vibration patterns can be analyzed to determine the current state of the road surface, including whether it is wet, dry, icy, or snowy, as shown in Fig. 2 [9]. With the increasing acceptance of autonomous vehicles, the undeniable significance of intelligent tires is becoming more apparent. These vehicles heavily rely on data obtained from sensors to make driving decisions. The provision of real-time feedback regarding parameters such as tire slip, road friction, and tire conditions has the potential to significantly enhance vehicle dynamic controls, thereby improving both safety and efficiency during the journey [1, 3, 7]. The consistency and reliability of data flow in tire sensors is demonstrated by the success of strain-based energy harvesters [9], which possess a self-sustaining nature. However, the field of tire technologies presents ample prospects for additional innovation. There is still potential for further development in the commercialization of TPMS energy harvesters [3]. The integration of contemporary methodologies for monitoring tire degradation not only enhances safety protocols but also advances the pursuit of sustainable lifecycle management [6]. The increasing prevalence of autonomous vehicles in our roadways will inevitably reshape vehicular performance and safety standards through the interaction with intelligent tires.

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Fig. 2 Various tire testing environment of a dry asphalt, b wet asphalt with 1 mm waterfilm, c wet asphalt with 4 mm waterfilm, d gravel, and e unpaved road [9]

3 Safety Considerations and Tire Technologies Safety continues to be a paramount concern within the domain of vehicle design. Given the growing complexities in contemporary automobiles and the incorporation of advanced technologies, the primary objective is to prioritize the safety and welfare of drivers, passengers, and pedestrians [1, 23, 25]. Tires serve as the sole connection between the vehicle and the ground, thus assuming a crucial role in influencing safety outcomes [1]. The advancements in tire technologies can be broadly classified into three key dimensions: 1. Design and Structural Advancements: The fundamental design and architecture of tires directly influence their grip, resilience to punctures, and adaptability across diverse climatic conditions [7]. Specific tread designs, for instance, have been observed to significantly impact stress distribution, with vertical tread designs recording the highest contact stress [38]. 2. Real-time Monitoring Systems: Advanced tire technologies have ushered in an era of real-time monitoring. Intelligent tire systems, a notable evolution in this domain, have capabilities that stretch beyond traditional monitoring. These systems can continually check parameters like tire pressure and temperature. This proactive monitoring notifies drivers about looming issues, potentially averting mishaps like loss of control or a blowout [3, 5]. Furthermore, innovative tire wear monitoring methodologies are pivotal not just for safety, but also for environmental and maintenance benefits [13]. The application of machine learning to accelerometer data is another breakthrough, allowing for precise tire force predictions under varied driving scenarios [39].

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3. Integration with Advanced Vehicle Control Systems: Tire technologies aren’t isolated; they play a collaborative role with advanced vehicle control mechanisms. Data extracted from intelligent tires act as input to stability control systems, refining vehicle handling and minimizing skidding or rollover possibilities [1, 23]. This synergy is even more pronounced in the domain of electric and autonomous vehicles. By offering granular data on tire slip, road friction, and other parameters, these smart tires facilitate meticulous control over vehicle dynamics—a quintessential requirement for the foolproof operation of autonomous vehicles [25–35, 41]. The real-time estimation of tire-road friction coefficients is making leaps in this domain, bringing forth improved accuracy and control [39, 45]. In summary, the importance of advanced tire technologies is heightened as the automotive landscape undergoes changes. The components in question are not merely auxiliary attachments to the automobile, but rather are undergoing a process of advancement and refinement, ultimately making substantial contributions to the overall safety and performance of contemporary vehicles.

4 Gaps and Future Directions Considering the pivotal role of tire technologies in vehicle safety and the growing trends in advanced vehicular systems, several research gaps have been identified. These gaps present opportunities for further advancement in the field of vehicle tire technologies. i. Energy Harvesting in Tires: Although advancements in strain-based energy harvesters have shown promise, there is still limited commercialization of TPMS energy harvesters [1, 3]. More research into nonlinear systems and efficient interface circuits can bridge this gap, ensuring the seamless integration of energy harvesters into the next generation of intelligent tires. ii. Machine Learning in Tire Monitoring: The potential of machine learning in evaluating tire forces, slip angles, and road surfaces is notable [9, 21, 50, 51]. However, the development of robust, real-time machine learning algorithms that can work under varied conditions remains a challenge. This especially concerns the interplay of tire dynamics, road conditions, and vehicular behavior. iii. Tire Wear and Life-Cycle Management: As studies [7, 11, 54] emphasize the ecological and safety implications of tire wear, there’s a pressing need to advance technologies that can effectively monitor, predict, and extend tire life, all while considering environmental impacts.

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iv. Integration with Autonomous Systems: The current advancements hint at the importance of tires in autonomous vehicle control [19, 23, 39, 48]. Yet, a comprehensive integration approach where tire technologies not only communicate but also effectively influence autonomous decision-making systems is still nascent. v. Material Innovation: The effect of different materials and processes on tire performance, such as in laser sintered materials and nitrile rubber, has been explored [35, 46]. A deeper understanding of these materials, their wear patterns, and their interaction with different road surfaces can further improve tire safety and durability. vi. Tire-Road Interaction: The study on tire-road friction and the influence of tread designs remains an essential topic [33, 38]. Newer research should focus on how changing urban infrastructure, like the advent of smart roads, influences these interactions. vii. Enhanced Control Algorithms: With DSPM models showing potential in reducing springback [4, 31] and innovative control strategies emerging for dualmotor autonomous steering systems [48], there remains a gap in combining these technologies. This is to ensure optimal control, stability, and safety across varying driving conditions and road types. viii. Environmental Considerations: With reference to CO2 emissions and the environmental benefits of tire retreading [11, 54], it’s imperative to look at the broader ecological impact of tires. This includes their full life cycle, from manufacturing to disposal, and how innovative recycling or repurposing methods can be developed. ix. Economic Aspects: The economic implications of tire technologies, especially regarding tire retreading and business opportunities from recycling [11, 13], necessitate a deeper exploration. There’s a potential gap in understanding how these technologies can be made affordable, scalable, and profitable for wider adoption. x. Standardized Testing and Verification: With new methodologies allowing third parties to verify vehicle properties from on-road tests [45], it’s crucial to establish standardized testing and verification procedures. This will ensure that the advancements in tire technologies are reliably assessed for their real-world applicability and safety implications. Future Direction Given the identified gaps, the future direction in vehicle tire technologies should aim at developing holistic, integrated systems. These systems should prioritize safety, eco-friendliness, and adaptability to the rapidly changing landscape of autonomous and electric vehicles. Collaborative research, bridging materials science, AI, and vehicular dynamics, will be the key to unlocking the next generation of intelligent, sustainable, and ultra-safe tire technologies.

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Acknowledgements The author acknowledge the Universiti Malaysia Pahang for their support and financial help under PGRS grant, PGRS220366, which has greatly helped in completing this study.

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Experimental of Hot Machining for Stainless Steel 316L Cutting Process Nur Cholis, M. A. H. Yusoff, Syh K. Lim, and Ahmad R. Yusoff

Abstract Stainless Steel 316L having excessive tensile power and resistance to temperature with excessive manganese content resulting high roughness during cutting process. The problem occurs when machining process conduct at hot conditions to soften the workpieces. To study the cutting parameters effect on surface quality and tool wear length, different temperatures were used for turning process in this study. The experiment conducted with hot machining process at temperature conditions at 200, 300 and 400 °C. The parameters of this experiment are cutting speed of 76–149 mm/min and feed rate of 0.11–0.22 mm/rev with constant value of depth of cut. The results showed the surface roughness affects the tool wear when machining at high feed rate and cutting speed compared to lower parameters conditions. The heating source temperature affects the surface roughness, area roughness parameter and tool wear in cutting process. In conclusion, the surface quality and tool wear improved at high feed rates and cutting speeds compared to lower parameters settings. Keywords Hot machining · Stainless steel 316L · Surface roughness

1 Introduction Nowadays Industries aim to produce parts that have a good surface texture and should last longer to be in usable condition. The automotive and aerospace sectors are seeking for novel materials and techniques to improve the component surfaces’ N. Cholis · M. A. H. Yusoff · S. K. Lim · A. R. Yusoff (B) Faculty of Manufacturing and Mechatronic Engineering Technology, Universiti Malaysia Pahang Al-Sultan Abdullah, 26600 Pekan, Pahang, Malaysia e-mail: [email protected] A. R. Yusoff Center for Advanced Industrial Technology, Universiti Malaysia Pahang Al-Sultan Abdullah, 26600 Pekan, Pahang, Malaysia N. Cholis Universitas Pembangunan Nasional Veteran Jakarta, Jakarta Selatan, Indonesia © The Author(s), under exclusive license to Springer Nature Singapore Pte Ltd. 2024 R. Abd. Aziz et al. (eds.), Intelligent Manufacturing and Mechatronics, Springer Proceedings in Materials 40, https://doi.org/10.1007/978-981-99-9848-7_13

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quality while utilising resources as efficiently as possible. [1]. Method of machining also take a part where conventional machine-like turning operation, in which the preheating against workpieces is generate by external heat can be implemented [2]. The technique is usually known as thermal enhanced machining, it was the cutting operation that using the high temperature ranging about 400–700 ºC. In general, hot machining extends tool life by reducing cutting force, improving machined surface smoothness, and increasing material removal rate [3]. The application of inflammable gases in terms as heat source to heat the workpiece that occurs are simple, more clean, easy to handle and cheaper than others hot machining method [3]. The influence of power and machining restrictions on the hot machining of very mechanically durable materials with significant hardness, as well as their favorable effects on wear, gadget life, material departure speed, surface dependability, and chip improvement. This suggests that the machinability of these materials’ improvement, lowering costs and increasing effectiveness [2]. Several parameters determine the cutting tool’s speed and movement. For each operation, these parameters are chosen, based on the material of the workpiece, the material of the tool, the size of the tool and others [4]. The hot machining is performed at the shear zone where the deformation occurs, and it results in a difference in the hardness of the cutting tool by making the work piece less harness in order to decrease the bonding energy and yield strength and make it more ductile [5]. Currently, it’s also given an impact to the surface roughness of the work piece, as the work piece more ductile and this leading to reduce shear strength and deformation hardening [6]. Flank wear was recorded at 5–7 min intervals during machining. As a criterion for tool breakage, 0.3 mm according to ISO measurement was chosen for carbide tools. Tool wear increased with increasing feed rate, and cutting forces increased under both room temperature and high temperature machining conditions [7]. The hot machining of AISI 4340 steel was explored by Trivedi et al. They employed a tungsten carbide cutting tool with a mixture of oxygen and acetylene gas as a heat source. At varied temperatures of 400, 600, and 800 °C, they investigated the individual and combined impacts of cutting parameters (cutting speed, feed rate, and cut depth) on surface roughness [8]. Due to its excellent strength and corrosion resistance, the machinability of stainless steel has garnered a lot of attention. [9]. Therefore, this study is conducted to study the effect of the cutting parameters on surface quality and tool wear length at different temperatures in turning process of stainless steel 316L.

2 Experiments Details The hot machining experiment is carried out using turning machine with flame torch assisted (MAP-Pro Gas). The rod Stainless Steel 316L as a workpiece. Turning tool holder MCLNR1616H12 and the tool cutting model number CNMG120408-HA was prepared as the cutting tool for these experiments. The thermography camera (FLUKE Ti-S20), infrared thermometer RS PRO 1327 K. In order to investigate

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Table 1 Machining parameters Cutting speed (mm/min)

Feed of rate (mm/rev)

Depth of cut (mm)

Temperature (°C)

76

0.11

1.8

200

102

0.18

149

0.22

76

0.11

1.8

300

102

0.18

149

0.22

76

0.11

1.8

400

102

0.18

149

0.22

machining effects of surface roughness, area roughness parameter and tool wear length is measured using LEXT OLS5000 microscope. The cutting speed is main cutting parameters that gives vital cutting movement. It very well may be conferred either on the cutting apparatus or on workpiece by either pivoting it or responding it. The feed rate is an assistant cutting movement is given by the feed speed. Generally, the course of feed speed is opposite to that of the cutting speed. The essential goal of feed speed is to eliminate material from a huge surface. The depth of cut is a tertiary cutting movement that gives important profundity of material that is expected to eliminate by machining. It is normally provided in the third opposite guidance. The machining parameters and their corresponding levels are tabulated in Table 1. The utilization of a torch flame as a heating method emerges as a straightforward and cost-effective approach, thereby maintaining consistent cost and machining quality. The torch is equipped with a valve to control the flame pack and move the cutting tool consecutively. It also has an extension connected to a cylinder of acetylene and an oxygen cylinder. With the knowledge that there was no contact between them, a digital infrared thermometer was used to measure the temperature of the heated work piece, as shown in Fig. 1.

3 Results The proper temperature detect on workpiece, The device that used in this circumstance is thermocouple to reading temperature during machining in running. From the graph the temperature during that circumstance was reach on ± 300 °C, where is can be defined that when the machining operation was conducting the temperature ricing. It’s definitely true due to prior experiment. The experiment was conducting the temperature against the workpiece during machining condition with the design of experiment result to set a certain level (high, medium and low). As the mechanical

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(a)

(b)

Fig. 1 a Schematic diagram. b Experimental setup

properties issues the workpiece temperature during machine need to consider as the surface roughness and tool wear length after the experiment. Figure 2 shows the comparison of workpiece condition between different temperature heat source during that time. The graphical can be described that the room temperature which is consecrated in 32 °C had a high temperature during machining. Temperature at 300 °C have a better machining temperature where it decreases trendline and lastly perform around 150 °C in terms of workpiece condition. Moreover, the workpiece temperature generates heat sources at 400 °C, as a result the good machining around 112.32 °C. Three different temperatures of experiments have been used to run under three parameters where the cutting velocity and surface roughness will be compared with

Fig. 2 Comparison between workpiece temperature, heat source and time

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experimental result. Figure 3 shows that the cutting velocity (mm/min) for every single temperature (32, 200, 300 and 400 °C) versus the surface roughness (Ra) that performs by 3D measuring laser microscope. Since, the best result to machining by flame heat source need to be focused on low feed rate. Cutting speed that comes with 76 mm/min was the best condition in order to cutting workpiece stainless steel 316L. Furthermore, the temperature also gives the big impact in machining at 400 °C for more soften during machining when it performed with low cutting parameter at 76 mm/min cutting velocity. In Fig. 4, it can be shown that when machining is done at various temperatures, the area roughness parameter may provide a graphical result that is increasing when compared to the cutting velocity. As the increasing of cutting speed the area roughness parameter also has been increasing in that circumstance this due to its high cutting speed will affect the area roughness parameter. Furthermore, the temperature was an important issue due to when the machining in raw condition got a poor result than machine by unconventional which is heating up in desired temperature. The best result among of this experiment is when machining at 149 rpm and performed it at 400 °C condition where will be carried of area surface roughness 2.011 Sa. The tool life does really decrease at a constant cutting speed. The longest tool life is obtained when vc = 76 mm/min and the shortest tool life occurs with vc = 149 mm/ min. Since, the graphical graph was showing the result of 3 cutting velocity which is 76 mm/min, 102 mm/min and 149 mm/min. The tool wear length is increasing when is performed a high cutting velocity and generated with low temperature. The results showed in Fig. 5, that the cutting speed plays a dominant role in determining the tool life. Figure depicts the relationship between cutting speed and

Fig. 3 The surface roughness with different temperature and cutting velocity

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Fig. 4 Area roughness parameter of cutting velocity with various temperature

Fig. 5 Cutting velocity versus tool wear length

the tool life in minutes. The graphical result of the force that been exerted during machining for the hot machining using uncoated carbide CNMG120408-HA with its specification 95HV.

4 Discussions Figure 6 illustrates how surface roughness rises with increasing cutting speed at different temperatures (200 °C, 300 °C, and 400 °C). The lowest Ra = 1.206 µm obtained with a cutting speed of 76 mm/min at a temperature of 400 °C. Furthermore,

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with a cutting speed of 149 mm/min, Ra = 3.189 µm (temperature 400 °C), the maximum surface roughness value is recorded. Figure 7 shows the relationship between the cutting speed and temperatures produced from the machining experiment. This study found that the higher cutting speed, the higher temperature. One interesting finding is the area surface roughness (Sa) = 2.011 µm (Vc = 76 mm/min) whereas Sa = 3.508 µm is the highest of area surface roughness condition under temperature 400 °C. The surface roughness of the workpiece is measured using the 3D Measuring Laser Microscope featured in the LEXT software. The point tracking measurement for the cutting speed 76, 102 and 149 mm/min of the workpiece and the temperature for 200, 300 and 400 °C. The tool life decreases at constant cutting speed. The longest

Fig. 6 Various of surface roughness measurement

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Fig. 7 Various of area surface topography with different temperature

tool life is obtained when Vc = 76 mm/min and the shortest tool life occurs with Vc = 149 mm/min. Since, the graphical graph was showing the result of three different cutting velocity which is 76 mm/min, 102 mm/min and 149 mm/min. The tool wear length is increasing when is performed a high cutting velocity and generated with low temperature, as shows in Fig. 8.

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Fig. 8 Tool wear length with different temperature

5 Conclusion In conclusion, the unconventional turning machining experiment showed that higher temperatures yield better results in terms of surface roughness, area roughness parameter, and tool wear. The study focused on analysing and studying the maximum parameters, such as feed rate and cutting speed, and their correlation with the heat source. Moreover, the effect of cutting parameters on the surface roughness of Stainless Steel 316L, whether using coated or uncoated tools, significantly impacted the surface roughness, area roughness parameter, and tool wear. Furthermore, the surface roughness obtained from the hot machining experiment had an impact on tool wear, particularly when machining at high feed rates and cutting speeds compared to lower parameter settings. The experiment revealed that the parameters and the temperature of the heating source in hot machining have an impact on surface roughness, area roughness parameters, and tool wear. The study findings demonstrated that lower feed rates and spindle speeds result in improved diameter and depth accuracy. Moreover, these

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lower settings also contribute to reduced values of surface roughness, the area roughness parameter, and tool wear. For future work, emphasis should be placed on several aspects, particularly the heating method. It is recommended to enlarge the area of the heating spot. Additionally, widening the range of machining parameters, such as higher feed rates, higher cutting speeds, and elevated temperature values, should be explored. Acknowledgements The authors are grateful to the Universiti Malaysia Pahang Al-Sultan Abdullah and the Centre for Advanced Industrial Technology for supporting to achieve this work.

References 1. Srinivas Kumar G, Mohana Reddy YV, Mohana Reddy BC (2023) Experimental study on the influence of turning process parameters on surface texture and material removal rate of composites by using Grey relational Taguchi technique. Mater Today Proc 76:556–563. https://doi.org/ 10.1016/j.matpr.2022.11.163 2. Abdulkareem Mohammed K, Abdulhameed JJ, Al-Ameen ES (2020) The effectiveness of hot machining process for the machinability of hard to cut materials: A review. In: IOP conference series: materials science and engineering. Institute of Physics Publishing. https://doi.org/10. 1088/1757-899X/870/1/012140 3. Pandey K, Datta S (2021) Hot machining of difficult- to-cut materials: a review. Mater Today Proc 2710–2715. https://doi.org/10.1016/j.matpr.2020.12.687 4. Patel MM, Patel SB (2016) A review on optimization of hot machining process. GRD J Eng 1 (Online). Available: www.grdjournals.com 5. Kathiravan C, Jamuna R (2020) Optimization of hot machining in en19 alloy steel by using taguchi method. Int Res J Eng Technol (Online). Available: www.irjet.net 6. Abdulkareem Mohammed K, Nazar Mustafa Al- Sabbagh M, Ali Farhan Ogaili A, Sabah AlAmeen E (2020) Experimental analysis of hot machining parameters in surface finishing of crankshaft 7. Parida AK, Maity K (2019) Analysis of some critical aspects in hot machining of Ti-5553 superalloy: experimental and FE analysis. Defence Technol 15(3):344–352. https://doi.org/10. 1016/j.dt.2018.10.005 8. Trivedi KM, Desai JV, Patel K (2014) Optimization of surface roughness for hot machining of AISI 4340 steel using DOE method. Int J Adv Eng Res Dev (IJAERD) 1(5) 9. Bagaber SA, Yusoff AR (2017) Multi-objective optimization of cutting parameters to minimize power consumption in dry turning of stainless steel 316. J Clean Prod 157:30–46. https://doi. org/10.1016/j.jclepro.2017.03.231

Enhancing Operational Excellence of Wood and Furniture Manufacturing Industry in Malaysia: The Role of Lean Culture as a Generative Mechanism Mohamad Zamir Haszainul, Azim Azuan Osman , Khairunnisa Abdul Aziz, Syed Radzi Rahamaddulla, and Ahmad Nazif Noor Kamar

Abstract This study addresses the research gap in lean manufacturing within the Malaysian wood and furniture industry. While proven effective in the Toyota Motor Company, the application of lean manufacturing practices in other companies remains uncertain. Therefore, this research aims to explore the role of lean culture as a generative mechanism for achieving operational excellence through the adoption of lean manufacturing practices. The proposed mediation research framework draws on a literature review. The independent variable in this study is lean manufacturing practices, encompassing work standardization, build-in quality, and just-in-time production. The mediator variable is lean culture, emphasizing respect for people and continuous improvement. Operational excellence serves as the dependent variable. Data were collected through a survey methodology from 193 wood and furniture manufacturing firms that participated in MTIB’s lean and 5S-good manufacturing practices programs. The collected survey data were analysed using PLS-SEM analysis in SmartPLS 4 software. The results reveal that both lean manufacturing practices and lean culture have a positive influence on operational excellence. Additionally, lean culture mediates the relationship between lean manufacturing practices and operational excellence. This study contributes to the existing knowledge by providing new statistical evidence of the associations between lean manufacturing practices, lean culture, and operational excellence in the context of the Malaysian wood and furniture industry. The findings emphasize the importance of incorporating lean practices and fostering a lean culture to achieve operational excellence. Keywords Lean manufacturing · Lean culture · Operational excellence

M. Z. Haszainul · A. A. Osman (B) · K. Abdul Aziz · S. R. Rahamaddulla · A. N. Noor Kamar Faculty of Industrial Management, Universiti Malaysia Pahang Al-Sultan Abdullah, 26300 Kuantan, Gambang, Malaysia e-mail: [email protected] © The Author(s), under exclusive license to Springer Nature Singapore Pte Ltd. 2024 R. Abd. Aziz et al. (eds.), Intelligent Manufacturing and Mechatronics, Springer Proceedings in Materials 40, https://doi.org/10.1007/978-981-99-9848-7_14

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1 Introduction Lean Manufacturing (LM) is a strategy that employs socio-technical practices to constantly improve manufacturing operations by reducing waste and enhancing value-added activities [1, 2]. Taiichi Ohno was credited as the founder of LM for introducing the Toyota Production System (TPS) to revive the Toyota Motor Manufacturing after World War II and thrive during 1973 global oil crisis. Meanwhile, John Krafcik was the one who first popularized the word “lean” to describe this strategy in the American manufacturing environment. Hence, LM is considered the Americanized version of TPS and is a more common term used by Western manufacturers and scholars [3, 4]. In Malaysia, LM was first formally implemented by automotive manufacturers in conjunction with the Malaysia Japan Automotive Industries Cooperation (MAJAICO) programme [4]. LM was then gradually spread to other industries such as electrical and electronics, food and beverages, iron and steel, aerospace composite as well as wood and furniture [5]. Despite this expansion, there remains a scarcity of academic studies on LM adoption specifically in the wood and furniture industry, both locally and globally [6, 7]. The wood and furniture industry makes a significant contribution to the Malaysian economy. According to the 2019 annual report published by the Malaysian Timber Industries Board (MTIB), the export value of timber and wood products reached RM 22.5 billion, representing a 1% increase from the previous year. This sector accounts for 2.2% of Malaysia’s total exports [8]. Notably, the MTIB plays a crucial role in organizing the Lean Management Programme for wood and furniture manufacturing firms in Malaysia. However. according to [9], LM adoption in the Malaysian wood and furniture industry is still nascent and its success is not yet promising. The adoption of Lean Manufacturing (LM) has been widely recognized as a means to achieve operational excellence in various industries. Companies such as Toyota Motor [10], AstraZeneca [11], IBM [12, 13], Harris Corporation [14], Cogent Power [15], Autoliv Inc. and Boeing [16] have successfully adopted LM to enhance their operational performance. However, alongside these success stories, there are also reported cases of failure [17–19], highlighting the need to investigate the factors that bridge the gap between successful and unsuccessful LM adoptions. David Mann, a well-known author and consultant in the field of Lean Management, has proposed that Lean Culture serves as the missing piece that can bridge the gap between successful and unsuccessful LM adoptions [20, 21]. However, despite this notion, there has been very limited academic study that has empirically examined and verified this association, particularly within the wood and furniture industry. Therefore, the objective of this study is to investigate the role of lean culture as a generative mechanism in achieving operational excellence through the adoption of LM. Lean Culture represents the ideal organisational culture that promotes the success and sustainability of Lean practices within manufacturing organisations [22]. By statistically analysing the relationship between LM adoption, lean culture formation, and operational excellence, this study seeks to provide valuable insights

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into the key factors that contribute to the successful implementation of LM in driving operational excellence. Understanding the role of lean culture as a generative mechanism is crucial for organizations in the pursuit of operational excellence. By exploring how lean culture influences the effectiveness of LM, this research will provide practical guidance for companies, enabling them to foster a culture that supports the sustained adoption of lean strategy.

2 Literature Review 2.1 Operational Excellence Operational excellence is a state where an organisation’s operations are characterised by exceptional performance, efficiency, and effectiveness [23–25]. Measuring operational excellence involves assessing various performance indicators and metrics that reflect an organisation’s day-to-day operations in achieving its objectives. The most common operational excellence measurement used in the Lean Management literature for statistical analysis is operational performance [26–28]. Operational performance reflects the effectiveness of internal operations within a manufacturing firm in terms of waste elimination. Typical indicators of operational performance include cost saving, product quality, resource productivity (labour, machinery, and equipment), manufacturing flexibility (product and volume mix) and achievement of on-time delivery [29, 30]. In line with this, the present study utilised these indicators as measurements of operational excellence, allowing for a valid and comprehensive evaluation of operational excellence in wood and furniture manufacturing firms.

2.2 Lean Manufacturing Practices Lean Manufacturing (LM), which originated from the Toyota Production System (TPS), encompasses a wide range of tools, techniques, and practices aimed at reducing waste in manufacturing operations. Previous studies have extensively examined and identified numerous lean practices. For instance, [31] compiled a list of 48 lean practices based on information extracted from 22 literature sources. Another study by Gurumurthy and Kodali [32] conducted a comparative analysis of published literature up to 2009 and identified a total of 65 lean manufacturing practices. The longest list, proposed by Pavnaskar et al. [33], comprised 101 lean practices. However, considering that the adoption of LM practices among wood and furniture manufacturing firms is still in its early stages, this study specifically focuses on the fundamental pillars and foundations of LM practices as introduced in TPS. These

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fundamental practices include Just-in-Time, Build-in-Quality, and Work Standardisation [10, 34], which are also referred to as lean building blocks [35, 36]. By concentrating on these building blocks, this research aims to measure the basic application of LM within the wood and furniture manufacturing firms in Malaysia.

2.3 Lean Culture Lean culture is described as the ideal organisational culture that is conducive for successful and sustainable adoption of Lean Manufacturing (LM) within business organisations [22]. Previous studies conducted by Bortolotti et al. [37], Cadden et al. [38] and Hardcopf et al. [26] aimed to identify and evaluate specific cultural profiles that support the implementation of lean manufacturing practices. Conversely, [34, 39, 40] assessed the existing organisational culture criteria in relation to the ideal culture necessary to foster the lean transformation journey. For this study, the lean culture dimensions developed by Loyd et al. [34] were adopted. These dimensions were inspired by the original concept of the Toyota Way (TW) culture, which emphasizes “Respect for People” and “Continuous Improvement” [41, 42]. The decision to use these dimensions was based on their alignment with the core principles of the Toyota Way (TW) culture and their relevance to the study’s focus on assessing the current organisational culture within wood and furniture manufacturing firms. The aim is to evaluate this current culture relative to the ideal culture that is suitable for supporting the lean transformation journey.

2.4 Research Model A research model refers to a network of associations among variables of interest in a research study that is logically developed, described, and explained [43]. In this study, a mediation research model was proposed, which included LM practices as the independent variable, Operational Excellence as the dependent variable and Lean Culture as the mediator (see Fig. 1). The research model presented in Fig. 1 consisted of four hypotheses that described the associations between LM practices, Lean Culture and Operational Excellence. These hypotheses were formulated based on several previous studies. Although positive association between LM practices and Operational Excellence (H1) was statistically evident in numerous previous studies [26–29, 44, 45], only few studies were conducted to empirically prove association between LM practices and Lean Culture (H2), Lean Culture and Operational Excellence (3) and indirect effect of LM practices on Operational Excellence through the formation of Lean Culture (H4). Nevertheless, qualitative evidence gathered from experts’ opinions and successful LM practitioners supports the notion that Lean Culture is both an enabler and a result of a successful LM adoption [10, 15, 46, 47]. Lean Culture emerges as a by-product or

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Fig. 1 Lean culture mediation model

outcome of LM adoption [48, 49] while also playing a significant role in determining the success of LM adoption (i.e., operational excellence) [16, 50]. This aligns with the concept of a mediator, which refers to a third variable that explains the generative mechanism through which the independent variable influences the dependent variable of interest [51–53].

3 Methodology This study adopted a survey research design to fulfill the proposed research objectives, as surveys are suitable for gathering quantitative data and testing causal relationships [43, 54]. This study aimed to test the causal relationship between LM practices, Lean Culture and Operational Excellence. Surveys provide a quick, cost-effective, efficient, and accurate means of gathering information about a population [55]. The target population of interest consists of 193 manufacturing firms who participated in the MTIB Lean Management Program and MTIB 5S-Good Manufacturing Practice Program. To determine the minimum sample size required for testing the research model, voluntary sampling was employed. Voluntary sampling is a non-probability sampling technique where potential respondents who are willing and qualified to participate in the survey are selected [56]. Using the G*Power calculator [57] and considering the number of predictors in the research model (e.g., two predictors pointing at the Operational Excellence construct) and standard parameters for behavioural research (effect size, f2 = 0.15; significance level, α = 0.05; and 80% statistical power), the calculated total sample size was determined to be 68 (see Fig. 2).

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Fig. 2 Sample size calculation using G*Power

For data collection, a self-administered questionnaire was designed with four sections representing the constructs under study and a section capturing respondent demographics. The questionnaire items were adapted from various sources, including [30, 34, 58]. To contact the representatives of wood and furniture firms, the MTIB directory was used to obtain their email addresses or mobile phone numbers. The questionnaire forms were distributed to these representatives using online channels such as email and social media platforms like WhatsApp and LinkedIn. Over the course of one month, the study successfully gathered a total of 73 responses, exceeding the minimum required sample size. With 73 samples, the produced results have a statistical power of 83%. These 73 eligible samples represented 73 wood industry and furniture manufacturers in Malaysia. Out of the 73 businesses that responded, the majority (83.56%) were engaged in furniture production, while timber and wood pallet producers accounted for 10.96% and 4.11% of the total, respectively. Interestingly, there was only one business (1.36%) focused on wood art. Examining the duration of lean implementation among the companies, it was found that the majority of them (50%) had implemented lean practices for less than three years. In contrast, 48.08% of the businesses adopted lean between 4 and 10 years ago, while a mere 1.92% had

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implemented it for more than 10 years. To gain further insights into the respondents’ demographics, the study also explored the personal information of individuals who completed the questionnaires on behalf of their companies. The majority of the respondents held middle management positions (67.12%), followed by firstline managers (27.4%), and top managers (5.4%). Some examples of job titles for first-line managers included production supervisor and lean facilitator, while middle managers held positions such as production manager, general manager, and production planner. The top managers in the study were directors. Overall, the study’s comprehensive findings shed light on the various aspects of lean implementation within the wood industry and furniture manufacturing sector in Malaysia.

4 Analysis and Findings This study utilised the partial least squares structural equation modelling (PLS-SEM) analysis to test the proposed research model. The PLS-SEM analysis consists of two phases: the measurement model and the structural model [59]. The analysis was performed using the latest version of SmartPLS software, which is version 4.0.9.5 [60].

4.1 Measurement Model Assessment In the PLS-SEM analysis, the assessment of the measurement model involved evaluating internal consistency reliability, convergent validity, and discriminant validity [61]. The summarized results of these assessments can be found in Tables 1 and 2. Composite reliability coefficients (Rho c) are used to assess the internal consistency reliability of constructs. In contrast, AVE (average variance extracted) values are utilized to evaluate convergent validity. The minimal criterion for convergent validity is to have an AVE of at least 0.50, while a Rho c of 0.70 or higher is considered appropriate [59]. As a result, all constructs met the composite reliability benchmark, with rho c ranging between 0.910 and 0.960. Similarly, all constructs surpassed the threshold for convergent validity, with AVE values ranging from 0.591 to 0.889. Next, this study assesses discriminant validity using hetereotrait-monotrait (HTMT) ratio. HTMT is the ratio between mean of all items’ correlations across constructs measuring different constructs and the mean of the average items’ correlations measuring the same construct [62]. According to Kline [63], HTMT ratios larger than 0.85 signify discriminant validity issues. Table 2 showed that all ratios were below 0.85. Hence, it was confirmed that there was no discriminant validity problem between all constructs in the measurement model.

152 Table 1 Internal consistency reliability and convergent validity

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Constructs

Loadings

LM Practices Just-in-Time

0.916

Build-in-Quality

0.950

Work Standardisation

0.962

Operational excellence Cost saving

0.733

Product quality

0.822

Employee productivity

0.744

Machine productivity

0.726

Product mix flexibility

0.819

Volume flexibility

0.737

Delivery performance

0.792

Lean culture Respect for people

0.935

Continuous improvement

0.948

Rho c

AVE

0.960

0.889

0.910

0.591

0.940

0.887

Note Rho c composite reliability, AVE average variance extracted Table 2 Discriminant validity list: HTMT ratio

Correlations

HTMT ratio

LM → LC

0.835

JIT → LC

0.825

JIT → RP

0.778

JIT → CI

0.810

JIT → OE

0.793

BIQ → LC

0.826

BIQ → RP

0.797

BIQ → CI

0.788

BIQ → OE

0.747

WS → LC

0.804

WS → RP

0.832

WS → CI

0.820

WS → OE

0.799

LM → OE

0.818

RP → OE

0.753

CI → OE

0.819

Note LM Lean Manufacturing, JIT Just-in-Time, BIQ Buildin-Quality, WS Work Standardisation, OE Operational Excellence, LC Lean Culture, RP Respect for people, CI Continuous improvement

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4.2 Structural Model Assessment Furthermore, the assessment of the structural model involves four key steps: collinearity assessment, significance testing, effect size analysis, and evaluation of model explanatory power [59] (Fig. 3). To address collinearity issues between predictor variables, the variance inflation factor (VIF) statistics were utilized. Hypothesis testing involved examining various values, including the path coefficient (β), t-value and p-value to determine the significance of the relationships. The effect size of each predictor variable was assessed using the f 2 coefficient, providing insights into the practical significance of the relationships. Lastly, the model’s explanatory power was evaluated by calculating the coefficient of determination, commonly referred to as R2 , which indicates the proportion of variance explained by the model. All the results from the assessment of the structural model were summarised in Table 3.

Fig. 3 Structural model of Lean Culture as a mediator between LM practices and Operational Excellence. Note Values on the arrow = path coefficients (t-values). Value inside the construct = R2

Table 3 The results of hypothesis testing Hypotheses

VIF

β

H1: LM → OE

4.802

0.327

H3: LC → OE

4.802

0.501

H2: LM → LC

1.000

0.890

29.632

H4: LM → LC → OE

–

0.446

3.149

p

f2

R2

2.032

0.021

0.064

0.640

3.136

0.001

0.150

< 0.001

0.389

0.789

0.001

–

–

t

Note One-tailed test, significant at t > 1.65. VIF variance inflation factor, β path coefficient, SD standard deviation, f 2 = effect size, LM Lean Manufacturing, OE Operational Excellence, LC Lean Culture

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Based on the results presented in Table 3, it is evident that there are no collinearity issues, as indicated by VIF statistics below 5 (VIF < 5) [59]. This confirms the stability and lack of bias in the results. Furthermore, the empirical t-values and pvalues demonstrate that all hypothesised relationships are statistically significant, with t > 1.65 and p < 0.05. Moreover, both LM practices and Lean Culture exhibit a positive influence on Operational Excellence, supported by the positive β coefficients. It is worth noting that LM practices also have a positive impact on Lean Culture. Furthermore, Lean Culture significantly mediates the relationship between LM practices and Operational Excellence. Hence, all hypotheses can be considered supported. The effect sizes indicate the magnitude of the relationships, with LM practices showing a small effect on Operational Excellence, Lean Culture showing a medium effect on Operational Excellence, and LM practices having a large effect on Lean Culture. These magnitudes are determined based on Cohen’s threshold [64]. Lastly, the R2 coefficient for Lean Culture and Operational Excellence indicates a substantial and moderate level of explanatory power, as indicated by Chin [65]. The result suggests that LM practices and Lean Culture effectively explains the variability observed in Operational Excellence.

5 Discussion This study contributes new empirical evidence to the existing body of knowledge by confirming the significant relationships between lean manufacturing practices, lean culture, and operational excellence, particularly in the wood and furniture manufacturing industry. Comparing these findings with previous studies, it is evident that several studies have also found a positive relationship between lean manufacturing practices and operational excellence. Specifically, [26, 27] found similar results in the transportation, machinery, electronics, and automotive manufacturing industries, respectively. These findings support the notion that lean manufacturing practices can lead to improved operational performance across different sectors. Regarding the relationship between lean culture and operational excellence, previous studies by Vlachos and Siachou [66] and Loyd et al. [34] also reported positive associations. Although these studies were conducted in different industries (i.e., oil and energy company and various manufacturing companies), the consistent findings suggest that lean culture plays a crucial role in achieving operational excellence. However, it is worth noting that there is no statistical evidence from previous studies specifically comparing the relationship between lean manufacturing practices and lean culture. Nevertheless, qualitative evidence from studies conducted by Liker [10], Hines et al. [15], Urban [46] and Novac and Mihalcea [47] supports the idea that lean culture emerges as a result of successful lean manufacturing adoption. This qualitative evidence aligns with the findings of the present study, indicating that the

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implementation of lean practices leads to the formation of lean culture, which, in turn, contributes to operational excellence. The findings also highlight the role of lean culture as a mediator between lean manufacturing practices and operational performance. Lean culture is well-suited to serve as a mediator based on the definition of a mediator as a third variable that represents the generative mechanism through which the independent variable influences the dependent variable of interest [51, 53]. In this study, lean culture is described as the ideal organisational culture that is conducive to the successful and sustainable adoption of Lean Manufacturing practices within business organizations. It is measured using two dimensions: respect for people and continuous improvement. Emiliani’s perspective further emphasises the significance of respect for people in distinguishing real lean from fake lean [67]. As a mediator, lean culture acts as the intermediary factor that explains the relationship between lean manufacturing practices and operational excellence. Lean manufacturing practices, such as work standardisation, build-in quality, and just-intime production, are the focal independent variables that directly impact operational excellence. However, it is through the establishment of a lean culture that these practices are effectively implemented and sustained within the organisation, leading to improved operational performance. The positive relationship between lean manufacturing practices and lean culture supports the notion that the adoption of lean practices contributes to the formation of a lean culture. Lean manufacturing practices embody the principles the Real Lean, and their implementation can shape the organisation’s culture. For example, standardised work processes require employee involvement, problem-solving, and teamwork, fostering a culture of continuous improvement and respect for people.

6 Conclusion In conclusion, this study contributes valuable empirical evidence supporting the significant relationships between lean manufacturing practices, lean culture, and operational excellence, particularly in the wood and furniture manufacturing industry. The findings align with previous studies that have also reported positive associations between lean manufacturing practices and operational excellence across various industries. Moreover, the study emphasizes the role of lean culture as a mediator, highlighting the importance of respect for people and continuous improvement in creating an organizational environment conducive to successful lean practice implementation. However, the study acknowledges several limitations that warrant further research for improvement. One significant limitation is the absence of a complete sampling frame for lean manufacturers in Malaysia’s wood industry. This limitation led to a relatively small sample size and potential sampling bias, reducing the generalizability and representativeness of the findings. Future research should address this limitation by establishing a comprehensive sampling frame that includes a wider range of

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lean manufacturers in the wood industry, ensuring a more robust and representative sample. Additionally, the study recognizes the small sample size as a common limitation in lean survey studies in Malaysia. Efforts to increase the sample size were hindered by time constraints and a lack of interest from organizations. Future research should allocate more time and resources to recruit a larger and more representative sample, enhancing the statistical power and generalizability of the findings. In summary, while this study provides valuable insights into the relationships between lean manufacturing practices, lean culture, and operational excellence in the wood and furniture manufacturing industry, the limitations, such as the absence of a complete sampling frame and small sample size, should be considered when interpreting the results. Future research should aim to overcome these limitations to obtain more comprehensive and generalizable findings in the field of lean manufacturing practices and culture. Acknowledgements The authors would like to acknowledge the contributions of each author in the write-up of this paper. The first author conducted the research and prepared the initial draft. The second author provided valuable guidance and feedback as the supervisor of the first author. The remaining authors actively participated in the revision and finalisation of the manuscript, utilising their knowledge and experience in the subject matter to enhance its quality.

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The Effects of Nitrogen-Purged Thermal Debinding and Post-sintering Parameters on Metal Injection Moulded Pulverised Aluminium Alloy Swarf Binded with 100 Vol% of Palm Stearin Sarah B. Yussoff, N. H. Mohamad Nor, H. Husain, and J. B. Saedon

Abstract Metal injection moulding (MIM) is manufacturing method of intricate, high-quality, and high-density parts at feasible costs and capability. In MIM, each phase is crucial the final part outcome beginning with feedstock making, followed by injection moulding, debinding, and lastly, sintering. In sintering, the powder particles are consolidated which induces part shrinkage and robustness. In this study, pulverised aluminium alloy swarf (PAAS) is binded with palm stearin as a standalone binder which is technically unorthodox since binders usually function with at least two components, if not more. Fortuitously, aluminium properties are continuously desired by almost any field or industry and MIM for aluminium is still being pursued and worked on for commercialisation. In this case, with the use of the standalone binder, the debinding and sintering phase are combined and the work and energy required to produce parts are reduced. Both thermal debinding and sintering are conducted within a controlled atmosphere of a constant flow nitrogen gas. The effects of different heating rate and soaking parameters for both thermal debinding and sintering are presented. Thermal debinding soaking temperature should be at 550 °C and below while the sintering soaking temperature should only be caught between 575 and 580 °C. Conclusively, the working samples for further research work or testing can be produced as the plausibility of particulate consolidation is clear. Keywords Metal Injection Moulding (MIM) · Pulverised Aluminium Alloy Swarf (PAAS) · Palm stearin

S. B. Yussoff · N. H. Mohamad Nor (B) · H. Husain · J. B. Saedon School of Mechanical Engineering, College of Engineering, Universiti Teknologi Mara, Shah Alam, Malaysia e-mail: [email protected] © The Author(s), under exclusive license to Springer Nature Singapore Pte Ltd. 2024 R. Abd. Aziz et al. (eds.), Intelligent Manufacturing and Mechatronics, Springer Proceedings in Materials 40, https://doi.org/10.1007/978-981-99-9848-7_15

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1 Introduction Metal injection moulding (MIM) is a mass production manufacturing method of intricate, high-quality, and high-density parts at feasible costs and capability. Some fields that use MIM made parts include automotive, printing, photography, medical equipment, and aerospace, to name a few. It is a branch of powder metallurgy that generally produces at least 10,000 parts and/or products units from metal powder in a cycle. In MIM, each phase is crucial for the outcome of the final part beginning with feedstock making, followed by injection moulding, debinding, and lastly, sintering [1] (Fig. 1). In feedstock making, metal powder particles sized below 20 µm or microns (10–6) are mixed with binding agents to create a homogeneous paste-like compound that is then broken up and hardened into pallet-side fractions. Do note that the binding agents are typically composed of more than one component, minimally two. The binding agent is crucial to provide a homogeneous or well-mixed feedstock compound whilst ensuring pseudoplasticity for the injection phase. Next, in the debinding phase, by several varying methods, most of the binder constituents or primary binder are removed except for the backbone or secondary binder, which is responsible for holding the part shape right before sintering. The secondary binder is usually removed via heat and decomposition right before sintering commences called thermal debinding [3–7]. In sintering, the powder particles are consolidated with one another which induces part shrinkage, and this is how the part robustness is produced. It is normally performed within an ambience of inert gas such as argon, helium or nitrogen to minimalise part oxidation and incineration. In this study, pulverised aluminium alloy swarf (PAAS) is bounded with a standalone (100 vol%) organic binder, the palm stearin (PSr), which is technically unorthodox since binders usually function with at least two components, if not more [2, 8]. As mentioned earlier, most binders consist of a primary and a secondary component where the secondary component acts as the shape holder once the part is removed from the mould. The primary component on the other hand usually contributes to the pseudo-plasticity of the feedstock required during the injection phase. Some researchers typically pair polyethylene (PE) with PSr to form a two-parts binder system with the former acting as the secondary binder component [9–13].

Fig. 1 General MIM phase sequence depiction [2]

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With the PSr acting as a standalone binder, debinding and sintering is combined into one phase, which in turn reduces work and energy required to produce a part. This is intentionalised to align with the current green initiative of the country. Additionally, the green part used for this study has a powder loading 65 vol% which is 5% higher than the common 60:40 powder-to-binder ratio [10]. With a higher powder loading, the shrinkage percentage is reduced and this would enhance the tolerance control for the final part. Another crucial aspect to look upon is of the PAAS or aluminium powder in general. To this day, the MIM of the non-ferrous metal itself in general has yet to be commercialised due to its properties compared to other metals typically manufactured via MIM such as various grades of stainless steel and titanium alloys. Since aluminium properties are continuously desired by almost any field or industry [14–16], MIM for aluminium is still being pursued and worked on for commercialisation.

2 Methodology 2.1 Thermal Debinding and Sintering Beginning with the green part injected such as shown in Fig. 2, the debinding phase, which only encases a single thermal debinding process, is combined with the sintering phase. According to Abd. Aziz’s work [10], only a single binder needs removal and occurs right before sintering begins. These two processes are performed within one equipment which is the glass tube furnace. For this work, the glass tube is filled with nitrogen flowing at 0.1L/min. The glass tube is fitted with the furnace that can heat up up to 1100 °C, where the sintering boat carrying the sample is placed and covered by alumina powder (Al2 O3 ). In Fig. 3, the thermal debinding and sintering profile shows that the cycle begins with thermal debinding from room temperature at rates varying between 0.3 and

Fig. 2 Green part of 65 vol% PAAS powder loading

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Fig. 3 Thermal debinding and sintering profile

1 °C/min. When at 420–550 °C, the temperature set holds between 30 and 300 min. As thermal debinding ends, sintering begins as the temperature hikes up again between 470 and 575 °C between the range of rate of 0.5–5 °C/min, and holds from between 60 and 300 min. The practice for sintering is to set the sintering temperatures approximately 20% lower than the presumed melting point (660 °C) [17]. Each parameter is factored in to observe the effects on the physical and microstructural conditions of the final part and is aimed to be further tested if the parts are completely consolidated. With obvious part shrinkage and consolidation, it signals successful sintering.

2.2 Microstructure Morphology Using the scanning electron micrograph (SEM), the microstructures are observed and finally the apparent defects are recorded. The surface and cross section of the final parts are depicted and compared for analysis to identify which parameter of thermal debinding and sintering had caused the microstructural differences.

2.3 Part Mass Loss Adequate mass-loss is an important indicator that signifies the complete removal of the PSr binder. The weight difference is measured in percentage using Eq. (1), by plugging in the variables of the percentage error formula, where mb, is mass before thermal debinding and sintering, mp , is mass of part post-thermal debinding and

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sintering.   Weight Percentage Difference = 100 mb − mp /mb

(1)

3 Results and Discussions 3.1 Thermal Debinding and Sintering Analysis Post-sintering Analysis The first step of the cycle is thermal debinding (as depicted in Fig. 3; thermal debinding and sintering profile). The PSr binder is removed and decomposed within a range of temperature where PSr is tested to decompose in nitrogen gas ambience via thermogravimetric analysis (TGA). Abolhasani [6] and Ikhwan [12] as well portray in their work that sintering occurs after with elevated range of temperatures that are between 5 and 25% below the material’s melting point (presumably 660 °C for the PAAS). Both thermal debinding and sintering are conducted within a controlled atmosphere of a constant flow of 0.1 L/min nitrogen gas. The total time taken to complete a cycle is between 16 and 40 h, depending on the heating rates applied, and this includes the cooling periods. To note, when alumina powder is not used, the heating pattern on a part is not distributed such as shown in Fig. 4. This confirms the findings of previous researchers’ practices mentioned. The heating rate applied to each thermal debinding and sintering varied from 0.3 to 5 °C/min, where thermal debinding usually conquers 70–85% of the time to complete one whole thermal debinding and sintering cycle. Though PSr is completely removed from each part post- sintering, none of them had good finishes and each part bears defects in accordance to the heating rate, soaking and temperature from respective thermal debinding and sintering steps. Most

Fig. 4 Non-distributed darkened edge region of final parts

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of the sintered parts are brittle to the touch and with slight pressure application, none of the samples qualify for further mechanical or physical testing other than observation and inspection of microstructures and defects. None the less, this work did observe necking within the microstructure of one of the sintered parts although visually that part is blistered and had no signs on shrinkage. The findings are discussed in the following section.

3.2 Post-sintering Analysis From ten (10) variation of parameter combinations, the inspection, analysis, microstructure morphology and defects are correlated with the thermal debinding and sintering parameters. There are six (6) parameters factored in which are the thermal debinding heating rate, thermal debinding holding duration, thermal debinding temperature, sintering heating rate, sintering holding duration and sintering temperature. In Table 1, several outcomes observed include brittleness, robustness, tightly packed particles, loosely packed particles, particle size segregation, and necking. As mentioned above, only one sample exhibited necking between particles and does not break, even when severely poked or stabbed with stainless steel utensils. Unfortunately, none of the samples are able to be further tested via physical or mechanical testing due to reasons stated before. Effects of Thermal Debinding Temperature. Firstly, at 420–550 °C of thermal debinding temperature, PSr is removed completely. When evaluated, the average weight difference in percentage is at 16.33% (refer to Table 1). During feedstock Table 1 Colour coded thermal debinding and sintering parameters Sample

Thermal Debind (°C/min)

Thermal Debind Temp.(°C)

SoakingTime (min)

0.3 0.4 0.5 0.6 0.7 1 2 3 7 2.2

0.5 0.5 1 0.3 0.5 0.5 0.3 0.5 0.5 0.3

470 470 470 470 550 500 500 500 420 470

30 60 60 120 180 300 300 300 300 120

Stunted sinter (enlarged particles)

no crack or bulge

sinter (necking)

Sintering HR (°C/min ) 5 1 0.5 1 0.5 0.5 0.5 1 1 1

Desired

Sintering Temp. (°C)

Soaking Time (min)

575 600 600 600 600 575 575 575 447 530

60 120 120 120 120 120 120 120 180 180

15.04 15.70 15.53 23.61 19.84 13.90 13.67 16.08 13.87 16.07 Avg.

Undesired

Unsure

16.33

Weight (%)

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making, each batch is prepared at 15 g at a time and the weight of 35 vol% of PSr accounted for about 20% of each batch. This as well indicates complete binder removal. Effects of Thermal Debinding Holding Duration. Here, it is unclear to whether holding at the set temperatures for more than 120 min is unsuitable or vice versa. Additionally, it is also unapparent when held for 300 min. But it is apparent that even 30 min of holding duration is sufficient to completely remove the binder. This is because the samples that are held between 120 and 300 min had similar microstructure morphology, although their physical appearances seem independent of the holding duration, shown in Fig. 5. While in Fig. 6, sample AL 0.7 has a flat cross section rather than a bulging one of sample AL 3. Effects of Thermal Debinding Heating Rate. Next, when looking into the heating rate for thermal debinding, at 1 °C/min, blistering and cracking (Fig. 7) can be seen on the surface of the final parts due to rapid evaporation of binder. This indicates that said thermal debinding heating rate is too high. Effects of Sintering Temperature. As we move on to the final and most crucial and complex part of MIM, this where sintering resides as its presence is mostly eluded. Beginning with the sintering temperature, it usually ranges from 5 to 20% below a

Fig. 5 a AL 0.7 and b AL 0.3; similar cross-sections but different physical appearance

Fig. 6 a AL 0.7 and b AL 3; AL 0.7 has a flat cross section rather than a bulging one of sample AL 3

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(a)

(b)

Fig. 7 a No shrinkage post-sintering; cracks formed; b sample with blistering post-sintering

melting point. In this case, the presumed PAAS is at 660 °C. This means that sintering temperature falls between about 530–630 °C. In this case, set temperatures are at 530, 575, and 600 °C. However, necking is not present at 530 and 600 °C (darkened outer region such in Fig. 9a), and at 615 °C the part fails to retain its shape. This means that the mentioned three temperatures are not the suitable for sintering the PAAS green part. However, at 575 °C, necking (Fig. 8a) is observed but since the sintering heating rate is too high, blistering and micro-cracks are present as well. At 600 °C, the final part (Fig. 8b) seemed to be darkened on the outer layer which signifies that the temperature might have been too high although it still retained its shape. Also, enlarged particle grains are observed and this is an indication that the consolidation process is stunted or interrupted as the temperature increased up to 600 °C. These larger particles indicate that the once smaller particles had consolidated and clumped up to one another but did not get to finish what they were doing as the temperature continued to rise above the suitable sintering temperature, which after analysis is assumed to be between 575 and 580 °C.

(a)

(b)

Fig. 8 a Necking and spherical morphing in particles. b Unchanged particle size, tightly packed

The Effects of Nitrogen-Purged Thermal Debinding and Post-sintering …

(a)

169

(b)

Fig. 9 a Enlarged particles, stunted consolidation. b Mixed between two significant particle size range

Effects of Sintering Heating Rate. Another aspect to discuss is the sintering heating rate. At 1 °C/min, all the parts sintered at that rate shows lower defective degree to none. Which makes 1 °C/min an ideal sintering heat rate. Although necking is observed even at 5 °C/min, a significantly faster rate, the defects occurred almost everywhere in the microstructure morphology (micro-cracks) (Fig. 8a) and even physically (blistering). Effects of Sintering Holding Duration. Lastly, the holding duration for sintering, the only sample that is consolidated is when it is held for only 60 min, maximum. Any other holding duration for sintering had no presence of necking or consolidation whatsoever. As proof, even when at 575 °C, the assumed sintering temperature, no necking is observed but interrupted consolidation (enlarged particles) when held for 120 min (Fig. 9a) to 180 min. It is even more apparent when a lower sintering temperature which is held at 530 °C for 180 min (Fig. 9b), no necking is observed and uneven clumps of larger particle grains. This implies that the holding duration for sintering PAAS is substantially lesser and can be between 50 and 80 min, any longer would hinder consolidation.

4 Conclusion In conclusion, due to a large or wide matrix factor of parameters, a viable sample for mechanical testing could not be produced. However, from observation, it is still possible to produce mechanical-testing-worthy samples with optimal parameter combinations. As such, the effects of different heating rate and soaking parameters for both thermal debinding and sintering are presented. Ideal thermal debinding heating rates should be held under 0.5 °C/min, as this promotes complete removal of the PSr binding agent within the shortest soaking

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duration of 30 min. That said, increased soaking duration is often practiced to ensure complete binder removal. Next, the thermal debinding soaking temperature should be kept at 550 °C and below to avoid any premature particulate agglomeration. Consequently, for the actual particle consolidation phase, which is during sintering, the heating rate can only be maxed at 3 °C/min, with the holding duration kept at less than 80 min. This is to devoid the sample of cracking defects due to rapid particulate amalgamation. Lastly, the sintering soaking temperature should only be caught between 575 and 580 °C as it is observed that at higher centigrade causes the sample to lose its form. Additionally, at any lower centigrade, it would reflect stunted particulate agglomeration and consolidation. As such, working samples for further research work or testing can be produced as the plausibility of complete particulate consolidation is apparent. This work means to pave way for aluminium alloy MIM using a single constituent organic binder (PSr) in such promotes not only improved energy efficiency during production but also in proving the capability of the standalone binder as a viable agent even with a “notorious” material such as aluminium. Acknowledgements The authors would like to express their gratitude to the School of Mechanical Engineering, College of Engineering, Universiti Teknologi MARA and the Malaysian Ministry of Education for research support.

References 1. Suwanpreecha C, Alabort E, Tang YT, Panwisawas C, Reed RC, Manonuku A (2021) A novel low-modulus titanium alloy for biomedical applications: a comparison between selective laser melting and metal injection moulding. Mater Sci Eng A 812 2. Yussoff SB (2023) Metal injection moulding of aluminium swarf using palm stearin as a standalone binder. Master Thesis UiTM 3. Côté R, Azzouni M, Demers V (2021) Impact of binder constituents on the moldability of titanium-based feedstocks used in low-pressure powder injection molding. Powder Technol 381:255–268 4. Rolere S, Soupremanien U, Bohnke M, Dalmasso M, Delafosse C, Laucournet R (2021) New insights on the porous network created during solvent debinding of powder injection-molded (PIM) parts, and its influence on the thermal debinding efficiency. J Mater Process Technol 295 5. Park DY, Oh Y, Hwang HJ, Park SJ (2018) An experimental approach to powder-binder separation of feedstock. Powder Technol 306:34–44 6. Abolhasani H, Muhamad N (2010) A new starch-based binder for metal injection molding. J Mater Process Technol 210(6–7):961–968 7. Asmawi R, Ibrahim MHI, Amin AM, Mustafa N, Alawi N (2014) Mixing study of aluminium waste as metal powder for waste polystyrene binder system in metal injection molding (MIM). Appl Mech Mater 660:239–243 8. Abd Aziz SN (2017) Effect of palm stearin as single based binder on properties of ceramic injection molded of hydroxyapatite for scaffold applications. Thesis, Universiti Teknologi Mara, Shah Alam 9. Zainon N, Omar MA, Sauti R, Marzuki M (2019) Elucidating the influences of torque and energy in determining optimal loading. 16:2144–2152

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10. Arifin A, Sulong AB, Muhamad N, Syarif J, Ramli MI (2014) HA/Ti6Al4V powder with palm stearin binder system—feedstock characterization. Appl Mech Mater 564:372–375 11. Basir A, Sulong AB, Jamadon NH, Muhamad N (2021) Feedstock properties and debinding mechanism of yttria-stabilized zirconia/ stainless steel 17-4PH micro-components fabricated via two-component micro-powder injection molding process. Ceram Int 47(14):20476–20485 12. Ikhwan M (2015) Developement of porous Ti-6Al-4V mix with palm stearin binder by metal injection moulding technique. Thesis, Universiti Teknologi Mara, Shah Alam 13. Shanmuganantha L, Khan MUA, Sulong AB, Ramli MI, Baharudin A, Ariffin HM, Abd Razak SI, Min Hwei Ng (2022) Characterization of titanium ceramic composite for bone implants applications. Ceram Int 48(16):22808–22819 14. Puga H, Barbosa J, Soares D, Silva F, Ribeiro S (2010) Recycling of aluminium Swarf by direct incorporation in aluminium melts. J Mater Process Technol 209(11):5195–5203 15. Qian M, Schaffer GB (2010) Sintering of aluminium and its alloys. In: Sintering of advanced materials. Woodhead publishing series in metals and surface engineering 16. Chintada S, Dora SP, Kare D, Doddi PRV (2021) Developments in sintered aluminium based composites. Metal Powder Rep 76(6):1–11 17. Abd Aziz SN, Ali NHM, Abu Bakar MA, Subuki I, Ismail MH (2015) The influence of single based binder of palm stearin in HAP feedstock on rheological properties used for ceramic injection moulding (CIM). Adv Mater Res 1134:220–224

Hybrid Machining: A Review on Recent Progress N. N. Nor Hamran, J. A. Ghani, R. Ramli, and W. M. F. Wan Mahmood

Abstract Hybrid manufacturing, a pioneering concept in modern industry, combines various manufacturing methods to achieve unparalleled performance and versatility. By seamlessly integrating diverse technologies, it overcomes limitations of individual techniques while leveraging their strengths. This review explores recent progress in hybrid manufacturing, including trends, performance outcomes, and challenges. Notably, there is a substantial trend towards combining traditional and additive manufacturing (59%). Processes like WAAM, LMD, SLM, FFF, and FDM gain traction, especially for materials like ferrous metals, non-ferrous metals, and composites. Performance outcomes are substantial. WAAM improves part performance, geometry control, efficiency, surface quality, and environmental impact. LMD integration enhances feature addition, stability, precision, and resource efficiency. SLM combined with subtractive methods enhances surface quality, mechanical properties, and intricate part feasibility. FFF combined with subtractive techniques addresses anisotropy, surface roughness, and geometric accuracy. Laser-assisted methods like LOMM and LAM enhance material removal, surface quality, and machining efficiency. Vibration-assisted techniques boost material removal rate, surface quality, and overall machining performance. However, challenges in hybrid machining are evident across multiple categories, including workpiece materials, machine tool development, process understanding, monitoring systems, heat affected zones, equipment costs, productivity, environmental impact, qualification procedures, and technology transfer. Overcoming these challenges requires interdisciplinary collaboration, innovative solutions, and technological advancements. Effectively addressed, hybrid machining has the potential to revolutionize manufacturing, significantly improving efficiency, precision, and sustainability.

N. N. Nor Hamran (B) Faculty of Manufacturing and Mechatronic Engineering Technology, Universiti Malaysia Pahang Al-Sultan Abdullah, 26600 Pekan, Pahang, Malaysia e-mail: [email protected] J. A. Ghani · R. Ramli · W. M. F. Wan Mahmood Faculty of Engineering and Built Environment, Centre for Materials Engineering and Smart Manufacturing, Universiti Kebangsaan Malaysia, UKM, 43600 Bangi, Selangor, Malaysia © The Author(s), under exclusive license to Springer Nature Singapore Pte Ltd. 2024 R. Abd. Aziz et al. (eds.), Intelligent Manufacturing and Mechatronics, Springer Proceedings in Materials 40, https://doi.org/10.1007/978-981-99-9848-7_16

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Keywords Hybrid machining · Hybrid manufacturing · Assisted manufacturing process · Additive manufacturing

1 Introduction In the dynamic world of modern manufacturing, the pursuit of more efficient, precise, and versatile production methods has led to the exploration of innovative techniques beyond traditional boundaries. Hybrid Manufacturing (HM), integrating various manufacturing processes, especially additive manufacturing (AM) and subtractive manufacturing (SM), has emerged as a promising paradigm. This fusion of manufacturing techniques enables the creation of intricate structures with enhanced material properties and precision. HM synergizes AM’s design flexibility and intricate part fabrication with SM’s precision and surface finish capabilities. This convergence benefits industries like aerospace, automotive, healthcare, and consumer goods by eliminating limitations of standalone manufacturing processes. Research articles show remarkable improvements in machining outcomes through HM compared to standalone methods. Recent times have seen growing interest in HM processes, with approximately 94 research articles published from 2019 to 2023. Despite considerable attention, there is a shortage of comprehensive review articles summarizing recent innovations in HM. Only a few reviews cover hybrid additive manufacturing, while others focus on hybrid electrochemical and electrical discharge processes, laser-based HM, and HM for specific materials or tools. This study aims to provide a comprehensive review of advancements in HM processes from 2019 to 2023. The paper is structured as follows: Sect. 2 discusses trends, and assesses machining outcomes. Section 3 addresses challenges in HM, and Sect.4 concludes the paper.

2 Hybrid Machining Techniques 2.1 Trends of Hybrid Machining This subsection reviews recent trends and advancements in HM. It analyzes a range of research articles from 2019 to 2023 in databases like ScienceDirect, Scopus, and IEEE Xplore, shaping the future of modern manufacturing. The findings are presented in Fig. 1, following a new proposed classification of HM processes and summarized in Table 1. Figure 1 shows that the majority of research articles (59%) involve processes in subgroup IIB, particularly with Direct Energy Deposition (DED) methods like Wire Arc Additive Manufacturing (WAAM) and Laser Metal Deposition (LMD). Other significant areas of research include Powder Bed Fusion (e.g., Selective Laser

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Hybrid Machining : Recent Combination Trends Subgroup IIA 6% Subgroup IB 3%

Subgroup IA 32%

Powder Bed Fusion 15% Other 59% Binder Jetting 3% Material Extrusion 5%

Direct Energy Deposition 36%

Subgroup IA

Subgroup IB

Subgroup IIA

Material Extrusion

Binder Jetting

Powder Bed Fusion

Direct Energy Deposition Fig. 1 Distribution of research articles on hybrid machining (2019–2023) based on the new proposed classification

Melting (SLM)) and Material Extrusion (e.g., Fused Filament Fabrication (FFF) and Fused Deposition Modeling (FDM)). Furthermore, Fig. 1 highlights established processes in subgroup IA (32%), with laser-based approaches being prominent. Vibration assistance and ultrasonic vibration processes indicate an interest in enhancing tool-material interaction and overall machining efficiency. Figure 2 illustrates the distribution of research papers in HM categorized by workpiece material type. The bar graph in Fig. 2 provided highlights the distribution of HM workpiece materials across different categories. The most prominent trend is the utilization of both ferrous metals (38.9%) specifically stainless steel alloys and non-ferrous metals (44.4%) especially Inconel 718 and Ti-6Al-4 V, and lightweight aluminum alloys such as Al 6061 T6 as workpiece materials. Composite materials also show promise with 8.3%, indicating their relevance in sectors like aerospace and automotive. This indicates an emerging trend in using HM for composite materials which are composed of multiple constituent materials. The presence of diverse materials such as displayed in Fig. 2 reflects ongoing research and development efforts to expand the scope of HM techniques. In summary, this data reflects a nuanced approach to HM research, aligning techniques with the unique characteristics of different workpiece materials.

Process

Reference

[1]

[9, 10]

[16, 17]

[21, 22]

[28, 29]

[39–44]

Process

Magnetic Field Assisted Powder Mixed

Focused Ion Beam

Thermally assisted

Electrochemical

Robotic

Cooling system

[19]

[12]

[3]

Reference

[60–67]

Laser assisted

[68–73] [74–81] [82–93]

WAAM Other DED

[58, 59]

[54, 55]

[48, 49]

[45]

[31–38]

[24–27]

[20]

[13–15]

[4–8]

Reference

LMD

Laser Cladding

[56, 57]

Laser-Induced Oxidation Assisted

LSF

SLM

DMD

DED

LPBF

DLMS

BJAM

FFF/FDM

Process

DLD

[30]

Powder bed fusion

Binder jetting

Material extrusion

Type

[50–53],

FSW and Machining

Turn Rolling [23] combined and Deep Rolling

Injection Moulding and Machining

Arc Welding and Milling

Gas Metal Arc Welding (GMAW) and Machining

Process

Subgroup IIB (Combined Traditional and Additive Manufacturing Routes

Ultrasonic vibrative assisted

[18]

[11]

[2]

Reference

Subgroup IIA (Traditional Manufacturing Routes)

Vibration assisted [46, 47]

Laser Shock Processing with Post-Machining

Laser Ablation and Implant Surface Treatment

Laser Ablation and Diamond cutting

Subgroup IB (Mixed Processes)

Subgroup IA (Assistive Processes)

Table 1 Research articles on hybrid machining (2019–2023) based on the new proposed classification

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40 30 20 10 0 Ferrous Metal

Non Ferrous Composite Metal Material

Non Metal

Organic Intermetallic Compound Alloy

Fig. 2 Distribution of research articles on hybrid machining categorized by workpiece material type (2019–2023)

2.2 Hybrid Machining Performance This subsection provides a concise overview of recent trends in HM processes: ● WAAM in HM: WAAM improves part performance, mechanical properties, geometry control, and deposition quality [74, 78]. It enhances process efficiency, surface quality, and environmental impact reduction [77, 80]. WAAM is flexible and compatible with various manufacturing scenarios [81]. ● LMD in HM: LMD adds complex features to pre-formed forgings, reducing postprocessing needs and improving resource efficiency. It ensures stability, precision, and machinability. Research focuses on cutting fluids and optimization. LMD’s applications include aviation parts and complex components. ● SLM in HM: Combining SLM with subtractive machining improves surface quality, precision, and mechanical properties. Studies examine phase transformation, process parameters, and practical applications. Cryogenic cooling enhances machining performance. ● FFF in HM: FFF’s cost-effectiveness is compared with machining approaches. HM addresses FFF limitations, mitigating anisotropy and surface roughness. The response of FFF components to machining is analyzed. Precision machining with laser processing enhances shape and surface quality. ● FDM in HM: FDM integrates dielectric components with metallic structures, optimizing performance. A hybrid system combines FDM with CNC machining for large-scale production. The combination of FDM with machining allows costeffective production of intricate components and products. ● Laser-assisted machining: Laser-Induced Oxidation Assisted Machining (LOMM) improves machinability [56]. LOMM is used to fabricate multiscale structures. Laser-Assisted Machining (LAM) enhances efficiency while controlling heat effects [94–97]. Green Ceramic Machining (GCM) and Green Ceramic Hybrid Machining (GCHM) aim to increase productivity and surface quality. Laser-Assisted Grinding (LAG) minimizes damage and enhances surface characteristics.

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● Vibration-assisted machining: Vibration Assisted Electrical Discharge Drilling (VA-EDD) improves material removal rate and surface finish. Ultrasonic vibration-assisted dry grinding is environmentally friendly and enhances surface quality. Ultrasonic-Assisted Drilling (UAD) is effective for micro-hole drilling. Proper horn design enhances machining efficiency. UAD improves hole quality and reduces thrust force in Cf/SiC composites.

3 Challenges in Hybrid Machining HM, as discussed in the previous Sect. (2.2), offers improved mechanical properties, enhanced surface quality, and better machinability and material removal. However, it still faces several challenges, summarized in Table 2. To effectively advance HM, these challenges need attention across workpiece, machine tool, process, and outcome categories. Addressing them requires interdisciplinary collaboration, including materials science, precision engineering, optimization, and environmental considerations. Developing novel solutions, advanced monitoring techniques, and improved simulations is vital. Standardized qualification procedures, operator training, and economic assessments are essential for seamless integration into various industries, enhancing manufacturing efficiency, precision, and sustainability.

4 Conclusion This paper reviews recent articles on HM, examining trends, machining outcomes, and associated constraints. The key conclusions are as follows: 1. Hybrid Machining Techniques: ● Hybrid approaches include assisted, mixed, traditional, and combined traditional/additive methods. ● Recent trends favor combined traditional/additive routes (59%), focusing on WAAM, LMD, SLM, FFF, and FDM. ● Workpiece materials: ferrous metals (specifically stainless steel alloys), nonferrous metals (such as Inconel 718 and Ti-6Al-4V, and lightweight aluminum alloys such as Al 6061 T6), and composites. 2. Hybrid Machining Performance: ● WAAM improves part performance, geometry control, efficiency, surface quality, and reduces environmental impact. ● LMD enhances stability, precision, resource efficiency, and adds complex features.

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Table 2 Challenges in hybrid machining Category

References

Challenge description

Workpiece

[98]

Machining of thin substrate

[99, 100]

Limited material diversity, mainly aluminum alloy suitable for effective additive manufacturing

Machine Tool

[101, 102]

Development of specific high-precision multi-axis tools with attributes like precise feed drives, exceptional stiffness, thermal stability, and minimal vibration

Process

[100, 103, 104]

Understanding process and parameters for desired results

[105, 106]

Controlling different machining philosophies and material removal mechanisms according to machine tool and workpiece attributes

[107]

Lack of design for high-pressure coolant delivery for efficiency and waste reduction

[101, 105]

Development of multiscale and numerical modeling for accurate simulation of hybrid micro-machining

[101, 106]

Improvement of monitoring systems to track parameters during micromachining

[108]

Controlling the heat affected zone

[103]

Expensive equipment costs

[100, 101]

Lack of novel hybrid micro-machining processes and limited energy resource diversity

[98, 99, 104, 105, 107, 109]

Higher surface and subsurface damages, especially in mechanical micromachining due to heat generation

[98, 104, 108, 109]

Achieving dimensional accuracy and precision, particularly in laser micromachining

[108]

Minimizing the formation of recast layer

[98]

Significant tool wear due to abrasive workpiece characteristics

[98, 109]

Slow process time leading to low productivity

[98]

Cleaning after machining

[98, 107]

Environmental hazards such as the impact of cryogenic coolant on the environment)

Outcome of the process (affecting the workpiece and cutting tool)

Outcome of the process (others)

(continued)

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Table 2 (continued) Category

References

Challenge description

[99, 103]

Insufficiency in qualification and certification procedures for skilled equipment operators

[101, 107]

Challenges in transferring technology to industries due to limited adoption, requiring further research on economic perspectives

● SLM combined with subtractive machining boosts surface quality, mechanical properties, and enables complex part fabrication. ● FFF combined with subtractive processes addresses anisotropy, surface roughness, and geometric accuracy. ● Laser-assisted processes (LOMM, LAM) improve material removal, surface quality, and efficiency. ● Vibration-assisted techniques (VA-EDD, ultrasonic vibration, ultrasonicassisted drilling) enhance material removal rate, surface quality, and machining performance. 3. Challenges in Hybrid Machining: ● Challenges in workpiece materials, machine tool development, process understanding, monitoring, heat affected zones, expenses, productivity, environmental impact, qualification procedures, and technology transfer. ● These challenges span various categories and require interdisciplinary solutions and technological advancements. ● Addressing these challenges can enhance manufacturing efficiency, precision, and sustainability in HM.

References 1. Rouniyar AK, Shandilya P (2019) Improvement in machined surface with the use of powder and magnetic field assisted on machining aluminium 6061 alloy with EDM. In: IOP conference series: materials science and engineering 2. Han J, Li L, Lee W, Lee WB (2019) Machining of lenticular lens silicon molds with a combination of laser ablation and diamond cutting. Micromachines 3. West JL, Betters ED, Schmitz T (2019) Low cost platform for hybrid manufacturing of light metals. Null 4. Urbanic RJ, Saqib S, Saqib SM, Saqib SM (2019) A manufacturing cost analysis framework to evaluate machining and fused filament fabrication additive manufacturing approaches. Int J Adv Manuf Technol 5. Ferreira I, Madureira R, Villa S, Jesus AMPD, Jesus AD, Machado M, Alves JL (2020) Machinability of PA12 and short fibre–reinforced PA12 materials produced by fused filament fabrication. Int J Adv Manuf Technol

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Sustainable Manufacturing Practices in the Sports Industry: A Review of Biodegradable Polymers for Sports Equipment Mohd Nizar Mhd Razali, Nurul Hasya Md Kamil, Ainur Munira Rosli, Amirul Hakim Sufian, and Teo Chong Yaw

Abstract The convergence of the global sports sector and the entertainment industry has increased sports equipment demand and highlighted the importance of sustainable manufacturing. This transition is driven by environmental concerns and renewable resource potential. Biodegradable polymers, which are environmentally friendly and have excellent physicochemical and mechanical properties, are becoming viable alternatives to non-renewable synthetic fibers. Polymers in sports equipment reduce environmental impact and boost domestic industries. Sustainable sports manufacturing explores and advances eco-friendly fiber-reinforced composites, natural composites, and hybrid fibers with nanoparticles. Natural fibers like coconut tree peduncle fiber are being studied as synthetic fiber substitutes in the automotive and marine industries. Due to their improved mechanical properties, sustainable fiberreinforced composites like Date palm and Kenaf fibers are gaining popularity in the sports industry. However, manufacturing issues like ultrasonic connection durability in shoe components and titanium marine part surface irregularities must be addressed. The review emphasizes biodegradable polymers in sports equipment. It thoroughly reviews sustainable sports manufacturing research and suggests new directions. Keywords Sustainable manufacturing · Sports industry · Biodegradable polymers · Natural fiber-reinforced composites · Hybrid fiber-based composites

M. N. Mhd Razali (B) · N. H. Md Kamil · A. M. Rosli · A. H. Sufian Faculty of Manufacturing and Mechatronic Engineering Technology, Universiti Malaysia Pahang Al-Sultan Abdullah, 26600 Pekan, Pahang, Malaysia e-mail: [email protected] T. C. Yaw INTI International College Penang, 1-Z, Lebuh Bukit Jambul, Bukit Jambul, 11900 Bayan Lepas, Pulau Pinang, Malaysia © The Author(s), under exclusive license to Springer Nature Singapore Pte Ltd. 2024 R. Abd. Aziz et al. (eds.), Intelligent Manufacturing and Mechatronics, Springer Proceedings in Materials 40, https://doi.org/10.1007/978-981-99-9848-7_17

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1 Introduction Sustainable Manufacturing in the Sports Industry The global sports sector has grown, converging with the entertainment industry thanks to technology and information. The integration has captivated billions worldwide [1–5]. This phenomenon has increased demand for sports equipment, prompting the industry to improve manufacturing and consider environmental impacts. Thus, sports equipment manufacturing has shifted toward environmentally sustainable manufacturing. The transition is driven by global environmental concerns and the recognition of renewable and sustainable resources [5–12]. The sports industry is interested in biodegradable polymers because they are environmentally friendly. These materials are environmentally friendly and have excellent physicochemical and mechanical properties, making them suitable for sports equipment [12–19]. They can replace expensive, non-renewable synthetic fibers like glass, carbon, and aramid [15–23]. Biodegradable polymers in sports equipment reduce environmental impacts and boost domestic industries by reducing imports [1–5]. Sustainable sports manufacturing research includes the development of environmentally friendly fiberreinforced composites [5–12], the integration of natural composites [3, 4], and the use of hybrid fibers with nanoparticles [15–23]. The above studies have shown that these substances often outperform non-renewable ones. Industries seeking eco-friendly materials prefer sustainable fibre-reinforced composites. Many sectors employ Polymer Matrix Composites (PMCs), which show potential [1–5]. Polymer matrix composites (PMCs) gain strength and fracture toughness from thermosets or thermoplastics [1–5]. Manufacturing methods considerably impact product design and performance. High thermal conductivity and dielectric characteristics make private military companies (PMCs) promising in microelectronics [1–5]. Industry 4.0 and ICT have changed seamless clothing development [5–12]. Seam-less synthetic and artificial polymer clothing is comfortable, fits well, and is inexpensive. Innovative clothing require current technology, integrating traditional materials with cutting-edge technology [5–12]. Natural fibers like coconut peduncle fiber can substitute synthetic [8–11]. Composites made with unsaturated polyester resin and fibers have exceptional mechanical properties, especially at 40 wt% [8–11]. Chemical interaction between fiber and matrix makes these composites suitable for automotive and marine applications [8–11]. Sports are embracing sustainable fiber-reinforced composites. Epoxy hybrid composites with date palm fiber (DPF) and kenaf (KF) enhance tensile strength and modulus [12–19]. Alkali reduces composite water absorption and thickness swelling [12–19]. Typha angustifolia-based NFRPCs are also important. Fiber orientation strongly impacts composite properties, as shown by the success of composites with 20% TFR in bidirectional (BD) orientation [15–23]. Building and automobile industries benefit from sustainable composites. Date palm fibers (DPF) in phenolic composites increase mechanical and thermal characteristics, especially following NaOH treatment [19, 22–29]. Sustainable composites are adaptable for building and automotive use [22–29]. Epoxy-embedded olive/bamboo hybrid

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composites exhibit better thermal stability [8]. OTS-B hybrid composite performs well, suggesting biological, automotive, and construction uses [8]. Date palm fiber reinforces polypropylene composites, demonstrating the value of sustainable biomaterials [9]. These synthet-ic composite alternatives have shown that treatments can considerably enhance tensile strength and modulus. These composites are great for eco-friendly products [9]. Besides material innovation, researchers have studied how different manufacturing methods affect bioplastic container durability and appearance [19]. These methods ensure that products are sustainable and meet sports industry standards. However, issues persist. Increasing ultrasonic shoe component connection durability remains a challenge [22–29]. A deeper study is needed to correct surface irregularities in titanium marine components made by particulate injection molding [8–12]. These challenges require ongoing sustainable sports manufacturing research. This review focuses on biodegradable polymers in sports equipment and provides a holistic view of sustainable sports manufacturing research and development. This statement emphasizes environmental responsibility, explains biodegradable polymers’ benefits, and reviews current research. It also identifies research gaps, guiding future research. This review promotes biodegradable sports equipment and sports industry sustainability.

2 Natural Fiber Reinforced Composites Due to their unique features and sustainability, more sectors are using natural fiber reinforced composites (NFRCs). The composites in this study are largely natural fibers and polymers. Strong, flexible, and lightweight, these composites have diverse uses [12–19]. NFRC PMCs are employed in numerous sectors. Recent additions include thermosets or thermoplastics to matrix polymers and fibers. Strength and fracture toughness define private military companies (PMCs). Manufacturing methods shape product design. Private military businesses (PMCs) offer potential in microelectronics due to their thermal conductivity and dielectric characteristics [1–5]. Renewable flax, hemp, and jute make natural fiber reinforced composites (NFRCs) sustainable. These fibers have less environmental impact than synthetic ones. These fibers strengthen composites’ structural and mechanical qualities. A sustainable polymer matrix joins fibers, dispersing stress and boosting composite robustness in varied situations. Selecting NFRCs reduces product environmental impacts and promotes a circular economy that maximizes resource utilization and eliminates waste. NFRCs are cheaper than synthetic composites economically. This makes them ideal for cost-sensitive applications. Locally sourced natural fibers can boost local economies and create agricultural and manufacturing jobs [11]. Plant-based natural fiber reinforced composites (NFRCs) use flax, hemp, jute, and bamboo fibers. Each fiber has unique properties. Flax fibers are known for their strength and stiffness, while bamboo fibers are known for their flexibility [3–9]. These natural plant fibers

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and a biodegradable matrix create a strong, eco-friendly composite. These composite materials are ideal for sports equipment due to their excellent mechanical properties. These fibers’ sustainable cultivation practices, which avoid synthetic fertilizers and pesticides, enhance their environmental benefits. Prioritizing plant-based fibers can boost local economies by increasing demand for indigenous crops and creating jobs [8–11]. The following fiber-reinforced hybrid composites were developed recently:

2.1 Utilization of Date Palm Fibers-Reinforced Hybrid Composites in the Sports Industry The utilization of Date Palm Fibers (DPF) as reinforcement in hybrid composites is emerging as a significant advancement within the sports sector. These fibers have historically been linked to various cultural and practical uses, primarily in regions such as the Middle East, where they are derived from the plentiful date palm trees [1– 5]. Nevertheless, the recognition of their inherent capacity in the composite industry has only been recently realized. The increasing emphasis on sustainability and the need for high-quality materials has brought attention to DPF as a valuable resource in the sports industry [5–12]. When incorporated into hybrid composites, typically in conjunction with other natural or synthetic fibers, DPF enhances the mechanical properties of the composite, resulting in increased strength and efficiency as it has higher content of lignin and lower cellulosic content, as shown in Fig. 1 [22–29]. DPF-infused composites are establishing a distinct presence within the realm of sports. The individuals are currently engaged in the manufacturing of athletic footwear, which provides the necessary durability without adding extra mass. This ensures that athletes experience both comfort and achieve their highest level of performance [8–11, 30–40]. Moreover, the significant level of impact resistance exhibited by these materials renders them highly suitable for use in protective gear, including helmets and pads, thereby enhancing safety measures for athletes. The integration of

Fig. 1 The view of a 20 µm and b 100 µm magnification of cross-section of date palm fibre [22]

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Fig. 2 Performance of date palm fiber composite [22]

diesel particulate filters (DPF) in sports equipment represents a commitment to environmental sustainability, surpassing their mere mechanical capabilities, as shown in Fig. 2. By leveraging an underutilized resource, the field of sports can effectively tackle the environmental challenges associated with waste and promote the adoption of a circular economic framework [12–19]. Furthermore, the incorporation of date palm fiber (DPF) into sports equipment provides a solution to the waste challenges associated with date palm cultivation, creating a symbiotic relationship between the environment and the industry.

2.2 Utilization of Banana Fiber-Reinforced Hybrid Composites in the Sports Industry Banana fiber-reinforced hybrid composites have recently gained attention as a promising innovation within the sports industry [1–5]. These fibers, which were previously considered waste, originated from the extensive cultivation areas of bananas in tropical and subtropical regions and were either disposed of or burned. This practice not only presented environmental challenges but also disregarded the intrinsic value of these fibers [5–12]. Due to advancements in material science and a heightened emphasis on sustainability, there has been a growing interest in the extraction and purification of these fibers for incorporation into hybrid composites. When combined with other natural or synthetic fibers, the resulting material demonstrates improved mechanical properties, rendering it suitable for a wide range of sports applications. Athletic footwear uses composite materials extensively. Banana fibers give the shoes strength and longevity [12–19]. The lightweight fibers ensure comfort and agility in the shoes, which is vital for athletes. Banana fiber-reinforced composites can also be used in sports helmets [15–23]. The composites improve athlete safety

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by resisting impact. This makes helmets absorb and disperse external pressures well. A major benefit of using banana fibers in composites is their sustainability [19]. The sports industry may reduce carbon emissions and banana agricultural waste by using these fibers. Banana fiber-reinforced hybrid composites are environmentally friendly and can improve sports equipment manufacture [30–40].

2.3 Utilization of Kenaf Fiber-Reinforced Hybrid Composites in the Sports Industry Kenaf fibers (KF) have gained increasing recognition in the sports industry due to their potential as reinforcement materials in hybrid composites. Kenaf, an indigenous plant found in certain regions of Africa and Asia, has historically been utilized for a diverse range of applications, such as the production of ropes, twines, and sackcloth. Nevertheless, the utilization of this technology in the field of composite materials has only emerged in recent years [12]. The growing focus on materials that are sustainable and environmentally friendly has elevated the prominence of kenaf fibers. When incorporated into hybrid composites, typically in combination with other natural or synthetic fibers, the addition of KF improves the overall mechanical and thermal characteristics of the material, as shown in Fig. 3 [12]. This characteristic renders it a viable candidate for high-performance applications within the sports industry. KF-reinforced composites are being studied for sports applications. Their evaluation is for athletic equipment like rackets, where strength-weight balance is crucial. Kenaf fibers’ inherent strength and low mass make rackets durable and maneuverable [1–5, 12]. Due to their high tensile strength and impact resistance, KF-reinforced composites are useful in making protective gear like shin guards and helmets. These features increase athlete safety protocols, minimizing injury risk [8–11]. Additionally, KF (kinetic friction) in sports equipment improves mechanical performance and shows the sports industry’s sustainability. Kenaf, a renewable resource, reduces environmental impact and fosters a circular economy. Kenaf cultivation improves soil health and reduces greenhouse gas emissions, highlighting its environmental benefits [12–19].

3 Manufacturing Techniques and Challenges 3.1 Ultrasonic Impact on the Strength Characteristics of Joining the Parts of Summer Shoes Ultrasonic welding is an advanced manufacturing technique that utilizes highfrequency ultrasonic acoustic vibrations to generate a weld in a solid-state manner. This particular technique demonstrates notable efficacy in the process of bonding

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Fig. 3 Mechanical properties of Kenaf—Date palm fiber hybrid [12]

plastics and analogous materials, rendering it a preferred option in diverse sectors, including the field of sports. For instance, in the sports shoe production, ultrasonic welding is frequently utilized to merge different shoe components, such as the upper and the sole [1–5]. The ultrasonic welding process generates heat through friction, melting the materials at the joint. As these materials cool, they solidify, forming a bond. This technique is swift and efficient, ideal for mass production. Additionally, the absence of adhesives or other supplementary materials enhances the sustainability of the manufacturing process. However, there are challenges. The strength of the joints is a primary concern. Factors like the materials used, joint design, and ultrasonic welding parameters (vibration amplitude, applied pressure, welding duration) can influence joint strength [1–5]. Some materials might not bond well under ultrasonic vibrations. Joint design can also affect bond strength. Hence, comprehensive research is essential to optimize these factors, ensuring durable and high-quality sports shoes.

3.2 Surface Irregularities in Titanium Marine Parts Formed by the Particulate Injection Moulding Process Particulate injection moulding is a manufacturing technique used to craft intricate, precision parts from metal or ceramic powders. The process involves blending powders with a binder to create a feedstock, which is then heated and injected into a mould. Once the mould is filled, the part is cooled, ejected, and the binder is removed, resulting in a dense, net-shape part [5–12]. This method is invaluable for crafting parts with complex shapes or intricate details. However, surface irregularities, such as pits or rough patches, can affect both the performance and aesthetic quality of the parts. In marine applications, where titanium is favored for its corrosion resistance and high strength-to-weight ratio, these irregularities can lead to increased friction

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and reduced efficiency [5–12]. Research is crucial to understand and prevent these irregularities. This might involve studying the effects of various process parameters or developing new techniques to enhance the surface finish of the parts.

3.3 Aesthetic Quality and Strength of Bioplastic Biocontainers at Different Substrate Volumetric Water Contents Bioplastic biocontainers, made from biodegradable polymers, offer an eco-friendly alternative to traditional plastic containers. Derived from plant-based polymers, these containers decompose naturally in a significantly shorter time, making them a sustainable packaging option [8–11]. However, manufacturing these bioplastic biocontainers presents challenges, particularly in maintaining their aesthetic quality and strength at varying substrate volumetric water contents. The water content can influence the bioplastic’s properties, leading to changes in the container’s appearance and performance [8–11]. For instance, high water content can render the bioplastic more flexible but less robust. Conversely, low water content can make it more brittle but stronger. Further research is vital to understand the water content’s impact on bioplastics and devise strategies to ensure container quality under different conditions. This could involve studies on the effects of varying water contents on bioplastic properties or the development of new processing techniques to control water content [8–11].

4 Gaps and Future Directions Within the manufacturing sector of the sports industry, especially with bioplastic biocontainers. Their resilience and visual appeal can vary, especially if they are subjected to variations in the volumetric water content of the substrate, particularly in shoe components. An extensive and diverse research strategy is required to address these issues. This strategy could entail conducting experimental research to explore the possible mixes of nanoparticles, biodegradable polymers, and natural fibers. Computational research can support these empirical studies by modeling material behaviors and providing efficacy predictions. Additionally, it is essential to improve and streamline the current manufacturing processes, adjust related parameters, and come up with creative solutions to address the problems that are currently facing the industry. Stronger connections, for example, could result from fine-tuning the ultrasonic welding process’ parameters. In the ongoing quest for environmentally friendly materials, some natural substitutes have gained prominence. One notable contender to replace traditional synthetic fibers is the fiber found in the peduncles of coconut trees. Its potential applications, which

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go beyond the sports industry to industries like automotive and marine, demonstrate its versatility. This points to a more widespread shift in the industry toward the use of sustainable materials. An interdisciplinary approach to research is necessary to close these gaps. This could include testing different combinations of natural fibers, nanoparticles, and biodegradable polymers through experimental studies. Computational studies that model material behavior and forecast performance outcomes could be a good addition to these. Furthermore, it is imperative to enhance current manufacturing methodologies, optimize parameters, and develop approaches to address obstacles. Acknowledgements The author is grateful to the Ministry of Higher Education for funding this study under the Fundamental Research Grant Scheme, grant number RACER/1/2019/TK05/UMP// 1. This research would not have been possible without their support of academic innovation. We also thank the Universiti Malaysia Pahang Al-Sultan Abdullah for their generous support and funding under grant RDU210312.

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Orthogonal Cutting Performance of Vegetable-Based Lubricants via Minimum Quantity Lubrication Technique on AISI 316L Amiril Sahab Abdul Sani , Zubaidah Zamri , Shahandzir Baharom, Mugilan Ganesan, and Norfazillah Talib

Abstract In this research, the workpiece material used is AISI316L stainless steel, which has higher corrosion resistance and is also difficult to machine at high speeds. The objective of this study is to determine the machining performance of 316L stainless steel using minimum quantity lubrication (MQL) and dry machining. The effects of MQL lubricants and dry machining are then studied and compared in terms of cutting performance, such as tool chip contact length, chip thickness, and cutting force (N). The MQL lubricants used are a bio-lubricant: Crude Tamanu Oil (CTO), Crude Jatropha Oil (CJO), Synthetic Ester (SE) and Refined Bleached and Deodorized Palm Olein (RBDPO). The cutting insert used in this study is an uncoated tungsten-carbide insert (WC) SPGN120308 to ensure that the surface of the carbide insert is in direct contact with the stainless-steel disc. The cutting and MQL parameters are set to be the same for both MQL and dry machining. After machining, the micrographic representations of the chip and inserts are magnified by examination with a scanning electron microscope using energy dispersive X-ray spectroscopy (SEM–EDX) to identify any material adhering to the rake face of the tool. It is found that SE gives the best machining performance compared to the CTO, CJO, RBDPO and dry machining. Nevertheless, CTO and other crude vegetable oils are exhibiting high potential to be used as bio-based metalworking fluids following chemical modifications to improve their anti-wear and anti-friction capabilities. Keywords Cutting performance · Orthogonal cutting · MQL · Lubrication · Plant-based oil

A. S. Abdul Sani (B) · Z. Zamri · S. Baharom · M. Ganesan Faculty of Manufacturing and Mechatronic Engineering Technology, Universiti Malaysia Pahang Al-Sultan Abdullah, 26600 Pekan, Pahang, Malaysia e-mail: [email protected] N. Talib Department of Manufacturing Engineering, Faculty of Mechanical and Manufacturing Engineering, Universiti Tun Hussein Onn Malaysia, 86400 Batu Pahat, Johor, Malaysia © The Author(s), under exclusive license to Springer Nature Singapore Pte Ltd. 2024 R. Abd. Aziz et al. (eds.), Intelligent Manufacturing and Mechatronics, Springer Proceedings in Materials 40, https://doi.org/10.1007/978-981-99-9848-7_18

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1 Introduction Machining, also called metal removal, is a subtractive manufacturing process in which material is removed from the workpiece layer by layer using cutting tools to achieve the desired shape and scale. The amount of heat flux flowing to the cutting tool during the cutting process has a major impact on tool wear as plastic deformation usually occurs in the shear zone of the metal being machined [1]. Metalworking fluids (MWF), also known as lubricants, are needed to reduce friction between worn parts on the surface, increase tool life, lower the cutting temperature, and improve machining efficiency and surface quality. They also act as lubricants, coolants, cleaning agents, and corrosion inhibitors when a protective lubricating layer is applied to metal-tometal sliding surfaces. This is because the chemicals in the lubricant can reduce the friction between the two contact surfaces of the materials and thus reduce the heat produced when the surface interacts [2]. Excellent cutting performance is achieved through the ability of metalworking fluids to provide lubrication and dissipate the heat, resulting in less heat generated at the cutting edge of the object being machined. MQL or minimal quantity lubrication uses a combination of compressed air and cutting fluids, which produce mist. The mist is dispersed on the surface contact between the tool and the workpiece, thus resulting in lower temperature production, and helps to improve the flow of the chips across the tools by providing lubrication and cooling down the contact surfaces. Cutting fluid flow rates in MQL are significantly lower than the conventional machining methods [3]. In comparison to dry cutting, MQL provided lubricating and cooling effects that increased tool life [4, 5]. Mineral oil is the most typical form of lubricant however the usage of mineral oil-based lubricant causes a variety of health issues and pollution [6]. Researchers expect that demand for oil-based mineral metalworking fluids will rise because of increased demand from emerging markets. It is commonly known that global mineral reserves are depleting and that all resources will be extracted from the earth’s crust one day [7, 8]. To deal with the issues, a new alternative has been explored to discover an alternative that can be the greatest option to replace the oil-based mineral metalworking fluids [9, 10]. The most suitable oil-based mineral alternative is vegetable oil; however, vegetable oil is a tricky non-toxic alternative making most research focused on how to utilize it as a metalworking fluid. It is due to vegetable oils having extremely high kinematic viscosity and viscosity index than mineral oil. However, vegetable oil does not emit poisonous gas during the machining, and more environmentally friendly. The fact that it is biodegradable and renewable is the most crucial element in selecting the oil as an alternative source for metalworking fluid [11]. Crude jatropha oil (CJO), Crude Tamanu oil (CTO), Synthetic ester (SE), and Refined Bleached Deodorised Palm Olein (RBDPO) are vegetable oils that were used in this experiment. In this research, the aim was to investigate the cutting performance of stainless steel 316L when employed with these lubricants via minimal quantity lubrication (MQL) techniques and comparing them with the dry machining.

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2 Methodology The workpiece material that is used in this research is AISI 316L stainless steel disc with a thickness of 2 mm. Stainless steel was chosen because of its great corrosion resistance and resistance to thermal oxidation. Due to its high yield strength, it has good energy absorption properties, and can sustain a high level of strength even at extremely high temperatures. AISI 316L has great manufacturing features. Because of the AISI 316L composition materials, the stainless steel has good chlorine resistance and corrosion cracking of stress resistance. Table 1 shows the composition of elements in AISI 316L.

2.1 MQL Lubricant Preparation The MQL lubricants used to conduct this machining experiments are Crude Jatropha Oil (CJO), Synthetic Ester (SE), Refined Bleached Deodorised Palm Olein (RBDPO) and Crude Tamanu Oil (CTO) as depicted in Fig. 1.

2.2 Workpiece Preparation The AISI 316L undergoes milling operations such as facing, centering, marking, patterning, pocketing, and island process to get the desired shape. Figure 2 shows the flow of the process for AISI 316L preparation in this experiment while Fig. 3 shows the specimen’s dimension. Table 1 AISI 316L disc specimen element composition [1]

Element present in AISI 316L disc

Composition (wt.%)

Carbon

0.025

Nitrogen

0.068

Sulphur

0.003

Phosphorus

0.025

Silicon

0.064

Manganese

1.680

Molybdenum Nickel Titanium Niobium Chromium

2.380 10.120 0.001 0.045 17.60

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Fig. 1 MQL lubricant sample; a RBDPO, b CTO, c CJO and d SE

Fig. 2 The process of preparing workpiece sample

2.3 Orthogonal Machining Orthogonal cutting process is a process where the cutting edge is perpendicular to rotation axis of the workpiece and was carried out on a CNC lathe machine ROMI C420. In this experiment, uncoated tungsten carbide (WC) inserts with the ISO number SPGN 120,308 are purchased. The indexable square shape of this insert has a positive rake angle of 5°. The inserts (brand: Korloy) are made of fine carbide grains that can withstand high-cutting tool edge wear indefinitely [12]. The distance between the nozzle orifice and the cutting insert is set to 8 mm. The angle of inclination of

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Fig. 3 The dimension of disc specimen

the nozzle should be 45° to make sure the dispersant of lubricant in contact with the insert and workpiece as depicted in Fig. 4 respectively [13]. After all the turning parameter was set, the MQL device’s pressure was released, and the lubricant began to disperse to ensure that the lubricant dispersion was stable. The orthogonal turning procedure of the workpiece with the cutting parameter is as follows [14]. It is started once the lathe machine has been filled with fog [15]. When turning begins, the MQL device must first disseminate the lubrication. The suggested MQL parameter is listed in Table 2. After that, all the chip samples are collected and measured for their thickness.

3 Results and Discussion 3.1 The Viscosity for Each Lubricant Sample The outcomes for each lubricant sample’s kinematic viscosities and the viscosity index (VI) are shown in Table 3. CJO possesses the highest viscosity index (VI) which is 310 and followed by SE, which is 187, and RBDPO, 172. This clearly demonstrates that CJO, although in a crude state, it can be a good lubricating oil by nature while CTO possesses the lowest viscosity index which is 142. The high VI indicates that the lubricant may maintain its effectiveness of keeping the oil layer protection film even at high temperature conditions [16].

3.2 Cutting Force Cutting force is one of the important characteristics in turning operations because it can determine the amount of power required for machining [17]. Shearing forces

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Fig. 4 Orthogonal cutting experimental setup

Table 2 Machining parameter setup

Parameter

Value

MQL outlet pressure

0.4 MPa

MQL spray flow rate

0.16 L/hr

Inner diameter of nozzle

2.5 mm

Tool edge-nozzle distance

8 mm

Inclination angle of nozzle

45°

Table 3 The viscosity value for each lubricants sample Lubricants

Viscosity index (VI)

Kinematic viscosity at 40° (mm2 /s)

Kinematic viscosity at 100 °C (mm2 /s)

SE

187

21.50

5.20

CTO

142

68.99

10.62

CJO

310

30.71

9.30

RBDPO

172

40.24

7.89

distort the material being cut while machining a ductile material, generated plastic deformation and ductile fracture on the metal layer (chips). Large cutting forces indicate the formation of high shear strains on the shear plane [18].

Orthogonal Cutting Performance of Vegetable-Based Lubricants … Table 4 Cutting force generated for each lubricant sample

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Lubricant sample

Cutting force (N)

Cutting speed (m/min)

100

125

150

Dry machining

2452.4

3566.65

3394.93

SE

1891.31

2092.04

2612.88

RBDPO

2317.98

2598.86

2951.90

CJO

2388.09

3264.34

3265.99

CTO

2216.41

3119.73

3222.01

Table 4 depicts the increasing pattern of cutting speed and cutting force. SE had an especially significant contribution in reducing the resulting cutting force. SE has a good impact on the workpiece and tool during machining since the cutting force is lowest. In other words, SE is suited as a cutting fluid for AISI 316L machining. The CJO and CTO achieved nearly equal results. The cutting force for dry machining is the most severe, which indicates that the tool and insert contact is less successful when no lubricant is present than for CJO, CTO, SE, and RBDPO.

3.3 Thickness of the Chips The type of metal being machined, whether brittle or ductile, as well as the temperature at the cutting zone, determine the chip thickness produced during machining. Friction between the insert and the workpiece causes this temperature to rise [19]. The fundamental impact on chip formation and thickness is high heat and stresses induced by high deformation resistance of cutting inserts and the material of the workpiece being cut [20]. The thickness of the chip is measured with a micrometer screw gauge. Table 5 shows that due to the lack of lubrication, Dry machining produces the highest average chip thickness while SE produces the lowest average chip thickness compared to CJO, CTO, and RBDPO. This is due to the greater friction and rubbing that happens during dry machining which affects the chip thickness and formation [21]. Table 5 The thickness of the chips for each lubricant sample

Lubricant sample

Chip thickness (mm)

Cutting speed (m/min)

100

125

150

Dry machining

0.36

0.43

0.50

SE

0.25

0.34

0.38

RBDPO

0.26

0.35

0.43

CJO

0.26

0.39

0.47

CTO

0.24

0.27

0.32

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Lubricant

Chip contact length

Cutting speed (m/min)

100

125

150

Dry machining

6.53

5.55

4.45

SE

4.24

3.89

3.27

RBDPO

4.99

4.46

3.58

CJO

6.13

5.34

4.24

CTO

5.78

5.12

3.98

3.4 Tool Chip Contact Length Tool chip contact is observed under an optical microscope. As depicted in Table 6, although SS 316L is a hard-to-machine material, SE lubricant able to reduce the tool chip contact length as the cutting speed increases from 100, 125 and 150. The lowest tool-chip contact length proves that the sticking and sliding region is smaller which mean the material removal rate is higher. Since no lubrication is used, dry machining produces the worst results in terms of tool chip contact length [5].

3.5 Tool Rake Surface Tool rake surface can be defined as the chip-flowing surface which is when chips generated by the shearing effect during machining have flowed over the rake surface and out of the cutting zone. The flow of the chips over the rake surface causes intense rubbing, which raises the cutting temperature [9]. As shown in Figs. 5 and 6, CJO and SE still show the existence of an insert element which is the tungsten (W) element which shows that the material of workpieces does not adhere to the tool rake surfaces. Differing to CTO as depicted in Fig. 7, it has a highly adhered material at the insert surfaces. Dry machining also reveals adhered material at the insert surfaces, but not to the same extent as CTO machining as shown in Fig. 8. In addition, the wear at CTO’s insert is obvious.

4 Conclusions From the results, SE gives the best machining performance compared to CTO, CJO, RBDPO, and DRY machining. This is because SE possesses higher viscosity index than CTO and RBDPO. As a result, SE has the lowest cutting force, finest chip, and minimum tool chip contact length, resulting in longer tool life and fewer tool wear. Next, the CTO gives the worst performance compared to CJO, SE, and DRY machining. CTO and RBDPO’s high kinematic viscosity values at low temperature

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Fig. 5 Element graph for CJO-150

Fig. 6 Element graph of SE-150

may result in fewer atomization molecules being dispersed across the cutting zones. The thicker oil may not offer enough lubrication around cutting, exposing more dry surfaces to the tool insert [2]. Nevertheless, CTO and RBDPO can still be used as metalworking fluid however further research on chemical modification needs to be done to improve their properties such as their anti-wear and anti-friction capabilities. Finally, using dry machining at low cutting speed or below 100 m/min is not ideal because it will damage the cutting tool.

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Fig. 7 Element graph of CTO-150

Fig. 8 Element graph of Dry machining-150

Acknowledgements The author acknowledges the financial assistance from the Ministry of Higher Education Malaysia and Universiti Malaysia Pahang Al-Sultan Abdullah (UMPSA) via the UMPSA internal grants (PGRS220371 and RDU230311) as well as the Fundamental Research Grants Scheme FRGS/1/2019/TK03/UMP/02/19 (University reference RDU1901145). The technical aid from UMPSA’s staff as well as the laboratory facilities are duly recognized for their supports and expertise.

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References 1. Amiril SAS, Rahim EA, Syahrullail S (2017) Tribological performance of modified jatropha oil containing oil-miscible ionic liquid for machining applications. J Mech Sci Technol 31:5675– 5685 2. Amiril SAS, Baharom S, Mamat NA, Mohd Rozlan AS, Talib N (2022) Materials today: proceedings, comparative evaluation of crude tamanu oil performance as metalworking. fluids 48:1783–1788 3. Amiril SAS, Zamri Z, Megat Ahmad Radzi PH, Sabri AM, Talib N (2022) Modified tamanu plant-based oil from Pahang Malaysia as biodegradable metalworking fluids. Mater Today Proc 75:39–45 4. Amiril SAS, Rahim EA, Hishamudin AZ (2019) Effect of nozzle distance and cutting parameters on MQL machining of AISI 1045. J Phys Conf Ser 1150:012045 5. Amiril SAS, Rahim EA, Sharif S, Sasahara H (2019) Machining performance of vegetable oil with phosphonium-and ammonium-based ionic liquids via MQL technique. J Clean Prod 209:947–964 6. Chan C-H, Tang SW, Mohd NK, Lim WH, Yeong SK, Idris Z (2018) Tribological behavior of biolubricant base stocks and additives. Renew Sustain Energ Revie 93:145–147 7. Grzesik W (2016) Advanced machining processes of metallic materials: theory, modelling and applications, 2nd edn. Elsevier, Netherlands 8. Reda ZKH, Nahed KA, Mai KF, Shakinaz TE (2021) Experimental investigation and process simulation of biolubricant production from waste cooking oil. J Biomass Bioenergy 144:105850 9. Jamaluddin NA, Talib N, Amiril SAS (2020) Tribological analyses of modified Jatropha Oil with hBN and graphene nanoparticles as an alternative lubricant for machining process. J Adv Res Fluid Mech Therm Sci 76:1–10 10. Mohamed SP, Mohamed NP (2019) Exploration, and enhancement on fuel stability of biodiesel: a step forward in the track of global commercialization, 1st edn. LAP LAMBERT Academic Publishing, UK 11. Amiril Sahab AS, Nor Athira J, Ahmad Shahir J, Norfazillah T (2021) Calophyllum-Inophyllum from Pahang Malaysia as biolubricant feedstock for industrial application. In: Osman Zahid MN, Abdul Sani AS, Mohamad Yasin MR, Ismail Z, Che Lah NA, Mohd Turan F (eds) Recent trends in manufacturing and materials towards industry 4.0. Lecture Notes in Mechanical Engineering. Springer, Singapore 12. Ong HC, Mahlia TMI, Masjuki HH, Norhasyima RS (2011) Comparison of palm oil, Jatropha curcas and Calophyllum inophyllum for biodiesel: a review. Renew Sustain Energy Rev 15:3501–3515 13. Panday A, Goindi GS, Singh N (2022) Material todays: proceedings. Evaluation of effect of oil viscosity in MQL turning of aluminum 6061. 48:1740–1747 14. Prasannakumar P, Edla S, Thampi AD, Arif M, Santhakumari R (2022) A comparative study on the lubricant properties of chemically modified Calophyllum inophyllum oils for bio-lubricant applications. J Clean Prod 339:130733 15. Rahim EA, Amiril SAS, Talib N (2018) Tribological interaction of bio-based metalworking fluids in machining process. In: Lubrication tribology, lubricants and additives. Intech Open Limited 16. Rama R, Chebattina K (2019) Tribological characteristics of Calophyllum ester based bio-lubricant—commercial engine oil blends. In: IOP Conference Series Material Science Engineering. IOP Publishing Ltd 17. Shahabuddin M, Masjuki HH, Kalam MA, Bhuiya MMK, Mehat H (2013) Comparative tribological investigation of bio-lubricant formulated from a non-edible oil source (Jatropha oil). J Ind Crops 47:323–330 18. Su Y, Gong L, Li B, Liu Z, Chen D (2016) Performance evaluation of nanofluid MQL with vegetable-based oil and ester oil as base fluids in turning. Int J Adv Manuf Technol 83:1083– 2089

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19. Szczotkarz N, Mrugalski R, Maruda RW, Królczyk GM, Legutko S, Leksycki K, D˛ebowski D, Pruncu CI (2021) Cutting tool wear in turning 316L stainless steel in the conditions of minimized lubrication. J Tribol Int 156:106813 20. Talib N, Sasahara H, Rahim EA (2017) Evaluation of modified jatropha-based oil with hexagonal boron nitride particle as a bio-lubricant in the orthogonal cutting process. Int J Adv Manuf Technol 92:371–391 21. Talib N, Sukor NFAM, Sabri AM, Abdullah H, Amiril SAS (2023) Experimental study on physical properties of modified jatropha oil-based nanofluids for machining purposes. Mater Today Proc 5:39–45

Prediction of Real Contact Area on Curvature Region in Hot Stamping Process of AA7075 Aluminium Sheet Muhammad Amir Iqbal Jefry , Mohamad Farid Mohamad Sharif , Wahaizad Safiei , and Suraya Sulaiman

Abstract Hot stamping process of AA7075 aluminium sheet is one of the forming methods used to produce high-strength structural components for automobiles despite their poor room-temperature formability. In this method, the hot aluminium sheet (also known as blank) must be cooled rapidly to prevent the formation of coarse precipitate, which could compromise the strength of the component. The real contact area between two solid surfaces is crucial as it determines the amount of heat transfer from the hot aluminium blank and the cold steel die, thereby affecting the cooling rate of the component formed. This study will use finite element analysis to predict the real contact area between multiple asperities on a flat AA7075 blank surface and a curved, asperity-free steel die surface under different displacements and localized loads. The resulting real contact area could be correlated as a function of displacement and localized load, for used in ANSYS simulation. Keywords Hot stamping · Real contact area · Aluminium sheet

1 Introduction Aluminium alloys, especially those in the AA7xxx series, are widely used in industry due to their advantageous characteristics, such as lightweight, durability, and resistance to corrosion. However, AA7075 alloys have poor formability at room temperature [1]. One attractive technique is to form them by utilizing hot stamping followed by artificial ageing to increase the part’s strength. Hot stamping, also known as hot forming or press hardening, is the process of forming blank while it is hot and then rapidly quenching it in the die [2]. In this process, the cooling rate is crucial since it determines the strength of material [3]. The cooling rate is highly dependent on the real contact area, which is where the hot blank and the cold die make contact during the stamping process. The real contact M. A. I. Jefry · M. F. Mohamad Sharif (B) · W. Safiei · S. Sulaiman Faculty of Manufacturing and Mechatronics Engineering Technology, Universiti Malaysia Pahang Al-Sultan Abdullah, 26600 Pekan, Pahang, Malaysia e-mail: [email protected] © The Author(s), under exclusive license to Springer Nature Singapore Pte Ltd. 2024 R. Abd. Aziz et al. (eds.), Intelligent Manufacturing and Mechatronics, Springer Proceedings in Materials 40, https://doi.org/10.1007/978-981-99-9848-7_19

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area governs the amount of heat transferred from the hot blank to the cold die, thereby affecting the final properties of the component. Nevertheless, only a fraction of the die’s and the blank’s surface areas will make contact. Real contact area (on a microscopic scale) between two surfaces is typically much lesser than nominal contact area (on a macroscopic scale) due to the existence of asperities [4]. There are a few reports about the prediction of the real contact area resulting from the flattening of surface asperity. Wilson and Sheu [5] suggested a 2D model to compute the real contact area in wedge-shaped asperities flattening under normal load and bulk strain using an upper bound technique. Similarly, the slip-line field was proposed by Sutcliffe [6] for the theoretical estimation of the real contact area in asperity flattening resulting from bulk deformation. He found that asperity deformation is influenced by high pressure between contacting asperities and bulk material deformation. Makinouchi et al. [7] simulated asperity flattening using a finite element model consisting of three triangular asperities with free sides, in which strain hardening analysis was considered. They were successful in matching the experimental and simulated real contact area as a function of height reduction during compression. This model was expanded by Ike and Makinouchi [8] to incorporate five asperities as well as a single asperity with periodic boundary conditions. They extended the original model, which only had free sides, by adding longitudinal stresses; therefore, they were able to examine varied degrees of subsurface deformation. Since the turn of the millennium, the use of numerical simulations has steadily increased due to advancements in numerical algorithms during the preceding several decades. Zhang et al. [9] performed a simulation of sinusoidal asperity flattening by numerically simulating local tool-workpiece contact to establish a local friction model that was based on specific tool and workpiece roughness. They then applied the model to perform a simulation of square cup deep drawing. Due to the variance in real contact area, they discovered that the local contact pressure is significantly greater than the mean contact pressure. A multiscale friction model was developed by Hol et al. [10], which takes into consideration the micromechanical friction mechanisms that occur during deep drawing process. The surface asperities are modeled by bars and statistical parameters. In addition to the asperity flattening under normal and tangential loads, the local material flow that occurs near rough tool surfaces was also considered. Nielsen et al. [11] employed triangular asperity flattening experiments and numerical simulations to determine the real contact area ratio for strain-hardening materials as a function of normal pressure and longitudinal bulk strain. Recently, Wu [12] developed a multiscale soft-contact model to investigate the behavior of rough surfaces in contact with coupled slipping and sliding as well as rolling. They discovered that the average asperity spacing is a significant factor that plays a role in the rise of the real contact area when the bulk plastic strain commenced. In contrast to the cold forming processes described above, hot stamping is a transient process in which the hot blank cools and the cold die heats during the stamping process. This phenomenon complicates the process of determining the accurate real contact area, as the material gets softer and more readily flattened at elevated temperature. The aim of this study is to develop a contact model between a flat AA7075 blank surface (with multiple asperities) and a curved, asperity-free

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stainless steel die surface at room temperature, using finite element. Then, the real contact area between the surfaces at different deformation and localized load are predicted. Finally, the correlation of the real contact area as a function of deformation and localized load are established.

2 U-Shaped Hot Stamping Tool and AA7075 Blank Surface Profile Figure 1 illustrates a U-shaped hot stamping tool comprises of stainless-steel punch and die. The AA7075 aluminium blank is stamped between the moving punch and the static die to produce a final U-shaped part when the tool is completely closed. In this study, only the 45-degree curvature part (in the red circle) will be modelled instead of the whole part. This is because there are too many asperities per unit length on the blank surface, making it difficult to model the entire part (consume so much time and costly). According to [13], there are approximately 15 asperity peaks per 1 mm of horizontal distance on the initial AA7075 aluminium blank surface, based on its profile (Fig. 2). It is to be noted that there is a significant disparity between the horizontal and vertical scales, thus the peaks and valleys appear to have steep slopes. Figure 3 depicts how the surface may be modelled based on the profile. On average, there are three parallel cylindrical segment asperities for each horizontal distance of 0.2 mm. The asperities are modelled as cylindrical rather than spherical shapes attributed to the effect of rolling process. For simplicity, it is assumed that all asperities have the same radius and height, 0.067 mm and 0.00067 mm, respectively. This asperity height is according to average root-mean-square roughness (Rq) value of initial AA7075 aluminium blank surface profile [13]. The segment width of each

Fig. 1 U-shaped hot stamping tool

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Fig. 2 Initial AA7075 aluminium blank surface profile [13]

Fig. 3 Multi-cylindrical segment asperities with uniform asperity height and radius [13]

asperity is 0.019 mm while the spacing between adjacent asperities is 0.067 mm. This spacing is too wide that there is the interaction between asperities could be disregarded. This model will be applied on blank upper surface.

3 Finite Element Model A commercial program ANSYS is used to predict real contact area at 45-degree curvature part. The 3D model is shown in Fig. 4, in which AA7075 blank is stamped between stainless steel moving punch and static die. The dimensions of the blank are 0.6 mm in length and 0.2 mm in height. The initial vertical gap between punch and blank is 0.0283 mm. Based on the model in Fig. 3, nine asperities are integrated on the blank upper surface. The asperities are consecutively labelled 1 to 9 from right to left. This simulation is performed in plane strain, and the von Mises yielding criterion is utilized to observe the deformation. The boundary conditions are applied to the model in such the displacement is set at the top surface of the punch and fixed support is set at the bottom surface of the die. The contacts of punch-blank and blank-die are assumed to be frictional with friction coefficient of 0.1. The finite element mesh consists of 42,543 four-node triangle elements comprising a total of 65,411 nodes. The real contact area can be calculated by first determining the nodal force of each asperity node. If the node has a load value, it is categorized as being in contact. Then, for each asperity, two coordinates of the nodes with minimum load ((x 1 , y1 ) and (x 2 , y2 )) are determined, and the distance for each asperity could be calculated as follows:

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Fig. 4 AA7075 blank is stamped between punch and die

Distance =

/

(x2 − x1 )2 + (y2 − y1 )2

(1)

4 Results and Discussions Table 1 presents the simulation outcome for five displacements. The colour contour in each sub-figure represents the stress experienced by the corresponding blank, punch and die, which varies with increasing displacement. Overall, the number of contact asperities increases as displacement increases. At the initial displacement (dz = 0.010 mm), there is no significant change in stress even though the punch has already contacted the first asperity, i.e., asperity #5. This stage mostly involves advancing the blank toward the die. As the edges of the blank lower surface approach the die (dz = 0.015 mm), the stress increases. Simultaneously, the middle of blank lower and upper surfaces start to stretch and compress, respectively. At this stage, two additional middle asperities deform, i.e., asperities #4 and #6. Further displacement leads to deformation of two more asperities, i.e., asperities #3 and #7. It is evident that the middle asperities (asperities #4 and #5) have been subjected to an excessive amount of stress, which may imply that they have

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Table 1 Simulation results for different displacement Stress distribution (MPa)

Displacement = 0.010 mm

Displacement = 0.023 mm

Displacement = 0.015 mm

Displacement = 0.026 mm

Displacement = 0.020 mm

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been completely flattened. According to the individual contact area data (not shown here), the contact areas of asperities #4 and #5 have reached their maximum contact area (based on the segment width of asperity). As soon as the displacement reaches 0.023 mm, the lower surface of the blank is completely attached to the die. There are currently seven asperities in contact with the punch (all asperities except #1 and #9). Finally, at dz = 0.026 mm, all nine asperities contact the punch. Based on the individual contact area data, four asperities are completely flattened, as indicated by the stress intensity. In general, displacement is proportional to stress and the quantity of asperities in contact. These outcomes demonstrate the importance of considering displacement level when analyzing the behavior of rough surfaces under various conditions. Figure 5 illustrates the relationship between the real contact area and the displacement. The real contact area is the sum of the individual contact areas between the asperities and the punch. The real contact area initially increases as more asperities come into contact. At dz = 0.002 mm, it is obvious that the rate of real contact area growth accelerates. This is the result of complete flattening of asperities #4, #5, and #6. Subsequently, asperities #2 through #8 have fully flattened at dz = 0.0026 mm, accounting for 25% of the nominal area. Note that the maximum proportion of real contact area that can be attributable to all nine asperities is 28.5%. Real contact area versus localized load is depicted in Fig. 6. Localized load does not refer to the overall punch load, but only to the localized portion of the load. The localized load could be determined by adding the loads carried by asperities. Initially, only asperity #5 contacts the punch, and its load value is relatively low. After providing additional load many asperities come into contact. As load exceeds F = 2.8 N, the real contact area begins to increase at a slower rate. This is due to the limitation of total real contact area, which is 28.5% as stated earlier.

Fig. 5 Percentage real contact area as a function of displacement

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Fig. 6 Percentage real contact area as a function of localized load

5 Conclusions The real contact area at the the hot aluminium blank/cold steel die interface governs the local cooling rate during hot stamping process of AA7075 aluminium sheet and determines the strength of high-strength structural components. The finite element method (ANSYS) has been used to analyze the characteristics of asperity deformation and to predict the real contact area between the hot aluminum blank and the cold steel die, particularly at the curvature region. It is found that as displacement rises, the asperities deform and completely flatten one by one, thus the real contact area increases. At the same time, localized load also increases as more asperities contact the punch. Further study is required to determine whether the real contact area resulting from the complete flattening merges with the non-asperity contact area (which is located between asperities). Finally, the correlation of the real contact area as a function of deformation and localized load has been established and could be utilized in ANSYS simulations.

References 1. Harrison N, Luckey S (2014) Hot stamping of a B-Pillar outer from high strength aluminum sheet AA7075. SAE Int J Mater Manf 7(3):567–573. https://doi.org/10.4271/2014-01-0981 2. Karbasian H, Tekkaya AE (2010) A review on hot stamping. J Mater Process Technol 210(15):2103–2118. https://doi.org/10.1016/j.jmatprotec.2010.07.019 3. Merklein M, Lechler J (2006) Investigation of the thermo-mechanical properties of hot stamping steels. J Mater Process Technol 177(1–3):452–455. https://doi.org/10.1016/j.jmatprotec.2006. 03.233 4. Tabor D (1951) The hardness of metals. Oxford University Press, Oxford

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5. Wilson WRD, Sheu S (1988) Real area of contact and boundary friction in metal forming. Int J Mech Sci 30(7):475–489. https://doi.org/10.1016/0020-7403(88)90002-1 6. Sutcliffe MPF (1988) Surface asperity deformation in metal forming processes. Int J Mech Sci 30(11):847–868. https://doi.org/10.1016/0020-7403(88)90010-0 7. Makinouchi A, Ike H, Murakawa M, Koga N (1988) A finite element analysis of flattening of surface asperities by perfectly lubricated rigid dies in metal working processes. Wear 128(2):109–122. https://doi.org/10.1016/0043-1648(88)90178-0 8. Ike H, Makinouchi A (1990) Effect of lateral tension and compression on plane strain flattening processes of surface asperities lying over a plastically deformable bulk. Wear 140(1):17–38. https://doi.org/10.1016/0043-1648(90)90119-U 9. Zhang S, Hodgson PD, Cardew-Hall MJ, Kalyanasundaram S (2003) A finite element simulation of micro-mechanical frictional behavior in metal forming. J Mater Process Technol 134(1):81–91. https://doi.org/10.1016/S0924-0136(02)00926-3 10. Hol J, Meinders VT, de Rooij MB, van den Boogaard AH (2015) Multi-scale friction modeling for sheet metal forming: the boundary lubrication regime. Tribol Int 81:112–128. https://doi. org/10.1016/j.triboint.2014.07.015 11. Nielsen CV, Martins PAF, Bay N (2016) Modelling of real area of contact between tool and workpiece in metal forming processes including the influence of subsurface deformation. CIRP Ann Manufact Technol 65(1):261–264. https://doi.org/10.1016/j.cirp.2016.04.126 12. Wu C, Zhang L, Qu P, Li S, Jiang Z, Wu Z (2022) A multiscale soft-contact modelling method for rough surfaces in contact with coupled slipping/sliding and rolling. Tribol Int 173:107627. https://doi.org/10.1016/j.triboint.2022.107627 13. Mohamad Sharif, MFB (2022) Thermal contact resistance modeling in AA7075 Hot Stamping. Doctoral dissertation

Formulation of Grease for Industrial Applications Mohd Najib Razali , Nasreldeen Ishag Obi, A. R. Muhammad Haziq, A. Azharul Aiman, M. S. Muhammad Arif Zakaria, and Najmuddin Mohd Ramli

Abstract The objective of this study is to formulate a multipurpose grease that is reliable, low cost, high performance, and eco-friendly using different base oil, thickener, and additives. The properties of the different grease formulations, such as dropping point, consistency, cone penetration, oil separation, and oil bleeding, were evaluated using standard methods. The grease chemical compounds were determined using the FTIR test. The findings of the study show that using lithium hydroxide in the formulation significantly increases the dropping point of grease, and additives used in this study have improved the performance of the grease. However, further study is needed to understand the optimum amount of each additive. Keywords Grease · Additives · Thickener · Dropping point

1 Introduction Grease is a semisolid substance made up of a base fluid, a thickener, and an additive. There are numerous varieties of grease available nowadays [1]. The rapid growth of industries has resulted in increased lubrication demand as well as an increase in the amount of waste oil created. Waste oil is classified as schedule waste because of its potential to endanger public health and the environment [2]. Grease’s function is to stay in contact with and lubricate moving surfaces without leaking out due to gravity, centrifugal force, or being squeezed out under pressure. Its most important practical requirement is that it retains its properties under shear forces at all temperatures encountered during use [3]. M. N. Razali (B) · N. I. Obi · A. R. M. Haziq · A. A. Aiman · M. S. M. A. Zakaria · N. Mohd Ramli Faculty of Chemical and Process Engineering Technology, Universiti Malaysia Pahang Al-Sultan Abdullah, 26300 Kuantan, Pahang, Malaysia e-mail: [email protected] N. Mohd Ramli MNR Multitech Sdn Bhd, Kompleks UMP Holdings, K02, Ground Floor, 26300 Gambang, Pahang, Malaysia © The Author(s), under exclusive license to Springer Nature Singapore Pte Ltd. 2024 R. Abd. Aziz et al. (eds.), Intelligent Manufacturing and Mechatronics, Springer Proceedings in Materials 40, https://doi.org/10.1007/978-981-99-9848-7_20

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Due to their outstanding heat tolerance (similar to sodium greases) and water resistance (similar to calcium greases), lithium greases are by far the most common grease on the market. Because of their greater dropping points and improved heat resistance, Lithium Complex Greases are preferred over conventional Lithium greases [4]. Grease is made up of over 90% base oil, which is mostly obtained from petroleum oil. However, due to limited petroleum reserves, the amount of petroleum oil is steadily reducing. Researchers have been looking into other raw materials that could be used to replace petroleum oil, such as vegetable oil, used cooking oil, used engine oil, ionic liquid, and more. Several studies have optimized the use of waste oil as a base oil to reduce dependency on crude oil and reduce the cost of production [5]. However, those attempts were not significant enough to reduce production costs or to enhance the quality of grease. In addition to that, the impact of additives and thickness in improving the performance of grease is not sufficiently investigated. Additives in lubricating grease can perform a variety of roles. This primarily entails enhancing favorable traits, reducing unfavourable properties, and imparting new properties. The objective of this study is to formulate a multipurpose grease that is reliable, low cost, high performance, and eco-friendly using different base oil, thickener, and additives. Then the performance of the formulated greases was analysed using dropping point testing, consistency testing, cone penetration test, oil separation test, oil bleeding test, and FTIR.

2 Methodology 2.1 Grease Producing Method (Base Oil Variation) See Table 1. Table 1 Formulations of grease for base oil variation Parameters

Name

Grease Grease A

Grease B

Grease C

%

g

%

g

%

g

Base oil

Lubricant A

83.61

166.22

–

–

–

–

Base oil

Lubricant B

–

–

81.22

162.43

–

–

Base oil

Lubricant C

–

–

–

–

82

164

Thickeners

12 HAS

14.91

30.82

17.30

34.61

16.52

33.04

Thickeners

Li-OH

1.48

2.96

1.48

2.96

1.48

2.96

Ratio

83.61:16.39

81.22:18.78

82:18

Formulation of Grease for Industrial Applications

2.1.1

223

Grease A, B and C Production

Greases A, B, and C were each prepared through a direct saponification process. Initially, raw materials, including lubricant oils A, B, and C, 12-HSA, and lithium, were readied and weighed into separate beakers for each grease. After melting 12HSA at 110 °C, 70% of the respective lubricant oils (A, B, and C) were introduced into separate beaker containing the molten 12-HSA. The mixtures were heated to 115 °C and stirred at 90rpm. Subsequently, Lithium hydroxide was dissolved in a specific quantity of distilled water at 60 °C, and the resulting solution was carefully added drop by drop to the mixed solutions. Stirring at 200 rpm ensued, and the temperature was raised to 165 °C to vaporize the distilled water from the greases through the saponification process. Upon complete removal of the water content, the remaining 30% of the respective lubricant oils (A, B and C) were integrated into the separate beaker for each of grease A, B and C. Lastly, stirring continued for approximately 20 to 30 min until achieving thorough homogenization in each case.

2.2 Grease Production Method (Thickener Variation) See Table 2.

2.2.1

Calcium Grease Production

To improve the effectiveness of the saponification reaction, a particular amount of water must be included with the raw materials for making a grease, such as calcium Table 2 Formulations of grease for thickener variation Name

Type raw materials

Formulation 1 calcium grease

Formulation 2 mixed grease

Formulation 3 alumnium grease

%

g

%

g

%

g

Lubricant A

Base oil

75

150

84.79

169.57

75

150

Calcium hydroxide

Thickener

6.69

13.38

1.15

2.3

–

–

Lithium hydroxide

Thickener

–

–

1.15

2.3

–

–

12-Hydroxystearic acid

Thickener

18.31

36.62

12.91

25.83

–

–

Alumnium isopropoxide

Thickener

–

–

–

–

8.35

16.7

Stearic acid

Thickener

–

–

–

–

11.19

22.38

Benzoic acid

Thickener

–

–

–

–

5.46

1092

Ratio Base oil: thickener

75:25

84.79:15.25

75:25

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grease. For the first steps, prepare and weigh each raw material, such as base oil, calcium hydroxide, and 12-HSA. At 110 °C, 12-HSA was heated till it melted for around 20 min. Next, 70% of the base oil was preheated at 110 °C. After 20 min, mix base oil and 12-HSA at 115 °C and stir it at 90 rpm. Meanwhile, calcium hydroxide was dissolved in distilled water at 60 °C. After fully dissolved, the calcium hydroxide solution was poured drop by drop into the mixed solution. Stirred the grease at 200 rpm, and the temperature was raised to 165 °C to evaporate the distilled water from the grease (3 to 4 h taken). Next, after the water was completely evaporated, the remaining 30% of the base oil was added, stirred around 20 min until it was completely mixed.

2.2.2

Mixed Grease Production

In the mixed grease of one aspect of the present invention, the content ratio of the grease (A) to the grease (B) is changed from the viewpoint of improving the load resistance. Firstly, prepare and weigh each raw material, such as base oil, calcium hydroxide, lithium hydroxide, and 12-HSA. At 110 °C, 12-HSA was heated till it melted for around 20 min. Furthermore, 70% of base oil was preheated at 110 °C. After 20 min, mix base oil and 12-HSA at 115 °C and stir it at 90 rpm. Meanwhile, calcium hydroxide and lithium hydroxide were dissolved in distilled water at 60 °C. After fully dissolved, each solution was poured drop by drop into the mixed solution. Stirred the grease at 200 rpm, and the temperature was raised to 165 °C to evaporate the distilled water from the grease (3 to 4 h taken). Next, after the water was completely evaporated, the remaining 30% of the base oil was added, stirred around 20 min until it was completely mixed.

2.2.3

Aluminum Grease Production

This procedure relates to a thickener component based on aluminum isopropoxide, stearic acid, and benzoic acid compound and the aluminum grease made therefrom with the addition of base oil. Stearic acid was heated at 90 °C till it melted for around 20 min. Then, at 100 °C, 28% of the base oil was heated (20–30 min). Mixed 28% base oil and stearic acid at 115 °C and stirred it at 100 rpm. Meanwhile, aluminum isopropoxide and 21% of base oil was mixed and stirred at 70 °C (20 min). The same goes with benzoic acid, and 21% of base oil was mixed and stirred at 70 °C (20 min). After that, mix all the solution and stir the grease at 200 rpm. The temperature was maintained at 100 °C (3 to 4 h taken). Distilled water was added drop by drop. Stir it until there is no water in it. The remaining 30% of base oil was added. Last, the grease was stirred for around 20 min until it was completely mixed.

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2.3 Grease Testing Methods

Test method

Procedure

Parameters/ results

1. Cone penetration testing

Approximately 400g of room temperature grease is placed in a cup. A cone is dropped into the cup for 5 s using a penetrometer. Penetration depth (P0) is recorded. The grease undergoes shearing with 60 strokes (P60), followed by retesting. The NLGI grade is determined using the NLGI grade chart [6]

P0 penetration depth, P60 penetration depth, NLGI grade

2. Dropping point test A thin grease film is smoothed into a small cup, placed into a test tube with a thermometer. The test tube is placed into a dropping point test rig. Temperature is increased gradually. When a droplet forms below the cup, it drops, indicating the grease’s thickener limit. Droplet formation temperatures are recorded to calculate the dropping point [7]

Dropping point temperature, block temperature, test tube temperature

3. Fourier Transform Infrared Spectroscopy (FTIR) analysis

The FTIR spectrometer is cleaned with ethanol. A grease Identified sample is placed on it, exposed to IR beams. The grease molecular absorbs the beams, emitting frequencies read by the identities FTIR. Molecular identities of the sample are identified [6]

4. Oil bleeding test

A hot plate is preheated to 60 °C. Fresh grease is placed on filter paper, excess wiped off, and the mask removed. The filter paper with grease is left on the hot plate for 2 h. Oil stain diameter is measured, and bleeding area is calculated using formulas. The same process is repeated with worked grease [8]

5. Oil separation test

An industrial oven is preheated to 100 °C. Empty beaker Oil and stainless-steel mesh are weighed. Grease sample separation (10g) is placed in the mesh, which is then assembled into percentage a conical sieve apparatus and placed in the oven for 30 h. After cooling, oil in the beaker is weighed to calculate oil separation percentage [8]

6. Consistency test (NLGI)

Grease is placed on a glass plate using a mask. Excess grease is removed, and the housing is placed on a calibrated scale. The glass plate with grease is inserted, pressed with weight for 15 s. NLGI grade is determined based on grease position on the scale [N/A]

Fresh grease bleeding area, worked grease bleeding area, percentage difference

NLGI grade

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3 Result and Disscussion 3.1 Base Oil Variant Results See Tables 3 and 4. The physical analysis has been tested for all types of grease produced from three different types of base oil. All type of grease has a semi solid state and differ in appearance which is light yellowish for SS Lube and Rachi lithium grease, while for greenlube lithium grease is dark yellowish. This is because the colour of the lubricant oil for greenlube is a little bit dark compared to the others [5]. The stiffness or consistency of grease is its most important feature. A grease that is too hard may not feed into lubricating zones, whereas a grease that is too fluid may leak out. The viscosity of the base oil and the type and amount of thickener added to determine the consistency of the grease. A grease’s consistency is its resistance to deformation by an applied force. The measure of consistency is called penetration. All the grease was prepared to an NLGI grade 2, which is multipurpose grease, and the amount of thickener was varied to obtain the same grease consistency, but only Greenlube lithium grease had a Table 3 Characterization of base oil Base oil

Lub B

Lub C

Lub D

Kinematic viscosity @, 100 °C (mm2 / 12.5 s)

Lub A

13.7

11.3

19

Falsh point (°C)

220

245

215

234

Boiling point (°C)

269

291

263

280

Density (Kg/m3 )

0.872

0.879

0.889

0.856

Appearance (colour)

Golden brown Amber (dark) Yellowish

Type

Mineral oil

Mineral oil

Mineral oil Mineral oil

Grade

SAE 40

20W 40

15W 40

Dark 20W 50

Table 4 Physical analysis for base oil variant No

Test

Test method

Grease formulation

1

Appearance

–

Lub A

Lub B

Lub C

2

Physical state

–

Semi solid

Semi solid

Semi solid

3

Consistency test (NLGI)

In house

2

3

2

4

Penetration worked, 60× (10−1 mm)

ASTM D-1403

292.4

239.8

287.3

5

Oil separation test (%)

In House

11

1

18

6

Oil bleeeding test (% Diff) In House

–8.26

11.49

–5.80

7

Dropping point (°C)

197

205

194.33

ASTM D2265-00

Formulation of Grease for Industrial Applications

227

different NLGI grade which is 3. This is because the amount of thickener to produce Greenlube lithium grease is slightly higher compared to another grease. In this way, the properties of the grease can be compared on the same NLGI grade basis. For the penetration test, all types of grease got the same NLGI grade same with the SKF consistency test [9]. The oil separation test is used to determine if the oil has the potential to separate from the lubricating grease. It monitors the separation of oil and grease at high temperatures for a set length of time. Oil’s ability to split during storage might be a significant characteristic. When the base oil separates from the other raw components in the grease, the remaining substance may alter the consistency, affecting the grease’s ability to perform as intended. As a result, Greenlube lithium grease had the lowest percentage value, which is 1, compared to the others have 11% and 18% for SS Lube and Rachi lithium grease. This shows that Greenlube lithium grease is the best grease for all three types because the percentage of oil separation was the lowest, almost 0. Bleeding is a condition when the liquid lubricant separates from the thickener. It is induced by high temperatures for a defined period of time and also occurs during long storage periods. As the oil separates from the grease, the thickener concentration increases, and plugging gets worse. As a result, percentage differences for SS lube, Greenlube, and Rachi is −8.28, 11.49, and −5.80. This shows that bleeding for SS Lube and Rachi lithium grease is reduced, meaning that the used grease is bleeding 8.28% and 5.80% less than fresh unused grease for SS Lube and Rachi lithium grease, while used grease for greenlube lithium grease bleeding 11.49% more than fresh grease [10]. The dropping point of grease is a measure of its heat resistance. As the temperature of the grease rises, so does its penetration until the grease liquefies and the desired consistency is lost. The temperature at which grease becomes fluid enough to drip is known as the dropping point. The dropping point is the highest usable temperature at which grease can maintain its structure and can apply [11]. Table 4 shows that greenlube lithium grease has the highest dropping point among the others, which is 205 °C, while SS Lube and Rachi lithium grease each 197 °C and 194.33 °C, respectively. This is because greenlube oil has the highest flash point making it has a higher dropping point.

3.2 Additive Variant Results Lithium complex greases have greater temperature stability when compared to ordinary lithium soap grease. Three additives, namely azelaic acid, boric acid, and sebacic acid, are studied. The additives selected are presumed to have an effect on the lithium complex grease in such a way that it increases the dropping point. As important as formulating the grease, the physical analysis is done on all the grease to obtain the physical characteristics of the grease. For the azelaic acid grease, it has an appearance of a brownish colour; meanwhile, for the boric grease and sebacic grease, they are light brownish and light yellowish, respectively. They all have an almost similar

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coloration due to the Li-OH being added into the grease as the thickener. Furthermore, because it is lithium complex grease, all the grease has a quite high dropping point. But out of all the greases, the azelaic acid grease has the highest dropping point at 255.67 °C. The boric acid grease and sebacic acid grease both did not pass the 200° C point but still had a high dropping point when compared to other greases that have no additives added to the grease. It is well known that additives such as azelaic acid increases the dropping point of the grease. That being said, boric acid and sebacic acid also increase the dropping point of the grease but not as well as using azelaic acid. Often sebacic acid is used in replacement for azelaic acid due to its availability and its lower price (Fig. 1 and Tables 5 and 6). As for the consistency of the grease, all of the greases achieved an NLGI grade of 2. This is perfect, whereas the range for multipurpose grease falls in this category. To be more specific, it falls within the range of NLGI grade 1 to 3. This is determined by performing the cone penetration test, and they had values of 292.1, 273.8, and

Fig. 1 FTIR analysis comparison (additive)

Table 5 Characterization of additives Parameters

Additives azelaic acid

Boric acid

Sebacic acid

Formula

C9H16O4

H3BO3

C10H18O4

Molar mass (g/mol)

188.22

61.83

202.25

Appearance

White powder

White crystalline

White powder

Melting point (°C)

111

160

137

Boiling point (°C)

286

300

294.5

Type

Soap

Soap

Soap

Water solubility

2.4 g/l at 20 °C

49.2 g/l at 20 °C

0.224 g/l at 20 °C

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Table 6 Physical analysis for additive variant No

Test

Test method

Grease formulation Azelaic grease

Boric grease

Sebacic grease

1

Appearance

–

Brownish

Light Brownish

Light Yellowish

2

Physical state

–

Semi-solid

Semi-solid

Semi-solid

3

Consistency test (NLGI)

In House

2

2

2

4

Penetration worked, 60× (10−1 mm)

ASTMD-1403

292.1

273.8

268.4

5

Oil separation test (%)

In House

1.2

1.6

17.3

6

Oil bleeeding test (% Diff)

In House

2.73

−5.03

−5.75

7

Dropping point (°C)

ASTM D2265-00

255.67

184.00

134.00

268.4, respectively, for azelaic, boric, and sebacic greases. The grade of the grease was obtained by reading the chart provided according to ASTM D-1403. All of the grease did well in this testing. The azelaic acid was nearest to the grade 1 value as more base oil was used in the formula. In contrast, the sebacic acid is nearest to the grade 3 value as less base oil was used in the formula and therefore is firmer. The oil separation test shows how much oil is separated from the grease after a period of time at a certain temperature. From the test conducted, 2 of the greases, which are azelaic acid grease and boric acid grease, both have a similar result having a percentage of 1.2 and 1.6, respectively. It is most desirable to have the lowest percentage possible as it means the oil stays in the grease as that is the main purpose of creating grease in difference to lubricating oils. But it also depends on where the grease is applied. Some may want this characteristic in their application. For the sebacic acid grease, the oil separation percentage is 17.3%, which is very high, well above the normal percentage, which is 5%. It can be said that the thickener does not hold the oil in the grease well, and this can be due to a lot of factors, but it is suspected that it is due to the incompatibility of the sebacic acid with the other raw materials. For the oil bleeding test, the main focus is to see if the grease bled more or less after the grease is worked in comparison to before the grease is worked. As a result, the azelaic acid grease has the nearest value to zero, which is 2.73%. The positive value here means that the grease bled 2.73% more after the grease was worked compared to before it was worked. On the other hand, both boric and sebacic acid grease have negative values of −5.03 and −5.75, respectively. In opposition to what has been said for the azelaic acid grease, the boric acid and sebacic acid grease bled 5% less after the grease was worked. In this test, the nearer the value to zero, the better. Therefore, the result produced by the azelaic acid grease is the best in this testing.

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4 Conclusion Investigating grease formulation using different types of base oils, thicknesses, and additives is very significant. The study’s findings suggest that utilising lithium hydroxide in the formulation greatly raises the dropping point of grease, and the additives employed in this study increased the grease’s performance. In addition to that, all formulated greases are economically competitive to commercial ones. However, to better compete with existing lubricating greases on the market, the performance of these developed greases must be further optimised with additional additives. Acknowledgements The authors wish to express their gratitude and appreciation for the financial support from the Ministry of Higher Education (MOHE), Malaysia for the Prototype Research Grant Scheme (PRGS KPT—RDU190806, Reference No.: PRGS/1/2019/ TK05/UMP/03/1 entitled Scale-Up Production of Electrical Contact Lubricant (G-Grease) for Middle Voltage Switchgear Application) and Universiti Malaysia Pahang Al-Sultan Abdullah for the Postgraduate Research Scheme (PGRS200354 entitled Formulation of Electrical Contact Lubricant for Middle Switchgear Application). The support from the Faculty of Chemical and Process Engineering Technology, Department of Chemical Engineering, Universiti Malaysia Pahang Al-Sultan Abdullah, Malaysia, and MNR Multitech Sdn Bhd is also acknowledged.

References 1. Cao Z, Xia Y, Ge X (2016) Conductive capacity and tribological properties of several carbon materials in conductive greases. Ind Lubr Tribol 68:577:585 2. Ren G, Li W, Li H, Fan X, Zhang L, Zhu M (2020) Regulating performance characteristics of lithium complex greases via dibasic acids. Lubr Sci 32(6):261–272 3. Nabi MN, Akhter MS, Rahman MA (2013) Waste transformer oil as an alternative fuel for diesel engine. Procedia Eng 56:401–406 4. Gow G (2010) Lubricating grease. In: Chemistry and technology of lubricants. Springer, pp 411–432 5. Japar NSA, Aziz MAA, Razali MN (2019) Formulation of fumed silica grease from waste transformer oil as base oil. Egypt J Pet 28(1):91–96 6. Lijesh KP, Khonsari MM (2019) On the assessment of mechanical degradation of grease using entropy generation rate. Tribol Lett 67(2):1–13 7. Kamel BM, Mohamed A, El-Sherbiny M, Abed KA, Abd-Rabou M (2017) Rheological characteristics of modified calcium grease with graphene nanosheets. Fullerenes Nanotub Carbon Nanostruct 25(7):429–434 8. Maruyama T, Saitoh T, Yokouchi A (2017) Differences in mechanisms for fretting wear reduction between oil and grease lubrication. Tribol Trans 60(3):497–505 9. Westerberg LG, Sarkar C, Lladós JF, Lundström TS, Höglund E (2017) Lubricating grease flow in a double restriction seal geometry: a computational fluid dynamics approach. Tribol Lett 65(3):1–17 10. Suhaila N, Japar A, Aizudin M, Aziz A, Razali MN (2018) Formulation of lubricating grease using Beeswax thickener. IOP Conf Ser Mater Sci Eng 342(1):12007 11. Kamel BM, Mohamed A, El Sherbiny M, Abed KA (2016) Rheology and thermal conductivity of calcium grease containing multi-walled carbon nanotube. Fullerene Nanotub Carbon Nanostruct 24(4):260–265

Materials

Effects of pH on Grain Size and Structure of ZnO Nanoparticle Synthesized via Sol–Gel Method for Enhanced Thermoelectric Materials Suraya Sulaiman , Tuan Muhammad Tuan Zahrin, Nadhrah Md Yatim , Mohd Faizul Mohd Sabri , and Mohamad Farid Mohamad Sharif

Abstract Zinc Oxide (ZnO) emerges as a potential thermoelectric material with high thermoelectric performance suitable for enhancing power harvesting applications efficiently. However, its intrinsic high thermal conductivity poses a challenge to achieving optimal thermoelectric performance. To address this, the nanostructuring approach has been employed, leveraging the creation of nanometer-scale grains to effectively reduce thermal conductivity. This paper investigates the impact of pH on the size of ZnO nanoparticles grains. The sol–gel method was used to synthesize the ZnO nanoparticles with various pH levels (7, 9, and 12). Subsequently, the resulting powder was then calcined at 800 °C for 1 h to produce pure ZnO powder. X-ray diffraction (XRD) analysis revealed a consistent hexagonal wurtzite structure across all pH levels, with the smallest crystallite sizes observed at pH 12 (34.52 nm), followed by pH 9 (34.72 nm), and pH 7 (40.38 nm). At pH 7 and 12, field emission scanning electron microscopy (FESEM) pictures displayed a hexagonal-like structure, whereas pH 9 revealed a nanorod-like structure. The average particle sizes were determined to be 84.56 nm at pH 12, 97.22 nm at pH 9, and 118.70 nm at pH 7, respectively. Energy-dispersive X-ray spectroscopy (EDX) analysis confirmed the high purity of the synthesized ZnO nanoparticles, with atomic percentages of Zn and O closely aligning with the stoichiometric composition. These results validate the substantial purity of the ZnO nanoparticles. Overall, the findings demonstrate that S. Sulaiman (B) · T. M. Tuan Zahrin · M. F. Mohamad Sharif Faculty of Manufacturing and Mechatronic Engineering Technology, Universiti Malaysia Pahang Al-Sultan Abdullah, 26600 Pekan, Pahang, Malaysia e-mail: [email protected] S. Sulaiman Faculty of Engineering, School of Mechanical Engineering, University Teknologi Malaysia, 81310 Johor, Malaysia N. Md Yatim Faculty Science and Technology, Universiti Sains Islam Malaysia, 71800 Nilai, Negeri Sembilan, Malaysia M. F. Mohd Sabri Faculty of Engineering, Department of Mechanical Engineering, Universiti Malaya, 50603 Kuala Lumpur, Malaysia © The Author(s), under exclusive license to Springer Nature Singapore Pte Ltd. 2024 R. Abd. Aziz et al. (eds.), Intelligent Manufacturing and Mechatronics, Springer Proceedings in Materials 40, https://doi.org/10.1007/978-981-99-9848-7_21

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increasing the pH values during synthesis leads to a reduction in both crystallite and particle sizes. This decrease in size is associated with lower thermal conductivity, thus offering the potential for improved thermoelectric performance. Keywords ZnO nanoparticles · Grain size control · Sol–gel synthesis · pH optimization · Crystallite size · Nanostructuring

1 Introduction Nowadays, the world is currently facing a worldwide energy catastrophe and environmental issues due to the increasing demand for limited natural resources, reliance on fossil fuels, and the carbon footprint generated by industrial processes [1, 2]. The inefficient utilization of waste heat further exacerbates these issues, as a significant amount of heat energy is lost without being converted into useful electricity [3–6]. Thermoelectric waste heat recovery systems offer a promising solution to this problem by generating electricity from waste heat [1, 3]. The effectiveness of these systems today, however, is still relatively low, typically ranging from 7 to 10% [1, 3, 7, 8]. Extensive research has been conducted on conventional thermoelectric materials for waste heat recovery systems. However, these materials suffer from drawbacks such as poor stability in high-temperature air, high toxicity, high cost, and limited availability of rare elements, making them less attractive and compatible for widespread application [9, 10]. Oxide materials, particularly ZnO, have been investigated as alternatives due to their stability and lower toxicity. However, the achieved figure of merit (ZT) values have not yet reached the target value of 1 [1, 3, 10], and limited studies have explored the effect of pH on ZnO nanoparticles [11]. The research aims to synthesize and characterize the ZnO nanoparticles at pH 7, 9 and 12, respectively. The influence of pH levels, nanoparticle size and morphology, and the purity of the synthesized ZnO powder are investigated.

2 Thermoelectric Performance and Characteristics The ZT values is used to quantify the performance and efficiency of thermoelectric materials in thermoelectric applications. A higher ZT value signifies a more efficient conversion of thermal energy into electricity. Theoretically, a ZT value equal to or greater than 1 is required to achieve a conversion efficiency of over 10% [1, 12]. In order to have superior thermoelectric performance, it is desirable to possess greater power factor (electrical conductivity and Seebeck coefficient), and lower thermal conductivity [1, 3, 13, 14]. Among various thermoelectric materials, n-type ZnObased has received significant attention due to its exceptional potential for producing a high-temperature thermoelectric generators. Numerous efforts have been dedicated

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to enhancing the thermoelectric generators capabilities of ZnO-based thermoelectric materials, including the incorporation of doping and co-doping with other elements. However, most literature reports indicate that the ZT for ZnO-based materials remains below 0.52 at 1100 K [3, 15] and 0.44 at 1000 K [3, 9]. As a result, alternative strategies such as nanostructuring and doping need to be explored to increase the ZT values and improve the thermoelectric performances of these materials [1, 3, 15]. Nanostructuring involves manipulating the structure of materials at the nanoscale, which leads to reduced grain sizes [16] and enhanced phonon scattering [3, 17, 18]. This, in turn, lowers the thermal conductivity and improves the overall thermoelectric performance of ZnO-based materials [1, 3]. Doping, on the other hand, entails introducing foreign elements into the ZnO lattice to modify its electrical and thermal transport properties [3]. Doping can increase the electrical conductivity by introducing additional charge carriers or optimize the Seebeck coefficient by modifying the electronic band structure [3, 10, 19]. The synergistic combination of nanostructuring and doping holds great promise for improving the ZT values of ZnO-based materials, ultimately contributing to more efficient thermoelectric waste heat recovery systems [1, 3, 15].

3 Strategies for Enhancing the ZT Values of Thermoelectric Materials In recent years, sustainable solution for energy harvesting has attracted a lot of interest in the ability of thermoelectric materials to convert waste heat into useful electrical energy. However, the inherent challenges associated with low thermoelectric efficiency have motivated researchers to explore various strategies for enhancing the ZT values of these materials. Among the most promising approaches are nanostructuring and doping, which have shown considerable potential in improving the ZT values and overall thermoelectric properties.

3.1 Nanostructuring Approach Nanostructuring plays an important role in the creation and growth of ultrafine, pure, and uniform grain sizes, which has significant implications for thermal conductivity and in thermoelectric materials. The thermal conductivity can be effectively decreased by refining particle sizes and enhancing phonon scattering at grain borders [1, 3, 20–22]. The lattice thermal conductivity significantly decrease as the grain size decreases to the nanoscale due to an increase in phonon scattering. This characteristic is highly advantageous for thermoelectric applications, as demonstrated in previous studies [3, 20]. In addition, nanostructuring not only facilitates achieving an energy filtering effect and electron confinement, but also causes the Seebeck coefficient to

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increase. Consequently, nanostructured thermoelectric materials exhibit a superior ZT values compared to conventional counterparts. Moreover, the pH of the synthesis medium can also have an impact on the morphology, encompassing both the shape and size of ZnO materials. The morphology of synthesized ZnO is significantly influenced by the relative ratios of H+ and OH− ions. The polymerization of metal–oxygen linkages variation can significantly impacted by changes in the concentration of H+ or OH− ions, leading in a diverse of ZnO structures [23, 24]. Notably, it has been observed that ZnO structures cannot be effectively produced at pH 6. This occurs because a higher concentration of H+ ions and lower concentration of OH− ions in the solvent [3, 24, 25]. Understanding the pH-dependent morphology control is crucial for tailoring the properties and performance of ZnO-based thermoelectric materials. By combining the nanostructuring approach with pH-dependent morphology control, researchers can explore innovative strategies to enhance the ZT values of materials and also improve thermoelectric performances, paving the way for more efficient energy conversion and utilization in various applications.

3.2 Doping Approach Doping, as a prominent strategy, holds great promise for improving the thermoelectric performance of materials. By introducing controlled amounts of impurities, dopants modify the behavior and physical characteristics of semiconductors, leading to enhanced thermoelectric properties. Among the various dopants, aluminum (Al) has emerged as a widely utilized choice in ZnO due to its compatibility with Zn2+ ions and efficient substitution with Al3+ ions [3, 12]. The addition of Al dopants in ZnO offers several advantages for thermoelectric applications. Firstly, doping with Al increases the carrier density, leading to improved electrical conductivity. This allows for more efficient transport of charge carriers, resulting in enhanced thermoelectric performance [3, 26]. Secondly, the presence of Al dopants refines the grain size of ZnO. Smaller grain sizes are beneficial as they reduce phonon scattering, thereby decreasing the lattice thermal conductivity [27]. Notably, studies have reported a linear relationship between the dopant concentration and key thermoelectric parameters in Al-doped ZnO. For instance, the electrical conductivity and Seebeck coefficient of Al-doped ZnO exhibit a proportional relationship with the dopant concentration [28]. This implies that careful control of the dopant concentration allows researchers to tailor the electrical and thermal transport properties of the material, thereby optimizing its thermoelectric performance. In the recent years, substantial advancement has been made in understanding the doping mechanisms and optimizing the dopant configuration in ZnO-based thermoelectric materials. This has resulted in the development of novel doping strategies, such as co-doping with other elements like gallium (Ga), nickel (Ni), and others [3]. Co-doping offers the potential to further improve the ZT values by adjusting the electronic band structure and optimizing the charge carrier concentration.

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4 Materials and Methods To synthesize the ZnO powder, 10 g of zinc acetate dihydrate (98%) was mixed with 15 mL of 95% ethanol solution. The mixture was continuously stirred using a magnetic stirrer for 30 min to ensure proper dissolution. Sodium hydroxide (NaOH) was then added gradually to the solution until the desired pH values of 7, 9, and 12 were achieved. The resulting mixture was further stirred using a magnetic stirrer at a temperature of 80 °C, allowing gelation to occur. The gel was carefully formed during this process. Subsequently, the gel was subjected to calcination at a temperature of 800 °C for a duration of 1 h. This calcination process facilitated the transformation of the gel into ZnO powder. The synthesized ZnO powder was subjected to characterization using various techniques. X-ray diffractometer (XRD) analysis was performed to determine the crystal structure and phase composition of the powder. Field Emission Scanning Electron Microscope (FESEM) analysis was carried out to examine the morphology and particle size of the ZnO powder. Additionally, Energy Dispersive X-Ray Analysis (EDX) was utilized to investigate the elemental composition of the synthesized powder. These characterization techniques provided valuable insights into the structural and morphological properties of the ZnO nanoparticles, which are crucial for understanding their potential applications in thermoelectric materials.

5 Results and Discussions 5.1 X-Ray Diffractometer (XRD) Analysis The XRD patterns obtained for the ZnO nanoparticles synthesized at pH 7, 9, and 12, with a calcination temperature of 800 °C, are presented in Fig. 1. The presence of sharp and strong diffraction peaks indicates that the ZnO nanoparticles possess a high degree of crystallinity and exhibit a single phase. Prominent diffraction peaks were observed at angles of 31.9°, 34.6°, 36.5°, 47.7°, 56.8°, 63.0°, 66.5°, 68.1°, 69.2°, 72.8°, and 77.1°, corresponding to the (100), (002), (101), (102), (110), (103), (200), (112), (201), (004), and (202) crystallographic planes, respectively. These peaks are consistent with the hexagonal wurtzite structure of ZnO [1, 3, 20]. The Debye–Scherrer formula (Eq. 1) was used to determine the average crystallite size of the ZnO nanoparticles. The symbol β, θ and λ in Eq. 1 denotes the full width at half maximum (FWHM) of the diffraction peak, the Bragg’s diffraction angle, and the X-ray wavelength, respectively. The average crystallite sizes for the samples obtained at pH 7, 9, and 12 were found to be 40.38 nm, 34.72 nm, and 34.54 nm, respectively, as illustrated in Fig. 2. These results indicate that the nanoparticle size decreases as the pH of the synthesis solution increases, suggesting a correlation between the reaction conditions and the resulting crystallite size.

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Fig. 1 XRD analysis at pH 7, 9 and 12 for calcination temperature of 800 °C Fig. 2 Crystallite size at pH 7, 9 and12 for calcination temperature 800 °C

D=

0.9λ βcosθ

(1)

The XRD analysis confirms the successful synthesis of highly crystalline ZnO nanoparticles with a well-defined hexagonal wurtzite structure. The observed variation in crystallite size with pH indicates the influence of the synthesis parameters on the final particle size, which can have implications for the thermoelectric performance of the material [3].

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5.2 Field Emission Scanning Electron Microscope (FESEM) Analysis The FESEM images of the synthesized ZnO nanoparticles at pH 7, 9, and 12 are presented in Fig. 3. The images reveal the hexagonal shape of ZnO nanoparticles at pH 7 and 12, while a rod-like structure is observed for pH 9. The presence of rod-like structures in the ZnO nanoparticles is advantageous for thermoelectric applications due to their one-dimensional nanostructure. Such structures facilitate more efficient carrier transport by reducing grain boundaries, surface defects, disorders, and discontinuous interfaces, compared to other types of structures [29]. It is worth noting that the shape of the nanoparticles is influenced by the quantity or ratio of H+ or OH− ions in the synthesis solution, which directly affects the polymerization of metal–oxygen linkages during the synthesis process [3, 23]. The particle size of the ZnO nanoparticles varied between 84.56 nm and 118.70 nm, which is approximately 40 nm larger than the average crystallite size. The particle size analysis revealed that the largest particle size of 118.70 nm was observed at pH 7, while the smallest particle size of 84.56 nm was obtained at pH 12. The particle size at pH 9 was found to be 97.22 nm, indicating an intermediate value. These results suggest an inverse relationship between the pH levels and both the crystallite and particle sizes of ZnO. Specifically, increasing the concentration of OH− ions above pH 9 lead to a decrease in the size of ZnO crystallites and particles, as the higher concentration of dissolved OH− ions during the ZnO synthesis at pH > 9 played a role in reducing the particle size [3, 24]. This reduction in size is beneficial for thermoelectric performance, as it contributes to lower thermal conductivity and an improvement in the figure of merit [1, 3]. The FESEM analysis provides valuable insights into the morphology and size characteristics of the synthesized ZnO nanoparticles. The observed variations in

Fig. 3 Morphology of ZnO at a pH 7, b pH 9 and c pH 12

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Fig. 4 EDX analysis of ZnO at a pH 7, b pH 9 and c pH 12

shape and particle size in response to pH conditions highlight the importance of controlling the synthesis parameters for tailoring the properties of thermoelectric materials.

5.3 Energy Dispersive X-Ray (EDX) Analysis The EDX images of the synthesized ZnO nanoparticles at pH 7, 9, and 12 are presented in Fig. 4. The EDX analysis provides valuable insights into the elemental composition and purity of the ZnO powder. The results indicate excellent purity, with a high concentration of Zn and O elements and very few impurities observed. The atomic percentages of Zn and O closely match the stoichiometric composition of ZnO. Specifically, at pH 7, the EDX analysis showed Zn and O atomic percentages of 69.44 and 30.56%, respectively. At pH 9, the corresponding percentages were 62.09% for Zn and 37.91% for O. Finally, at pH 12, the atomic percentages were 71.18% for Zn and 28.82% for O. These results confirm that the synthesized ZnO powder solely consists of Zn and O components, demonstrating high purity. The EDX analysis further validates the successful synthesis of ZnO nanoparticles with the desired chemical composition. The high purity and stoichiometric composition of ZnO nanoparticles are essential for achieving optimal thermoelectric performance.

6 Conclusions In conclusion, the synthesis of ZnO nanoparticles using the sol–gel method at different pH values and 800 °C calcination temperatures was successfully achieved. The XRD analysis confirmed the presence of the hexagonal wurtzite structure in all

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the synthesized ZnO nanoparticles. The smallest crystallite sizes were obtained at pH 12 (34.52 nm), followed by pH 9 (34.72 nm), and pH 7 (40.38 nm), indicating that pH affects the crystallinity of ZnO nanoparticles. FESEM images revealed that the synthesized ZnO nanoparticles exhibited a nanorod-like structure, with the smallest average particle size observed at pH 12 (84.56 nm), followed by pH 9 (97.22 nm), and pH 7 (118.70 nm). The homogeneity and consistent size of the ZnO nanoparticles were consistent with the XRD results, indicating good crystallinity. Based on the XRD and FESEM analysis, it can be concluded that pH 12 is the optimal condition for obtaining ZnO nanoparticles with desirable crystalline structure and morphology. The EDX analysis further confirmed the purity of the synthesized ZnO nanoparticles, with atomic percentages of Zn and O close to the stoichiometric composition. Overall, this study demonstrates the influence of pH on the structural and morphological properties of ZnO nanoparticles. These findings contribute to the understanding of the synthesis parameters and provide valuable insights for the development of thermoelectric materials with enhanced performance. Acknowledgements The author acknowledges the support and funding provided by the Ministry of Higher Education of Malaysia (MOHE) through the Fundamental Research Grant Scheme (FRGS) under Grant No. FRGS/1/2022/STG05/UMP/03/1. (University reference RDU220130) and Universiti Malaysia Pahang Al-Sultan Abdullah (UMPSA) for laboratory facilities as well as additional financial support under Sustainable Research Collaboration Grant funded by UMPSA, IIUM & UiTM under Grant No. RDU200744. The author also expresses gratitude to the Faculty of Manufacturing and Mechatronic Engineering Technology, Universiti Malaysia Pahang Al-Sultan Abdullah (UMPSA). Their contributions and support were invaluable in the successful completion of this research project.

References 1. Sulaiman S, Izman S, Uday MB, Omar MF (2022) Review on grain size effects on thermal conductivity in ZnO thermoelectric materials. RSC Adv 12:5428–5438 2. Singh S (2021) Energy: crises, challenges and solutions. Wiley, pp 1–17 3. Sulaiman S, Izman S, Uday MB, Omar MF (2022) Review of the nanostructuring and doping strategies for high-performance ZnO thermoelectric materials. Crystals 12:1076 4. Zaferani SH, Jafarian M, Vashaee D, Ghomashchi R (2021) Thermal management systems and waste heat recycling by thermoelectric generators—an overview. Energies 14:5646 5. Jantrasee S, Moontragoon P, Pinitsoontorn S (2016) Thermoelectric properties of Al-doped ZnO: experiment and simulation. J Semicond 37:092002-1–092002–8 6. Orr B, Akbarzadeh A, Mochizuki M, Singh R (2016) A review of car waste heat recovery systems utilising thermoelectric generators and heat pipes. Appl Therm Eng 101:490–495 7. Jouharaa H, Khordehgaha N, Almahmoud N, Delpech B, Chauhan A, Tassou SA (2018) Waste heat recovery technologies and applications. Therm Sci Eng Progress 6:268–289 8. Jouharaa H, Zabnienska-Gora A, Khordehgaha N, Doraghia Q, Ahmada L, Normana L, Axcella B, Wrobella L, Daid S (2021) Thermoelectric generator (TEG) technologies and applications. Int J Thermofluids 9:100063 9. Jood P, Mehta RJ, Zhang Y, Peleckis G, Wang X, Siegel RW, Borca-tasciuc T, Dou SX, Ramanath G (2011) Al-doped zinc oxide nanocomposites with enhanced thermoelectric properties. Nano Lett 11:4337–4342

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Effect of Different Shape ZnO Nanoparticles on the Thermal Conductivity of ZnO Nanofluids Tengku Nur Azza Tengku Ahmad Faizal, Radhiyah Abd Aziz , and Suraya Sulaiman

Abstract Remarkable thermal conductivity improvement in nanofluids containing only a small proportion of nanoparticles, as well as their outstanding thermo-physical properties with no or low-pressure drop penalty, greater transport properties, and significant heat transfer enhancement, drew many researchers to nanofluids. The main goal of this research is to investigate the effect of various shapes of Zinc Oxide (ZnO) nanoparticles on the thermal conductivity of ZnO nanofluids; i.e., nanospheres and nanoplates. The synthesized ZnO undergoes several physico-chemically characterized by various techniques. The appearance of pure hexagonal wurtzite phase structures of ZnO nanoparticles is revealed by X-ray diffraction (XRD) structural analysis. The surface morphologies of ZnO nanoparticles were studied using a field emission scanning electron microscope (FESEM), which successfully revealed nanosphere and nanoplate shapes. Fourier transforms infrared spectroscopy (FTIR), analysis confirms the presence of Zn–O stretching. Brunauer Emmett Teller (BET) analyse showed that nanosphere which had the smaller size particle thus larger surface area. The stability and absorbance of ZnO nanospheres and nanoplates based on nanofluid were evaluated using UV–Vis spectrum methods in this paper. Finally, the C-therm analysis data showed thermal conductivity of nanofluid with nanosphere shape is higher than nanoplate. Keywords Nanofluid · Nanosphere · Nanoplate · Thermal Conductivity

1 Introduction Metal particles the size of nanometers is dissolved in manufacturing heat transfer liquids such as ethylene glycol, water, or engine oil to establish an innovative category of engineered fluids through high thermal conductivity. Many industrial sectors, such as transport, machining, chemical reaction, and electronics, rely heavily on T. N. A. Tengku Ahmad Faizal · R. Abd Aziz · S. Sulaiman (B) Faculty of Manufacturing and Mechatronic Engineering Technology, Universiti Malaysia Pahang Al-Sultan Abdullah, 26600 Pekan, Pahang, Malaysia e-mail: [email protected] © The Author(s), under exclusive license to Springer Nature Singapore Pte Ltd. 2024 R. Abd. Aziz et al. (eds.), Intelligent Manufacturing and Mechatronics, Springer Proceedings in Materials 40, https://doi.org/10.1007/978-981-99-9848-7_22

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heating and cooling fluids. Nanofluids are primarily used for heat transfer enhancement, reduced consumed fluids, and cost reduction in the industry well as system miniaturization. The single most critical issue confronting humanity in the next 50 years has been identified as energy, particularly the serious terawatt challenge while minimizing carbon emissions and global warming [1]. Over 70% of the energy we use today is formed in or through in the form of heat. Given the significant rise in global energy demand, improving heat transmission and minimizing energy waste due to inefficient use has become an increasingly critical task. Nanofluids have been investigated as a new alternative fluid solution for improving the efficiency and profitability of thermal systems in industrial, commercial, and residential settings [2]. Due to the thermal characteristics of nanoparticles, adding nanoparticles to cutting fluid such as coolant during machining also considerably reduces the high temperature induced by high velocities and higher cutting speed. As a result, by adding nanoparticles is able to reduce the stress on product surface area and capacity to fabricate a fine surface roughness [3]. Thermal transfer improvement varies depending on the type of nanoparticle used. Carbon nanotubes (CNTs) have a high aspect ratio of about 2000 and a thermal conductivity of roughly 3000 W/mK. ZnO is an abundantly available ceramic material, due to its varied properties; it shows an imperative part in heat transfer applications. ZnO nanoparticles have various advantages, including high availability and ease of preparation, excellent thermal properties, high economic prospects, and superior water stability when compared to other nanoparticles, lack of toxicity, non-flammable, and eco-friendliness. The suspension of nanoparticles in fluids to generate extremely effective heat transfer fluids also has been the issue of plentiful research. Nanofluids have recently sparked a lot of interest due to their significantly improved thermal properties. Consequently, the majority of research efforts to present this fascinating issue have focused on evaluating the “effective” thermophysical properties of mixtures which include properties such as thermal conductivity.

2 Materials and Methods 2.1 Materials The following reagents are used to synthesize ZnO nanosphere and nanos particles: zinc acetate dihydrate (Zn(CH3 COO)2 2H2 O), methanol, cetyltrimethyl ammonium bromide (CTAB), sodium hydroxide (NaOH), ethanol and distilled water.

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2.2 Methodolgy For the nanosphere, firstly, using a magnetic stirrer, 140 ml ethylene glycol was used to dissolve 0.004 mol zinc acetate dihydrate (Zn(CH3 COO)2 2H2 O). The solution was then placed in a stainless-steel autoclave lined with Teflon (225 mL). The autoclave was tightly enclosed and then placed in the oven. Temperatures were raised from room temperature within 20 min and were raised to 160 °C and maintained for 5 h. The autoclave was normally cooled down to room temperature when the reaction was completed. Centrifugation at 5000 rpm for 30 min was used to isolate the white products and then follow by washing, dispersing again in methanol, and drying for 24 h at 120 °C, the characterization test is performed. Then, for nanoplate, CTAB (0.25 g) and NaOH (6.72 g) were mixed in 70 ml of distilled water at room temperature and vigorously stirred. Then, while stirring continuously, 8.12 g of zinc acetate dihydrate (Zn(CH3 COO)2 2H2 O) was dissolved in 70 ml of distilled water and added to the afore mentioned solution. The result of solution was then heated at 90 °C for 15 h in a Teflon-lined stainless-steel autoclave. Centrifugation was used to isolate the white solid product from the solution, which was then washed four times with distilled water and ethanol before being dried in the air at 80 °C. The nanoparticles then undergo several characterizations.

2.3 Preparation of ZnO Nanofluids ZnO nanoparticles with different shapes, the identical mass nanosphere and nanoplate were dispersed in 20 ml ethylene glycol each. To ensure homogenous nanoparticle dispersion in the base fluid, the mixture was nonstop stirred for 1 h and sonicated for 3 h at volume concentration 0.04% and the mass of ZnO particles will be determined using the formula volume concentration. Lastly, another characterization test will be conducted to analyze the stability and thermal conductivity for both nanofluid samples.

2.4 Characterization of ZnO Nanoparticles Crystal structure analysis of samples was performed using CuKα radiation, (λ = 1.5406 Å) in the region of 2θ between 20º and 80º. Field Emission Scanning Electron Microscope (FESEM) was utilized to examine the morphology and particle size of the nanoparticles. Fourier Transmission Infrared (FTIR) was utilized to determine the chemical bonding of the molecule, which was then used to make ZnO nanoparticles. To determine the specific surface, the Brunauer Emmett Teller (BET) technique was utilized.

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2.5 Characterization of ZnO Nanofluids UV–Vis spectrophotometer (UV–Vis) measurements were utilized to illustrate the colloidal stability of the dispersions quantitatively. The rate at which heat travels through a material is measured by thermal conductivity. The patented Modified Transient Plane Source (MTPS) method is used in the C-therm TCi. The one-sided interfacial heat reflectance sensor provides a steady heat source to the sample for a brief period of time. Thermal conductivity and effusivity are immediately measured, providing a thorough description of the sample’s thermal properties. Thermal conductivity measurement is fast and straightforward because the results are given in real-time.

3 Result and Discussion 3.1 ZnO Nanoparticles Characterization The XRD patterns for ZnO shown in Fig. 1 for nanosphere and nanoplate prepared using the hydrothermal process are pure hexagonal wurtzite structures. For nanosphere, the peak is recognized to originate with miller indices (100), (002), (011), (012), (110), (013), (200), (112), (021), (004) and (022) while for nanoplate is (100), (002), (101), (102), (110), (103), (200), (112), (201), (004) and (202). The highest intensity peak in the spectra of the samples was (011) planes for the nanosphere while (101) for the nanoplate of ZnO. Most of the diffraction patterns matched the hexagonal wurtzite ZnO pattern in the Inorganic Crystal Structure Database (ICSD) with the code number (PDF 01–082-9744) for nanosphere while (PDF 01–082-7494) for nanoplate. As a result, this research is supported by [7]. The Scherrer equation was utilized to compute the average crystallite size of ZnO based on the entire width at half the maximum of the crystal. The Full Width Half Maximum (FWHM) is the most important diffraction peak was calculated and the average crystallite size for the ZnO nanosphere is 23.70 nm while for nanoplate is 24.80 nm. FESEM was used to analyse the surface morphology of the produced zinc oxide nanoparticles. FESEM image of a ZnO nanostructure produced by the hydrothermal technique in a solution at 160 °C for 6 h, Fig. 2(a) depicts a dense nanosphere, while Fig. 2(b) depicts a nanoplate after 15 h at 90 °C undergoing a hydrothermal process. As shown in Fig. 2(a), a large quantity of sphere ZnO nanostructures formed, and the structures are mostly uniform. Meanwhile, Fig. 2(b) shows that the morphology of particles is not in a uniform shape due to the plane’s attractions. Based on the graph of Fig. 3, the functional group of ZnO NPs was identified in this FTIR spectra. All of the main peaks’ intensities in transmittance mode for the wavenumber range 400–4000cm−1 for both nanosphere and nanoplate ZnO nanoparticles can be seen in Fig. 3. The band positioned between 431 and 457 cm−1 corresponds to Zn–O stretching mode which confirms the formation of ZnO [8]. From

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Fig. 1 XRD pattern of a nanosphere and b nanoplate of ZnO nanoparticles

Fig. 2 Morphology of a nanosphere and b nanoplate of ZnO nanoparticles

FTIR spectra, the presence of strong peaks in the higher regions at 3479 and 3451 are due to the stretching vibration of hydroxyl (OH) group. The H2 O and glycol functional groups on ZnO crystal surfaces, which acts as a surfactant in ZnO processing and moisture content in the air, create these –OH bending and stretching vibration peaks. The peaks around 1637 and 1653 cm−1 are the result of C = O amide I and amide II groups. The peak presents at 1416 and 1420 cm−1 are due to –C–H bending vibration band since there is a partially converted aldehyde or ketone present [9]. The Brunauer–Emmett–Teller (BET) was used to determine the specific surface area of nanosphere and nanoplate of ZnO nanoparticles. The specific surface area, pore size, and volume distribution of the BET surface were examined using the BET method in a nitrogen adsorption–desorption test to acquire more about it. The N2 adsorption–desorption isotherm of the two samples resembles to type IV isotherm with a hysteresis loop are shown in Fig. 4(a) and (b). As depicted in Fig. 4(a) and (b), the amount of quantity adsorbed is higher for nanosphere compared to nanoplate due to a decrease in size which is confirmed by the high value of the surface area.

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Fig. 3 FTIR spectra of a nanosphere and b nanoplate of ZnO nanoparticles

Nanospheres with a higher BET surface area and mesoporosity may help transport electrolyte ions through porous channels and provide a greater number of active sites, improving the composite’s electrochemical performance and possibly assisting in the achievement of high thermal conductivity properties. Table 1 summarises the BET data for synthesize compounds. These results support the findings of adsorption/ desorption isotherms. Table 1 lists the particle parameters of the samples, such as surface area, pore size, and volume distributions. The BET surface area was 22.93 m2 /g for nanosphere while 8.08 m2 /g for nanoplate. For instance, the specific area of the sample nanosphere is about 3 times higher than the nanoplate. The DSSCs benefit from their huge surface area and varied pore size because they help with massive dye loading and electrolyte permeability. Porosity and specific surface area of active material are widely recognized to play important roles in photoanodes of DSSCs devices [10].

3.2 ZnO Nanofluid Stability Measurements The absorption spectrum of the ZnO nanosphere and nanoplate of nanofluids on day 2 and day 14 were compared using UV–Vis spectrophotometry in this study. Figure 5 (a) and 5 (b) show that for the nanosphere, the smaller the particle, the higher the absorbance, and this trend was maintained from day 2 to day 14 than nanoplate as nanoplate is bigger in size. Nanoparticles quickly aggregate in nanofluids to form

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Fig. 4 Gas adsorption isotherm curve of nanosphere and nanoplate of ZnO nanoparticles

Table 1 BET surface area, pore diameter and pore volume distribution of synthesized samples in two different shapes Sample

BET/m2 /g

Pore size/4V/A by BET

Pore volume/cm3 /g

Nanosphere

22.9373 m2 /g

137.245 A

0.0787

Nanoplate

8.0866 m2 /g

190.23 A

0.0384

agglomerates of increasing size, and since nanoplate particles are denser than the base fluid, they are more prone to agglomeration compared to the nanosphere. Finally, when the absorbance lowers, the stability of the nanofluid decrease due to a decrease in the number of particles on the top of the base fluid which cause fewer nanoparticles to absorb the light during analysis. Lastly, for a nanosphere that had a small particle size, the density of the nanosphere is lower thus the nanoparticle is slow to settle down. So, there are still a lot of nanoparticles that are still stable in the based fluid. This indicates that the larger the nanoparticle size, the stronger the early agglomeration of the nanofluid which causes lower absorbance. It is also can be seen in the Fig. 6, where the color changes of the ZnO nanofluid from Day 1 until Day 14.

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Fig. 5 UV–Vis spectra of nanosphere and nanoplate ZnO nanoparticles for Day 1 and Day 14

Fig. 6 Condition of a Day 2 of (ethylene glycol, nanoplate and nanosphere); b Day 14 of (ethylene glycol, nanoplate and nanosphere)

3.3 ZnO Nanofluid Thermal Conductivity Measurements The relative thermal conductivity of ZnO nanofluid increased as the temperature increased, as illustrated in Fig. 7. The Brunauer–Emmett–Teller (BET) research verified that the nanosphere with the highest thermal conductivity belonged to the nanosphere with the highest surface area. The main influence of nanoparticle shape on thermal conductivity was considered to be a change in surface area. The utilization of spherical nanoparticles in nanofluids has various advantages over other shapes, including enhanced stability and reduced clogging problems. From the abovementioned experimental data, it can be decided that nanoparticles with a larger surface area have a higher nanofluid thermal conductivity. In nanoparticles, a material’s surface area is frequently more reactive than its center, hence a bigger surface area indicates that the particle is more reactive.

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Fig. 7 Thermal conductivity for nanosphere and nanoplate shape of ZnO nanofluid and ethylene glycol as reference base nanofluid

The thermal conductivity of nanofluids rises as particle size decreases, according to the study. Theoretically, two mechanisms support this pattern: Brownian motion of nanoparticles and liquid layering surrounding nanoparticles, as it would experience larger micro convection effects, resulting in a higher rise in thermal conductivity [11]. Experiment data currently available tends to confirm such hypotheses, with a better quantitative match. However, ZnO nanofluid with nanoplate shape has lower thermal conductivity than base fluid due to agglomeration and sedimentation caused by the strong Vander-Walls force of attraction between particles, which condensed the effective area of the interaction, lowering the thermal conductivity of the nanofluids [12].

4 Conclusion In summary, the ZnO NPs were successfully synthesized based on the optimised parameters and using a hydrothermal process. The optimised parameter shape used for synthesized ZNO nanoparticles was nanosphere and nanoplate. This research also successfully characterized the chemical, and physical of nanoparticle and nanofluid properties. For the XRD analysis, the crystal structure had been successfully identified. The crystal structure was a pure hexagonal wurtzite structure. The highest peaks for crystal plan for nanosphere are (011) and nanoplate is (101) with the average crystallite size of the nanosphere is 23.7 nm while for nanoplate is 24.8 nm by

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using the Scherer equation. Then, for FESEM, the analysis proved that the surface morphology of produced ZnO using hydrothermal process but different materials depict nanosphere and nanoplate shape. After that, from FTIR analysis, ZnO NPs successfully revealed the peaks of formation of Zn–O stretching vibration which is at 457 cm−1 for nanosphere and 432 cm−1 for nanoplate. Following, the BET analysis that the highest adsorption capacity corresponds to the adsorption of nanosphere shape, which had the smaller size particle and thus larger surface area. The amount of quantity of N2 adsorbed is higher for nanosphere compared to nanoplate due to a decrease in size which is confirmed by the high value of the surface area. As for UV–Vis, the analysis represented the stability of nanofluid from time onwards. It is shown, that the nanofluid with nanosphere shape is still stable after 14 days than nanoplate. It also revealed that nanoplate ZnO nanoparticles have a higher density which causes the nanoparticles to be easy to settle down due to the larger particle size. Additionally, the thermal conductivity of ethylene glycol, nanosphere and nanoplate of ZnO nanofluid was determined by C-therm. The results indicated that the nanosphere has the highest thermal conductivity followed by ethylene glycol and nanoplate of ZnO as the nanofluid with nanoplate shape tends to have low thermal conductivity than the base fluid because of agglomeration as a result of the strong Van-der-Walls force of attraction between the particles that lowered the interaction’s effective area that lead to lowering thermal conductivity. Acknowledgements I would like to thank the Ministry of Higher Education Malaysia for the financial aids and Universiti Malaysia Pahang Al-Sultan Abdullah and its staff for the laboratory facilities and financial support from the fundamental research grant scheme FRGS/1/2019/STG07/ UMP/02/7 (University Reference RDU1901205) and FRGS/1/2022/STG05/UMP/03/1 (University Reference RDU220130).

References 1. Smalley RE (2005) Future global energy prosperity: the terawatt challenge. MRS Bull 30(6):412–417 (2011) 2. Yu W, France DM, Choi SUS, Routbort JL (2007) Review and assessment of nanofluid technology for transportation and other applications. https://doi.org/10.2172/919327 3. Singh DK, Pandey DK, Yadav RR, Singh D (2012) A study of nanosized zinc oxide and its nanofluid. Pramana J Phys 78(5):759–766. https://doi.org/10.1007/S12043-012-0275-8 4. Glasgow RE, Estabrooks PA, Ory MG, Ory MG, Ory MG (2020) Characterizing evolving frameworks: issues from Esmail et al. (2020) review. Implementation Sci 15(1):1–3. https:// doi.org/10.1186/S13012-020-01009-8/METRICS 5. Sen SK, Paul TC, Dutta S, Hossain MN, Mia MNH (2020) XRD peak profile and optical properties analysis of Ag-doped h-MoO3 nanorods synthesized via hydrothermal method. J Mater Sci Mater Electron 31(2):1768–1786. https://doi.org/10.1007/S10854-019-02694-Y/ FIGURES/14 6. Nallusamy S, Sujatha K (2021) Experimental analysis of nanoparticles with cobalt oxide synthesized by coprecipitation method on electrochemical biosensor using FTIR and TEM. Mater Today Proc 37(Part 2):728–732. https://doi.org/10.1016/J.MATPR.2020.05.735

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7. Wang L, Kang Y, Liu X, Zhang S, Huang W, Wang S (2012) ZnO nanorod gas sensor for ethanol detection. Sens Actuators, B Chem 162(1):237–243. https://doi.org/10.1016/J.SNB. 2011.12.073 8. Thongam DD, Gupta J, Sahu NK (2019) Effect of induced defects on the properties of ZnO nanocrystals: surfactant role and spectroscopic analysis. SN Appl Sci 1(9):1–14. https://doi. org/10.1007/S42452-019-1058-3/TABLES/2 9. Xiong G, Pal U, Serrano JG, Ucer KB, Williams RT (2006) Photoluminescence and FTIR study of ZnO nanoparticles: the impurity and defect perspective. Physica Status Solidi (C) Curr Top Solid State Phys 3(10):3577–3581. https://doi.org/10.1002/PSSC.200672164 10. Akbulut M, Alig ARG, Min Y, Belman N, Reynolds M, Golan Y, Israelachvili J (2007) Forces between surfaces across nanoparticle solutions: role of size, shape, and concentration. Langmuir 23(7):3961–3969. https://doi.org/10.1021/LA062613G 11. Patel J, Parekh K (2018) Effect of size and morphology on stability and thermal conductivity of ZnO nanofluid. J Nanofluid 7:284–291. https://doi.org/10.1166/jon.2018.1454 12. Wen D, Lin G, Vafaei S, Zhang K (2009) Review of nanofluids for heat transfer applications. Particuology 7(2):141–150. https://doi.org/10.1016/J.PARTIC.2009.01.007

Carbon Nanotube-Reinforced Polymer Composites for Biomedical Applications Mohd Nizar Mhd Razali, Nurul Najwa Ruzlan, and Amirul Hakim Sufian

Abstract The utilization of carbon nanotube-reinforced polymer composites (CNTRPCs) has been recognized as a significant breakthrough in the field of material science, owing to their exceptional amalgamation of characteristics. The incorporation of carbon nanotubes (CNTs) into a polymer matrix results in a composite material that combines the notable mechanical strength, electrical conductivity, and thermal stability exhibited by CNTs with the inherent flexibility of polymers. The process of integration leads to the development of improved composite materials that are suitable for a wide range of applications, and possess the ability to modify their properties according to specific application requirements. CNT-RPCs have established a distinct position within the field of biomedicine, specifically in the domains of bone implantation, tissue engineering, regenerative medicine, and drug delivery. These cells offer notable benefits including biocompatibility, electrical conductivity, and efficient drug distribution. Moreover, the incorporation of carbon nanotubes (CNTs) into polymers has demonstrated significant advancements in the fields of electronics, aerospace, and medicine. Cutting-edge modeling techniques utilizing deep learning are currently being implemented to enhance and optimize these composite materials. The present analysis provides an in-depth exploration of the advancement, attributes, and utilization of carbon nanotube-reinforced polymer composites (CNT-RPCs) in the field of biomedicine. Notably, recent advancements, obstacles, and prospects pertaining to this revolutionary material are emphasized. Keywords Carbon nanotube-reinforced polymer composites · Biomedical applications · Bioactivity · Bioresorbable implants · Material characterization

M. N. Mhd Razali (B) · N. N. Ruzlan · A. H. Sufian Faculty of Manufacturing and Mechatronic Engineering Technology, Universiti Malaysia Pahang Al-Sultan Abdullah, 26600 Pekan, Pahang, Malaysia e-mail: [email protected] © The Author(s), under exclusive license to Springer Nature Singapore Pte Ltd. 2024 R. Abd. Aziz et al. (eds.), Intelligent Manufacturing and Mechatronics, Springer Proceedings in Materials 40, https://doi.org/10.1007/978-981-99-9848-7_23

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1 Introduction of Carbon Nanotube-Reinforced Polymer Composites The emergence of carbon nanotube-reinforced polymer composites (CNT-RPCs) has led to significant advancements in the field of material science, as these composites exhibit a remarkable amalgamation of properties. The incorporation of carbon nanotubes (CNTs) into a polymer matrix presents a composite material that combines the exceptional mechanical strength, superior electrical conductivity, and admirable thermal stability of CNTs with the flexibility and formability of polymers [1–26]. The incorporation of diverse mechanical, electrical, and thermal characteristics greatly enhances the composite material, rendering it appropriate for a broad spectrum of applications [1, 8, 26–29]. Furthermore, the versatility of the material is augmented by the ability to modify these properties by manipulating the concentration of carbon nanotubes (CNTs) and their dispersion within the polymer matrix. The material’s adaptability enables it to fulfill specific application requirements [29–36]. Due to their biocompatibility, mechanical robustness, and electrical conductivity, carbon nanotube-reinforced polymer composites (CNT-RPCs) are unique in biomedicine. Bone implantation research is noteworthy. They reduce stress shielding problems caused by standard implants since their mechanical properties can be modified to match natural bone [25, 29–39]. CNT-RPCs’ electrical conductivity helps osteoblasts connect and proliferate, which is essential for osseointegration [29]. Their potential applies to tissue engineering and regenerative medicine. Modified CNT-RPCs with a wide surface area are appropriate for cellular adhesion and proliferation, which are needed for tissue regeneration [36]. CNT-RPCs can improve electrically responsive cells including neurons and muscle cells due to their electrical conductivity, making them useful in regenerative medicine [36]. CNTs’ enormous surface area accommodates more medicines, and their interaction with the polymer matrix controls drug release, makes targeted drug delivery is possible, as shown in Fig. 1 [39].

Fig. 1 CNTs’ enormous surface area improve bioactivity [39]

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Carbon nanotubes (CNTs) in polymers have changed electronics, medicine, and aerospace [1–8, 19–26]. CNTs and polymers work well together, making CNTRPCs promising. CNT-RPCs can be employed in orthopedic bone implants [1, 29]. The orthopaedic market will reach US$79.5 billion, driving need for biocompatible, mechanically strong, and durable materials [29]. CNT-containing Mg-Zn biocomposites kill E. coli and S. aureus and have strong mechanical properties [1]. Metallic implants emit debris and cause cytotoxicity [29]. Such advances could alleviate these issues. CNT conductivity matters in electronics and sensors. High electrical conductivity of polymers containing CNTs enables for several applications, including flexible and stretchable electronics, which are becoming more relevant in our digital age [2, 26]. According to Fazi et al. [5], CNTs combined with polymeric films offer a unique conductivity and stretchability, making them potential wearable electronics and sensor possibilities. With CNT-RPCs, computational approaches have improved. Using deep learning models and the large online literature helps optimize composites [15]. So et al. [15] made ABS/CNT composites with better electrical and mechanical properties using this approach. Aerospace and automotive use CNT-RPCs. The weight-tostrength ratio, high thermal conductivity, and wear resistance make them necessary for parts under regular mechanical stress or high temperatures [8, 19, 22]. Airplane wings and vehicle bodies are examples. CNTs and other reinforcements minimize delamination-induced composite damage. Increasing fracture propagation resistance in CFRP composites enhanced with cellulose nanofibers may improve key component longevity and safety [22]. This review aims to provide a comprehensive account of the recent advancements in the development and utilization of carbon nanotube-reinforced polymer composites (CNT-RPCs) in the field of biomedicine. Commencing with a clarification of the characteristics and techniques employed in the production of the material, this discussion will transition into a comprehensive examination of its application in the fields of bone implants, tissue engineering, and drug delivery. This study will additionally focus on techniques to enhance the biological activity of these composite materials, while also examining emerging patterns and challenges within this field.

2 Advances in Biomedical Applications 2.1 Use of Carbon Nanotube-Reinforced Polymer Composites in Bone Implants Carbon nanotube-reinforced polymer composites (CNT-RPCs) have revolutionized bone implant applications due to their many characteristics. These qualities are due to carbon nanotubes (CNTs) and their mutually advantageous polymer matrix interactions. The mechanical strength, electrical conductivity, and thermal stability of carbon nanotube-reinforced polymer composites (CNT-RPCs) make them intriguing

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Fig. 2 Elastic Modulus comparison of bio-compatible material with PEEK [29]

biomedical breakthroughs, as shown in Fig. 2 [29]. PEEK is biocompatible, chemically resistant, and mechanically strong, hence previous researchers suggested it for bone implants. However, limited bioactivity and bone bonding limit polyetheretherketone (PEEK) bone implants [29]. Previous study recommended carbon nanotubes in PEEK. Carbon nanotubes (CNTs) in polyetheretherketone (PEEK) matrix improve mechanical characteristics, allowing exact bone mimicry. This crucial finding may alleviate stress shielding, a common issue where implants unintentionally lower bone tissue stress. Implant degradation and failure often result from stress shielding [29]. Additionally, electrical conductivity in carbon nanotubes (CNTs) helps osteoblasts attach and grow. The adhesion and proliferation of osteoblasts on the implant surface are necessary for osseointegration, the structural and functional integration of the implant with the bone tissue. Implant lifespan and stability matter. In example, bredigite (Br; Ca7MgSi4O16)–carbon nanotubes (CNTs) enhanced MgZn alloy microhardness and compressive strength, where its microhardness and compressive strength improved 57% and 72% [1]. Simulated bodily fluids reduced composite material degradation by 50%. The composite material was also effective against resistant organisms including E. coli and S. aureus. Thus, with these properties, it is appropriate to utilize CNT-RPCs for bone implants [1].

2.2 Role in Tissue Engineering and Regenerative Medicine In the ever-evolving world of tissue engineering and regenerative medicine, carbon nanotube-reinforced polymer composites (CNT-RPCs) have emerged as powerful contenders, thanks to their unique set of attributes. CNT-RPCs combine CNTs’ mechanical strength, electrical conductivity, and thermal stability with polymers’ flexibility and adaptability. The fusion described has great potential for use in materials that need structural integrity and biocompatibility. Scaffolds, which aid cellular proliferation and tissue regeneration, are one of the main uses of carbon nanotubereinforced polymer composites (CNT-RPCs). Scaffolds help cells adhere, grow, and

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MXene CNT

Fig. 3 Innovation of MXene/CNT composites [11]

specialize by creating a favorable three-dimensional structure. They help develop functional tissue by doing this. MXene-CNT composites’ properties and utility were extensively analyzed by Mohajer et al. [36], improving our understanding of their contributions. MXenes, two-dimensional materials, have a high specific surface area and are functionalized. With the mechanical and electrical properties of carbon nanotubes (CNTs), the MXene-CNT composite is ideal for tissue engineering, as shown in Fig. 3 [11]. The MXene-CNT composites’ large surface area attracts and promotes cell attachment and proliferation. The mechanical robustness of regenerated tissue protects it and ensures structural reinforcement. For electrically responsive cells like neurons and muscle cells, carbon nanotubes (CNTs)’ intrinsic electrical conductivity ensures optimal development and performance. Functionalization is another benefit of MXenes. This suggests that composites can strategically attach bioactive molecules. Bioactivity is increased by deliberately adding this substance, which boosts cellular adhesion, proliferation, and differentiation. When considering their collective characteristics, MXene-CNT composites are leading scaffold materials for tissue engineering.

2.3 Potential in Drug Delivery Systems Carbon nanotube-reinforced polymer composites (CNT-RPCs) exhibit promising prospects in drug delivery platforms. These novel materials combine carbon nanotubes (CNTs) and polymers to create a compelling combination. Carbon nanotubes (CNTs)’ exceptional mechanical strength, electrical conductivity, and thermal stability combined with polymers’ adaptability and malleability make these composites ideal for structural durability and controlled therapeutic agent release. Zhao et al. [39] investigated the effects of carbon nanotube (CNT)-reinforced hydroxyapatite (HAP) composite coatings on titanium substrates for drug delivery. Hydroxyapatite (HAP), the main component of bone minerals, occurs naturally as calcium apatite. The biocompatibility and bioactivity of this material make it ideal for implant

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coating. The matrix’s mechanical properties and drug release efficiency improve with CNTs. Carbon nanotubes (CNTs), which have a large surface area, improve drug loading, which is essential for therapeutic efficacy [11]. Physical adsorption and chemical binding help attach drugs to carbon nanotubes. The large surface area of carbon nanotubes (CNTs) ensures their drug binding capacity. Optimizing CNT-polymer matrix interaction can also modulate drug release. Carbon nanotube (CNT) concentration, dispersal, polymer matrix alignment, and functionalization can be used to modulate release kinetics. This precise control mechanism allows the creation of carbon nanotube-reinforced polymer composites (CNT-RPCs) that release pharmaceuticals at predetermined rates over time. This implies that controlled drug release may be possible with CNT-RPCs. Implants must be able to release drugs locally to prevent infections and promote tissue integration, boosting their efficacy and longevity. Carbon nanotube-reinforced polymer composites (CNT-RPCs) are promising drug delivery systems due to their versatility, adaptability, and unique properties [11].

3 Enhancing the Bioactivity of Polymer Composites In the context of biomedical applications, particularly in the field of implants, this characteristic guarantees the seamless integration of introduced materials with the pre-existing biological tissues, thereby ensuring the attainment of both functional and durable outcomes. The advent of polymer composites has facilitated the attainment of improved bioactivity. Carbon nanotubes (CNTs) possess remarkable mechanical strength, electrical conductivity, and thermal resilience, making them a highly suitable choice for enhancing the structural integrity of polymer composites. The incorporation of carbon nanotubes (CNTs) into polymer matrices has been demonstrated to significantly enhance the characteristics of the resulting composite, encompassing its mechanical, electrical, and thermal properties. Table 1 presents a comprehensive overview of significant research and advancements that exemplify the potential of incorporating carbon nanotubes (CNTs) and other bioactive materials into polymer composites.

4 Research Gap and Future Expectation 4.1 Challenges and Limitations in Current Research i. Fabrication Hurdles—Making composites from polymers reinforced with carbon nanotubes (CNTs) is difficult due to their unique characteristics. This composite material depends on CNT dispersion and alignment in the polymer matrix. Evenly dispersed carbon nano-tubes (CNTs) increase a composite’s

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Table 1 Significant research and advances of carbon nanotubes (CNTs) potential Category

Description

Possible innovation

Bone implants and orthopedics

Mg-Zn alloy containing bredigite and CNTs increased microhardness and compressive strength. The composite was also antibacterial against E. coli and S. aureus. PEEK, a top bone implant material, has osseointegration difficulties that can be fixed by bioactive glass [1, 29]

Design of advanced polymer composites that integrate CNTs for improved cell adhesion, proliferation, and differentiation

Advanced modeling & prediction

A pioneering study by earlier researchers used deep learning to construct bioactive acrylonitrile–butadiene–styrene/CNT composites. Data-centric analysis of CNT content, dispersion, and orientation led to improved materials [15]

Implementation of AI-based tools that aid in predicting optimal compositions of polymer composites for varied biomedical applications

Tribological & mechanical enhancements

Previous researchers probed into the effects of carbon and cellulose-based nanofillers in carbon fiber-epoxy composites. The study underscored the importance of these fillers in enhancing not just the mechanical properties but also the bioactivity of the composite [19]

Exploration into the potential of diverse nanofillers in reinforcing composites for biomedical applications

Safety & delamination

Previous study tackled the challenge of delamination in carbon-fiber-reinforced polymer composites by integrating cellulose nanofibers. This addition not only mitigated delamination but also highlighted the biocompatibility of cellulose, promoting cell adhesion and proliferation [22]

Continued research into addressing structural challenges in composites, with a keen eye on enhancing bioactivity

mechanical and electrical qualities. Carbon nano-tubes (CNTs) cluster, making composite materials non-uniform. Nonuniform dispersion can degrade material characteristics and performance in real-world applications. ii. Characterization Barriers—To employ carbon nanotube-reinforced polymer composites (CNT-RPCs) effectively, one needs grasp their comprehensive properties. Extensive mechanical, electrical, thermal, and tribological (friction, lubrication, and wear) study is needed. The Miao et al. study emphasized tribological features. Machinery and biological implants with moving parts need this. Composite component dependability and durability are hard to forecast and guarantee without rigorous characterization. iii. Biomedical Concerns—Biomedicine is interested in CNT-RPCs for drug delivery and implants. Despite promising first results, these materials’ biocompatibility must be completely explored, especially given their long-term impacts. These composites’ long-term effects on biological systems are assessed. CNTs are also suspected of being harmful. The impact of releasing these particles into the body or environment must be considered for safety.

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4.2 Future Expectation on the Unexplored Domains of CNT-RPCs Bioresorbable implants, those designed to be naturally absorbed by the body over time, represent a relatively uncharted domain for CNT-RPCs. These implants present a clear advantage, as they can negate the need for a follow-up surgical procedure for implant removal. However, the marriage of this technology with CNT-RPCs is still in its early stages. Moreover, while the idea of enhancing bioactivity of CNT-RPCs is discussed, there hasn’t been a detailed and systematic approach to understanding how parameters like CNT content, dispersion, and orientation can impact it. For future research endeavors, there are clear pathways that can be pursued: i. Bioresorbable CNT-RPCs Development: This involves selecting the right bioresorbable polymer matrices and calibrating the CNT content and dispersion to strike a balance between mechanical strength and controlled degradation. ii. Thorough Biocompatibility Assessment: Before any clinical application, it is essential to evaluate these composites’ compatibility with biological systems both in lab settings (in vitro) and in live organisms (in vivo). iii. Structured Bioactivity Studies: Research should be designed to provide clear insights into how variations in composite formation can influence its bioactivity, allowing for more precise tailoring of CNT-RPCs for specific applications. Acknowledgements The author would like to thank Universiti Malaysia Pahang Al-Sultan Abdullah (UMPSA) for funding this study under grant number PGRS220368 from Postgraduate Research Grants Scheme (PRGS). This research would not have been possible without their support of academic innovation.

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Utilization of Coal Bottom Ash as Lightweight Aggregate in Concrete Production: A Review Mohammad I. Al Biajawi , Rahimah Embong , Adli Hilmi Azmi, and Norasyikin Ismail

Abstract Concrete is one of the building materials most in demand worldwide. Nevertheless, the increasing demand for concrete in the global construction sector requires an increase in the extraction of natural resources such as stone, sand, and various similar materials, resulting in the degradation of the natural environment. Consequently, the demand for construction aggregates has increased tremendously in the last decade. Currently, they are sourced from the main stone and sand deposits. Aggregates, one of the components of concrete, if indiscriminately extracted from primary resources, would cause an environmental problem. In particular, the large quantities of residual materials generated by coal combustion have underscored the need to develop viable reuse options for these high-volume pollutants. Coal Bottom Ash (CBA) is a type of industrial waste generated from coal combustion in thermal power plants. Due to their harmful impacts on the natural world and the health of the general population, the huge amounts of CBA waste generated annually by thermal power plants and improper disposal in landfills have caused major environmental problems. This review study aims to highlight the findings to date on using CBA as a lightweight aggregate in concrete production. Specifically, the effects of CBA as a lightweight aggregate on fresh and mechanical properties of concrete are discussed. Overall, concrete’s fresh and mechanical properties can be improved by using CBA as a lightweight aggregate in appropriate amounts. However, further studies are needed to assess the possibility of employing CBA as a lightweight aggregate in large quantities to produce high-performance concrete that is also durable. Keywords Coal bottom ash · Lightweight aggregate · Fresh properties · Mechanical properties · Sustainable development · Lightweight application

M. I. Al Biajawi · R. Embong (B) · A. H. Azmi Faculty of Civil Engineering Technology, Universiti Malaysia Pahang Al-Sultan Abdullah, Persiaran Tun Khalil Yaakob, 26300 Gambang, Pahang, Malaysia e-mail: [email protected] N. Ismail Faculty of Chemical and Process Engineering Technology, Universiti Malaysia Pahang Al-Sultan Abdullah, Persiaran Tun Khalil Yaakob, 26300 Gambang, Pahang, Malaysia © The Author(s), under exclusive license to Springer Nature Singapore Pte Ltd. 2024 R. Abd. Aziz et al. (eds.), Intelligent Manufacturing and Mechatronics, Springer Proceedings in Materials 40, https://doi.org/10.1007/978-981-99-9848-7_24

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1 Introduction Currently, worldwide growing populations, manufacturing, and, in certain areas, economic development are expanding. As a result of the above facts, the construction sector has grown significantly in recent decades [1, 2]. Furthermore, structural concrete is the preferred building material for most civil engineering projects [3]. It has high water resistance and can be made into a variety of different formats [4]. Currently, the production of cement requires up to 1.5 billion tonnes of cement, 12 billion tonnes of sand and rock, and 1 billion tonnes of water annually [5]. This demonstrates that the global production of concrete consumes vast quantities of raw materials and primary resources. Since huge amounts of concrete are produced every day, even a minimal reduction in the negative footprint per tonne of concrete has potential environmental benefits [6]. This minimization could be performed by evaluating the ingredients of the concrete, in particular the content of Portland cement (PC) [7, 8]. Consequently, increasing need for concrete in field of construction, which uses conventional weight aggregates such as gravel and granite, has dramatically reduced aggregates deposits, causing catastrophic environmental damage [9, 10]. Likewise, the focus on sustainable products has also increased recently. The increasing demand for environmental sustainability has led scientists to investigate the use of waste or recycled resources as alternative building materials [11–13]. Lightweight concrete, as specified in the standard EN 206–1, has a density of less than 2,000 kg/m3 . Lightweight concrete can be divided into six density classes, ranging from 800 kg/m3 with a classification of 200 kg to 1,600 kg/m3 with a classification of 2,000 kg [14]. However, lightweight aggregates derived from industrial wastes such as fly ash, slag, and CBA ash have paved the way for environmentally friendly materials [15]. Nevertheless, the unavailability of industrial processes in emerging and poor countries has not brought them much benefit. A significant portion of the cost can be saved if the mass of the structure is reduced [16]. Lightweight construction has been used in industrialized countries for some time and has proven to be cost effective. It served both structural safety and economic sustainability. The lighter the structure, the more flexible it is [17]. The most common method of producing lightweight products is through the use of lightweight aggregates. Lightweights are often divided into two categories: natural and artificial. The artificial aggregates are further divided into two categories: industrial wastes and altered naturally occurring substances [18]. The industrial wastes used as lightweights include pulverised shale, pulverised fuel ash, and CBA wastes. Shale, vermiculite, and perlite, are employed as lightweights in the building sector, along with other naturally occurring minerals that require further processing ( by applying high temperatures), are used as lightweight construction materials in the building sector [19]. Presently, industrial waste such CBA are being employed as lightweight aggregates in building due to increased environmental issues [20, 21]. Researchers have experimented with using CBA as lightweight aggregate to replace conventional concrete in the building of structural components and roads [22]. Accordingly, the primary purpose of this research is to provide a review of previous research that has addressed the fresh concrete properties,

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mechanical performance of CBA as lightweight-in concrete. This paper is intended to provide a summary of previous studies on the application of CBA as lightweight aggregates in the production of concrete.

2 Sustainable Development from Recycled CBA Nowadays, environmental sustainability is the most important issue on the globe. It meets the needs of the current community without threatening the potential of subsequent generations to achieve their goals [23]. It encompasses techniques that could provide highly effective means to benefit the environment and mankind [24]. The process of sustainable development entails a gradual change in the economic growth of the country [25, 26]. The primary goal of this expansion is to satisfy the wants and needs of society as a whole. In order to fulfill the fundamental requirements of human life, the desire for components like as food, clean air and water, clothing, a place to live, efficient and risk-free means of transportation for people and goods, efficient and safe methods of waste disposal, production and housing structures, and energy sources is constantly increasing [27]. The United Nations (UN) [28] established the comprehensive Agenda 21, which outlines actions to be implemented at the local, regional, and global levels by important groups, governments, and agencies in all areas where humans influence on the surrounding. The goal is to make wise decision between economic expansion, goals, and environmental sustainability. [29, 30]. The coal combustion industry emphasizes local and international policies, standards, and regulations, life cycle assessment (LCA), chain management, greenhouse gas emissions, novel mining methods, waste minimization, and energy generation as key factors in ensuring its long-term viability [31]. In fact, there has been a worldwide recognition that concrete plays an important role in the modern construction business, namely in infrastructure, development, and modernization for the expanding economy. In addition, it is essential to point out that the building materials sector remains one of the largest users of environmentally conscious products [32, 33]. For all these reasons, sustainable concrete is among the most crucial concerns being discussed in the concrete manufacturing sector around the world. The main objectives include reducing pollution and carbon dioxide (CO2 ), further reducing natural resources, making better use of recyclable materials, creating durable and effective structures, and designing the thermal resistance of concrete in a building lowers its electrical consumption. required to heat or cool the structure.

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3 Physical Properties and Chemical Compositions of CBA as Lightweight Aggregate To predict the performance of CBA as a concrete lightweight aggregate, its physical properties must be accurately characterized [34]. The most studied physical properties are its size, shape, structure, weight, and water absorption. In general, CBA has the appearance of a darker form of sand to gravel, but it has its own distinct physical and chemical properties [20, 21]. Furthermore, CBA is a granular substance consisting of particles ranging in size from fine to coarse. For use as a lightweight aggregate, it is usually sieved to a maximum particle size of 5 mm. In terms of physical properties, CBA particles are often irregularly shaped and are coarse-grained. The specific gravity of a substance is defined as the ratio of the density of that substance to the density of water [35, 36]. Studies recommend using CBA as a lightweight aggregate in both fine and coarse forms. The results show that CBA as a lightweight aggregate has different specific gravity values. The specific gravity of CBA varied between 1.79 and 2.61, depending on a variety of factors, such as the origin of the coal and the presence of voids in CBA. The reason for the differences in specific gravity is due to the coal used to generate electricity. In addition, the degree of combustion temperatures and pulverization affect the physical properties of CBA. According to previous studies [37, 38] were observed that the density of CBA ranged from 1200 to 1620 kg/m3 which is lower than density of conventional concrete without CBA. In another study, Muthusamy et al. [39] observed that the specific surface area of CBA was lower compared to that of fine aggregate replacement in the concrete mixture. In most studies, the water absorption of CBA varies. The percentage of water absorbed by porous CBA ranged from 2.8 to 24.80%. Overall, Lighter weight of CBA particles could be beneficial for lighting concrete, but considerable water absorption is required to serve as an internal curing water reservoir in concrete production. On the other hand, the chemical composition of CBA is illustrated in the table. X-ray fluorescence (XRF) analysis of CBA as lightweight aggregate shows that its major chemical compositions are silicates (SiO2 ), aluminates (Al2 O3 ), and iron oxide (Fe2 O3 ), along with modest amounts of calcium (Ca), magnesium (Mg) [40] as shown in table. According to the ASTM C618 [41] standard, there are two grades of CBA that are categorized as pozzolanic materials: Class F and Class C for CBA, respectively. To be classified as class F pozzolanic properties, the total content of SiO2 , Al2 O3 and Fe2 O3 must be more than 70%. Whereas to be classified as class C, it must contain 50% of the sum of the chemical composition of SiO2 + Al2 O3 + Fe2 O3 . The existence of silica in CBA could enhance pozzolanic reactivity, leading to an alkali-silica reaction and increasing the strength properties of the material. Numerous previous studies [42, 43] have investigated the mineralogical characterization of CBA as a lightweight aggregate for concrete production using X-ray diffraction and found small changes in the peak of crystalline structure, which could be due to the irregular shape of CBA. The inclusion of unburned carbon in CBA as a lightweight aggregate could improve the performance of concrete. Consequently, the use of CBA as a

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lightweight aggregate in the production of concrete could reduce the amount of tricalcium aluminate and dicalcium silicate while increasing the amount of tri-calcium silicate, which increases the durability of concrete against sulphate attack. Besides that, an increasing amount of CBA as lightweight aggregate into the concrete mixture can increase the silica content and improve the pozzolanic reactivity of the materials. The improvement in performance is due to the pozzolanic activity of calcium (OH)2 and silica during the hydration process, which leads to the formation of calcium silicate hydrate (C–S–H) [44, 45].

4 Fresh Concrete Properties of CBA as Lightweight Aggregate The workability of fresh concrete is determined by the slump test, which measures the settling of the concrete mix when the mold is lifted. In the case of lightweight concrete, the light mixture results in a lower slump because gravity affects the slump value [46]. The workability of concrete containing CBA as lightweight aggregate in concrete production is affected. On the other hand, the integration of CBA as a lightweight aggregate up to 30% leads to an increase in the workability of concrete production [47]. According to study by [48] was observed that the fresh properties (workability) of concrete with CBA as lightweight aggregate replacement in the range from 10%, to 100% in concrete production. The finding shows an increase in the workability flow by 16, 20, 26, 29, 32, 35, 30, and 24 mm, respectively. Despite their improved workability, CBA grains do not absorb all the water when the slump test is completed. The second reason for using CBA as a lightweight aggregate is that the consistency of the mix can be better maintained than with conventional fine aggregates in concrete mixes. In confirm, another previous study by [49] was evaluated the workability of CBA as lightweight aggregate with various replacement level (0, 25%, 50%, 75%, 100%) in the concrete mixture. The results were observed that the workability was increased with increased the replacement of CBA as lightweight aggregate expect 50% was decreased. The reason for decreased the slump values is due to increase the specific surface area in the ratio, also and uniform particles shape, and texture. On the contrary, several previous studies [40, 50] have observed the impact of CBA as lightweight aggregate of workability in the concrete mixture. The results showed that workability was decreased as CBA as lightweight aggregate increased in the concrete production. The reduction due to higher CBA content that lead to higher water demand and porous particles led to decrease the values compared to control workability without CBA in concrete mixtures. According to study by [51] was found the workability of CBA as lightweight aggregate decreased for 0, 25, 50, 75, 100 the reduction by 110, 90, 95, 100, 40 mm respectively, compared to concrete mixture without CBA. The redaction due to inter particles’ friction between aggregate particles, which was generated from the increased CBA and the water demand for

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CBA was decreased. In confirm with another study by [52] was reported that the workability was increased as CBA lightweight aggregate increased in the concrete mixture. In general, the workability (slump values) of concrete containing CBA as a lightweight aggregate was reduced in some experiments and improved in others. This was due to a number of reasons, including the fact that the CBA particles absorbed the moisture content of the mix, as well as differences in the size, quantity, and water content of the CBA during concrete production.

5 Mechanical Concrete Properties of CBA as Lightweight Aggregate In this section, previous studies on flexural strength, compressive strength, modulus of elasticity, and split tensile strength are discussed where CBA was used as a lightweight aggregate in the production of concrete. The effects of CBA as a lightweight aggregate on the mechanical performance of concrete. For instance, In accordance with a study by [49] the effect of CBA as a lightweight aggregate with replacement ratios of (0, 25, 50, 75, 100%) after 7, 28, and 90 days of curing on the mechanical properties of concrete mix was investigated. The results showed that the strength properties improved with increasing age of curing. The strength properties increased gradually and also showed improvement in strength properties with 50% replacement of CBA as lightweight in the concrete mix. On the 28th day of curing, compressive strength values of 39 MPa, 43 MPa, 41 MPa, 33 MPa, and 31 MPa were obtained, with 0, 25, 50, 75, and 100% replacement of CBA as lightweight aggregate, respectively. For the modulus of elasticity, values of 26 MPa, 18 MPa, 16 MPa, 14 MPa, and 11 MPa were determined, with the CBA replaced as lightweight aggregate at a ratio of 0, 25, 50, 75, and 100%, respectively. The reduction in other replacement ratios is due to the lower density of lightweight aggregates compared to conventional aggregates. previous studies [53] have shown that the optimal use of CBA as a lightweight aggregate in proportions up to 20% increases the strength properties of concrete mixtures. The improvement results from the higher fineness of CBA as a lightweight aggregate compared to conventional fine aggregate. The inclusion of a sufficient amount of CBA is also influenced by this significant characteristic. According to another study by [54] demonstrated a reduction in all replacement ratios (10, 20, 30, and 40%) for CBA as lightweight aggregate in concrete mixture. The decrease is due to CBA as lightweight aggregates are more porous and absorb more mixed water than fine aggregates in concrete mixes, resulting in a harder mix. Another study by [55] was found the strength properties of CBA as lightweight with replacement ratios (0, 25, 50, 75, 100%) lead to decreased at 28 day of curing compared to normal concrete. Reduction due to lower strength of CBA results in a greater number of failures; longitudinal fracture lengthens. However, normal concrete with fine aggregate deteriorates more at the contact between the aggregate and the cement matrix.

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In addition, several previous studies [56, 57] observed that the strength properties of CBA as lightweight aggregate increased compared to conventional concrete. For instance, study by [58] investigated the influence of CBA as light aggregates with an alternative ratio of (12.5, 25%) on the mechanical properties of the concrete mixture. The results showed that the compressive strength increased at 28 and 56 days for all replacement ratios, while it decreased at 1 and 7 days in the early ages compared to normal concrete specimens. The splitting tensile strength of CBA as a lightweight aggregate was decreased at all replacement ratios and at all ages of curing compared to normal concrete. The reduction was due to the higher water absorption in the replacement specimens. Overall, the strength properties of CBA as a lightweight aggregate were improved at a certain replacement ratio. Most studies have shown that the suitable replacement ratio is up to 20%. The increase in strength is due to several factors, such as the fineness of CBA as a lightweight aggregate compared to fine aggregates, and the incorporation of an appropriate amount of CBA.

6 Conclusion CBA as a lightweight aggregate form has excellent potential for use as a construction material. Because it possesses physical properties and chemical compositions similar to coarse and fine aggregates, it can also be used as a building material in addition to cement. CBA is a viable waste resource to produce building materials, particularly lightweight aggregates for the manufacturing of concrete. Due to the higher hardness and smaller particle size of this waste material, it is suitable as a fine partial aggregate to produce concrete or mortar. The results show that combining the right proportion of CBA as a lightweight aggregate effectively improves the mechanical properties and acid attack, which requires further exploration on other durability characteristics Exploring alternative innovative mixing approaches could enable the use of a larger amount of CBA as a lightweight aggregate in the production of a variety of specific forms of concrete, such as fiber-reinforced, polymer, architectural concrete, and numerous other types. To expand the use of CBA in the construction sector, further studies need to be conducted on the material’s potential as a lightweight aggregate, its durability, and its use in engineered building materials. Furthermore, the use of CBA as a lightweight aggregate would reduce the amount of primary resources needed to produce concrete and limit the amount of CBA that is landfilled as a hazard to the environment. Acknowledgements The authors would like to thank the Ministry of Higher Education for providing financial support under Fundamental Research Grant Scheme (FRGS) No. (FRGS/1/ 2022/TK01/UMP/02/5 (university reference RDU(220112) and Universiti Malaysia Pahang ALSultan Abdullah (UMPSA) for laboratories facilities as well as additional support under internal grant No. RDU 223313.

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Role of Nanomaterials in Improving Pozzolanic Properties of Blended Cement: A Review Haneen Abdel-Jabbar , Rahimah Embong , and Mohammad I. AlBiajawi

Abstract Nanoscience and nanotechnology are the most commonly used keywords in today’s academic and professional circles. Nanomaterials have emerged as a significant technological advancement, showcasing exceptional properties in various fields such as mechanical, electrical, and thermal applications. The cement industry has also witnessed the integration of nanomaterials due to their remarkable characteristics. This review article investigates the potential of utilizing nanoparticles as substitutes for cement, benefiting from their advantageous characteristics such as small particle size, high reactivity, and large surface area. Furthermore, this paper provides a summary of prior research studies that have analyzed the impact of nanoparticles on various concrete properties, including workability, mechanical strength, and durability. The insights gained from this review will significantly enhance our understanding of the potential applications and advantages of nanomaterials in the cement industry, thus paving the path for future advancements in cement technology. Keywords Nano · Durability · Pozzolanic · Hydration · Mortar · Environment

1 Introduction Nanotechnology has a significant influence in the construction field and has developed long-lasting, high-performance building materials. The fundamental qualities of conventional building materials have been improved mainly due to the unique scientific advances in the field of nanotechnology, which have made it possible to utilize a variety of nanoscale materials with diverse features [1]. Nanotechnology has several applications in various industries, and the concrete industry is no exception. However, most nanotechnology applications in the concrete industry are still limited to laboratory research [2]. H. Abdel-Jabbar · R. Embong (B) · M. I. AlBiajawi Faculty of Civil Engineering Technology, Universiti Malaysia Pahang Al-Sultan Abdullah, Persiaran Tun Khalil Yaakob, 26300 Gambang, Pahang, Malaysia e-mail: [email protected] © The Author(s), under exclusive license to Springer Nature Singapore Pte Ltd. 2024 R. Abd. Aziz et al. (eds.), Intelligent Manufacturing and Mechatronics, Springer Proceedings in Materials 40, https://doi.org/10.1007/978-981-99-9848-7_25

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Nanotechnology has emerged as a highly effective approach for addressing various challenges associated with concrete components. By serving as strength enhancers, nanomaterials have demonstrated the ability to significantly improve the strength of concrete without the need for additional cement. As a result, the overall volume of concrete required for a given construction project can be reduced, this implies that when employed as cement reducers, nanomaterials can effectively decrease the amount of cement needed to achieve the desired concrete strength [3, 4]. Nanomaterials approximately constitute 70% of the total volume of a structure, highlighting their significant contribution to the overall construction process [4, 5]. Typically, concrete is composed of approximately 12% cement and 80% aggregate by mass. Concrete usage on a large-scale result in significant consumption of natural resources [6, 7]. Consequently, this extensive demand on concrete leads to environmental concerns and potential problems [8]. For example, Malaysia’s production of cement reached 1214 thousand tons in May 2022 [2, 9]. To mitigate the environmental impact, there is a need to find alternative materials that can give the properties of cement when combined with other raw materials to produce concrete [10, 11]. Pozzolan is defined as a substance containing silica and alumina, which possesses inherent cementitious properties [11, 12]. When it comes in contact with moisture it reacts with calcium hydroxide at normal temperatures, resulting in the formation of compounds that exhibit strong cement-like characteristics [13]. The involvement of secondary reactions is of utmost importance in the utilization of pozzolanic materials, as these reactions take place after the initial hydration process of cement. These reactions involve the interaction between pozzolans and free calcium hydroxide to produce the calcium silicate hydrates (C–S–H) phase, which greatly enhances the strength of concrete [14, 15]. This review paper provides an overview of the recent developments in the utilization of nanomaterials as pozzolanic additives, including the types of nanomaterials used, and their effects on the properties of cementitious materials. The challenges and prospects of utilizing nanomaterials as pozzolanic additives are discussed, highlighting the opportunities for further research and development in this field.

2 Nanomaterials Production Nanoparticles are materials with sizes smaller than 100nm. They can take the form of fibers, powders, or liquids. The 7th International Conference on Nanotechnologies suggests several common types of nanomaterials, including nonporous structures, nanoparticles, nanotubes, nanofibers, nano-dispersions (colloids), nanostructured surfaces, films, as well as nanocrystals and nanoclusters [16]. Two basic strategies, top-down and bottom-up, are examples of the numerous procedures that have been suggested to produce nanomaterials. Figure 1. illustrates the top-down method, which is characterized by the development of nano products from materials of regular size through shrinking the original material’s dimensions utilizing specialized size reduction procedures beginning at the molecular level [17].

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Fig. 1 Strategies for nanomaterials production

The cost of nanomaterials can vary depending on different factors, one of the primary influences on nanomaterial pricing is the method of production and modification employed by the suppliers. Additionally, the level of purity is another significant factor that can impact the cost of nanomaterials, as purity increases, the price tends to rise significantly [18].

3 Role of Nanomaterials with Blended Cement Recently, many studies have been conducted on different materials to study the possibility of using them as an alternative to cement in concrete. Tests were conducted on fly ash, a by-product of coal combustion and one of the most promising materials that can be used as an alternative to cement. Also, rice husk biochar which is derived from agricultural waste has been studied as a sustainable cement material. Studies have also been conducted on volcanic rocks, such as silica fume, which have high potency and can contribute to improving the performance of concrete. Moreover, the use of biochar derived from wood waste represents another sustainable option for enhancing the properties of concrete. Therefore, by incorporating these complementary materials, the construction industry can reduce its reliance on traditional cement while achieving comparable or enhanced concrete properties [19, 20]. The physicochemical properties of nanomaterials, including their high melting point, exceptional strength-to-weight ratio, electrical and thermal conductivity, catalytic activity, light absorption, and dispersion, have led to their widespread recognition in various technological advancements. Using nanomaterials in concrete offers a means to enhance its performance by decreasing the porosity of cement. Nanoparticles play a crucial role in forming a denser interfacial transition zone within the concrete matrix. Furthermore, when nanoparticles are incorporated into the cement mixture, they contribute to reinforcing the material, yielding high-strength, durable, and long-lasting concrete structures [21]. The addition of nanoparticles in cementitious systems can lead to an increase in water absorption due to their expansive surface area, this phenomenon, in turn, reduces the amount of free water available within the mixture, ultimately impacting

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its workability. It is crucial to consider this aspect when incorporating nanoparticles into cementitious systems, as reducing workability may be challenged in terms of application and forming the desired structures. Proper adjustments in the mix design, such as; optimizing the water-to-cement ratio, or adding superplasticizers, may be necessary to maintain an appropriate level of workability [22]. Concrete mix performance can be improved, by adding Nanomaterials such as nano-silica (SiO2 ), titanium oxide (TiO2 ), nano-iron (Fe2 O3 ), and alumina oxide (Al2 O3 ). Integrating concrete nanomaterials enhances pore structures, mechanical properties, and longevity of concrete [23]. Nano SiO2 and nano TiO2 are two widely used nanomaterials in various applications, and nano-TiO2 specifically offers notable advantages in cementitious systems. One of its key benefits is its ability to eliminate residual water content, thus effectively reducing the emission of pollutant gases that may occur during the hydration process. On the other hand, when Silica (SiO2 ) is added to the concrete mix which is one of the main components of cement, the setting time, water permeability, and mechanical properties are all improved. Additionally, the inclusion of nano-SiO2 improves resistance to chemical solvents, meanwhile, the temperature at which the geo-polymer will start to harden increases as a result of the addition of Nano silica particles [23, 24]. Also, when nano-iron oxide (Fe2 O3 ) is mixed with concrete, it produces compacted, solid structures with less porosity than traditional concrete. Nano-Fe2 O3 can be added to materials to increase their compressive strength, torsional strength, fracture resistance, and resistance to water penetration. The calcium ferrite hydrate (C–F–H) phase, which is produced when iron oxide nanoparticles are added, may have a stronger lubricating effect due to pozzolanic action. On the other hand, with the addition of Nano-Al2 O3 , concrete becomes stronger, better able to withstand thermal stress, and has a greater elastic modulus [23]. Table 1 shows the used nanomaterials. Furthermore, when concrete is incorporated with nanomaterials and subjected to high temperatures, it exhibits improved compressive and flexural strength, particularly up to a temperature threshold of 250 °C. This demonstrates the potential of using nanomaterials to enhance the thermal performance and mechanical properties of concrete under elevated temperature conditions [24]. In conclusion, incorporating Nanoparticles into concrete has a profound positive influence on its performance and durability. Nanomaterials, characterized by Table 1 Nanomaterials used Name of nano particles

Area

Major application

Nano Silica (SiO3 )

Concrete

Reinforcement in mechanical strength, rapid hydration

Nano-Titanium (TiO2 )

Concrete

Increased degree of hydration, Self-cleaning

Nano-Aluminum (Al2 O3 )

Asphalt, concrete

Increased serviceability

Nano-Iron (Fe2 O3 )

Concrete

Increased compressive strength, Abrasion-resistant

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their small particle size and expanded surface area, offer numerous advantages that contribute to the enhancement of various properties, such as; flexural strength, split tensile strength, compressive strength, abrasion resistance, water permeability, and pore structure, by reinforcing the concrete matrix, nanoparticles improve its mechanical properties and fortify its resistance against external forces. Furthermore, they decrease water permeability, enhance the pore structure, and enhance the compactness of the concrete, resulting in improved durability and heightened resilience against environmental factors.

4 Nanomaterials as Pozzolanic The construction industry, in particular, has witnessed the promising potential of nanomaterials as pozzolanic additives in cementitious materials. Pozzolanic materials, when combined with calcium hydroxide, undergo chemical reactions to form additional cementitious compounds, resulting in enhanced strength, durability, and overall performance of concrete. By incorporating nanomaterials as pozzolanic additives, there is an opportunity to improve the properties of cementitious materials [15]. A study conducted by Huigang Xiao et al. focused on investigating the effects of both pozzolanic and non-pozzolanic nanomaterials on cement-based materials. The study revealed significant improvements in various properties when pozzolanic nanomaterials, including nano-silica and nano-alumina, were incorporated. These materials demonstrated a positive impact on compressive strength, reduction in porosity, and enhanced microstructural characteristics of the blended materials. The pozzolanic nanomaterials reacted with calcium hydroxide, leading to the formation of additional hydration products, thereby promoting the development of strength and enhancing the durability of the cement-based materials. Furthermore, the inclusion of non-pozzolanic nanomaterials, such as carbon nanotubes and graphene, resulted in improved tensile and flexural properties of cement-based materials. The study’s findings underscore the potential of both pozzolanic and non-pozzolanic nanomaterials to significantly enhance the performance and properties of cement-based materials, paving the way for the development of more robust and durable construction materials [25].

5 Fresh Concrete Properties Fresh concrete exhibits several significant properties that play a crucial role in its workability and handling during construction. It is influenced by factors such as water content, aggregate properties, and the use of admixtures. Consistency which refers to the fluidity or stiffness of fresh concrete is another important property. Setting time is a key characteristic that determines the transition of concrete from a

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plastic state to a hardened state. Due to their large surface area and water absorption capacity, nanoparticles can affect the workability of concrete by reducing available water content. A decrease in workability is observed when nanoparticles are incorporated. However, in certain applications, such as; casting pavement and shotcrete, the inclusion of nanoparticles can enhance cohesiveness and prevent segregation. Careful consideration and adjustment of the concrete mixture are necessary to strike a balance between workability and the benefits provided by nanoparticles [26]. Replacement of 3% and 4% nano silica (SiO3 ) by cement weight, correspond to a decrease in 58%, 57.2%, and 60% flow-ability values, respectively [27, 28]. While the replacement of 5% nano titanium (TiO2 ) results in a 31.2% reduction in flowability [29]. Partial replacement of 2% nano-aluminum (Al2 O3 ) by weight leads to a 70% reduction [30]. Also, the replacement of 2% nano iron (Fe3 O4 ) results in a 60% reduction in flowability [31]. Depending on the type and concentration of the nanomaterials used, they can either accelerate or retard the setting process. Nanoparticles with high reactivity can promote faster hydration and lead to a shorter setting time. Conversely, certain nanomaterials may impede water movement and delay hydration, resulting in a longer setting time. Replacement of 4% and 3% Nano silica (SiO3 ) correspond to the reduction of 12.5% and 60% of setting time value [27, 32]. Replacement of 5% nano titanium (TiO2 ) results in a 45% reduction in setting time [5]. Partial replacement of 2% and 3% nano-aluminum (Al2 O3 ) leads to a 55% and 7% reduction in setting time [30, 32]while the replacement of 2% nano iron results in a 55% reduction in setting time [31]. Table 2 shows a summary of the impact of different nanomaterials with blended cement. Table 2 Impact of nanomaterials Name of Nano particles

Percentage %

Finding

Ref

Nano Silica (SiO3 )

3

Decrease in flow-ability

[27]

4

Decrease in flow-ability and setting time

[4]

2

Decrease in setting time

[3]

Nano-Titanium (TiO2 )

5

Decrease in setting time and flow-ability

[5, 23]

Nano-Aluminum (Al2 O3 )

2

Decrease in flow-ability and setting time

[30]

3

Decrease in setting time

[32]

2

Decrease in workability and setting time

[31]

Nano-Iron (Fe3 O4 )

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6 Hardened Concrete Properties The mechanical characteristics of hardened concrete, including compressive strength and splitting tensile strength, play a crucial role in determining its durability and robustness. Numerous tests are conducted to evaluate these properties. A study conducted by Hongjian Du et al. [33, 34] focused on exploring the utilization of nano-silica in concrete. The researchers discovered that increasing the nano-silica percentage contributed to enhanced durability in comparison to previous studies. Conversely, the addition of nano-silica particles caused a densifying effect on the concrete’s microstructure. This densification resulted in the formation of additional internal micro-cracks, as observed in a separate study by Utsev et al. [21]. These micro-cracks aid in energy dissipation and can improve the overall toughness and durability of the concrete. Furthermore, Zhang et al.‘s research indicated that incorporating nano-silica into cement and slag mixtures accelerated the hydration process and reduced the dormant period implying that the presence of nano-silica particles facilitated the initial stages of cement hydration, leading to expedited strength development and an overall enhancement in the mechanical properties of the concrete. A study conducted by Nazari et al. investigated the effects of incorporating nano-TiO2 particles into concrete, which resulted in higher split tensile and flexural strength compared to concrete without these particles [35]. The study found that cement could be partially replaced with nano-TiO2 particles up to a maximum limit of 2.0%, with the optimal replacement level being 1.0%. However, to further enhance the split tensile strength, the study suggested using more suitable reinforcements, such as needle-type nanoparticles. Similarly, the addition of nano-Al2 O3 particles significantly increased the compressive strength of concrete, as observed by Nazari et al. [35]. Overall, the incorporation of nanomaterials such as nano-silica, nano-TiO2 , and nano-Al2 O3 in concrete has the potential to enhance its mechanical properties, durability, and overall performance. These findings highlight the positive impact of nanomaterials in improving the microstructure and properties of mortars, offering promising opportunities for the development of high-performance construction materials.

7 Application of Nanomaterials The emergence of nanomaterials has revolutionized civil engineering, particularly in the concrete industry. Nanomaterials offer exceptional properties and superior performance compared to bulk materials. By incorporating nanomaterials into concrete, engineers have been able to enhance its strength and durability, this led to the development of eco-friendly or green concrete, which maintains its strength while reducing environmental impact. The use of nanomaterials has opened up new possibilities for

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creating stronger, more durable, and sustainable concrete structures, contributing to the advancement of the construction industry [36]. Nanotechnology has made significant advancements in the development of specialized coatings for construction materials. For example, titanium dioxide (TiO2 ) coatings on glass surfaces provide sterilization and resistance to fouling, thanks to their catalytic properties and hydrophilic nature. Other specialized coatings, such as anti-graffiti coatings, temperature control coatings, and energy-saving coatings, have also been developed using nanomaterials [21]. In the realm of steel structures, the incorporation of copper nanoparticles within the grain boundaries of low-carbon, high-performance steel has led to enhanced properties, including improved corrosion resistance and weldability. Nanomaterials applications in the chemical industry as substitutes for environmentally harmful chemicals, and ongoing research and development in nanotechnology hold promise in addressing climate change and energy-related challenges [37]. However, it is important to note that while some commercially available “Nano-consumer products” claim environmental benefits, their primary objective may not solely be environmental conservation. Nonetheless, the utilization of nanomaterials in various applications, such as self-cleaning surfaces, contributes to energy and water conservation by reducing the need for extensive cleaning and minimizing the use of cleaning chemicals [38]. In conclusion, nanomaterials have significantly impacted the field of engineering, particularly in civil engineering, by improving the properties and performance of construction materials such as concrete and steel [39].

8 Conclusion In this review, the utilization of nanoparticle materials in blended cement was investigated, focusing on properties related to the fresh state, and mechanical strength. Incorporating nanoparticles, with their smaller particle sizes and larger surface areas compared to cement, was found to increase the water content needed for workability, which negatively affected the mixture’s workability. However, higher replacement ratios of nanoparticles improved compressive strength by enhancing hydration and forming a compact microstructure with well-dispersed nanoparticles. Different nanoparticles also increased flexural strength to an optimal level. Furthermore, nanoparticle incorporation reduced water absorption, as their small size filled the pores in hardened cement paste, resulting in a denser and less permeable structure. Overall, nanotechnology is expected to play a significant role in advancing cement and concrete technology, expanding possibilities for both conventional and unconventional cement materials in construction. However, the widespread adoption of nanotechnology faces obstacles. The high production cost of nanomaterials requires specialized equipment and advanced technologies. Addressing potential health and environmental risks associated with nanomaterials necessitates extensive research and regulatory frameworks. Scaling up and integrating nanotechnology into existing systems pose practical challenges, while the lack of standardized testing protocols

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and regulations specific to nanotechnology further complicates its implementation. Public perception and acceptance are vital, requiring transparent dialogue to address concerns and build trust. Acknowledgements The authors would like to thank Ministry of Higher Education (MOHE) or Kementerian Pendidikan Tinggi Malaysia for providing financial support under fundamental research grant Scheme (FRGS) No. (FRGS/1/2022/TK01/UMP/02/5 (university reference RDU(220112) and Universiti Malaysia Pahang AL-Sultan Abdullah (UMPSA) for laboratories facilities as well as additional support under internal grant No. RDU 223313.

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A Comparative Study of Conventional and Hybrid Nanofluids Performance in Machining Processes Norasilah Karumdin, Ahmad Shahir Jamaludin, Mohamad Rusydi Mohamad Yasin, Nurul Nadia Nor Hamran, and Mohd Amran Md Ali

Abstract This research provides an extensive review of the use of conventional and hybrid nanofluids in various machining processes. Due to their enhanced thermal characteristics, nanofluids, which consist of colloidal suspensions of nanoparticles in a base fluid, have become an increasingly popular field of study. These features make nanofluids an excellent alternative for cooling and lubricating during machining operations, improving both the efficiency and quality of the machined components. The paper compares conventional and hybrid nanofluid performance in several machining processes, examines their environmental and economic consequences, and highlights research gaps and future direction. Despite nanofluids’ promising performance, various problems and constraints remain, including the stability of the nanoparticle dispersion, possible health and environmental hazards, and the high costs of nanofluid production. The study discovers that overcoming these problems via thorough and comparative investigations, as well as a greater knowledge of the mechanisms behind nanofluids’ performance in machining, would be critical to achieving their full potential. Keywords Conventional nanofluids · Hybrid nanofluids · Machining processes · Thermal properties · Nanoparticle dispersion

N. Karumdin · A. S. Jamaludin (B) · M. R. Mohamad Yasin · N. N. Nor Hamran Faculty of Manufacturing and Mechatronic Engineering Technology, Universiti Malaysia Pahang Al-Sultan Abdullah, 26600 Pekan, Pahang, Malaysia e-mail: [email protected] M. A. Md Ali Faculty of Manufacturing Engineering, Universiti Teknikal Malaysia Melaka, Hang Tuah Jaya, Durian Tunggal, 76100 Melaka, Malaysia © The Author(s), under exclusive license to Springer Nature Singapore Pte Ltd. 2024 R. Abd. Aziz et al. (eds.), Intelligent Manufacturing and Mechatronics, Springer Proceedings in Materials 40, https://doi.org/10.1007/978-981-99-9848-7_26

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1 Introduction to Nanofluids in Machining Processes Nanofluids have recently gained considerable attention as a noteworthy subject of investigation within the area of machining processes. The fluids under consideration in this study are composed of base fluids combined with nanoparticles. These fluids possess improved thermal properties, rendering them highly suitable for the purposes of cooling and lubrication in machining operations [1–4]. Previous studies have demonstrated that the utilisation of nanofluids in machining operations, specifically grinding and milling, yields notable enhancements in process efficiency. This improvement is attributed to the reduction in heat generation and friction, resulting in the enhancement of machined part quality and the prolongation of tool lifespan [1– 15]. In addition, the utilization of nanofluids in machining operations exhibits environmental friendliness, thus encouraging the adoption of sustainable manufacturing methodologies [3, 16–25]. Notwithstanding these benefits, the untapped potential of nanofluids in machining operations remains to be comprehensively investigated, thus warranting additional scholarly inquiry in this domain. Conventional nanofluids refer to engineered colloidal suspensions consisting of nanoparticles dispersed within a base fluid. The nanoparticles, which are commonly composed of metals, oxides, or carbon nanotubes, are evenly distributed within a foundational fluid, such as water, oil, or ethylene glycol. The nanoparticles possess distinct characteristics, including a notable surface area-to-volume ratio and improved thermal conductivity, which contribute to the nanofluids’ exceptional thermal properties. Consequently, these nanofluids have proven to be highly efficient in facilitating heat transfer in various applications [1–12]. Conventional nanofluids have been applied in various machining processes, including grinding, milling, and turning. In these applications, nanofluids serve as coolants and lubricants, reducing heat generation and friction at the cutting zone, thereby improving the efficiency of the machining process and the quality of the machined parts. For instance, in a previous study [1], water-based nanofluids were used in ultrasonic vibration-assisted grinding, resulting in a significant reduction in grinding forces and surface roughness (Fig. 1). Another previous study had also [3] reported improved cutting force performance in the end milling process of Aluminum Alloy 6061-T6 using a tri-hybrid nanofluid. Despite the promising performance of conventional nanofluids in machining processes, several challenges and limitations exist. One of the main challenges is the stability of the nanoparticle dispersion in the base fluid. Over time, it has been observed that nanoparticles have a tendency to agglomerate and settle, leading to potential implications for the performance of the nanofluid [1–12]. The main aim of this review is to offer a thorough examination of the utilization of conventional and hybrid nanofluids in various machining procedures. This review will examine the efficacy of nanofluids in different machining operations, analyzing their benefits and drawbacks, as well as the challenges linked to their application. Additionally, it will compare the performance of conventional and hybrid nanofluids in machining processes and discuss the environmental and economic implications associated with their utilization.

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Fig. 1 Microscopic representations of three distinct nanoparticles, Al2 O3 , multiwall carbon nanotube (MWCNT), and graphite (left to right) [1]

2 Comparative Analysis on Hybrid Nanofluids Application Hybrid nanofluids have garnered considerable attention as a viable solution in diverse machining applications due to their composition, which comprises multiple types of nanoparticles dispersed within a base fluid. The motivation behind the development of these sophisticated nanofluids stems from the aspiration to exploit the advantageous characteristics of various nanoparticles, consequently augmenting the overall efficacy of the nanofluid. An example of a hybrid nanofluid is one that incorporates both metal and oxide nanoparticles, thereby leveraging the superior thermal conductivity of metal nanoparticles and the enhanced stability of oxide nanoparticles [1–12]. Numerous studies have provided evidence of the enhanced efficacy of hybrid nanofluids in the context of machining operations. In their study, a hybrid nanofluid composed of Al2 O3 and graphite had been employed as a coolant during ultrasonic vibration-assisted grinding [1]. The utilisation of this nanofluid led to a reduction in grinding forces and specific energy when compared to alternative coolant options. In a separate investigation, previous researcher had documented enhanced cutting force efficacy during the end milling procedure of Aluminium Alloy 6061-T6 through the utilisation of a tri-hybrid SiO2 -Al2 O3 -ZrO2 nanofluid. The results of this study indicate that hybrid nanofluids may provide enhanced cooling and lubrication capabilities in machining operations when compared to conventional nanofluids. Both conventional and hybrid nanofluids have demonstrated promising outcomes in diverse machining processes. However, hybrid nanofluids tend to display superior performance as a result of their distinctive amalgamation of various nanoparticle types. In the context of ultrasonic vibration-assisted grinding, the utilisation of a hybrid Al2 O3 /graphite nanofluid has been found to yield reduced grinding forces and specific energy when compared to alternative coolants [1, 9, 19]. Likewise, the implementation of a tri-hybrid SiO2 -Al2 O3 -ZrO2 nanofluid has shown enhanced cutting force performance during the end milling process of Aluminium Alloy 6061-T6 [3]. The findings of these studies indicate that the utilisation of hybrid nanofluids has the potential to provide improved cooling and lubrication capabilities in machining operations when compared to conventional nanofluids. However, the use of nanofluids

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Fig. 2 Environmental impact comparison for various cutting fluid [21]

in machining operations also presents environmental and economic consequences. On the environmental front, nanofluids, particularly those based on biodegradable and non-toxic materials, can contribute to more sustainable machining practices, as shown in Fig. 2 [3, 21]. However, potential health and environmental risks associated with the use of nanoparticles remain a concern. Economically, while the use of nanofluids can improve the efficiency of machining processes and extend tool life, the production of nanofluids, especially hybrid nanofluids, can be more complex and costly compared to conventional fluids [23]. Therefore, a careful cost–benefit analysis is necessary when considering the adoption of nanofluids in machining processes.

3 Current Trend Related to Conventional and Hybrid Nanofluids Application in Various Machining Processes Table 1 provides a comprehensive overview of the current trends in the application of Conventional and Hybrid Nanofluids in various machining processes. It is organized based on related studies and their experimental conditions, summarizing the key findings of each. The studies are categorized by various parameters such as the type of workpiece used, the type of nanofluid applied, the material of the nanofluid, the type of cutting tool used, and the specific nanofluid material. The key understanding that can be drawn from the table are as follows: ● Nanofluid Minimum Quantity Lubrication (MQL) generally outperforms dry machining and conventional MQL in terms of surface roughness, tool wear, and cutting temperature, particularly when the workpiece is Inconel 718 or Ti–6Al–4 V [26, 27, 29, 35, 47, 48].

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Table 1 Comprehensive overview of the current trends in the application of Conventional and Hybrid Nanofluids in various machining processes Similarity in Experimental Conditions

Summary of the key findings

Workpiece: Inconel 718

Nanofluid MQL generally performs better than dry machining and conventional MQL, resulting in improvements in surface roughness, tool wear, and cutting temperature [26, 27, 29, 35, 47, 48]

Nanofluid Type: Hybrid

Hybrid nanofluids show significant improvements in cutting forces, heat dissipation, surface roughness, and tool wear compared to conventional fluids. They are also environmentally friendly and can potentially replace conventional fluids [13, 28, 32–34, 36–40, 43, 45, 46, 51, 53]

Nanofluid Material: Contains Carbon Nanotubes or Graphene

These nanofluids perform better than dry machining and conventional MQL, resulting in improvements in machined surface roughness and tool flank wear [26, 29, 35, 47]

Cutting Tool: Tungsten Carbide

Tungsten carbide tools, when used with hybrid nanofluids, result in significant reduction in surface roughness, cutting temperature, and cutting forces. They also improve heat dissipation [13, 28, 34, 36–38, 46, 51, 53]

Nanofluid Material: SiO2 -Al2 O3 -ZrO2

The tri-hybrid nanofluid application is environmentally safe, thus promoting sustainable manufacturing compared to the conventional working fluid. The responses studied were reduced significantly when tri-hybrid nanoparticles present at the cutting interface with higher MQL flow rate and concentration [3, 42]

Workpiece: Ti–6Al–4V

Nanofluid MQL performs better than traditional dry cutting, resulting in significant reductions in tool-tip temperature, cutting force, depth of flank wear, and product surface roughness [27, 29, 31, 35, 47]

Nanofluid Material: Contains Carbon Nanotubes

Nanofluid MQL performs better than dry machining and conventional MQL, resulting in improvements in machined surface roughness and tool flank wear [26, 27, 29, 30, 44]

Nanofluid Material: Contains Multiple Different Nanoparticles

Hybrid nanofluids containing multiple different nanoparticles show significant improvements in cutting forces, heat dissipation, surface roughness, and tool wear compared to conventional fluids. They are also environmentally friendly and can potentially replace conventional fluids [28, 38, 41, 46, 53, 54] (continued)

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Table 1 (continued) Similarity in Experimental Conditions

Summary of the key findings

Cutting Tool: Uncoated WC–Co

Uncoated WC–Co tools, when used with nanofluids, perform better than dry machining and conventional MQL, resulting in improvements in machined surface roughness and tool flank wear [26, 29, 35, 47, 48]

Nanofluid Material: Contains Al2 O3

Hybrid nanofluids containing Al2 O3 show significant improvements in cutting forces, heat dissipation, surface roughness, and tool wear compared to conventional fluids. They are also environmentally friendly and can potentially replace conventional fluids [28, 38, 41, 46, 53, 54]

● Nanofluids containing carbon nanotubes or graphene perform better than dry machining and conventional MQL, resulting in improvements in machined surface roughness and tool flank wear [26, 27, 29, 30, 44]. ● Hybrid nanofluids, particularly those containing multiple different nanoparticles or Al2O3, show significant improvements in cutting forces, heat dissipation, surface roughness, and tool wear compared to conventional fluids. They are also environmentally friendly and can potentially replace conventional fluids [3, 42]. ● Tungsten carbide tools and uncoated WC–Co tools, when used with hybrid nanofluids, result in significant reduction in surface roughness, cutting temperature, and cutting forces. They also improve heat dissipation [26, 29, 35, 47–56]. ● The application of tri-hybrid nanofluid (SiO2 -Al2 O3 -ZrO2 ) is environmentally safe, promoting sustainable manufacturing compared to the conventional working fluid. The responses studied were reduced significantly when tri-hybrid nanoparticles were present at the cutting interface with higher MQL flow rate and concentration [3, 42].

4 Research Gaps and Future Directions The application of nanofluids, particularly hybrid nanofluids, in machining processes has demonstrated significant advantages over conventional fluids and dry machining. These benefits include improved surface roughness, reduced tool wear, and enhanced heat dissipation. In addition, it should be noted that specific types of nanofluids possess advantageous environmental characteristics, thereby establishing them as a potentially viable remedy for the implementation of sustainable manufacturing methodologies. Despite the significant advancements in the utilisation of conventional and hybrid nanofluids in machining processes, there are still several areas of research that remain unexplored. One significant limitation in the existing literature is the lack of comprehensive and comparative investigations pertaining to the

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performance evaluation of different types of nanofluids in diverse machining operations. The prevailing body of research predominantly concentrates on a singular category of nanofluid and a specific machining technique, thereby constraining the capacity to derive comprehensive generalisations regarding the efficacy of nanofluids in machining operations. One notable area of research that requires further investigation is the insufficient comprehension of the underlying mechanisms that contribute to the efficacy of nanofluids in the field of machining. Although it is acknowledged that nanofluids possess improved thermal properties that enhance their performance, the precise mechanisms by which they influence the machining process are still not well understood. Hence, it is recommended that future investigations focus on undertaking comprehensive and comparative analyses concerning the efficacy of diverse categories of nanofluids in relation to different machining procedures. These studies would provide a comprehensive comprehension of the potential of nanofluids in machining and assist in determining the optimal nanofluid varieties for various machining procedures. Furthermore, it is necessary to conduct additional research in order to clarify the mechanisms that underlie the performance of nanofluids in the context of machining. This could involve experimental studies to investigate the interactions between the nanoparticles, the base fluid, and the workpiece material. Theoretical studies could also be beneficial in developing models that can predict the performance of nanofluids in machining. Acknowledgements The author thanks the Ministry of Higher Education for supporting this study through the Fundamental Research Grant Scheme (FRGS), grant number FRGS/1/2022/TK10/ UMP/02/57. Their support has been key to this research. The author also appreciates the University of Malaysia Pahang Al-Sultan Abdullah for their support and financial help under grant RDU Number RDU210365, which has greatly helped in completing this study.

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Influences of Various Particle Sizes of Coal Bottom Ash as Supplementary Cementitious Material on the Pozzolanic Properties Mohammad I. Al Biajawi , Rahimah Embong , Andri Kusbiantoro , and Haneen Abd Aljabbar

Abstract The development of the world population shows a similar upward trend in the use of cement in the construction sector and rising tendency in the production of cement. These two occurrences considerably promote rise in the production of greenhouse gas (carbon dioxide) emission levels and coal ash from thermal power plant disposal, both are environmentally hazardous. Coal-fired power plants produce industrial by-products, such as coal-bottom ash (CBA), which has good pozzolanic properties and can be used as cement substitute to improve the quality of CBA as a pozzolanic material. The aim of this research is to examine the impacts of different particle sizes on the effective use of CBA as a cementitious substance to improve pozzolanic reactivity. CBA was collected from Tanjung Bin, sieved through various screen diameters, and then ground until 95 ± 1% of the particles met the ASTM C618 requirement of 45 µm for classification as pozzolanic substances. To evaluate the pozzolanic reaction of CBA based on the strength activity index (SAI), CBA was ground to same fineness as cement. Five substitution levels were used. To obtain SAI data, 10, 20, 30, 40, and 50% cement were partially substituted. The results showed that all the milled CBA samples exhibited pozzolanic characteristics and that the compressive strength of the milled CBA mortar improved with the curing age up to 20% substitution. The successful utilize of CBA as a pozzolanic materials and partial replacement for cement. Keywords Coal bottom ash · Strength activity index · Compressive strength · Pozzolanic properties · Particle size · Chapelle test

M. I. Al Biajawi · R. Embong (B) · H. A. Aljabbar Faculty of Civil Engineering Technology, Universiti Malaysia Pahang Al-Sultan Abdullah, Persiaran Tun Khalil Yaakob, 26300 Gambang, Pahang, Malaysia e-mail: [email protected] A. Kusbiantoro Department of Civil Engineering Technology, Faculty of Engineering Technology, Universiti Tun Hussein Onn Malaysia, 84600 Pagoh, Johor, Malaysia © The Author(s), under exclusive license to Springer Nature Singapore Pte Ltd. 2024 R. Abd. Aziz et al. (eds.), Intelligent Manufacturing and Mechatronics, Springer Proceedings in Materials 40, https://doi.org/10.1007/978-981-99-9848-7_27

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1 Introduction A pozzolan can potentially be characterized as siliceous as well as an aluminous and siliceous substance. It contains some or more cementing properties. However, the cementing properties require an increase in moisture content and a chemical reaction with calcium hydroxide that occurs at a suitable temperature to produce a material with exceptional cementing properties [1, 2]. In addition, pozzolanic products are frequently employed to partially replace ordinary Portland cement (OPC) to produce concrete or mortar characteristics features based on the needs of the consumers and to minimize the price of concrete mixture by reducing the amount of OPC utilized. The utilize of pozzolans as a partial replacement for (OPC) could achieve several objectives, the most important of which is to reduce the amount of waste produced by upstream industries, as well as the amount of land required for final disposal of the waste. Other objectives include optimizing concrete production costs and reducing CO2 emissions. Coal combustion contributes to approximately 27% of the world’s electricity generation and 38% of the world’s energy supply. Coal combustion is expected to account for 47% of global electricity generation by 2030 [3]. This is in response to growing energy demand. Fly ash (FA) and CBA are the two primary byproducts of burning coal in a thermal power plant [4]. Electrostatic precipitators in the chimney capture the FA. This is a more manageable form of the unburned residue that has just risen from the combustion zone [5]. CBA is a significant residual waste that dissolves and accumulates at the base of the incinerator; 15–25% of the amount of coal ash generated [6, 7]. The improper disposal of CBA could pollute groundwater supplies and surrounding soil, resulting in loss of wildlife and greater restrictions on land use. Consequently, CBA characteristics are affected by a number of variables, including the degree of coal grinding, the combustion temperature in the combustion chamber, and the type of burner and location of the thermal power plant [8]. Numerous pozzolanic substances, including FA [9], palm oil fuel ash, and rice husk ash, was investigated. CBA is characterized by a remarkably high content of silica and an amorphous structure that allows it to be ground into a powder materials that can be utilized either as a pozzolanic substance or as a cement additive [10, 11]. These properties are described in the guidelines published by ASTM C618 [12]. CBA is characterized by these properties. This is because CBA is able to undergo a chemical reaction with other substances when it interacts with water, resulting in the formation of a cementitious component [13]. In addition, many previous studies [14, 15] have shown that FA is recognized as a pozzolanic material and has been used in part as an alternative for OPC in the fabrication of mortar and concrete. It has been shown that this material can be used in a technically practical manner. However, numerous studies [16, 17] have been conducted to examine potential alternatives to landfilling CBA by investigating the possibility of its use in mortar and concrete mixes. Numerous research [18, 19] investigations have experimented with the use of CBA as a complete or partial substitute for fine aggregate in concrete construction. According to the findings of a study conducted by Ganesan et al. [20] evaluating the properties of concrete using CBA as a partial an alternative for fine aggregate, it was

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observed that the essentially usable substances of CBA can be employed as a sand for making concrete that will sustain for a long time. Another experimental work by Hooi-Jun et al. [21] examined the CBA of unburned coal with various particle sizes of 64, 73 and 150 µm as supplementary cementitious material. They observed that the application of CBA with various particle sizes only slightly impacted the compressive strength of the mortar. Kim [22] investigated the improvement of CBA as a substance with pozzolanic properties and showed that CBA through No. 40 sieve (425 µm) and powdered CBA at an alternative proportion of 30% and a long curing time of 91 days can result in mortar with compressive strength comparable to FA. According to the studies discussed previously, the use of CBA as a supplementary cementitious material with different fineness for pozzolanic properties in mortar mixes has not been investigated to any significant extent. However, the main objective of this experiment is to investigate the pozzolanic properties and SAI of CBA. To evaluate the strength characteristics of CBA, the material is examined at different sizes. To determine the degree of pozzolanic activity in CBA, the Chap-pell test and (SAI) were applied.

1.1 Materials and Experimental Producer 2 Materials In this experimental work, OPC, river sand, tap water, CBA with various grinding sizes were used to prepare the samples for this experimental study. The river sand aggregate employed in this experimental work met the standard guidelines of ASTM C778-13. The specific gravity, water absorption, and fineness modulus of the sand were 2.66, 1.75, and 3.80, respectively. Tap water was utilized for sample preparation. CBA was collected from the Tanjung Bin thermal power station located in Johor state, Malaysia. The various size of the original CBA and the ground CBA (Type A with 3000 cycle and Type B with 5000 cycle and Type C with 7000 cycle) particles were used in this study. After observation, it can be stated that the original CBA has rather a coarse texture, is porous in nature, and resembles a volcanic substance in shape, as shown in Fig. 1. The SEM image of CBA seen in the shows that the substance has irregular, glittery, round, and porous particles as shown in Fig. 1. To remove all traces of moisture from the CBA, they were dried in an electrically heated oven at a temperature of 105 C for 24 h. The next step was sieving CBA at 300 µm to remove coarse particles. Next step the original CBA was placed into Los Angeles machine until get the required fineness. The size of steel ball was used is 50 mm and the number of steel balls was 20 balls. Afterward, the ground CBA was sieved in order to reach a residue less than 35% in sieve 45 µm in compliance with ASTM C618 [12].. The color of CBA was changes from original CBA to ground CBA. The original CBA has a grey color, which turns into a dark grey color due to the grinding process.

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Fig.1 Original CBA and SEM morphology of original CBA

2.1 Specimen Preparation and Testings A total of six various mortar mixes were produced, each having a ratio of 1: 2.10: 0.50 for the cement, sand and w/c and a ratio of 0.58 for the water-binder ratio. Mortar ingredients containing CBA were prepared with a CBA content of 10, 20, 30, 40 and 50% mass replacement of OPC. Table 1 presents the material compositions of the mortar mixes that were made and tested as part of this study. Mortar mixture was designed with grade 35 MPa which is suitable to be used in various construction applications. To produce the samples, the components were first mixed in a small blender. After that the samples were placed into the cube sizes 50 mm × 50 mm × 50 mm with 3 layers. After a period of 24 h, the samples were removed from the molds and immediately placed in water to allow them to harden in water before being tested. The ambient temperature in the laboratory was between 25 and 30 ºC, and the relative humidity was between 70 and 80%. The compressive strength was evaluated according to ASTM C109/C109 standards. In addition, the strength index (SAI) is calculated in accordance with ASTM C311 guidelines. The water absorption test was done according to the British Standards BS EN 1881–122. The Chapelle activity test of CBA was investigated in accordance with the guidelines given in NF P 18–531. Table 1 Mix proportion of mortar mixes (g) Mix ID

Cement

Sand

CBA

Water

CBA0

1700

3600

0

850

CBA10

1530

3600

170

850

CBA 20

1360

3600

340

850

CBA 30

1190

3600

510

850

CBA 40

1020

3600

680

850

CBA 50

850

3600

850

850

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3 Results and Discussion 3.1 Chapelle Test for Pozzolanic Properties In the present research, the pozzolanic reaction of CBA could include evaluated in an oblique approach by assessing the amount of Ca(OH)2 that was consumed. The occurrence of additional C–S–H compounds in cementitious substances is thought to be connected with a larger usage of Ca(OH)2 by activated silica. This structure could make it easier to cover the spaces and improve the cementitious substance’s overall strength characteristics. In addition, Chapelle activity is a method of measuring the amount of CaO consumed by pozzolans; the higher the value of Chapelle reactivity, the higher the pozzolanic reactivity of the sample. Figure 2 shows the CaO values of the different sizes constitutes based on the modified Chapelle test and calculated according to standard NF P 18–531. According to the findings of the Chapelle test shown in the Fig. 4, the CBA with type B consumed the most CaO. The expected result is consistent with the higher silica content of this powder. However, the influence of the low strength and delayed pozzolanic activity of the unprocessed CBA on the amount of CaO consumption was comparatively insignificant. For the other fineness grades of CBA (types A, B, and C), the pozzolanic reactivity is increased, resulting in a higher proportion of silica in the samples. According to the findings of previously conducted study of chemical oxides and pozzolanic reactivity, the different sizes of CBA showed the optimum and recommended type B with high pozzolanic activity. However, the improvement was because of additional C-S-H product in the sample, which lead to the improvement in terms of mechanical performance of the mortar sample.

3.2 Compressive Strength and Strength Activity Index (SAI) Based on 7, 14 and 28 days, three different fineness levels and five different amounts of CBA were used to determine the optimum combination. Figure 3 shows the compressive strength of composite mortar with different CBA particle sizes at different curing times. At different CBA contents, the compressive strength initially improved up to a cement replacement of 20% and then started to decrease with increasing CBA content. For all CBA types (A, B, and C), the optimal replacement ratio for CBA was 20% at all curing ages. However, due to a pozzolanic reaction occurring between CBA and cement, they are improved at an early age, which is consistent with the results of Chandra and Bjornstrom et al. [23] reported predicted that C–S–H development from cement hydration results in faster strength increase than C–S–H formation due to the interaction between pozzolan and portlandite (also known as pozzolanic behavior) at an early age. The compressive strength of CBA (type A) at early ages was lower than that of the control specimens in the mortar mix. However, as the curing time increases, the compressive strength of the mortar

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Fig. 2 Pozzolanic reactivity of CBA at various particle’s size

may increase significantly. The compressive strength of CBA10 was 29.469 MPa at 7 days of age and 41.067 MPa at 28 days of age, corresponding to an increase of 109.142%, showing that CBA activity was limited in the initial stage but improved with time. As the grinding time increased, the particle size of the CBA decreased, which significantly increased the compressive strength of the cement mortar. After 14 days, the 20 mass % CBA partially displaced the OPC to initiate hydration products in the mortars, resulting in an early increase in compressive strength, supporting the findings of Cheriaf et al. [24] who noted that the pozzolanic activity of CBA with lime was extremely low prior to 14 days and that it began to increase after 28 days. For CBA (Type B), the optimal size and a significant increase in compressive strength were observed in comparison with standard specimens. The compressive strength of the mortar specimens increased by up to 20% after 7 days of curing. Thereafter, the compressive strength of all concrete mixes at higher curing with higher substitution ratios of CBA type B was below the compressive strength of the standardized mix. Additionally, this was also noted by Rafieizonooz et al. [25] when fly ash was used as a substitute for cement in the mix. On the other hand, the pozzolanic reaction had not started to any significant extent after 28 days, so the early strength was attributed to the presence of cement. Table 2 shows the compressive strength and SAI of CBA Type (A, B, and C) based mortars at different curing ages of 7, 14, and 28 days of curing. The SAI for CBA Type (A, B and C) specimens at 28 days curing exceed 75%, which fulfill the requirement of calcined natural pozzolan in ASTM C618. The experimental results demonstrate that the compressive strengths of the CBA Type (A, B,

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Fig. 3 Compressive strength results for CBA with various sizes at 7, 14, and 28 days of curing

Fig. 4 Water absorption results for CBA with various sizes at 28 days of curing

C) mortars increased with increasing curing age up to 20% replacement, respectively. According to the results for CBA Type A the compressive strength for CBA0, CBA10, CBA20, CBA30, CBA40, and CBA50 had compressive strength values 28.468, 29.469, 21.179, 17.955, 15.272, 11.449 MPa, respectively. The compressive strengths developed continuously until the ages of 28 days of curing up to 20% replacement ratio. For CBA Type B the SAI was improved up to 30% in all curing ages which is comply with the standard ASTM C 618 [15]. According to the results for CBA Type B for the SAI showed the optimum results compared to other fineness. Overall, according to the results for the SAI was observed that up to 20% in all CBA Types was found the limitation of the standard as per the specifications of ASTM C311, the modified mix must achieve 75% of the control mix strength after 7 days and 85% of it after 28 days of curing.

3.3 Water Absorption Figure 4 shows the water absorption result of CBA Type (A, B, and C) with various replacement ratio for cement-based mortars at 28 days of curing. The quantity of CBA as cement replacement with various grinding sizes influences the water absorption. Figure 4 shows that the mortar mixture with Type B exhibit to the lowest water

*

14

28

7

Type B 14

28

7

Type C 14

28

26.470 [78.023]

22.444 [66.156]

19.09 [56.269]

14.31 [42.180]

CBA 21.179 [74.39] 20

CBA 17.955 [63.071] 30

CBA 15.272 [53.646] 40

CBA 11.449 [40.217] 50

15.727 [41.797]

20.98 [55.758]

24.789 [65.880]

28.928 [76.880]

41.067 [109.142]

Compressive Strength (MPa)—[Strength Activity Index ratio]

37.374 [110.16]

CBA 29.469 [103.51] 10

11.624 [40.832]

20.612 [72.404]

23.002 [80.799]

29.759 [105.129]

32.275 [113.370]

14.531 [42.778]

25.766 [75.947]

28.752 [84.749]

37.199 [109.647]

40.344 [118.918]

15.969 [42.440]

28.309 [75.236]

31.599 [83.979]

40.879 [108.643]

44.171 [117.39]

9.297 [32.658]

16.570 [58.206]

19.743 [69.351]

25.216 [88.577]

28.290 [99.375]

11.612 [34.227]

20.711 [61.078]

24.679 [72.744]

31.628 [93.226]

35.369 [104.253]

12.882 [34.236]

22.765 [60.502]

27.118 [72.071]

34.759 [92.3778]

39.637 [105.342]

CBA 28.468—[100.00] 33.926—[100.00] 37.627—[100.00] 28.468—[100.00] 33.926—[100.00] 37.627—[100.00] 28.468—[100.00] 33.926—[100.00] 37.627—[100.00] 0

CBA Type A Type 7

Table 2 Compressive strengths and strength activity indices of mortar samples

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absorption value compared to other grinding sizes. However, mortars with Type A showed the highest values for water absorption compared to other grinding sizes. Furthermore, mortar with varies griding sizes recorded the increase in the water absorption when increase the replacement ratio. Mortar mixes recorded an increment in percentage of water absorbed as larger quantity of CBA with various Grinding sizes is integrated in the mix. It seems that, excessive use of CBA with various grinding sizes as partial cement re-placement causes formation of more voids which rises the water absorption of mortar.

3.4 Relation Between Compressive Strength and Water Absorption Figure 5 demonstrates the relation between Water absorption and compressive strength of the CBA for mortar mixture at 28 days of curing age. The result indicates the reduction in compression strength leading to a decrease with increase the ratio also, in water absorption. For mortar with CBA with type A as cement replacement the data were correlated to a polynomial equation Fc = −0.0453x2 + 2.4636 × and with coefficients of correlation R2 = 0.0511. For mortar with CBA with type B as cement replacement the data were correlated to a polynomial equation Fc = −0.0595 × 2 + 3.1882 × and with coefficients of correlation R2 = 0.0549. For mortar with CBA with type C as cement replacement the data were correlated to a polynomial equation Fc = -0.0523 × 2 + 2.7697 × with coefficients of correlation R2 = 0.0066. On the other hand, the water absorption for mortar with CBA with type A as cement replacement the data were correlated to a polynomial equation y = −0.0119 × 2 + 0.8117 × with coefficients of correlation R2 = 0.8532. the water absorption for mortar with CBA with type B as cement replacement the data were correlated to a polynomial equation y = −0.0111 × 2 + 0.7809 × with coefficients of correlation R2 = 0.2316. the water absorption for mortar with CBA with type C as cement replacement the data were correlated to a polynomial equation y = −0.0114 × 2 + 0.7927 × with coefficients of correlation R2 = 0.2949.

4 Conclusion Based on the results, the followed conclusions can be drawn: ● From the chemical composition for the original CBA, CBA with Type A, B, and C of constituent materials, it was ascertained that can be used as supplementary cementitious materials in accordance with ASTM C 618 in the limitation of the standard guidelines.

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Fig. 5 Relevance between compressive strength and Water absorption

● Comparing the CBA with various fineness sizes that were prepared for investigating the pozzolanic reaction, all samples of CBA had pozzolanic properties and developed compressive strength that increased at certain level of replacement and with the curing age. ● From Chapelle test, an increase in the fineness of CBA, significantly increased the Chappelle reactivity. However, the highest pozzolanic activity of CBA with Type B is the optimum fineness recommended through this experimental work. ● For the compressive strength was found the optimum replacement ratio to be used as cement replacement with CBA Type (A, B, and C) was found 20% in all curing ages. ● For the SAI was found the optimum fineness CBA (Type B) and had improvement in accordance with standard. ● Overall, 20% of cement replacement with CBA Type (A, B, C) and CBA (Type B) was determined as the optimal amount to replace the cement as supplementary cementitious materials in mortar it had an improvement in strength compared to the control mortar. Hence, it is recommended to further investigate the mechanical behavior of CBA in various concrete applications. Acknowledgements The authors would like to thank Ministry of Higher Education (MOHE) or Kementerian Pendidikan Tinggi Malaysia for providing financial support under fundamental research grant Scheme (FRGS) No. (FRGS/1/2022/TK01/UMP/02/5 (university reference RDU(220112) and Universiti Malaysia Pahang AL-Sultan Abdullah (UMPSA) for laboratories facilities as well as additional support under internal grant No. RDU 223313.

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References 1. Malhotra VM, Mehta PK (1996) Pozzolanic and cementitious materials, CRC Press 2. AlBiajawi MI, Embong R, Muthusamy K (2021) An overview of the utilization and method for improving pozzolanic performance of agricultural and industrial wastes in concrete. Mater Today: Proc 3. Ankur N, Singh N (2021) Performance of cement mortars and concretes containing coal bottom ash: a comprehensive review. Renew Sustain Energy Rev 4. Kusbiantoro A, Hanani A, Embong R (2019) Pozzolanic reactivity of coal bottom ash after chemically pre-treated with sulfuric acid. In: Materials science forum, Trans Tech Publications Ltd, pp 212–216 5. Yadav VK, Gacem A, Choudhary N, Rai A, Kumar P, Yadav KK, Abbas M, Ben Khedher N, Awwad NS, Barik D (2022) Status of coal-based thermal power plants, coal fly ash production, utilization in India and their emerging applications. Minerals 12:1503 6. Al Biajawi MI, Embong R, Muthusamy K, Ismail N, Obianyo II (2022) Recycled coal bottom ash as sustainable materials for cement replacement in cementitious composites: a review. Construct Build Mater 338:127624 7. Embong RB (2019) Pozzolanic and strength properties of mortar containing chemically pretreated coal bottom ash, doctor of philosophy 8. Zhou H, Bhattarai R, Li Y, Si B, Dong X, Wang T, Yao Z (2022) Towards sustainable coal industry: turning coal bottom ash into wealth. Sci Total Environ 804:149985 9. Kusbiantoro A, Embong R, Abd Aziz A (2018) Strength and microstructural properties of mortar containing soluble silica from sugarcane bagasse ash. In: Key engineering materials, Trans Tech Publ, pp 269–274 10. Kusbiantoro A, Embong R, Shafiq N (2017) Adaptation of eco-friendly approach in the production of soluble pozzolanic material. Int J Des Nature and Ecodynam 12:246–253 11. Embong R, Kusbiantoro A, Muthusamy K, Ismail N (2021) Recycling of coal bottom ash (CBA) as cement and aggregate replacement material: a review. In: IOP conference series: earth and environmental science, IOP Publishing, pp 12035 12. American Society for Testing and Materials (2019) ASTM C618–19, Standard Specification for Coal Fly Ash and Raw or Calcined Natural Pozzolan for Use in Concrete, Annual Book of ASTM Standards, pp 5 13. Grabias-Blicharz E, Franus W (2023) A critical review on mechanochemical processing of fly ash and fly ash-derived materials. Sci Total Environ 860:160529 14. Ramjan S, Tangchirapat W, Jaturapitakkul C, Chee Ban C, Jitsangiam P, Suwan T (2021) Influence of cement replacement with fly ash and ground sand with different fineness on alkali-silica reaction of mortar. Materials 14:1528 15. Amran YHM, Soto MG, Alyousef R, El-Zeadani M, Alabduljabbar H, Aune V (2020) Performance investigation of high-proportion Saudi-fly-ash-based concrete. Results in Eng 6:100118 16. Tamanna K, Raman SN, Jamil M, Hamid R (2023) Coal bottom ash as supplementary material for sustainable construction: a comprehensive review. Constr Build Mater 389:131679 17. Guan X, Wang L, Mo L (2023) Effects of ground coal bottom ash on the properties of cementbased materials under various curing temperatures. J Build Eng 69:106196 18. Shariati M, Kamyab H, Habibi M, Ahmadi S, Naghipour M, Gorjinezhad F, Mohammadirad S, Aminian A (2023) Sulfuric acid resistance of concrete containing coal waste as a partial substitute for fine and coarse aggregates. Fuel 348:128311 19. Babajide Olabimtan S, Mosaberpanah MA (2023) The implementation of a binary blend of waste glass powder and coal bottom ash as a partial cement replacement toward more sustainable mortar production. Sustainability 15:8776 20. Ganesan H, Sachdeva A, Petrounias P, Lampropoulou P, Sharma PK, Kumar A (2023) Impact of fine slag aggregates on the final durability of coal bottom ash to produce sustainable concrete. Sustainability 15:6076

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21. Ng J, Al Bakri Abdullah MM, Tan SJ, Sandu AV, Hussin K (2018) Characterisation and understanding of Portland cement mortar with different sizes of bottom ash. Adv Cement Res 30:66–74 22. Kim HK, Lee HK (2016) Autogenous shrinkage reduction with untreated coal bottom ash for high-strength concrete. ACI Mater J 113:277–285 23. Chandra S, Björnström J (2002) Influence of superplasticizer type and dosage on the slump loss of Portland cement mortars—Part II. Cem Concr Res 32:1613–1619 24. Cheriaf M, Rocha JC, Pera J (1999) Pozzolanic properties of pulverized coal combustion bottom ash. Cem Concr Res 29:1387–1391 25. Rafieizonooz M, Mirza J, Salim MR, Hussin MW, Khankhaje E (2016) Investigation of coal bottom ash and fly ash in concrete as replacement for sand and cement. Constr Build Mater 116:15–24

Optimizing DC Alloy Properties: Impact of T6 Heat Treatment at High Solution Temperatures on β-AlFeSi Phase Transformation Mohamad Rusydi Mohamad Yasin, Muhammad Syamim Mazlan, and Nurul Nadia Nor Hamran

Abstract Aluminum–Silicon (Al-Si) alloys are widely used in Die-Casting (DC) applications due to their low thermal expansion and excellent mechanical properties. Nevertheless, iron inclusion in the composition is sometimes seen as disadvantageous due to its tendency to create brittle β-AlFeSi phase precipitates, which may result in a decrease in the alloy’s ductility. Hence, the regulation of the β-AlFeSi phase is of paramount importance to further improve mechanical characteristics. Heat treatment is a well-recognized technique used to manipulate the shape of the β-AlFeSi intermetallic phase and enhance its properties. This research aims to comprehensively examine the impacts of modified T6 heat treatment on the A380 Al-Si alloy. The heat treatment procedure included manipulating the solution temperature and examining its impact on the microstructure and mechanical characteristics of the alloy. The results of our study indicate that a T6 solution temperature of 515 °C for a short duration is the most effective in dissolving the β-AlFeSi phase and enhancing the elongation of the DC alloy to 3.39%. The observed temperature facilitates the conversion of the β-AlFeSi phase to the α-AlFeSi phase, which is known to have fewer adverse effects on the properties of the alloy. The observed enhancement in elongation, a critical indicator of ductility, indicates that subjecting Al-Si alloys to high-temperature heat treatment might serve as a viable approach for augmenting their mechanical characteristics. The results emphasize the potential efficacy of using high-temperature heat treatment as a feasible approach for enhancing the characteristics of Al-Si alloys. Keywords Aluminum–Silicon (Al-Si) alloy · Material morphology · Heat treatment

M. R. Mohamad Yasin (B) · M. S. Mazlan · N. N. Nor Hamran Faculty of Manufacturing and Mechatronic Engineering Technology, Universiti Malaysia Pahang Al-Sultan Abdullah, 26600 Pekan, Pahang, Malaysia e-mail: [email protected] © The Author(s), under exclusive license to Springer Nature Singapore Pte Ltd. 2024 R. Abd. Aziz et al. (eds.), Intelligent Manufacturing and Mechatronics, Springer Proceedings in Materials 40, https://doi.org/10.1007/978-981-99-9848-7_28

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1 Introduction The β-AlFeSi phase, which is often seen in die casting (DC) Al-Si alloys, is well recognized for its negative effect on the overall quality of the resulting alloy products. The phase under consideration, distinguished by its needle-shaped morphology, functions as a stress concentrator, resulting in a notable decrease in the quality index of the alloys [1–7]. The presence of acicular morphology in this phase leads to the development of localized stress concentrations, which might lead to premature failure when subjected to cyclic loading conditions [6, 7]. The strength and durability of the finished product are of paramount significance in the die-casting business, hence giving rise to a notable issue. The conversion of the β-AlFeSi phase to the less deleterious α-AlFeSi phase has been widely used in industrial settings. The process of achieving this transition is often accomplished by the use of element control techniques. These techniques entail the manipulation of the alloy composition to promote the creation of the α-AlFeSi phase [8]. Nevertheless, this methodology is not devoid of its limitations. The manipulation of elemental composition has the potential to induce several adverse consequences, including the generation of intermetallic compounds, which may detrimentally influence the mechanical and chemical characteristics of the alloy [9]. The presence of intermetallic compounds inside an alloy has the potential to adversely affect its mechanical characteristics, hence reducing its suitability for certain applications. In light of the limitations inherent in element control approaches, heat treatment has emerged as a viable alternative strategy for mitigating the adverse consequences of AlFeSi intermetallic compounds [10]. The process of heat treatment encompasses the deliberate use of controlled heating and subsequent cooling to modify the microstructure of an alloy, hence inducing changes in its inherent characteristics. The efficacy of this approach in mitigating the occurrence of detrimental β-AlFeSi phase and facilitating the development of the preferable α-AlFeSi phase has been shown. However, heat treatment is not as widespread as expected due to a few major hurdles. The first issue is die casting. Air may be trapped in aluminum alloy during solidification. Heat treatment expands entrapped air, creating surface protuberances [11]. This might weaken the product and harm its aesthetics. The alloy microstructure may be affected by heat treatment, the second worry. The effect of heat treatment on alloy phase formation is important. The Si phase may coarsen by heat treatment [2]. For applications requiring strength and durability, coarsening may degrade the alloy’s mechanical qualities. This study uses T6 heat treatment with a high temperature of the solution and short duration to overcome these issues. This method prevents heat treatment concerns such needle-like intermetallic phases and blisters [12]. T6 heat treatment comprises solution and artificial aging. Solution heat treatment dissolves undesirable phases by heating the alloy. After that, the alloy is immediately quenched to stabilize the microstructure. After that, artificial aging is done at a lower temperature to precipitate the right phases. The restricted diffusion rate of iron (Fe) within aluminum (Al) allows for high solution temperatures, making this method effective [13].

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Prior research has shown that acicular iron phase platelets have the ability to undergo dissolution at the defective sites of crystals when subjected to hightemperature heat treatment, leading to a reduction in their length [3]. This finding has significance as it implies that subjecting the material to high-temperature heat treatment may successfully convert the deleterious β-AlFeSi phase into the less deleterious α-AlFeSi phase. Within defective regions of the crystal lattice, the atoms of Si, Fe, or manganese (Mn) exist in an elevated energy state and exhibit a propensity to transition towards a state of lower energy. The dissolving process may be expedited with the use of heat treatment, therefore enhancing the conversion of the β-AlFeSi phase to the α-AlFeSi phase [14]. The modification of an alloy’s microstructure via the heat treatment process is a critical factor that enables the enhancement of its characteristics. In addition to conventional heat treatment techniques, several investigations have used the non-equilibrium heat treatment approach, whereby the alloy is subjected to temperatures above the customary solution heat treatment temperature [4]. The outcome of this phenomenon leads to a dissolving effect, thereby reducing the duration of the β phase [15–20]. This methodology has shown notable efficacy in mitigating the occurrence of the β-AlFeSi phase, hence enhancing the mechanical characteristics of the alloy. Nevertheless, it is crucial to acknowledge that this approach may not be appropriate for every scenario, since it has the potential to result in the creation of more undesired stages. A separate investigation was carried out to examine the effects of heat treatment on die casting alloys. It was shown that the disintegration occurring inside the β phase may lead to dissolution [5, 21–23]. This implies that the heat treatment procedure not only facilitates the conversion of the β-AlFeSi phase to the α-AlFeSi phase, but also encourages the dissolution of the β phase, hence augmenting the characteristics of the alloy. Nevertheless, it is worth mentioning that the α-AlFeSi phase fraction remains unaffected by heat treatment, as seen in both experiments [16–20, 24–27]. The aforementioned statement highlights the intricacy of the heat treatment procedure and emphasizes the need for meticulous regulation of the process variables in order to attain the intended outcomes. Therefore, the aim of this research is to investigate the influence of solution temperature on short-time T6 heat treatment process, with the purpose of identifying the optimal heat treatment condition that may effectively enhance the mechanical properties of the alloy. The morphologies of the phases that encompassed Fe were investigated to study the changes in size and proportion at different solution temperatures. The present research offers significant insights on the impact of heat treatment on the microstructure of the alloy and the correlation between the microstructure and the characteristics of the alloy [27–30]. The analysis also includes an examination of the impact on the mechanical characteristics by a comparison of the elongation of the heat-treated samples. The measurement of elongation serves as a significant indicator of the ductility of an alloy, and advancements in elongation might signify an augmentation in ductility, which has great importance in several practical applications.

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2 Methodology The study employed commercial die casting aluminum alloy A380, a hypoeutectic alloy known for its excellent castability and mechanical properties. The alloy exhibits a liquidus temperature of 594 °C and a solidus temperature of 528 °C. The A380 alloy composition, as depicted in Table 1, comprises a combination of aluminum along with several additional elements including silicon, copper, iron, manganese, nickel, zinc, and magnesium. The A380 alloy was casted into standard tensile test bars with dimensions following the ASTM E 8 M-04 as outlined in Table 2. These samples were used for mechanical testing and microscopic observation. This standard was chosen due to its widespread acceptance and use in the industry for evaluating the tensile properties of metallic materials. The samples subsequently underwent a T6 heat treatment process. This heat treatment process is known for its ability to significantly enhance the mechanical properties of Al-Si alloys. However, blistering, a common problem during the heat treatment of die casting parts, was a major concern. To mitigate this, a short-time heat treatment with high-temperature was adopted, followed by water quenching. The solution temperatures were set at 450, 500 , 515 and 530 °C, with a 30-min solutionization duration for each setting. This temperature range was chosen based on prior investigations demonstrating successful transformation of the β-AlFeSi phase to the α-AlFeSi phase. Quenching the samples in water ‘freezes’ the microstructure and locks in the desired phases after solution treatment. The samples were then aged at 125 °C for 4 h to precipitate appropriate phases and improve the alloy’s characteristics. After heat treatment, samples were tensile tested for elongation. To establish statistical significance, the tensile test used 15 samples per condition. The heat treated samples were polished, etched and examined under an optical microscope for intermetallic phase morphologies. Five fields were measured and averaged to reveal needle-like characteristics in the β-needles. Together, these data determined the average beta phase length for heat-treatment conditions. This method allows for a detailed study of heat treatment’s impact on A380 alloy microstructure and mechanical properties. Table 1 Composition of A380 alloy Element

Si

Cu

Fe

Mn

Ni

Zn

Mg

Al

Wt%

9.0

3.5

1.0

0.4

0.3

0.3

0.2

Bal

Table 2 Dimensions Specification for standard tensile bar for ASTM E 8M—04 Feature

Gage length, G

Diameter, D

Radius of filler, R

Length of reduced section, A

Dimensions (mm)

30.0 ± 0.1

6.0 ± 0.1

6.0

36.0

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3 Results and Discussion The proportion and shape of AlFeSi phases were transformed by heat treatment, particularly solution temperature fluctuation. This transformation was evident in the changes observed in the microstructure of the samples subjected to different heat treatment conditions. At a solution temperature of 450 °C, no significant change in the AlFeSi phase was observed. The β-AlFeSi phase remained dominant, as shown in Fig. 1a, b. This could be attributed to the relatively low temperature, which may not have been sufficient to promote the dissolution of the β-AlFeSi phase and the formation of the α-AlFeSi phase. This finding aligns with previous studies that have reported the persistence of the β-AlFeSi phase at lower heat treatment temperatures [7]. However, elevating the solution temperature to 515 °C altered the intermetallic phase. As can be seen in Fig. 1c, the β-AlFeSi phase dissolves and its proportion decreases. Elevated temperatures facilitated the dissolution of the β-AlFeSi phase, a crucial step in the transition to the α-AlFeSi phase. The discovery supports prior

Al

Si

β-AlFeSi

α-AlMnFeSi

(a)

(b)

(c)

(d)

Fig. 1 Morphologies of short-time heat-treated A380 samples with solution temperatures of a 450 °C, b 500 °C, c 515 °C and d 530 °C

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Fig. 2 Graph of elongation versus solution temperature of A380 alloy

Elongation (%)

studies indicating a decrease in β-AlFeSi phase proportion with increasing heat treatment temperature [8]. Increasing the solution temperature to 530 °C greatly enhanced the α-AlFeSi phase fraction, as seen in Fig. 1d. Temperature increase led to enhanced solubility and development of the β-AlFeSi phase. The study indicates that heat treatment at high temperatures can enhance the α-AlFeSi phase, resulting in less detrimental effects on alloy characteristics [31]. The findings shed light on how solution temperature affects AlFeSi phase change after heat treatment. The authors stress that high-temperature heat treatment can improve Al-Si alloy characteristics. This treatment transforms the β-AlFeSi phase into the α-AlFeSi phase, improving the alloy’s properties [32]. The effect of solution temperature on the elongation of the alloy was another critical aspect of this study. Elongation is a measure of an alloy’s ductility, and improvements in elongation can indicate enhanced ductility, which is crucial for many applications. The results of the tensile tests, as shown in Fig. 2, revealed a clear relationship between solution temperature and elongation. As the solution temperature increased from 450 °C to 515 °C, there was a significant improvement in elongation. Specifically, the elongation increased from 1.62% at 450 °C to 3.39% at 515 °C. This improvement can be attributed to the transformation of the β-AlFeSi phase to the α-AlFeSi phase, which is known to enhance the alloy’s ductility [33]. The increase in elongation with solution temperature up to 515 °C suggests that the heat treatment process facilitated the dissolution of the β-AlFeSi phase and the formation of the α-AlFeSi phase, thereby improving the alloy’s ductility [34]. However, further increase in the solution temperature to 530 °C resulted in a significant reduction in elongation to 1.18%. This reduction could be due to the over-dissolution of the αAlFeSi phase or the formation of other detrimental phases at higher temperatures [33]. This finding underscores the importance of carefully controlling the heat treatment parameters to achieve the desired improvements in the alloy’s properties. These findings indicate that 515 °C is the best solution temperature for alloy elongation. This temperature favors the transition of β-AlFeSi to α-AlFeSi while preventing over-dissolution or production of detrimental phases [34]. These discoveries can help improve Al-Si alloy heat treatment procedures. The solution temperature during heat treatment plays a pivotal role in the transformation of the β-AlFeSi phase, as evidenced by the changes in the size and fraction 4 3.5 3 2.5 2 1.5 1 0.5 0 440

460

480

500

Solution Temperature (°C)

520

540

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of this phase with increasing temperatures. The morphology of the β-AlFeSi phase, characterized by its needle-like structure, did not exhibit any significant change at a solution temperature of 450 °C. This suggests that this temperature may not be sufficient to initiate the transformation of the β-AlFeSi phase [4]. However, as the solution temperature was increased to 500 °C, the β-AlFeSi phase began to transform. This transformation was characterized by a decrease in the size of the β-AlFeSi phase and an increase in the fraction of the α-AlFeSi phase [35]. This implies that 500 °C is the minimal temperature required for the transformation of the β-AlFeSi phase. This finding aligns with previous studies that have reported similar temperature thresholds for the transformation of the β-AlFeSi phase [36]. The platelet-like Al–Fe-Si phase causes stress concentrations and is harmful [1]. These stress concentrations can cause premature failure under cyclic loads. Reducing the β-AlFeSi phase can improve the alloy’s mechanical characteristics and offset its negative consequences [5]. Experimental data indicate that higher solution temperatures reduce the β-AlFeSi phase, leading to significant improvement in the alloy’s mechanical characteristics. However, higher solution temperatures can coarsen silicon particles. This coarsening lowers the alloy’s quality index [37]. Therefore, the use of solution temperatures in the heat treatment should not be very high and closed to the solidus temperature. According to the study, optimally solution temperature should be kept at 515 °C. Heat treatment at this temperature can convert and dissolve the β-AlFeSi phase, improving mechanical characteristics without coarsening silicon particles [37].

4 Conclusions In summary, our research elucidates that precise regulation of solution temperature during the heat treatment process yields notable enhancements in the mechanical characteristics of Al-Si alloys. The study suggests that a temperature of at least 500 °C is necessary for the conversion of the β-AlFeSi phase. The study determines that the most favorable temperature for the short time solution was 515 °C. At the given temperature, the elevated heat efficiently causes the dissolution of the β-AlFeSi intermetallic phase, resulting in a notable enhancement of the elongation characteristic of the Al-Si alloy. Enhancements in elongation might signify an improved level of ductility, which holds great importance in numerous practical applications. The aforementioned discovery highlights the potential of utilizing high-temperature heat treatment as a feasible approach to enhance the characteristics of Al-Si alloys through the facilitation of the transition from the β-AlFeSi phase to the α-AlFeSi phase. Further investigation is warranted to explore the impact of additional heat treatment parameters on the transformation of AlFeSi phases and the consequent mechanical characteristics of Al-Si alloys.

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Acknowledgements The authors wish to extend their sincere appreciation to the Ministry of Higher Education (MoHE) and University Malaysia Pahang for their kind financial support, which facilitated the execution of this research endeavor. The study greatly benefited from the financial support received from the Fundamental Research Scheme (FGRS) FRGS/1/2022/TK10/UMP/02/67 and the University Malaysia Pahang’s Fundamental Research Grant RDU220317. These funds played a crucial role in enabling the study to obtain necessary materials, conduct experiments, and analyze the collected data.

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Fracture Behaviour of Zirconia-Reinforced Lithium Silicate Glass–Ceramic Composite Afifah Z. Juri, Animesh K. Basak, and Ling Yin

Abstract Fracture mechanisms in zirconia-reinforced lithium silicate glass– ceramic (ZLS) materials are important to evaluate its performances under loadbearing applications. However, due to its inherent brittleness nature, it is difficult to observe fracture behaviour. Hence, it is imperative to understand the fracture behaviour of the ZLS material. This study investigated the fracture behaviour of pre-crystallized ZLS glass–ceramic materials at nano-scale length using micropillar compression technique inside of scanning electron microscopy (SEM). Micropillar structures with dimension of 3 µm in diameter and 9 µm in length was fabricated using fibre ion beam milling inside SEM. Flat diamond puncher with 5 µm diameter was used to conduct the compression test. Compression properties (Young’s modulus, mechanical strengths (yield, fracture, compressive), ductility, resilience and toughness of the ZLS material were determined. The fractured micropillar of the pre-crystallized ZLS was observed during and after the compression using SEM. Pre-crystallized ZLS revealed micrropillar compression induced mushroom defect, micro cracking and delamination as its mode of fracture mechanisms. It had Young’s modulus of 62 ± 7 GPa, yield strength of 1850 ± 31 MPa, fracture strength of 1987 ± 25 MPa, ultimate compressive strength of 2010 ± 47 MPa, ductility of 4 ± 1%, resilience of 71 ± 4 J/m3 and toughness of 126 ± 9 J/m3 . This study provided fundamental micro compression mechanisms associated to fracture behaviour of precrystallized ZLS for development of new microstructural design for these material for high quality dental restorations. Keywords Behaviour · Compression · Fracture · Mechanical properties · Zirconia-reinforced lithium silicate glass–ceramic A. Z. Juri (B) · L. Yin Department of Electrical and Mechanical Engineering, Faculty of Science Engineering and Technology, The University of Adelaide, Adelaide, South, Australia e-mail: [email protected] A. Z. Juri Department of Mechanical and Manufacturing Engineering, Faculty of Engineering and Built Environment, Universiti Kebangsaan, Bangi, Malaysia A. K. Basak Adelaide Microscopy, The University of Adelaide, Adelaide, South, Australia © The Author(s), under exclusive license to Springer Nature Singapore Pte Ltd. 2024 R. Abd. Aziz et al. (eds.), Intelligent Manufacturing and Mechatronics, Springer Proceedings in Materials 40, https://doi.org/10.1007/978-981-99-9848-7_29

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1 Introduction In response to the need for restorative materials with superior mechanical strength and aesthetic qualities, a novel type of glass ceramic called zirconia-reinforced lithium silicate glass–ceramic (ZLS) has been developed. [1]. Fabrication of ZLS restoration such as crowns, bridges, inlays, onlay, and veneers, computer-aided design / computer-aided manufacturing (CAD/CAM) technologies are used. This material is contain roughly 10 wt% of zirconia (ZrO2 ) in the glassy phase [2] and a reinforcing crystalline phase to result in improved mechanical properties [3]. ZLS has gained preference over the widely recognized lithium disilicate glass ceramic because it significantly reduces the time required for dental restoration production [4]. Clinical studies shows promising results of a 99% survival rate was achieved when ZLS materials were used as partial crowns on sixty-nine patients within a three year observation [4]. ZLS material are available in the dental market as pre-crystallized blanks. Precrystallized ZLS has a homogenous fine crystals microstructure with average grain size of less than 100 nm and consist of lithium metasilicate and lithium orthophosphate crystals [5]. Moreover, it is associated with low strength of 180 MPa [6]. Hence, it is preferred due to ease of machining process. Afterward, crystallization process are subjected to the machine pre-crystallized ZLS to achieve higher mechanical properties. Micropillar compression technique offers provides for a visual high resolution images of deformed micropillar sample to study their deformation behaviour [7]. The micropillar structure is milled using a focused ion beam milling process within the context of scanning electron microscopy (SEM). Subsequently, a flat punch is employed to compress the micropillar. Additionally, by utilizing an in-situ scanning electron microscopy (SEM) setup, it becomes possible to record SEM videos capturing the entire micropillar compression test. This allows for the generation of a series of SEM images depicting the compression process, which aids in the investigation of the primary deformation and damage mechanisms [8]. In micropillar compression of GaAs crystal in room temperature revealed that at 1 µm diameter micropillar did not split but at higher of 2.3 µm diameter splitting was observed originated from intersecting slip planes [9]. Compression induced plastic deformation was possible when compressed brittle ceramic at elevated temperature of 200 °C and 400 °C using micropillar compression technique [7]. Micropillar compression was also used to measure the mechanical properties of nanocrystalline Cr2 AlC coating, reporting a vast improvement of compressive strength of 5 times higher than the Cr2AlC, bulk material [10]. The micro pillar compression studies [7–10] have provided valuable insights into the behavior and deformation of materials when subjected to small volume contact loads, which is crucial for predicting their responses in real-world applications. Even though studies on investigating the mechanical behavior and properties of ZLS materials have been conducted using indentation technique. However, a broad research gaps in ZLS mechanical properties, deformation and damage mechanisms still remain unclear. The objective of this study is to investigate the fracture behavior

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Table 1 Chemical composite of pre-crystallized ZLS material [13] Component

SiO2

Li2 O

K2 O

P2 O5

Al2 O3

ZrO2

CeO2

wt. %

51

7.5

3.2

9.9

3.5

16.8

3.4

of pre-crystallized ZLS material by conducting micropillar compression experiments within a scanning electron microscopy.

2 Methodology A rectangular block of pre-crystallized ZLS with dimension 10 mm × 10 mm × 12 mm was selected for this study. The material is commonly used for dental restoration as crown, inlay, only and bridges [11]. Table 1 shows the chemical composition of pre-crystallized ZLS material. The material contain 58 ± 2 wt % glassy phase and 40 ± 2 wt % crystalline phase [12]. Pre-crystallized ZLS samples were obtained from slicing the rectangular block into 10 mm × 10 mm × 2 mm using a diamond saw machine. Standard metallographic process were conducted on the samples to produce mirror surface finish. Grinding processes were performed on the 10 mm × 10 mm surface using 600–1200 grit sand papers on grinding machine and water as lubricant. This is followed by polishing process using diamond paste of 6 µm and 1 µm grit sizes. Figure 1 shows the experimental set-up for the micropillar compression test. The pre-crystallized micropillars with dimension of 3 µm in diameter and 9 µm in height were fabricated using fibre ion beam milling inside SEM. The micropillar were built using hard milling with 30 kV and polishing milling from 2.8 nA to 90 pA to fabricate the micropillar structure. The compression were performed using 5 µm flat diamond punch at strain rate of 10−3 s−1 corresponding to loading rate of 3 nms−1 and unloading rate of 50 nms−1 were applied.

3 Result and Discussion Figure 2 shows SEM micrographs of the pre-crystallized ZLS during micropillar compression test and corresponding stress–strain curve. Figure 2a shows the undeformed ZLS micropillar structure before compression, revealing micropillar structure of 3 µm in diameter. During loading, the compressive force increases resulting in the mushrooming effect and crack initiation and propagation, as shown in Fig. 2b. The flat punch induces enough stress exceeding the material tolerant stress causing material fragmentation and pulverization resulting in material being pushed out and creating the mushrooming effect. At unloading, Fig. 2c depicts fractured micropillar structure of the pre-crystallized ZLS material. As the compressive force increase, the crack

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Flat diamond punch

Sample

Fig. 1 Experimental set-up

propagation leads to the large fracture and ultimately failure. Similar mushrooming effect was found in compression of TiSiN/Ag multilayer coating with micropillar diameter of 1 µm and loading strain rate of 4 × 10−3 s−1 [14]. Figure 2d shows the stress–strain curve of the pre-crystallized ZLS during compression. The material underwent elastic deformation until 0.03 strain then followed by yield point. The crack initiation and propagation occurred after yielding. The plastic deformation region showed stress drop and increment. This may due to the crack initiation and propagation that occurred (Fig. 2b) resulting in the stress drop. However for bulk metallic glass with micropillar diameter of 3 µm and constant displacement control of 1 nms−2 the stress drops observed during micropillar compression were correlated to multiple shear band formations and propagations [15]. The shear band occurred mostly near the corner of the top surface due to tapering effect. Table 2 shows the compression properties of the pre-crystallized ZLS material. The material had Young’s moduli of 62 ± 7 GPa. This value is in the range with the value obtained from manufactured of 70 GPa [6]. However, the study Young’s moduli value was underestimated by 32% compared to Young’s moduli value obtained from nanoindentation of pre-crystallized ZLS using Berkovich indenter at loading rate of 0.5 mN/s. This shows different mechanical testing influence to the mechanical properties of pre-crystallized ZLS material. It is of interest to compare ultimate compressive strength of pre-crystallized ZLS glass ceramic to zirconia polycrystalline ceramic material [16]. Zirconia polycrystalline ceramic had strength of 6500 MPa which is 3 times higher than pre-crystallized ZLS glass ceramic strength of 2010 ± 47 MPa. This shows that polycrystalline ceramic is stronger than zirconia reinforced glass–ceramic. Figure 3 shows SEM micrographs of pre-crystallized ZLS fractured micropillar structures after compression. Figure 3a shows crack splitting failure mode could be

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Fig. 2 SEM micrographs of the pre-crystallized micropillar structure a before loading; b during loading; c after unloading of the flat diamond punch d corresponding stress–strain curve

Table 2 Compression properties of pre-crystallized ZLS

Mechanical properties Young’s modulus

Pre-crystallized ZLS 62 ± 7 GPa

Yield strength

1850 ± 31 MPa

Ultimate tensile strength

2010 ± 47 MPa

Fracture strength

1987 ± 25 MPa

Ductility

4 ± 1%

Resilience

71 ± 4 J/m3

Toughness

126 ± 9 J/m3

observed for pre-crystallized ZLS at nano scale length mechanical testing. Similar splitting failure was also reported in micropillar compression of GaAs crystal with micropillar structure of 2.3 µm in diameter [9]. A detailed micrographs in Fig. 3a shows fragmentation and pulverization of pre-crystallized ZLS crystals due to compressive force. Figure 3b shows severe bending and microcrakings induced by the compressive force. The micropillar structures in Fig. 3 are still intact to the surface even after the compression test indicating the compressive force is insufficient to break off the structure.

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Fig. 3 Fracture micropillar structure of the pre-crystallized ZLS

At nano scale mechanical testing, the brittle nature of the pre-crystallized ZLS could be seen. For brittle material, it is challenging to understand its fracture due to its inherent brittleness nature. However, due to technological advancement it is possible to create micropillar structure of glass ceramic and understand its responses under compression test. This study shows that for a brittle material such as pre-crystallized ZLS it is possible to observe plastic deformation in form of severe bending. For macro or micro scale length mechanical testing it will be difficult to fabricate cylindrical shape of the pre-crystallized material. Further, when micro or macro compression is conducted the material will fail by brittle fracture unable to observe ductile deformation occurring before brittle fracture deformation. This suggests that micropillar compression testing at micro-scale is beneficial in investigating brittle material behaviour and fracture mechanisms.

4 Conclusion This study investigates the fracture behaviour of pre-crystallized ZLS by using micropillar compression technique, as summarize as follow: (a) Pre-crystallized ZLS had dominant brittle fracture but ductile deformation was also observed. (b) Stress drops in pre-crystallized ZLS corresponds to crack initiation and propagation induced during compression. (c) Pre-crystallized ZLS showed compression induced severe bending, microcrackings and axial crack splitting fracture behaviour. Acknowledgements The authors would like to thank staffs of Adelaide Dental School, Adelaide microscopy and School of Electrical and Mechanical Engineering at the University of Adelaide (UoA) for experimental assistance. This work was supported by the UoA Health Societies FAME Strategy Grant 2022.

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References 1. Elsaka SE, Elnaghy AM (2016) Mechanical properties of zirconia reinforced lithium silicate glass-ceramic. Dent Mater 32:908–914 2. Krüger S, Deubener J, Ritzberger C, Höland W (2013) Nucleation kinetics of lithium metasilicate in ZrO2 -bearing lithium disilicate glasses for dental application. Int J Appl Glass Sci 4:9–19 3. Ghaffari M, Alizadeh P, Rahimipour MR (2012) Sintering behavior and mechanical properties of mica-diopside glass–ceramic composites reinforced by nano and micro-sized zirconia particles. J Non Cryst Solids 358:3304–3311 4. Rinke S, Pfitzenreuter T, Leha A, Roediger M, Ziebolz D (2020) Clinical evaluation of chairsidefabricated partial crowns composed of zirconia-reinforced lithium silicate ceramics: 3-year results of a prospective practice-based study. J Esthet Restor Dent 32:226–235 5. Xiang ZX, Chen XP, Song XF, Yin L (2020) Responses of pre-crystallized and crystallized zirconia-containing lithium silicate glass ceramics to diamond machining. Ceram Int 46:1924– 1933 6. Vita Suprinity Technical and Scientific Documentation (2014) VITA Zahnfabrik H. Rauter GmbH & Co. KG, Germany 7. Howie PR, Korte S, Clegg WJ (2012) Fracture modes in micropillar compression of brittle crystals. J Mater Res 27:141–151 8. Kurdi A, Basak AK (2021) Micro-mechanical behaviour of selective laser melted Ti6 Al4 V under compression. Mater Sci Eng A 826:141975 9. Östlund F, Howie PR, Ghisleni R, Korte S, Leifer K, Clegg WJ, Michler J (2011) Ductile–brittle transition in micropillar compression of GaAs at room temperature. Philos Mag 91:1190–1199 10. Yuan J, Zhou S, Wu H, Wang Z, Zhang Y, Zhou G, Wang A (2023) Ultrahigh strength-ductility of nanocrystalline Cr2 AlC coating under micropillar compression. Scrip Mater 235:115594 11. Belli R, Wendler M, de Ligny D, Cicconi MR, Petschelt A, Peterlik H, Lohbauer U (2017) Chairside CAD/CAM materials. Part 1: measurement of elastic constants and microstructural characterization. Dent Mater 33:84–98 12. Hurle K, Belli R, Götz-Neunhoeffer F, Lohbauer U (2019) Phase characterization of lithium silicate biomedical glass-ceramics produced by two-stage crystallization. J Non-Cryst Solids 510:42–50. https://doi.org/10.1016/j.jnoncrysol.2019.01.027 13. Belli R, Lohbauer U, Goetz-Neunhoeffer F, Hurle K (2019) Crack-healing during two-stage crystallization of biomedical lithium (di) silicate glass-ceramics. Dent Mater 35:1130–1145 14. Dang C, Olugbade T, Fan S, Zhang H, Gao L, Li J, Lu Y (2018) Direct quantification of mechanical responses of TiSiN/Ag multilayer coatings through uniaxial compression of micropillars. Vacuum 156:310–316 15. Dubach A, Raghavan R, Löffler JF, Michler J, Ramamurty U (2009) Micropillar compression studies on a bulk metallic glass in different structural states. Scr Mater 60:567–570 16. Camposilvan E, Anglada M (2016) Size and plasticity effects in zirconia micropillars compression. Acta Mater 103:882–892

Characterisation of the Physico-Chemical Properties of Emulsion Polymerised Poly(N-isopropylacrylamide) Ernest Hsin Nam Yong , Kim Yeow Tshai , Ai Bao Chai , Siew Shee Lim , Ing Kong , and Eng Hwa Yap

Abstract Poly(N-isopropylacrylamide) (PNIPAM) is a functional polymeric material with various applications in industries such as drug delivery, tissue engineering, and wound dressing. PNIPAM can exist in both crosslinked and linear architectures, and the choice of synthesis method can greatly affect its material properties. While commercially available PNIPAM is costly, in-house synthesis via emulsion polymerization can be a cost-effective alternative for research purposes. This paper presents a detailed fabrication technique for synthesizing PNIPAM via emulsion polymerization, along with a thorough characterization of its physico-chemical properties. Successful synthesis of PNIPAM was confirmed through FTIR spectrums showing characteristics of amide I (C = O) stretching at 1635 cm−1 , amide II (CN) stretching at 1531 cm−1 , (−CH3 ) symmetrical deformation bend at 1388 cm−1 , (−NH) stretching at 3284 cm−1 , as well as the (−CH3 ) symmetric and asymmetric vibrations at 2876 cm−1 and 2968 cm−1 , respectively. The lower critical solution temperature (LCST) of the synthesized PNIPAM was determined using DSC analysis, measured at ~ 33 °C. The thermal responsive hydrophilic-hydrophobic phase transition behavior across LCST was demonstrated through physical observation of the PNIPAM-H2 O mixture, where a clear solution at 25 °C apparently turned into turbid at 40 °C. With Zetasizer static light scattering (SLS) technique, the measured average particle size was 250.5 nm, distributed over a narrow range of 140–520 nm, with a polydispersity index (PDI) of 0.090. The reproducibility as verified using Zetasizer dynamics light scattering technique over 3 batches of the synthesized PNIPAM revealed that the largest standard deviation for particle size and PDI were merely 4.7 nm and 0.020, respectively. With Zetasizer SLS and Debye plot techniques, the molecular weight of the synthesized PNIPAM was determined at 381,000 Da. Current E. H. N. Yong · K. Y. Tshai (B) · A. B. Chai · S. S. Lim Faculty of Science and Engineering, University of Nottingham Malaysia, 43500 Semenyih, Selangor, Malaysia e-mail: [email protected] I. Kong Department of Engineering, La Trobe University, Melbourne, VIC 3086, Australia E. H. Yap School of Intelligent Manufacturing Ecosystem, Xi’an Jiaotong-Liverpool University, Suzhou, China © The Author(s), under exclusive license to Springer Nature Singapore Pte Ltd. 2024 R. Abd. Aziz et al. (eds.), Intelligent Manufacturing and Mechatronics, Springer Proceedings in Materials 40, https://doi.org/10.1007/978-981-99-9848-7_30

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results show that the synthesized PNIPAM has similar characteristics to commercially available PNIPAM, which highlights the importance of careful synthesis and characterization to achieve desired material properties. This research can potentially pave the way for the development of customized PNIPAM with specific properties for a wide range of applications. Keywords Emulsion polymerization · Poly(N-isopropylacrylamide) · Smart polymer · Tissue engineering

1 Introduction The development of smart polymeric materials that are sensitive to external stimuli e.g., temperature, pH or light, offers great prospect to the fields of tissue engineering, biomedicine, drug delivery and wound dressing. Thermal responsive polymer, poly(N-isopropylacrylamide) (PNIPAM) exhibits a sharp and reversible phase transition between hydrophilicity and hydrophobicity across its lower critical solution temperature (LCST), reported at ~ 32 °C. PNIPAM is an attractive polymer for tissue engineering owing to its biocompatibility and the proximity of its LCST to human physiological temperatures. The thermally induce interchangeable properties between hydrophilicity and hydrophobicity of PNIPAM holds great potential for enhancing attachment of anchorage-dependent cells in its hydrophobic phase e.g., above 32 °C [1–3], whereas in its hydrophilic phase PNIPAM could facilitate a non-invasive cell harvesting mechanism through spontaneous release of cells [1, 4]. Despite its advantages, commercially available PNIPAM mostly come at high cost and have limited option in the range of molecular weight, which can limit its use. Additionally, published literatures on synthesis of PNIPAM mostly involved crosslinked PNIPAM hydrogels [5–7] and reports on synthesis of crosslinker free or linear PNIPAM are scarce. In this work, thermally sensitive uncrosslinked smart polymer PNIPAM was synthesized using the emulsion polymerization technique. In a typical polymerization processes, well-controlled environment is required to synthesize PNIPAM with good batch-to-batch reproducibility, while specific control over polymerization process parameters e.g., ratio of compositions, heating and agitation, could significantly dictate the monomer-polymer conversion and its final properties such as capability to demonstrate thermal responsiveness, molecular structure, particle size and particle size distribution, as well as molecular weight to name but a few. The resulting physico-chemical properties of the PNIPAM following emulsion polymerization were adequately characterized through a series of techniques e.g., Fourier transform infrared (FTIR) spectroscopy, differential scanning calorimetry (DSC), Zetasizer dynamic and static light scattering, and visual observation of changes in physical state demonstrating hydrophilicity and hydrophobicity of the PNIPAM across its LCST.

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2 Materials and Methods 2.1 Materials The materials used in this work include 97% assay N-isopropylacrylamide (NIPAM) with molecular weight, Mw = 113.16 g/mol as monomer, potassium persulfate (KPS) with Mw = 270.32 g/mol as the thermal initiator and 99% Sodium dodecyl sulfate (SDS) with Mw = 288.38 g/mol as surfactant. Activated carbon, celite and n-hexane were used for recrystallization of NIPAM prior to polymerization. All chemicals and dialysis sacks with molecular weight cut-off of 12,000 DA were purchased from Sigma Aldrich.

2.2 Recrystallization of NIPAM Boiling n-hexane was added dropwise to ~ 6g of NIPAM in a 100ml conical flask and continuously swirled until NIPAM crystals are observed to be fully dissolved. An additional drop of boiling n-hexane was added as excess to prevent precipitation of NIPAM. Approximately 30–50 mg of activated carbon was added to the hot NIPAM solution and swirled for 2 min to remove high molecular weight and colored impurities. 40–60 mg of celite was added and the solution swirled for further 2 min to allow adsorption of activated carbon on celite. The hot mixture was gravity filtered through a fluted filter paper into a 100 ml conical flask and the filtered solution was left to cool to allow recrystallization of NIPAM under ambient temperature. The NIPAM crystals were transferred to a petri dish and left to dry overnight in an oven maintained at 50 °C.

2.3 Synthesis of PNIPAM Recrystallized NIPAM measured ~ 2 g and SDS measured ~ 0.08 g e.g., 4% w/ w, to NIPAM monomer were added into beaker containing 200 ml distilled water (pH at ~ 5). The mixtures were subjected to magnetic stirring at 200 rpm for 5 min under an ambient environment. Upon dissolution of the recrystallized NIPAM and SDS, the solution was transferred into a 2L cylindrical jacketed reactor flask to be heated up to 80°C, under constant stirring at 100rpm using an anchor type impeller and purged with nitrogen gas for 20 min. Approximately 0.02g KPS e.g., 1% w/w to NIPAM monomer, was then added to the mixtures in the reactor flask to initiate polymerization. The temperature and stirring rate were maintained throughout a synthesis duration of 4 h. After 4 h, the mixtures were quenched in a water bath and subsequently transferred into dialysis sacks for dialysis against distilled water for 7 days, where fresh distilled water was replenished twice daily. The dialyzed mixture

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was left within a freezer for a day at − 18 °C and subsequently lyophilized in a freeze dryer for 48 h at − 59 °C and 0.012 mbar.

2.4 Characterization of PNIPAM Fourier transform infrared (FTIR) spectroscopy analysis was conducted using Perkin Elmer (Frontier FT-IR/FIR, USA) spectrometer to investigate the functional groups specific to PNIPAM at wavenumber 400–4000 cm−1 with 16 scans and 4 cm−1 resolution. Freeze dried samples were used in all analyses. Differential scanning calorimetry (DSC) analysis was conducted using the Mettler Toledo (simultaneous TGA/DSC 1, USA) instrument for characterization of the LCST. The analysis was performed in the temperature range of 30–60°C, at a heating rate of 10°C /min, under constant nitrogen gas flow of 20 ml/min. 5.6360 mg of synthesized PNIPAM sample was used for the analysis. The thermal responsive behaviour can be visually observed in a solution containing 0.01g of PNIPAM dissolved in 10ml of distilled water in a clear glass vial. The glass vial containing the PNIPAM solution was immersed in a water bath of 40 °C for 2 min and the turbidity of the solution was observed and compared to as it was at room temperature. Increase in turbidity of PNIPAm solution indicates phase separation of PNIPAM from water, which can be attributed to the phase transition of PNIPAM across its LCST. The particle size and particle size distribution were characterized in terms of average hydrodynamic diameter and its polydispersity index (PDI), respectively. These were measured by dynamic light scattering (DLS) at 173° scattering angle using the Zetasizer (Nano ZS, UK). PNIPAM solutions of 1 mg/ml dissolved in HPLC grade MeOH filtered through 0.22 µm syringe filter were used for DLS measurement. The reproducibility of synthesized PNIPAM was also evaluated in terms of consistency of its particle size and average PDI between batches, with three repeated measurements for each batch (n = 3). The molecular weight of PNIPAM was determined by static light scattering (SLS) using the Zetasizer (Nano ZS, UK). The Debye constant was computed after obtaining the change in refractive index (RI) against concentration of PNIPAM in MeOH, giving the refractive index increment (dn/dc) in the form of the gradient on a straightline plot. The set of concentrations were prepared by serial dilution from a stock solution of 0.03 g/ml, and the RIs were determined by a refractometer (Atago 1T, Japan). A Debye plot was generated with the computed Debye constant, from a set of concentrations of PNIPAM in HPLC grade MeOH. The Debye constant, K , can be given by Eq. 1. K = 4π 2 n 2

(dn/dc)2 λ4 N A

(1)

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where n represents the refractive index of solvent, λ represents the wavelength of light in vacuum, N A is the Avogadro’s number and c the concentration of the solute. The molecular weight can be obtained by determining the inverse of the y-intercept of the Debye plot.

3 Results and Discussion 3.1 Functional Group and Monomer-Polymer Conversion FTIR spectrums of recrystallized NIPAM monomer, commercial PNIPAM and the PNIPAM synthesized in this work are showed in Fig. 1. The peak at 1619 cm−1 signified characteristic of C = C stretching (indicated by vertical dashed line) is not seen in the PNIPAM spectrum, confirming polymerization of the alkenes. A new broader peak appears at 1635cm−1 belongs to characteristic of the amide I (C = O) carbonyl stretching. The characteristic peaks of the polymer at 1388 cm−1 , 1531 cm−1 , 2876 cm−1 , 2968 cm−1 , and 3284 cm−1 can be assigned to symmetrical deformation of (-CH3 ) bend, amide II (C-N) stretch, symmetric (-CH3 ) vibration, asymmetric (-CH3 ) vibration and stretching of the (-NH) group, respectively [8]. The synthesized PNIPAM show similar peaks with commercial PNIPAM further confirming PNIPAM was successfully synthesized.

Fig. 1 FTIR spectra of recrystallized NIPAM, commercial PNIPAM and synthesized PNIPAM

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Fig. 2 DSC thermogram of the synthesized PNIPAM

3.2 LCST of Synthesized PNIPAM The DSC thermogram of the synthesized PNIPAM is shows in Fig. 2. The endothermic peak at ~ 33 °C indicates the characteristic LCST of synthesized PNIPAM. This agrees well with the DSC curve of PNIPAM as reported in literature [9].

3.3 Thermal Responsive Phase Transition The thermal induced phase transition of the synthesized PNIPAM is shown in Fig. 3. At 25°C e.g., below the LCST, the synthesized PNIPAM dissolved in ddH2 O and appear to be relatively clear i.e., PNIPAM and water form a homogenous phase, Fig. 3a. When heated to 40°C, the solution turned into turbid due to the precipitation of PNIPAM from the water, Fig. 3b. This shows that the synthesized PNIPAM exhibit its characteristic thermal responsive behavior [10]. Figure 3c shows schematic of the coil-to-globule transition of PNIPAM molecules across its LCST in water. Below its LCST, PNIPAM chains associate with water molecules and appear in its coiled state, giving a clear solution. Above its LCST, PNIPAM chains self-associate into a globular state and expelling surrounding water, forming a cloudy solution.

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Fig. 3 Synthesized PNIPAM exhibiting phase transition across its LCST (a) at 25 °C, (b) at 40 °C, and (c) schematic showing coil to globule transition of PNIPAM chains in water

3.4 Particle Size and Particle Size Distribution The particle size and distribution of synthesized PNIPAM samples as characterized using SLS analysis of the Zetasizer is shows in Fig. 4. It can be observed that the particles were distributed over a narrow range of 140–520 nm. The computed average hydrodynamic diameter i.e., average particle size was 250.5 nm. The average hydrodynamic diameter fitted within the range of particle size of polymers synthesized via emulsion polymerization, ranging 10 nm to 1µm [11]. The PDI as computed from Eq. 2 was 0.090. It is worthwhile to note that PDI can range from a value of 0 to 1, measuring the spread of particle size distribution with values below 0.1 being monodispersed particles and above 0.1 signifying polydisperse particles [12]. P DI =

Fig. 4 Particle size and particle size distribution of synthesized PNIPAM

 σ 2 d

(2)

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Fig. 5 a. Diffusion of monomer from monomer reservoir into growing polymer particles across the aqueous phase, and b. Diffusion of well dispersed monomer across the aqueous phase into growing polymer particles

where σ and d represent the standard deviation and average particle diameter, respectively. Figure 5 shows schematic demonstrating the effect of monomer dispersion on the monomer diffusion and subsequent growth of polymer particles. Poor dispersion of monomer due to insufficient agitation could led to relatively limited monomer diffusion into polymer particles, forming polymer particles in a broad size range, as showed in Fig. 5a. Optimum monomer dispersion from monomer droplets could be achieved at appropriate agitation rate, which facilitate formation of uniform particle growth, as showed in Fig. 5b [13].

3.5 Batch-To-Batch Reproducibility The batch-to-batch reproducibility of synthesized PNIPAM was evaluated by Zetasizer DLS measurement of particle size and its distribution. The standard deviation for particle size were 3.5, 4.7 and 0.21 nm for batch 1, batch 2 and batch 3, respectively while the standard deviation for PDI were 0.020, 0.004 and 0.007 for batch 1, batch 2 and batch 3, respectively. The small standard deviation between each particle size and PDI measurement suggests good sample reproducibility.

3.6 Molecular Weight The molecular weight of the synthesized PNIPAM was determined using Zetasizer static light scattering (SLS). The refractive index increment (dn/dc) of PNIPAM in

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MeOH was computed to be 0.2021 ml/g, as shown by the gradient of the refractive index plotted against concentration in Fig. 6. The Debye plot, showed in Fig. 7 can be constructed as a plot with intensity of scattered light (K ·c/R) against concentration of solute, where K , c and R represents the Debye constant, concentration of solute and Rayleigh ratio (ratio of scattered light to incident light of the sample), respectively. The inverse of the y-intercept of the Debye plot gives the molecular weight of a polymer. The linear Rayleigh equation can be given by Eq. 3, where the terms A2 and Mw are the second virial coefficient and molecular weight, respectively. From the equation, as concentration becomes zero, (K ·c/R) equals 1/Mw , which makes the yintercept the inverse of molecular weight. The second virial coefficient, A2 represent the particle interaction strength and is correlated to solubility of the sample, where

Fig. 6 Plot of refractive index against concentration of synthesized PNIPAM in MeOH

Fig. 7 Debye plot of synthesized PNIPAM in MeOH. (r represent correlation coefficient)

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larger value indicates greater tendency of agglomeration. The value of A2 can be computed from 1/2 of the Debye plot gradient (since gradient = 2 A2 ). K · c/Rθ = (1/Mw + 2 A2 c)

(3)

The molecular weight of synthesized PNIPAM as computed from the Debye plot was 381,000 Da.

4 Conclusions PNIPAM was successfully synthesized via emulsion polymerization at a constant agitation rate of 100 rpm, as identified through FTIR analysis. The polymerization process shows great batch-to-batch reproducibility as indicated by statistical analysis on particle size. The synthesized PNIPAM exhibit thermal responsive behavior in ddH2 O by visual observation across its LCST, which was characterized at ~ 33 °C through DSC analysis. The synthesized PNIPAM yielded monodispersed particles distribution (PDI = 0.09) with average hydrodynamic diameter of 250.5 nm. The molecular weight of the synthesized PNIPAM as characterized by Zetasizer SLS technique was 381,000 Da. Acknowledgements This work was supported in part by the Department of Mechanical, Materials and Manufacturing Engineering, University of Nottingham Malaysia, and Ministry of Higher Education (MOHE) Malaysia under the Fundamental Research Grant Scheme (FRGS) FRGS/1/ 2017/STG05/UNIM/02/1.

References 1. Yamada N, Okano T, Sakai H, Karikusa F, Sawasaki Y, Sakurai Y (1990) Thermoresponsive polymeric surfaces; control of attachment and detachment of cultured cells. Die Makromolekulare Chemie, Rapid Communications 11:571–576 2. Lang X, Patrick AD, Hammouda D, Hore MJ (2018) Chain terminal group leads to distinct thermoresponsive behaviors of linear PNIPAM and polymer analogs. Polymer 145:137–147 3. Contreras-Cáceres R, Schellkopf L, Fernández-López C, Pastoriza-Santos I, Pérez-Juste J, Stamm M (2015) Effect of the cross-linking density on the thermoresponsive behavior of hollow PNIPAM microgels. Langmuir 31(3):1142–1149 4. da Silva RM, Mano JF, Reis RL (2007) Smart thermoresponsive coatings and surfaces for tissue engineering: switching cell-material boundaries. Trends Biotechnol 25(12):577–583 5. Marta MM, Jacek J, Juan MG, Stefan J, Sergio EM (2020) Kinetics of the thermal response of poly(N-isopropylacrylamide co methacrylic acid) hydrogel microparticles under different environmental stimuli: a time-lapse NMR study. J Colloid Interface Sci 580:439–448 6. Manja K, Majda SS, Karin SK (2012) UV Polymerization of poly(N-Isopropylacrylamide) hydrogel. Mater Technol 46:87–91

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7. Ansari MJ, Rajendran RR, Mohanto S, Agarwal U, Panda K, Dhotre K, Manne R, Deepak A, Zafar A, Yasir M, Pramanik S (2022) Poly(N-isopropylacrylamide)-based hydrogels for biomedical applications: a review of the state-of-the-art. Gels 8(454) 8. Sun B, Lin Y, Wu P (2007) Structure analysis of poly(N-isopropylacrylamide) using nearinfrared spectroscopy and generalized two-dimensional correlation infrared spectroscopy. Appl Spectrosc 61(7):765–771 9. Czakkel O, Berke B, Laszlo K (2019) Effect of graphene-derivatives on the responsivity of PNIPAM-based thermosensitive nanocomposites—a review. Eur Polymer J 116:106–116 10. Schild H (1992) Poly(N-isopropylacrylamide): experiment, theory and application. Prog Polym Sci 17(2):163–249 11. Chern C (2006) Emulsion polymerization mechanisms and kinetics. Prog Polym Sci 31(5):443– 486 12. Raval N, Maheshwari R, Kalyane D, Youngren-Ortiz S, Chougule M, Tekade R (2019) Importance of physicochemical characterization of nanoparticles in pharmaceutical product development. In: Tekade R (ed) Basic fundamentals of drug delivery. Academic Press, London, pp 369–400 13. Yong EHN, Lim SS, Gan S, Tshai KY (2019) The effect of agitation rate on the free radical polymerization of N-isopropylacrylamide. In: 4th international conference on the science and engineering of materials, Kuala Lumpur

Synergistic Effect of Electrolyte and Electrode in Nickel Cadmium Aging Battery Performances Mohd Najib Razali , Mohd Sabri Mahmud , Syahirah Syazwani Mohd Tarmizi , and Mohd Khairul Nizam Mohd Zuhan

Abstract The number of charge and discharge cycles that the battery can complete before losing its performance is called a battery life cycle. The life cycle of a battery is one of the important aspects in making sure the whole system process runs smoothly within the expected timeline. Each of the batteries has a different range of life cycle depending on their type, brand, materials of the batteries and how it is used. Several tests were conducted to compare the performance of the batteries used in the system. There were three parts of this performance test which are analyzing the physical characteristics of the Nickel–Cadmium battery, conducting characterization on electrolyte, and conducting the characterization on the electrode of the batteries which includes pH, conductivity, ICP-OES and BET analysis. The physical characteristics were based on the features and benefits of the batteries and also their technical specifications. In this study, the aging battery performances of three different rechargeable energy storage system: Battery A, Battery B, and Battery C. Each battery represents a distinct. From the result, Battery A showed the best aging battery performances compared to B and C Batteries. Battery A had the highest conductivity value and surface area from the tests conducted. Keywords Nickel–Cadmium · Life cycle · Performances · Aging

M. N. Razali (B) · M. S. Mahmud Faculty of Chemical and Process Engineering Technology, Universiti Malaysia Pahang Al-Sultan Abdullah, 26300 Kuantan, Pahang, Malaysia e-mail: [email protected] S. S. Mohd Tarmizi Ground Floor, MNR Multitech Sdn Bhd, KompleksUMPHolding, K02 Gambang, Pahang, Malaysia M. K. N. Mohd Zuhan Pusat Pengajian Diploma, Universiti Tun Hussein Onn, HabPendidikanTinggiPagoh, Jalan Panchor, KM1 Johor Pagoh, Malaysia © The Author(s), under exclusive license to Springer Nature Singapore Pte Ltd. 2024 R. Abd. Aziz et al. (eds.), Intelligent Manufacturing and Mechatronics, Springer Proceedings in Materials 40, https://doi.org/10.1007/978-981-99-9848-7_31

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1 Main Text Battery is a device that produces electrons through electrochemical reactions in a cell containing positive (+) and negative (-) terminals, called anode and cathode, respectively, and electrolyte. Chemical energy is transformed to electrical energy from potential difference between the two terminals of different material that were connected to the electrolyte [1]. A separator is often used to prevent the anode and cathode from touching [2]. In the nickel–cadmium (Ni–Cd) battery, the electrodes used were nickel oxide hydroxide and metallic cadmium. Usually, the anode is made of cadmium metal while the cathode is made up of nickel oxide hydroxide. Numerous sizes and capacities varying from portable sealed types interchangeable with carbon-zinc dry cells to large ventilated cells can be obtained from Ni–Cd batteries [3]. The utmost advantage of the Ni–Cd batteries is their abilities to convey full rated capacity at high discharge rates. Similarly, Ni–Cd batteries provide excellent cycle life and work efficiently at low temperatures with a fair capacity [4]. The Ni–Cd battery is regularly used in several applications for example in emergency lights, medical devices, alarm systems and portable electric tools. The Ni–Cd batteries are also convenient to keep and able to work in different conditions without affecting their performances [5]. Ni–Cd batteries have a relatively low energy density (45–80 W.kg- 1) among other rechargeable batteries but it has a lot of energy that gets discharged slowly. Nevertheless, it also comes with a long service life where the number of charge or discharge cycles until their capacity is decreased by 80% is 1500 cycles. Furthermore, Ni–Cd batteries have a long shelf life and are able to work firmly at low temperatures (down to -40 °C) and also produce low internal resistance [6]. The manufacturing, usage, storage, and disposal of the batteries will negatively affect the environment. Different issues may occur as the various applications involve a huge number of batteries with dissimilar types and sizes of the batteries. Unfortunately, cadmium is a highly toxic metal, and it contributes to the high amount of municipal solid waste specifically from the disposal of Ni–Cd batteries [7]. As the disposal of toxic cadmium will deteriorate the environment, all parties may reduce the usage of metal cadmium in selected sectors which align with Sustainable Development Goals (SDG) 12, responsible consumption and production. Hence, the best way to alleviate this problem is to increase the performance of the batteries by increasing the shelf life of the batteries. Three samples of Ni–Cd batteries, denoted as A, B, and C, were investigated in this paper. These batteries were retrieved from a main electricity utility company and represent different batches of Ni–Cd batteries used in their power storage system. These batteries originated from three different manufacturers. These batteries have been used at local power stations as emergency backup power and switchgear and protection systems. The problem arises when these batteries including lifecycle, performance, and durability are not standardized with guarantee and technical data provided by the manufacturers. These issues ultimately bring detrimental effect to

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the end user in term of batteries lifespan falls shorter than what is specified by the manufacturer. Shorter batteries lifespan will incur additional cost, restrict the operating time of systems reliant on Ni–Cd batteries, extra maintenance and replacement schedules and adverse effect to the environment as shorter lifespan may contribute to a higher accumulation of discarded Ni–Cd batteries [8, 9] [10]. Hence, this study is conducted to identify the factors that affect the Ni–Cd batteries performance based on electrode and electrolyte classification. This performance study has been divided into two parts which are the characterization of the electrode and the characterization of the.

2 Methodology 2.1 Liquid Electrolyte Dismantle There were three commercial batteries which were denoted as A, B, and C. The batteries were dismantled by using a metal cutter to cut the casing. Next, the electrolyte was drained from the battery into a glass jar. Each battery electrolyte was placed into a separate jar before being transferred into the centrifuge tube. The electrolyte from each battery was labeled accordingly before the analysis was conducted.

2.2 Solid Electrode Dismantle After the electrolyte was drained into the glass jar, the remaining liquid was drained to dry the inner part of the electrode. Then, the metal plates were removed from the casing. The metal plate was cut to obtain the powdery material from the positive and negative electrodes. The powder was placed into a container and labeled accordingly before further analysis was carried out.

2.3 Material Characterizations 2.3.1

PH Analysis

The electrolyte in the battery consists of potassium hydroxide solution (KOH. The equipment used for pH analysis is HQ11D Portable pH Meter for Water analysis from Hatch (Colorado, U.S.). The test was conducted with a calibrated pH meter prior to analysis.

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Conductivity Test

The ability of an electrolyte solution to conduct electricity is measured by its conductivity (or specific conductance). The S.I. unit for conductivity is Siemens per meter (S/ m). The conductivity test was carried out at room temperature (25 °C) using a portable multi-range HI8633 EC meter (Hanna Instrument, Romania) with HI76301W fourring conductivity probe and with an internal temperature sensor. The standard test method for determining the resistivity of electrical conductor is ASTM B 193–87. The instrument offers four measurement ranges from 0.0 µS/cm to 199.9 mS/cm with a ± 1% FS (percentage of full scale) accuracy. The test was carried out at T of 25.7 ± 0.1 °C. The dilution was conducted to reduce the conductivity to within the range of the equipment capacity/range. Deionized water was used as a diluent in the dilution process of KOH measurement. The dilution ratio was used in the dilution method of deionized water and electrolyte. 30 ml of electrolyte from each battery was diluted with 30 ml of deionized water for every dilution ratio.

2.3.3

Inductively-Coupled Plasma Optical Emission Spectroscopy (ICP-OES)

Perkin Elmer Inductively-Coupled Plasma Optical Emission Spectroscopy (ICPOES) at Pusat Biotropik, UMP was used to analyze elements in the samples of electrolyte and electrode. There are many analysis standards using likely similar steps to nitrate digestion. One of them that is related to the in-house method using ICP-OES is ASTMC1875. The solid samples were digested by using 6 ml of HNO3 and 2 ml of H2O2 in a vessel after being introduced to the HTC safety shield of the microwave oven. After the digestion, the solution was transferred to a 50-ml volumetric flask and diluted to mark with 2% HNO3. The aqueous solutions were directly analyzed by ICP-OES without digestion. The standard for elements was prepared by initial stock of 100 ppm by using a 50-ml volumetric flask. They were then further diluted the HNO3 into concentrations ranging from 0 to 50 ppm by using HNO3. The internal quality control by employing standard check analysis was also done by using HNO3 in volumetric flasks. The standard was checked at every 10 test solutions and the value must be below 20% of the original values. The analysis for each standard was run according to the in-house procedure provided by the supplier following the above-mentioned standard. The concentration of the samples was calculated as follows: Sample Concentration =

(Actual − Blank) × 50 × Dulution Factor ) W eight in gram

(1)

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Specific Surface Area

The specific surface area for all samples was obtained using Brunauer–Emmett– Teller (BET) Method by utilizing Micromeritics 3flex (Micromeritics, USA) surface area analyzer. The sample (~0.02 g) in fine powder form was filled in the sample tube. The sample was degassed at 230 °C in the heating mantle under nitrogen flow of at least 4 h to eliminate moisture and volatile compounds which were physically adsorbed on the material surface. Then, it was transferred to the test channel, and analysis was started after flushing with nitrogen gas for several minutes. The holder tube was immersed in liquid nitrogen to allow the adsorption of nitrogen gas onto the surface. The desorption process after adsorption quantifies the adsorbed nitrogen molecules.

3 Results and Discussion 3.1 Characterization of Electrolyte 3.1.1

PH and Conductivity

Based on Table 1, all samples showed a pH of above 14 due to the high concentration of potassium hydroxide (KOH). The conductivity of the electrolyte for the batteries was presented in Table 1 and Fig. 1. For fresh batteries, the battery A electrolyte showed the highest conductivity at 268 mS/cm while Battery C electrolyte showed the lowest conductivity at 197 mS/cm. For aging batteries, all batteries, in general, showed an increment in the conductivity value with battery A showing the highest conductivity of 292 mS/cm and similarly, battery C showing the lowest conductivity at 197 mS/cm. Battery A had the highest conductivity as compared to other brands. Table 1. pH and Conductivity Result. No

Battery

Ph

Conductivity–fresh (mS/cm)

Conductivity– aging

1

A

> 14

268

292

3

B

> 14

226

250

5

C

> 14

197

219

3.1.2

ICP OES (Elemental Analysis)

Elements in the aqueous electrolyte are water-soluble ionic substances. Elements in the alkaline electrolyte are normally from chloride substances [11]. Salts and bases of cadmium and nickel originating from electrodes are normally insoluble in water

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Conductivity (mS/cm) 350 300 250 200 150 100 50 0 A Conductivity - fresh (mS/cm)

B

C Conductivity – aging (mS/cm)

Fig. 1 Conductivity comparison of fresh samples and aging samples of the batteries

that lead to sediment formation at the bottom of the electrolyte. This was clearly seen from the physical observation of the aging batteries. All batteries use potassium hydroxide (KOH) alkaline as an electrolyte substance to transmit the electron and charges. Other elemental impurities present may pose two characteristics, either enhancing the charge storage capacity of the battery or increasing the conductivity. Further clarification can be made by comparing the performance test of the batteries. Figure 2 shows element concentrations in the electrolyte of fresh batteries. The element of potassium was dominant in all electrolytes indicating that all electrolytes were the KOH type. Nevertheless, all samples show different concentrations. The lowest content was shown by battery C while the highest content was shown by battery A. Other elements or impurities were shown accordingly. Both B samples and C samples had significant impurities. The presence of sodium in the KOH electrolyte may help increase storage but decrease the conductivity and the current of electricity. Magnesium and calcium were also present in traces of the batteries that similarly have the same effect on sodium. The ratio between MOH and potassium (Ratio OH:K) element concentration for each sample reveals the other metal that forms alkaline. Sodium hydroxide may have been used in the electrolyte in small amounts in the A sample. The use of hydroxide alkaline other than potassium in C was very significant. This may contribute to different behavior to charging and discharging of the battery. Important elements such as cadmium, nickel and cobalt from the electrode of aging batteries were not present in the electrolyte of aging batteries. Figure 3 shows the elements in an aging electrolyte. The sodium element was significantly present in all samples. Comparison between metal hydroxide and potassium reveals that all aging samples had more hydroxide than the fresh sample except C. Hence, the current from the aging battery might be decreased except the battery C. All analyses of elements in the electrodes and electrolytes will be meaningful if they were compared with test performance of the batteries as they directly affect

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Elements in Fresh Electrolytes 120000

1.6 1.4

100000

1.2 80000

1

60000

0.8 0.6

40000

0.4 20000

0.2

0

0 A K

Na

B Sr

Li

Mg

C Ca

Bi

Zn

Ratio OH:K

Fig. 2 Elements in Fresh Electrolytes

Elements in Aging Electrolytes 1.14 1.12 1.1 1.08 1.06 1.04 1.02 1 0.98 0.96 0.94

120000 100000 80000 60000 40000 20000 0 A K

Na

B Sr

Li

Mg

C Ca

Bi

Zn

Ratio OH:K

Fig. 3 Elements for Aging Electrolyte

either the capacity of the electric charges or current. Conductivity of the electrolytes was compared to the potassium element. As shown in Fig. 4 and 5, conductivity was low for fresh and aging samples of battery.

3.2 Characterization of Electrode 3.2.1

Surface Area Analysis

Nitrogen adsorption–desorption analyses were performed to determine the specific surface area of the electrode materials. Results of gas adsorption studies for fresh and aging batteries were summarized in Table 3. Generally, specific surface area

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300

96745

250 200

60850

100000 80000

1265

260

1175

20000

3390

100 2775

40000

16590

150

4062.5

60000

1577.5

Concentration (ppm)

120000

108890

346

50 0

0 A

K

B

Na

Li

C

Ca

Conductivity

132840

Fig. 4 Comparison between Concentration of Elements and the Conductivity of Fresh Electrolytes

300 250

79415

100000

200

60000

150 19382.5

80000

100 975

1550

687.5

20000

7955

40000 1272.5

Concentration (ppm)

120000

350

107645

140000

0

50 0

A K

B Na

Li

Ca

C Conductivity

Fig. 5 Comparison between Concentration of Elements and the Conductivity of Aging Electrolytes

contributes to the overall rate of charging and discharging mechanism; and the higher the surface area, the higher the electrolyte contact can be adsorbed to the material surfaces [9, 10]. For fresh positive electrodes, the A sample showed the highest surface area (219.3 m2 /g) compared to other samples, and B reported the lowest value (106.1 m2 /g). After undergoing charge–discharge cycling, the trend was similar, with. A showing the highest surface area (153.2 m2 /g) and B showing the lowest surface area (123.9 m2 /g). For fresh negative electrodes, the C sample showed the highest surface area (14.7 m2 /g) and the B sample showed the lowest surface area properties of 3.5 m2 /g. After aging, the C sample showed the highest surface area of 28.6 m2 /g, and B showed the lowest surface area of 4.3 m2 /g. For negative electrodes, a higher

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surface area will be able to facilitate faster oxygen recombination and a high rate of overcharge is possible. A comparison of the surface area before and after aging is depicted in Fig. 6. For the positive electrode, A shows a deviation of surface area shrinkage after capacity cycling. For the negative electrode, C shows an increment of surface area after capacity cycling. Other samples did not show any significant increment/shrinkage properties.

Positive Electrode BET Surface Area Ageing (m2/g)

BET Surface Area Fresh (m2/g) 250 200 150 100 50 0

A

C

B

(a)

Negative Electrode BET Surface Area Fresh (m2/g) 30

BET Surface Area Ageing (m2/g) A

20 10 0 C

B

(b) Fig. 6 Surface area comparison for fresh and aging sample for (a) positive and (b) negative electrode

348 Table 2 The tabulated surface properties of the studied materials determined from BET method analysis

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Sample

BET Surface Area (m2 /g) Fresh

Aging

C

140.8

140.3

B

106.1

123.9

A

219.3

153.2

C

14.7

28.6

B

4.3

4.6

A

8.5

10.0

Positive Electrode

Negative Electrode

4 Conclusion This study is mainly focused on the characterization of the electrolyte and electrode of the batteries. The data collected can be used to identify the effect of the battery components on the performance of the batteries. Based on the analysis conducted, it is observed that battery samples showed the best properties compared to others. Battery A has the highest conductivity value for new and aging batteries. Higher conductivity can improve the capacity of the battery at higher discharge rates as more ions can pass through at a particular time. For BET analysis, the surface area of battery A was the highest for negative electrodes while for positive electrode battery C had the highest surface area for both fresh and aging batteries. Acknowledgements The authors are grateful for the financial support given by the Universiti Malaysia Pahang (UMP) for the Internal Grant - RDU202403 entitled Material Testing and Evaluation Process for Battery Performance and Durability in TNB Distribution. The assistance provided by the Faculty of Chemical and Process Engineering Technology and Universiti Malaysia Pahang, Malaysia is also acknowledged. The authors wish to express their gratitude and appreciation for the financial support from the Ministry of Higher Education (MOHE), Malaysia for the Fundamental Research Grant Scheme (FRGSKPT-RDU160129, Reference Number: FGRS/1/2016/TK02/UMP/ 03/2 entitled Rheological and Structural Characterisation of Emulsified Modification Bitumen Synthesized from Industrial Wastes) and the Universiti Malaysia Pahang Al-Sultan Abdullah for the Internal Grant (RDU160324). The support from the Faculty of Chemical and Natural Resources Engineering and Universiti Malaysia Pahang Al-Sultan Abdullah, Malaysia are also acknowledged.

References 1. Chailleux E, Queffélec C, Borghol I, Farcas F, Marceau S, Bujoli B (2021) Bitumen fractionation: Contribution of the individual fractions to the mechanical behavior of road binders. Constr Build Mater 271:121528. https://doi.org/10.1016/j.conbuildmat.2020.121528 2. Abdullin AI, Emelyanycheva EA (2020) Water-bitumen emulsions based on surfactants of various types. J. Chem. Technol. Metall. 55:73–80

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3. A.H. Nour, R.M. Yunus, H. Anwaruddin, Water-in-crude oil emulsions: Its stabilization and demulsification,J.Appl.Sci.7(2007)3512–3517.https://doi.org/10.3923/jas.2007.3512.3517. 4. M.N. Razali, N. Mohd Ramli, K.N. Mohd Zuhan, M. Musa, A. Hamid Nour, Coating and insulation effect using emulsified modification bitumen, Constr. Build. Mater. 260 (2020) 119764. https://doi.org/10.1016/j.conbuildmat.2020.119764. 5. M.N. Razali, S.N.E. Mohd Isa, N.A. Md Salehan, M. Musa, M.A. Abd Aziz, A.H. Nour, R.M. Yunus, Formulation of emulsified modification bitumen from industrial wastes, Indones. J. Chem. 20 (2020) 96– 104. https://doi.org/10.22146/ijc.40888. 6. Mendell MJ, Macher JM, Kumagai K (2018) Measured moisture in buildings and adverse health effects: A review. Indoor Air 28:488–499. https://doi.org/10.1111/ina.12464 7. Abdel-Rahim IR, Nafady NA, Bagy MMK, Abd-Alla MH, Abd-Alkader AM (2019) Fungiinduced paint deterioration and air contamination in the Assiut University hospital, Egypt. Indoor Built Environ. 28:384–400. https://doi.org/10.1177/1420326X18765256 8. Biles CL, Cluck T, Howard A (2017) Nonsteroidal Anti-inflammatory Drugs (NSAIDS) Inhibit the Growth and Reproduction of Chaetomium globosum and Other Fungi Associated with Water-Damaged Buildings. Mycopathologia 182:1025–1036. https://doi.org/10.1007/s11046017-0188-7 9. M.N. Razali, M. Luqman Hakim, M. Effendi, M. Musa, R.M. Yunus, Formulation of bitumen from industrial waste, ARPN J. Eng. Appl. Sci. 11 (2016) 5244–5250. 10. M.N. Razali, T.A.P. Asaithamby, N. Mohd Ramli, M.K.N. Mohd Zuhan, M. Musa, A. Hamid Nour, Rheological Characterization of Emulsified Bitumen from Industrial Waste, Adv. Mater.Res.1163 (2021) 148–157. https://doi.org/10.4028/www.scientific.net/amr.1163.148. 11. Hou S, Chen C, Zhang J, Shen H, Gu F (2018) Thermal and mechanical evaluations of asphalt emulsions and mixtures for microsurfacing. Constr Build Mater 191:1221–1229. https://doi. org/10.1016/j.conbuildmat.2018.10.091

Behaviour of Palm Oil Fuel Ash (POFA) as Partial Material Replacement in Oil Palm Shell (OPS) Reinforced Concrete Beam Sharifah Syed Mohsin, Mohd Asmawi Md Desa, Khairunisa Muthusamy, Nur Farhayu Ariffin, Fadzil Mat Yahaya, and Saffuan Wan Ahmad

Abstract Investigation on potential of using palm oil fuel ash (POFA) as part of cement, sand or coarse aggregate replacement in concrete is not new. However, most of the published work has focused on the mechanical properties even though determining the potential of using POFA as a material replacement in oil palm shell (OPS) concrete, especially at the structural level, is required to fully utilize the waste produced from the palm oil industry while also conserving the natural resources needed to produce concrete. Thus, this paper presents the behavior of POFA as a partial material in OPS reinforced concrete beams. In this work, all the gravel is 100% replaced with OPS to produce lightweight aggregate concrete. Then, POFA is used as 20% of cement, sand or OPS replacement in the concrete mixture and cast into cubes and reinforced concrete beams. The beam dimensions cast are 150 mm width, 200 mm height, and 1500 mm long, tested as simply supported under fourpoint bending test. From the results, POFA as cement replacement in OPS reinforced concrete beam showed higher strength and ductility compared to the control beam, whereas comparable results are obtained from POFA as OPS replacement in the OPS reinforced concrete beam. Keywords Palm oil fuel ash · Oil Palm shell reinforced concrete beam · Material replacement · Structural behaviour

S. Syed Mohsin (B) · K. Muthusamy · N. F. Ariffin · F. Mat Yahaya · S. Wan Ahmad Faculty of Civil Engineering Technology, Universiti Malaysia Pahang Al-Sultan Abdullah, Gambang, 26300 Kuantan, Pahang, Malaysia e-mail: [email protected] M. A. Md Desa BYG Architecture, 12A, Arratoon Road, Georgetown, 10050 Penang, Malaysia © The Author(s), under exclusive license to Springer Nature Singapore Pte Ltd. 2024 R. Abd. Aziz et al. (eds.), Intelligent Manufacturing and Mechatronics, Springer Proceedings in Materials 40, https://doi.org/10.1007/978-981-99-9848-7_32

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1 Introduction 1.1 Oil Palm Shell (OPS) Concrete Concrete is one of the most versatile construction materials but has a high density ranging from 2200 to 2600 kg/m3 . The heavyweight of conventional concrete leads to difficulties in transportation, handling, and reduced stability in load-bearing elements. These issues have driven interest in developing structural lightweight concrete with lowered density while maintaining adequate strength. One way of lowering concrete density is by using lightweight aggregates rather than conventional (gravel or stones) aggregates. Agricultural waste products like oil palm shell (OPS) have shown good results [1–3] and is one of the potential alternatives to be used as sustainable light-weight aggregate. OPS is abundantly available in tropical region, such as Malaysia as by-product of palm oil productions. It has low bulk density and high toughness. The present work investigates the full replacement of conventional coarse aggregates with OPS in concrete mixtures. Rather than partial substitution, this study utilizes OPS as the sole coarse aggregate component.

1.2 Palm Oil Fuel Ash (POFA) in OPS Reinforced Concrete Palm oil fuel ash (POFA) is a solid residue that is generated in substantial quantities as a byproduct from combustion processes in palm oil mills. In palm oil production, the leftover palm fibers and shells are usually disposed of and burned off. The burning of this agricultural waste produces an ash known as palm oil fuel ash or POFA. As global palm oil production continues to increase, so does the output of this residual ash material. Characterization studies have revealed the significant pozzolanic properties of POFA, which lends to its potential application as a supplementary cementing material in concrete mixes [4–6]. A pozzolan is a siliceous material that contains reactive silica, which can react with calcium hydroxide released during cement hydration to form additional strengthenhancing calcium silicate hydrate gel in the concrete matrix. Chemical analysis shows POFA contains over 50% silicon dioxide (SiO2 ) content in the form of amorphous silica, as well as alumina and iron oxide [7, 8]. Its composition allows it to meet international standards for classification as a pozzolanic material, typically between Class C and Class F. This makes POFA a viable partial substitute for Portland cement in concrete from a chemical perspective. Previous investigations on incorporating POFA as a replacement material for portions of cement [4–8] or sand [9–12] in concrete mixtures have demonstrated positive results. Replacement levels of 5–20% have shown improved strength and durability properties compared to plain concrete. The promising outcomes indicate the strong potential for POFA’s usage as a sustainable supplementary material to partially

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replace traditional concrete ingredients. Wider adoption would reduce dependency on natural resources and make productive use of the abundant agricultural waste. However, most studies have focused on the material performance of POFA as partial cement or sand replacement in mortar [6] or material level [4, 5, 9, 11], with limited work published regarding structural behavior. This paper helps fill that knowledge gap by presenting results investigating the use of POFA as partial replacements for cement, sand and oil palm shell (OPS) in structural OPS reinforced concrete beams. The structural impact provides crucial insight for safer incorporation of POFA in construction applications.

2 Methodology 2.1 Materials Four concrete mixtures were considered in the present work. The mixtures consisted of cement, sand, water and OPS as the coarse aggregate, as shown in Table 1. No gravel was included in any of mix design. Instead, OPS obtained from Kilang Sawit Felcra, Maran Berhad was used at 100% as the coarse aggregate to produce lightweight aggregated concrete (LWAC). Additionally, the POFA utilized in this study was obtained from Kilang Sawit Sungai Jernih, Pahang. The POFA was classified as Class C pozzolanic ash in accordance to ASTM C618-08 [13]. Ordinary Portland Cement (OPC) and river sand were used for the concrete mixture. Superplasticizer was also added to improve the workability of the concrete, with a designed slump of 85 mm. Table 1 Mix design OPS reinforced concrete beam Control (kg) (B1) Material

POFA replacement (kg) Cement (B2)

Sand (B3)

OPS (B4) 25.6

OPS

32

32

32

POFA

0

8.7

15.14

6.4

OPC

43.5

34.8

43.5

43.5

Water

19.58

19.58

19.58

19.58

Sand

75.69

75.69

60.55

75.69

Superplasticizer

0.445

0.445

0.445

0.445

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2.2 Preparation Process The experimental methodology began with preparation of the key materials—oil palm shell (OPS) and palm oil fuel ash (POFA). The collected OPS was pre-processed by washing, rinsing and air drying under sunlight for 24 h to remove surface dust and oil residue. The dried OPS was then sieved using a 5 mm mesh to obtain the target aggregate size fraction. Only OPS retained on the 5 mm sieve was used as coarse aggregate in the concrete mixtures. While previous studies recommended OPS sizes of 10–15 mm, it was difficult to obtain OPS in this range during the current work. This is attributed to advances in oil palm cultivation focused on generating smaller fruits with higher oil yield. Thus, the present study was limited to OPS with minimum diameters of 5 mm. Similarly, the collected POFA was oven-dried for 24 h to eliminate moisture before sieving through a 300 μm mesh tray to remove larger particulates. The POFA was then finely ground for 30,000 cycles in a grinding machine to comply with fineness specifications for Class C pozzolan as per ASTM C618-08. This processed POFA could then be incorporated as a partial cementitious material replacement. For the experimental phase, each concrete mixture was cast into six 150 mm cubes for compression tests and a beam of 150 mm width, 200 mm height, and 1200 mm length for structural testing. The beam formwork was fabricated and assembled within the Concrete Laboratory at Universiti Malaysia Pahang. Longitudinal tension and compression reinforcement of 2H12 bars were provided. The shear reinforcement consisted of R6-50 stirrups at 150 mm spacing in the end spans, and R6-200 stirrups in the mid-span.

2.3 Testing Three experimental tests were performed in this study. First, to evaluate the fresh concrete, a slump test was conducted per BS EN 12,390-2 [14] to assess workability after mixing and before casting. Second, hardened concrete cube specimens were tested for compressive strength at 7 and 28 days of age as per BS EN 12,390-3 [15]. The cubes were demolded after 1 day and cured in water tanks up to the test date. Finally, flexural testing of the reinforced concrete beams was carried out on day 28 using a four-point bending setup shown in Fig. 1. The load was applied under displacement control at a slow monotonic rate compliant with BS EN 12,390-5 [16]. The beams were cured identically to the cubes before testing.

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Fig. 1 Reinforcement detailing and loading arrangement

3 Results and Discussion 3.1 Compressive Strength The compressive strength results obtained from cube testing are presented in Fig. 2. Evidently, all specimens incorporating 20% POFA as a partial replacement exhibited higher compressive strengths relative to the control on both the 7th and 28th day. The control specimen B1 attained 11.69 and 12.79 MPa on days 7 and 28, respectively. While the mix design targeted 15 MPa, this was not achieved for the control likely due to batch-to-batch variations and a larger OPS size distribution than prior studies. Remarkably, the POFA specimens all surpassed 15 MPa by day 28. Specimen B2, with 20% cement replacement by POFA, showed optimal performance with 17.23 and 20.76 MPa on days 7 and 28. Both the cement and sand replacement mixtures exceeded 15 MPa even by day 7. These results indicate B2 and B4 would satisfy minimum strength requirements of 17 MPa for structural concrete applications [1, 3].

3.2 Load—Deflection Curve of OPS Reinforced Concrete Beam The results of the four-point bending test on the OPS reinforced concrete beams are presented as load–deflection curves as shown in Fig. 3. Key parameters extracted from the load–deflection curves, as summarized in Table 2, include load at yield (Py ) and its corresponding deflection (δy), maximum load (Pmax ) representing load-carrying capacity and its deflection (δmax ), ultimate load (Pu) and associated deflection (δu), and the ductility ratio (μ). It can be observed that 20% replacement of POFA in

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7 Days

Compressive strength (MPa)

25

28 Days

20.76 20 15

17.23 12.79 11.69

16.22 14.47

19.09 16.68

10

B1 (control)

B2 (cement replacment)

B3 (sand replacement)

B4 (OPS replacement)

Fig. 2 Compressive strength of the OPS concrete on 7th and 28th days

sand, cement, and oil palm shell increased the load at yield (Py ) and maximum load carrying capacity (Pmax ) of OPS reinforced concrete beams. For beam B2 (cement replacement), the increases in Py and Pmax were 54% and 7%, respectively, compared to beam B1 (control). Moreover, beam B2 exhibited the highest ultimate load at failure compared to the other beams. This is attributed to the pozzolanic effect of POFA as a cement replacement in the OPS reinforced concrete. Beam B3 (sand replacement) saw Py increase by 48% but Pmax decrease slightly by 5%, compared to beam B1. Nevertheless, only beams B2 and B3 exhibited significantly higher ductility, with μ increasing by 69% and 126% for B2 and B3,

Fig. 3 Load–deflection curves of OPS reinforced concrete beam containing POFA

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Table 2 Strength and ductility from load–deflection curve Type

Py

δy

Pmax

δmax

Pu

δu

μ = δu / δy

B1

44.78

5.20

77.72

12.20

75.80

14.40

2.77

B2

68.89

6.04

82.97

27.98

81.30

28.33

4.69

B3

66.06

5.73

73.95

34.10

72.92

35.91

6.27

B4

62.11

5.88

78.99

8.98

77.88

10.70

1.82

respectively. This demonstrates that POFA can be used as a partial cement or sand replacement in OPS reinforced concrete beams and structural elements. Additionally, beam B4 showed increases in Py of 39% and Pmax of 2% compared to beam B1. However, beam B4 displayed the lowest ductility and failed prematurely compared to the control beam B1, indicating it may not be suitable for construction applications. This is because reinforced concrete beams must possess both adequate strength and ductility to function as robust structural members.

3.3 Cracking and Mode of Failure The first crack loads and failure modes of the tested beams are summarized in Table 3. The control beam B1 cracked initially at the lowest load of 17.45 kN. Incorporating 20% POFA as a partial replacement resulted in higher first crack loads, indicative of the crack propagation resistance imparted by the pozzolanic POFA. Beam B2 with cement replacement exhibited the maximum first crack load of 51.97 kN, followed by 33.08 kN for B3 (sand replacement) and 28.88 kN for B4 (OPS replacement). The cracking patterns and failure modes shown in Fig. 4 reflect the first crack results. Beams B2 and B3 failed in a ductile manner with extensive flexural cracking starting from the tensile face of the midspan prior to ultimate failure. In contrast, beams B1 and B4 developed some initial flexural cracks at midspan but experienced abrupt shear failures. As the load increased, more pronounced cracking formed between the loading points and supports due to high shear stresses. The replacement of cement or sand by POFA appears to enhance flexural capacity and ductile failure response.

Table 3 First cracking load and type of failure

Beam

1st crack load (kN)

Mode of failure

B1

17.45

Shear

B2

51.97

Bending

B3

33.08

Bending

B4

28.88

Shear

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Fig. 4 Cracking pattern of the beams a B1, b B2, c B3, and d B4 at failure

4 Conclusion This study evaluated POFA as a partial replacement for cement, sand, and OPS in OPS-reinforced concrete beams. The results demonstrate that POFA is most effectively utilized as a cement replacement, which significantly enhanced the load at first crack, load-carrying capacity, ductility, and crack propagation resistance until failure. The pozzolanic reactivity of POFA complements the cement hydration in the OPS beams, conferring these improvements. In contrast, partially replacing OPS with POFA is not recommended for OPS-reinforced beams, although the strength increased over the control beam B1. No gains occurred in ductility or cracking behavior, as beam B4 exhibited a brittle shear failure like B1. In summary, the ideal application of POFA is as a 20% partial cement replacement in OPS-reinforced concrete beams, providing strength and ductility benefits.

References 1. Aslam M, Shafigh P, Jumaat MZ (2016) Oil-palm by products as lightweight aggregate in concrete mixture: a review. J Cleaner Prod 126:56–73

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2. Mehdi M, Shafigh P, Aslam M (2018) Optimum oil palm shell content as coarse aggregate in concrete based on mechanical and durability properties. Adv Mater Sci Eng 2018, Article ID 4271497 3. Syed-Mohsin SM, Azimi SJ, Namdar A (2014) Behaviour of oil palm shell reinforced concrete beams added with kenaf fiber. Appl Mech Mater 567:351–355 4. Altwair NM, Kabir S (2010) Palm oil fuel ash (POFA): An environmentally-friendly supplemental cementitious material for concrete production. In: International conference on material science and 64th RILEM annual week in Aachen—MATSCI, pp 234–247 5. Ali N, Mohd Sobri MHA, Hadipramana J, Abdul Samad AA, Mohamad N (2017) Potential mixture of POFA and SCBA as cement replacement in concrete—a review. MATEC Web of Conferences 103:01006 6. Hamada HM, Yahaya F, Muthusamy K, Humada A (2019) Effect of incorporation POFA in cement mortar and desired benefis: a review. IOP Conf Ser: Earth and Environ Sci 365:012060 7. Muthusamy K, Zamri NA (2015) Short term investigation on sulphate resistance of oil palm shell lighweight aggregate concrete containing palm oil fuel ash as partial cement replacement. Res J Appl Sci Eng Technol 11(1):91–94 8. Pone J, Ash A, Kamau J, Hyndman F (2018) Palm oil fuel ash as a cement replacement in concrete. Modern Approaches on Mater Sci 1(1):4–8 9. Hashim NH, Muhd Sidek MN, Md Noor N, Roselli SR, Mohd Yusoff MA, Saiful Bahari MFS (2019) Utilisation of palm oil fuel ash (POFA) as sand replacement for fresh and hardened concrete by using powder and liquidation method. J Phys: Conf Ser 1349 10. Mat Azhar NAS, Hashim NH, Muhd Sidek MN, Abdul Halim NAI, Newman A, Mohd Fauzi MA (2022) Effect of low inclusion of palm oil fuel ash (POFA) as partially sand replacement to the performance of mortar. J Build Pathol Rehab 7:41 11. Hashim NH, Muhd Sidek MN, Roselli SR, Yahaya MA, Hasan D, Ding JD (2022) Potential of palm oil fuel ash (POFA) as partially sand replacement on mortar performance. AIP Conf Proc 2532:040007 12. Al-Shwaiter A, Awang H, Khalaf MA (2022) Performance of sustainable lightweight foam concrete prepared using palm oil fuel ash as sand replacement. Constr Build Mater 322:126482 13. ASTM C618–08 (2008) Standard specification for coal fly ash and raw or calcined natural pozzolan for use in concrete. West Conshohocken 14. BS EN 12390–2 (2000) Testing hardened concrete—workability of test specimens. British Standard Institution, London 15. BS EN 12390–3 (2000) Testing hardened concrete—compressive strength of test specimens. British Standard Institution, London 16. BS EN 12390-5 (2000) Testing hardened concrete—flexural strength of test specimens. British Standard Institution, London

Crash Performance of Automotive Bio-Composite Crash Box Using Finite Element Analysis S. Y. Soh, C. S. Hassan , M. F. M. Nazer , A. R. Abd Hamid , L. J. Yu , N. F. Abdullah , N. Abdul Aziz , and R. A. Ilyas

Abstract Sustainable materials have been increasingly used in the automotive industry for low-load demanding applications such as dashboards, non-structural interior components, and spare tire covers. The adoption of bio-composites has environmental benefits because their lightweight properties contributed to reduced vehicle weight, resulting in less fuel consumption and car exhaust emissions in the long run. Natural fibres, on the other hand, had but have yet to be adopted in highload automotive applications due to a lack of current research. This paper investigates the crashworthiness of oil palm empty fruit bunch (OPEFB) fibre/epoxy and kenaf fibre/epoxy bio-composites as materials for thin-walled hexagonal crash boxes and compares the results to conventional metal and synthetic fibre composite crash boxes. The simulation is based on the Research Council for Automobile Repairs (RCAR) low-speed structural crash test protocol, whereby the impact occurs at a speed of 15kmh-1. When compared to steel, the bio-composites improved specific energy absorption by 197% for OPEFB fibre/epoxy and 209% for kenaf fibre/epoxy composites but lacked the material strength to achieve higher impact energy absorption and a structured folding mechanism. In comparison, kenaf fibre/epoxy composite outperforms OPEFB fibre/epoxy composite in terms of crashworthiness, with 188% higher crush force efficiency and 122% higher energy absorbed. Keywords Crash Box · Biocomposite · Crashworthiness · FEA

S. Y. Soh · C. S. Hassan (B) · M. F. M. Nazer · A. R. A. Hamid · L. J. Yu · N. F. Abdullah Faculty of Engineering, Technology and Built Environment, UCSI University, 56000 Cheras, Kuala Lumpur, Malaysia e-mail: [email protected] N. A. Aziz Department of Mechanical and Manufacturing, Universiti Putra Malaysia, 43400 Serdang, Malaysia R. A. Ilyas Faculty of Engineering, Universiti Teknologi Malaysia, Johor Bahru, 81310 Johor, Malaysia © The Author(s), under exclusive license to Springer Nature Singapore Pte Ltd. 2024 R. Abd. Aziz et al. (eds.), Intelligent Manufacturing and Mechatronics, Springer Proceedings in Materials 40, https://doi.org/10.1007/978-981-99-9848-7_33

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1 Introduction Vehicle front end are designed with crumple zone that collapse in layers and absorb impact during deformation. The deformation provides a cushion to reduce the time required for the automobile to reach complete halt; therefore, exerting less impact on passengers, potentially saving their lives. Automotive crash box is a critical component included in front bumper system for absorbing the impact energy. The performance is assessed based on its crashworthiness, which demonstrates the ability to absorb energy during an impact in a safe manner to protect occupants. Crashworthiness properties are defined as the response to an impact load and are typically measured using energy absorption (EA) and specific energy absorption (SEA) capability. EA is the measure of energy absorbed during collision while SEA denotes the energy absorbed per unit mass of the absorber. EA and SEA can be calculated as Eqs. (1) and (2) [1]: S

E = ∫ F(x)d x

(1)

0

where s is the crash displacement and F denotes the impact force; and SE A =

EA M

(2)

where M represents the total mass of the structure. For energy absorbing structure, the higher the SEA the better. The peak load on a component is the maximum load that a component can withstand without experiencing severe permanent deformity. A high peak load is ideal for slow speed and low-energy impacts to avoid irreversible deformation, which would be considered as structural damage. Some important characteristics for a good energy absorption property is the difference between peak load and mean load should be small, to reduce sudden deceleration during impact. The mean load and crushing distance should be high to absorb more energy and increase duration of impact. Mean load (Fmean ) can be calculated by dividing energy absorbed with deformation displacement shown in Eq. (3) [2]. Fmean =

EA x

(3)

Crush force efficiency (CFE) is defined as the ratio of the mean load over peak load. Mean and peak loads are vital to evaluate because they are closely associated to the deceleration which the vehicle’s occupants will experience. If CFE ratio is approximately equal, the structure is crushing at a level close to the peak load, reducing deceleration fluctuations. Meanwhile, if CFE ratio is not nearly constant, there will be abrupt changes in deceleration, which is detrimental for a vehicle’s safety considerations. In general, the closer the CFE ratio approaches one, the greater the energy absorption of the structure. Crush force efficiency can be calculated with

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Eq. (4) [2]. CFE =

Fmean × 100% F peak

(4)

Compared to conventional materials such as steel, bio-composites are known to have low weight-high strength ratio. A 5% to 10% decrease in automotive weight leads to 1.3 to 3.6% fuel savings respectively, by mass reduction it also decreases fuel consumption, car emissions and air pollution. Several studies have studied the effectiveness of various bio-composites with fibers such as kenaf, oil palm, coir, rice husk, and abaca as substitution for conventional material in automotive crash box. Rusu et al. [3] noted that despite the promising benefits of bio-composites theoretically in low load applications such as door panels and spare tire covers, further research and testing is needed to prove the capability of bio-composites to cope with highly demanding applications in short term scenario such as high thermomechanical performance required in an impact. Consistency of bio- composites results are also an issue. As example from research by Rozite et al. [4] shows despite flax fiber having better theoretical mechanical stiffness property compared to glass fiber, the variation of results of flax fiber fluctuated between 50 and 100 GPa while Eglass maintained consistency of around 72 GPa. For that reason, the adoption of bio-composites in automotive for demanding applications are progressing relatively slow. Shaik Dawood et al. [5] discovered significant advantage of composite over conventional metals is specific energy absorbed (SEA) due to the composite’s excellent strength to weight ratio. The study shows that by carefully selecting design parameters, energy absorption capabilities of crash boxes built of composite materials can be increased to a level comparable to that of conventional metal tubes. Hassan et al. [6] compared crashworthiness of aluminium and OPEFB fibre/epoxy composite as bumper beam material and observed that the composite impact time was increased by 89%, resulting in lesser deceleration. Several other studies [7–12] have also shown that natural fibre has a high potential for energy absorption application. The primary goals of the system at low speeds up to 15 km/h is to limit car parts damage and minimize repair costs. At medium speeds between 15 and 40 kms per hour, the primary objective is to safeguard pedestrians caught in the accident. Lastly, at high speeds greater than 40 km/h, the main concern is to direct impact forces propagating through the car body in such a way that a planned deformation occurs and does not implode [13]. The Research Council for Automobile Repairs (RCAR) conducted low velocity impact test by impacting a car into a barrier at a speed of 15 km per hour [14]. Under RCAR test conditions, crash box should deform and prevent damage to structural parts such as engine, longitudinal beam, and driver’s compartment. Crash box can be easily replaced, resulting in a significant reduction in repair costs. Following a low-speed frontal impact, only cheaper components such as the bumper rail, crash box, and interconnected components like radiator should be repaired. In this paper, simulation work was done to investigate the feasibility of using OPEFB and kenaf fiber to reinforce epoxy to form a bio-composite as automotive

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crash box material in low velocity impact of 15 km/h and compared to synthetic composites of carbon fiber/epoxy as well as conventional metal 1018 grade steel.

2 Methodology The material properties of the conventional metal, 1018 steel, carbon fibre reinforced epoxy composite, OPEFB fibre reinforced epoxy composite and kenaf fibre epoxy composites used in this analysis were adapted from previous experimental studies [6, 15, 16] and the rule of mixture (ROM) calculation. The crash box was modeled as a hexagonal thin-walled tube, as shown in Fig. 1, and subjected to a free-falling impactor mass. The thin-walled hexagonal tube was chosen for the analysis because it has been shown to absorb the most energy when compared to other cross-sectional shapes [17]. The hexagonal tube was given dimensions of 50mm on each side, a total perimeter of 300mm, a length of 350mm, and a thickness of 2mm. A rigid wall was created and placed directly above the z-axis on the model, leaving a 0.01 mm gap between the two objects, to serve as the impactor. The impactor was modeled with only one allowable translational displacement and all other translational and rotational degrees of freedom were fixed. The impact velocity of the impactor along the z-axis going downwards was set to 15 kmh−1 [14] in accordance with the Research Council for Automobile Repairs (RCAR) low-velocity impact

Fig. 1 Hexagonal tube model

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Fig. 2 Fiber orientation of hexagonal tube of 0 degree to the load

protocol. The mass was assumed to be 25% of that of a compact car weighing 1000 kg, giving the impactor a total mass of 250 kg. This estimate is based on a single crash box absorbing at most 25% of a car’s mass. The crash box’s bottom was constrained in all translational and rotational directions. A "Mixed" mesh type was used with a 4 mm element size, resulting in a hexagonal tube with 13,356 elements and 1335 nodes and a rigid plate with 12,250 elements and 1425 nodes. The “Automatic Surface to Surface” contact algorithm was used to define the contact interaction between the tube and the rigid plate while “Automatic Single Surface Contact” was used to define contact between the tube body itself. The Coulomb friction coefficient was set to 0.1 for all contact surfaces. Figure 2 depicts the fibre orientation for the hexagonal tube, which was oriented 0 degrees to the load and parallel along the axial crushing axis.

3 Results and Discussion 3.1 Structural Deformation Figure 3 displays the deformation characteristics of the four types of crash box materials. It can be observed that only the rigid impactor in steel crash box simulation rebounded after axial impact of 18.5 ms and a crash box displacement of 37.3 mm. Carbon fiber/epoxy composites crash boxes continued to absorb energy and deform by 129 mm until 70.7 ms when the impactor started to rebound. Lastly, both OPEFB fibre and kenaf fibre reinforced epoxy composites crash boxes did not rebound the impactor with impact simulation lasted for a maximum of 91.4 ms and 85.8 ms

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respectively. Both crash boxes were nearly completely crushed with 349 mm of displacement for OPEFB fibre/epoxy composites, and 334 mm displacement for kenaf fibre/epoxy composites. The quick rebound of the impactor in steel simulation correlates with the high stiffness of the material and high initial peak load absorbed of 246 N. Meanwhile OPEFB fibre/epoxy, kenaf fibre/epoxy and carbon fiber/epoxy composites continue to absorb load and store energy through plastic deformation for long duration. The steel material in Fig. 3a folded extensionally at the upper region of the tube. The deformation resembles a folding mechanism of the tubes, giving a progressive collapse. OPEFB fibre/epoxy, kenaf fibre/epoxy and carbon fibre/epoxy composites on the other hand showed irregular folding patterns throughout their deformation length. All materials did not exhibit significant buckling, torsion, or fragmentation, which would result in poor crashworthiness performance. By solely observing the deformation characteristics, it can be seen that OPEFB fiber/epoxy, kenaf fiber/epoxy, and carbon fiber/epoxy composites outperformed other materials by lengthening the crash duration, thereby promising a reduction in the inertia effect experienced by the passengers. Figure 3b shows deformation pattern for the carbon fibre/epoxy composites crash box. The crushing mechanism of the carbon/epoxy crash tube seems to involve inward collapse of the nearest region to the impact, followed by compression of the deformed region before initiating another inward collapse, and this deformation process is then repeated. The deformation of OPEFB fibre/epoxy and kenaf fibre/epoxy crash tubes, shown in Fig. 3c and d respectively, reveals severe structural collapse and unstructured folding when compared to steel and carbon fibre/epoxy tubes under the same loading conditions. The lack of stiffness allowed both bio-materials composites to deform through multiple irregular folding patterns quite easily, resulting in significantly less energy absorption compared to steel, which absorbed the energy in one folding sequence. The main difference between these two crash boxes is the region from which deformation starts occurring. The OPEFB composite deformed from the upper region, while the kenaf composite started deforming from the bottom region near the fixed bottom nodes.

3.2 Force–displacement Characteristics Force–displacement diagrams for steel, OPEFB fibre/epoxy, kenaf fibre/epoxy and carbon fiber/epoxy materials tested in this study are presented in Fig. 4a. From these figures, it is noticeable that the energy (area under the graph) absorbed by the crash boxes due to dynamic axial loading for steel is the highest, followed by Carbon Fibre/ Epoxy, kenaf fibre/epoxy and lastly OPEFB fibre/epoxy composites. It can be observed closer in Fig. 4b, that the line for both steel and carbon fibre/ epoxy composites crash boxes curved back at around 37.3mm and 129 mm respectively. The resultant displacement refers to the displacement of the rigid impactor

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Fig. 3 Front view deformation behavior a Steel, b Carbon fibre/epoxy, c OPEFB fibre/epoxy, and d Kenaf fibre/epoxy crash box

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Fig. 4 Force displacement graphs

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which is assumed to be in full contact with the crash box as the crash box crushes. The line curving backward represents the rebounding of the impactor. Even with a significantly shorter impact time at 18.5 ms and a. shorter crushing distance of 37.3 mm, steel material was able to absorb the most energy due to its high young modulus value among all four materials at 195.8 GPa. A high Young’s modulus value contributes to the crash box being stiffer and more inelastic, it requires more energy absorbed to plastically deform at a lesser deformation length. Figure 4c compares OPEFB fibre/epoxy and kenaf fibre/epoxy composites crash boxes’ force–displacement curve which reveals both materials continued to be displaced until the simulation limit. The available length of 350mm is not sufficient for the deformation to halt the impactor. Although both graphs seem to have a very similar area under the force–displacement graph, investigation of internal energy proved the kenaf fibre/epoxy composites crash box to have a slight edge. It is observed that for both bio-composites tubes, there is a spike in energy absorption as displacement gets larger. This is due to the increased energy needed to further compress an already partially compressed crash box nearing the end of impact time.

3.3 Energy Absorption Performance The maximum energy absorption is found by plotting internal energy as a function of time, as shown in Fig. 5. It is observed that steel crash box has the highest maximum energy absorption at 2.12 kJ followed by carbon fibre/epoxy composites crash box at 2.02 kJ, kenaf fibre/epoxy composites crash box at 782 kJ and OPEFB fibre/epoxy composites crash box at 638 J.

Fig. 5 Internal energy-time graph of steel, carbon fibre/epoxy, opefb fibre/epoxy and kenaf fibre/ epoxy crash box

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Table 1 Energy absorption capacity of different crash box materials Material

Mass (kg) Maximum energy absorption Specific energy absorption (J/ (J) kg)

Steel

1.5162

2120

1398.25

Carbon fibre/epoxy

0.3247

2020

6221.03

OPEFB fibre/epoxy 0.2316

638

2754.31

Kenaf fibre/epoxy

782

2931.38

0.2668

Table 1 provides a summary of the energy absorption capabilities of all crash box profiles. When the energy absorbed is compared to the weight of each material, carbon fibre/epoxy composite has the best specific energy absorption capability with 6221.03 J/kg, followed by kenaf fibre/epoxy composites at 2931.38 J/kg, OPEFB fibre/epoxy composites at 2754.31 J/kg, and steel with 1398.25 J/kg. Specific energy absorption capability of all three composites are higher than steel due to a lower density and lower young’s modulus leading to a longer crushing distance. Carbon fibre/epoxy composite showed the best strength-to-weight ratio with a good balance between material strength and stiffness. Carbon fibre/epoxy composites have the highest SEA increase compared to steel at 4.44 times. Both OPEFB fibre/epoxy and kenaf fibre/epoxy composites have a similar SEA increase to steel at around 2 times.

3.4 Crush Force Efficiency Table 2 displays the peak and mean load, as well as the crush force efficiency (CFE) of each of the four materials. To ensure occupant safety, the initial peak crush force, which is the source of high-intensity deceleration, must be thoroughly investigated. It can be seen that the force required to initiate damage is lower for bio-composites crash box materials than for carbon fiber/epoxy composites and steel crash boxes, which is desirable because a high amount of force eventually leads to a higher level of deceleration on passengers [7]. The CFE for OPEFB fibre/epoxy composites crash box however was found to be approximately 25% lower than the CFE for carbon fiber/epoxy composites and 73% lower steel crash box, respectively. Kenaf fiber/ epoxy composites, on the other hand, had a higher CFE by approximately 42% than carbon fiber/epoxy composites and a lower CFE by approximately 49% than steel crash box. This has prompted a thorough evaluation of the structural configuration of the bio-composites crash box, as, while it exhibited longer impact duration and lower peak force than conventional crash box material, the low CFE may indicate a random change in the mode of deformation during the crash analysis, and thus structural components may fail catastrophically. Lower CFE also indicates a drop in the crushing force after the first peak which then resulted in the loss of total energy absorbed [18], as depicted in Table 1.

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Table 2 Crashworthiness parameters of different crash box materials Material

Peak load (N)

Mean load (N)

Crush force efficiency (%)

Steel

246

56.84

23.10

Carbon fibre/epoxy

188

15.66

8.33

OPEFB fibre/epoxy

29.1

1.83

6.28

Kenaf fibre/epoxy

19.8

2.34

11.82

Generally, it has been observed that bio-composites do not perform as well as conventional materials. Possible reasons for this include the fact that the stiffness and strength of bio-composites may be inferior to those of more conventional materials. This suggests that the bio-composite crash box has a lower energy absorption capacity, as it deforms more easily under an impact load [19]. The natural variation of the bio-composite material may both contribute to the poorer stiffness and strength [20].

4 Conclusion Traditional steel automotive crash boxes are heavy, contributing to long-term fuel consumption and pollution from car exhaust emissions. Bio-composite materials, which are lighter and more environmentally friendly, could be used as an alternative material, but their potential in high-demand applications such as crash impact is still largely unknown. The goal of this investigation is to investigate the crashworthiness of a bio-composite crash box made of oil palm empty fruit bunch (OPEFB) fibre reinforced epoxy and kenaf fibre reinforced epoxy composites. Crashworthiness, energy absorption capacity, and dynamic response were studied in comparison to steel and carbon fiber/epoxy materials. It has been found that while Kenaf fibre/epoxy and OPEFB fibre/epoxy composites had longer impact duration and lower peak force than steel crash boxes, which is desirable from occupants safety perspective, the energy absorption capability and CFE were not comparable to steel crash boxes. It was also discovered that the triggered folding mechanism was not structured. Further research on the fibre orientation, configurations, triggering scheme, and design along with the cost and manufacturing reliability, is required to accelerate bio-composite implementation in high-performance demand automotive components and realise the environmental benefits. Acknowledgements The authors acknowledge UCSI University for providing the internal funding for this project grant code: CERVIE REIG grant number REIG-FETBE-2021/040.

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References 1. Hanfeng Y, Youye X, Guilin W, Qixiang Q, Yufeng D (2015) Multiobjective optimization for foam-filled multi-cell thin-walled structures under lateral impact. Thin Wall Struct 94:1–12. https://doi.org/10.1016/j.tws.2015.03.031 2. Li Z, Yu Q, Zhao X, Yu M, Shi P, Yan C (2017) Crashworthiness and lightweight optimization to applied multiple materials and foam-filled front end structure of auto-body. Adv Mech Eng 9(8):168781401770280. https://doi.org/10.1177/1687814017702806 3. Rusu D, Boyer SA, Lacrampe M-F, Krawczak P (2011) Bioplastics and vegetal fiber reinforced bioplastics for automotive applications. In: Pilla S (ed) Handbook of bioplastics and biocomposites engineering applications, New Jersey, Wiley & Sons, Inc.; pp 397–449. https://doi.org/ 10.1002/9781118203699.ch15 4. Rozite L, Varna J, Joffe R, Pupurs A (2011) Nonlinear behavior of PLA and lignin-based flax composites subjected to tensile loading. J Thermoplast Compos Mater 26(4):476–496. https:// doi.org/10.1177/089270571142 5. Shaik Dawood MSI, Ahmad Ghazilan AL, Shah QH (2017) Finite element analysis of a composite crash box subjected to low velocity impact. In: IOP conference series: materials science and engineering, vol 184. pp 012017. https://doi.org/10.1088/1757-899X/184/ 1/012017 6. Hassan CS, Durai V, Sapuan SM, Abdul Aziz N, Zuhri MYM (2018) Crash performance of oil palm empty fruit bunch (OPEFB) fibre reinforced epoxy composites bumper beam using finite element analysis. Int J Automot Mech Eng 15(4):5826–5836. https://doi.org/10.15282/ijame. 15.4.2018.9.0446 7. Hassan CS, Qiang P, Sapuan SM, Abdul Aziz,N, Zuhri MYM, Ilyas RA (2021) Unidirectional oil palm empty fruit bunch (OPEFB) fibre reinforced epoxy composite car bumper beam— effects of different fibre orientations on its crash performance. In: Sapuan SM, Ilyas RA (eds) Biocomposite and synthetic composites for automotive applications, Woodhead Publishing, pp 233–253. https://doi.org/10.1016/B978-0-12-820559-4.00009-2 8. Khalid M, Ratnam CT, Chuah TG, Ali S, Choong TSY (2008) Comparative study of polypropylene composites reinforced with oil palm empty fruit bunch fibre and oil palm derived cellulose. Mater Des 29(1):173–178. https://doi.org/10.1016/j.matdes.2006.11.002 9. Jawaid M, Abdul Khalil HPS, Abu BA (2010) Mechanical performance of oil palm empty fruit bunches/jute fibre reinforced epoxy hybrid composites. Mat Sci Eng A 527(29–30):7944–7949. https://doi.org/10.1016/j.msea.2010.09.005 10. Nasution H, Pandia S, Maulida, Sinaga MS (2015) Impact strength and thermal degradation of waste polypropylene (wPP)/oil palm empty fruit bunch (OPEFB) composites: effect of maleic anhydride -g-polypropylebe (MAPP) addition. Proc Chem 16:432–437. https://doi.org/ 10.1016/j.proche.2015.12.075 11. Hassan CS, Durai V, Sapuan SM, Abdul Aziz N, Zuhri MYM (2018) Mechanical and crash performance of unidirectional oil palm empty fruit bunch fibre-reinforced polypropylene composite. BioResources 13(4):8310–8328. https://doi.org/10.15376/biores.13.4.8310-8328 12. Wong KP, Hassan CS, Qiang P, Sapuan SM, Abdul Aziz N, Zuhri MYM (2021) Crash behaviour of unidirectional oil palm empty fruit bunch fibre-reinforced polypropylene composite car bumper fascias using finite element analysis. Funct Compos Struct 3:044001. https://doi.org/ 10.1088/2631-6331/ac33b7 13. European Aluminium Association (2013) The aluminium automotive manual, applications-car body-crash management systems 14. Research Council for Automobile Repairs (2017) RCAR Low-speed structural crash test protocol 15. Gliszczynski A (2018) Numerical and experimental investigations of the low velocity impact in GFRP plates. Compos B Eng 138:181–193. https://doi.org/10.1016/j.compositesb.2017.11.039 16. Hernandez C, Maranon A, Ashcroft IA, Casas-Rodriguez JP (2013) A computational determination of the Cowper-Symonds parameters from a single Taylor test. Appl Math Model 37(7):4698–4708. https://doi.org/10.1016/j.apm.2012.10.010

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17. Tarlochan F, Samer F, Hamouda AMS, Ramesh S, Khalid K (2013) Design of thin wall structures for energy absorption applications: enhancement of crashworthiness due to axial and oblique impact forces. Thin Wall Struct 71:7–17. https://doi.org/10.1016/j.tws.2013.04.003 18. Reddy TJ, Rao YVD, Narayanamurthy V (2018) Thin-walled structural configurations for enhanced crashworthiness. Int J Crashworthiness 23(1):57–73. https://doi.org/10.1080/135 88265.2017.1306824 19. Isaac CW, Ezekwem C (2021) A review of crashworthiness performance of energy absorbing composite structure within the context of materials, manufacturing and maintenance for sustainability. Compos Struct 257. https://doi.org/10.1016/j.compstruct.2020.113081 20. Li X, Wang Y, Xu X, Cao X, Li R (2021) Energy absorption characteristics of crash box of new honeycomb core structure with foam-filler. Int J Automot Technol 22(1):221–230. https:// doi.org/10.1007/s12239-021-0022-6

The Tribological Performance of Nano-Activated Carbon as Solid Additives in Modified Calophyllum Inophyllum Based-Metalworking Fluid Zubaidah Zamri , Amiril Sahab Abdul Sani , Radhiyah Abd Aziz , Ainaa Mardhiah Sabri , and Norfazillah Talib

Abstract Biolubricants have attracted attention in today’s market as a new alternative to commercial lubricants due to their environmentally friendly and renewable properties. The refinement of bio-lubricants has improved their tribological and physical properties. However, to optimize the performance of lubricants when machined under high-temperature conditions, additives must be added to the lubricant. In this study, the tribological properties of modified Calophyllum inophyllum (MTO) oil combined with nano-activated carbon (NAC) as additives were investigated using the four-ball wear test method. This bio-lubricant consists of modified Calophyllum inophyllum oil in combination with NAC at concentrations of 0.01, 0.025, and 0.05 wt%. The coefficient of friction for the balls and their wear diameter are evaluated and compared. The kinematic viscosity and viscosity index of MTO were tested according to ASTM standards. The results show that a lubricant with added NAC is more effective in reducing wear and friction than a bio-lubricant without nanoactivated carbon. The bio-lubricant combined with NAC reduced the wear diameter of the lubricated balls compared to the bio-lubricant without additives. The nanoadditives have converted the sliding effect into a ball-bearing effect between the interfaces of the balls, creating a better oil protective film that helps form a gap between the mating surfaces during tribological testing. Keywords Nano-activated carbon · Modified calophyllum inophyllum oil · Tribology

Z. Zamri · A. S. Abdul Sani (B) · R. Abd Aziz Faculty of Manufacturing and Mechatronic Engineering Technology, Universiti Malaysia Pahang, 26600 Pekan, Pahang, Malaysia e-mail: [email protected] A. M. Sabri · N. Talib Department of Manufacturing Engineering, Faculty of Mechanical and Manufacturing Engineering, Universiti Tun Hussein Onn Malaysia, 86400 Batu Pahat, Johor, Malaysia © The Author(s), under exclusive license to Springer Nature Singapore Pte Ltd. 2024 R. Abd. Aziz et al. (eds.), Intelligent Manufacturing and Mechatronics, Springer Proceedings in Materials 40, https://doi.org/10.1007/978-981-99-9848-7_34

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1 Introduction The lubricant has been used for decades to decrease friction and wear between surfaces in contact and to reduce heat formation during continuous motion between the mating surfaces [1]. For instance, lubricant is used in the automotive industry and other industrial areas as a cooling agent, metalworking fluids, engines, and hydraulic pumps. Lubricants originally derived from mineral-based oil such as petroleum due to their efficacy to reduce wear, have good hydrolysis stability and economical properties [1]. However, petroleum-based oil possesses poor biodegradability, poor flash point value, and high toxicity [2, 3]. The increasing understanding of worker health concerns and environmental pollution is the main objective for the development of lubricants derived from renewable resources [4]. Lubricants from petroleum-based contain a variety of complicated mixtures made up of countless chemical compounds. Additionally, these bio-lubricants perform better in terms of being ecologically friendly and toxic-free, making them a viable substitute for petrochemical products. Bio-based lubricants have been acknowledged and utilized as engine oil, biodiesel, metalworking fluid, and hydraulic oil. Bio-based lubricants are often derived from vegetable oil and animal fat [5]. However, due to competition between the feedstock industry and the lubricant industry, bio-lubricant prices are more expensive than mineral-based lubricants [6]. To overcome this issue, the non-edible source has been utilized as an alternative and several modifications have been made to ensure this non-edible vegetable oil is suitable for use according to ASTM standards [7]. In this study, the Tamanu oil (Calophyllum Inophyllum), was selected for its exceptional rheological and tribological characteristics, owing to its sustainable, and biodegradable nature. Tamanu, being a non-edible plant, has make it a favourable option for substituting traditional sources of lubricating oil. From an edible plant thus eliminating the edible oil from being used as a lubricant [8]. However, crude Tamanu oil (CTO) cannot compete with the synthetic ester (SE) in today’s marketplace due to its inherent properties, which include extremely high viscosity, poor thermal and oxidative stability, and a high amount of monounsaturated acid [9]. To improve the existing physical and chemical properties of Tamanu oil for metalworking fluid applications, chemical modification is used. The chemical modification involves the elimination of the hydrogen component on the beta-carbon positive side of the DNA structure by using a catalyst to initiate the chemical processes [3]. To enhance the efficiency and performance of lubricants, additives are used to aid in reducing friction and wear produced by the cutting tool while also lowering energy loss in the system [10]. The dispersion of a small weight percentage of nanoparticles can help to provide a gap between the cutting tool and the workpiece surface. In the synthesizing process of nano-fluid, the size and concentration of nano-additives play a major role in their tribological performance [11]. Lubricants that have nano-additives with adequate concentration can significantly reduce friction and wear as they formed an excellent tribo-film layer protecting the surface [12]. In this study, the CTO triglyceride structures are altered chemically by using the catalysts sodium methoxide (NaOCH3)

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377

and trimethylolpropane (TMP) ester [13]. The inclusion of nano-activated carbon from Tamanu shells was evaluated at various concentrations for its effectiveness in assisting in reducing the wear formed on the ball. The tribological performance of MTO at various concentrations of NAC was investigated using a four-ball test to determine the potential of the newly developed metalworking fluids (MWF).

2 Methodology 2.1 Chemical Modification for Crude Tamanu Oil (CTO) The crude Tamanu oil (CTO) was transformed into a bio-based metalworking fluid (MWF) using a chemical modification process and the inclusion of additives to enhance the tribological and physicochemical properties of the oil. Fatty acid methyl ester (FAME) was created by chemically modifying the CTO utilizing a two-step acid-based transesterification technique. To produce modified Tamanu oil (MTO), FAME was mixed with trimethylolpropane (TMP) ester and 1% weight sodium methoxide (NaOCH3) at a molar ratio of 3.5:1 for 24 h as the catalyst for the reaction. As shown in Fig. 1, the transesterification process was executed in a flask with three necks and a Graham condenser on top.

Fig. 1 Transesterification process

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2.2 Nano-Activated Carbon (NAC) Synthesis Process The main material used for the nano-activated carbon is Tamanu shells and the process is depicted in Fig. 2. The shell was dried under 12 heating bulbs with 100 W for 24 h to dry up the shells after husk extraction from the shells. Subsequently, the shell is charred in the furnace for 2 h at 450 °C after it undergoes a cleaning process in an ultrasonic machine for 3 h. The charred shells were ground in pestle and mortar for the first phase of the size reduction process. Then, a sieve of 30 µm in size was used to filter the carbon powder. In the second size reduction process, the ball-milling process is carried out for 24 h at 350 rpm to reduce the size of the carbon powder to 1 µm. The carbon powders were activated by using a chemical activation process with sodium hydroxide (NaOH) as an activation agent at a molar ratio of 1:2.5. The carbon powder was soaked for 24 h before it is carbonized in the furnace for 2 h at 450 °C to activate the pores. After the activation process, the pH of the powder was neutralized with hydrochloric acid (HCl) and distilled water until a pH of 7 was reached. After neutralization, the powder was filtered with a filtration bottle and dried in a vacuum oven at 100 °C for 5 h. Then, the activated carbon powder undergoes the final phase of the size reduction process by using the ball-milling process. The parameters for

Fig. 2 Synthesis process for nano-activated carbon (NAC); a Dried and charred Tamanu shells, b ball-mill machine, c activation process and d nano-activated carbon powder

The Tribological Performance of Nano-Activated Carbon as Solid … Table 1 Ball-milling parameters

379

Parameters

Value

Weight per ball

7.5–7.8 g

Number of balls

23

Milling speed

350 rpm

Milling hours

24–72 h

the ball-milling process are shown in Table 1 below. Then, the size and surface morphology of the nano-activated carbon is analyzed under FESEM (JEOL).

2.3 Dispersion Process of NAC into the Biobased MWFs MTO was mixed with nano-activated carbon (NAC) at different concentrations of 0.01, 0.025, and 0.05 wt%, respectively (the additive concentration was calculated based on the weight of the MTO sample). MTO and NAC were mixed using an ultrasonic device for 2 h at 60 °C. Figure 3 shows the appearance of MTO before and after the addition of NAC. Table 2 shows the prepared MTO samples with and without the addition of NAC. Subsequently, the physicochemical and tribological properties of the lubricants were tested according to ASTM D445 (kinematic viscosity), ASTM D2270 (viscosity index), and ASTM D4172 (four-ball wear test).

Fig. 3 Lubricant sample: a Modified Tamanu Oil (MTO), b MTO1, c MTO2 and d MTO3

380 Table 2 The descriptions of the MTO samples for this study

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Sample

Concentration of additives (wt.%)

MTO

–

MTO1

0.01

MTO2

0.025

MTO3

0.05

2.4 Tribological Test The research on metalworking fluid’s tribological properties revolves mainly around friction and wear mechanisms. Figure 4a shows the DUCOM TR-30 L four-ball tribotester used to perform the tribology test in this research, which follows the ASTM D4172 standard method. The ball used in this test is a chromium steel ball (AISI 52,100) with a diameter of 12.7 mm and a hardness value in the range of 62 to 66 HRC. Three fixed steel balls were assembled in the ball cup, secured with a retaining ring, and covered with 10 ml of lubricant. The fourth ball, called the rotating ball, was attached to the collet, and tightened on the spindle. Figure 4b shows the setup diagram for the test sample. After the tribological test, the wear scar diameter (WSD) was measured on the three steel balls supported in the ball cup to determine the effectiveness of the oil used to minimize wear. After the test, the topological surfaces of the three-ball bearing were identified using an optical microscope (Olympus BX51M metallurgical microscope) and the coefficient of friction (COF) for each lubricant sample was determined using Winducom software. The results for WSD and COF of all lubricant samples were compared to a reference oil, which is a synthetic ester (SE). SE is the commercial metalworking fluid for MQL applications derived from mineral oil.

3 Result and Discussion 3.1 Rheological Properties Figure 5 displays the viscosity index and kinematic viscosity at 40 and 100 °C for each lubricant sample. When temperatures change during the machining process, kinematic viscosity is essential for preserving the lubricant’s fluidity. MTO and MTO with nano-additives had higher kinematic viscosities than SE (5.20 mm2 /s), demonstrating the lubricant’s potential to form tribo-films and withstand high-temperature conditions. As depicted in the graph, SE possesses the lowest kinematic viscosity and viscosity index while MTO and MTO with nano additives have excellently improved their kinematic viscosity and viscosity index. While for the viscosity index of MTO (198.03), has increased by 31.84% after the modification process compared to SE(150.21) indicating the effectiveness of the chemical modification technique in

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Fig. 4 Tribological test for lubricants; a DUCOM TR -30 L four-ball tribo-tester and b Ball-pot containing lubricant and three stationary balls

altering the triglyceride structure of Tamanu oil by replacing the beta carbon with triglyceride ester structure [14]. MTO3 has the highest viscosity index (236.15) and kinematic viscosity(6.80) due to the high concentration of nano-activated carbon in the oil as depicted in Table 3 below. The high content of nano-activated carbon has decreased the space for the particles to move in the oil [15]. The nanofluids become denser and more viscous than other lubricant samples.

3.2 Results for Tribological Performance of Each Lubricant Sample Table 4 shows the tribological performance of the lubricants in terms of their coefficient of friction (COF) and wear scar diameter value (WSD). The nano-activated carbon presence in the fluid was able to generate a lubricating film between the contact surfaces that acted as a cushion layer protecting the interface of the balls from direct load applied, improving the COF and WSD values [16]. Furthermore, the nanoparticles have generated a rolling effect at the mating surfaces, potentially converting sliding motion into ball-rolling motion [17]. The fatty acids in MTO provided effective lubrication properties as they contained fatty acids that can produce a lubricant layer that attaches to the contact surfaces [18]. The polar carboxyl group in the fatty acids remained tightly packed, providing a sufficient lubricating coating

382

Z. Zamri et al. Viscosity index Kinematic viscosity at 40 °C Kinematic viscosity at 100 °C

300

Viscosity index

50

200

40 30 100 20 10 0

2

60

Kinematic viscosity (mm /s)

70

0 SE

CTO

MTO

MTO1

MTO2

MTO3

Sample

Fig. 5 Viscosity index against kinematic viscosity of lubricants sample chart

Fig. 6 Worn surface after tribological test; a MTO1, b MTO2, and c MTO3 Table 3 Rheological properties of lubricant samples Physical properties

Temp (°C)

Density (g/cm3)

40

0.97

100

0.91

Kinematic viscosity 40 (mm2 /s) 100

24.43

Viscosity index

–

SE

MTO

MTO1

MTO2

MTO3

0.93

0.93

0.95

0.98

0.86

0.87

0.88

0.93

25.81

26.00

26.44

26.37

5.20

6.10

6.17

6.25

6.80

150.21

198.03

200.27

200.17

236.15

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Table 4 Tribological results after four-ball wear test Lubricant sample

Wear scar diameter (µm)

Coefficient of friction (COF)

SE

779.30

0.102

MTO1

674.70

0.064

MTO2

724.20

0.055

MTO3

739.50

0.059

that may reduce friction [1]. Moreover, among three nano-activated carbon concentration ratios, MTO2 has presented an excellent improvement of COF(0.055) and better WSD(724.20 µm) surface. There was less formation of deep grooves on the scar surface of MTO2 compared to MTO3 as depicted in Fig. 5. While for MTO1, the concentration of nano-activated carbon is not enough to fill the gaps between the contact surface and for MTO3, the concentration of nano-activated carbon has exceeded the needs and cause agglomeration of nano activated carbon between the contact surface [19]. This situation proved that an adequate quantity of nanoparticles can provide a smooth rolling motion between the contact area as there will be no agglomeration between particles at the interface (cf. Fig. 6) thus lowering the COF value.

4 Conclusion In this research, the tribological performance of four MTO samples as the ecofriendly lubricant was examined by conducting physical and tribology test using a four-ball wear test, and the performance of this eco-friendly lubricant were compared with SE. The presence of nano-activated carbon has significantly improved the physical properties of the MTO. The addition of 0.05 wt% of nano-activated carbon in MTO shows the highest viscosity index of 236.15 respectively. While the inclusion of 0.025 wt% of nano-activated carbon in MTO is the optimum concentration based on the results obtained from the COF value and scar formation on the ball after the tribology test. MTO2, which is MTO + 0.025 wt% has the smallest COF value and less groove formation on the ball. Based on the overall results, the addition of nano-activated carbon has excellently improved the tribological properties of the MTO and their performance has exceeded the SE fluid. In conclusion, MTO with nano-activated carbon could replace the application of SE as an eco-friendly metalworking fluid and reduce the dependency on mineral-based metalworking fluid for a sustainable machining process.

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References 1. Bart JCJ, Gucciardi E, Cavallaro S (2013) Biolubricants. 2nd edn. Woodhead Publishing, Cambridge 2. Jamaluddin NA (2020) Tribological analyses of modified Jatropha oil with hBN and graphene nanoparticles as an alternative lubricant for machining process. J Adv Res Fluid Mech Therm Sci 2(76):1–10 3. Talib N, Sukor NFAM (2022) Materials today: proceedings. 48:1831–1835 4. Shahabuddin M (2013) Comparative tribological investigation of bio-lubricant formulated from a non-edible oil source (Jatropha oil). J Industr Crops Product 47:323–330 5. Abdul Sani AS (2017) Tribological performance of modified Jatropha oil containing oilmiscible ionic liquid for machining applications. J Mech Sci Technol 31:5675–5685 6. Adenuga AA (2020) Synthesis of quality biodiesel from Calophyllum inophyllum kernels through reactive extraction method, optimization of process parameters and characterization of the products. J Renew Energy 145:2530–2537 7. Rahim EA (2018) Tribological interaction of bio-based metalworking fluids in machining process. J Tribol Int 120:520–534 8. Azad AK (2016) Prospects, feedstocks and challenges of biodiesel production from beauty leaf oil and castor oil—a nonedible oil sources in Australia. J Renew Sustain Energy Rev 61:302–318 9. Srikant RR, Rao PN (2017) Sustainable machining, 1st edn. Springer International Publishing, New York 10. Dai W (2016) Roles of nanoparticles in oil lubrication. J Tribol Int 102:88–98 11. Kumar CS (2020) Friction and wear behavior of chemically modified Sal (Shorea Robusta) oil for bio based lubricant application with effect of CuO nanoparticles. J Fuel 282 12. Zolkefli AA (2021) Tribology effect on turning machine process using Jatropha oil with AC nanoparticle. J Res Progr Mech Manufact Eng 2:267–273 13. Abdul Sani AS, Zamri Z (2023) Materials today: proceedings. In: Nurul, Akmal CL, Zulhelmi I (eds) IM3F 2022,vol 5. Elsevier, Netherlands, pp 39–45 14. Jahirul MI (2015) Physio-chemical assessment of beauty leaf (Calophyllum inophyl-lum) as second-generation biodiesel feedstock. J Energy Rep 1:204–215 15. Dambatta YS (2018) Comparative study on the performance of the MQL nanolubricant and conventional flood lubrication techniques during grinding of Si3N4 ceramic. Int J Adv Manuf Technol 96:3959–3976 16. Ranjan N (2022) Tribological study of iron infused carbon tubes additive in gearbox, engine, and vegetable-based lubricant. J Tribol Int 171 17. Makhesana MA (2022) Analysis of vegetable oil-based nano-lubricant technique for improving machinability of Inconel 690. J Manufact Process 77:708–721 18. Sharma BK (2006) Chemical modification of vegetable oils for lubricant applications. J Am Oil Chem Soc 83:129–136 19. Nagabhooshana N (2020) Evaluation of tribological characteristics of nano zirconia dispersed biodegradable canola oil methyl ester metalworking fluid. J Tribol Int 151

Formulation of NSF H2 Food-Grade Grease from Vegetable-Base Oils Mohd Najib Razali , Nur Syahirah Juhari , Nur Kholis Zulkifli , Najmuddin Mohd Ramli , and Mohd Khairul Nizam Mohd Zuhan

Abstract Vegetable oil is a potentially non-toxic, safe source, sustainable and costeffective of obtaining environmentally friendly lubricants. This study aims to formulate NSF H2 food-grade greases from three types of vegetable base-oils (VBO): palm oil (fresh and used), coconut oil (fresh and used), and castor oil. Lithium12-hydrostearic acid, azelaic acid, and butylated hydroxytoluene were used as a thickening agent, complexing agent and an additive, respectively. Similar ratios of base oils, thickener, and additive were used in all five grease formulations and were tested based on ASTM. The physical properties of the oils were characterised for water content, viscosity, flashpoint, and thermal stability. The chemical composition and functional groups of the oils was evaluated via GC–MS and CHNOS elemental analysis, and FTIR. The formulated greases were analysed for consistency, dropping point, stability, oil bleeding, and thermal analysis. The analysis shows the grease made of vegetable base-oils (VBO) exhibit high dropping points exceeding 200 °C and NLGI 2 for fresh palm oil, used palm oil, and castor oil-based greases, and NLGI 1 and 3 for fresh and used coconut oil-based grease, respectively. Castor oil shows high bleeding with 22.88%, the greases made of fresh palm oil and fresh coconut oil have moderate oil bleeding of 1.20–7.55%. Keywords NSF H2 food-grade grease · Vegetable-based oils · Palm oil · Coconut oil · Castor oil

M. N. Razali (B) · N. S. Juhari · N. K. Zulkifli · N. Mohd Ramli Faculty of Chemical and Process Engineering Technology, Universiti Malaysia Pahang Al-Sultan Abdullah, 26300 Kuantan, Pahang, Malaysia e-mail: [email protected] N. Mohd Ramli MNR Multitech Sdn Bhd, K02, Ground Floor, Kompleks UMP Holding, 26300 Gambang, Pahang, Malaysia M. K. N. Mohd Zuhan Pusat Pengajian Diploma Universiti Tun Hussein Onn Malaysia, Hab Pendidikan Tinggi Pagoh, , KM1, Jalan Panchor, 84600 Pagoh, Johor, Malaysia © The Author(s), under exclusive license to Springer Nature Singapore Pte Ltd. 2024 R. Abd. Aziz et al. (eds.), Intelligent Manufacturing and Mechatronics, Springer Proceedings in Materials 40, https://doi.org/10.1007/978-981-99-9848-7_35

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1 Introduction A lubricant such as grease is an essential part of machinery’s mechanical operation. Food-grade greases are specially manufactured for the grease lubrication of machinery approved for food and beverage processing, packaging industry, and pharmaceutical industries where there is contact tendency with the grease [1, 2]. Grease is used to lubricate joints, bearings, hooks, conveyor belts, and trolleys for energy savings, prolong service life, minimize downtime, and reduce maintenance time of equipment and machinery [3, 4]. Variety of base oil, thickening agent, and additives could be used to formulate the semisolid structure of grease [5, 6]. The thickening agent acts as a sponge to hold the lubricating base oil in place, while the additive could comprise various compounds added to enhance the life and performance of the grease. Food-grade grease could be classified as H1, H2 or H3 by NSF International (previously known as National Sanitation Foundation), an independent American body that conducted product testing, inspection, and certification for the environment and public health [7]. Food-grade lubricant with NSF rating H1 is mainly used in pharmaceutical, food or beverages production industries that may accidentally come into contact with the products. NSF rating H2 lubricants are used in places where it is unlikely for the grease to come into contact with the foodstuff and pharmaceutical products. H3 is lubricant is used as soluble oil to prevent corrosion and to clean equipment used in the industries before the operation [1]. L. S. Kheang and C. Y. May emphasized in their findings the performance characteristics of base fluids that comply with the NSF H2 standard. This data will be the baseline to measure the rigor and reliability of the grease formulation [7]. Highly purified and high viscosity index mineral oils, such as polyalphaolefin and white oil with excellent high and low-temperature resistance and good oxidation stability are regularly used as lubricants in food handling machinery for incidental food contact. However, these non-polar synthetic oils have low natural lubricity, additive solubility, and natural solvency. The non-biodegradable substances of these oils are also unsafe for the environment. Furthermore, these oils are costly than vegetable oils (VBO). Lubricants based on green raw materials with high lubricity (e.g., VBO) have increased interest in numerous applications, particularly those related to the food industry [8]. Lubricant grease from VBO is sustainable with high biodegradability, exceptional physical and chemical properties (e.g., high viscosity index), low evaporation loss, high ignition point, and good shear resistance. By substituting mineralbased oils with VBO, environmentally friendly lubricating greases can be produced. In general, VBO is much cheaper than ester-based oils, thus providing greater potential for efficient use in base oils as lubricants. VBO are also more economical than highly purified food-grade mineral oils. Furthermore, the grease used for food industries should offer high thermal stability, oxidation stability, and hydrolytic stability. The main purpose of this study is to formulate National Sanitary Foundation (NSF)

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rating H2 food-grade grease [21] from different vegetable-based oils and evaluate the formulated grease properties.

2 Materials and Methods 2.1 Materials Three different types of VBO were used to formulate food-grade grease: palm oil (fresh and used), coconut oil (fresh and used), and castor oil. Fresh palm and coconut oils were obtained from a local grocery store, used palm and coconut oils were acquired from domestic use, while castor oil was purchased from Orioner Hightech Sdn. Bhd. Lithium-12-hydrostearic acid (Li-12-HSA) was used as a thickener and butylated hydroxytoluene (BHT) was used as an additive. Both chemicals were purchased from Gardner Global Enterprise. Li-12-HSA was used as a thickener due to excellent extreme pressure, wear, corrosion, and wide-temperature advantages [9]. BHT is a synthetic antioxidant [10] and frequently added to food as a preservative [11, 12]. BHT is used to enhance vegetable oil performance as the base oils are known for their low oxidative stability. In this experiment, used palm oil and used coconut oil were pre-treated to remove unwanted contaminants, such as suspended solids. The oil was filtered using a strainer to remove any residues and contaminants and then transferred into a new container.

2.2 Formulation of Food-Grade Grease 600 g of grease was prepared for every base oil. The base oil was fixed at 71% (w/w) and BHT was set at 3% (w/w) initially, whereas the amount of thickener was varied until a viscous or grease-like texture was formed. The saponification process started by heating the base oil to 60 °C in a 500 ml beaker. BHT and Li-12-HSA were slowly added and mixed under an overhead stirrer with a propeller-type impeller (IKA RW20 overhead stirrer, Staufen, Germany) at 200 rpm. Vigorous mixing was continued for 2–4 h or more until a thick, homogenised mixture or grease- like structure was formed. Next, the grease obtained was homogenised using a hand-held homogeniser (Ultra Turrax T-25, Ika, Staufen, Germany) at 10,000 rpm for 45–60 min at room temperature to obtain homogenised grease as a final product.

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2.3 Characterisation of Base Oils The base oils were characterised for their chemical composition and functional groups via Fourier transform infrared (FTIR) with a wavelength of 400–4,000 cm−1 to obtain the spectra on a Nicolet iS5 FTIR spectrometer (Thermo Fisher Scientific, Massachusetts, USA). A CHNOS elemental analyser (Elementar, model Vario Macro Cube) was used to determine the elemental percentage of carbon (C), hydrogen (H), nitrogen (N), and sulfur (S) contained in the base oils. The fatty acid composition of a particular base oil was determined by gas chromatography-mass spectrometry (GC–MS) analysis using Agilent-7890 equipped with HP-INNOWAX column. The column temperature was programmed at 185–250 °C with helium as the carrier gas. The fatty acid composition was identified by gas chromatography and mass spectrometry (GC–MS). Fatty acid methyl ester (FAME) was prepared for each vegetable oil for analysis by mixing 0.2 ml of the oil and 4 ml of hexane as a solvent, and then added with 4 ml of 1 M of NaOH in methanol. FAME was identified using Agilent-7890 equipped with HP-INNOWAX column. The column temperature was programmed at 185–250 °C with helium as the carrier gas [13]. The physical properties of the oils were evaluated for water content, flashpoint, dynamic viscosity, and thermal stability. The water content in the base oil was determined using KF Titrino (model 787 KF Titrino; Metrohm,Herisau, Switzerland). In this analysis, a drop of the sample was injected into 50 ml anhydrous ethanol before HYDRANAL-methanol dry was added, and the machine was set at the KFT mode. The flashpoint analyser used was Koehler K16591 rapid flash closed-cup tester. The standard part of lubricant specification is usually flashpoint evaluation. According to the American Society for Testing and Materials (ASTM), the flashpoint is the lowest temperature at which an ignition source can ignite a sample vapour (lubricant) under specified conditions. The viscosity of the base oil was determined using a viscometer (Brookfield, LVDV II 6890). Viscosity is a measure of the fluid flow resistance induced by its molecular structure. The molecular composition generates internal friction. When shear stress or tensile stress is applied when the fluid is in contact with a solid boundary, this internal friction will prevent gradual deformation. Thermal stability was evaluated using thermogravimetric analysis (TGA). The test was carried out using a TGA Q500 thermogravimetric analyser (TA Instruments) conducted in the air environment with a ramping temperature of 40–600 °C and the heating rate of 10 °C/min. TGA was carried out by steadily increasing the sample’s temperature in the furnace to observe the loss of volatile components indicated by the decrease in weight.

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2.4 Characterization of Formulated Grease Grease analysis is used to determine the formulated food-grade grease’s stability, quality, and properties. The grease’s physical and chemical analysis involved and dropping point, stability and consistency test by cone penetration tests, oil bleeding, and thermal analysis by TGA. The analysis data can be used as part of the predictive maintenance strategy to monitor grease conditions and grease performance changes over time. Consistency test was carried out to determine the stiffness of the grease by cone penetration test. The penetration test were conducted and compared to National Lubricating Grease Institute (NLGI) consistency grade in the range from 000 to 6. The NLGI grades defined the consistency of the grease and its appearance at room temperature. The consistency of the grease (NLGI grade) was compared before (unworked) and after the grease stroke cycle (worked) as per ASTM D-217 to determine grease mechanical stability The dropping point is used to determine the temperature at which grease changes from a semisolid to a liquid state. Equation 1 can be used to obtain the dropping point based on the experimental data    BT − O D P  ... DP (◦ C) = ODP +   3

(1)

where ODP is the thermometer reading when the first drop occurs, and BT is the block oven temperature when the first drop falls. In the oil bleeding test, a fixed amount of grease was put on a piece of paper provided. The sample was heated for 2 h at 60 °C according to the grease test kit’s recommended operating condition (SKF TKGT-1 Grease Test Kit). The base oil released from the grease created a stain on the paper, where the bleed area reported is equivalent to a circle.

3 Results and Discussion The Characterisation results of base oils are shown in Table 1 for water content, flashpoint, and viscosity. The result shows that the used palm oil and used coconut oil contain slightly higher water content with the values of 2.25 and 2.59%, respectively, compared to other VBO. Grease with high water content may cause rust, corrosion, and bearing damage [14]. Water content influence the quality, usability, and chemical properties of grease. These properties can affect the grease rheology, processability, and shelf life that induce accelerated machinery breakdown due to further degradation, deterioration, leakage, and reduced oil flow by oxidation [14]. On the other hand, the flashpoint test is a standard part of base oil’s characterisation, which indicates the safety hazards of a lubricant in the matter of fire and explosion [15]. From the results obtained, all VBO have high flashpoints beyond 200 °C, while the flashpoints of fresh coconut oil, used coconut oil, and castor oil exceed 290 °C. VBO are safe to be used because the materials with high flashpoints

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Table 1 Base oils characterisation Characterisation

Fresh palm oil

Used palm oil

Fresh coconut oil

Used coconut oil

Castor oil

Water content (%) 0.81

2.25

0.74

2.59

0.99

Flashpoint (°C)

228

218

293

>299

>299

Viscosity (cP) @ 40 °C

56,003

61,262

43,541

49,549

65,266

are less flammable and less hazardous [16]. Castor oil has the highest viscosity with 65,266 cP than other base oils. VBO contain low to high molecular chains of fatty acids. The volatility of low molecular fatty acids contributes to a lower flashpoint. Viscosity determines the operating temperature and application of base oils. High viscosity base oils can be used in high-speed and high-temperature applications. Besides, the base oil viscosity affects consistency, low base oil viscosity leads to high consistency, and vice versa [17] Table 2 shows the CHNS analysis results. The analysis was done to detect the amount of S content in the base oils. A lower S decreases oxidation and corrosion [18]. The result shows that used palm oil contains the lowest S content than other base oils. There is no significant difference between the percentage of C, H, N, and S for different base oils. Therefore, VBO is compounds with low S content, which is an element that could cause corrosion to mild steel and also damage the environment [19]. GC–MS was utilised to identify the fatty acids composition present in the respective vegetable based-oils as shown in Table 3. Castor oil displays distinct properties compared to other base oils, which is dominantly consisted of C18:1 (ricinoleic acid) [20], whereas fresh palm oil, used palm oil, fresh coconut oil, and used coconut oil primarily consist of C18:1 (oleic acid). Mahmud et al. (2015) stated that oleic acid is the most preferred fatty acid in VBO for lubrication because oleic acid distribution in a naturally-occurring ester base stock is vital in oil performance with high proportions [21]. Nevertheless, castor oil that is rich with ricinoleic acid has high viscosity, making it a good lubricant. Table 2 CHNS analysis results Characterisation

Fresh palm oil

Used palm oil

Fresh coconut oil Oil

Used coconut oil

Castor oil

C (%)

0.95

0.92

0.76

0.71

0.94

H (%)

0.15

0.16

0.14

0.12

0.12

N (%)

0.003

0.003

0.002

0.003

0.004

S (%)

0.03

0.003

0.04

0.05

0.03

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Table 3 Fatty Acids Composition of the Vegetable Base Oils Fatty acid

Fresh palm oil

Used Palm oil

Fresh coconut oil

Used coconut oil

Castor oil

C14:0 (Myristic acid)

–

–

0.20

–

–

C16:1 (Palmitoleic acid)

–

–

0.42

–

–

C18:0 (Stearic acid)

0.68

0.61

16.32

6.82

–

69.37

62.94

67.50

70.70

C18:1 (Oleic acid) C18:1 (Vaccenic acid)

0.29

–

–

0.29

C18:1 (Ricinoleic acid)

–

–

–

–

C18:2 (Linoleic acid) C18:3 (α-Linolenic acid)

29.34

–

35.44

14.99

–

C20:1 (Eicosenoic acid

–

21.48

0.18

11.65 –

62.90

17.10

–

0.98

FTIR is a useful analytical tool for detecting functional groups and characterising covalent bonding information. By generating IR absorption spectra, FTIR can classify chemical bonds in molecules. Figure 1 shows the comparison of FTIR spectra for all VBO. The band specifies slightly to almost no difference between all the bands for each oil. Edible fats and oils are triglycerides consisting of a hydroxyl functional group (–OH) and a carboxyl group (–CO).

3.1 Analysis of Formulated Grease Dropping point test and consistency for unworked and worked grease is shown in Table 4. The dropping point test determines the cohesiveness of the oil and thickener of a grease. Fresh palm oil, used palm oil and used coconut oil-based grease show highest dropping points at above 211 °C. Fresh coconut oil-based grease show slightly lower dropping point at 210.3 °C, while castor oil-based grease shows the lowest

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Fig. 1 FTIR spectra of different base oils

dropping point at only 207 °C. The result indicates that the drop point temperature resulting from the additive and thickener percentage in the formulated food- grade grease did not vary as BHT and Li-12-HSA are known to have high-temperature tolerance [9]. The penetration test is the primary method to measure the consistency of a lubricant using the cone penetration. The unworked and the worked penetration of new greases is an attribute of the NLGI grease consistency classification system. Grease consistency was measured at room temperature before and after the sample was subjected to 60 double strokes [22]. Grease with a higher number tends to stay in place and is a good choice when leakage is a concern.

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Table 4 Dropping point test and consistency for unworked and worked grease Type of grease

Dropping point Unworked Worked grease consistency (60-stroke) grease consistency

Fresh palm oil

211.3 °C

NLGI 2

NLGI 1

Used palm oil

211.7 °C

NLGI 2

NLGI 1

Fresh coconut oil 210.3 °C

NLGI 1

NLGI 1

Used coconut oil 211.3 °C

NLGI 2

NLGI 2

Castor oil

NLGI 2

NLGI 2

207.0 °C

The result obtained for unworked palm oil-based grease (fresh and used), used coconut oil-based grease and castor oil-based grease the consistency of NLGI 2, whereas fresh coconut oil possesses the consistency of NLGI 1. The 60 double strokes of the greases (worked penetration) were consistent for all the greases expect for palm oil-based grease (fresh and used) that show changes in the consistency and softening effect (NLGI 2 to NLGI 1) due to mechanical stress. The choice of consistency depends on the applications and operating conditions, such as temperature, pumpability, and speed. For normal use in most applications, such as bearings, the consistency of grease is usually between NLGI 1 and 3. The grease hardness prevents the bearing from slipping out and gives good sealing capacity. Nevertheless, thickener network degradation can affect grease bleed and quality, grease consistency, and determine the grease life within a bearing [23]. The oil bleeding test is presented in Table 5. Bleeding is an analysis to determine the grease ability to release oil [24]. The result indicates the percentage difference between circle areas for a fresh sample and used sample. Grease made of fresh coconut oil shows the least oil bleeding with 1.20%, followed by used coconut oil with 4.77%. The greases from used palm oil and fresh palm oil show moderate oil bleeding with 7.41 and 7.55%, respectively. Castor oil that has high viscosity does not bleed too much compared to the base oil with lower viscosity. The grease made of castor oil as the base oil obtained the highest oil bleeding with 22.88%. It shows that lithium-based grease can hold fresh coconut oil and used coconut oil better than fresh palm oil and used palm oil. However, this grease has the least attraction toward castor oil. The ability of the grease to release oil is important as it indicates the grease ability to keep the mechanical part separated and keep the area well lubricated, thus prolonging machine life. However, excessive oil release through bleeding will cause unnecessary losses of the oil and lead to grease dry-out, and more frequent relubrication is needed due to the depletion of the base oil. Furthermore, mechanical stress by 60-stroke worked penetration that was applied prior to the testing could further contribute to higher bleeding due to intensive shearing or vibration. The TGA results of the formulated greases are shown in Fig. 2. The results obtained show that the greases undergo two major stages of weight loss, in which these stages may be due to the loss of excessive water content and volatile components in the greases and the degradation of greases when subjected to an extremely high temperature. Upon reaching 600 °C, about 5%–6% residue of the greases remained.

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Table 5 Oil bleeding test Type of grease

Bleed area of fresh sample (mm) Bleed area of used sample (mm) %Diff

Fresh palm oil

1356.14

1458.58

7.55

Waste palm oil

1406.92

1511.13

7.41

Fresh coconut oil

1441.26

1458.58

1.20

Waste coconut oil 1356.14

1424.04

4.77

815.66

22.88

Castor oil

663.77

Fig. 2 TGA analysis of different base oils

The TGA for the grease made of fresh palm oil shows 29.7% weight loss at 225– 348 °C and complete decomposition at 450.43 °C with 5.1% residue. For the grease made of used palm oil, 43.44 and 45.14% of weight loss were recorded at 180– 335.80 °C and 335.80–500 °C, respectively, with 5.6% residue. The grease made of fresh coconut oil shows moderate weight loss of 29.18% at 275–345 °C and 40.90% at 340–453.24 °C with 5.885% residue. The grease made of used coconut oil shows weight loss of 34.48% when subjected to heat at 225–345 °C and 38.46% at 348.09– 465 °C with 5.5% residue. Meanwhile, the grease made of castor oil shows moderate weight loss of 21.94% when subjected to heating at 322.85 °C and further weight loss of 46.52% at 470 °C with 6.35% residue. The grease made of fresh coconut oil shows early decomposition by observing the weight loss compared to other oils. Furthermore, the used oils show comparable thermal stability. Palm oil-based grease shows superior thermal stability, whereas castor oil shows moderate thermal stability.

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4 Conclusions The result shows that different grease formulations have different consistency, penetration, hardness, dropping point, oil bleeding, and thermal stability. The formulated greases have the consistency (worked penetration) of NLGI 1 for palm oil-based grease (fresh and used) and fresh coconut oil-based grease, NLGI 2 for used coconut oil and castor-oil based grease, respectively. The dropping points are 207 °C for castor oil-based grease, 210 °C for fresh coconut oil-based grease, and 211 °C for the grease made of used coconut oil, and fresh and used palm oil. The overall performance shows that palm oil has the advantages of being more physically favourable toward higher performance as grease-based lubricant, but the grease made of coconut oil and castor oil could also be utilised. The grease made of coconut oil shows early decomposition by observing the weight loss compared to other oils. Furthermore, the used oils also show comparable thermal stability. Palm oil-based grease shows superior thermal stability, while castor oil shows moderate thermal stability. VBO-formulated greases have a relatively low drop point temperature, unstable weight loss under high temperature, and high bleeding area. Furthermore, all of the greases are formulated with only a slight difference in the percentage of thickener and additive. It can be concluded that different types of VBO have different grease properties, which can be utilised as an environmental and cheaper base oil in grease manufacturing. However, additional research is needed to gain a comprehensive understanding of the mechanisms involved in developing an optimal industry-specific system. This work will contribute to creating a more effective and efficient system for practical application. Acknowledgements The authors wish to express their gratitude and appreciation for the financial support from the Universiti Malaysia Pahang Al-Sultan Abdullah for the Internal Grant (RDU220335) entitled Elucidation of Chitosan Formation Mechanism As An Additive For Enhancing Non-Soap Food Grade Grease Performance. The support from the Faculty of Chemical and Process Engineering Technology and MNR Multitech Sdn. Bhd. is also acknowledged.

References 1. McGuire N (2019) Incidental contact lubricants for the food industry. Tribol Lubricat Technol 75(12):18–24 2. Shetty P, Mu L, Shi Y (2020) Polyelectrolyte cellulose gel with PEG/water: toward fully green lubricating grease. Carbohydr Polym 230:115670 3. Jianjun Q, Huajie Q, Zhongpu W, Yunxia L (2020) Self-repairing properties of complex titanium grease containing hydroxyl silicate. Tribol Int 149:105685 4. Singh KK, Prabhu R, Choudhary S, Pramanik C, John NS (2019) Effect of graphene and MoS2 flakes in industrial oils to enhance lubrication. ACS Omega 4(11):14569–14578 5. Razali MN, Aziz AA, Athirah WN, Hamdan WM, Adilah NSM, Yunus RM (2017) Synthesis of grease from waste oils and red gypsum. Aust J Basic Appl Sci 11(3):154–159 6. Japar NSA, Aziz MAA, Razali MN, Zakaria NA, Rahman NWA (2019) Preparation of grease using organic thickener. Mater Today Proc 19:1303–1308

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7. Lught PM (2016) Modern advancement in lubricating grease technology. Tribol Int 97:467–477 8. Cecilia JA, Plata DB, Saboya RMA, de Luna FMT, Cavalcante CL, Rodríguez-Castellón E (2020) An overview of the biolubricant production process: challenges and future perspectives. Processes 8(3) 9. Mayasari EJ, Bakri R, Fibria M (2019) The effect of antioxidant additives on the characteristics of food-grade grease using castor oil (Ricinus communis L.) as the base oil. IOP Conf Ser Mater Sci Eng 496(1):12060 10. Zahid MA, Seo J-K, Parvin R, Ko J, Yang H-S (2019) Comparison of butylated hydroxytoluene, ascorbic acid, and clove extract as antioxidants in fresh beef patties at refrigerated storage. Food Sci Anim Resour 39(5):768–779 11. Permal R, Chang WL, Chen T, Seale B, Hamid N, Kam R (2020) Optimising the spray drying of avocado wastewater and use of the powder as a food preservative for preventing lipid peroxidation. Foods 9(9) 12. Naseer B, Iqbal S, Wahid N, Jamshaid Qazi H, Nadeem M, Nawaz M (2021) Evaluation of antioxidant and antimicrobial potential of rutin in combination with butylated hydroxytoluene in cheddar cheese. J Food Process Preserv 45(1) 13. Abdulbari HA, RMY, AHN, NMK (2011) Lubricating grease from spent bleaching earth and waste cooking oil: tribology properties. Int J Phys Sci 6(20):4695–4699 14. Gurt A, Khonsari M (2020) An overview of grease water resistance. Lubricants 8(9) 15. Sadeghalvaad M, Dabiri E, Afsharimoghadam P (2019) Lithium lubricating greases containing carbon base nano-additives: preparation and comprehensive properties evaluation. SN Appl Sci 1(3):264 16. Yuan S, Ji C, Han H, Sun Y, Mashuga CV (2021) A review of aerosol flammability and explosion related incidents, standards, studies, and risk analysis. Process Saf Environ Prot 146:499–514 17. Vyavhare K, Aswath PB (2019) Tribological properties of novel multi-walled carbon nanotubes and phosphorus containing ionic liquid hybrids in grease. Front Mech Eng 5 18. Saleh TA (2020) Characterization, determination and elimination technologies for sulfur from petroleum: toward cleaner fuel and a safe environment. Trends Environ Anal Chem 25:e00080 19. Xia D-H et al (2019) Sulfur induced corrosion (SIC) mechanism of steam generator (SG) tubing at micro scale: a critical review. Mater Chem Phys 233:133–140 20. Taieb Brahimi F, Belkhadem F, Trari B, Othman AA (2020) Diazole and triazole derivatives of castor oil extract: synthesis, hypoglycemic effect, antioxidant potential and antimicrobial activity. Grasas y Aceites 7(4):e378 21. Gasni D, Fikri I, Latif M (2020) Tribological study of addition oleic acid in palm and coconut oils as bio-lubricants. Mater Sci Forum 22. Chatra S, KR, Lugt PM (2021) The process of churning in a grease lubricated rolling bearing: channeling and clearing. Tribol Int 153:106661 23. Zhou Y, Bosman R, Lugt PM (2019) A master curve for the shear degradation of lubricating greases with a fibrous structure. Tribol Trans 62(1):78–87 24. Ren G, Zhang P, Ye X, Li W, Fan X, Zhu M (2021) Comparative study on corrosion resistance and lubrication function of lithium complex grease and polyurea grease. Friction 9(1):75–91

Multiple Exciton Generation in MoS2 Nanostructures: A Density Functional Theory Study Nur Hidayati Ain Natasha Makimin, Saifful Kamaluddin Muzakir , Nur Farha Shaafi , Muhammad Zamzuri Abdul Kadir , and Ruziana Mohamed

Abstract Excitonic solar cell which fabricated using quantum confined semiconducting material that exhibits multiple exciton generation (MEG) is speculated could achieve theoretical photovoltaic conversion efficiency more than 60%. However, the expected efficiency has yet to be reached to date. Specific size and morphology of a quantum confined semiconducting material needs to be studied to determine the presence of MEG. The objective of this study is to verify the occurrence of MEG in few realistic cluster models of MoS2 using density functional theory (DFT) calculations. Small MoS2 nanocrystals were modelled using GaussView 5.0 software, which later validated as realistic using harmonic frequency calculations analysis executed by Gaussian 09W software. The presence of MEG in realistic models of MoS2 nanocrystals was studied using time-dependent density functional theory (TD-DFT) calculations. The output of the work is summarized as the followings, (i) (MoS2 )n with n = 2, 4, 6, 8 and 12 models were established as realistic, (ii) the size of the nanocrystal models are smaller than its exciton Bohr radius (ca. 1.61 nm) i.e., 0.54, 0.62, 0.95, 1.09 and 1.57 nm respectively, and (iii) all calculated MoS2 nanoparticle models exhibit MEG. Therefore, a practical technique that could synthesize MoS2 nanocrystals with similar structure or geometry with that of the evaluated models would materialize a device with practical photovoltaic conversion efficiency more than 60%.

N. H. A. N. Makimin · S. K. Muzakir (B) Faculty of Industrial Sciences and Technology, Universiti Malaysia Pahang Al-Sultan Abdullah, Lebuh Persiaran Tun Khalil Yaakob, 26300 Kuantan, Pahang, Malaysia e-mail: [email protected] N. F. Shaafi Universiti Malaysia Sabah, Jalan UMS, 88400 Kota Kinabalu, Malaysia M. Z. Abdul Kadir International Islamic University Malaysia, Bandar Indera Mahkota, 25200 Kuantan, Malaysia R. Mohamed Faculty of Applied Sciences, Universiti Teknologi MARA, 40450 Shah Alam, Selangor, Malaysia © The Author(s), under exclusive license to Springer Nature Singapore Pte Ltd. 2024 R. Abd. Aziz et al. (eds.), Intelligent Manufacturing and Mechatronics, Springer Proceedings in Materials 40, https://doi.org/10.1007/978-981-99-9848-7_36

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Keywords Density functional theory · Multiple exciton generation · Nanostructures

1 Introduction Solar cell is an electronic device that uses the photovoltaic effect to transform the energy of light into electrical energy. Solar cells can be classified into three groups based on the chronology and the photoactive materials used in their fabrications, i.e., (i) the first-generation solar cell which utilizes single crystals of Si or GaAs as main light absorber, (ii) the second-generation solar cell or the thin film solar cell which fabricated using amorphous Si:H, polycrystalline Si, CdTe or copper indium gallium selenide (CIGS), and (iii) the third-generation solar cell which utilizes dye molecules, quantum dots or perovskite materials as main light absorber.

1.1 A Comparison Between the Theoretical and Practical Efficiency of a Solar Cell Theoretical efficiency of bulk semiconducting materials-based solar cells is determined to be ca. 30%. This is due to the limitation of generation of one exciton upon absorption of one photon in bulk semiconducting material. The efficiency of solar cells could be increased more than 60% upon changing the bulk semiconducting material to quantum dots as the main light absorber [1]. Quantum dots are material with size smaller than their exciton Bohr radius. The exciton Bohr radius is the distance between hole (in valence band) and excited state electron (in conduction band). Therefore, a study of a specific size and morphology that could exhibit MEG in targeted material is crucial to break the limitation of bulk semiconductor-based solar cells. Nonetheless, despite the promising attributes of the quantum dots, the highest photovoltaic (PV) conversion efficiency of quantum dots solar cell (QDSC) that has been recorded is only ca. 18.1% to date [2].

1.2 Breaking the Theoretical and Practical Limit of PV Conversion Efficiency of a Solar Cell Quantum confined semiconducting materials that are capable of producing more than one exciton per absorption of one photon (E photon > bandgap, E g ) would surpass the overall theoretical PV conversion efficiency of a solar cell more than 60%. The peculiar band structure (i.e., expanded, unique and discrete energy levels) of the small-sized semiconducting materials is liable for the massive rise in theoretical

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PV conversion efficiency [3]. Absorption of photon with sufficient energy would excite an electron from the highest occupied molecular orbital (HOMO) to the lowest unoccupied molecular orbital (LUMO); which a hole would be left in the LUMO— the electron–hole pair is known as an exciton. Figure 1a shows the mechanism of MEG which involves (i) excitation of electron in the HOMO − 0 to the LUMO + 1, (ii) relaxation of the excited electron from LUMO + 1 to LUMO + 0 and emission of secondary photon with energy equals to the ~E g of the material, (iii) absorption of the secondary photon by a neighbouring electron, and (iv) excitation of the neighbouring electron. Cumulative generated exciton per absorbed photon energy is two (MEG is likely to occur) [4, 5]. The bulk semiconducting materials however are not capable of producing MEG due to the closely separated energy levels in the conduction band. An electron would be excited from the valence band maximum to the conduction band upon absorption of photon (E photon > E g ). The excited state electron would undergo a relaxation from the high energy level to the lower energy levels. However, multiple small relaxations could be expected, and therefore the excess energy of the excited state electron is released as heat to the surroundings [6]. The cumulative emitted heat could be Fig.1 a Presence of MEG in a quantum confined semiconducting material, b MEG is not present in bulk light absorber due to excessive energy loss from heat dissipation during relaxation of exciton to the lowest energy level of unoccupied molecular orbital [7]

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absorbed by the neighbouring electron; however insufficient to initiate a secondary excitation (MEG is unlikely to occur).

1.3 The Candidate to Be Studied MoS2 with narrow bandgap (1.29 eV) [8] is aimed for the study. The MEG is hypothesized would occur in small MoS2 nanocrystal below its exciton Bohr radius (1.62 nm) [9]. The small quantum confined structure MoS2 has different chemical, structural and optoelectronic properties in comparison with that of the bulk analogue. Figure 2a shows significant increment of publications from the year 2000 to 2021; which correlated to the increasing number of research activities and initiatives in the field of MoS2 applications in PV technology. Note the difference of number of publications between the initiatives i.e., bulk-based (Fig. 2a) and nanomaterial-based (Fig. 2b) MoS2 solar cells are in the scale of hundreds. This observation indicates new opportunities to investigate the fundamental properties (optical and electronic) of small MoS2 nanocrystals, which would shed light on the issue of insignificant PV conversion efficiency of quantum dots solar cells.

2 Methodology Realistic MoS2 models were built based on a well-established bulk crystallography profile. The internal coordinates of a basic MoS2 crystal structure (i.e., bond angles, bond lengths and dihedral angles) were replicated in three dimensions using z-matrix coordinates during the basic crystal modelling stage. The prepared models were later optimized to the lowest energy structure through a series of calculations. The interactions (potential and kinetic energy) between electron, proton, neutron, and correlation-exchange energy between two neighbouring electrons in the same orbital were taken into considerations [1]. The prepared models were optimized to the lowest energy structure using density functional theory (DFT) calculations at Becke’s three parameter hybrid method with the Lee, Yang and Parr (b3lyp) correlation functional [10, 11], and lanl2dz basis set. Therefore, an accurate description of binding energy, surface states, trap states, and surface stabilization would be provided [2]. The optimized structures were then analysed using harmonic frequency calculations. Models which showed negative frequencies were discarded during this stage – an indication of non-realistic models. The unoccupied (UMO) and occupied molecular orbitals (OMO) of the realistic models were calculated using time-dependent density functional theory (TD-DFT) at a similar level of theory with that of the optimization procedure. The occurrence of MEG was analysed based on a simple simulation of excitation using a photon source with energy two folds of the bandgap of the MoS2 models (E photon = 2E g ).

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Fig. 2 Number of papers published from 2000 to 2021; generated from ISI Web of Science using keywords a ‘MoS2 ’ and ‘solar cell’, b ‘MoS2 nanoparticles’ and ‘solar cell’

3 Results and Discussion 3.1 Realistic Models of MoS2 Five (MoS2 )n models where n = 2, 3, 6, 8 and 12 were built, optimized, and validated as realistic using harmonic frequency analysis. The excited state electron density (LUMO) and ground state electron density (HOMO) were mapped based on TDDFT calculations (Fig. 3). Uniform distribution of LUMO are observed in small models i.e., n = 2, 3 and 6. However, localization of LUMO densities are observed in bigger models i.e., n = 8 and 12; which are mainly at Mo atoms. MoS2 crystals with uniform LUMO distributions would indicate efficient excited state electron injection

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Fig. 3 a, b, c are visualization of HOMO, and d, e, f are visualization of LUMO for some of the realistic models i.e., (MoS2 )3 , (MoS2 )6 and (MoS2 )8 respectively

from a fluorophore to a metal oxide semiconductor in an excitonic solar cell [12]. Therefore, a laboratory technique that could synthesize MoS2 nanocrystals with similar structure/geometry with that of the (MoS2 )2 , (MoS2 )3 , and (MoS2 )6 ; could be an early step to break the limitation of the theoretical PV conversion efficiency of a bulk semiconductor-based solar cell.

3.2 MEG Occurrence Analysis The calculated excited state energy levels of the realistic models i.e., (MoS2 )2 , (MoS2 )3, (MoS2 )6, (MoS2 )8, and (MoS2 )12 were analysed using TD-DFT based on the minimum requirement of excitation source i.e., E photon = 2E g . An electron excitation upon absorption of a photon with sufficient energy would occur from a negative energy level of ground state to a negative energy level of excited state (known as bonding energy level). The highly energized electron would then undergo a relaxation to the lowest excited state energy level. Subsequently, the emitted photon would therefore be absorbed by the neighbouring electron which could lead to a formation of secondary exciton –indicates a possibility of the MEG to occur. The electron transitions from the ground state to the excited state, and MEG occurrence in the predicted realistic models were summarised in Table 1. The MEG is likely to occur in the predicted realistic models i.e., MoS2 )2 , (MoS2 )3, (MoS2 )6, (MoS2 )8, and (MoS2 )12 . Nonetheless, an electron transition from a negative energy level of ground state to a positive energy level of excited state (anti-bonding energy level) would contribute

Multiple Exciton Generation in MoS2 Nanostructures: A Density … Table 1 Electronic transitions in realistic MoS2 models

403

Structure and size

Properties

Details

(MoS2 )2 0.54 nm

Bandgap

2.1889 eV

Ground state

HOMO − 0 (−6.7963 eV)

Excited state

LUMO + 12 (−0.1197 eV)

MEG occurrence

Likely to occur

Bandgap

1.3674 eV

Ground state

HOMO − 0 (−4.3171 eV)

Excited state

LUMO + 9 (−1.6109 eV)

MEG occurrence

Likely to occur

Bandgap

1.7151 eV

Ground state

HOMO − 0 (−7.4100 eV)

Excited state

LUMO + 9 (−3.9537 eV)

MEG occurrence

Likely to occur

Bandgap

1.2550 eV

Ground state

HOMO − 0 (−6.8238 eV)

Excited state

LUMO + 20 (−1.6163 eV)

MEG occurrence

Likely to occur

Bandgap

0.9543 eV

Ground state

HOMO − 0 (−3.8748 eV)

Excited state

LUMO + 20 (−2.0027 eV)

MEG occurrence

Likely to occur

(MoS2 )3 0.62 nm

(MoS2 )6 0.95 nm

(MoS2 )8 1.09 nm

(MoS2 )12 1.57 nm

irrelevantly to the MEG occurrence [13]. The absorbed photon with E photon = 2E g could be sufficient to liberate the electron from the unoccupied molecular orbitals. The highly energised electron would therefore not undergo the relaxation to the lowest excited state energy level. The trends of increasing bandgap upon MoS2 size reduction below its exciton Bohr radius in Fig. 4a, is an indicator of quantum confinement effect which alters the energy levels of a semiconducting material. The (MoS2 )2 , (MoS2 )3, (MoS2 )6, (MoS2 )8, and (MoS2 )12 realistic models would exhibit the targeted size of 0.54, 0.62, 0.95, 1.09, and 1.57 nm with the bandgap of 2.1889, 1.3674, 1.7151, 1.2550, and 0.9543 eV respectively.

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Fig. 4 The trends of a increasing bandgap, b decreasing number of electronic transitions with decrement of cluster size. Fitted data are denoted by solid lines

Furthermore, the number of electronic transitions decreases with the decrease of cluster size as observed in Fig. 4b. This observation is due to the discrete energy levels upon expansion of energy levels of small MoS2 nanocrystals in the range of strong quantum confinement effect.

4 Conclusion In conclusion, realistic models of (MoS2 )n where n = 2, 3, 6, 8 and 12 with bandgap of 2.1889, 1.3674, 1.7151, 1.2550 and 0.9543 eV respectively; have been established and validated using a sequence of density functional theory calculations. The optoelectronic properties of the models were studied, which clearly showed that the MEG could occur upon absorption of photon with energy two folds of their bandgaps in the range of 1.909–4.3778 eV. The source of photon with specified energy is correlated to red to ultraviolet light; which is abundantly available on the surface of the Earth. Acknowledgements This work is funded by the Research & Innovation Department of Universiti Malaysia Pahang Al-Sultan Pahang, Universiti Teknologi MARA and International Islamic University of Malaysia through Sustainable Research Collaboration Grant (RDU 200711).

References 1. Murphy JE, Beard MC, Norman AG, Ahrenkiel SP, Johnson JC, Yu P, Mi´ci´c OI, Ellingson RJ, Nozik AJ (2006) PbTe colloidal nanocrystals: synthesis, characterization, and multiple exciton generation. J Am Chem Soc 128(10):3241–3147 2. Green MA, Dunlop ED, Hohl-Ebinger J, Yoshita M, Kopidakis N, Hao X (2022) Solar cell efficiency tables (version 59). Photovoltaics 30:3–12

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3. Shockley W, Queisser HJ (1961) Detailed balance limit of efficiency of p-n junction solar cells. J Appl Phys 32(510) 4. Padilha LA, Bae WK, Klimov VI, Pietryga JM, Schaller RD (2013) Response of semiconductor nanocrystals to extremely energetic excitation. Nano Lett 13(3):925–932 5. McGuire JA, Joo J, Pietryga JM, Schaller RD, Klimov VI (2008) New aspects of carrier multiplication in semiconductor nanocrystals. Acc Chem Res 41(12):1810–1819 6. Beard MC, Johnson JC, Luther JM, Nozik AJ (2015) Multiple exciton generation in quantum dots versus singlet fission in molecular chromophores for solar photon conversion. Phil Trans R Soc A 373(2044):20140412 7. Nozik AJ (2011) Multiple exciton generation in semiconductor quantum dots. Chem Phys Lett 457(1):2–11 8. Yang K, Liu T, Zhang XD (2021) Bandgap engineering and near-infrared-II optical properties of monolayer MoS2 : a first-principle study. Front Chem 9 9. Jia GY, Liu Y, Gong JY, Lei DY, Wang DL, Huang ZX (2016) Excitonic quantum confinement modified optical conductivity of monolayer and few-layered MoS2 . J Mater Chem C 4:8822– 8828 10. Lee C, Yang W, Parr RG (1988) Development of Cole-Salvetti correlation-energy formula into a functional of the electron density. Phys Rev B 37(2):786–789 11. Frisch MJ, Trucks GW, Schlegel HB, Scuseria GE, Robb MA, Cheeseman JR, Scalmani G, Barone V, Mennucci B, Petersson GA, Nakatsuji H, Caricato M, Li X, Hratchian HP, Izmaylov AF, Bloino J, Zheng G, Sonnenberg JL, Hada M, Ehara M, Toyota K, Fukuda R, Hasegawa J, Ishida M, Nakajima T, Honda Y, Kitao O, Nakai H, Vreven T, Montgomery Jr JA, Peralta JE, Ogliaro F, Bearpark M, Heyd JJ, Brothers E, Kudin KN, Staroverov VN, Kobayashi R, Normand J, Raghavachari K, Rendell A, Burant JC, Iyengar SS, Tomasi J, Cossi M, Rega N, Millam JM, Klene M, Knox JE, Cross JB, Bakken V, Adamo C, Jaramillo J, Gomperts R, Stratmann RE, Yazyev O, Austin AJ, Cammi R, Pomelli C, Ochterski JW, Martin RL, Morokuma K, Zakrzewski VG, Voth GA, Salvador P, Dannenberg JJ, Dapprich S, Daniels AD, Farkas Ö, Foresman JB, Ortiz JV, Cioslowski J, Fox DJ (2009) Gaussian 09, Revision B.01. Gaussian Inc., Wallingford, CT 12. Muzakir SK, Alias N, Yusoff MM, Jose R (2013) On the missing links in quantum dot solar cell: a DFT study on fluorophore oxidation and reduction process in sensitized solar cells. Phys Chem Chem Phys 38(15):16275–16285 13. Shaafi NF, Muzakir SK, Kadir MFZ, Aziz SB (2019) A density functional theory study on multiple exciton generation in lead chalcogenides. Mol Cryst Liq Cryst 693(1):57–65

Relationship Between Strength Development and Porosity of Epoxy-Based Mortar Nur Farhayu Ariffin, Sharifah Maszura Syed Mohsin, Khairunisa Muthusamy, Fadzil Mat Yahaya, and Saffuan Wan Ahmad

Abstract Epoxy resin is conventionally combined with a hardener for the purpose of curing. However, prior research has indicated the potential for epoxy resin to undergo curing in the presence of calcium hydroxide originating from cement hydration. This current study delves into the utilization of commercially accessible epoxy resin without a hardener as an additive in mortars, aiming to enhance mortar strength. The mortar formulations were created with a cement to fine aggregate mass ratio of 1:3, a water-cement ratio of 0.48, and varying epoxy content at 5, 10, 15, and 20% of the cement weight. Subsequent to formulation, the mortars underwent periods of dry curing as well as 5 days of wet curing followed by additional dry curing, all within a tropical environment. The outcomes of the study revealed that the optimal epoxy content for the wet-dry curing process was 10%. Mortars containing 10% epoxy demonstrated notably heightened compressive and flexural strengths compared to the control mortar that lacked epoxy. Over extended dry curing periods, the strength progression of the epoxy-altered mortars exhibited continuous enhancement. Concurrently, the porosity of mortars incorporating epoxy experienced a reduction as the curing duration increased. These findings indicate the viability of epoxy resin devoid of a hardener as a polymeric admixture to augment both the strength and durability of mortars. The ideal epoxy proportion for effective wet-dry curing was determined to be 10%, while the improvement in mortar strength persisted with extended periods of dry curing. Furthermore, the curing period exerted a decreasing influence on the porosity of mortars modified with epoxy. Keywords Epoxy resin without hardener · Epoxy mortar · Strength performance

N. F. Ariffin (B) · S. M. Syed Mohsin · K. Muthusamy · F. Mat Yahaya · S. Wan Ahmad Faculty of Civil Engineering Technology, Universiti Malaysia Pahang Al-Sultan Abdullah, Lebuhraya Tun Razak, 26300 Gambang, Pahang, Malaysia e-mail: [email protected] © The Author(s), under exclusive license to Springer Nature Singapore Pte Ltd. 2024 R. Abd. Aziz et al. (eds.), Intelligent Manufacturing and Mechatronics, Springer Proceedings in Materials 40, https://doi.org/10.1007/978-981-99-9848-7_37

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1 Introduction Epoxy resin is a commonly employed material in the repair of concrete structures. Typically, the presence of a hardener is essential to initiate the curing process of epoxy resin. Without the hardener, epoxy resin remains in an unhardened state, limiting its utility. However, this study delves into an innovative approach by investigating the use of epoxy resin without a hardener within mortar applications. The hypothesis is that epoxy resin has the potential to undergo hardening through a reaction with hydroxyl ions produced during the cement hydration process. This research holds significant promise as it could open pathways for novel concrete repair techniques, particularly in tropical climates where humidity and temperature variations influence traditional curing processes. Moreover, adopting epoxy mortar without a hardener introduces a potentially cost-efficient alternative that aligns with resource conservation objectives and reduces the environmental footprint associated with conventional epoxy-hardener systems. Previous research [1] has indicated that epoxy resin without a hardener exhibits slower and weaker hardening properties compared to epoxy resin with a hardener, particularly at ambient temperatures. This challenge prompts the exploration of new curing methodologies that can harness the hardening potential of epoxy resin even without traditional hardener additives. To address this, the current study employs two distinct curing methods suitable for the tropical environment in Malaysia. This approach involves a comprehensive analysis of the interaction between epoxy resin and the cement hydration process, aiming to unravel the mechanisms behind the development of mortar strength and the evolution of mortar porosity. By shedding light on the intricate interplay between epoxy resin and cement hydration, this study contributes to advancing concrete repair practices and materials, particularly in challenging climatic conditions.

2 Methodology 2.1 Materials Obtained from the Holcim Cement Manufacturing Company of Malaysia and adhering to the ASTM C150 standard, the material was utilized. In ordinary Portland cement (OPC), a key component is calcium oxide, which plays a pivotal role. The successful hydration process of OPC hinges upon an adequate supply of calcium oxide. This process of hydration typically entails a range of calcium silicates, such as alite and belite, forming the fundamental of cement hydrate. Furthermore, tricalcium aluminate and calcium aluminoferrite, prominent constituents, are also inherent within cement hydrate compositions. The arrangement of cement hydrates can be observed in Fig. 1, illustrating their configuration through FESEM morphology analysis.

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Fig. 1 FESEM morphology of cement hydrates without addition of epoxy resin

Table 1 Properties of epoxy resin Epoxy equivalent

Molecular weight

Density, (g/cm3 , 20 °C)

Viscosity, (MPa ・s, 20 °C)

Flash point, (°C)

184

380

1.16

10,000

264

The fine aggregate used in this study is widely known as river sand, sourced locally, with a specific gravity of 2.62 and a fineness modulus of 2.85. To prepare it for experimentation, the initial stage entails placing the fine aggregates in an oven for drying, followed by a process of wetting until it reaches a state known as the saturated surface-dry condition. The epoxy resin utilized in the mixture was Diglycidyl Ether of Bisphenol A Type, and it is employed without the inclusion of a hardener in the mix. To ensure its integrity, the epoxy resin is stored at room temperature to prevent any potential damage. The mixture consists of varying epoxy content, ranging from 5 to 20%, and the characteristics of the pure epoxy resin can be found in Table 1. Specifically, a higher viscosity epoxy resin was selected to meet the requirement of effective interaction between the epoxy resin without a hardener with hydroxyl ions. The viscosity of the chosen epoxy resin plays a pivotal role in facilitating the reaction between the epoxy resin and the hydroxyl ions.

3 Experimental Procedure Following the guidelines of JIS A 1171 [2], the formulation of epoxy-modified mortar entailed thorough blending of materials at specified ratios. The cement to fine aggregate mass ratio remained consistent at 1:3, while the epoxy content varied, encompassing percentages of 5, 10, 15, and 20% relative to the cement quantity. Additionally, a water-cement ratio of 0.48 was applied. To ensure the desired consistency of the mixture, as measured by the flow diameter, it was maintained within the range of 170 ± 5 mm. For subsequent testing, mortar cube specimens measuring 70

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× 70 mm were cast for the evaluation of compressive strength, while prism specimens with dimensions of 40 × 40 × 160 mm were prepared for flexural strength testing. These specimens were subjected to a curing period of 28 days. Additionally, for the comparison, a control specimen composed of ordinary Portland mortar was also cast. Two distinct curing methods were applied to the epoxy-modified mortar without a hardener: wet-dry curing and dry curing. In the wet-dry curing regimen, the specimens were initially exposed to damp burlap for a period of two days, followed by immersion in water for a continuous five-day period. Subsequently, the specimens were removed from the water and placed at room temperature for an additional 21 days. Conversely, the dry curing regimen commenced with an initial curing phase under damp burlap for two days, followed by subsequent curing at room temperature, which extended for 26 days. For the conventional mortar, water curing was employed as the curing procedure. A compressive strength and flexural strength of the cubic and prism specimens were evaluated following the guidelines stipulated by ASTM C109 [3] and ASTM C348-08 [4], respectively.

4 Results and Discussions Density test. The measurement of physical properties, specifically the density of the epoxy mortar, was conducted upon the completion of a 28-day curing period, as depicted in Fig. 2. The density of the epoxy-modified mortar fell within a range of 2020–2160 kg/m3 , with an average value of approximately 2089 kg/m3 . Interestingly, the standard mortar exhibited a density that was quite similar, indicating that the incorporation of epoxy had a minimal impact on density. The average density of the regular mortar was recorded at 2200 kg/m3 , and the disparity between the densities of epoxy-modified and standard mortar was not notably significant. The introduction of the polymer resulted in a reduction of approximately 5% in the density of the epoxymodified mortar. Despite the epoxy-modified mortar having a slightly lower density compared to the standard mortar, it demonstrated a higher compressive strength [5]. This suggests that the density variation did not significantly influence the mortar’s strength [6]. Compressive strength. The compressive strength of epoxy mortars with varies percentage was illustrated in Fig. 3. The graph portrayed the compressive strength results obtained from all tested samples following a 28-day curing period. The mortar containing 10% epoxy content had exhibited superior compressive strength, recording at 36 MPa, surpassing the strength of the other samples. These findings highlighted the potential of epoxy resin without a hardener in mortar to achieve higher levels of strength. This effect could be attributed to the presence of hydroxyl ions originating from the cement hydration process within the mortar. The epoxy chains had interacted with these hydroxyl ions from cement hydrates, contributing to the formation of a denser mortar structure [7].

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2200

Fig. 2 Diameter of flow test versus epoxy content Density (kg/m3)

2150 2100 2050 2000 1950

Average

1900

Compressive Strength (MPa)

38 Dry cured Wet-dry cured

36 34 32 30 28 26 24 22 20

5

10

15

20

Epoxy Content (%)

Fig. 3 Compressive strength with different curing regime versus percentage of epoxy content

However, it was essential to emphasize that an increase in epoxy content beyond 10% had resulted in a decrease in compressive strength. This decline was attributed to the inclusion of significant quantities of epoxy resin that had not undergone the hardening process within the epoxy-modified mortars. A similar outcome had been observed in prior research conducted by [8], which had explained that the reduction in compressive and flexural strengths of mortar containing epoxy resin without a hardener at epoxy content levels of 20% or higher had been due to the presence of a notable amount of unhardened epoxy resin within the modified mortars. This unhardened epoxy resin had disrupted the bonding within the mortar. Additionally, the graph had illustrated the compressive strength of epoxy mortars subjected to different curing regimes. As previously mentioned, two curing methods had been applied to the mortars: wet-dry curing and dry curing. According to the graph, wet-dry curing had led to higher compressive strength compared to dry curing. For instance, a mortar with 5% epoxy content subjected to dry curing had exhibited a compressive strength of 32 MPa, while the same mortar undergoing wet-dry curing had displayed a superior strength of 34 MPa. Notably, the highest compressive strength had been observed with 10% epoxy content under wet-dry curing conditions, having reached a strength of 36 MPa. Conversely, dry curing had resulted in a

Fig. 4 Flexural and tensile strength versus percentage of epoxy content

N. F. Ariffin et al.

Tensile Strength (MPa)

412 4.5 4.0 3.5 3.0 2.5 2.0 1.5 1.0 0.5 0.0

Dry curing

0

5

10

Wet dry curing

15

20

Epoxy Content (%)

compressive strength of only 33 MPa for the same conditions. As the epoxy content had exceeded 10%, a decline in compressive strength had been observed under both curing regimes. The higher compressive strength observed in the wet-dry curing process can be attributed to the more conducive conditions it provides for cement hydration and epoxy polymerization. The presence of hydroxyl ions, which are necessary to enhance the durability and density of epoxy mortar, makes wet-dry curing particularly suitable. These findings align with the outcomes from other researchers [9], who also showed that the polymerization of epoxy resin significantly contributes to the improvement in concrete strength. Flexural and Splitting Tensile test. The splitting tensile strength test results for epoxy mortar and normal mortar were displayed in Fig. 4. Notably, normal mortar exhibited lower tensile strength than epoxy-modified mortars. Among all the epoxy resin percentages exposed to wet-dry curing conditions, the 10% epoxy resin content in epoxy-modified mortar had displayed the highest splitting tensile strength. However, when the epoxy resin content exceeded 10%, the tensile strength had started to decrease. Specifically, the 10% epoxy content had recorded 3.1 MPa with dry curing and 3.8 MPa with wet-dry curing. In contrast, normal mortar had reported a tensile strength of 2.3 MPa, nearly 40% lower than that of the 10% epoxy-modified mortar. The highest splitting tensile strength observed with the 10% epoxy content was likely due to the rapid consumption of hydroxyl ions produced during the early stages of Portland cement hydration. This rapid consumption had been related to the high reactivity of epoxy resin itself [10]. Consequently, it had accelerated the hydration and polymerization of specimens, leading to the formation of higher volumes of reaction products. Moreover, the 10% epoxy resin content in epoxy-modified mortar had been sufficient to react with hydroxyl ions, reducing the volume of pores and resulting in higher splitting tensile strength than normal mortar. Relationship between Compressive, Flexural and Tensile Strengths. The regression line approach was to analyze the overall data, using compressive strength as the predictor parameter and flexural and splitting strength as response parameters. The

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413 4.0

y = 0.03x + 1.59 R² = 0.90

2.5

3.5 3.0

y = 0.051x + 1.6728 R² = 0.94

2.0

2.5 2.0

1.5

1.5

1.0

1.0 0.5

Tensile Linear (Tensile)

Flexural Linear (Flexural)

Flexural Strength (MPa)

Splitting Tensile Strength (MPa)

3.0

0.5 0.0

0.0 20

25

30

35

40

Compressive strength (MPa) Fig. 5 Relationship between compressive, flexural and splitting tensile strengths of 10% epoxymodified mortar in 28 days

coefficients of the linear regression equation, along with the correlation coefficient for the entire dataset, are presented in Fig. 5. From the figure, it is evident that this relationship resulted in correlation coefficients of 0.90 and 0.94 for tensile and flexural strength of epoxy mortar, respectively. Additionally, the figure illustrates that as compressive strength increases, so do the flexural and splitting tensile strengths. The statistical analysis results from this equation indicate a strong correlation between compressive, flexural, and splitting tensile strengths. This linear relationship underscores the high potential of using 10% epoxy resin added to the mixture without a hardener in construction. The results of the strength tests reveal that epoxy mortar with 5% epoxy resin exhibits properties almost identical to those of the 10% epoxy-modified mortar. This similarity arises because the amount of epoxy resin is nearly the same in both specimens. However, in the case of the 5% epoxy content specimen, the amount of epoxy resin was insufficient to react with hydroxyl ions, resulting in lower compressive strength compared to the 10% epoxy resin specimen at 28 days. This implies that the amount of epoxy resin in the 5% epoxy-modified mortar was fully utilized at an early age. Conversely, in specimens with 15 and 20% epoxy resin, the excessive amount of unhardened epoxy resin renders unsuitable for use due to their lower strength performance. Consequently, it becomes evident that 10% epoxy resin in the epoxy-modified mortar mixture is the optimal mix design, performing well both at an early and later age. Strength development. Figure 6 shows the strength development of 10% epoxy mortar after 180 days of different curing regimes compared to normal mortar. The graph showcases a significant trend wherein the compressive strength of 10% epoxy mortar steadily increases beyond the 180-day curing period, regardless of the curing method. In contrast, normal mortar experiences a strength increase until approximately 120 days, after which it stabilizes. Notably, the 10% epoxy mortar subjected

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Fig. 6 Strength development of epoxy-modified mortar after 180 days

to wet-dry curing displays continuous strength gains even beyond the 180-day duration. Additionally, the strength development of 10% epoxy mortar under dry curing aligns with that of the epoxy mortar under wet-dry curing, although at a slower pace. This investigation of incorporating epoxy resin without a hardener into mortar compositions aligns with the findings in reference [11], which suggest that the interaction between epoxy resin and hydroxyl ions leads to the formation of robust bonds and the creation of durable concrete structures. In summary, the outcomes of this study underscore the potential of epoxy resin, without the need for a hardener, as a valuable additive for enhancing mortar strength and durability over extended periods, reaffirming its effectiveness as a practical admixture. Initial Surface Absorption test. An initial surface absorption test (ISAT) was conducted on both normal mortar and epoxy mortar with varying epoxy resin content at 28 days of age. Readings were taken at intervals of 10, 30, 60, and 120 min, and the numerical absorption values obtained from the specimens are presented in Fig. 7. At 28 days, it’s evident that at the 10-min interval, the ISAT readings were as follows: 0.35 ml/m2 /s for normal mortar, 0.25 ml/m2 /s for 5% epoxy mortar, 0.23 ml/ m2 /s for 10% epoxy mortar, 0.18 ml/m2 /s for 15% epoxy mortar, and 0.317 ml/m2 / s for 20% epoxy mortar. As the testing duration increased, the rate of absorption gradually decreased. The figure illustrates that all types of epoxy-modified mortar exhibited a lower water absorption rate compared to the normal mortar specimen. This characteristic indicates that epoxy resin played a role in reducing the permeability of water into the mortar [12]. In general, the performance of epoxy-modified mortar, as observed from the results of water absorption and the initial surface absorption test, can be attributed to the interaction between epoxy resin and hydroxyl ions. After the

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0.40 Normal 5% 10% 15% 20%

Absorption (ml/m2/s)

0.35 0.30 0.25 0.20 0.15 0.10 0.05 0.00 0

20

40

60

80 Time (min)

100

120

140

Fig. 7 Initial surface absorption of different types of epoxy-modified mortar and normal mortar

initial reaction was completed, the unhardened epoxy resin within the mortar would react with hydroxyl ions to fill the pores within the specimen, significantly reducing water flow [13].

5 Conclusions In summary, this study has unveiled several significant findings that contribute to the advancement of epoxy mortar, particularly when used without the need for a hardener. It has been determined that the optimal epoxy content, which maximizes compressive strength, flexural strength, and splitting tensile strength, is set at 10%. Among the various curing methods tested, wet-dry curing has emerged as the most efficient and suitable approach to enhance the effectiveness of epoxy mortar which effectively complements both cement hydration and epoxy polymerization. Furthermore, the correlation observed between compressive, flexural, and tensile strengths emphasizes the potential of utilizing epoxy resin in mortar even without the presence of a hardener. This research highlights the promising feasibility of incorporating epoxy resin as an additive in mortar compositions without the need for a hardener. Additionally, this innovative approach holds great promise for enhancing the performance of concrete structures, especially in tropical climates. Acknowledgements The authors would like to thank the Ministry of Higher Education and University Malaysia Pahang Al-Sultan Abdullah for providing financial support under Fundamental Research grant RDU230301 and for laboratory facilities.

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References 1. Ohama Y, Miyamoto Y (2004) Effects of mix proportioning factors on properties of epoxymodified mortars without hardener, containing nitrite-type hydrocalumite, concrete under severe conditions: environment & loading, CONSEC ’04 2. JIS A 1171 (2016) Test Methods for polymer-modified mortar 3. ASTM C 109/ C 109M (2020) Standard test method for compressive strength of hydraulic cement mortars 4. ASTM C348-21 (2021) Standard test method for flexural strength of hydraulic-cement mortars 5. ASTM C230 (2021) Standard specification for flow table for use in tests of hydraulic cement 6. ASTM C191 (2021) Standard test methods for time of setting of hydraulic cement by vicat needle 7. Ota M, Ohkubo T, Ochi M, Ohama Y (2015) Effects of long-term dry curing on strength development of initially combined wet/dry-cured and steam-cured hardener-free epoxy-modified mortars. Adv Mater Res 1129:339–344 8. Li P, Lu W, An X, Zhou L, Du S (2021) Effect of epoxy latexes on the mechanical behavior and porosity property of cement mortar with different degrees of hydration and polymerization. Materials 9. Ohama Y, Ochi M, Kumagai S, Ota M (2006) Strength development and epoxy resin-cement interaction in hardener-free epoxy-modified mortars. Brittle Matrix Compos 8:315–322 10. Jo Y (2006) Basic properties of epoxy cement mortars without hardener after outdoor exposure. Constr Build Mater 22:911–920 11. Kim WK, Kim DM, Ryu HS, Park WJ, Ham SM (2017) Properties of hardener-free epoxymodified mortars utilizing pyrolysis tar replacement. Constr Build Mater 12. Huseien GF, Sam ARM, Faridmehr I, Baghban MH (2021) Performance of epoxy resin polymer as self-healing cementitious materials agent in mortar. Materials (Basel) 13. Lukowski P (2016) Studies on the microstructure of epoxy-cement composites. Archiv Civil Eng

Modification of Cement Brick’s Properties Using Recyclable Paper Egg Tray S. Surol, M. Y. Chow, A. R. Abd Hamid, D. Syamsunur, J. L. Ng, H. Jusoh, H. K. Lehl, N. F. Abdullah, E. E. Hussin, and N. I. F. Md Noh

Abstract To reduce waste and develop sustainable building solutions, it is becoming more and more crucial to use alternative materials. This research sought to determine if egg trays might be used to modify cement bricks to enhance their qualities. The cellulose fibers in the paper egg tray, which are the main source of organic elements and are created from pulp, assist fill the gap left by the absence of cement in the mixture and may even enhance the thermal insulation capabilities of the bricks. Egg tray waste was added in varying proportions (20, 30, and 40%) to the cement mixture, and the resulting bricks were tested for compressive strength and water absorption at different curing periods (7, 14, and 28 days).In order to produce concrete with the necessary attributes, such as strength, durability, workability, and setting time, the proper amounts by 1:1:3 using mold 200 × 100 × 60 mm. The results showed that the addition of egg tray had a significant effect on the compressive strength and water absorption of the cement bricks. As the proportion of egg tray increased, both compressive strength and water absorption rates also increased. Incorporating egg tray waste as an addition to cement bricks offers an approach to waste disposal that is favorable to the environment. Keywords Cement bricks · Recyclable materials · Bricks properties

S. Surol (B) · M. Y. Chow · A. R. Abd Hamid · D. Syamsunur · J. L. Ng · H. Jusoh · H. K. Lehl · N. F. Abdullah · E. E. Hussin Faculty of Engineering, UCSI University, Cheras, 56000 Kuala Lumpur, Malaysia e-mail: [email protected] A. R. Abd Hamid e-mail: [email protected] N. I. F. Md Noh College of Engineering, Universiti Teknologi MARA, 40450 Shah Alam, Selangor, Malaysia © The Author(s), under exclusive license to Springer Nature Singapore Pte Ltd. 2024 R. Abd. Aziz et al. (eds.), Intelligent Manufacturing and Mechatronics, Springer Proceedings in Materials 40, https://doi.org/10.1007/978-981-99-9848-7_38

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1 Introduction The construction industry is one of the largest consumers of energy and resources globally, with building construction responsible for a significant amount of carbon dioxide emissions. Cement, a key ingredient in construction, is produced and consumed in large quantities and is a major source of emissions due to the complex chemical reactions involved in its production. The civil construction industry is increasingly seeking sustainable strategies, such as the use of natural renewable resources and industrial waste, to reduce its environmental impact. One such sustainable solution is the use of paper egg trays as a modifier for cement-lime bricks. The pulping process used to create paper egg trays results in cellulose fibres that can be used to improve the characteristics of cement-based materials. Using agricultural materials such as natural fibre will increase the mechanical properties of brick [1] such as using banana fiber in reinforced composites can lower sub-structure building costs and increase durability. Studies demonstrated that an increase in recycled fibres in the composite results in a reduction in thermal conductivity and bulk density values. Additionally, flexural strength increases in the fibre content range up to 4%, with higher fibre proportions leading to a gradual decrease in the value of fibre content [2]. Furthermore, research on the recycling of various types of wood pulp and wastepaper fibres to produce fibre cement composites has shown a significant impact on the mechanical and physical properties [3]. The addition of cellulose fibres in concrete results in a decrease in compressive strength of control concrete at 0.5% volume fraction. However, cellulose fibre leads to a significant increase in flexural strength and maximum deflection, indicating the fibre’s strong link and suitability for use as concrete reinforcement. Additionally, the use of cellulose fibres in concrete results in a 24% reduction in water penetration depth and a 42% decrease in the coefficient of permeability compared to control concrete, indicating improved watertightness [4]. Lignocellulosic fibres’ key advantages as cement additives include their low density, low cost, nonabrasive nature, capacity to fill structures to high filling levels, low energy consumption, and wide range of fibres [5]. Therefore, research about building materials based on renewable resources like recycled fibres is needed. This paper discusses the use of cellulose fibres from paper egg tray as reinforcement in cement lime brick. Wood pulp is the primary source of natural fibres used in cementbased polymers. Cement composites were made using recycled fibres made from used cartons and papers. The research of the physical characteristics of specimens that had been subjected to a 28-day hardening process revealed a clear correlation between thermal conductivity and fibre concentration [6]. The aim of this study is to investigate the effects of incorporating cellulose fibres from paper egg trays into cement bricks. The results of this study have the potential to offer an environmentally friendly solution for waste management while improving the sustainability of the construction industry. Cement brick can have recycled and renewable materials added to them to enhance their qualities and lessen cracking problems such as cellulose-containing recycled egg

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trays. The qualities of cement bricks can be greatly enhanced by fibres, and the postcracking behaviors and crack control can be enhanced using fibres in cementitious matrices. The formation of wider cracks can be avoided, as well as drying shrinkage cracking and plastic shrinkage cracking, by including fibres into the cement brick mixture. Fibers can boost the brick’s hardness, making it more robust over time and less prone to cracking [7]. The tension and lack of durability in cement products cause them to quickly shatter when subjected to impact loads or thermal shock. To solve these kinds of problems, fiber reinforcing of cement bond materials might be used. Cellulose is one of the fibers used in cement bonding materials. Because cellulose fibers provide the requisite durability, fire resistance, high strength, and toughness properties, they can be utilized to modify cement. Cellulose fibers are a desired option for ecologically responsible construction practices since they are sustainable and renewable [8]. Since the egg tray will act as waste and have an influence on the environment, to address the flaws in cement goods and protect the environment. This means that by creating new items using the new technology, paper egg trays can be recycled. In addition to addressing the problem of brittleness and cracking in cement products, the idea of adding cellulose fiber from paper egg trays into cement lime bricks also provides an environmentally acceptable solution by recycling waste material.

2 Methodology In this study, few experiments were carried out. To check the gradation of the sand particles, the sieve analysis test of sand was performed. This test is crucial because the quality of the brick might be impacted by the distribution of sand particles in the sand volume. Second, the water absorption test was used to evaluate the bricks’ durability, quality, and weathering behaviors. Thirdly, the compressive strength test is also carried out in this lab to determine the strength that both cement bricks can withstand. Table 1 provides a list of the materials used to make cement brick. Table 1 Materials used to make cement brick Materials

Description

Sand

Diameter less than 2 mm, grading of sand according to ASTM C778

Hydrated lime

It is a dry, colorless crystalline powder that is manufactured by treating calcium oxide with water

Cement

Ordinary Portland cement (OPC). Chemical composition and general compressive strength according to ASTM C180

Egg tray

Cellulose fiber gained from paper egg tray

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2.1 Preparation of Paper Slug Egg trays were shredded into small pieces and soaked in water for 12 h. The soaked egg trays were then blended until they formed a pulp. The pulp was then sieved and pressed to remove excess water. The resulting pulp was dried at room temperature.

2.2 Preparation of Samples The dry materials, namely cement, lime and sand, were batched by weight to determine the proportion of each specimen. The mix design ratio of cement-lime brick was fixed at 1:1:3 (Cement-Lime-Sand) with a water-cement ratio of 0.6. The replacement volume of cement with egg tray was varied at 20, 30, and 40% to investigate the effect of paper egg tray content on the properties of the bricks. Pilot tests were conducted to determine the suitable mix design ratio. The mixture was mixed thoroughly using a trowel and molded with a mould size of 200 mm in length, 100 mm in width, and 60 mm depth. The mold was filled with three layer of mixture and tamped 25 times for each layer. The specimens were left to set for 24 h and then removed from the mold. The cement-lime bricks were cured at room temperature for 7, 14, and 28 days (Figs. 1, 2). Fig. 1 Mixing of materials

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Fig. 2 Filling mixture into the mold

2.3 Mix Proportion The mix design of cement, lime, and sand ratio is a crucial aspect in the construction industry. It involves determining the appropriate proportions of each material to create a concrete mix with desired properties, such as strength, durability, workability, and setting time. The mix design is 1:1:3 where one part of cement, one part of lime, and three parts of sand were used (Table 2). Table 2 Mix design of cement-lime-sand ratio 1:1:3 with various percentages of sand and egg tray Cement

Egg tray

Lime

Sand

Cement water ratio

Percentage (%) ratio

100 1

0 0

100 1

100 3

0.6

Percentage (%) ratio

80 0.8

20 0.2

100 1

100 3

0.6

Percentage (%) ratio

70 0.7

30 0.3

100 1

100 3

0.6

Percentage (%) ratio

60 0.6

40 0.4

100 1

100 3

0.6

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2.4 Sample’s Testing A total of 72 specimens were prepared for water absorption and compression tests. Each specimen was labeled according to its mixture proportion and the date of fabrication. The water absorption test was performed in accordance with ASTM C6717 to determine the percentage of water absorbed by the bricks. The compression test was conducted using a compressive test machine to determine the compressive strength of the bricks in accordance with ASTM C109/C109M-16.

3 Result and Discussion The results indicate that the incorporation of egg tray in the mixtures has a significant effect on the water absorption rate of the resulting bricks. The data shows that the 100% cement mixture had the lowest water absorption rate across all time periods tested, indicating its superior durability compared to the other mixtures. However, as the proportion of egg tray in the mixtures increased, so did the water absorption rate. The 60% cement and 40% egg tray mixture had the highest water absorption rate at all time periods, followed closely by the 70% cement and 30% egg tray mixture.

3.1 Water Absorption Rate of Cement Brick. The water absorption rate of cement bricks with various amount of egg tray are shown in Fig. 3. The results indicate that the incorporation of egg tray in the mixtures has a significant effect on the water absorption rate of the resulting bricks. The data shows that the 100% cement mixture had the lowest water absorption rate across all time periods tested, indicating its superior durability compared to the other mixtures. However, as the proportion of egg tray in the mixtures increased, so did the water absorption rate. The 60% cement and 40% egg tray mixture had the highest water absorption rate at all time periods, followed closely by the 70% cement and 30% egg tray mixture. The rate of increase varied depending on the proportion of egg tray in the mixture. The 80% cement and 20% egg tray mixture had increased in water absorption rate from 7 to 14 days, with an increase of 3.51%. This can be attributed to the porous nature of the egg tray, which continues to absorb water even after the initial curing period. Similarly, the 70% cement and 30% egg tray mixture had large increased in water absorption rate, with an increase of 4.05% from 7 to 14 days. The 60% cement and 40% egg tray mixture had the smallest increase in water absorption rate, with an increase of only 1.12%. This suggests that the high percentage of egg tray in the mixture had already contributed to the high-water absorption rate after 7 days of curing. Comparing the water absorption rate at 28 days to that at 14 days, the rate slightly decreased for the 100% cement mixture, from 11.34 to 11.25%.

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For the 80% cement and 20% egg tray mixture, the water absorption rate decreased from 16.65 to 15.02%, a decrease of 1.63%. This decrease in water absorption rate can be attributed to further curing and hardening of the materials over time, which reduces their porosity and ability to absorb water. In contrast, the water absorption rate increased for the 70% cement and 30% egg tray mixture and the 60% cement and 40% egg tray mixture. The 70% cement and 30% egg tray mixture had an increase of 0.12% in water absorption rate, from 18.86 to 18.98%. The 60% cement and 40% egg tray mixture had the largest increase in water absorption rate, from 21.89 to 22.27%, an increase of 0.38%. The higher water absorption rate in modified bricks can be attributed to the presence of organic materials in the egg tray, which creates pores in the brick and allows water to penetrate more easily. The organic materials, such as cellulose and lignin, can also absorb and retain moisture, contributing to the increased water absorption rate of the modified bricks. These findings suggest that although incorporating egg tray into cement-lime brick has potential benefits such as reducing waste and cost, it also results in lower water resistance of the resulting bricks (Tables 3, 4).

Fig. 3 Influence of egg tray content on water absorption rate after 7, 14, and 28 days

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Table 3 Result of water absorption rate for bricks at 7,14, and 28 days Mixture

7 days (%)

14 days (%)

28 days (%)

100% cement

10.93

11.34

11.25

80% cement/20% paper tray, lime & sand

13.14

16.65

15.02

70% cement/30% paper tray, lime & sand

14.81

18.86

18.98

60% cement/40% paper tray, lime & sand

20.77

21.89

22.27

Table 4 Classification of bricks regarding with water absorption test Brick class

Maximum water absorption (%)

First

20

Second

22

Third

25

Heavy-duty machine-made bricks

5

3.2 Compressive Strength of Cement Brick The compressive strength of cement lime bricks with various amounts of egg tray are shown in Fig. 4. The study found that incorporating egg tray in cement-lime brick has a significant effect on the properties of the resulting bricks. The data indicates that the 70% cement and 30% egg tray mixture consistently showed the highest compressive strength, while the 100% cement mixture consistently showed the lowest compressive strength. This suggests that the egg tray, which contains cellulose fibres, helps to improve the overall strength of the concrete by providing additional reinforcement to the cement matrix. However, the data also revealed that the compressive strength of the mixtures containing egg tray decreased over time, possibly due to the egg tray fibres absorbing moisture and causing shrinkage or acting as weak points in the structure of the bricks. Possible explanations for this include the absorption of moisture by egg tray fibres causing shrinkage and the fibres acting as weak points in the structure of the bricks. The 70% cement and 30% egg tray mixture consistently showed the highest compressive strength at all three time points of 7, 14, and 28 days. This indicates that this mixture had a more optimal balance of cement and aggregates, which resulted in stronger bonds and a higher compressive strength (Table 5). Based on the data collected, it can be observed that the compressive strength values of all the brick samples, except for the 100% cement mixture brick, fall within the range of 1.5–2.5 N/mm2 , which is typical for sun-dried bricks. This suggests that the manufacturing process used for these samples, which involved modifying the brick mixture with natural fibres, was effective in producing bricks of comparable strength to traditional sun-dried bricks. However, it is important to note that the compressive strength value of the 100% cement mixture brick was found to be lower than 1.5 N/ mm2 , indicating that this mixture may not be suitable for construction projects that require higher strength and durability. It is likely that the egg tray, which is a waste

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Fig. 4 Influence of mixture content on compressive strength at 7, 14, and 28 days

Table 5 Result of compressive strength at 7, 14, and 28 days Compressive strength (N/mm2 ) Time (days) 100% cement 80% cement/20% 70% cement/30% 60% cement/40% egg tray, lime & sand egg tray, lime & sand egg tray, lime & sand 7

0.635

2.102

2.552

2.288

14

0.875

1.904

2.514

2.219

28

0.98

1.754

2.299

2.17

material that contains cellulose fibres, helped to improve the overall strength of the concrete by providing additional reinforcement to the cement matrix. This suggests that the addition of egg tray to the mixture negatively impacts the long-term strength and durability of the bricks. A possible explanation for this decrease in compressive strength is that the egg tray fibres may have absorbed some of the moisture from the mixture, causing shrinkage and reducing the overall strength of the bricks. The strength however occupied with the standard of the sun-dried bricks which were between ranges of 1.5–2.5 N/mm2 (Table 6).

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Class

Compressive strength (N/mm2 )

First class brick

10

Second class brick

7

Building brick

3.5

Sundried brick

1.5–2.5

4 Conclusion Based on the experiment’s findings, it can be said that using egg trays as an additive when building bricks has a favourable effect on the bricks’ compressive strength. In comparison to the typical cement lime brick built of 100% cement, the modified bricks, which contained varying amounts of egg tray, demonstrated better compressive strength. The compressive strength of the changed bricks, however, gradually declined while that of the regular bricks increased. Despite this, compared to standard bricks, the changed bricks still had a higher compressive strength. This might be because of the modified brick’s egg tray material having a higher porosity or water permeability, which can cause the brick to deteriorate over time. This is a noteworthy discovery since it suggests that the modified brick may not be as resilient to water penetration as the standard brick in terms of durability or longevity. The inclusion of the egg tray material in the mixture may be one rationale for the modified brick’s greater water absorption rate. The substance used for the egg trays might be more porous or water permeable than the cement used to make regular bricks, which would increase the rate at which water would be absorbed. In conclusion, the inclusion of egg tray material in the modified brick mixture suggests a potential for a long-lasting and environmentally friendly replacement in the building sector. The addition of egg tray material improves the modified brick’s compressive strength, making it a competitive alternative to the standard brick. Additionally, the usage of egg tray materials offers a waste management solution and lessens the demand for cement, which has a large carbon footprint. When choosing the right brick for a construction project, the increased water absorption rate and lesser density compared to a regular brick should be considered.

5 Recommendation It is important to look at the modified brick’s lower density and increased water absorption rate in more detail to increase the qualities without sacrificing compressive strength. The usage of additives or different materials can be investigated. The modified brick should also be assessed for its long-term weather resistance, durability, and capacity to tolerate severe temperatures, wetness, and other environmental variables. To ensure the lifespan and sustainability of the modified brick, it is also

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important to research how aging will affect its qualities. Thirdly, it should be investigated whether firing the modified egg tray brick at high temperatures might increase its compressive strength and water absorption rate. However, this design can be used for lightweight wall used such as fencing wall and interlocking bricks. Acknowledgements The author would like to express their gratitude towards team members of the Faculty of Engineering, UCSI University for their continuous support and guidance throughout the research.

References 1. Ranjitham GK (2019) Study on effect of banana fiber on performance of soil cement brick. Int Res J Eng Technol IRJET 6(2):2935–0056 2. Nadezda V (2015) Cellulose fibres used in building material. In: Proceedings of REHVA annual conference 2015. advanced HVAC and natural gas technologies, Riga, Latvia. https://doi.org/ 10.7250/rehvaconf.2015.031 3. Hospodarova SS (2015) Possibilities of using cellulose fibres in building materials. In: IOP conference series: materials science and engineering 2015.https://doi.org/10.1088/1757-899X/ 96/1/012025 4. Harshbab R (2020) Influence of cellulose fibre addition on self-healing and water permeability of concrete. Case Stud Constr Mater 12(062020):e00324. https://doi.org/10.1016/j.cscm.2019. e00324 5. Larissa D (2019) Textile natural fibres production regarding the agroforestry approach. SN Appl Sci 1:914. https://doi.org/10.1007/s42452-019-0937-y 6. Bentchikou M (2012) Effect of recycled cellulose fibres on the properties of lightweight concrete composite matrix. Constr Build Mater 34:451–456. https://doi.org/10.1016/j.conbuildmat.2012. 02.097 7. Anas M (2020) Fiber reinforced concrete: a review. In: Engineering proceedings 12th international civil engineering conference (ICEC-2022). https://doi.org/10.3390/engproc20220 22003 8. Yanling Z, Chao D, Swetha Kumari B, Zhibin H, Yonghao N (2022) Molded fibre and pulp products as green and sustainable alternatives to plastics: a mini review[J]. J Bioresour Bioprod 7(1):14–25.https://doi.org/10.1016/j.jobab.2021.10.003

Performance Test of Emulsifiers for Bitumen Emulsion Mixture Mohd Najib Razali , Hana Syakirah Md Hadun, Abdurahman Hamid Nour , Najmuddin Mohd Ramli , and Mohd Khairul Nizam Mohd Zuhan

Abstract The research revealed that when the surface temperature is lower than the ambient air temperature, it can result in condensation, hence facilitating the proliferation of mould and fungi. The issue at hand pertains to locations such as hospital operating theatres, where it is imperative to uphold a temperature that is lower than the ambient surroundings. The objective of the study was to address this issue through the development of Emulsified Modified Bitumen (EMB) utilising 3 distinct emulsifiers (non-ionic, cationic and anionic) in order to offer coating and insulation capabilities. The research employed industrial-grade bitumen (60/70) that was enhanced with recycled used oil and combined with three distinct types of emulsifiers in order to generate three distinct formulated EMBs (C, B, and A). In this work, three distinct emulsifiers were employed in order to produce Emulsified Modified Bitumen (EMB). In the experimental setup, EMB A employed a specific anionic emulsifier known as 2-bromostearic acid, while EMB B utilised a distinct cationic emulsifier termed didodecyldimethylammonium bromide. Lastly, EMB C employed a non-ionic emulsifier known as polyethylene glycol. EMB B exhibited superior performance compared to the other two formed EMBs, as it demonstrated the most favourable characteristics in terms of viscosity, rheological behaviour, and flash point. Additionally, it yielded the most rapid rate of drying, taking only 8 h, and exhibited favourable adhesiveness characteristics without any instances of flaking. However, while considering emulsion stability, it was observed that only 1.67% of the water separated from the original volume of water. As a result, EMB A exhibited the most favourable performance. The research findings indicate that the cationic M. N. Razali (B) · H. S. Md Hadun · A. H. Nour Faculty of Chemical and Process Engineering Technology, Universiti Malaysia Pahang Al-Sultan Abdullah, 26300 Kuantan, Pahang, Malaysia e-mail: [email protected] N. Mohd Ramli MNR Multitech Sdn. Bhd, K02 Ground Floor, Kompleks UMP Holdings, 26300 Gambang, Pahang, Malaysia M. K. N. Mohd Zuhan Pusat Pengajian Diploma Universiti Tun Hussein Onn Malaysia, Hab Pendidikan Tinggi Pagoh, KM1, Jalan Panchor, 84600 Pagoh, Johor, Malaysia © The Author(s), under exclusive license to Springer Nature Singapore Pte Ltd. 2024 R. Abd. Aziz et al. (eds.), Intelligent Manufacturing and Mechatronics, Springer Proceedings in Materials 40, https://doi.org/10.1007/978-981-99-9848-7_39

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emulsifier, referred to as EMB B, demonstrates superior suitability for EMB formulations intended for coating applications. Conversely, the anionic emulsifier, known as EMB A, is found to significantly enhance the stability of emulsions. Keywords Bitumen · Fungi · Emulsified modified bitumen · Recycled base oil · Emulsifier · Performance · Coating

1 Introduction Bitumen is a substance that is generated as a byproduct in the process of refining crude oil. It is distinguished by its sticky stickiness and thick, black colour. When subjected to heat, it becomes pliable, while maintaining its non-volatile nature at normal room temperature [1]. Emulsified Modified Bitumen (EMB) is a composite material composed of bitumen, water, used oil, and an emulsifier. Bitumen exhibits insolubility in water, necessitating the inclusion of an emulsifier in the aqueous medium to facilitate the fragmentation of bitumen into smaller particles and maintain its dispersion within the liquid suspension [2]. The outcome of this process yields a bitumen emulsion, a fluid substance composed of water, bitumen, and an emulsifying agent, wherein small droplets of bitumen are evenly dispersed within the water [2, 3]. This dissertation examines the necessity of producing EMB (emulsified modified bitumen) from industrial waste as a viable substitute for existing products. It highlights the limited research conducted on the investigation of modified bitumen derived from industrial waste [4]. Condensation is a prevalent factor contributing to the presence of moisture, hence potentially resulting in adverse effects on the structural integrity of buildings, indoor air quality, and the proliferation of mould. Condensation can manifest when moist air interacts with a surface barrier that encompasses an underlying piping network, alongside the presence of unvented or inadequately vented surface outlets. Moisture infiltration into buildings can occur through a variety of channels, including wall, door, floor, window, and roof leaks. Healthcare institutions, such as hospitals, have the potential to foster the proliferation of mould or fungi within the infrastructure or on internal surfaces, so impacting susceptible populations. The issue of indoor air pollution poses a substantial threat to human health on a global scale, with biological agents, including mould and fungi, being recognised as contributors to this kind of pollution [5]. The utilisation of Emulsified Modified Bitumen (EMB) in conjunction with a suitable emulsifying agent as an interior surface coating and insulation within the operation theatre presents an optimal resolution for mitigating issues arising from dampness and moisture induced by condensation. The formulations of EMB investigated in this study are derived from recycled oil and incorporate three distinct emulsifying agents. The utilisation of recycled oil serves to mitigate the reliance on primary materials and address the prevalent concern of industrial waste in Malaysia. The EMB material possesses waterproof properties and is capable of functioning as

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a moisture barrier. Moreover, the implementation of EMB has the potential to mitigate the impact of heat transmission from the external environment to the operation theatre and the building, particularly in cases when low temperatures are required. This technology offers thermal insulation capabilities, hence enhancing the overall efficiency of the system. The objective of this research endeavour is to generate Emulsified Modified Bitumen (EMB) by the manipulation of emulsifier types, with the purpose of examining the effects on the performance and compositions of the resulting EMB coating when applied to a dry wall substrate. In order to accomplish this goal, a number of investigations have been outlined. These encompass the analysis of unprocessed materials, the creation of EMB through the utilisation of three distinct emulsifying agents, the analysis of each variant of formulated EMB, the development of a model utilising a plasterboard substrate, and the execution of performance assessments in accordance with the designated ASTM standards, encompassing stability, drying, and adhesion tests.

2 Materials and Technique 2.1 Raw Materials Bitumen of industrial grade (60/70) quality from Kemaman Bitumen Corporation (KBC) and recycled oil from Pentas Flora Sdn. Bhd. were combined to create modified bitumen for this study (MB). The modified bitumen was then mixed with a water-emulsifier mixture to produce the final Emulsified Modified Bitumen (EMB) product. Three types of emulsions were used as emulsifying agents, including nonionic (Polyethylene glycol) from Aladdin, cationic (Didodecyldimethylammonium bromide) from Macklin and anionic (2-Bromostearic acid) from Langchem. Comparisons were made between the three EMB formulations (EMB A, EMB B, and EMB C) and an industrial bitumen emulsion (Atlaskote), as well as a control sample of modified bitumen without the water-emulsifier mix. The purpose of the comparisons was to assess its effectiveness and define the formulated EMB.

2.2 Methods Bitumen 60/70, a semi-solid at room temperature, was heated to 160 °C for 30 min to become a liquid for this study. Then, using a mechanical stirrer (IKA C-MAG HS 7) with three blades, 180 g of the heated bitumen was combined with 120 g of recycled used oil. The modified bitumen took 90 min to make at a 450 rpm mixing rate and a governing temperature of 190 °C. At last, the temperature of the modified bitumen was reduced to 100 °C [4].

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Table 1 EMB formulations using three distinct emulsifier classes EMB type

Type of emulsion

Raw material

Ratio

EMB A

Anionic 2-Bromostearic acid

• Bitumen grade 60/70 • Recycled used oil • Anionic emulsifier Deionised water

Bitumen: 180 g Used oil: 120 g Emulsifier: 3 g Deionised water: 59 ml

EMB B

Cationic Didodecyldimethylammonium bromide

• Bitumen grade 60/70 • Recycled used oil • Cationic emulsifier Deionised water

Bitumen: 180 g Used oil: 120 g Emulsifier: 3 g Deionised water: 59 ml

EMB C

Non-ionic Polyethylene glycol hexadecyl ether

• Bitumen grade 60/70 • Recycled used oil • Non-ionic emulsifier Deionised water

Bitumen: 180 g Used oil: 120 g Emulsifier: 3 g Deionised water: 59 ml

Control sample

No emulsion

Bitumen grade 60/70 only mixed with used oil

Bitumen: 180 g Used oil: 120 g

Atlas

Industrial bitumen emulsion

Atlaskote

–

Forty weight percent of the modified bitumen sample was used in this study, and it was heated to 75 °C while being mixed at 450 revolutions per minute. The emulsifying agent (3 g) was diluted with 60 ml of deionized water and stirred at 200 rpm for 30 min while the modified bitumen was being mixed and heated. Emulsified Modified Bitumen (EMB) was created by adding a water-emulsifier solution to the modified bitumen and mixing the resulting substance for 60 min [2, 3, 6, 7]. This process was repeated for every potential emulsifier (EMB A, EMB B, and EMB C). The formulation ratio and control sample used for each formulated EMB are shown in Table 1.

2.3 Characterisation of Raw Material In this research project, the penetration test was conducted according to American Standard Testing Methods ASTM D5-06. This test is used to measure the consistency of the bituminous material. A higher value of penetration indicates a softer consistency. The penetration value is the vertical distance that the point of a standard needle penetrates into the bituminous material under specific conditions of load, temperature, and time. This distance is measured in one tenths of a millimeter. Bitumen’s softening point was measured using ASTM D36-95, an American standard for laboratory testing. An electric bath, a thermometer, a heater, a shouldered ring, and a ring holder and assembly were used in the experiment (beaker). After

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heating the sample, it was poured into the two shoulder rings to overflow. This was then left to cool at room temperature for at least 30 min. After the excess bitumen had hardened, it was removed with a hot knife. The assembled apparatus including ball centring guides, rings, and a thermometer was placed in the tub. Each ball centring guide was then filled with a ball. The heater was then used to gradually heat the water in the tub from below. The softening point is the average temperature at which a ball encased in bitumen can roll down a slope of 250 mm (1 inch). In this research paper, the term “flash point” refers to the lowest temperature at which a substance can evaporate and form a flammable mixture with air that can be ignited for a brief moment in the presence of a flame. The melting point of oil is an important factor in determining the operating range of a substance. This physical property is used to measure the flammability and volatility of a substance. The flash point of the raw material was established by means of an American Standard Testing Methods, ASTM D93-02a as a part of its characterization.

2.4 Characterisation of Formulated EMB In this research, the viscosity of the samples was measured using a rotational viscometer with a rotational speed of 50 rpm using a plate geometry of 1 mm in a Malvern Instruments set up. The average viscosity was calculated from 10 points taken during the measurement. The oscillatory test was conducted using a controlled shear stress rheometer equipped with a parallel geometry of 1 mm within a temperature range of 0–50 °C. This test was aimed at investigating the material phase transition using temperature sweep tests. The oscillatory test quantifies the sample’s stiffness in addition to its viscoelastic characteristics, which are determined by the microstructure of the material as well as the timescale or frequency over which the deformation is applied [7]. Similar techniques to those used in flash point analysis for raw material characterization were also applied to the flash point test.

2.5 Performance Test of EMB Formulations In this research, the emulsion stability of all formulated EMB samples was tested by taking 100 ml samples from each formulation and testing them for stability under gravity at room temperature. The amount of water separated from the emulsion was measured and recorded after three days using a glass measuring cylinder. This method is considered the best indicator of emulsion stability. Using Eq. (1) below, we were able to determine the separation efficiency (e) as a percentage of the water observed in the measuring cylinder: %W ater separation, e =

V olume o f water r esolved, ml × 100 Original V olume o f water, ml

(1)

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The time taken for the EMB formulation coating on the dry wall to dry was analysed using the standard test method according to ASTM D1640-95. Two types of testing were conducted in this standard, namely set-to-touch time and dust-free time, to ensure that the coating was fully dried [8]. The adhesiveness of the EMB formulation coating was measured using the tape test ASTM D3359-09, which is a standard test method for evaluating the adhesion of a coating material on a substrate. This test is important to ensure that the coating material adheres to the substrate for the expected service life, as the substrate and its surface preparation have a significant effect on the adhesion of coatings. The rate of adhesion is assessed using the depicted scale in the tape test method, which includes placing and removing pressure-sensitive tape over cuts produced in the film.

3 Results and Discussion Table 2 presents a comprehensive summary of the characterization of the raw ingredients employed in the production of bitumen emulsions. The raw materials utilised in the process consisted of recycled used oil sourced from Pentas Flora Sdn. The abbreviation “Bhd.“ typically refers to a private limited company in Malaysia. The procurement of industrial grade bitumen (60/70) is facilitated through Kemaman Bitumen Corporation (KBC). In order to endure the elevated operating temperature of the production process, which reaches 190 °C, the formulation of an emulsified modified bitumen mixture necessitates the utilisation of a primary raw material with a significantly high flash point. The recycled used oil lacks penetration and softening points as it exists in a completely fluid state, whereas the bitumen (60/70) possesses penetration and softening points due to its semi-solid nature, necessitating the evaluation of consistency using penetration tests [7]. The study involved the evaluation of three different types of EMB formulations, along with a control sample (a formulation without emulsion) and an industrial bitumen emulsion obtained from Atlaskote. The characterization of these samples was conducted through various tests, including viscosity testing, moisture content testing, and flash point testing. Table 3 presents the viscosity data for the three types of EMB formulations, including the control sample and the industrial bitumen emulsion obtained from Atlaskote. The viscosity of bitumen refers to its inherent ability to resist flow, serving Table 2 Raw material characterization Material

Flash point (°C)

Bitumen (60/70)

262

Recycled used oil

65

Penetration point at 25 °C

Softening point

Min.

Max.

Min.

Max.

60

70

45

52

N.A

N.A

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as an indicator of its resistance to deformation under shear stress or tensile stress. According to a study conducted by [9], it has been shown that the performance of coating application is enhanced when the viscosity reading of the EMB formulation is lower. Out of the three EMB formulations, it was observed that EMB B exhibited the most minimal viscosity measurement, specifically recording a value of 41,433.72 centipoise (cP). While the Atlaskote standard industrial bitumen emulsion has a relatively low viscosity of 367.75 cP, EMB B’s viscosity remains significantly elevated. The elevated viscosity of this substance presents challenges when attempting to utilise it as a coating due to its significant internal resistance to flow. Consequently, it is not practical, particularly for applications involving spray coating [10, 11]. An elevated viscosity level can lead to an uneven application of the coating. In order to enhance the applicability of the EMB formulation as a coating, it is necessary to provide an additional solvent to decrease its viscosity. Drying the samples in an oven is a standard method for determining moisture content. Drying in an oven makes use of convective heat, generated by blowing or circulating hot air. When compared to other thermogravimetric techniques, ovendrying procedures provide accurate and comprehensive moisture measurements. Table 4 presents the moisture content data for the developed EMB, industrial bitumen emulsion (Atlaskote) and control sample. According to previous research [12], there exists a correlation between moisture content and viscosity, where an increase in moisture content leads to a decrease in viscosity. Table 4 shows that the moisture content varies greatly between the samples, with the control sample having the lowest moisture level and the industrial bitumen emulsion (Atlaskote) having the highest. At 367.75 cP, the Atlaskote bitumen emulsion sample is the least viscous of the four samples testedThe control sample, on the other hand, had the highest viscosity value of 63,346.29 cP and the lowest moisture Table 3 Viscosity data

Type of formulation

Viscosity (cP)

EMB A (anionic)

47,980.68

EMB B (cationic)

41,433.72

EMB C (non-ionic)

46,138.06

Control sample (without emulsion)

63,346.29

Atlaskote

Table 4 Moisture content data

367.75

Sample

Moisture content (%)

EMB A

21.88

EMB B

21.88

EMB C

21.22

Control sample

14.81

Atlaskote

40

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Sample

Flash point (°C)

EMB A (Anionic)

200.2

EMB B (Cationic)

208.1

EMB C (Non-ionic)

202.0

Control sample (without emulsion)

250.0

Atlaskote

267.3

content. The control sample, on the other hand, had the highest viscosity value of 63,346.29 cP and the lowest moisture content. This observation demonstrates a negative correlation between the moisture content of a sample and its viscosity value. In order to enhance the EMB formulation, it is necessary to augment the moisture content by introducing additional solvent, hence ensuring a sustained low viscosity level. The feasibility of coating applications is facilitated by the low viscosity of the substance. Oscillatory rheology is employed to examine the mechanical properties and viscoelastic strength of emulsified bitumen, with the aim of identifying significant deformations resulting from substantial strains. The flash point data for all of the samples are presented in Table 5. The literature demonstrates that all of the samples exhibit flash points that exceed 200 °C. Among the three varieties of formulated EMB, it can be observed that EMB B possesses the greatest flash point. The attainment of a high flash point is crucial for the effective use of the formulated EMB in interior coating applications under standard room temperature conditions, as well as for outdoor coating purposes in normal atmospheric conditions. The drying process is typically regarded as a critical aspect in coating applications. The efficiency of the application may be impacted. The performance and quality of a wall coating are enhanced with a higher drying rate. The rheological characteristic pertaining to the oscillatory test is the rate at which a substrate undergoes deformation and transitions into a solid state. Based on the rheological test results, it can be shown that the EMB B (cationic) emulsifier exhibits the highest degree of deformation and thus leads to a more rapid drying rate, as indicated in Table 6. The pace of drying is contingent upon the speed at which the moisture in the sample coating undergoes evaporation. According to the data presented in the table, it can be observed that the Atlaskote sample coating exhibits a significantly accelerated drying rate in comparison to the coatings of the other samples. This may be attributed to the fact that the Atlaskote sample possesses the highest moisture content among all the samples. The moisture content with the highest value leads to the viscosity with the lowest value, hence facilitating a more rapid drying process. The categorization of the adhesion test outcome is in accordance with the guidelines established in ASTM D3359-09. The data shown that allows for the classification of the percentage of area eliminated into distinct grading categories. The industrial grade bitumen emulsion (Atlas) is classified as 3B, indicating that the total area removed ranges from 5 to 15%. In the present context, it is observed that those categorizations of EMB C, EMB B, and EMB A share a common attribute, namely

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Table 6 The EMB coating’s drying rate Sample

Time taken to completely dry (at room temperature) (h)

EMB A (anionic)

24

EMB B (cationic)

8

EMB C (non-ionic)

20

Based sample (without emulsion)

32

Atlaskote

0.083

a classification of 5B. Furthermore, it is noted that the cumulative extent of removal in these categories amounts to 0% of the entire area. The tabulation of adhesive properties has been completed and is shown in Table 7. The findings unequivocally demonstrate that the industrial-grade bitumen emulsion (Atlas) exhibits suboptimal adherence to the substrate (drywall). On the other hand, it is noteworthy that all variants of emulsified modified bitumen have superior adhesion capabilities. Table 7 summarises the adhesion test results for all samples. The results of this study demonstrate that the industrial grade bitumen emulsion (Atlas) exhibits inferior adhesion to the substrate (drywall), but the three variants of emulsified modified bitumen exhibit superior adhesion performance. Inadequate adhesion is a characteristic shown by coatings, which can result in detrimental effects on the underlying substrate. This deficiency hinders the coating’s ability to shield the substrate from external factors, including water and heat, hence compromising its protective function. The insufficient bonding between the coating and the substrate is the primary cause for the material’s poor adherence [33]. This particular factor has the potential to induce delamination of the covering material from the substrate. In order to effectively safeguard the substrate against water and heat, it is imperative that the coating possesses a uniform and steadfast adherence [33]. The optimisation of this attribute is crucial for all formulations that have been implemented for the aim of coating.

4 Conclusions The study conducted various analyses to determine the best emulsifier for Emulsified Modified Bitumen (EMB) formulation. Based on the analyses, the EMB B formulation with the cationic emulsifier didodecyldimethyl ammonium bromide gave the best results and performance. The rheological, viscoelastic, and flash point readings of EMB B were the most accurately characterised. When compared to the standard industrial bitumen emulsion, which still exhibits some flaking even after drying, it dried at a much faster pace and exhibited superior adhesiveness capabilities with no flaking effect. However, the anionic emulsifier performed better in terms of emulsion stability because its HLB value is less than that of the cationic emulsifier, which makes it more stable. Overall, the study successfully achieved its objectives of formulating EMB using three types of emulsifiers, developing a substrate model using drywall,

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Table 7 The adhesion test results for all samples Samples

Classification Percent area removed (%) Result

EMB A

5B

0

EMB B

5B

0

EMB C

5B

0

Control sample 3B

10

Atlaskote

15

3B

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characterising raw materials and formulated EMB, conducting performance testing for the EMB coating. Acknowledgements The authors wish to express their gratitude and appreciation for the financial support from the Ministry of Higher Education (MOHE), Malaysia for the Fundamental Research Grant Scheme (FRGS KPT – RDU160129, Reference Number: FRGS/1/2016/TK02/ UMP/03/2 entitled Rheological and Structural Characterisation of Emulsified Modification Bitumen Synthesized from Industrial Wastes) and the Universiti Malaysia Pahang Al-Sultan Abdullah for the Internal Grant (RDU160324). The support from the Faculty of Chemical and Natural Resources Engineering and Universiti Malaysia Pahang Al-Sultan Abdullah, Malaysia are also acknowledged.

References 1. Chailleux E, Queffélec C, Borghol I, Farcas F, Marceau S, Bujoli B (2021) Bitumen fractionation: contribution of the individual fractions to the mechanical behavior of road binders. Constr Build Mater 271:121528. https://doi.org/10.1016/j.conbuildmat.2020.121528 2. Abdullin AI, Emelyanycheva EA (2020) Water-bitumen emulsions based on surfactants of various types. J Chem Technol Metall 55:73–80 3. Razali MN, Mohd Ramli N, Mohd Zuhan KN, Musa M, Hamid Nour A (2020) Coating and insulation effect using emulsified modification bitumen. Constr Build Mater 260:119764. https:// doi.org/10.1016/j.conbuildmat.2020.119764 4. Razali MN, Mohd Isa SNE, Md Salehan NA, Musa M, Abd Aziz MA, Nour AH, Yunus RM (2020) Formulation of emulsified modification bitumen from industrial wastes. Indones J Chem 20:96–104. https://doi.org/10.22146/ijc.40888 5. Abdel-Rahim IR, Nafady NA, Bagy MMK, Abd-Alla MH, Abd-Alkader AM (2019) Fungiinduced paint deterioration and air contamination in the Assiut University hospital, Egypt. Indoor Built Environ 28:384–400. https://doi.org/10.1177/1420326X18765256 6. Razali MN, Luqman Hakim M, Effendi M, Musa M, Yunus RM (2016) Formulation of bitumen from industrial waste. ARPN J Eng Appl Sci 11:5244–5250 7. Razali MN, Asaithamby TAP, Mohd Ramli N, Mohd Zuhan MKN, Musa M, Hamid Nour A (2021) Rheological characterization of emulsified bitumen from industrial waste. Adv Mater Res 1163:148–157. https://doi.org/10.4028/www.scientific.net/amr.1163.148 8. ASTM Standard D1640–95 (2003) Standard test method for drying, curing , or film formation of organic coatings. West Conshohocken, PA. https://doi.org/10.1520/D1640_D1640M-14R18 9. Holý M, Remišová E (2019) Analysis of influence of bitumen composition on the properties represented by empirical and viscosity test. Transp Res Procedia 40:34–41. https://doi.org/10. 1016/j.trpro.2019.07.007 10. Shafabakhsh G, Ani OJ, Mirabdolazimi SM (2021) Rehabilitation of asphalt pavement to improvement the mechanical and environmental properties of asphalt concrete by using of nano particles. J Rehabil Civ Eng 9:1–20. https://doi.org/10.22075/JRCE.2019.17407.1326 11. Monu K, Pandey GS, Singh S (2020) Performance evaluation of recycled-concrete aggregates and reclaimed-asphalt pavements for foam-mix asphalt mixes. J Mater Civ Eng 32:04020295. https://doi.org/10.1061/(asce)mt.1943-5533.0003356 12. You L, Dai Q, You Z, Zhou X, Washko S (2020) Stability and rheology of asphalt-emulsion under varying acidic and alkaline levels. J Clean Prod 256:120417. https://doi.org/10.1016/j. jclepro.2020.120417

Tensile Properties and Potential Applications of Leucaena-Silicone Biocomposite Muhammad Hamizan Hidzer , Abdul Hakim Abdullah , Wan Mohd Nazri Wan Abdul Rahman , Fazlina Ahmat Ruslan , and Jamaluddin Mahmud

Abstract The Leucaena plant possesses numerous medicinal properties and functionalities that make it highly valuable in the field of medicine. In order to harness this exceptional capability, Leucaena was incorporated into silicone rubber to create a biocomposite material. The primary objective of this study was to investigate the influence of different Leucaena fibre contents (0, 4, 8, 12, and 16 wt%) on the tensile behaviour of silicone biocomposites. Tensile tests were conducted on the silicone biocomposites, which are soft composites, in accordance to the ASTM D412 standard. Due to the nonlinear and large-deformation characteristics of the material, the silicone biocomposites were assumed to be hyperelastic, and their tensile properties were quantified using the Mooney-Rivlin hyperelastic constitutive equation. The findings show that the values of the Mooney-Rivlin material constants, C1 and C2, for the Leucaena-Silicone Biocomposite increased as the fibre content increased to 16 wt%, from 0.0423 to 0.0471 MPa for C1. The maximum elongation was seen in pure silicone, which experienced a hyperelastic stretch ratio of 13.27 before breaking. However, the stretch ratio dropped to 9.79 before fracture at 16 weight percent. Calculations revealed a 74% improvement in stiffness and a 26% drop in stretch ratio for the silicone biocomposite with 16 wt% fibre content. Thus, it can be concluded that the reinforcement of Leucaena fibre has a more pronounced effect on the stiffness rather than the elongation of silicone rubber under uniaxial tension. Lastly, the quantified properties are compared to those of other materials for benchmarking purposes and exploring potential applications. Keywords Leucaena · Silicone rubber · Biocomposite · Tensile properties · Stretch

M. H. Hidzer · A. H. Abdullah · F. A. Ruslan · J. Mahmud (B) College of Engineering, Universiti Teknologi MARA, 40450 Shah Alam, Selangor, Malaysia e-mail: [email protected] W. M. N. Wan Abdul Rahman Faculty of Applied Sciences, Universiti Teknologi MARA Pahang, 26400 Jengka, Pahang, Malaysia © The Author(s), under exclusive license to Springer Nature Singapore Pte Ltd. 2024 R. Abd. Aziz et al. (eds.), Intelligent Manufacturing and Mechatronics, Springer Proceedings in Materials 40, https://doi.org/10.1007/978-981-99-9848-7_40

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1 Introduction One of the ways to improve the properties of a material is by combining two materials, so that the superior properties from both materials could be combined. This idea has led to the emergence of improved materials, defined as composite materials. Introducing the use of natural materials in producing composite materials may lead to promoting green materials, defined as biocomposite materials or biocomposites. The idea of greener materials or biocomposites has motivated the current study to explore reinforcing natural fibers into engineering materials due to environmental concerns, Plant-based natural Fibres have emerged as a promising area in the realm of reinforced polymer composite materials. Based on Mahmud et al. [1], these fibres offer lightweight and cost-effective solutions due to their lower density, remarkable material properties, and exceptional moulding adaptability. Hence, there exists a necessity for a novel resolution to tackle this challenge. In response to this concern, environmentally friendly materials have emerged as a viable alternative to substitute synthetic fibres in the realm of polymer composites. A lot of natural fibre use in industry such as construction, automotive, aerospace, household and electrical board [2, 3]. Over the past few decades, biocomposite materials have emerged as a valuable alternative in various applications, offering significant contributions to sustainability, industrial ecology, eco-efficiency, and green chemistry [4]. Natural fibres exhibit excellent mechanical properties and have the added advantage of being lightweight. When compared to synthetic fibres, natural fibres offer numerous benefits including affordability, desirable specific strength properties, low density, and biodegradability [5]. Natural Fibres offer several advantages, including their environmentally friendly nature, complete biodegradability, non-toxic properties, and their ability to generate income for rural and agricultural communities [6]. These factors contribute to the cost-effectiveness and lightweight nature of biocomposite materials, attracting considerable attention for their further development. These materials have the potential to replace synthetic fibres with natural fibres, offering significant advantages. The white leadtree, or Leucaena Luecocephala, belongs to the Fabaceae family and is a flowering tree species. It is native to Central and South America but has been introduced and cultivated in many tropical and subtropical regions around the world [7]. Leucaena Luecocephala, one of the adaptable leguminous trees, has been identified as a possible slope plant. Additionally, L. Luecocephala has recently come to light as a viable plant for the revegetation of lagoon ash in China due to its high tolerance and survival [8]. The bark, seeds, and leaves of the tree have been used in traditional medicine for various ailments. L. Luecocephala (lmk) DeWit is one of the plants that has lately been utilised as an alternate and supplemental treatment for diabetes [9]. Forest biodiversity as a natural resource requires greater investigation to recognise its potential as a source of herbal medicine, notably for diabetes treatment [10]. In terms of composite materials, Leucaena leucocephala stem also has been used as saw dust filler in Wood Plastic Composite (WPC) mix with

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thermoplastic polymer [11]. Other works include producing commercial Leucaena composite particleboards [12]. Currently, limited studies have focused on reinforcing Leucaena with silicone, indicating a lack of comprehensive research on the mechanical properties and potential applications of Leucaena-silicone biocomposite materials. Therefore, the objective of this study is to develop a novel biocomposite material by reinforcing Leucaena with silicone rubber. The study aims to quantify, analyse, and compare the tensile properties of the Leucaena-silicone biocomposite, specifically investigating how the fibre content of Leucaena influences the stiffness and deformation characteristics of the biocomposites. Establishing these characteristics are important for exploring the suitability of Leucaena-Silicone Biocomposite as an organ substitute, in terms of materials deformation behaviour.

2 Experimental Setup 2.1 Raw Material and Matrix The Leucaena fibres were processed from the Leucaena logs, harvested from the locally planted trees in the universiti farm in Jengka, Pahang. The silicone matrix used is EcoFlex 00-30 Platinum Cure Silicone rubber, which was purchased from Castmech.

2.2 Specimen Preparation and Fabrication The preparation of Leucaena involved several steps. Firstly, the stems were trimmed to a length of approximately 10 cm, and the bark was carefully removed. Subsequently, the Leucaena stems were air-dried at room temperature and then transferred to a tray for further drying in a drying oven set at 100 °C for 24 h. To obtain a powdered form, the dried Leucaena was crushed into small chip particles using a crusher machine. It was then milled using a planetary mono mill at 300 rpm for 30 min, with this process repeated four times. The resulting material was sieved to obtain a uniform fine powder with a particle size of 100 um. For the mixing process, five specimens were prepared for each of the five different Fibre content variations (0, 4, 8, 12, and 16 wt%). This process was closely controlled, involving the precise measurement of the powder weight, the preparation of an accurate Fibre-matrix content solution, continuous stirring of the mixture, and maintenance of specific laboratory conditions. Finally, the mixture solution was poured into respective steel moulds (ASTM D412) and allowed to solidify at room temperature for approximately 4 h.

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Fig. 1 Specimen dimension in millimeter (mm) for Leucaena-silicone (ASTM 412)

2.3 Uniaxial Tensile Test The tensile test was conducted following the guidelines set forth by the American Society for Testing and Materials (ASTM) standard which is ASTM D412. The dimensions of the specimens can be seen in Fig. 1. Each specimen was tested using the Universal Testing Machine (SHIMADZU AG-IS 50kN) at a constant speed of 500 mm/min. The testing machine is equipped with a standard Crosshead and Load Cell (SHIMADZU SFL-50KNAG Code B with CAL cable) accessories with a Standard-Precision Type (1/500, ± 1%) of measurement accuracy (within ± 1% indicated test force (at 1/500 to 1/1 load cell rating).

2.4 Quantifying the Hyperelastic Behaviour Since the materials used in this study are soft and highly elastic, their deformation behaviour follows that of rubbery materials. Therefore, it is assumed that these materials would adhere to the principles of hyperelastic theory. The deformation behaviour can be represented using a hyperelastic stress-stretch relation. Hence, hyperelastic constitutive equations were employed in this study to describe the deformation behaviour of silicone rubber and Leucaena-silicone biocomposite under tensile load. In this study, the constitutive equation based on Mooney-Rivlin hyperelastic model was selected as it is one of the most commonly used hyperelastic models [13, 14]. Compared to the Neo-Hookean and Ogden models, Mooney-Rivlin model is easily applied and practical model, even though the equation is not as simple as the NeoHookean model. In terms of accuracy, Mooney-Rivlin model could provide good results in comparison to the more complicated models, such as Ogden hyperelastic model. These models are considered isotropic, incompressible, and hyperelastic, and they are expressed in terms of the engineering stress (σE)—stretch (λ) relation under uniaxial load, as shown in Eq. (1). 1 σE = λ

[( )( )] 2C2 1 2 2C1 + λ + λ λ

(1)

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Equation (1) is expressed in terms of engineering stress-stretch, (σ E − λ), relation, the engineering stress–strain, (σ E − ε), data obtained previously from the uniaxial tensile tests as mentioned in mechanical testing are converted into engineering stress– stretch, (σ E − λ) relation using Eq. (2) [15]. λ=1+ε

(2)

where λ is the stretch value and ε is the strain value (m/m). The stretch, λ, or also known as extension ratio is defined as the ratio of stretched length to unstretched length. In most published work related to hyperelasticity, the term stretch, λ, is more commonly used (rather than extension ratio) as the constitutive equations for the hyperelastic models are expressing the relationship between Engineering Stress, σE , and stretch, λ. In addition, specifically for the case of hyperelastic materials which are having large elongation values, the strain values will also be large. Therefore, plotting and explaining the large-deformation behaviour of hyperelastic materials based on engineering stress–stretch, (σE − λ) relationship would be more practical, rather than engineering stress–strain, (σE − ε) relationship which is commonly used to explain the deformation behaviour of stiffer materials (non large-deformation behaviour). The stretch, λ, or also known as extension ratio is derived from Eq. (2), where, engineering strain, ε, is the ratio of the elongation with respect to the original length. Therefore, the unit of engineering strain, ε, is m/m or unitless. Similar to engineering strain, ε, the unit of stretch, λ, is also m/m or unitless. A curve fitting procedure is performed using the engineering stress-stretch curve obtained from the experiments as a reference, aiming to find accurate matching curves by applying Eq. (1). These matching curves represent the material constant parameters that effectively describe the mechanical properties of the investigated materials. The engineering stress-stretch data sets are established based on Eq. (1), and validated data sets are utilized as input to determine the Mooney-Rivlin material constants, C1 and C2, for the silicone biocomposites. The Solver Tool in Microsoft Excel is employed to implement the curve-fitting technique and determine the values of the material constants, C1 and C2. These determined values of C1 and C2 represent the measured elastic properties that characterize the nonlinear behaviour of the new silicone biocomposites. The C1 values are then used to plot the stress-stretch curves for the Leucaena-Silicone biocomposites, enabling the determination of their tensile properties and illustrating the hyperelastic behaviour of both pure silicone and Leucaena-Silicone biocomposites.

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3 Results and Discussion The stress-stretch curves in Fig. 2 show the tensile behaviour of Leucaena-Silicone Biocomposite specimens for various fibre content compositions of 0, 4, 8, 12, and 16 wt% using the average data. The measured and quantified tensile properties corresponding to the Leucaena fibre content are presented in Table 1. The stress-stretch curves shown in Fig. 2 show the uptrend for all compositions. The pure silicone rubber specimen at 0 wt% shows the highest stretch ratio and the greatest elongation among the specimens reinforced with Leucaena fibre at 4, 8, 12, and 16 wt%. Furthermore, the uniaxial tensile force generates extremely nonlinear elastic behaviour in pure silicone specimens. Similar trend has been highlighted by Jusoh et al. [16] and Haris et al. [17], even though they used different fibre 1.1 1 0.9

Stress, σE (MPa)

0.8 0.7 0.6 0.5 0.4

0%

0.3

4%

0.2

8%

0.1

12% 16%

0 1

2

3

4

5

6

7

8

9

10

11

12

13

14

Stretch, λ Fig. 2 Non-linear large-deformation behaviour (average values and standard deviation) of Leucaena-silicone biocomposite under uniaxial tension for different wt% composition

Table 1 Tensile properties (averaged values) were obtained from the experiment for Leucaena-silicone biocomposite

Fibre weightage (%)

Material constant, C1 and C2 (MPa) C1

C2

0

0.0423

− 0.1353

4

0.0442

− 0.1339

8

0.0450

− 0.0965

12

0.0462

− 0.0649

16

0.0471

− 0.0358

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materials. This behaviour can be attributed to the continuous crosslinking of the polymer chain within the matrix, resulting in enhanced elasticity [18]. Generally, the tensile test is conducted to evaluate a material’s resistance to gradually applied uniaxial tensile loads, then are quantified through various tensile properties. Due to its higher sensitivity to deformation, the pure silicone specimen experiences more elongation while under stress, as shown by the concave tendency of the curve. In contrast, Leucaena fibre reinforced into silicone rubber it exhibits a linear curve trend when subjected to stress as its enhanced resistance to deformation under load. This study emphasizes the enhancement of the mechanical properties of silicone rubber through the incorporation of Leucaena fibre. The Mooney-Rivlin model’s material constants C1 and C2, which show that the specimen with a 16 wt% fibre content has the greatest value of 0.0471 MPa, are particularly remarkable in Table 1. These results are consistent with recent research on biocomposites made of Kenaf and Arenga Pinnata, which suggests that stiffer materials have higher material constants than pure silicone rubber. Overall findings show that as fibre content increases, the MooneyRivlin material constants C1 and C2 for the Leucaena-Silicone biocomposite rise from 0.0423 to 0.0471 MPa. These values correspond to the hyperelastic behaviour of pure silicone and Leucaena-Silicone biocomposites. The stress-stretch curves obtained using the C1 and C2 values give insight into the tensile qualities and indicate the improved stiffness of the Leucaena biocomposite over pure silicone rubber. Similar behaviour was observed by Chiulan et al. [19], who found that increasing the fibre content in silicone rubber resulted in a decreased stretch ratio when compared to a no-filler composite. The inclusion of fibre was shown to raise the stiffness of the matrix, but decrease its brittleness, explaining the decrease in ultimate stress as the fibre concentration increased in the current investigation. Chiulan et al. [19] also reported a similar trend in which adding 1% of Silica nanoparticles in silicone rubber has reduced the elongation ratio of the biocomposite compared to pure silicone. Based on Shang et al. [20], who explored a composite material comprised of silicone rubber reinforced with carbon nanotubes as a filler. The results indicated the similar pattern, with the tensile modulus increasing in tandem with the increase in fibre content. Table 2 compares the Mooney Rivlin-material constant of the Leucaena-Silicone biocomposite (present study) to comparable materials created by other researchers. The tensile stiffness of the present material is clearly between that of Connective Tissues and goat skin, showing the potential application of Leucaena-Silicone biocomposite to recreate or bio-mimic the deformation of certain tissues.

4 Conclusion This study successfully presents a new form of biocomposite material, consisting of silicone matrix reinforced with natural fibre, namely Leucaena, with the long-term aim is to produce useful and practical green materials. The study examines the effect of adding Leucaena fibre on the tensile behaviour of a silicone biocomposite. Overall, the stiffness of the soft composites is increased by the inclusion of reinforcement. It

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Table 2 Mooney-Rivlin material constants, C1 and C2 values of current study compared to other studies Material constant

Material type

References

10.1–16.1 kPa

Porcine orbital fat and connective tissue in eye (OFCT)

[21]

− 5.0 to − 2.7 kPa

3.8–7.1 kPa

Human orbital fat and connective tissue in eye (OFCT)

[21]

9.4 kPa

82 kPa

Forearm skin

[22]

17.97 kPa

11.3 kPa

Nylon + silicone (ecoflex)

[23]

42.3 to 47.1 kPa

− 135.3 to − 35.8 kPa

Leucaena-silicone biocomposite

Current study

0.14 MPa

0.023 MPa

Silicone rubber

[24]

0.3 MPa

0 MPa

Human skin

[25]

0.5 MPa

0 MPa

Silicone rubber (B452)

[25]

1.0 MPa

0.9 MPa

Silicone rubber (Sil8800) [25]

8.6240 MPa

2.9634 MPa

Acrylic elastomer

39.34 to 55.37 MPa

− 44.52 to − 61.84 MPa

Fresh goat skin unshaved [27]

C1

C2

− 11.2 to − 7.1 kPa

[26]

is interesting to note that the reinforced Leucaena fibre impacts the silicone rubber’s stiffness more than its elongation ratio when comparing the percentage increment of tensile stiffness and elongation. In addition, for benchmarking reasons and to investigate prospective applications, the quantifiable attributes are compared to those of other materials. Compared to Kenaf- and Arenga Pinnata-Silicone biocomposites, the Leucaena-Silicone biocomposites are stiffer but still lie within the range of connective tissues and skin. This finding proves that based on their deformation behaviour, the Leucaena-Silicone biocomposites has the potential to be used as a tissue or organ substitute. Other than that, Leucaena-Silicone biocomposites could also be used for cushioning applications, such as racket grips, anti-slip mats and drink coasters due to their soft and elastic characteristics.

References 1. Mahmud S, Hasan KMF, Jahid MA, Mohiuddin K, Zhang R, Zhu J (2021) Comprehensive review on plant fiber-reinforced polymeric biocomposites. J Mater Sci 56(12):7231–7264 2. Tataru G, Guibert K, Labbé M, Léger R, Rouif S, Coqueret X (2019) Modification of flax fiber fabrics by radiation grafting: application to epoxy thermosets and potentialities for siliconenatural fibers composites. Radiat Phys Chem 170(2019):108663 3. Nurazzi NM et al (2021) A review on mechanical performance of hybrid natural fiber polymer composites for structural applications. Polymers (Basel) 13(13):1–47

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4. Safri SNA, Sultan MTH, Jawaid M, Jayakrishna K (2018) Impact behaviour of hybrid composites for structural applications: a review. Compos Part B Eng 133:112–121 5. Hapuarachchi TD, Ren G, Fan M (2007) Fire retardancy of natural fibre reinforced sheet moulding compound. Appl Compos Mater 14:251–264 6. Jusoh AF, Rejab MRM, Siregar JP, Bachtiar D (2016) Natural fiber reinforced composites: a review on potential for corrugated core of sandwich structures. MATEC Web Conf 74:7–11 7. Tim TK (2012) Edible medicinal and non-medicinal plants. Springer 8. Cheung KC, Wong JPK, Zhang ZQ, Wong JWC, Wong MH (2000) Revegetation of lagoon ash using the legume species Acacia auriculiformis and Leucaena leucocephala. Environ Pollut 109(1):75–82 9. Syamsudin, Sumarny R, Simanjuntak P (2010) Antidiabetic activity of active fractions of leucaena leucocephala (lmk) dewit seeds in experiment model. Eur J Sci Res 43(3):384–391 10. Syamsudin D (2006) The effects of Leucaena leucocephala (lmk) De Wit seeds on blood sugar levels: an experimental study. Biology 2(1):49–52 11. Wan Abdul Rahman WMN, Johari NAN, Sarmin SN, Mohd Yunus NY, Japarudin Y, Mahmud J, Khairuddin MN (2020) Leucaena leucocephala: a fast-growing tree for the malaysian particleboard industry. BioResources 15(4):7433–7442 12. Sa’ad MF, Yunus NY, Rahman HA, Rahman WMNWA (2019) Leucaena particleboard: a commercial trial. Bioresources 14(2):3506–3511 13. Manan NFA, Noor SNAM, Azmi NN, Mahmud J (2015) Numerical investigation of Ogden and Mooney-Rivlin material parameters. ARPN J Eng Appl Sci 10(15):6329–6335 14. Martins PALS, Jorge RMN, Ferreira AJM (2006) A comparative study of several material models for prediction of hyperelastic properties: application to silicone-rubber and soft tissues. Strain 42(3):135–147 15. Zainal Abidin NA, Othman N, Zulkefli AH, Mahmud J (2022) Quantifying and predicting tensile properties of curcuma longa-silicone biocomposite. Medziagotyra 28(3):347–352 16. Jusoh NAI, Manssor NAS, Rajendra PN, Mahmud J (2023) The effect of reinforcing Moringa Oleifera bark fibre on the tensile and deformation behaviour of epoxy and silicone rubber composites. Pertanika J Sci Technol 31(4):895–1910 17. Haris NFN, Yahaya MA, Mahmud J (2022) Tensile properties of silicone biocomposite reinforced with waste material (Hevea brasiliensis Sawdust): experimental and numerical approach. BioResources 17(3):4623–4637 18. Abidin NAZ, Mahmud J, Manssor NAS, Abd Rahim NNC (2022) Physical and mechanical properties of bamboo-silicone biocomposites (BaSiCs). BioResources 17(3):4432–4443 19. Chiulan I, Panaitescu DM, Radu ER, Frone AN, Gabor RA, Nicolae CA, …, Chinga-Carrasco G (2020) Comprehensive characterization of silica-modified silicon rubbers. J Mech Behav Biomed Mater 101(September 2019):103427 20. Shang S, Gan L, Yuen MCW, Jiang SX, Mei Luo N (2014) Carbon nanotubes based high temperature vulcanized silicone rubber nanocomposite with excellent elasticity and electrical properties. Compos Part A Appl Sci Manuf 66:135–141 21. Kao PH, Lammers SR, Tian L, Hunter K, Stenmark KR, Shandas R, Qi HJ (2011) A microstructurally driven model for pulmonary artery tissue. J Biomech Eng 133(5) 22. Diridollou S, Patat F, Gens F, Vaillant L, Black D, Lagarde JM, …, Berson M (2000) In vivo model of the mechanical properties of the human skin under suction. Ski Res Technol 6(4):214–221 23. Guan E, Smilow S, Rafailovich M, Sokolov J (2004) Determining the mechanical properties of rat skin with digital image speckle correlation. Dermatology 208(2):112–119 24. Watton PN, Ventikos Y, Holzapfel GA (2009) Modelling the mechanical response of elastin for arterial tissue. J Biomech 42(9):1320–1325 25. Polyzois GL, Tarantili PA, Frangou MJ, Andreopoulos AG (2000) Physical properties of a silicone prosthetic elastomer stored in simulated skin secretions. J Prosthet Dent 83(5):572–577 26. Meunier L, Chagnon G, Favier D, Orgéas L, Vacher P (2008) Mechanical experimental characterisation and numerical modelling of an unfilled silicone rubber. Polym Test 27(6):765–777

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27. Kim B, Lee SB, Lee J, Cho S, Park H, Yeom S, Park SH (2012) A comparison among NeoHookean model, Mooney-Rivlin model, and Ogden model for Chloroprene rubber. Int J Precis Eng Manuf 13(5):759–764

Enhancing Water-Based Mud Properties with Sodium Lignosulfonate Polymer and Silicon Dioxide Nanoparticles: A Study on Interfacial Tension and Aging Behavior Norida Ridzuan , Chung King Ling , and Ahmad Syahmi Tajarazhar

Abstract Water-based mud (WBM) is extensively utilized as a drilling fluid because of its cost-effectiveness and eco-friendly nature. This study aims to investigate the effect of adding sodium lignosulfonate (SLS) polymer on the interfacial tension (IFT) between polymer solution and crude oil. Silicon dioxide (SiO2 ) nanoparticles and SLS polymer were used at different concentrations to evaluate their impact on WBM properties and aging behavior. Various tests were performed to evaluate the mud density, pH, rheological properties, fluid flow behavior, filtration properties, and surface tension of the WBM. From the results, the addition of 3.2 wt% SLS polymer resulted in the lowest IFT. The apparent viscosity (AV) and plastic viscosity (PV) increased with nanoparticle concentration but decreased with polymer addition. The yield point and gel strength decreased and increased with the addition of nanoparticles and polymer, respectively. A concentration of 1.6 g of SLS polymer was found to be optimal as it lowered viscosity. Nanoparticles increased filtration properties, while polymers decreased filtration properties as their concentration increased. The optimal concentration of nanoparticles in WBM was found to be 0.8 g. In conclusion, nanoparticles increased rheological and filtration properties, while the polymer decreased these properties. Keywords Water-based Mud · Nanoparticles · Sodium lignosulfonate polymer · Aging behavior

N. Ridzuan (B) · C. K. Ling · A. S. Tajarazhar Faculty of Chemical and Process Engineering Technology, Persiaran Lebuh Tun Khalil Yaakob, Universiti Malaysia Pahang Al-Sultan Abdullah, 26300 Gambang, Pahang, Malaysia e-mail: [email protected] © The Author(s), under exclusive license to Springer Nature Singapore Pte Ltd. 2024 R. Abd. Aziz et al. (eds.), Intelligent Manufacturing and Mechatronics, Springer Proceedings in Materials 40, https://doi.org/10.1007/978-981-99-9848-7_41

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1 Introduction In petroleum engineering, drilling fluid or drilling mud is a viscous fluid mixture circulated through a wellbore during drilling operations in both onshore and offshore oil and gas exploration and production. Drilling mud serves various purposes, such as cooling and lubricating the drill bit, transporting cuttings to the surface, stabilizing the wellbore, and managing formation pressure, subsurface pressure, well stability, and corrosion [1, 2]. In the selection of drilling mud, the type of formation encountered in terms of strength, porosity and permeability, temperature and pressure of the formation, ecological & environmental considerations, and cost need to be considered [3]. Drilling mud can be divided into three categories: synthetic drilling mud, drilling mud with an oil base, and drilling mud with a water base [2]. Properties such as density, rheological properties, gel strength, and filtration properties under various temperatures and pressures conditions are directly related to the effectiveness of the drilling mud. WBM is the best choice for drilling applications because they are cost-effective, ecologically friendly, and non-hazardous [4]. Various types of additives are utilized to manipulate the properties of drilling mud. These include incorporating weighting agents, viscosifiers, fluid loss control agents, emulsifiers, lubricants, corrosion inhibitors, salts, and pH control agents [5]. For example, barite, hematite, calcium carbonate, and polymers are weighting agents used for density control. Density control plays a crucial role in preventing formation damage during drilling operations. If the drilling fluid density exceeds the formation pressure, it can cause fluid invasion into the formation and leading to potential fluid losses. The normal density value for water-based drilling mud, also known as freshwater mud, typically ranges between 8.4 pounds per gallon (ppg) and 9.5 ppg. In terms of drilling mud viscosity, typical materials like bentonite, sepiolite, attapulgite, and organophilic clays are utilized to facilitate the removal of cuttings from the bottom of the borehole. These materials also enhance the mud’s ability to suspend the cuttings and weighting agents when the mud circulation is halted. The drilling mud filtrate losses through the porous to the adjacent borehole formation can be prevented by the production of a thin, impermeable filter cake by the filtration control agents. Bentonite, polymers, starches, thinners, dispersants, and deflocculants are the filtration control agents [6]. The addition of the polyacrylamide can also reduced drilling fluid loss and filter cake thickness [7]. Optimizing alkalinity and pH in WBM is accomplished using alkalinity and pH-control additives. The frequently used materials to regulate the pH of drilling mud at 8.0 to 10.5 are soda ash (Na2 CO3 ), hydroxides or sodium (NaOH), potassium (KOH), and calcium (CaOH2 ) [8]. Many drilling problems are influenced by drilling mud properties such as lost circulation, stuck pipe, shale heaving, and others. Shale inhibitors, such as polymers, nanoparticles, and inorganic salts, can be included in the drilling mud formulations to reduce the hydration and shale swelling drilling process [9]. It is known that drilling mud loss is a common issue while drilling wells. Natural cracks in the drilled rocks, induced fractures caused by drilling mud pressure exceeding the earth’s fracturing

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stress, cavernous formations, and extremely permeable formations are the factors that affect drilling mud loss from boreholes to the surrounding earth formations [10]. Therefore, polymers in WBM can moderate mud density and keep the borehole stable. Additionally, it has advantageous rheological characteristics, which mainly showed better shear thinning behavior and a suitable flow pattern [11]. Nanoparticles can be added to drilling mud to overcome drilling problems like swelling and fluid loss. Low-cost, highly effective, and environmentally friendly water-based drilling mud can be produced using silica nanoparticles additives [12]. SiO2 nanoparticles have great capability to enhance the rheological and filtration properties of polymeric WBM compared to titanium oxide nanoparticles [13]. Silica nanofluid in the drilling mud demonstrated the greatest surface tension reduction [14]. This phenomenon arises from the behavior of polymers when they interact with nanoparticles. As the polymers absorb the nanoparticles, they are subsequently driven to the fluid’s surface. The presence of additional polymer molecules at the surface enhances the reduction of surface tension (SFT) to a critical micelle concentration (CMC). CMC is a parameter used to determine the minimum amount of surfactant needed to lower the maximum SFT at which micelles can form in water [15]. Lower SFT in drilling mud helps in improving oil recovery and eliminating drilling issues like clogged pipes [14]. The problem with previous fillers added to drilling mud lies in their limited effectiveness and potential drawbacks. For example, calcium carbonate is the previous filler or additive used for drilling mud. However, it can dissolve in acid-bearing formations, leading to a loss of bridging properties. Calcium carbonate is also less effective in controlling fluid loss compared to other additives, potentially impacting wellbore stability and overall drilling performance. Nanoparticle-infused drilling mud offers excellent rheological properties, optimal filtration control, high suspension stability, good lubrication, and high anti-pollution power. The rate of heat transfer between the drilling mud and drill bit can increase with the addition of nanoparticles because the specific surface area of the drilling mud molecules increases [16]. From an environmental aspect, nanoparticles in drilling mud are better than conventional additives because nanoparticles are usually added in small quantities and low concentrations [17]. This research’s goal is to determine the effect of the addition of SLS polymer on the interfacial tension between polymer solution and crude oil and to investigate the effect of the addition of silicon dioxide (SiO2 ) nanoparticles and sodium lignosulfonate (SLS) polymer on the properties and ageing behavior of the water-based drilling mud.

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2 Materials and Methods 2.1 Preparation of Water-Based Drilling Mud (WBM) Basic WBM was prepared by first adding 18 g of bentonite powder in 350 mL of fresh water into the mud mixer. The container was placed on the blender, and the stirrer was turned on. While stirring, the bentonite was gradually added to the mixture until fully combined, which took approximately 15 min. Next, 0.05 g of soda ash powder and 5 mL of 0.1 M sodium hydroxide solution were added, and the mixture was stirred again. To achieve density control, 5 g of barite, serving as a weighting agent, was introduced into the mud and thoroughly stirred until complete mixing or dissolution occurred. For basic WBM containing polymers or nanoparticles, the same amount of SLS polymer and SiO2 nanoparticles (0.00, 0.2, 0.4, 0.8, and 1.6 g) were used. These components were added to the basic WBM and mixed for 15 min to achieve a uniform mixture. To create nano WBM with polymers, 0.8 g of SiO2 nanoparticles and varying amounts of SLS polymer (0.2, 0.4, 0.8, and 1.6 g) were added to the mixture and stirred using the mud mixer.

2.2 Characterization of the Drilling Mud 2.2.1

Interfacial Tension (IFT) Between Polymer Solution and Crude Oil

The interfacial tension between the two phases was measured using a Du-Noüy ring RG 11. A solution of the SLS polymer was mixed with 50 mL of distilled water. The liquid was then added to a sample vessel in two stages, with the heavier polymer solution added first, followed by the lighter crude oil.

2.2.2

Mud Density and pH Measurement

A mud balance was used to calculate the mud’s density. When the bubble is below the centerline, the density at the rider’s edge towards the mud cup was measured. The pH of the drilling mud was determined using a pH meter.

2.2.3

Rheological Properties

A Fann viscometer was used to test the rheological properties of drilling mud. The rotational rates used to test viscosity were 3, 6, 100, 200, 300, and 600 rpm. The relationships below can be used to calculate the plastic viscosity (µp ), apparent

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viscosity (µa ), and yield point (Yb ): Plastic Viscosity (cP), µp = (600 rpm reading) − (300 rpm reading)

(1)

Apparent Viscosity (cP), µa = (600 rpm reading)/2

(2)

) ( Yield Point lb/100ft2 , Yb = (300 rpm reading) − µp

(3)

The 10 s and 10 min gel strength were measured by stirring the mud for 10 s at high speed. Then, the mud was allowed to stand undisturbed for 10 s and 10 min and the highest reading obtained after starting rotation at 3 rpm was recorded as 10 s gel and 10 min gel strength respectively.

2.2.4

Fluid Flow Behavior

The flow behavior was determined at room temperature of 24 °C with a logarithmic shear rate ramp from 0.1 to 100 s−1 to obtain a viscosity curve by using MCR 72 rheometer.

2.2.5

Filtration Properties

To measure the filtration properties of the drilling mud, a mud filter press was employed. After subjecting the press to a pressure of 100 psi for 30 min, the volume of the resulting filtrate was measured using a graduated cylinder and reported in milliliters as the API filtrate. The thickness of the filter cake on the filter paper was then determined using a Vernier caliper, with the measurement being taken to the nearest 1/32 inch.

2.2.6

Surface Tension Measurement

The drilling mud surface tension was measured using a Du-Noüy ring RG 11 method (DCAT) according to DIN 53,914.

2.2.7

Ageing Effect

The aging cell was put into the rotating oven and the aging cell was heated up to 200 °C for 24 h. The properties of the drilling mud were tested after the ageing effect.

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3 Results and Discussion 3.1 Effect of Polymer Concentration on the Interfacial Tension (IFT) Between Crude Oil and Water Figure 1 shows the effect of SLS polymer concentration on the IFT between polymer solution and crude oil. The IFT decreases with the addition of polymer concentration. The initial IFT between polymer solution and crude oil is 17.57 mN/m, which falls most significantly when reaching 0.4 wt% of SLS to become 4.33 mN/m. The IFT reduction gradually reached 0.93 mN/m with an increase in SLS concentration of 3.2 wt%. The polymer molecule gradually becomes denser toward the polar substance when the polymer concentration is added. The hydrophilic part and hydrophobic part will be absorbed in the interfacial surface between water and oil which causes a reduction in the IFT. The monomer starts to combine and form micelles once the polymer concentration approaches CMC. As concentration increases after CMC, micelle concentration increases without significantly raising monomer concentration [18]. Reduction in IFT will result in easy removal of oil residue on the wellbore surface [19]. As the force of attraction between the molecules at the interface between polymer solution and crude oil drops, IFT values fall, indicating an increase in oil recovery [20].

Interfacial tension (mN/m)

18

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16 14 12 10 8 6

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3.2 Effect of Nanoparticles and SLS Polymer on the Mud Density in WBM The mud density is important in controlling wellbore stability and formation pressure. Figure 2 below shows the effect of nanoparticles and SLS polymer on the mud density in WBM. Drilling mud densities were taken before ageing (BA) and after ageing (AA) effect with the addition of SiO2 nanoparticles and SLS polymer. From the results, the mud density remains constant at 8.7 ppg when an amount of 0.2, 0.4, and 0.8 g of SLS polymer is added to basic WBM. The mud density before and after ageing remains almost unchanged with an average of 8.7 ppg when amounts of 0.2, 0.4, 0.8, and 1.6 g of SiO2 nanoparticles are added to the drilling mud respectively. According to the data obtained with the addition of polymer in nano WBM before the ageing effect, the significant change in mud density occurs when the amount of polymer is increased from 0.8 to 1.6 g, resulting in a reduction of 2.75% from 8.7 to 8.46 ppg. This is because it has inherently lower densities compared to the other components of drilling mud. When these lower-density polymers are added, they contribute to reducing the overall density of the drilling mud. The mud density from 0.2 to 0.8 g of polymer in nano WBM remains constant at 8.7 ppg. Overall results before and after ageing showed that adding polymer to nano WBM had no significant impact on mud density. By comparing the effect of nanoparticles and the polymers WBM before the ageing effect, there is little or no effect on the overall performance of the mud density when adding nanoparticles and polymers. In the formulation of WBM, the weighting agent of WBM is barite. Drilling efficiency also depends on the mud density because a lower mud density will cause a higher penetration rate or drill rate. In contrast, a higher mud density will prevent any formation of fluid enter the wellbore.

Mud density (ppg)

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0.4

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Concentration (g) Basic WBM (BA) Polymer (BA) Nanoparticles (BA)

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Fig. 2 Effect of nanoparticles and polymers concentration on the mud density

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3.3 Effect of Nanoparticles and Polymer on the pH in WBM The results of the pH values of the different amounts of nanoparticles and polymer added to the WBM are presented in Fig. 3. The pH values show a slight decline from 0.4 to 1.6 g of polymer in WBM. The pH values slightly decrease from a concentration of 0.2 g nanoparticles to 0.8 g nanoparticles before ageing. Then, the pH value increases by 0.68% at a concentration of 1.6 g of nanoparticles before ageing. After ageing, 0.2 g, 0.4 g, 0.8 g, and 1.6 g of nanoparticles have pH values of 9.07, 9.08, 8.78, and 8.85, respectively. The data obtained for the pH of the different concentrations of polymer in nano WBM is shown in Fig. 3. From 0.2 to 1.6 g of polymer, the pH value before and after ageing shows a slight reduction. The pH value from 0.2 to 1.6 g of polymer before ageing decreases from 9.89 to 9.76 respectively while the pH value from 0.2 to 1.6 g of the polymer in nano WBM after ageing decreases from 7.90 to 7.11 respectively. It implies that the pH will decrease due to the addition of a polymer in nano WBM because polymer interactions with water which cause a reduction in the concentration of free hydrogen ions in the solution, resulting in a decrease in pH. By comparison, a decrease in pH value by adding nanoparticles and polymers from a concentration of 0.2 to 0.8 g was observed. It was seen that all pH values measured both before and after ageing are alkaline which is higher than pH 7.0 (neutral). pH control is crucial in preventing corrosion of drilling equipment and casing pipes. High pH (alkaline) conditions can lead to corrosion, while low pH (acidic) conditions can cause acidic corrosion. By maintaining the appropriate pH range of the drilling mud, typically slightly alkaline between 8.0 to 10.5, corrosion of metal surfaces in contact with the drilling mud can be minimized, extending the lifespan of equipment, and ensuring well integrity. Therefore, maintaining the pH of the drilling mud within a defined standard range can prevent the corrosion of materials and equipment. From the overall results, it can deduce that the lowest pH 11

pH

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0.4

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Concentration (g) Basic WBM (BA) Polymer (BA) Nanoparticles (BA)

Basic WBM (AA) Polymer (AA) Nanoparticles (AA)

Fig. 3 Effect of nanoparticles and SLS polymers concentration on the pH

1.6

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obtained is with the addition of 0.8 g of nanoparticles, which indicates that 0.8 g of nanoparticles is the optimal concentration used compared to others.

3.4 Effect of Nanoparticles and SLS Polymer on the Rheological Properties in WBM 3.4.1

Apparent Viscosity (AV)

Figure 4 shows the effect of nanoparticles and polymers on the apparent viscosity in WBM. When the effects of nanoparticles and polymer are compared, apparent viscosity increases with the addition of nanoparticles to WBM while AV value decline with the addition of polymer in WBM and in nano WBM. The AV rises with the nanoparticle concentration because the nanoparticles have a high surface area and a small volume, which enhances the contact between the nanoparticles and the surface of bentonite connected by chemical bonds[20]. The AV value with polymer addition in nano-WBM is lower than the AV in WBM with nanoparticles only. This indicates that the AV of WBM can be reduced by adding polymers. The AV after ageing is greater than the AV before ageing because of the increased temperature-induced aggregation and flocculation of the clay platelets as well as the dehydration of the clay platelets, which increases the viscosity of the drilling mud.

Apparent viscosity (cP)

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Concentration (g) Basic WBM (BA) Polymer (BA) Nanoparticles (BA)

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Fig. 4 Effect of nanoparticles and polymers concentration on the AV

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Plastic viscosity (cP)

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0

0

0.2

0.4

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1.6

Concentration (g) Basic WBM (BA) Polymer (BA)

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Fig. 5 Effect of nanoparticles and polymers concentration on the PV

3.4.2

Plastic Viscosity (PV)

Figure 5 shows the trend of plastic viscosity for drilling mud when the different amount of nanoparticles and polymer was added. If compared to the effect of nanoparticles and polymer before ageing, PV increases with the concentration of nanoparticles while PV decreases with the polymer concentration. The drill string will be more vulnerable to differential pipe sticking because of the increase in viscosity brought on by the rise in solid content [21]. From the results before ageing in Fig. 5, the PV obtained with polymer addition is half of the PV with nanoparticles addition. Nanoparticles had induced a thickening behaviour and the polymer acted as thinners in WBM. The optimal PV value in drilling is said to be the lowest since the mud can drill quickly due to its low viscosity.

3.4.3

Yield Point (YP)

The yield point (YP) is the ability of the drilling mud to carry out the produced cuttings during the drilling process. The effect of nanoparticles and polymer concentration on yield point is shown in Fig. 6. Before ageing, the YP from 0.2 to 0.8 g of nanoparticles decreases from 5.67 lb/100 ft2 to 4.1 lb/100 ft2 respectively. The degradation of YP before ageing could be attributed to the agglomeration of SiO2 nanoparticles on clay plates present in bentonite, which decreased the mud’s total electrostatic potential [21]. When nanoparticles are added to WBM, the YP value increases more than when the polymer is added. Comparing nanoparticles with polymers, it can be seen that the presence of polymers has a lower YP value than the WBM without the addition of polymer. So, nano WBM can carry cuttings without the addition of polymer because of the stronger attraction interactions between active clay particles in the mud under flowing circumstances.

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Yield point (lb/100ft2)

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Concentration (g) Basic WBM (BA) Polymer (BA)

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Fig. 6 Effect of nanoparticles and polymers concentration on the yield point

3.4.4

Gel Strength

Gel strength is defined as the smallest shearing stress needed to initiate a slipwise movement of fluid under static conditions. Gel strength is responsible for the removal of drilling products by suspending drilling fluid components and cuttings [22]. The effect of nanoparticles and polymer concentrations on gel strength at 10 s and 10 min is shown in Fig. 7. From both graphs of 10 s and 10 min gel strength, the values obtained before ageing slightly decrease as the amount of nanoparticles added increases because it is deflocculation in nature. On the contrary, the gel strength for 10 s and 10 min after ageing tends to increase as the concentration of nanoparticles increases. For the formulations of polymer in nano WBM, the gel strength for 10 s before and after the ageing effect shows small changes or is unaffected as polymer concentration increases. On the other hand, the gel strength for 10 min before and after the ageing effect increases as the amount of polymer added increases. The concentration range of 0.8 to 1.6 g of SLS polymer exhibits the largest improvement in gel strength, suggesting better-cutting suspension. Compared to adding nanoparticles and polymer before hot rolling and ageing, the gel strength for 10 s is almost the same at the same concentration of nanoparticles and polymer. From Fig. 7b, the gel strength for 10 min with the addition of nanoparticles is much higher than with the addition of polymers. To summarize, nanoparticles can be used to control the gel strength of the drilling mud.

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Fig. 7 Effect of nanoparticles and polymer concentration on the gel strength at a 10 s; b 10 min

3.5 Effect of Nanoparticles and Polymer on the Fluid Flow Behavior in WBM Figure 8 depicts the variation profile of the shear rate-viscosity of the different drilling muds with the addition of nanoparticles and polymer in WBM before the ageing effect. From the results, the viscosity shows a reduction as the shear rate increases which indicates that the drilling mud exhibits shear thinning or pseudoplastic flow behaviour. The shear forces applied during higher shear rates disrupt the network structures formed by the nanoparticles within the fluid. These networks, formed due to particle interactions and entanglements, contribute to the higher viscosity

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observed at lower shear rates. As the networks are disrupted, the flow resistance decreases, leading to a reduction in viscosity. For addition of polymer in WBM, the long polymer chains within the fluid tend to align themselves in the direction of the shear flow when shear forces are applied. As the shear rate increases, this alignment becomes more pronounced. The aligned chains create a more streamlined flow, reducing the resistance to flow and resulting in lower viscosity.

Fig. 8 Effect of nanoparticles and polymer concentration on the fluid flow behaviour before ageing effect. a WBM with nanoparticles; b WBM with nanoparticles and polymer

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3.6 Effect of Nanoparticles and SLS Polymer on the Filtration Properties in WBM 3.6.1

Fluid Loss

The volume of drilling formulation base fluid that is injected into the formation as a result of the pressure differential between the hydrostatic and formation pressures is known as the filtrate loss. Figure 9 shows the effect of nanoparticles and polymer concentration on the filtrate loss in WBM before and after the ageing effect. It has been shown that increasing the number of nanoparticles causes the filtration volume to decrease, which results in the filter cake’s permeability reducing as the amount of solids increases. The filtrate loss was increased when the polymer concentration increased in nano WBM. The highest fluid loss obtained before ageing is at a concentration of 1.6 g of SLS polymer which is 34.67 mL in 30 min. Similarly, the fluid loss at a concentration of 1.6 g of SLS polymer after ageing was increased by 40.26% compared to 0.2 g of SLS polymer. From the overall results of the filtrate loss before ageing, the fluid loss was increased with adding polymer in WBM while filtrate loss decreased with adding nanoparticles in WBM. So, nanoparticles has improved the filtration characteristics which can reduce the volume of drilling mud invaded into the formation [23]. SiO2 nanoparticles can be known as a filtrate reducer, which improved the stability of the WBM colloidal system [24].

Fluid loss (mL/30 min)

50 40 30 20 10 0 0

0.2

0.4

0.8

Concentration (g) Basic WBM (BA) Polymer (BA)

Basic WBM (AA) Polymer (AA)

Fig. 9 Effect of nanoparticles and polymers concentration on the fluid loss

1.6

Mud cake thickness (1/32 inch)

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30

20

10

0

0

0.2

0.4

0.8

1.6

Concentration (g) Basic WBM (BA) Polymer (BA)

Basic WBM (AA) Polymer (AA)

Fig. 10 Effect of nanoparticles and polymers concentration on the mud cake thickness

3.6.2

Mud Cake Thickness

A layer made up of solid drilling mud particles that have been deposited due to the pressure difference between the wellbore and formation pressure is known as a mud filter cake. Figure 10 illustrates the effect of nanoparticles and polymer on WBM mud cake thickness before and after the ageing effect. Before ageing, the mud cake thickness is 0.122, 0.14, 0.103, and 0.125 inches for concentrations of 0.2, 0.4, 0.8, and 1.6 g of nanoparticles, respectively. As the concentration of nanoparticles increases up to 1.6 g, the mud filter cake thickness increases from 0.117 to 0.166 inch after ageing. However, before and after ageing, the mud cake thickness increases with increasing polymer concentration in nano WBM. It shows an increment of 65.15% from the concentration of 0.2–1.6 g of polymer. From the overall results in Fig. 10, the mud filter cake thickness increases when the concentration of polymer increases while the mud filter cake thickness decreases with the addition of nanoparticles in WBM. Filtrate loss is related to the mud cake thickness, which depends on the filter cake permeability. Compared to Figs. 9 and 10, the addition of 0.8 g of nanoparticles has only 18.67 mL of filtrate loss with a mud cake thickness of 0.103 inch, which is lower than others. It is concluded that 0.8 g of nanoparticles is the optimal concentration added to WBM.

3.7 Effect of Nanoparticles and Polymer on the Surface Tension in WBM Figure 11 shows the surface tension of different concentrations of nanoparticles and polymers in WBM. There was a reduction in SFT when nanoparticles or polymers were added to the WBM. At nanoparticle concentrations ranging from 0.2 g to

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Surface tension (mN/m)

100 80 60 40 20 0 0

0.2

0.4

0.8

1.6

Concentration (g) Basic WBM (BA) Polymer (AA)

Basic WBM (AA) Nanoparticles (BA)

Polymer (BA) Nanoparticles (AA)

Fig. 11 Effect of nanoparticles and polymers concentration on the surface tension

1.6 g, the SFT before ageing decreases from 76.1 to 67.13 mN/m. When 1.6 g of nanoparticles were added, the SFT decreased by 4.45% after the ageing effect. When combined with the polymer in nano WBM, the SFT shows significant reductions, with a 23.05% reduction before and a 15.17% reduction after ageing. Since the SLS polymer is also a surfactant, it triggers a behavioural mechanism of nanoparticle absorption with surfactants; as the surfactants begin to absorb the nanoparticles, they are effectively pushed to the fluid’s surface, where there is a bigger reduction in SFT when there are more surfactant molecules present [14]. As the results indicated, both nanoparticles and polymers will decrease the SFT when concentration increases. As the polymer is added to the nano WBM, the SFT is lower than the WBM without the addition of the polymer. Oil recovery is improved and drilling issues like stuck pipes are reduced when the surface tension in the drilling mud is lower.

4 Conclusion The SiO2 and SLS polymer have a significant effect on the properties of the drilling mud. The addition of nanoparticles into WBM can enhance the properties of drilling mud because the rheological properties and filtration properties were all improved with an increment in the contents of nanoparticles. By adding nanoparticles into the drilling mud, wellbore instability, excessive filtrate volume, pipe sticking, and shale swelling issues might be avoided. On the other hand, the filtration properties, AV, and PV demonstrate a reverse relationship with the added amount of SLS polymer which indicates the SLS polymer can be used as a mud thinner. Among all the drilling mud properties listed above, the optimal concentration of nanoparticles added to WBM is 0.8 g because it has a lower mud filter cake thickness and a lower pH value.

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The limitation of this study is that different drilling conditions, such as temperature, well depth, and lithology, may not have been thoroughly investigated. In conclusion, the current research builds upon previous knowledge and provides more detailed insights into the advantageous effects of nanoparticles in WBM. It establishes a stronger correlation between nanoparticle content and mud performance, leading to potential solutions for addressing drilling challenges and optimizing the efficiency of the drilling process. Acknowledgements Sincere appreciation to all the Faculty of Chemical and Process Engineering Technology (FTKKP) laboratory staff for their advice, training, and knowledge during the research project. Conflicts of Interest The authors declare no conflict of interest. Funding The successful completion of this research project was made possible by the financial support received from the Ministry of Education (MOE), Malaysia, through the Fundamental Research Grant Scheme (RDU 1901060, reference number FRGS/1/2018/TK02/UMP/03/1) and Fundamental Research Grant from Universiti Malaysia Pahang Al-Sultan Abdullah (RDU230034). The authors express their gratitude for this funding assistance.

References 1. Mohamed S, Salehi S, Ahmed R (2021) Significance and complications of drilling fluid rheology in geothermal drilling: a review. Geothermics 93:102066 2. Hamoodi A, Rahimy AA, Khalid AW (2018) The effect of proper selection of drilling fluid on drilling operation in Janbour Field. Am Sci Res J Eng 39(1):224–234 [Online] 3. Ahmed AW, Kalkan E (2019) Drilling fluids; types, formation choice and environmental impact. Int J Latest Technol Eng 8(12):66–71 4. Parate NB, Studies E (2021) A review article on drilling fluids, types, properties and criterion for selection. J Emerg Technol Innovat Res 8(9):463–484 5. Jacob NCG, Frank O, Ebube OF, Hezekiah-Braye O (2021) Effect of microbes on drilling fluid formulation. Int J Adv Eng Res Sci 8(5):491–498 6. Karakosta K, Mitropoulos AC, Kyzas GZ (2021) A review in nanopolymers for drilling fluids applications. J Mol Struct 1227:129702 7. Roodbari P, Sabbaghi S (2021) Investigating the properties of modified drilling mud with barite/ polyacrylamide nanocomposite. SPE Drill Complet 36(4) 8. Otitigbe FE (2021) Evaluation of pH of drilling fluid produced from local clay and additives. J Appl Sci Environ Manag 25(4):561–566 9. Solling T, Kamal M, Hussain S (2021) Surfactants in upstream E&P. Springer Nature, Switzerland 10. Liang T et al (2017) Formation damage due to drilling and fracturing fluids and its solution for tight naturally fractured sandstone reservoirs. Geofluids 2017 11. Qi L (2014) The application of polymer mud system in drilling engineering. Procedia Eng 73:230–236 12. Hamad BA, Xu M, Liu W (2021) Performance of environmentally friendly silica nanoparticlesenhanced drilling mud from sugarcane bagasse. Part Sci Technol 39(2):168–179 13. Esfandyari A, Harati S, Kolivandi H (2021) Colloids and surfaces a : Physicochemical and engineering aspects evaluation of rheological and filtration properties of a polymeric waterbased drilling mud in presence of nano additives at various temperatures. Colloids Surfaces A Physicochem Eng Asp 627:127128

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14. Abang GN, Pin YS, Ridzuan N (2021) Application of silica (SiO2 ) nanofluid and Gemini surfactants to improve the viscous behavior and surface tension of water-based drilling fluids. Egypt J Pet 30(4):37–42 15. Ramesh M, Sakthishobana K (2021) Significance of biosurfactants in oil recovery and bioremediation of crude oil. Green Sustain. Process Chem Environ 211–226. 16. Farahbod F (2021) Experimental investigation of thermo-physical properties of drilling fluid integrated with nanoparticles: Improvement of drilling operation performance. Powder Technol 211–226 17. Paydar P, Ahmadi M (2017) Characteristics of water-based drilling mud containing Gilsonite with Boehmite nanoparticles. Bull la Société R des Sci Liège 86:248–258 18. Alpandi AH, Inasyah FA, Sidek A, Husin H, Junin R, Jaafar MZ (2021) Critical micelle concentration, interfacial tension and wettability alteration study on the surface of paraffin oil-wet sandstone using saponin. IOP Conf Ser Mater Sci Eng 1153(1) 19. Paz M, Mba E (2016) Flexible transparent conductor film using graphene-carbon nanotubes. Universiti Teknolgy Petronas, Thesis 20. Imuetinyan H, Agi A, Gbadamosi A, Junin R, Oseh J (2022) Oil-water interfacial tension, wettability alteration and foaming studies of natural surfactant extracted from Vernonia Amygdalina. Pet Res 7(3):350–356 21. Al-Zubaidi NS, Alwasiti AA, Mahmood D (2017) A comparison of nano bentonite and some nano chemical additives to improve drilling fluid using local clay and commercial bentonites. Egypt J Pet 26(3):811–818 22. Medhi S, Chowdhury S, Gupta DK, Mazumdar A (2020) An investigation on the effects of silica and copper oxide nanoparticles on rheological and fluid loss property of drilling fluids. J Pet Explor Prod Technol 10(1):91–101 23. Anter ES, Sayed GH, Abdou MI, Abdel-Rahman NR, Ahmed HE, Negm NA (2020) Preparation and evaluation of nonionic polyurethane polymers in improving the rheological properties and filtrate loss control of water base muds. Egypt J Chem 63(11):4273–4283 24. Cheraghian G (2021) Nanoparticles in drilling fluid: a review of the state-of-the-art. J Mater Res Technol 13:737–753

Effect of Heat Treatment on Hardness and Microstructure of Titanium Alloy (Ti6Al4V) via Laser Powder Bed Fusion (LPBF) Farhana Mohd Foudzi , Abu Bakar Sulong , Norhamidi Muhamad , Nabilah Afiqah Mohd Radzuan , Intan Fadhlina Mohamed , Fathin Iliana Jamhari , Minhalina Ahmad Buhairi , Ngoi Hui Lin, Lai Yu Hung, Chun Chuan Chia, and Kim Seah Tan

Abstract Laser powder bed fusion (LPBF) is one of additive manufacturing (AM) processes which emits high power lasers on powder coatings to produce 3D end products. The combination of main processing parameters such as laser power, velocity scanning, hatching distance and layer thickness resulted to volumetric energy density (VED) which influence the performance of 3D products. For metals, residual stresses are often caused by repeated fusion and solidification of molten metal on each printed layer which may reduce the performance of 3D end products if not eliminated. Heat treatment is often employed to overcome such issue. In this work, the effect of heat treatment on the hardness and microstructure of titanium alloy (Ti6Al4V) printed

F. Mohd Foudzi (B) · A. B. Sulong · N. Muhamad · N. A. Mohd Radzuan · I. F. Mohamed · F. I. Jamhari · M. Ahmad Buhairi Advanced Manufacturing Research Group, Universiti Kebangsaan Malaysia, 43600 Bangi, Selangor, Malaysia e-mail: [email protected] Department of Mechanical and Manufacturing Engineering, Faculty of Engineering and Built Environment, Universiti Kebangsaan Malaysia, 43600 Bangi, Selangor, Malaysia N. H. Lin NXP Malaysia Sdn Bhd, 2, Jalan SS 8/2, Sungai Way Free Trade Industrial Zone, 47300 Petaling Jaya, Selangor, Malaysia L. Y. Hung Engineering Department, Sime Darby Oils, 2, Jalan PJU 1A/7, 47301 Ara DamansaraPetaling Jaya, Selangor, Malaysia C. C. Chia Greatech Integration (M) Sdn Bhd, Plot 287, Lengkok Kampung Jawa 1, Bayan Lepas Free Industrial Zone Phase 3, 11900 Bayan Lepas, Pulau Pinang, Malaysia K. S. Tan Oryx Advanced Materials Sdn Bhd, Plot 69(d) & (E), Lintang Bayan Lepas 6, Bayan Lepas Industrial Zone, Phase 4, 11900 Bayan Lepas, Penang, Malaysia © The Author(s), under exclusive license to Springer Nature Singapore Pte Ltd. 2024 R. Abd. Aziz et al. (eds.), Intelligent Manufacturing and Mechatronics, Springer Proceedings in Materials 40, https://doi.org/10.1007/978-981-99-9848-7_42

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via the LPBF process was investigated. It was found that at high VED, the hardness was reduced by 20% from 417.35HV (untreated) to 333.37HV (heat-treated). Microstructure analysis shows that phase changes from α (untreated) to α + β phase after the heat treatment. Such combination of phases improves the product’s stiffness. The findings from this study can be applied to other Ti6Al4V products such as automotive and medical implants where suitable performance is achievable. Keywords Titanium alloy Ti6Al4V · Laser powder bed fusion · Hardness · Microstructure

1 Introduction Among AM manufacturing methods, laser bed powder fusion (LPBF) has attracted the most attention due to its ability to print metal 3D objects. LPBF offers lasers to produce complex 3D objects, layer-by-layer construction of molten metals [1]. Among the factors that influence the production of AM, the volumetric energy density (VED), which directly affects the nature of the parts being built, is a major factor in the selective laser dilution process (SLM). VED (J/mm3 ) is defined in the equation, where P is laser power (W), V is the scan speed (mm/s), h is the hatching distance (μm), and t is the thickness of the layer (μm) [2]. In addition, AM contributes to less scrap compare with other conventional manufacturing methods such as injection molding and casting [3]. ( V ED

J mm3

) =

V

( mm ) s

P(W ) × h(μm) × t(μm)

(1)

The material used in this study is titanium alloy (Ti6Al4V). Ti6Al4V is a metal alloy which has two phases with high corrosion resistance, high bio compatibility and high strength. These properties give the ability to be used in various fields such as aerospace, chemical, marine, automotive and biomedical [4]. One of the most successful Ti6Al4V applications is the biological interaction between implants and bones. This application has a combination of mechanical, topological, physical and chemical properties. This is why Ti6Al4V has been widely used in the orthopaedic field due to its high strength:mass ratio, good bio-compatibility, superior corrosion resistance and lower elastic modulus compared to stainless steel and cobalt alloys [5]. Titanium alloys, Ti6Al4V have several phases such as α and β phase, which means it has a higher strength than the durable steel alloy and revealed a greater processing option. At low to moderate temperatures, Ti6Al4V has low density and good strength, making it popular in the aerospace, automotive, and medical industries applications [6]. If the cooling rate from the heated temperature to room temperature is fast enough, α + β alloy converts martensitically. The manufacture of SLM Ti6Al4V

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has an acicular dominated martensite microstructure, which produces high strength and low ductility [7]. Due to the microstructure of martensites, high-density SLM components usually have high yield strength but limited ductility. According to a study, balling phenomena can be eliminated by reducing scanning speed or increasing laser power, both intrinsically resulting in increased VED in Ti6Al4V materials [8]. Laser energy is absorbed by the first layer of powder, leading to powder dilution. The liquid phase volume is mainly dependent on VED during a single linear laser scanning, and smaller amounts of liquid phase are usually produced from lower VED. According to a study from [9] when the VED is very low, weak metallurgical bonding between the laser adjacent to the track or the liquid layer will result in relatively low density. On the other hand, if the VED is very high, the evaporation of the powder will also reduce the relative density. Therefore, relatively high relative density fails to obtain when the VED is too low or too high. The tensile strength and compression in an object are applied during heating or cooling work where the residual stress will be generated at the time of LPBF printing. Residual stress is important in the strength and ability of objects, especially 3D component for required applications [10]. Among the processing parameters, scanning speed and laser power are important for determining the residual stresses to be generated in 3D printing products. The deviations are laser power, scanning speed, layer height and hatching distance [11]. Other research shows that layer thickness is the most significant parameter affecting the density of the finished parts [12]. Heat treatment has been used in reducing residual stress in metal AM, improving machine ability, welding, structural stability, fracture resistance and temperature strength [13] Manipulation in mechanical properties is achieved by heating the metal to a phase transition temperature. Referring to a study [14] with heat processing temperatures rising above transus temperatures, acicular martensite temperature will be achieved. According to [15], heat treatment will make the martensite structure fine transformed into a mixture of α and β, where the phase is present as a fine needle line. This study has received similar results to the study [13] with the facts in the α and β phases, there is more phase volume, in the β structure during water quenching. Microhardness determines the range of light loads using a diamond curve to create a curve that is measured and converted to the hardness value of the annealed Ti6Al4V substrate enhances mechanical properties. Heat treated samples provide a statistically more stable modulus value. The micro-structure of lamellar (α + β) evenly distributed when a low cooling rate is used following heat treatment under β transus. This increases the hardness through the effect of strengthening the vanadium solid solution. The microstructure provides the information used to determine whether the structural parameters are within a specific specification. Analytical results are used as acceptance or rejection criteria. According to the study [16] during heat treatment conditions, residual stress is reduced and potentially eliminated where phase transitions α' to α + β present when they are at 600 °C. When the samples are subjected to a heat treatment at 800 °C, the Ti6Al4V alloy microstructure shows that the phase is α + α' . The α-phase with dislocation plate leads to its result in a prolonged decline. Moreover, this indicates that the martensite transition temperature can drop to below 800 °C.

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2 Methodology In this work, titanium alloy (Ti6Al4V) Grade 23 powder with a chemical composition of 90% titanium, 6% aluminium, 4% vanadium, 0.25% iron and 0.2% oxygen was used. The particle size range of the Ti6Al4V powder is 21.69–48.84 μm with a median size of 32.70 μm. Based on SEM, it was observed that the particles are in spherical shape with a less smooth surface, as shown in Fig. 1. The printing process was conducted using a RenAM 500E (Renishaw) 3D printer which comes with a smart gas flow control, kinematic repeater and built-in camera. Table 1 shows the processing parameter (printing parameters) were constructed based on the default processing parameters for Ti6Al4V in LPBF. The default processing parameters is denoted as P2 (69.44 J/mm3 ). To investigate the effect of heat treatment on the hardness and microstructure, the VED was varied for all samples. Lower and higher VED were chosen as P1 (51.28 J/mm3 ) and P3 (90.91 J/mm3 ), respectively. Heat treatment is a post-process that can improve the performance, mainly mechanical properties of 3D products. During heat treatment, the stored residual stress will be released. In this work, annealing was chosen as the heat treatment. Figure 2 shows the heating profile of such heat treatment used in this work [17]. Figure 3a shows printed Ti6Al4V sample, Fig. 3b dimension and building orientation and Fig. 3c top view of upskin. Cubic design with 0° of building direction was Fig. 1 Micrograph of Ti6Al4V powder articles

Table 1 Processing parameters Sample

Laser power (W)

Layer height (μm)

Scan speed (mm/s)

Hatch distance (μm)

Volumetric energy density (J/mm3 )

P1

200

0.4

1500

0.65

51.28

P2

200

0.4

1200

0.60

69.44

P3

200

0.4

1000

0.55

90.91

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Fig. 2 Heating profile for the heat treatment (annealing) on as-built Ti6Al4V samples

chosen due to its isotropic properties. That means the hardness and microstructure are almost similar regardless which skin (upskin or core skin).

Fig. 3 Ti6Al4V cubic samples a printed sample, b dimension and building orientation, c top view (upskin) of sample

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3 Results and Discussion Hardness and microstructure were compared before and after heat treatment. The comparison was conducted only on the upskin due to its isotropic properties. Take note that A and HT stands for as-built (untreated samples) and heat-treated samples, respectively.

3.1 Effect of Heat Treatment on Hardness Based on Table 2, Ti6Al4V as-built samples (untreated samples) have higher hardness values compared to heat treated samples. In this study, P3A sample has the highest hardness value but also the most deteriorated in hardness where the hardness for P3HT is reduced by 20%. In contrast, P1A has the lowest hardness with the value of 379.63HV while 317.95HV for P1HT. Similar trend is also seen for P2 where the hardness reduced after the treatment. In terms of VED, the hardness increases as the VED increased. This is due to the hardening of martensitic α as the VED increases from 51.28 J/mm3 (P1) to 90.91 J/mm3 (P3). However, the formation of acicular α' which takes place after heat treatment reduces the hardness and resulted to higher stiffness and higher strength of heat-treated samples. Heat treatment shows that it can make the surface harder to withstand fractures and fatigue. However, the findings of this study found that the results were different from [18] where heat treated samples have higher hardness than that of heat treatment samples. Such difference may be due to the variation of VED used in this study. In addition, higher hardness after heat treatment as reported in [18] is also may be due to the high temperature used on a different alloy grade which is Ti6Al4V Grade 5. In contrast, the findings of this study are similar to a study reported in [19] where the hardness decreases when the heat treatment is conducted at 800 and 900 °C. However, when higher heating temperatures (> 900 °C) are employed, the hardness increases Table 2 Hardness for untreated and heat-treated samples Reading

Untreated (no heat treatment) P1A

P2A

Heat-treated (with heat treatment)

P3A

P1HT

P2HT

P3HT

1

358.70

351.80

420.30

306.50

301.10

321.30

2

360.50

355.60

404.60

312.60

310.40

328.20

3

379.40

367.70

407.20

317.30

316.50

334.40

4

386.70

370.90

413.70

317.15

327.00

338.80

5

395.20

385.20

423.10

317.60

327.80

339.20

6

397.30

409.40

435.20

336.40

330.90

340.50

Avg

379.63

380.21

417.35

317.95

321.56

333.73

SD

± 16.79

± 21.25

± 11.31

± 10.01

± 11.69

± 7.58

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and reaches the maxima values. Therefore, the findings of this work are equivalent and comparable to those of the previous study [19]. In addition, heat treatment at higher temperature (> 935 °C) should be performed to obtain optimal results for heat treated samples.

3.2 Effect of Heat Treatment on Microstructure For the microstructure analysis, it was found that the microstructure in α + β phase are similar with the phase-phase predictions when the heat treatment is conducted at 935 °C with a holding time of 8 h. Figure 4 shows the comparison between the untreated; A (without heat treatment) with heattreated; HT (with heat treatment) for all samples (P1. P2 and P3). Figure 4 shows the phase transition from α to α + β phases after heat treatment and the increased of acicular α' when VED increased for untreated samples (P1A, P2A and P3A). However, it was also expressed in the β (darker region) in heat-treated samples whereas untreated sample was supplemented with α' and α. The ratio of α + β is different in each sample and the significant β ratio produces a stronger sample. In contrast, higher content of α (lighter area) phase expressed a softer sample. In the circle marked in Fig. 4 (P1A), short and coarse needle lines were observed while P3A shows long and smooth needle lines. The existence of long and thin acicular α enhances the hardness and produce a strong sample while the short and coarse needle line indicated the existence of a softer sample. In this microstructure analysis, with the employment of heat treatment, the β phase resulted to samples having higher hardness. On the other hand, the presence of fine and long needle lines in untreated samples shows that untreated samples have higher hardness. Such formation may be due to the stored residual stress that was formed during the printing process. In addition, by decreasing the VED, α lamellae was observed to be coarser due to the formation of acicular α' . This can be observed in Fig. 4 (P1A) where the lowest VED leads to coarser and shorter acicular α' . As the VED increases, α lamellae becomes clearer and the acicular α' is longer and finer, as observed in P3A. It is also found that the heat treatment triggered the formation of β at α phase boundary. At the same time, the formation of β is higher than the formation of α. This is due to the change in phase α to martensitic phase α, which is significantly more severe at higher heat treatment temperatures. The bound microstructure is produced by the colony plate such as α phase that appears in the previous β grain, and the granular boundary is decorated by α grains. As the VED increases, the original α' is completely decomposed into the martensitic α phase and the β phase layer. The initial structure of LPBF martensitic α was drastically transformed into elongated α details embedded in the boundary area of β phase. Heat treatment also resulted in the lamellae phase α evaporation with the thickness and formation of a globular in the boundary area. In terms of machining parameters, higher VED resulted to higher microhardness. This is because as higher VED used during LPBF printing, a better refinement of

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Fig. 4 Micrographs of Ti6Al4V cubic samples (Left) Untreated samples (without heat treatment), (Right) heat-treated sample (with heat treatment)

grain occurs where the width and spacing of α' martensite decreases which resulted in improving the hardness value [20]. However, take note that VED is the summation of the relation between the four main processing parameters. Therefore, a suitable correlation between the four main processing parameters is important to obtain the desired mechanical properties such as hardness.

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4 Conclusions The effect of heat treatment on the hardness and microstructure was successfully conducted. In addition, the hardness and microstructure were also compared for untreated and heat-treated samples. It was found that as the volumetric energy density (VED) increases, the hardness for untreated samples are increased. In addition, the hardness for untreated samples was found to be higher than that of heat-treated samples. This is because VED contributes to the hardening of the martensitic phase which resulted to higher hardness. As for heat-treated samples, due to the removal of residual stress, the hardness was found to be reduced up to 20% compared to untreated samples. For the microstructure analysis, it was found that as the VED increases, finer α lamella with long and thin needle lines were observed due to the increasing formation of acicular α' . At the same time, α lamellar phase will be extended and coarser compared to the sample without heat treatment due to the change in α phase to the martensitic α. After heat treatment, formation of α + β phase occurred due to heat treatment. Such formation improves the stiffness and strength of the heat-treated samples which may be suitable for automotive and bioimplants applications. Acknowledgements The authors would like to acknowledge Ministry of Higher Education (MOHE) for funding under the Fundamental Research Grant Scheme (FRGS) (FRGS/1/2019/ TK03/UKM/02/5) and Center for Research and Instrumentation (CRIM) Universiti Kebangsaan Malaysia (UKM) under the Geran Universiti Penyelidikan (GUP) (GUP-2021-015) for this project.

References 1. Song X, Zhai W, Huang R, Fu J, Fu MW, Li F (2022) Metal-based 3D-printed micro parts & structures. Encyclopedia of materials: metals and alloys, pp 448–461 2. Gu H, Gong H, Pal D, Rafi K, Starr T, Stucker B (2013) Influences of energy density on porosity and microstructure of selective laser melted 17-4PH stainless steel. In: 2013 International solid freeform fabrication symposium, University of Texas at Austin 3. Bandyopadhyay A, Heer B (2018) Additive manufacturing of multi-material structures. Mater Sci Eng R Rep 129:1–16 4. Bartolomeu F, Faria S, Carvalho O, Pinto E, Alves N, Silva FS, Miranda G (2016) Predictive models for physical and mechanical properties of Ti6Al4V produced by selective laser melting. Mater Sci Eng, A 663:181–192 5. Bartolomeu F, Dourado N, Pereira F, Alves N, Miranda G, Silva FS (2020) Additive manufactured porous biomaterials targeting orthopedic implants: a suitable combination of mechanical, physical and topological properties. Mater Sci Eng, C 107:110342 6. Ali H, Ma L, Ghadbeigi H, Mumtaz K (2017) In-situ residual stress reduction, martensitic decomposition and mechanical properties enhancement through high temperature powder bed pre-heating of selective laser melted Ti6Al4V. Mater Sci Eng, A 695:211–220 7. Lui EW, Xu W, Pateras A, Qian M, Brandt M (2017) New development in selective laser melting of Ti–6Al–4V: a wider processing window for the achievement of fully lamellar α + β microstructures. Jom 69(12):2679–2683 8. Guo YL, Jia LN, Kong B, Huang YL, Zhang H (2018) Energy density dependence of bonding characteristics of selective laser-melted Nb–Si-based alloy on titanium substrate. Acta Metallurgica Sinica (English Letters) 31(5):477–486

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9. Han J, Yang J, Yu H, Yin J, Gao M, Wang Z, Zeng X (2017) Microstructure and mechanical property of selective laser melted Ti6Al4V dependence on laser energy density. Rapid Prototyping J 23(2):217–226 10. Xiao Z, Chen C, Zhu H, Hu Z, Nagarajan B, Guo L, Zeng X (2020) Study of residual stress in selective laser melting of Ti6Al4V. Mater Des 193:108846 11. Yadroitsev I, Yadroitsava I, Bertrand P, Smurov I (2012) Factor analysis of selective laser melting process parameters and geometrical characteristics of synthesized single tracks. Rapid Prototyping J 18(3):201–208 12. Sun J, Yang Y, Wang D (2013) Parametric optimization of selective laser melting for forming Ti6Al4V samples by Taguchi method. Opt Laser Technol 49:118–124 13. Omoniyi PO, Akinlabi ET, Mahamood RM (2021) Heat Treatments of Ti6Al4V Alloys for Industrial Applications: An Overview. IOP Conf Ser Mater Sci Eng 1107(1):012094 14. Santos PCP, Correa EO (2021) Effect of duplex aging heat treatment on the stress corrosion cracking behavior of Ti-6Al-4V α+β titanium alloy in methanol. Mater Res 24(3):20200456 15. Vrancken B, Thijs L, Kruth JP, Van Humbeeck J (2012) Heat treatment of Ti6Al4V produced by selective laser melting: microstructure and mechanical properties. J Alloy Compd 541:177–185 16. Tsai MT, Chen YW, Chao CY, Jang JSC, Tsai CC, Su YL, Kuo CN (2020) Heat-treatment effects on mechanical properties and microstructure evolution of Ti-6Al-4V alloy fabricated by laser powder bed fusion. J Alloy Compd 816:152615 17. Qian M, Xu W, Brandt M, Tang HP (2016) Additive manufacturing and postprocessing of Ti-6Al-4V for superior mechanical properties. MRS Bull 41(10):775–784 18. Wang M, Wu Y, Lu S, Chen T, Zhao Y, Chen H, Tang Z (2016) Fabrication and characterization of selective laser melting printed Ti–6Al–4V alloys subjected to heat treatment for customized implants design. Prog Nat Sci Mater Int 26(6):671–677 19. Yan X, Yin S, Chen C, Huang C, Bolot R, Lupoi R, Kuang M et al (2018) Effect of heat treatment on the phase transformation and mechanical properties of Ti6Al4V fabricated by selective laser melting. J Alloy Compd 764:1056–1071 20. Buhairi MA, Foudzi FM, Jamhari FI, Sulong AB, Radzuan NAM, Muhamad N, Mohamed IF, Azman AH, Harun WSW, Al-Furjan MSH (2023) Review on volumetric energy density: influence on morphology and mechanical properties of Ti6Al4V manufactured via laser powder bed fusion. Prog Add Manuf 8:265–283

Effect of Curing Regimes Towards Carbonation Resistance of Green Lightweight Aggregate Concrete Containing POFA as Partial Cement Replacement Nur Azzimah Zamri , Khairunisa Muthusamy , Mohd Hanafi Hashim , Hamizah Mokhtar , and Muhammad Nazrin Akmal Ahmad Zawawi

Abstract In construction, carbonation is one of the major causes of reinforced concrete deterioration at site. Concrete carbonation causes embedded steel reinforcements to corrode, which resulted in concrete expansion and cracking. Concurrently, awareness towards reducing waste disposed by palm oil industry namely palm oil fuel ash (POFA) that have an impact towards environment has initiated researchers to convert these waste materials towards more environmentally friendly building materials. Meanwhile, palm oil clinker (POC), another waste generated from palm oil industry is abundantly produced which causes soil erosion. The present investigation looks into the effect of POFA content as partial cement replacement towards carbonation resistance of palm oil clinker lightweight aggregate concrete (POC LWAC). Performance of control palm oil clinker lightweight aggregate concrete and palm oil clinker lightweight aggregate concrete containing POFA as partial cement replacement under different curing regimes have been investigated in this research by using prisms of 100 mm × 100 mm × 500 mm that were water and air cured before subjected to carbonation test. The test results indicate that suitable integration of POFA content would results in pozzolanic reaction and filling effect which are beneficial in minimizing the pore size and volumes, thus reducing the carbonation rate and promotes better durability towards carbonation. Integration of 10% POFA considerably enhanced the carbonation resistance of POC lightweight aggregate concrete compared to other mixes. The test also shows that between the two different curing N. A. Zamri (B) · H. Mokhtar Civil Engineering Studies, College of Engineering, Universiti Teknologi MARA Pahang, Bandar Tun Abdul Razak, 26400 Jengka, Malaysia e-mail: [email protected] K. Muthusamy · M. N. A. Ahmad Zawawi Faculty of Civil Engineering Technology, Universiti Malaysia Pahang Al-Sultan Abdullah, Lebuhraya Persiaran Tun Khalil Yaakob, 26300 Kuantan, Malaysia M. H. Hashim Kolej Komuniti Pekan, Jalan-Pekan-Kuantan, Kampung Batu Satu Peramu, 26600 Pekan, Malaysia © The Author(s), under exclusive license to Springer Nature Singapore Pte Ltd. 2024 R. Abd. Aziz et al. (eds.), Intelligent Manufacturing and Mechatronics, Springer Proceedings in Materials 40, https://doi.org/10.1007/978-981-99-9848-7_43

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regimes, water curing resulted in better results in terms of carbonation resistance as it evident from the low porosity result conducted. Keywords Carbonation · Palm oil fuel ash · Palm oil clinker · Durability

1 Introduction Carbonation is the result of carbon dioxide (CO2 ) from the atmosphere attack in the concrete pore fluid that reacts the surface of fresh concrete. This process gradually penetrates deeper into the concrete that resulted in steel reinforcement corrosion. Therefore, various researches have been conducted to reduce the risk of carbonation in concrete. Among the efforts are the utilization of pozzolanic material in concrete production. Research by Kim et al. [1] incorporates three pozzolanic blended concrete mixtures including fly ash, silica fume and nanosilica. From the results, it can be found that the concrete containing nanosilica and silica fume showed the best carbonation resistance. Other researchers also integrate pozzolan in concretes which resulted in increasing carbonation resistance [2, 3]. Thus, this research emphasizes the use of POFA in OPC LWAC where it has not yet been implemented which will benefit various parties. However, optimal content of POFA will lead to increase in carbonation resistance and is dependent on curing condition adopted carbonation is that optimum amount of cement replacement with POFA decreases carbonation. From the research done by Tang et al. [4], 10% POFA replacement contribute towards better carbonation resistance. Replacing too much cement by POFA decreases the carbonation resistance as higher than optimum replacement resulted in higher carbonation depth. POFA has a slower activity reaction compared with OPC. According to [5] when a very high amount of POFA is incorporated in concrete, it requires a longer time to develop a better resistance. It is therefore suggested that a higher amount of POFA to replace cement is not recommended for carbonation resistance. At the same time, millions of tons of waste are generated from palm oil industry. In 2021, Malaysia produced 18.1 million tons of crude palm oil (CPO) [6]. However, a considerably small fraction is converted into value-added products while a large percentage is left underutilized [7]. Annually, approximately 0.06 million tonnes of palm oil fuel ash (POFA) [8] and huge amount of palm oil clinker (POC) were generated [9]. The quantity of waste from this industry does not only creates difficulty to dispose at landfill, but also causes contamination of air, soil and water. For example, POFA and POC are dumped at the nearby landfill, not only occupies valuable land but also causing environmental pollution and health hazards. Therefore, in order to overcome this problem, research has been initiated to convert this material to become more profitable value especially in the construction industry.

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Table 1 Mix proportion of 1 m3 green lightweight aggregate concrete with POFA Material

kg/m3 M0

M1

M2

M3

M4

Ordinary Portland cement

480

432

384

336

288

Palm oil fuel ash

0

48

96

144

192

Sand

750

750

750

750

750

Palm oil clinker

565

565

565

565

565

Water

216

216

216

216

216

Superplasticizer

4.8

4.8

4.8

4.8

4.8

2 Materials and Method 2.1 Materials In this study, the concrete was made of six main ingredients namely palm oil clinker (POC), palm oil fuel ash (POFA), ordinary Portland cement (OPC), fine aggregate, water and superplasticizer. Palm oil clinker and palm oil fuel ash were collected from nearby palm oil mill in the state of Pahang. The palm oil clinker was cleaned from any impurities such as soil or insect with clean water first before crushed using jaw crusher into smaller sizes. The collected palm oil fuel ash was also sieved using 300 µm sieve to acquire smaller particle ash and also to prevent other impurities from entering the concrete. For fine aggregate, river sand of passing 1.18 mm sieve was used to assist towards more compact concrete. For mixing and curing purpose, tap water was used throughout this research. Type A water-reducing admixtures in accordance to [10] was used throughout this research.

2.2 Mix Proportion In this investigation, the mix proportions adopted are displayed in Table 1 namely M0, M1, M2, M3 and M4. In M1, M2, M3 and M4 mixes, the binder was substituted by POFA in the amounts of 10, 20, 30, and 40%. Meanwhile in M0 mix, the binder used was entirely from ordinary Portland cement. The mix proportion for 1 m3 of green lightweight aggregate concrete with POFA is summarize in Table 1.

2.3 Testing Methods In this research, carbonation testing was conducted to examine the resistance of POC lightweight aggregate concrete containing POFA towards carbon dioxide intrusion.

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These testing is essential as it is associated with the steel reinforcement corrosion. The degree of carbonation rate was determined by measuring the carbonation depth in mm. The carbonation testing was based on the standard by [11]. In this study, 90 concrete prisms with the size of 100 × 100 × 500 mm3 were made. Water curing and air curing were used for curing the specimens. Then, the specimens were tested for carbonation the age of 7, 28 and 60 days. For water curing, the specimens were immersed in water tank until the age of testing while for air curing, the specimens were left outside of the laboratory until the age of testing. Phenolphthalein indicator solution was used to figure out the affected depth from the concrete surface. This white crystalline material was dissolved in alcohol with 1% solution. On the testing day, the specimens were split up, cleaned and brushed. The indicator solution was then sprayed to the surface of concrete. The depth of colourless region was measured using Vernier calliper which indicated the degree of carbon dioxide induced as shown in Fig. 1. The indicator would remain colourless when sprayed on carbonated area which shows that the concrete had contact with acid, suggesting carbonation. On the other hand, the indicator would change to pink colour when contact with non-carbonated area which shows the presence of base. Porosity test was also conducted in order to examine the voids in the concrete by referring to [12]. In this research, total of 30 concrete cubes of 100 mm × 100 mm × 100 mm were prepared. After 28 days water curing, the concrete was dried inside oven for 24 h (h) (Mo ). After the specimen was removed from oven, it was cool in a desiccator to a temperature of 20–25 °C and the mass was determined (Md ). The specimen was then covered with tap water, and boiled at 100 °C for 5 h in water bath. The specimen was allowed to cool for 24 h. The specimen moisture was removed by a towel and the mass was determined (Ma ). All the data were recorded and the porosity was calculated using Eq. 1 according to [12]. Fig. 1 Carbonation testing

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Porosity(%)

Md − Mo × 100 M d − Ma

483

(1)

3 Results and Discussion 3.1 Carbonation Figure 2 depicts the carbonation depth of POC LWAC containing 0, 10, 20, 30 and 40% POFA when subjected to two different curing condition namely water curing and air curing. The carbonation data was collected from 7 days up to 60 days of curing age. From the data presented, it shows that no carbonation was detected for the first seven days of curing age. The carbonation started at the age of 28 days for M3 and M4 under air curing. The carbonation depth is around 0.3 to 1.0 mm and increases by duration of exposure. The mechanism of carbonation involves the penetration of CO2 into the concrete porous system, reducing the pH around the reinforcement and initiate the corrosion process. Hence, it is important to produce high quality concrete in order to prevent or minimize CO2 penetration. As expected, water curing proves to be efficient as it assists POC LWAC towards better carbonation resistance due to complete hydration process in the presence of adequate water. Among the method that can be employed to reduce carbonation is the use of pozzolanic materials. Calcium silicate hydrate (C-S-H) gel produced from the pozzolanic reaction covers the fine pores inside the concrete internal structure thus reducing the carbonation intrusion. In this research, the depth of carbonation was reduced considerably when 10% POFA was utilized in POC LWAC. In other words, the replacement of optimum amount of POFA was found to be effective in reducing

Fig. 2 Carbonation depth of green concrete containing POFA

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Fig. 3 Porosity of POC LWAC containing POFA

the intensity of carbonation. In this research, the results follow the same trend as [1– 3]. The result was supported by investigation done by Tang et al. [4] in which inclusion of 10% POFA produce higher carbonation resistance due to its better micro-filling. In contrast, 40% cement replacement by POFA replacement shows insignificant results as it increased the carbonation depth by when subjected to air curing.

3.2 Porosity As illustrated in Fig. 3, it is apparent that the use of 10% POFA as cement replacement has the lowest porosity value. In this case, the filler effect of POFA refines and improves the concrete porosity. The same trend was observed by other researcher [13] who also investigated the effect of partial replacement of cement by pozzolanic material towards the porosity of normal weight concrete. It could be seen that as the percentage of POFA cement replacement is increased beyond the optimum amount, i.e., 10%, the higher, the porosity value exhibited. The addition of larger amount of POFA increases water demand thus produces lower compaction concrete. Fresh concrete should be compacted sufficiently so that capillary voids are completely removed. Based on Fig. 3, the porosity value is much larger when 40% POFA replacement was incorporated. According to [14], the size of capillary voids is much larger at the interfacial zone. Adding too much POFA resulted in the reduction of cement thus decreases the binding capacity between aggregates and cement. Porosity of concrete composed of large pores has detrimental effects on the durability performance of the concrete. Thus, based on the porosity result acquired, it is evident that lower porosity value due to inclusion of 10% POFA resulted in higher carbonation resistance of

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POC LWAC. Contrarily, higher carbonation rate when replacing cement with 40% POFA is due to the higher porosity as a result of larger capillary pores.

4 Conclusion The present findings show that palm oil fuel ash with optimum amount can be used as partial cement replacement with proper curing to produce palm oil clinker lightweight aggregate concrete exhibiting higher durability towards carbonation than control specimen. Success in utilizing palm oil fuel ash in lightweight aggregate concrete production would reduce the amount of cement used and contribute towards cleaner environment. Adequate amount of water would assist towards complete hydration process leading to more compact concrete and in turns increase the concrete resistance towards carbonation. Acknowledgements The authors would like to thank all the lecturers and technical staff of Universiti Malaysia Pahang Al-Sultan Abdullah for the assistance and co-operation received in conducting the experimental work. The financial support received from Universiti Malaysia Pahang Al-Sultan Abdullah through grant RDU1703109 are also gratefully acknowledged.

References 1. Kim JJ, Youm KS, Moon JA (2020) Study on conversion fraction and carbonation of pozzolan blended concrete through 29Si MAS NMR analysis. Appl Sci 10(19):6855 2. Seo JH, Amr IT, Park SM, Bamagain RA, Fadhel BA, Kim GM, Hunaidy AS, Lee HK (2018) CO2 uptake of carbonation-cured cement blended with ground volcanic ash. Materials (Basel) 5(11):2187 3. Santos BS, Albuquerque DDM, Ribeiro DV (2020) Effect of the addition of metakaolin on the carbonation of Portland cement concretes. IBRACON Struct Mater J 13(1):1–8 4. Tang WL, Lee HS, Vimonsatit V, Htut T, Singh JK, Wan Nur Firdaus WH, Alharthi N (2019) Optimization of micro and nano palm oil fuel ash to determine the carbonation resistance of the concrete in accelerated condition. Materials 12(130):1–19 5. Aprianti SE (2017) A huge number of artificial waste material can be supplementary cementitious material (Scm) for concrete production—a review Part II. J Cleaner Prod 142:4178–4194 6. Malaysian Palm Oil Board (2021) Annual Report 2021, https://mpoc.org.my/annual-report2021/. Accessed 06 June 2023 7. Focus Malaysia (2019) Boost for Malaysia’s biogas industry, https://focusmalaysia.my/. Accessed 06 June 2023 8. Yap SP, Alengaram UJ, Jumaat MZ (2013) Enhancement of mechanical properties in polypropylene and nylon–fibre reinforced oil palm shell concrete. Mater Des 49(2013):1034– 1041 9. Kanadasan J, Abdul Razak H (2014) Mix design for self-compacting palm oil clinker concrete based on particle packing. Mater Des 56:9–19 10. ASTM C494 (2017) Standard specification for chemical admixtures for concrete. West Conshohocken. ASTM International PA

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11. BS EN 14630 (2006) Products and systems for the protection and repair of concrete structurestest methods determination of carbonation depth in hardened concrete by the phenolphthalein method. The British Standard London 12. ASTM C642 (2013) Standard test method for density, absorption, and voids in hardened concrete. ASTM International, West Conshohocken, PA 13. Setina J, Gabrene A, Juhnevica I (2013) Effect of pozzolanic additives on structure and chemical durability of concrete. Procedia Eng 57:1005–1012 14. Singh N, Singh SP (2016) Review paper: reviewing the carbonation resistance of concrete. J Mater Eng Struct 3(2016):35–57

Advancements in 1D Nanostructure-Enhanced Carbon/carbon Composites for Aerospace Structures Ahmad Shahir Jamaludin, Ainur Munira Rosli, Mohd Zairulnizam Mohd Zawawi, Ismayuzri Ishak, and Roshaliza Hamidon

Abstract The ongoing development of carbon composites for aerospace applications has resulted in significant progress within the industry. However, despite the promising results observed in controlled environments, the application of these materials to extensive, practical situations, such as aerospace engineering, presents significant challenges. The primary difficulties primarily revolve around the elevated expenses involved in the production of carbon composites, thereby posing a financial concern for their widespread incorporation into aerospace endeavors. Moreover, the realization of highly complex aerospace structures that possess both expansive dimensions and intricate designs, while consistently achieving optimal performance, remains an ongoing challenge that has not been fully overcome. Considerable attempts have been undertaken to improve the thermal stability and mechanical characteristics of these composites by integrating nanostructures and various polymer matrices. However, it is crucial to attain a homogeneous dispersion of these nano-additives and comprehend their mutually beneficial interaction with the matrix material. The significance of maintaining the quality and uniformity of composite materials is emphasized by the significant previous studies, particularly in applications such as ultrasonic welding, microwave absorption, and structural integrity when subjected to different stressors. Future research should prioritize the exploration of innovative manufacturing techniques, which involve the utilization of automated and highly accurate fabrication tools. These endeavors have the potential to facilitate the widespread and economically feasible utilization of carbon composites in the field of aerospace engineering.

A. S. Jamaludin (B) · A. M. Rosli · M. Z. Mohd Zawawi · I. Ishak Faculty of Manufacturing and Mechatronic Engineering Technology, University Malaysia Pahang Al-Sultan Abdullah, 26600 Pekan, Pahang, Malaysia e-mail: [email protected] R. Hamidon Faculty of Mechanical Engineering & Technology, Universiti Malaysia Perlis, Pauh Putra Campus, 02600 Arau, Perlis, Malaysia © The Author(s), under exclusive license to Springer Nature Singapore Pte Ltd. 2024 R. Abd. Aziz et al. (eds.), Intelligent Manufacturing and Mechatronics, Springer Proceedings in Materials 40, https://doi.org/10.1007/978-981-99-9848-7_44

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Keywords Carbon composites · Aerospace structures · Nanostructure-enhanced composites · Carbon fiber-reinforced polymer composites · Composite repair and maintenance

1 Introduction to Carbon Composites in Aerospace Structures The aerospace industry relies more on carbon composites due to their high strengthto-weight ratio, thermal stability, and environmental degradation resistance. The unique properties of these materials make them ideal for aerospace structures that must withstand extreme temperatures and environmental conditions [1–10]. Recent technological advances have produced carbon/carbon composites with improved 1D nanostructures [11–20]. Aerospace structures’ thermal and mechanical properties improve when one-dimensional nanostructures are added to next-generation composites’ carbon matrix [21–35]. These nanostructures improve carbon composite efficiency and durability by enhancing their intrinsic properties [36–52]. These advances enable the design and manufacturing of aerospace structures with higher strength-toweight ratios and thermal and environmental stress resistance [24, 48, 52], attracting the aerospace companies interest in using CFRP composites [16–30]. Composite materials with a polymer matrix impregnated with carbon fibers are ideal for aerospace applications due to their rigidity, temperature resistance, and low weight [26, 29]. The synergistic effects of carbon fibers and resins have allowed the development of a wide range of carbon fiber-reinforced polymer (CFRP) composites that meet aerospace requirements [31–45]. Recycling epoxy resins and composites used in the aerospace industry is important for the environment. Transition-metalcatalyzed protocols recycle epoxy resins and composites. This process recycles these materials chemically and recovers bisphenol-A and undamaged fibers [1]. Continuous advancement in carbon composites and pioneering research are expected to yield even more durable materials, ensuring their aerospace dominance. The advancements, applications, and challenges of carbon composites in aerospace structures will be examined in the following sections [46–56]. The review critically analyzes the latest developments in the incorporation of 1D nanostructures into carbon/carbon composites, assessing their impact on aerospace mechanical and thermal properties and identifying current challenges and future avenues for optimized fabrication and large-scale integration.

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2 Recent Advances in Carbon Composites 2.1 1D Nanostructure-Enhanced Carbon/Carbon Composites The addition of 1D nanostructures to carbon/carbon composites advances aerospace materials. The proposed method incorporates one-dimensional nanostructures like CNTs or graphene nanoribbons into a carbon matrix, as shown in Fig. 1 [19]. These nanostructures improve carbon composites’ thermal and mechanical properties [1– 12]. The high aspect ratio and thermal conductivity of these nanostructures are their main advantages. Carbon nanotubes have thermal conductivity greater than copper. Due to thermal gradients, these materials’ thermal properties are crucial in aerospace applications. CNTs’ improved thermal conductivity improves heat dissipation, reducing thermal damage to structures and systems. Several studies and experiments support the merits of 1D nanostructure-enhanced composites. For instance: ● Thermal and Mechanical Improvements: Research into 1D MgCo2O4’s properties revealed that rod-like nanostructures demonstrated specific capacitance of approximately 752 Fg−1 , underlining the potential for enhanced electrochemical performance attributed to the rod-like structures [24]. ● Microwave Absorption Performance: Investigations into 1D structures for microwave absorption, such as the TiO2 @Co/C@Co/Ni microtube composite, have unveiled superior microwave absorption capabilities, emphasizing the significance of 1D structural designs [48]. ● Magnetic Properties for EM Wave Attenuation: The fabrication of a 1D carbon matrix framework designed for EM wave attenuation at a low frequency presented an effective absorption band of 1.3 GHz at 2 mm thickness, suggesting its potential for future applications [32].

1D Needle like Structure

Nanoribbon

Helical Nanoribbon

Fig. 1 From 1D nanostructures to 3D carbon nanotube transformation [19]

Carbon Nanotube

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While 1D nanostructures have improved properties, their scalability, matrix uniformity, and production cost remain issues [33–48]. Thus, optimizing nanostructure integration, and investigating their use in advanced aerospace applications may be part of future research objectives.

2.2 Carbon Fiber-Reinforced Polymer Composites Strength and light weight have revolutionized the aerospace industry with carbon fiber-reinforced polymer composites (CFRPs). Carbon fibers are added to polymer matrices to make CFRPs. The combination of these materials maximizes each component’s benefits. Thus, this composite has improved mechanical properties for aerospace applications [52]. Due to their carbon fibers, CFRPs can withstand most mechanical load. They have high tensile strength, stiffness, thermal conductivity, and low thermal expansion. Therefore, aerospace applications’ rigorous mechanical and thermal requirements are ideal [52]. The polymer matrix binds fibers and transfers load. The matrix material protects fibers, distributes loads evenly, and shapes and stabilizes the composite, as shown in Fig. 2. It is needed to choose the polymer matrix carefully to achieve the desired carbon fiber reinforced polymer (CFRP) properties. Epoxy and other thermosetting resins are popular for their adhesion and deformation resistance. Previous research shows transition metals can recycle epoxy resins and composites. This suggests sustainable materials [1]. Research has also focused on nanoscale CFRP modifications to improve performance. Carbon fiber reinforced polymers (CFRPs) with graphene nanoplatelets (GnP) and silicon carbide nanowires (SiCnw) improve thermal and mechanical properties [52]. Understanding CFRP damage is crucial for aerospace applications [15]. Advanced carbon fiber reinforced polymers (CFRPs) can withstand aerospace conditions. Additionally, the thickness of carbon fiber reinforced polymer (CFRP) composite plies can significantly affect interlaminar shear strength. The interlaminar shear strength (ILSS) of 8-ply CFRP composites was higher than 6-ply composites

Lower magnification

Higher magnification

Fig. 2 Optical micrographs of GnP/SiCnw-5 wt% interleaved CFRP [52]

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[28]. This shows composite strength depends on ply thickness. Carbon fiber reinforced polymers (CFRPs) are essential in aerospace due to their strength, rigidity, and low mass. Research in this field could lead to more efficient and sustainable aerospace materials.

3 Challenges and Limitations on Carbon Composites Application 3.1 Thermal Stability and Mechanical Properties Due to their strength-to-weight ratio, corrosion resistance, and thermal stability, carbon composites have transformed the aerospace industry. However, the growing demand for improved performance has created many challenges and limitations with these composites. Improving carbon composites’ thermal stability and mechanical properties is a major challenge. These composites can withstand thermal stresses, but prolonged exposure to extreme temperatures, especially in aerospace applications, can degrade them. The composite material’s degradation can reduce its strength, stiffness, and performance, posing safety risks in critical applications [1]. Nanostructures in carbon composites may solve this problem. Nanostructures can improve composite materials’ thermal and mechanical properties. Research shows that GnP/ SiCnw nanostructured films improve the thermal and mechanical properties of CFRP [52], as shown in Fig. 3. However, nanostructure efficacy depends on many factors. The type, concentration, and distribution of nanostructures in the composite are crucial. A homogeneous distribution is difficult but essential for the composite’s reliable and consistent performance. Uneven nanostructure clustering can cause localized stress. This can cause composite material failure prematurely. Hybridization enhances carbon composites. Glass fibers strengthen PC foam by increasing thermal stability and cell density [25]. In another study, silicone

Fig. 3 Various properties of neat CFRP and film interleaved CFRP [52]

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matrix carbon nanotubes (CNTs) and conductive sponges (CSs) created a composite material with good thermal and electrical conductivity. This bodes well for hybrid composites [31, 33]. Production and quality assurance of enhanced composites are becoming more complicated as technology advances. Fabrication consistency, industrial scalability, and long-term reliability need more research and optimization. Carbon composites are promising for aerospace and other demanding applications. The challenges of improving thermal stability and mechanical properties must be acknowledged. Nanostructures and hybrid materials may solve these issues as research advances, and understanding their implications and trade-offs is crucial.

3.2 Damage Detection and Quality Control Materials engineering still struggles to identify damage and ensure quality in composite materials, especially those containing carbon fibers. Complicated composite structures often have multiple layers and interwoven fibers, which makes them harder to build [36–48]. These complexities may hide defects. Internal damage in composite materials is a major concern. In critical applications like aerospace, even small damages can compromise the material’s structural integrity, posing significant risks. Although several techniques are available for damage detection, they come with their set of limitations, such as: ● Visual Inspection: The most direct approach has significant constraints. Visual inspection is subjective. The inspector’s expertise may miss minute or subsurface flaws, especially in the composite material’s internal strata. Small imperfections can propagate and intensify under operational strains. This can cause major malfunctions [2–11]. ● Ultrasonic Testing: ultrasonic welding (USW) uses sound waves to find material flaws. Additionally, a 250 µm electrodeposit (ED) thickness produces a stronger weld than a 50 µm ED. The procedure is laborious and depends on the operator’s skill. It involves identifying damage, assessing its magnitude, and assessing structural stability effects [2]. ● Robotic Systems: One study used a mobile thermographic inspection robot to assess composite material damage. The system picked up barely perceptible impact damage. Positional instability reduces the system’s effectiveness, showing that even sophisticated systems face complex damage detection challenges [26]. Environment and structural stress damage composites, especially aerospace composites. Minor flaws can become major ones. Identification and progression of initial damage are involved. Composite structures require advanced sensors and diagnostics for real-time health monitoring. This embedded diagnostic capability may help identify damages quickly, saving money and lives. Carbon composite damage detection and quality control have improved, but more research and innovation are needed. Implementing study findings may improve damage detection.

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4 Research Gaps and Future Directions The multifaceted field of carbon composites, particularly in aerospace applications, has been marked by significant technological breakthroughs. However, numerous challenges persist, necessitating a closer examination of existing gaps and contemplation of novel research directions. While carbon composites have displayed exceptional utility in controlled research environments, the real test lies in their effective translation into large-scale, real-world applications such as following conditions. ● Cost Implications: One of the most significant barriers is the elevated production cost associated with carbon composites, which can be inhibitive for expansive aerospace projects. ● Manufacturing Hurdles: The fabrication of large and complex structures without compromising on the quality and performance of carbon composites is an ongoing challenge. Maintaining consistency and uniformity during the scaling up process is crucial. ● Properties and Stability: Ensuring the thermal stability and mechanical robustness of carbon composites is paramount. Despite efforts to integrate nanostructures and various polymer matrices, disparities in distribution and inconsistencies in composite characteristics are observed [25, 51]. Comprehensive studies delving into the effect of different polymer matrices and their synergistic interplay with nanostructures are needed. Given the challenges enumerated, future research trajectories might encompass: ● Revolutionizing Manufacturing: There’s an imperative need to develop advanced manufacturing techniques that can enable large-scale production while upholding the structural and functional integrity of carbon composites. Embracing innovative fabrication methods can mitigate challenges associated with scaling [26, 49]. ● Dynamic Morphological Investigations: Research on the transformation of nanostructures, as observed in Ag+ -coordinated supramolecular structures, might shed light on how structural evolution can be manipulated for enhanced composite properties [19]. ● Understanding and Enhancing Thermal Behavior: Previous studies highlight the importance of thermal properties [25, 36, 38], there’s a clear directive for more concentrated research efforts in this area. Strategies to improve thermal stability and conductivity in composites, possibly by employing hybrid supported fillers or leveraging thermophysical properties of novel materials, could be revolutionary [11, 38]. In conclusion, the advancements made in the domain of carbon composites for aerospace applications serve as a foundation upon which future research can build. Addressing the current challenges and venturing into the recommended research avenues will not only bridge existing knowledge gaps but also propel the aerospace sector into a new era of innovation and sustainability.

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Acknowledgements The authors express their gratitude to the Ministry of Higher Education (KPT) for their generous support provided through the Fundamental Research Grant Scheme (FRGS) under grant number FRGS/1/2022/TK10/UMP/02/57, as well as to the University Malaysia Pahang AlSultan Abdullah for the internal grant RDU210365. The research has been significantly impacted by their dedication to scholarly investigation.

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The Potential of Nanomaterials for Improving Tire Rolling Resistance Mohd Nizar Mhd Razali, Ahmad Noor Syukri Zainal Abidin, Mohamad Rusydi Mohamad Yasin, Amirul Hakim Sufian, and Nurul Nadia Nor Hamran

Abstract Tire design and manufacturing have undergone substantial transformations, with innovations spanning from the incorporation of nanomaterials to advanced spoke design techniques. Despite these advancements, critical gaps remain in our understanding of tire-pavement interactions, particularly under varied conditions and with different tire materials. Existing research offers crucial insights into traction influences, predominantly for off-road scenarios, but the dynamics of diverse pavement interactions warrant deeper exploration. Further challenges include achieving consistent nanomaterial dispersion within the tire’s rubber matrix and evaluating potential environmental and health impacts of these materials. Future research directions should prioritize a holistic approach that accounts for both tire and pavement characteristics, aiming to improve noise reduction, performance, and safety. Additionally, an eco-centric lens should guide the synthesis and application of nanomaterials in tire manufacturing, ensuring sustainability alongside innovation. Addressing these focal areas can pave the way for optimized, safe, and environmentally responsible tire solutions. Keywords Tire performance · Nanomaterials · Tire-pavement interaction · Tire design · Material nonlinearity

1 Introduction The significance of tire performance in the domain of vehicle operation cannot be overstated, as it has a profound influence on fuel efficiency, safety, and the overall quality of the vehicle’s performance. Rolling resistance is a crucial factor that significantly influences tire performance. It refers to the amount of energy dissipated when a tire rolls while bearing a load. The dissipation of energy primarily occurs as heat as a result of the viscoelastic properties of the materials that are essential to the M. N. Mhd Razali (B) · A. N. S. Zainal Abidin · M. R. Mohamad Yasin · A. H. Sufian · N. N. Nor Hamran Faculty of Manufacturing and Mechatronic Engineering Technology, Universiti Malaysia Pahang Al-Sultan Abdullah, 26600 Pekan, Pahang, Malaysia e-mail: [email protected] © The Author(s), under exclusive license to Springer Nature Singapore Pte Ltd. 2024 497 R. Abd. Aziz et al. (eds.), Intelligent Manufacturing and Mechatronics, Springer Proceedings in Materials 40, https://doi.org/10.1007/978-981-99-9848-7_45

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construction of tires [1–9]. There exists a direct correlation between the degree of rolling resistance and fuel consumption. A decrease in rolling resistance leads to an increase in fuel efficiency due to the reduced energy required to overcome the resistance. This ultimately results in lower fuel consumption over a given distance [8–18]. In addition to its impact on fuel efficiency, the tire’s comprehensive performance plays a crucial role in determining the functionality of a vehicle. Factors such as tread design, tire pressure, and constituent materials significantly impact vehicle handling and safety through their influence on tire traction [5–7, 19–21]. The maintenance of a dependable grip on the road is crucial for ensuring effective traction, which in turn enables safe acceleration, deceleration, and changes in direction for the vehicle [22–29]. Furthermore, the interaction between the tire and road surfaces plays a significant role in the generation of noise emitted by the vehicle [26–33]. This particular interaction has the potential to induce noise generation as a consequence of tire vibration and the enclosed air cavity, which plays a significant role in the overall noise, vibration, and harshness (NVH) characteristics of the vehicle [1–11]. Addressing and minimizing such noises is a crucial focal point in modern vehicle design. The implementation of this technology not only enhances the level of comfort experienced by individuals within the space, but also effectively reduces the levels of noise pollution, thereby providing advantages to the surrounding environment as a whole [33–40]. From an ecological perspective, the enhancement of tire performance has the potential to greatly reduce the release of greenhouse gas emissions. This becomes increasingly crucial given the rising prevalence of electric vehicles. The range of a vehicle is significantly impacted by the rolling resistance of its tires. With the increasing energy efficiency of electric vehicles compared to internal combustion engine vehicles, the utilization of tires with low rolling resistance can enhance their attractiveness. The conservation of energy has the potential to increase the driving distance of electric vehicles, thereby improving their overall utility [1, 12–18]. The purpose of this review is to provide a comprehensive understanding of current research on the potential of nanomaterials to enhance tire performance, with a specific emphasis on reducing rolling resistance. This study explores the complex relationship between tires and pavement, examining the impact of different tire and ground characteristics on traction. Additionally, it investigates the potential use of nanomaterials in tire manufacturing and analyzes how tire design and material nonlinearity affect tire performance [19–21, 40].

2 Tire-Pavement Interaction and Noise Reduction and Influence of Tire and Soil Parameters on Traction The complex interaction between tires and pavement affects vehicle performance and noise. This interaction illustrates the dynamic tire tread-road surface interface. The process is affected by tire pressure, tread design, road surface texture, temperature,

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and moisture [1]. The origin of rolling noise or tire-pavement interaction noise is important. The tire vibrates when the road is uneven, causing noise. These vibrations travel through the tire and vehicle structure, causing noise inside and out [1]. This interaction also affects tire rolling resistance, which is energy dissipated as heat during moving a loaded tire. Road surface characteristics can affect tire deformation, increasing rolling resistance and fuel consumption. To improve fuel efficiency and reduce environmental impact, tires and pavement interactions must be understood and optimized [8–11]. Tire noise has been reduced by changing tire design, materials, and road surface characteristics. Air pumping noise, a major component of tire noise, can be reduced by certain tread patterns [1]. The use of nanomaterials and bio-based elastomers in tire manufacturing has also reduced noise. Enhancing the tire’s vibration absorption reduces vibration transmission [12–14, 26–32, 36–39]. Texture and coarseness of road surfaces affect noise modulation. Numerous studies have shown that refined road textures reduce tire noise. To ensure road safety, these modifications must be balanced with performance metrics like skid resistance and lifespan [12–14, 26–32]. Noise abatement has made progress, but there are still many research opportunities. Innovative tire designs and advanced materials to reduce noise and improve tire performance are expected [19–21, 29–35, 40]. Investigating the complex interaction between tires and pavement, while understanding their unique characteristics and collective behavior, may lead to new noise-reduction strategies. This research can integrate noise reduction, tire functionality, and safety measures to improve driving and ecological sustainability.

2.1 Impact of Tire Parameters on Traction Traction, the frictional force between a tire and its surface, determines a vehicle’s performance range. A vehicle’s amplitude affects its acceleration, deceleration, and direction. Tire pressure, tread design, and manufacturing materials affect traction [5– 11], as shown in Fig. 1. Tire pressure controls and adjusts traction. Insufficient tire inflation increases surface contact, which may improve traction. However, this tradeoff increases rolling resistance and tire degradation. Under-inflation causes more tire surface to contact the road. This increased contact increases friction and heat, which accelerates tire wear and fuel consumption [22–25]. However, overpressurized tires may reduce contact patch size and traction. Due to reduced rolling resistance, this may improve fuel efficiency. Overinflated tires become rigid and lose their ability to conform to the road. Frictional forces decrease as the tire’s interaction with the road decreases [5–7]. Tire traction dynamics depend on blueprint design. The tread pattern channels water away from the contact area, affecting the tire’s adhesion in wet conditions. For instance, deep and wide grooved tires disperse water well, reducing hydroplaning risk. Hydroplaning occurs when tires lose contact with the road due to water. In slipperiness or off-road terrain, tire tread depth affects traction. Deep treads improve traction and mechanical cohesion by embedding into the surface [5–7].

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Fig. 1 ThermoRIDE system an experimental device to study tire traction [5]

Tire manufacturing materials are crucial to traction. Malleable rubber compositions may improve adhesion in cold climates, but they wear out quickly. Pliable materials can better follow terrain contours due to their inherent property. Thus, enhanced conformity expands the interaction domain and increases friction. However, stress can cause excessive deformation in these materials, increasing rolling resistance and wear [8–14]. The use of nanomaterials in tire production could balance traction and durability. Nanomaterials’ small size and large surface area can improve rubber blends’ mechanical properties [15–18]. Thus, this can lead to tires with better traction and durability, improving vehicle safety and efficiency.

2.2 Role of Soil Parameters on Traction Off-road vehicles’ traction is heavily influenced by soil parameters. The tire-soil interaction is affected by soil characteristics and tire properties and designs. Soil type, moisture content, and surface roughness affect tire-soil traction off-road [22– 25]. Due to their particle sizes and shapes, sandy, clayey, and loamy soils have different traction properties. Sandy soils’ large, spherical particles can shift or roll under the tire, reducing traction. Clayey soils have smaller, flatter particles that can adhere to each other, increasing traction. Under wet conditions, the above soils are slipperier. Loamy soils, which contain sand, silt, and clay, have balanced traction properties [22–25]. The presence of moisture can affect soil traction. The lubricating effect of water in soils reduces traction. Water reduces the coefficient of friction between the tire and soil particles, making the surface slipperier. However, a little moisture can increase soil particle cohesion and traction. Thus, soils with a slight moisture may have better traction than dry or wet soils [22–25]. The tire-soil contact area can change due to vegetation and rocks, causing surface roughness changes that affect traction. Rough surfaces may increase mechanical interlocking and traction. However, excessively

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rugged terrains can damage tires or make riding uncomfortable [22–25]. Numerous academic studies have shown the importance of tire designs and materials in these interactions. For instance, bio-based elastomers can provide different traction properties on different soil compositions than traditional rubber [36–39]. The mechanical properties of tires, which are affected by natural oils and gel particles, can also affect their performance in different terrains [12–14]. Sand and mud may be better for tires with deeper tread or specific tread patterns [2, 12–14]. Off-road vehicle design and operation require a thorough understanding of soil parameters and traction. Understanding soil conditions and developing driving strategies can help choose tires and optimize vehicle performance in off-road terrain. This knowledge improves offroad vehicle performance and adaptability, making off-road driving safer and more efficient.

3 Nanomaterials in Tire Manufacturing 3.1 Use of Nanomaterials in Tire Manufacturing The inclusion of nanomaterials in tire manufacturing represents a transformative advancement, unlocking the potential for markedly better tire performance. Owing to their distinct attributes such as extensive surface area and exceptional mechanical robustness, nanomaterials can augment the attributes of rubber compounds integral to tire fabrication [8–14]. Consequently, the outcome is tires exhibiting enhanced longevity, superior grip, and minimized rolling resistance. Such features can be pivotal in achieving better fuel economy and eco-friendliness [8–11]. Nano silica stands out as one of the pivotal nanofillers integrated into tire treads. Its multifunctional role encompasses not only fortifying the rubber but also diminishing tire rolling resistance, which culminates in reduced fuel expenditure. However, integrating silica particles uniformly within the rubber matrix remains a daunting task. The reason being the abundant silicon hydroxyl groups on their surface, leading to an uneven dispersion of the nanofiller. Such disparities can be detrimental to the tire’s holistic performance [8–11]. Historically, the role of silane coupling agents was pivotal in tailoring silica to enhance its amalgamation within the rubber matrix. Yet, this method poses environmental risks due to the copious release of volatile organic compounds (VOCs), detrimental to both ecological balance and worker safety [8–11, 15–18]. Addressing this conundrum, the innovation of epoxidized solution polymerized styrene-butadiene rubbers (ESSBRs) emerged as game-changing macromolecular coupling agents. Capable of reacting seamlessly with the silicon hydroxyl groups present on the silica surface, ESSBRs execute this without VOC emissions, marking a significant stride towards sustainable tire manufacturing [15–18]. This ingenious technique not only streamlines the integration of nanosilica within the rubber matrix but also eradicates the detrimental VOC discharges. Proven to augment the attributes of silica/

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rubber nanocomposites, the ESSBRs strategy holds immense promise for the future incorporation of nanomaterials in tire design [15–18].

3.2 Challenges and Solutions in Nanomaterial Application Nanomaterials in tire production have many benefits, but they also have drawbacks. The homogeneous distribution of nanomaterials in the rubber matrix is crucial. Nanomaterials must be properly dispersed to maximize their potential. Agglomerates in rubber compounds can weaken structurally and reduce mechanical properties. Dispersion requires careful control of mixing parameters and nanomaterial-rubber compatibility. Agglomerated nanomaterials become stress concentrators, causing premature rubber compound failures [15–18]. The environmental and health effects of nanomaterials are another issue. Conventional silane coupling agent modification of silica emits harmful volatile organic compounds (VOCs). The volatile organic compounds (VOCs) have negative environmental effects and pose significant occupational health risks. Nanomaterials’ effects on human health and the environment are unknown and need further study. The small size of these organisms allows them to overcome biological obstacles, which may have negative effects. Therefore, thorough research is needed to assess nanomaterial risks and develop effective mitigation strategies [15–18]. The scientific community is persistently seeking solutions. A notable method is using ESSBRs as macromolecular coupling agents. These agents react with silicon hydroxyl groups on silica surfaces without releasing volatile organic compounds. The above procedure improves sili-ca/rubber nanocomposites and reduces VOCs, making it a more environmentally friendly alternative to silane coupling agents [15– 18]. Research on bio-based synthetic elastomers [26–32] and poly(dibutyl itaconatebutadiene) copolymer nanocomposites [36–39] suggests a sustainable and environmentally friendly way to reduce ecological risks and promote sustainable development. Environmentally friendly nanomaterial production using sustainable resources or non-harmful solvents is also growing. This is followed by the development of non-toxic nanomaterials or protective coatings to reduce nanomaterial release [12–18].

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4 Tire Design and Material Nonlinearity 4.1 Impact of Spoke Design on Tire Performance The performance of a tire is not exclusively determined by its design; rather, the material properties and their nonlinear characteristics also contribute significantly to its overall performance. The presence of material nonlinearity, specifically in nonpneumatic tires, presents numerous challenges when attempting to forecast and evaluate tire performance across different circumstances. Numerous research studies have elucidated that the amalgamation of distinct spoke designs with specific nonlinear materials can result in notable improvements in tire performance. As exemplified by a thorough investigation [19–21], the significance of Polyurethane (PU) material characteristics and their interplay with various spoke configurations was underscored. The study utilized advanced three-dimensional finite element method (FEM) simulations to provide valuable insights into the relationship between material nonlinearity and spoke design, and its impact on achieving optimal tire performance. Additionally, it has been indicated that specific combinations have the potential to result in improved load distribution, decreased stress concentrations, and enhanced overall durability [19–21]. Furthermore, it has been discovered that through the modification of the tire’s material properties in combination with the adjustment of the spoke design, manufacturers can attain particular desired results, such as enhanced rolling resistance, improved traction, or increased ride comfort. Furthermore, the significance of selecting appropriate materials is heightened when taking into account the aspect of environmental sustainability. In contemporary tire manufacturing, there has been a notable shift towards the utilization of bio-based elastomers, as shown in Fig. 2 [29]. This shift is primarily motivated by the potential of these materials to mitigate environmental pollution and foster sustainable development [26–32]. The utilization of bio-based elastomers, in conjunction with novel spoke designs, has the potential to facilitate the development of tire solutions that are not only high-performing but also environmentally sustainable [19–21, 26–32]. Thus, it is crucial to recognize the significant role of tire design, particularly spoke configuration, in addition to the essential consideration of the material’s inherent properties and its nonlinearity. Collectively, these factors contribute to the tire’s performance, longevity, and overall adaptability to diverse road conditions [19–21, 26–32].

4.2 Material Nonlinearity in Tire Design The nonlinear behavior of materials, termed as material nonlinearity, denotes their atypical response to the forces exerted upon them. Specifically, such materials don’t exhibit a direct relationship between deformation and the applied stress. When considering tire design, this nonlinearity becomes especially pivotal as it influences various performance parameters, including traction, rolling resistance, and

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Fig. 2 Epoxidation process schematic of Styrene Butadine Rubber [29]

wear resistance. In recent research, material nonlinearity was explored in-depth, considering its implications on tire performance [19–21]. The study highlighted that the introduction of different materials could produce varied levels of nonlinearity, subsequently affecting the tire’s overall behavior. For example, the integration of Solution-polymerized Styrene-Butadiene Rubber (SSBR) and Butadiene Rubber (BR) yielded tires exhibiting commendable wet-skid resistance and low rolling resistance [40]. Wet-skid resistance, a metric gauging a tire’s capability to maintain grip on moisture-laden surfaces, is paramount for ensuring vehicular safety. Conversely, low rolling resistance pertains to a tire’s efficiency in moving across surfaces, with direct implications on fuel consumption and, thereby, environmental impact. Further enriching the discourse on material enhancements in tires, the use of Epoxidized Styrene-Butadiene Rubber (ESSBR) emerged as a notable strategy [15–18]. Deployed as a macromolecular coupling agent, ESSBR establishes potent chemical bonds between the rubber matrix and silica filler. This not only augments the dispersion of the filler within the rubber matrix but also significantly bolsters the tire’s resistance to wear [15–18]. Given the ever-increasing demands for extended tire durability and lifespan, such findings accentuate the paramount importance of understanding and leveraging material nonlinearity in tire designs.

5 Research Gaps and Future Directions Tire design and manufacturing have advanced in nanomaterial integration, spoke design, and soil parameter-traction relationships. However, we must address our understanding gaps. The dynamics of tire-pavement interaction are important and need further study. Previous research has shed light on how soil parameters affect traction, especially for off-road vehicles. However, pavement conditions and their

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effects on tire designs and material compositions must be studied [5–7]. Nanomaterials’ potential in tire manufacturing is also untapped. Tires can improve performance, but obstacles remain. Ensure nanomaterials are evenly distributed in the rubber matrix. The potential environmental and health effects of these nanomaterials are still unknown [15–18, 40]. Based on gaps, several research trajectories can be identified, including: 1. Studies consider both tire characteristics and pavement conditions. The goal is to reduce tire noise and improve performance. This research could help develop advanced tire designs and materials that adapt to different pavement conditions. Research on environmentally friendly nanomaterials in the tire industry is crucial for improving vehicle safety and performance [8–11, 22–25]. 2. This involves creating new nanomaterial production and application methods that address environmental and health issues. The long-term effects of nanomaterials in tires must also be examined [15–18, 33–39]. In conclusion, research has made significant advances, but there are still unexplored areas that need further study. Future efforts can guide the development of optimized, safe, and environmentally conscious tire solutions by focusing on these areas. Acknowledgements The author extends sincere appreciation to the Ministry of Higher Education for their invaluable support of this study via the Fundamental Research Grant Scheme, with the grant reference RACER/1/2019/TK05/UMP//1. Their dedication to nurturing academic inquiry and progress was indispensable to this research. Further gratitude is directed to the Universiti Malaysia Pahang Al-Sultan Abdullah for their steadfast support and financial aid, as recognized by grant RDU Number RDU210312.

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Effect of Doping Nickel/Cobalt Ions on Structural, Optical, Morphological and Photocatalytic Efficiency of Zinc Oxide Ain Nor Annisa Hussin , Nurul Fatihah Norapandi , Nurjannah Salim , and Nurul Huda Abu Bakar

Abstract Zinc oxide (ZnO) has been proven as one of the most researched semiconductors photocatalyst because of its non-toxic nature and physical stability. The efficiency of ZnO as photocatalyst can be improved by doping with transition metals like cobalt (Co) and nickel (Ni). Nevertheless, the interaction between the transition metals with ZnO for photocatalytic studies is still unclear. The present work intrigued to compare the structural, optical, and morphological properties over photocatalytic activity of Co- and Ni-doped ZnO at shorter irradiation time. The results demonstrated that with the addition of Co and Ni dopants, the intensity of the x-ray Diffraction (XRD) patterns decreased suggesting that Co2+ and Ni2+ successfully incorporated to the Zn2+ sites in the crystal. Meanwhile, Fourier Transform Infrared Spectroscopy (FTIR) spectra confirmed the presence of bands assigned to the Zn–O and the absorption peak were quenched with the doping of Ni and Co. The morphological studies using Scanning Electron Microscopy (SEM) shows the heterostructures of ZnO with Co and Ni. The ZnO exhibits irregular nano-grain distribution consisting of tightly packed sphere and ellipsoidal particles while the Co–ZnO and Ni–ZnO samples exhibit quasi-spherical and rod-shaped surface morphologies. The BET isotherms denoted that the samples are classified as type IV which is mesoporous. It is noteworthy that by doping, the energy bandgap decreased from 3.11 eV (ZnO) to 2.98 eV (Co–ZnO) and 3.02 eV (Ni–ZnO). Results revealed that Co-ZnO exhibited better photocatalytic performance within 30 min of irradiation at lower loading of 10 and 30 mg/ml. Keywords Dopants · Photocatalyst · Heterostructure · Transition metals

A. N. A. Hussin · N. F. Norapandi · N. Salim · N. H. Abu Bakar (B) Faculty of Industrial Sciences and Technology, Universiti Malaysia Pahang Al-Sultan Abdullah, 26300 Gambang, Pahang, Malaysia e-mail: [email protected] © The Author(s), under exclusive license to Springer Nature Singapore Pte Ltd. 2024 R. Abd. Aziz et al. (eds.), Intelligent Manufacturing and Mechatronics, Springer Proceedings in Materials 40, https://doi.org/10.1007/978-981-99-9848-7_46

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1 Introduction Nowadays, zinc oxide (ZnO) nanoparticles have attracted much attention in the UV absorption applications especially in degradation of pollutants [1]. Previous research also revealed that ZnO nanoparticles have great potential in solar cells, piezoelectric devices, medicines, transistors, textiles, rubber products, light emitting diodes, food packaging and biosensors [2–6]. Intrinsically, ZnO is an n-type semiconductor with a direct large band-gap of 3.30 eV and can crystalize as a hexagonal wurtzite structure. For many years, there are a lot of research has been done to modify the ZnO nanoparticles such as doping it with transition metals (TMs) namely Fe, Ni, Mn, Co and Cu [7–9]. It is observed that each of the ZnO doped TMs exhibit profound and improve properties especially in the band gap, morphology, and structural properties [10]. In this regard, the photocatalytic activity of ZnO doped TMs is also improved due to the enhancement in its energy band gap. Without doping, the photocatalytic applications of ZnO are deterred because of its fast electron–hole (e–h) pair recombination and experience photo-corrosion. The optical properties of ZnO doped TMs are one of the major contributors for a successful photocatalysis activity. The near-band gap emission is due to their combination of free electrons in the conduction band and holes in the valence band. In addition, the photoluminescence feature of the ZnO is attributed to a broad band emission within the visible region, due to transitions involving defect states. Among the transition metals, Co and Ni exhibit similar ionic number and can be replaced with Zn2+ ions with little distortion to the crystal lattice [11]. Previously, Codoped ZnO nanorods were created, and the performance of alizarin red photocatalytic degradation was improved. Additionally, Kuriakose et al. [12] produced Co-doped ZnO nanodisks and nanorods and it was observed could improve photocatalytic activity due to the efficiency of charge separation and surface area. On the other hand, Ni-doped ZnO shows unique behavior while retaining some characteristics of the host. Although it has been reported that the photocatalytic activity of Coand Ni-doped ZnO are improved, the comparison between Co-ZnO and Ni-ZnO photocatalytic efficiency related to the structural and optical properties are still remain unclear. The Co and Ni dopants expected said could improve the photocatalytic activity by creating new energy level in the energy band gap. Hence, it is crucial to study the aforementioned Co–ZnO and Ni-ZnO nanomaterials as photocatalyst and determine the optical properties qualitatively and quantitatively with the help of energy band gap processing using UV–Vis by tuning their concentrations. The interaction of Co and Ni dopants with ZnO upon sol–gel processes are expected to offer various forms of structure and morphological properties at nanoscale level. In addition, the enhancement in the photocatalytic activity of the Co- and Ni-doped ZnO might be observed with the increment number of surface-active sites and formation of ZnO nanorods; especially when doped with Co, which results in higher adsorption of O2 molecules and OH ions for the degradation process of methylene blue (MB). Therefore, the present work investigated the

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structural, optical and morphological properties of the Co- and Ni-doped ZnO using of x-ray Diffraction (XRD), Fourier Transform Infrared Spectroscopy (FTIR) and Scanning Electron Microscopy (SEM). Meanwhile, the photocatalytic activity of the samples was observed with an irradiation time of 30 min to evaluate the effect of MB degradation at a shorter time.

2 Experimental 2.1 Materials Zinc acetate dihydrate [Zn(CH3 COO) 2 H2 O], Sodium hydroxide (NaOH), cobalt (II) acetate tetrahydrate [Co(CH3 COO)2 •4H2 O] (MW = 249.08 g/mol), nickel (II) acetate tetrahydrate [NiCH3 COO)2 •4H2 O] (MW = 248.86 g/mol) and absolute ethanol. Each chemical was of analytical grade and can be used right away without additional purification.

2.2 Synthesis of Co- and Ni-Doped ZnO Zinc acetate dihydrate [Zn(CH3 COO)·2 H2 O] was dissolved in 200 ml of ethanol at room temperature and mixed using magnetic stirrer until cleared and transparent sol achieved. Sodium hydroxide (NaOH) was used as a source of oxygen where 0.02 M of NaOH with 200 ml of ethanol solution was gently added to the sol and stirred for 60 min. The sol then went through the centrifuge process which was set at 5000 rpm for 20 min until white precipitate settled down at the bottom of the centrifuge tube. The precipitates were dried at 50 °C for 15 min in an oven and finally, the dry precipitates were annealed in a furnace at 300 °C for 12 h to attain suitable crystallinity and properties of ZnO according to the previous method [13, 14]. In the meantime, the Co and Ni dopants were introduced into the zinc sol using similar method. 0.2 M nickel (II) acetate tetrahydrate [Ni(CH3 CO2 )2 ·4 H2 O] and 0.2 M cobalt (II) acetate [Co(CH3 COO)2 ·4H2 O] was dissolved in 200 ml of ethanol to generate aqueous solutions of in dopant concentrations, separately with zinc sol at room temperature and was stirred using magnetic stirrer. A clear sol was formed and similar procedure demonstrated above for ZnO synthesis was used to obtain Coand Ni-doped ZnO nanomaterials. The samples were labelled as ZnO, Co–ZnO and Ni–ZnO, respectively.

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2.3 Characterizations The as-prepared ZnO, Co–ZnO and Ni–ZnO powder were further characterized using x-ray Diffraction (XRD) (Rigaku) to determine the crystal structure and phase formation of the samples at 2θ scan range of 20–80°. From the obtained XRD data, the crystallite size was calculated using the Debye Scherer’s formula (Eq. 1) as follows: D=

κλ Qcosθ

(1)

where, κ is the shape factor (0.94), D is crystallite size, λ is wavelength (1.54 Å), Q is full maxima half width, and θ is the diffraction angle. Fourier Transform Infrared Spectrometer (FTIR) (Perkin Elmer (Model Spectrum 100)) was used to investigate the functional group of the samples. The characterization was performed using a Potassium Bromide Disk (KBr) method at a spectral range from 4000 to 400 cm−1 . The pore size distribution and surface area of the samples was further characterized using Brunauer–Emmett–Teller (BET) (MICROMERITICS MODEL:ASAP2020) at a temperature 350 °C. The surface morphology of the samples was observed using scanning electron microscopy (SEM) (JEOL) at 5.0 kV with magnification × 10 000. UV–visible absorption measurements were performed by using a UV–Vis spectrophotometer (Lambda 25, Perkin Elmer). The energy band gap was determined using a Tauc plot (Eq. 2): (ahv)n = A(hv − E g )

(2)

where, A is a proportionality constant, hv is the incident photon energy, α is the absorption coefficient, n = 1/2 for the direct bandgap of ZnO.

2.4 Photocatalytic Degradation The photocatalytic analysis was conducted in a typical degradation experiment where 10 mL methylene blue (MB) solution with a concentration of 10 mM was continuously stirred with the ZnO, Co–ZnO and Ni–ZnO powder in the dark to ensure establishment of an adsorption–desorption equilibrium on the surface of the photocatalyst samples. Pure MB solution was considered as the initial MB concentration before the start of irradiation while the degradation of the MB solution and photocatalyst was placed under UV lamp at a distance of approximately 10 cm. The concentrations of the samples in MB solution were varied at 10, 30 and 50 mg/ml and the samples were irradiated for 30 min to analyze the effect of degradation at shorter time. After irradiation, the samples were quickly drawn out of the MB suspension using a syringe with a nylon filter and observed using UV–Vis spectrophotometer.

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3 Results and Discussion 3.1 Structural Analysis The crystal structure of the ZnO, Co-ZnO and Ni-ZnO samples were determined by XRD characterization technique, as shown in Fig. 1a. From the XRD pattern, prominent x-ray diffraction lines at 2θ = 31.97°, 36.56°, 56.78° and 62.67° are observed. The diffraction peaks could be indexed as (1 0 0), (1 0 1), (1 1 0), and (1 0 3), respectively, which correspond to the hexagonal wurtzite phase of ZnO [15]. Nevertheless, with addition of Co and Ni dopants the intensity of the peaks decrease suggesting that Co2+ and Ni2+ successfully incorporated into the Zn2+ sites in the crystal [16]. In addition, it can be seen that when Co and Ni ions were introduced, the diffraction peaks shift to higher angles, suggesting that the unit cell contracting to occupy the ions. The width is also broadening due to the formation of smaller average diameters as a result of increase in disorder on Co2+ and Ni2+ . In this regard, the crystal size was found to reduce from 14.8 nm for ZnO to 8.57 nm and 8.15 nm for Co–ZnO and Ni–ZnO, respectively. The FTIR spectra in Fig. 1b reveal the presence of absorption bands assigned to the O–H vibrations (~ 3445 cm−1 ) and aromatic and aliphatic C–H moieties (~ 2926.87 and 2850.05 cm−1 ), respectively. The intensity of the absorption bands decreased dramatically for Ni-ZnO sample denoting more moisture was released during calcination. Strong C=O stretching vibrations at 1630 cm−1 were observed in pure ZnO, compared to Ni–ZnO and Co–ZnO samples and the results are in agreement with previous study [17]. The spectroscopic analysis confirmed the presence of bands. assigned to the Zn–O (~ 450 cm−1 ) and the intensity of the band were quenched with addition of Ni and Co dopants. The result implies that there were impurities (Ni and Co dopant) which existed near ZnO surface [18]. It can be clearly seen that

Fig. 1 a XRD patterns and b FTIR spectra of ZnO, Co–ZnO and Ni–ZnO

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the bands were also shifted towards higher wavenumbers. In this regard, a strong vibration of the. Co–O–H moiety was responsible for the broad peak at ~ 1114 cm−1 whereas broad band at ~ 680 cm−1 is assigned to the Ni–O stretching band. The result was consistent with that reported elsewhere which confirm the formation of NiO nanoparticles [19]. BET is also utilized to determine the surface area and pore size of the samples [20]. The nitrogen adsorption/desorption isotherms and pore size distributions of ZnO, Co-ZnO, and Ni-ZnO samples are shown in Fig. 2. The figure shows that the isotherms are classified as type IV and the hysteresis loops as type H3. According to the IUPAC recommendations, the type IV isotherms are given by mesoporous adsorbents. The result is attributed to the mesoporous structure of ZnO and it is in agreement with the previous study [21]. Meanwhile, ZnO recorded the smallest specific surface area (28.11 m2 /g) with pore volume and pore diameter of 0.0674 cm3 /g and 9.59 nm, respectively. In contrast, Co–ZnO exhibits a specific surface area of 35.05 m2 /g followed by pore volume and pore diameter of 0.0452 cm3 /g and 5.12 nm, respectively. However, Ni–ZnO recorded specific surface area, pore volume, and pore diameter of 91.09 m2 /g, 0.0680 cm3 /g, and 2.99 nm, respectively.

Fig. 2 Adsorption–desorption isotherms of ZnO, Co–ZnO and Ni–ZnO

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The properties like optical and catalysis of the pure ZnO, Co–ZnO, and Ni– ZnO can be discussed from the specific surface area results. It can be seen that Ni– ZnO has the largest surface area, which means that it would provide more reaction and adsorption sites for the photocatalytic processes by improving the transport of charge carriers on its surface [22]. However, it was observed that the smaller pore diameter of Ni–ZnO could limit the charge carriers’ transport on the surface, reducing the photocatalytic degradation of methylene blue (MB). Meanwhile, the value of the pore diameter of ZnO is too large, which subsequently decreases the surface area available for charge carriers’ transport. Therefore, it was proposed that Co–ZnO has an appropriate surface area and pore diameter ratio that could facilitate the photodegradation of MB. Lower pore volume of Co–ZnO is also believed to contribute to stable rate of the adsorption of MB during for photocatalysis.

3.2 Morphological Study The morphology, shape, and distribution of the ZnO, Co–ZnO and Ni–ZnO was investigated using SEM. Figure 3a shows the morphology of ZnO where the sample exhibits irregular nano-grain distribution with diameters between 180–472 nm consisting of tightly packed sphere and ellipsoidal particles. Meanwhile, Fig. 3b illustrates the heterostructures of quasi-spherical and rod-shaped surface morphologies that result from doping Co ions to ZnO. It is noteworthy that by doping, the particle size has changed and larger nanorods have been obtained. The diameters between nanostructured systems in the form of nanorods were between 410 and 506 nm. On the other hand, Fig. 3c shows that the Ni–ZnO particles have diameters in the range of 261–1266 nm. The compositional analysis of all samples was confirmed with EDX analysis and the results show the existence of elements Zn, Ni, Co and O. It can be concluded that dopant materials (Co and Ni) concentrations are gradually increasing in the primary nuclei of ZnO.

3.3 Optical Analysis The band gap energies of ZnO, Co–ZnO and Ni–ZnO were calculated from absorption spectra using Tauc’s equation as shown in Eq. (2). The ZnO is classified under direct band gap semiconductor because of its large exciton binding energy. When Co and Ni were doped into ZnO, the optical energy gap, Eg was found to be significantly reduced. The drop in Eg is attributed to a band edge shift brought on by doping. There is an increased of sp-d interactions between band electrons and localized d-electrons of dopant ions substituting the Zn2+ ions. The decrease in band gap energy and the electronic transition of dopant materials detected were proof that Ni and Co were incorporated into the ZnO lattice. Figure 4 shows that ZnO has a bandgap value, Eg of 3.11 eV, which is in agreement with the values reported by previous study [23]. On

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Fig. 3 Surface morphology and elemental composition of a ZnO, b Co–ZnO and c Ni–ZnO

the other hand, the Co-ZnO and Ni-ZnO samples show heterojunction characteristics in their energy band gap i.e., Eg1 and Eg2 due to the interface between two regions of dissimilar semiconductors of unequal band gap. It is also suggested that the energy band gap values differ due to the crystalline and amorphous structures of ZnO and dopants as shown in XRD results. Besides that, the reduction in the band gap energy to 2.98 eV and 3.02 eV for Co–ZnO and Ni–ZnO, respectively is in accordance with the structural results which caused the decrease in quantum confinement as particle size increases (with addition of Co and Ni dopants). Additionally, the doping process improves the efficiency of the development of nano heterojunctions on the catalyst surface improves the separation of charge carriers.

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Fig. 4 Tauc’s plot for direct band gap energies for ZnO, Co–ZnO and Ni–ZnO

3.4 Photocatalytic Activity Test Figure 5 shows the comparison of UV–visible absorption spectra of an aqueous solution of 10 mM MB dye with photocatalysts Co–ZnO and Ni–ZnO under irradiation with UV light for duration of 30 min. For better comparison on the effect for each dopant, the pure ZnO absorbance data is recorded in Appendix 1. The characteristic absorption peak of MB at approximately 664 nm is monitored as a function of catalyst concentration (10 mg/ml, 30 mg/ml and 50 mg/ml). From the result, it can be seen that MB is degraded after irradiation of 30 min consisting Co–ZnO and Ni– ZnO photocatalyst. Interestingly, Co–ZnO shows better photodegradation at lower concentration (10 mg/ml and 30 mg/ml) indicating the effectiveness of catalyst as compared to Ni–ZnO (which need 50 mg/ml). It is suggested that the formation of Co–O–H has facilitate the photocatalysis mechanism. Equation 3 elaborate the mechanisms when UV light irradiate the MB with the photocatalyst samples. The MB was adsorbed onto the Co–ZnO and Ni–ZnO nanostructures which lead to the generation of electron–hole (e— h+ ) pairs in ZnO. Meanwhile, Eq. 4 shows the photogenerated electrons in the conduction band of ZnO interact with the oxygen molecules adsorbed on ZnO to form superoxide anion radicals. Finally, the reactive hydroxyl radicals and superoxide radicals react with MB dye adsorbed on ZnO nanostructures and lead to its degradation resulting in its colourless form as shown in Eq. 5–7. ZnO + hv → e− (CB) + h + (VB)

(3)

e− + O2− → (·O2− )

(4)

h + + OH− → ·OH

(5)

·OH + organic dye → degradation products

(6)

·O2− + organic dye → degradation products

(7)

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Fig. 5 Photocatalytic degradation of MB for ZnO, Co–ZnO and Ni–ZnO

For better insight, the UV–Vis spectra for pure ZnO presented in Appendix 1 (Fig. 6) shows that when the concentration of ZnO photocatalyst increase, the MB was degraded accordingly. The photocatalytic degradation of an organic dye involves adsorption of the dye onto the surface of ZnO similar to the abovementioned mechanism.

4 Conclusion Through the sol–gel approach, ZnO, Co-ZnO and Ni–ZnO nanomaterials have been created for the intention of MB degradation. High photodegradation of MB dye was achieved by 0.3 g catalyst Co–ZnO due to the formation of Co–O–H in the ZnO crystal structure. The shift in crystallinity that happened in the ZnO thin films with the Co doping may be responsible for these photocatalytic effects. Besides, Co–ZnO exhibits appropriate surface area and pore diameter ratio with lower pore volume successfully contribute to a stable rate of the adsorption of MB during for photocatalysis. It is also revealed that energy band gap, Eg for Co–ZnO is lower as compared to Ni–ZnO at 2.98 eV and 3.02 eV, respectively. The results confirmed a decrease in the quantum confinement caused by the rise in particle size due to the interaction between ZnO and Co nanoparticles. Also, the work revealed that degradation of MB was successfully achieved by Co–ZnO at 30 min of irradiation time, which can be a breakthrough for future modification of the structure over the photocatalytic activity. Acknowledgements The authors would like to acknowledge the facilities and funding provided by the Universiti Malaysia Pahang for the final year project and in the form of grant RDU220311.

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Fig. 6 Photocatalytic degradation of MB for ZnO

Appendix 1 Photocatalytic Activity Test for Pure ZnO References 1. Khan SH, Pathak B (2020) Zinc oxide based photocatalytic degradation of persistent pesticides: A comprehensive review. Environ Nanotechnol Monit Manag 13:100290. https://doi.org/10. 1016/j.enmm.2020.100290 2. Dihom HR, Al-Shaibani MM, Mohamed RMSR, Al-Gheethi AA, Sharma A, Khamidun MHB (2022) Photocatalytic degradation of disperse azo dyes in textile wastewater using green zinc oxide nanoparticles synthesized in plant extract: a critical review. J Water Process Eng 47:102705. https://doi.org/10.1016/j.jwpe.2022.102705 3. Shafi MA, Bouich A, Fradi K, Guaita JM, Khan L, Mari B (2022) Effect of deposition cycles on the properties of ZnO thin films deposited by spin coating method for CZTS-based solar cells. Optik 258:168854. https://doi.org/10.1016/j.ijleo.2022.168854 4. Smaoui S, Chérif I, Hlima HB, Khan MU, Rebezov M, Thiruvengadam M, Lorenzo JM (2023) Zinc oxide nanoparticles in meat packaging: a systematic review of recent literature. Food Packaging and Shelf Life 36:101045. https://doi.org/10.1016/j.fpsl.2023.101045 5. Salinas RA, Orduña-Díaz A, Obregon-Hinostroza O, Dominguez MA (2022) Biosensors based on zinc oxide thin-film transistors using recyclable plastic substrates as an alternative for realtime pathogen detection. Talanta 237:122970. https://doi.org/10.1016/j.talanta.2021.122970 6. Ta¸sdemir A, Akman N, Akkaya A, Aydın R, Sahin ¸ B (2022) Green and cost-effective synthesis of zinc oxide thin films by L-ascorbic acid (AA) and their potential for electronics and antibacterial applications. Ceram Int 48(7):10164–10173. https://doi.org/10.1016/j.ceramint. 2021.12.228 7. Okeke IS, Agwu KK, Ubachukwu AA, Ezema FI (2022) Influence of transition metal doping on physiochemical and antibacterial properties of ZnO nanoparticles: a review. Appl Surf Sci Adv 8:100227. https://doi.org/10.1016/j.apsadv.2022.100227 8. Benrezgua E, Deghfel B, Zoukel A, Basirun WJ, Amari R, Boukhari A, Mohamad AA (2022) Synthesis and properties of copper doped zinc oxide thin films by sol-gel, spin coating and dipping: a characterization review. J Mo Struct 1267:133639. https://doi.org/10.1016/j.mol struc.2022.133639 9. Selvanayaki R, Rameshbabu M, Muthupandi S, Razia M, Florence SS, Ravichandran K, Prabha K (2022) Structural, optical and electrical conductivity studies of pure and Fe doped ZincOxide

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18. 19.

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A. N. A. Hussin et al. (ZnO) nanoparticles. Mater Today Proc 49:2628–2631. https://doi.org/10.1016/j.matpr.2021. 08.045 Sharma D, Jha R (2017) Transition metal (Co, Mn) co-doped ZnO nanoparticles: effect on structural and optical properties. J Alloy Compd 698:532–538. https://doi.org/10.1016/j.jal lcom.2016.12.227 Saleem S, Jameel MH, Akhtar N, Nazir N, Ali A, Zaman A, Althubeiti K (2022) Modification in structural, optical, morphological, and electrical properties of zinc oxide (ZnO) nanoparticles (NPs) by metal (Ni, Co) dopants for electronic device applications. Arab J Chem 15(1):103518. https://doi.org/10.1016/j.arabjc.2021.103518 Kuriakose S, Satpati B, Mohapatra S (2014) Enhanced photocatalytic activity of Co doped ZnO nano disks and nanorods prepared by a facile wet chemical method. Phys Chem Chem Phys 16(25):12741–12749. https://doi.org/10.1039/C4CP01315H Isai KA, Shrivastava VS (2019) Photocatalytic degradation of methylene blue using ZnO and 2% Fe–ZnO semiconductor nanomaterials synthesized by sol–gel method: a comparative study. SN Appl Sci 1:1–11. https://doi.org/10.1007/s42452-019-1279-5 Amit Kumar S (2012) A comparative analysis of structural, optical and photocatalytic properties of ZnO and Ni doped ZnO nanospheres prepared by sol gel method. Adv Mater Lett 3(4):350– 354. https://doi.org/10.5185/amlett.2012.5344 Mohan AC, Renjanadevi BJPT (2016) Preparation of zinc oxide nanoparticles and its characterization using scanning electron microscopy (SEM) and X-ray diffraction (XRD). Procedia Technol 24:761–766. https://doi.org/10.1016/j.protcy.2016.05.078 Hammad TM, Salem JK, Harrison RG (2013) Structure, optical properties and synthesis of Co-doped ZnO superstructures. Appl Nanosci 3:133–139 Al-Ariki S, Yahya NA, Al-A’nsi SAA, Jumali MH, Jannah AN, Abd-Shukor R (2021) Synthesis and comparative study on the structural and optical properties of ZnO doped with Ni and Ag nanopowders fabricated by sol gel technique. Sci Rep 11(1):11948 Thangeeswari T, George AT, Kumar AA (2016) Optical properties and FTIR studies of cobalt doped ZnO nanoparticles by simple solution method. Indian J Sci Technol 9(1):4 Sharma AK, Desnavi S, Dixit C, Varshney U, Sharma A (2015) Extraction of nickel nanoparticles from electroplating waste and their application in production of bio-diesel from biowaste. Int J Chem Eng Appl 6(3):156 Justine M, Prabu HJ, Johnson I, Raj DMA, Sundaram SJ, Kaviyarasu K (2021) Synthesis and characterizations studies of ZnO and ZnO-SiO2 nanocomposite for biodiesel applications. Mater Today Proc 36:440–446 Kołodziejczak-Radzimska A, Markiewicz E, Jesionowski T (2012) Structural characterisation of ZnO particles obtained by the emulsion precipitation method. J Nanomater 2012:15–15 Torres-Martínez LM, Cruz-López A, Juárez-Ramírez I, Meza-de la Rosa ME (2009) Methylene blue degradation by NaTaO3 sol–gel doped with Sm and La. J Hazard Mater 165(1–3):774–779 Hong R, Huang J, He H, Fan Z, Shao J (2005) Influence of different post-treatments on the structure and optical properties of zinc oxide thin films. Appl Surf Sci 242(3–4):346–352

Properties of Kenaf Fibre Filled with Natural Rubber/Thermoplastic Polyurethane Composites Nur Amirah Ayuni Jamaludin, Nurjannah Salim , Nurul Huda Abu Bakar , and Rasidi Roslan

Abstract Due to their advantages over conventional reinforcement materials, natural fibres have recently attracted the attention of scientists and engineers, and the construction of natural fibre composites has been a topic of interest for several years. The use of natural fibres has enabled the creation of composites that are lighter and less expensive than those presently on the market, such as fiberglass-reinforced polymer composites. This study presents the results of an investigation into the effects of alkaline treatment with sodium hydroxide (NaOH) on the properties of kenaf-filled natural rubber (NR) and thermoplastic polyurethane (TPU) composites. The treated kenaf fiber, TPU, and NR were mixed using a single-screw extruder machine. Three sample preparation ratios were prepared: sample 1 (TPU:200 g), sample 2 (TPU:200 g, NR:10 g), and sample 3 (kenaf:10 g, TPU:200 g, NR:10 g). The samples produced were subjected to tensile and impact tests to determine the stress–strain curve for the percentage of elongation and tensile stress values. Sample 1 was found to have the highest Young’s modulus, followed by sample 2. In conclusion, adding natural rubber to kenaf/TPU composites improved their properties of the composites produced. Keywords Kenaf · Natural rubber · Thermoplastic polyurethane · Composites

N. A. A. Jamaludin · N. Salim (B) · N. H. Abu Bakar · R. Roslan Faculty of Industrial Sciences and Technology, Universiti Malaysia Pahang Al-Sultan Abdullah, Lebuh Persiaran Tun Khalil Yaacob, 26300 Kuantan, Pahang, Malaysia e-mail: [email protected] N. Salim · N. H. Abu Bakar · R. Roslan Advanced Intelligent Materials Centre, Universiti Malaysia Pahang Al-Sultan Abdullah, Lebuh Persiaran Tun Khalil Yaacob, 26300 Kuantan, Pahang, Malaysia © The Author(s), under exclusive license to Springer Nature Singapore Pte Ltd. 2024 R. Abd. Aziz et al. (eds.), Intelligent Manufacturing and Mechatronics, Springer Proceedings in Materials 40, https://doi.org/10.1007/978-981-99-9848-7_47

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1 Introduction In a few applications over the last few decades, polymers have largely supplanted traditional metals and minerals. Polymers have advantages over traditional materials, making them viable. Processing simplicity, efficiency, and cost savings of polymers are the main benefits. In most of these applications, fillers and fibers are used to alter the characteristics of polymers to meet the demands of high strength and high modulus. When comparing certain qualities, fiber-reinforced polymers have an advantage over other traditional materials. Due to the advantages, they offer over conventional reinforcement materials, natural fibres have recently attracted the attention of scientists and engineers, and the development of natural fibre composites has been a topic of interest for several years. These natural fibres are inexpensive, have a low density, and possess several distinctive characteristics. In contrast to other reinforcing fibres, these are biodegradable and abrasion resistant. Their properties are comparable to those of other reinforcement fibres, and they are readily available [1]. Natural fibers are advantageous for the environment and economy. Additionally, these natural fibers exhibited excellent mechanical and physical qualities. Owing to their abundant and inexpensive renewable resources, which represent lower maintenance costs, researchers have suggested that natural fibers are more cost-effective in terms of raw materials than synthetic fibers. Natural fibers also have benefits because they neutrally release carbon dioxide (CO2) after their life cycle. As a result, there were no adverse health impacts because the particles were biodegradable and intended for inhalation. Natural fibers have a lower density than conventional materials, making them lighter fibers for polymer composites. Natural fibers, including hemp, jute, sisal, and kenaf, are frequently mixed with conventional petroleum-based polymers, such as polypropylene and polyethylene [2]. Petroleum is a finite resource, and its extraction for manufacturing plastic and composite materials depletes these nonrenewable resources. As petroleum reserves diminish, it is crucial to find alternative materials that are both sustainable and renewable. Plastics have a long decomposition time, often taking hundreds of years to degrade in the environment. This leads to persistent pollution and its accumulation in landfills and ecosystems. Kenaf can be used as a potential alternative to plastic and petroleum-based materials in the production of composites. Kenaf is a fast-growing plant that belongs to the hibiscus family and has been recognized for its high cellulose content, which makes it suitable for various applications including composite materials [3]. Kenaf fibers offer several advantages for composite production. First, they have excellent tensile strength and stiffness, making them suitable as reinforcing matrix materials. Second, kenaf fibers are renewable and biodegradable, which makes them more environmentally friendly than petroleum-based alternatives. Additionally, kenaf has a lower density than most plastics, which can result in weight reduction in the composite structures. In a review of study Ludvíková [4], the annual kenaf species of The Malvaceae family, which is utilized as a source of versatile fiber, is distinguished by its high biomass and rapid development. In comparison to other

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natural fiber-reinforced materials, kenaf is economical and commercially accessible [5]. Due to its importance in the production of industrial raw materials, kenaf is commonly known as industrial kenaf. Glass, aramid, and carbon fibres are examples of synthetic fibres used to reinforce thermoplastic polyurethane (TPU). The three most important characteristics of thermoplastic polyurethane are its high abrasion resistance, superior mechanical properties with rubber-like flexibility, and tear resistance. Polyols and isocyanates are two of polyurethane’s primary components [5]. High abrasion resistance, excellent mechanical qualities with rubber-like elasticity, and tear resistance are the three most important characteristics of thermoplastic polyurethane [6]. Abdullah [7] stated that additional reinforcements or blends can be used to enhance the performance of TPU and expand the potential uses of the composite. Additionally, composites address environmental concerns owing to their eco-friendliness, recyclability, and biocompatibility. Natural rubber is frequently utilized in a wide range of applications, including gloves, machinery components, and tire treads. It is frequently used in applications where resistance to abrasion, wear, and erosion is necessary, as well as resistance to electromagnetic fields and damping or shock-absorption properties. By combining natural rubber with other rubber materials, the rubber industry often enhances their properties and expands the applications of other rubber materials. Currently, there is much information on the manufacturing of kenaf fibers reinforced with TPU [5–8]. However, there are very few studies on the use of natural rubber as a filler in kenaf/TPU fiber-reinforced composites. Therefore, in this study, the characteristics of kenaf fibers blended with thermoplastic polyurethane and natural rubber were examined. The impact of NaOH sample preparation on kenaf fiber-filled TPU-NR composites was evaluated using physical and mechanical analyses. The incorporation of natural rubber in kenaf/TPU-reinforced composites is expected to improve their properties.

2 Methodology 2.1 Sample Preparation The formulation of the composite ratios is presented in Table 1. Kenaf fibres were treated by soaking them in a 6% sodium hydroxide (NaOH) solution for 24 h. The treated kenaf fibers were then cleaned and allowed to dry for Table 1 The formulation of kenaf-filled TPU-NR composites

Samples

TPU (g)

Kenaf (g)

Natural rubber (g)

Sample 1

200

–

–

Sample 2

200

10

–

Sample 3

200

10

10

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24 h at 100 0 C. Thermoplastic polyurethane (TPU) was then placed in the extruder to prepare sample 1. Similar to sample 2, the combined TPU and kenaf composites were ground into tiny cube-shaped particles and placed into the extruder. Sample 3 involved the addition of TPU, NR, and kenaf to the extruder at 180 0 C. The 40-tonne hot press equipment was used to press three of the samples, which were then molded into sample boards with dimensions of 3 mm × 150 mm × 150 mm. The sample board was prepared and cut according to the specifications of the testing specimen.

2.2 Tensile Test Throughout tensile testing, the samples were measured under a forceful pulling force. To determine the tensile strengths of the 3D-printed samples, tests were conducted. The tensile tests were conducted in accordance with ASTM D638. A Universal Testing Machine with a constant crosshead speed of 5 mm/min and a 10-kN stress test was used to conduct the test. Utilizing the stress–strain curve, the percentages of elongation and tensile stress values were calculated.

2.3 Impact Test Experiments were conducted to determine the effects of fibre orientation and length on the impact resistance of these composites. The impact resistance of the manufactured composites was evaluated in accordance with ASTM standards. The experimental results demonstrated the composites’ significant impact on the impact strength. By incorporating reinforcements comprised of kenaf fibres with a specific orientation, the impact strength can be substantially increased.

2.4 Water Absorption Ten samples with dimensions of 20 mm × 20 mm × 3 mm were fabricated from composite materials in accordance with ASTM D570. Ten samples of each type of composite were prepared to measure the thickness swelling. All samples underwent a 24-h, 60 °C oven-drying procedure. After drying in an oven, samples were cooled in desiccators containing silica gel granules before water absorption testing. A water absorption test was conducted on the samples by immersing them in distilled water for seven days. The weight gain compared to the sample’s initial oven-dry weight was then recorded. The weight was determined using a weighing instrument. In a controlled environment, three samples of every formulation were evaluated (50% RH). The following was manually computed for water absorption:

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Water Absorption Percentage(%) =

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W2 − W1 × 100% W1

where; W1 = Weight of sample before soaking W2 = Weight of sample after soaking.

2.5 Determination of the Density The composite was cut into squares of dimensions 10 mm × 10 mm × 3 mm. Using sandpaper with a grit of 1200, a smooth and glossy surface was created on a square solid piece. Using a densimeter XS205 Mettler Toledo balance, the developed composite’s density was determined in accordance with ASTM D792. The test consisted of five samples of each ratio. The readings of density were then logged. The density is determined with the following formula: Density(ρ) =

Mass(m) V olume(v)

2.6 Scanning Electron Microscopy (SEM) Using scanning electron microscopy (SEM), the surfaces of the kenaf fibres and their attachment to the matrix were examined. All outcomes were compared to the results of the samples. It was determined the modulus, tensile strength, elongation at break, hardness, resilience, and water absorption. The SEM analysis of the fibres revealed surface modifications caused by chemical treatment.

2.7 Differential Scanning Calorimetry (DSC) This test was conducted to determine the decrease in crystallinity and thermal composition of the composites. Differential scanning calorimetry (DSC) was carried out between 30 and 500 °C at a heating rate of 10 °C/min. The glass transition temperature (Tg), thermal stability, melting temperature, and heat capacity of kenaf containing TPU-NR were determined. A composite weighing between 1 and 5 mg was placed in the crucible, and the DSC curve of heat flow versus temperature was determined.

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3 Results and Discussions 3.1 Tensile Properties Tensile characteristics refer to the ability of a material to resist tension pressure. They provide information on the elastic limit, elongation, proportional limit, area decrease, tensile strength, yield point, and other properties. Figure 1 shows the tensile strength results for samples 1 (TPU), 2 (TPU and kenaf), and 3 (TPU, kenaf, NR). Sample 3 achieved the highest tensile strength at 5.43 × 10–5 MPa, followed by sample 1 at 2.917 × 10–5 MPa and sample 2 at 1.95 × 10–5 MPa. Natural rubber was added to TPU and kenaf, which increased sample 3’s tensile strength. This enhances the mechanical properties of the material, including its tensile strength, impact resistance, and elongation. The increase in tensile strength of kenaf fibres is attributable to their alkaline treatment. Through the destruction of hydrogen bonds, the elimination of impurities, and the depolymerization of cellulose, the alkaline treatment improves the interfacial bonding and overall strength of fibres, indicating an increase in the fibres’ stiffness or rigidity. High interfacial roughness and enhanced fibre integrity result in increased load transfer and deformation resistance. Natural rubber is a toughening agent that reduces brittleness and enhances energy absorption capacity [9]. Figure 2 shows the Young’s modulus results for the TPU, Kenaf, and NR samples, with 74.33 MPa, 45.84 MPa, and 73.57 MPa, respectively. The Young’s modulus of the TPU-kenaf composite lower than that of pure TPU. Natural fibers such as kenaf reduce the stiffness of the composite [9]. The reduction in Young’s modulus of composite materials depends on the fiber intake and other elements. TPU has a higher Young’s modulus but adding it to a composite made of kenaf fibers may reduce it, as natural fibers are less stiff. However, the tensile modulus of sample 3 slightly increases to 73.57 MPa. To increase the composite material’s strength and stiffness, reinforcements can be added; however, the exact effect depends on factors such as fibre number, orientation, and matrix material compatibility. The strengthening of the fiber–matrix interface enables efficient stress transmission during flexural loading, resulting in a substantial increase in flexural strength. The NaOH treatment results in Fig. 1 Tensile strength of TPU, TPU-Kenaf and Kenaf-TPU-NR

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Fig. 2 Young’s modulus of TPU, TPU-Kenaf, and TPU-Kenaf-NR

morphological changes to the morphology of kenaf fibres. Increased surface roughness and the exposure of more active spots on the fibre surface result in an increase in the fibre’s mechanical interaction with the matrix. The discovered morphological changes are a significant contributor to the increased flexural strength of the composite material [5].

3.2 Izod Impact Properties The impact strength results show that sample 2 (TPU Kenaf) had the highest impact strength, with an impact strength of 0.423 kJ/m2 , as shown in Fig. 3. Kenaf fibres in the TPU matrix provide extra support, distributing stress, and preventing cracks from spreading. This enhanced load transmission prevents delamination or debonding during impact [10]. The impact strength of sample 3 (TPU Kenaf NR) decreased slightly to 0.423 kJ/m2 compared to that of sample 2. This is because of the different chemical structures of natural rubber and TPU, which may limit their compatibility. Phase separation within a mixture can weaken the material and reduce its impact resistance. The TPU has the lowest impact strength (0.39 kJ/m2 ) and can have different degrees of stiffness and hardness. TPUs with higher hardness or stiffness often have less impact strength because they are stiffer, tougher, and more likely to fracture or shatter during impacts or pressures [11].

3.3 Determination of Density Test The density of the treated kenaf-filled TPU-NR polymer composites increased with increasing TPU composition. Sample 1 had a density of 1.47 g/cm3 , while TPUKenaf had 1.67 g/cm3 and TPU-Kenaf-NR had 1.83 g/cm3 . Sample 3 had the highest density owing to its natural rubber (NR) content, indicating a higher specific gravity. The interfacial bonding between TPU and kenaf fibers can be improved by adding

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Fig. 3 Impact strengths of TPU, TPU-Kenaf, and TPU-Kenaf-NR

Fig. 4 Density of TPU, TPU-Kenaf, and kenaf filled with TPU-NR

natural rubber, which has a higher density than the TPU-Kenaf composite [12]. Figure 4 shows the results of the density tests for all sample types.

3.4 Water Absorption Test Figure 5 shows that the polymer composites with higher TPU contents had low water absorption. Natural rubber-filled kenaf fibers absorbed more moisture. Kenaf filled with TPU-NR had the highest water absorption compared to TPU alone, while TPUfilled kenaf showed the lowest average water absorption after 7 days of immersion in distilled water. The increased moisture absorption in sample 3 due to the presence of natural fiber and natural rubber in the composite as this will contribute to available hydroxyl group to react with water molecule. Treating a fiber decreases its hydrophilicity and improves the interfacial interaction, preventing water collection. Kenaf treated with 6% OF NaOH solution before drying is polar and hydrophilic, with a significant amount of hydroxyl group present (Table 2).

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Fig. 5 Water absorption of the samples before and after 7 days of immersion in distilled water for TPU, kenaf-filled TPU, and kenaf-filled TPU-NR

Table 2 Average results of all samples before and after immersion in distilled water for 7 days Samples

Before immersed in distilled water (g)

After 7 days immersed in distilled water (g)

TPU

2.138

Kenaf filled TPU

2.380

3.844

Kenaf filled TPU-NR

2.376

11.752

5.419

3.5 Differential Scanning Calorimetry (DSC) The test aimed to determine the chemical and thermal properties of the samples. The results shown in Fig. 6 and Table 3 show the exothermic processes for all types of composites. TPU exhibited peaks at 198.2 and 338.3 °C, while kenaf filled with TPU showed peaks at 213.35 and 335.75 °C. Kenaf fibres can enhance strength and stiffness, altering glass transition temperature and TPU chains’ mobility. Moisture absorbed by kenaf fibers can affect the thermal characteristics of TPU composites, particularly during glass transition. Moisture can act as a plasticizer, reducing the glass transition temperature (Tg) and potentially displacing the peaks. Kenaf filled with TPU and NR had a higher endothermic reaction at 417.4 °C, which was slightly higher than that of TPU (408.69 °C). Natural rubber, with its remarkable elasticity and glass transition behaviour, often has a lower Tg than TPU, as shown in Fig. 6.

3.6 Scanning Electron Microscopy (SEM) SEM was used to examine the characteristics of the kenaf filled with thermoplastics and rubber. Representative SEM images of the surface control samples of TPU,

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Fig. 6 DSC Thermogram of TPU, Kenaf-filled TPU and Kenaf-filled TPU-NR

Table 3 DSC results of TPU, Kenaf filled TPU and Kenaf filled TPU-NR

Sample

T g1 (°C)

T g2 (°C)

T m (°C)

TPU

198.24

338.3

408.69

Kenaf filled TPU

213.35

355.72

417.4

Kenaf filled TPU-NR

211.05

254.1

336.6

Kenaf filled with TPU, and Kenaf filled with TPU and NR are displayed in Fig. 7. From Fig. 7b, c shows the well-blended between TPU, fiber and natural rubber. The enhanced tensile strength, elongation at break, and tensile modulus of the kenaf-filled TPU and NR were a result of good fiber-matrix bonding relationship.

Fig. 7 The magnification of SEM at 2000 × : a TPU, b Kenaf filled with TPU, and c Kenaf filled with TPU and NR

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4 Conclusion The results show that kenaf filled with TPU and NR has the highest tensile strength of 5.43 × 10–5 MPa, compared to TPU alone and 1.95 × 10– 5 MPa. When kenaf and TPU were treated, the tensile modulus decreased, and the impact strength increased. The densities of TPU, kenaf filled with TPU, and kenaf filled with TPU-NR increased. The water absorption test showed increased moisture absorption owing to the presence of kenaf and TPU. The thickness swelling in TPU, kenaf filled with TPU, and TPU-NR composites increased by 25%. DSC studies showed that kenaf filled with TPU and NR had the lowest glass transition temperature (Tg) and endothermic reaction (336.6 °C), indicating that the elasticity of natural rubber has less glass transition behavior than TPU alone. However, moisture behavior in kenaf increased the endothermic reaction at 417.4 °C. The results demonstrate that as additional fibres were added and additional of NR, the effective transmission of stress during testing improved, leading to increased tensile strength, elongation at break, and tensile modulus in kenaf-filled TPU and NR. Acknowledgements The authors would like to thank Universiti Malaysia Pahang Al-Sultan Abdullah for providing laboratory space and additional funding under the Internal Fundamental Research grant RDU200340.

References 1. Saheb DN, Jog JP (1999) Natural fiber polymer composites: a review. Adv Polym Technol J Polym Process Inst 18(4):351–363 2. Akil H, Omar MF, Mazuki AM, Safiee SZAM, Ishak ZM, Bakar AA (2011) Kenaf fiber reinforced composites: a review. Mater Des 32(8–9):4107–4121 3. El-Shekeil YA, Sapuan SM, Abdan K, Zainudin ES (2012) Influence of fiber content on the mechanical and thermal properties of Kenaf fiber reinforced thermoplastic polyurethane composites. Mater Des 40:299–303 4. Ludvíková M, Griga M (2019) Transgenic fiber crops for phytoremediation of metals and metalloids. In: Transgenic plant technology for remediation of toxic metals and metalloids. Academic Press, pp 341–358 5. Saba N, Paridah MT, Jawaid M (2015) Mechanical properties of kenaf fibre reinforced polymer composite: a review. Constr Build Mater 76:87–96 6. Akhtar MN, Sulong AB, Radzi MF, Ismail NF, Raza MR, Muhamad N, Khan MA (2016) Influence of alkaline treatment and fiber loading on the physical and mechanical properties of kenaf/polypropylene composites for variety of applications. Prog Nat Sci Mater Int 26(6):657– 664 7. Abdullah NS, Salim N, Roslan R (2022) Properties of seaweed fiber reinforced polypropylene composite: effect of alkaline treatment. In: Macromolecular symposia, vol 402, no 1, p 2100448 8. Khalifa M, Anandhan S, Wuzella G, Lammer H, Mahendran AR (2020) Thermoplastic polyurethane composites reinforced with renewable and sustainable fillers–a review. Polym Plast Technol Mater 59(16):1751–1769 9. Salehudiin NM, Salim N, Roslan R, Bakar NHA, Sarmin SN (2023) Improving the properties of kenaf reinforced polypropylene composite by alkaline treatment. Mater Today Proc 75:156–162

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10. Ahmad Nadzri SNZ, Hameed Sultan MT, Md Shah AU, Safri SNA, Basri AA (2020) A review on the kenaf/glass hybrid composites with limitations on mechanical and low velocity impact properties. Polymers 12(6):1285 11. Noor Azammi AM, Sapuan SM, Ishak MR, Sultan MTH (2018) Mechanical and thermal properties of kenaf reinforced thermoplastic polyurethane (TPU)-natural rubber (NR) composites. Fibers Polym 19:446–451 12. PoomalaiSiddaramaiah P (2005) Studies on poly (methyl methacrylate) (PMMA) and thermoplastic polyurethane (TPU) blends. J Macromol Sci Part A Pure Appl Chem 42(10):1399–1407 13. Bondan AT (2019) Natural rubber composites for solid tyre used for forklift tensile properties and morphological characteristics. J Phys Conf Ser 1282(1):012061 14. Manaila E, Craciun G, Ighigeanu D (2020) Water absorption kinetics in natural rubber composites reinforced with natural fibers processed by electron beam irradiation. Polymers 12(11):2437

State-of-the-Art Developments and Perspectives on Multifunctional Magnetic Soft Composites (MMSCs) Ahmad Shahir Jamaludin, Nurul Najwa, Mohd Zairulnizam Mohd Zawawi, Ahmad Rosli Abdul Manaf, and Roshaliza Hamidon

Abstract The field of material science and engineering has seen a growing interest in Multifunctional Magnetic Soft Composites (MMSCs) due to their unique magnetic properties, flexibility, and diverse range of functionalities. These composite materials, which possess magnetic responsiveness and adaptability, have been utilized in various fields such as soft robotics and biomedical advancements. Significantly, the incorporation of MMSCs into soft robotic systems has facilitated the ability to navigate complex environments and perform precise object manipulation, thereby surpassing the capabilities exhibited by conventional rigid robots. Moreover, MMSCs have demonstrated potential in various biomedical applications, such as drug delivery systems, medical textiles, and targeted therapies. The progress in fabrication techniques, such as 3D printing, and the integration of novel insulating layers have significantly advanced research on MMSCs, leading to improvements in their characteristics and expanding their range of potential applications. Nevertheless, notwithstanding these notable progressions, there exist certain lacunae in the research, specifically pertaining to the comprehension of time-dependent electric conductivity of MMSCs in high-electric fields and the investigation of symmetry-breaking actuation mechanisms. By addressing these knowledge deficiencies and effectively utilizing the untapped potential of MMSCs in unexplored areas such as high-voltage systems and diverse biomedical applications, there is a possibility of significantly transforming their influence in multiple sectors. Future research endeavors should give priority to these areas, in order to ensure the ongoing evolution of MMSCs and their crucial role in shaping technological advancements.

A. S. Jamaludin (B) · N. Najwa · M. Z. Mohd Zawawi · A. R. Abdul Manaf Faculty of Manufacturing and Mechatronic Engineering Technology, Universiti Malaysia Pahang Al-Sultan Abdullah, 26600 Pekan, Pahang, Malaysia e-mail: [email protected] R. Hamidon Faculty of Mechanical Engineering and Technology, Universiti Malaysia Perlis, Pauh Putra Campus, 02600 Arau, Perlis, Malaysia © The Author(s), under exclusive license to Springer Nature Singapore Pte Ltd. 2024 R. Abd. Aziz et al. (eds.), Intelligent Manufacturing and Mechatronics, Springer Proceedings in Materials 40, https://doi.org/10.1007/978-981-99-9848-7_48

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Keywords Multifunctional magnetic soft composites · Soft robotics · Micro-electromechanical systems · Biomedical applications · Magnetization profiles

1 Introduction to Multifunctional Magnetic Soft Composites Multifunctional Magnetic Soft Composites (MMSCs) have garnered attention in material science and engineering due to their unique magnetic properties, flexibility, and diverse functionalities [1–15]. The magnetic properties of these composites distinguish them. Their versatility goes beyond magnetism, making them essential in many applications [8–19]. MMSCs’ magnetic properties define them [20–35]. The ability to regulate these characteristics in response to a magnetic field has many applications [36–50]. The use of MMSCs in sensing applications is important. These magnetic sensors detect and measure magnetic changes [6–8]. The subject’s magnetic properties also affect actuation. Actuators use MMSCs’ magnetic properties to move precisely [51–56]. The actuators use calibrated magnetic fields to control responses, making them ideal for precise adjustments [22, 39, 44, 56]. Magnetism is only one aspect of MMSCs. The softness of these materials gives them an advantage over conventional magnetic materials. The malleability of this characteristic allows for new applications, especially in soft robotics, which is rapidly evolving. MMSC-equipped soft robots can navigate complex environments, adapt to different terrains, and manipulate delicate objects with greater precision than rigid robots. The scientific community has been fascinated by the above attributes, leading to extensive research and advancement. Citations show that many studies have investigated the incorporation of MMSCs into soft robotic systems [1, 4, 11, 14, 22]. In addition to robotics, MMSCs have biomedical applications. Programmable shape-changing materials and their adaptability have applications in drug delivery systems, medical textiles, and targeted cancer therapies [23, 28, 56]. Magnetically responsive mesenchymal stem cells (MMSCs) can undergo morphological changes in response to external stimuli, particularly magnetic fields, making them ideal for these functions. Materials and fabrication methods used to develop MMSCs are diverse and evolving. 3D printing technologies [2, 19, 29, 35], innovative insulating layers [3, 10, 16, 34, 35], and magnetic inks and fillers [7, 9, 17, 33] are driving MMSC development. These advances improve attributes and enable more complex, versatile systems. The purpose of this review paper is to thoroughly examine MMSC research and advances. This review will discuss the significance of MMSCs, recent research advances, challenges and future directions in this field.

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2 Innovations in Soft Multi-material Magnetic Fibers Soft magnetic materials play a pivotal role in micro-electromechanical systems (MEMS) and various other technological advancements. These materials, characterized by their ease of magnetization and demagnetization, provide a foundational component for the development of a broad spectrum of devices. Magnetic Sensors: Soft magnetic materials in sensors enable the measurement of alterations in magnetic fields. This change is then translated into usable data, often providing real-time feedback in diverse applications from automotive systems to consumer electronics [2–16]. i. Actuators: These devices capitalize on the properties of soft magnetic materials to transform energy into motion. Controlled by the magnetic field’s influence, actuators find uses in everything from medical devices to industrial machinery. Advances in 3D printing techniques have further elevated their potential. For instance, research investigating the morphology and magneto-mechanical properties of 3D printed materials found that magnetic properties can vary based on nozzle diameter and material composition, a vital insight for customized actuation [2]. ii. Energy Harvesters: Energy harvesters exploit soft magnetic materials to convert magnetic energy into electrical energy. The efficiency and capacity of these devices can determine their application, from powering small electronic devices to contributing to larger energy grids [16]. iii. Soft Magnetic Composites (SMCs): These are evolving as pivotal components in the MEMS landscape. For instance, a study on SiCNFe ceramics, doped with iron, highlighted their potential as effective soft magnetic materials for MEMS devices [9]. This ceramic not only exhibits impressive magnetic properties but also has a diverse application range, including magnetic sensors and energy harvesters. Soft Multi-Material Magnetic Fibers: Bridging Wearable Tech and Soft Robotics Soft multi-material magnetic fibers have advanced wearable tech and soft robotics. Wearable electronics and soft robotics could use the intricate fibers’ magnetic field-responsive designs, as shown in Fig. 1. Textiles can be seamlessly integrated with these fibers, improving wearable technology. These sensors can monitor body temperature and environmental changes in garments. These garments’ actuation can be used to make self-adjusting clothing and footwear [11]. However, these fibers offer a novel soft robotics solution to rigid robotic system issues. These fibers make soft robots suitable for medical devices and search and rescue missions due to their adaptability, flexibility, and resilience. Fibers can deform over 1000% and lift 370 times their weight [11]. High accuracy in fiber production, even with 300 µm diameters, enables intricate robotic systems [11]. Fashion that changes shape or color in response to a magnetic field and remotely adjustable medical bandages can be made from these novel magnetic textiles [11]. Materials science and engineering progress

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Fabric respond to magnetic field 1

Core: MRE 20 Cladding: Genioplast

H field Magnetic domain design Robotic prosthesis Fig. 1 Soft multi-material magnetic fibers as wearable robotic [11]

connect wearable tech and soft robotics in these objects, as these fibers are versatile and multifunctional [11]. Digitally Printable Magnetic Liquid Metal Composite for Recyclable Soft-Matter Electronics Advanced soft-matter electronics make printable magnetic liquid metal composites. This novel composite has high electrical conductivity, fluidity, and magnetic sensitivity due to liquid metals and magnetic particles. The composite material was developed to make recyclable soft-matter electronics [12]. It reduces electronic waste and offers a sustainable alternative to conventional electronics. Digital printing is possible with this composite. It allows customized electronic devices to fit different shapes and surfaces. Wearable and flexible electronics are growing fast, so adaptability is key. Manufacturing has changed with printable biphasic liquid metal composites. Nickel replaces expensive silver particles, making the material cheaper and more effective [12]. This composite material’s stretchable circuits and magnetic switches expand its uses. This composite material allows magnetism in pliable materials [12]. Magnetically responsive soft materials for soft robotics and biomedical devices [1] and integrated magnetic fibers for soft robotics and medical textiles [11] demonstrate magnetic property integration into soft materials. The magnetic liquid metal composite integrates these realms to solve modern electronic problems. Finally, magnetic liquid metal composites improve soft-matter electronics. The material’s unique properties and digital printing ability make it ideal for wearable and flexible electronics.

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3 Enhancing Performance of Soft Magnetic Composites Soft magnetic composites (SMCs) are pivotal in the realm of electronics and magnetism, offering unique properties that are essential for a myriad of applications. The magnetic characteristics and thermal conductivity of these composites are paramount for their optimal performance. By understanding and manipulating these properties, it the efficiency and functionality of devices that utilize these materials are significantly enhanced.

3.1 Integration of Al2 O3 Insulation Layer Due to their potential use in electric motors, power electronics, and high-frequency devices, soft magnetic composites (SMCs) have garnered research attention in recent years. A pioneering study examined the incorporation of an aluminum oxide (Al2 O3 ) insulating layer into iron-silicon-chromium (FeSiCr) soft magnetic composites (SMCs) [10], as shown in Fig. 2. Sol–gel, a versatile method that produces highquality insulating layers, was used to integrate the layers. The Al2 O3 insulation layer improved FeSiCr SMC magnetic properties. Eddy currents are a major issue for SMCs. A varying magnetic field generates circulating currents in a conductor. These currents may increase thermal generation and power dissipation in the material. The Al2O3 insulation layer reduces eddy current losses and speeds up magnetization and demagnetization [10]. The research also showed that adding Al2 O3 to soft magnetic composites (SMCs) increased their thermal conductivity. Effective heat dissipation is crucial, especially for high-performance composites. The device’s increased thermal conductivity efficiently dissipates heat generated during operation, reducing the risk of damage or performance degradation [10]. Soft magnetic composites (SMCs) are good for electric motors, especially 3D flux SMC motors [28]. The addition of efficient insulation layers like Al2 O3 can improve motor performance, improving electric drive efficiency and sustainability. In conclusion, FeSiCr SMCs with Al2 O3 insulation layers are a Calcined 700°C, high vacuum Argon, 1 hour

Compacted at 1200MPa

toroidal-shaped Fig. 2 Preparation steps of FeSiCr SMCs [10]

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major magnetic material advancement. This study aims to reduce eddy current losses and improve thermal conductivity to enable high-performance magnetic devices and systems.

3.2 Influence of Metal Oxide Insulating Layers The magnetic properties of many materials depend on metal oxide insulating layers. Insulating layers, usually made of aluminum oxide, silicon dioxide, and other compounds, can significantly affect a material’s magnetic properties. These layers change magnetic permeability and coercivity [3]. The ability of a material to generate a magnetic field within its structure is called magnetic permeability. However, coercivity measures the material’s demagnetization resistance. These traits determine a material’s suitability for magnetic sensors, actuators, and energy harvesting devices. The Fe-Si-Cr composite is highly regarded in academia as a soft magnetic material due to its high magnetic permeability and low coercivity. This material is ideal for fast magnetization and demagnetization applications. A comprehensive study examined how metal oxide insulating layers affect Fe-Si-Cr systems’ magnetic properties [3]. The Fe-Si-Cr system’s magnetic properties were greatly affected by these insulating layers. The most effective insulating layer among the metal oxides investigated was zirconium dioxide (ZrO2 ), which had the best magnetic properties, as shown in Fig. 3 [3]. A study examined the use of Aluminum Oxide (Al2 O3 ) as an insulating layer to improve soft magnetic composites (SMCs) [10]. The research found that Al2 O3 insulation coating improved SMC core loss, resistivity, quality factor, and thermal conductivity. This emphasizes the importance of metal oxide insulating layers for magnetic material efficiency. Other metal oxides studied included TiO2 , MgO, and CaO [3]. Each oxide has unique benefits and can be customized for specific applications. Nano-sized SiO2

Fig. 3 Various Fe-Si-Cr soft magnetic core and Fe-Si-Cr/AOx soft magnetic composite cores performance [3]

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and Ni-Zn/Cu-Zn ferrite grains were tested as insulating layers. The study found that ferrite increased magnetic properties [16]. In conclusion, metal oxide insulating layers improve magnetic properties in various materials. Various research studies suggest that strategic measures can help magnetic materials improve performance and application.

4 Research Gaps and Future Directions Despite the remarkable progress in multifunctional magnetic soft composites (MMSCs), there remain several unexplored areas and potential avenues for research. Gaps in Current Research: ● Electrical Properties: While MMSCs have been rigorously analyzed for their mechanical, electrical, and magnetic attributes, there’s a noticeable gap in understanding their time-dependent electric conductivity, especially under high-electric fields. This knowledge is pivotal for MMSCs’ integration into high-voltage systems. ● Actuation Mechanisms: The current body of research on magnetic-responsive composites for soft robotics and active metamaterials is commendable. However, there’s a pressing need to delve deeper into symmetry-breaking actuation mechanisms. Such advancements could exponentially expand MMSCs’ functional capabilities. ● Biomedical Applications: MMSCs have shown promise in specific biomedical applications, like pH and temperature-sensitive drug delivery using magnetic iron oxide incorporated mesenchymal stem cells. Yet, there’s vast potential in other areas like tissue engineering and medical imaging that remains untapped. ● Programmable Magnetization: While some studies have ventured into MMSCs with programmable magnetization profiles, there’s a need to further explore methods to control these profiles. This would allow MMSCs to be more adaptable across diverse tasks and environments. Future Research Recommendations: ● Electric Conductivity Studies: Future endeavors should focus on understanding the time-dependent electric conductivity of MMSCs in high-electric fields. This would necessitate the creation of innovative experimental techniques and models. ● Symmetry-breaking Actuation: Research should be directed towards the development of MMSCs capable of asymmetric actuations, enhancing their versatility in various applications. ● Broadening Biomedical Applications: There’s a vast scope for MMSCs in the biomedical sector. Comprehensive in vitro and in vivo studies should be undertaken to assess the biocompatibility, safety, and effectiveness of MMSCs in diverse medical applications.

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● Advanced Magnetization Techniques: To truly harness the potential of MMSCs, research should be geared towards advanced fabrication methods, like 3D printing and nanofabrication. This would enable the creation of MMSCs with customizable magnetization profiles and geometries. In conclusion, while MMSCs have made significant strides in various domains, there’s still a vast expanse of untapped potential. Addressing the identified gaps and focusing on the recommended areas can pave the way for groundbreaking innovations in this field. Acknowledgements The author wishes to convey heartfelt gratitude to the Ministry of Higher Education for their substantial backing of this study through the Fundamental Research Grant Scheme (FRGS), under the grant number FRGS/1/2022/TK10/UMP/02/57. This research would not have been feasible without their commitment to nurturing academic discovery and innovation. The Universiti Malaysia Pahang Al-Sultan Abdullah is also thanked for their invaluable support and financial aid under the grant RDU Number RDU210365.

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