3D Printing for Energy Applications 1774691019, 9781774691014

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3D Printing for Energy Applications

本书版权归Arcler所有

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3D PRINTING FOR ENERGY APPLICATIONS

Mukesh Pandey

ARCLER

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www.arclerpress.com

3D Printing for Energy Applications Mukesh Pandey

Arcler Press 224 Shoreacres Road Burlington, ON L7L 2H2 Canada www.arclerpress.com Email: [email protected]

e-book Edition 2023 ISBN: 978-1-77469-538-8 (e-book)

This book contains information obtained from highly regarded resources. Reprinted material sources are indicated and copyright remains with the original owners. Copyright for images and other graphics remains with the original owners as indicated. A Wide variety of references are listed. Reasonable efforts have been made to publish reliable data. Authors or Editors or Publishers are not responsible for the accuracy of the information in the published chapters or consequences of their use. The publisher assumes no responsibility for any damage or grievance to the persons or property arising out of the use of any materials, instructions, methods or thoughts in the book. The authors or editors and the publisher have attempted to trace the copyright holders of all material reproduced in this publication and apologize to copyright holders if permission has not been obtained. If any copyright holder has not been acknowledged, please write to us so we may rectify. Notice: Registered trademark of products or corporate names are used only for explanation and identification without intent of infringement.

© 2023 Arcler Press ISBN: 978-1-77469-101-4 (Hardcover)

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ABOUT THE AUTHOR

Prof. Dr. Mukesh Pandey is multi-skilled professional with around 30 years of rich exposure and versatile experience in Industries, Administration, Academics , Research domains and institution building. He received his B.E. from SATI Vidisha, M.Tech. from N.I.T. Bhopal and Ph.D. from RGPV, Bhopal. He played an instrumental role in the establishment of Rajiv Gandhi Technical University Bhopal, Madhya Pradesh since it’s inception in 1999. He served as Rector(Pro Vice Chancellor), Director SoEEM & Dean of Faculty of Energy Technology. He has looked after as Coordinator for establishing IIIT, Bhopal (under PPP Mode by MHRD). He held various administrative positions as Director (R&D), Coordinator of RGPV- NBA Nodal Centre, Dy. Registrar, Member of Engineering Accreditation Evaluation Committee [EAEC] and Moderation Committee of NBA(National Board of Accreditation). Professor Pandey works in the area of Renewable Energy and Environment having focus on Solar Thermal Energy and he has developed an Energy Technology Park at RGPV, Bhopal by making use of the renewable energy resources; Solar Roof Top Plant on University Building, Energy Systems, Solar Thin Film systems, Solar wind Hybrid System, , Bio-Diesel Reactor, CO2 Carbon Sequestration Unit, Dual Rotor Wind Turbine etc. Professor Pandey has an iconic track record of quality teaching, innovation and research he has been Principal Investigator of many Govt. Funded Projects by DST, MNRE, MPCST, AICTE etc including Principal Investigator of Innovative & Breakthrough Technology based 30KW CL-CSP SOLAR international R&D PROJECT (India-Japan Joint Venture Project) installed in RGPV campus. He has also facilitated as Reviewer for many national and international journals of repute and associated with many academic and research organizations at various levels. Over the past several years he has taught M.Tech. and Ph.D. Research Scholars in the areas of Energy, Environment, Direct Energy Conversion and Integrated Energy Systems and has been key-note speaker and resource person at several International and National Conferences and programmes.

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TABLE OF CONTENTS

List of Figures ........................................................................................................xi List of Tables ...................................................................................................... xvii Preface........................................................................ ................................... ....xix Chapter 1

Introduction 3D Printing Technology ....................................................... 1 1.1 Introduction ........................................................................................ 2 1.2 Additive Manufacturing and its Types ................................................... 4 1.3 Ingredients Utilized for Digital Fabrication Technology in Fabricating Industry ...................................................................... 8 1.4 Digital Fabrication’s Usage in Manufacturing Technology ................. 13 References .............................................................................................. 19

Chapter 2

Applications of 3D Printing in Electrochemical Energy Devices .............. 25 2.1 Introduction ....................................................................................... 26 2.2 3D-Printing Electrodes for Applications Using Electrochemical Energy ........................................................................................... 29 2.3 Structure of the Support of 3D-Printed .............................................. 32 2.4 3D-Printed Electrolyzer Devices ........................................................ 42 2.5 Electrochemical Energy Storage and 3D Printing ............................... 45 References ............................................................................................... 61

Chapter 3

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Gas-Phase 3D Printing of Functional Materials ...................................... 75 3.1 Introduction ....................................................................................... 76 3.2 Background and History ................................................................... 78 3.3 Deposition Manifold Head ............................................................... 80 3.4 Sald Aided Digital Fabrication’s Features ............................................ 86 3.5 Future Possibilities and Summary ...................................................... 88 References ............................................................................................... 89

Chapter 4

3D Printing Technology for Solar Cells ................................................... 95 4.1 Introduction ....................................................................................... 96 4.2 Printing Technologies History for Photovoltaic Cells........................... 96 4.3 Three-Dimensional Printing ............................................................... 97 4.4 Photovoltaic Cells Flexibility and There Modules ............................... 98 4.5 Solar Concentrators ......................................................................... 100 4.6 3D Printed Solar Panels.................................................................... 102 4.7 Future Prospects .............................................................................. 105 References ............................................................................................. 107

Chapter 5

3D Printed Components for Flexible Supercapacitors ........................... 111 5.1 Introduction ..................................................................................... 112 5.2 Synthesis Techniques of 3D Printed Capacitor .................................. 114 5.3 3D Printed Supercapacitors Characterization ................................... 115 References ............................................................................................. 123

Chapter 6

Three-Dimensional Printing of Piezoelectric Materials ........................ 127 6.1 Introduction .................................................................................... 128 6.2 Piezoelectric Materials .................................................................... 128 6.3 Poling ............................................................................................. 132 6.4 Mathematical Representation of the Charge Piezoelectric Constant ...................................................................................... 153 6.5 Summary ......................................................................................... 154 Reference ............................................................................................. 155

Chapter 7

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3-D Printing of Rechargable ED Batteries ............................................. 163 7.1 Introduction ..................................................................................... 164 7.2 Three-Dimensional Printing Technology ........................................... 165 7.3 Battery Materials .............................................................................. 169 7.4 Li-Based 3D-Printed Materials For REBS........................................... 173 7.5 Mtal-Based 3D Printed Materials For REBS....................................... 184 7.6 Application of Three-Dimensional Printing Battery ........................... 187 7.7 Package Approaches of Three-Dimensional Printed REBS ................. 191 7.8 Benefits of Three-Dimensional Print Battery ..................................... 193 7.9 Disadvantages of Three-Dimensional Print Battery ........................... 194 References ............................................................................................. 195 viii

Chapter 8

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3D Printed Fuel Cells ............................................................................ 207 8.1 Introduction ..................................................................................... 208 8.2 Dense Thin Electrolytes .................................................................... 213 8.3 High Operating Porous Electrodes and Functional Layers................. 216 8.4 Performance of Full Solid Oxide Fuel Cells ...................................... 217 8.5 Future Prospects .............................................................................. 218 References ............................................................................................. 220 Index ..................................................................................................... 225

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LIST OF FIGURES Figure 1.1. FDM additive manufacturing technology’s graphic diagram Figure 1.2. The procedure of an archetypal way of 3D printing Figure 1.3. Market Segmentation of Additive Manufacturing Items Figure 1.4. A metal fragment that is digitally fabricated Figure 1.5. Items of polymer fashioned through digital fabrication Figure 1.6. Ceramic items made by additive manufacturing Figure 2.1. 3D printing, photolithography, and nanoarchitectonics are examples of electrochemical energy electrode creation and modification processes. Figure 2.2. In the literature, there are numerous structures of electrodes 3D-printed created for splitting of water. Basket shape (A) [Ambrosi & Pumera, 2018]. Mesh shape (B) [Ambrosi & Pumera, 2018]. [Ambrosi et al., 2016] Ribbon form (C). [Foster et al., 2017] (D) Circular form. Springer Nature, 2017. All rights reserved. (E) A void-shaped circular. With permission from ref Browne et al. (2018), reproduced/adapted. American Chemical Society. All rights reserved. (F) The form is square. [Browne et al., 2019] Wiley and Sons, Inc., Wiley and Sons, Inc., Wiley & Sons, Inc (G) Mesh with a square shape. [Su et al., 2019] Figure 2.3. Influence of 3D-printed electrode structure on efficiency of photoelectrochemical. (A) 0 conical arrays, (B) 216 conical arrays, and (C) 407 conical arrays on TiO2Ti electrodes. (D) At the same voltage, photoelectrochemical performance of TiO2Ti-centered electrodes with 0 (black), 217 (blue), and 407 (red) conical arrays. (Gannarapu et al., 2016). Figure 2.4. (A) Diagram of the 3D-printing procedure, from design of electrode to printed electrode modification. (B) IrO2 metal is electrodeposited on the electrode from 3D-printing. (C) Pt metal is electroplated onto the electrode from 3D-printing. (D) Ni metal is electroplated onto the 3 electrode from 3D-printing. (E) LSV curves for water splitting for modified 3D-printed electrodes. (Ambrosi & Pumera, 2018) ALD onto a stainless steel 3D-printed electrode and (G) the ALD procedure. (Browne et al., 2019) (F, G). (H) Microconical arrays electrode design and (I) anodization procedure (Gannarapu et al., 2016) Figure 2.5. (A) Diagram of the 3D-printing procedure, from design of electrode to printed electrode modification. (B) IrO2 metal is electrodeposited on the electrode from 3D-printing. (C) Pt metal is electroplated onto the electrode from 3D-printing. (D) Ni metal is electroplated onto the 3 electrode from 3D-printing. (E) LSV curves for water splitting for modified 3D-printed electrodes. (Ambrosi & Pumera, 2018) ALD onto a

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stainless steel 3D-printed electrode and (G) the ALD procedure. (Browne et al., 2019) (F, G). (H) Microconical arrays electrode design and (I) anodization procedure (Lee et al., 2017) Figure 2.6. Electrolyzer devices made with PEM 3D printing. (A) The PEM electrolyzer device is depicted schematically. (B) Images of a bipolar plate as-printed, (C) a bipolar plate that has been changed with silver paint (D) formation of other silver layer by electrodeposited. (E) I.V. arcs of an electrolyzer with the bipolar plates displayed in panel (D). (AE) (Chisholm et al., 2014) (AE) (AE) (AE) (AE) (FH) Channel structure for bipolar plates from 3D-printing, and (I) IV arcs of electrolyzer devices from 3D-printing constructed with the bipolar plates depicted in panes (FH). (F−I) (Yang et al., 2018) Figure 2.7. Alkaline electrolyzer devices manufactured in 3D. (A-C) FDM and SLM 3D printed alkaline electrolyzer device; (D) LSV arcs in panels for for the electrolyzer device (A-C). (Ambrosi & Pumera, 2018) (A.D.) (E) A FDM-based alkaline electrolyzer device. Electrodes for the electrolyzer in panel (E) made of SLA (F). (G) Electrolyzer device LSV with without and with electrodeposited Ni, the Ti electrodes from panels (E and F). (Hornés et al., 2021) Figure 2.8. (A) Slurry recipe, (B) tape casting, (C) extrusion, and (D) 3D printing are the stages for energy-storage devices from 3D printing using FDM. (Maurel et al., 2020) (E) formulation of materials, (F) generation of printable inks by modifying the rheology, (G) 3D printing, and (H) post-processing are the stages for DIW 3D printing. (EH) (Yang et al., 2019) Figure 2.9. (A) Rate capability of electrodes from 3D printing made up of numerous active materials [106]. (B) Rate capability of electrodes from 3D printing with numerous MnO2 load stackingings. (Zhang et al., 2020). Figure 2.10. Battery constituents 3D-printed in many forms: Ink Writing 3D-printed (A) a current collector, (B) an anode, (C) a cathode, and (D) finished device, as well as (E) the electrochemical response. [123] (AE) (AE) (AE) (AE) (AE) 3D-printed fibre cathode and anode (F), installation on a cell with fibre shape (G), and electrochemical performance (H). (FH) (FH) (FH) (FH) (FH) (FH (I) A comparison of the rate capabilities of three different types of 3D-printed batteries. (Liu et al., 2018). FDM 3D-printed components for a (K) coin cell (J). (L) The electrochemical efficiency of the FDM battery. Figure 2.11. 3-D printed electrodes of lithium-ion battery with a lattice offers passages for lithium to travel into the electrode efficiently Figure 2.12. Schematic of the process to 3D-print solid electrolyte structures Figure 2.13. Different 3D printed forms of batteries (a) Construction strategies, (b) electrode architecture, (c) battery conewfiguration Figure 2.14. Imminent suggestion in the area of electrochemical energy storage and conversion and 3D printing

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Figure 3.1. a) Closeness spatial atomic layer deposition (SALD) system (b) In a normal close-proximity SALD head, the 3D arrangement of the different parts (c) On substrate top, Close view of the deposition head bottom (d) Image of a traditional head fixed in our SALD system, presenting pipes and connections’ complex set Figure 3.2. (a) For the different types of gases, 3D arrangement of the internal distribution channels:green shows metallic precursor, blacks represents exhaust in black ,red shows co-reactant,and blue shows inert gas. (b) Clear resin prints head. Distribution channels can be noticed. (c) With fittings, printed head which is ready to plug and show in the system of spatial atomic layer deposition (SALD). (d) Bottommost view ,with dissimilar outlet designs, of two different heads. e) Heads’ in-situ printing from Formlabs in a Form 2 in clear resin(f) The head design similar to 3D printed in metal. Figure 3.3. a) 3D illustration of 2 printed heads having diverse outlet measurements (5.0 cm vs. 2.50 cm). b) 3D illustration of a head intended for round shape placement in stationary spatial SCVD (CVD) manner. ZnO circles having dissimilar thickness are displayed (coordinating with depositions of 1.0, 1.50, and 2.0 min). c) 3D illustration of a custom head having 2 unlike precursor outlets made of metal intersecting on the middle area of the deposition location and 3D outlook of the consequential multilayer design that can be attained through a head like this. d) EDS analyses and paralleling SEM images of a ZnO/Cu2O/ZnO pile placed through a 2-metal precursor head presented in (c). Figure 3.4. a) Scheme of a customized design spatial atomic layer deposition (SALD) pen. b) Image of a SALD pen following a 3D print. c) Observation from the base of the SALD pen approach where the concentric circular gas outlets permitting deposition in every direction can be seen. d) Scheme of the SALD pen situated in a 3D table. e) Picture of the printed SALD pen mounted in the 3D table and designing a ZnO circle. f) ZnO circle and g) LMGP initials on a Si wafer composed with the 3D printed SALD pen. Figure 4.1. (a) Illustration using FDM technique of three dimensional printing (b) schematic of nature-influenced fractal electrode in printed Figure 4.2. (a) A lab-to-fab translation instrument used for solution-processed solar cells based on a slot-die coater of 3D-printer (b) roll-to-roll printing of perovskite solar cells, designed with ability to use at large-scale. Figure 4.3. (a) Attachment of an unplanarized array of Si solar micro-cell by spanning silver microelectrodes put in by 3D printing ; (b) response of current (I)–voltage (V) of and an array of 14-microcell linked by silver microelectrodes and a single silicon solar microcell; (c) Si ribbons printed by spanning ITO microelectrodes; and (d) three dimenional structure of ITO strips. Figure 4.4. (a) Before and after chemical smoothening of a three dimensional-printed compound parabolic solar concentrator (CPC); the larger surface is showed by insets . (b) Main focal ring of sunlight of a silver-coated CPC (c) A CPC and separate enclosure

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that can be used to form an exterior trap of light. (d) from the entering side, the reflection in the parabolic curve is seen in this perspective of the CPC. The red encircles two wrinkles in the concentrator. Figure 4.5. Solar cell created at the CSIRO Figure 4.6. Behind the solar cell ,(UC-PV) tool schematic with combined optics. (b) a bifacial silicon solar cell ,one of the parabolic concentrators connected is shown in detail. The UC phosphor is linked to the parabolic concentrator’s exit aperture. (c) A CPC optics’ 2D array of integrated with a standard two-dimensional array of the UCSC. The spaces between the layers are merely there to show how they work. Figure 5.1. A capacitor - 3D printed Figure. 5.2. (a) Diagram of the process of DIW of 3D printed adaptable MSCs having Fe2O3/graphene/Ag electrodes. Images of (b) interdigitated silver pattern arrays - 3D printed, (c) hybrid-dimensional electrode arrays - 3D printed and (d) a 3D printed MSC in a bending Figure 5.3. (a) Images of the found electrode ink at various time periods (the inset illustrating the ink extrusion state out of a micronozzle). (b) MSC electrodes and XRD patterns of Fe2O3 NPs. (c) Image and (d, e) SEM photographs of MSC electrodes - 3D printed. Figure 5.4. (a) CV plots at 10 mV s−1 scan rate, (b) GCD plots at 2 mA cm−2 current density, and (c) device areal capacitances of different 3D printed MSCs. (d) CV plots, (e) GCD plots, (f) Nyquist curve and (g) protracted cycling stability of Fe2O3/graphene/ Ag MSCs comparable to those of formerly recorded MSCs. Figure 5.5. (a) 3D printed Fe2O3/graphene/Ag MSCs Bending test showing great flexibility. (b) CV plots at various bending angles and (c) capacitance retention all along the cyclic bending of 3D printed Fe2O3/graphene/Ag MSCs. (d) Image, (e) CV plots and (f) GCD plots of MSC units linked in parallel and series. Figure 6.1. Corona release method, the live wire ionizes the nearby molecules of air over the specimen surface having no needle. There is no bodily touch between the corona electrode and the specimen surface. Figure 6.2. Piezoelectric Polyvinylidene fluoride printing arrangements. Figure 6.3. Graphic of IPC procedure model: (a) three-dimensional printing of Polyvinylidene fluoride film, (b) Corona poling procedure(51). Figure 6.4. Contact poling configures the electrical arrangement of the specimen. The upper electrode of the specimen seems to be in connection with the electrode of poling. The base plate (on which the specimen is rested) is grounded. Figure 6.5. Printing using Digital Projection Figure 6.6. The patchwork of piezoelectric microstructures printed utilizing Digital Printing Projection Figure 6.7. Solution evaporation dependent three-dimensional printing

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Figure 6.8. (a) Diagramatic demonstration of the PμSL system & the three-dimensional printing procedure flow is depicted from figure (b) to figure (g)( Chen et al., 2017). Figure 6.9. three-dimensional printing of piezoelectric detectors Figure 6.10. Schematic representation of (a) Experimental system for piezoelectric resultant current calculation & (b) specimen and electrode structure (18). Figure 6.11. Three-dimensional printing utilizing Stereolithography (MIP-SL)

Mask-Image-Projection-based

Figure 6.12. Near-field electrospinning method Figure 6.13. The three-dimensional printed automatic foot pressure detector Figure 7.1. 3-D printed film by film to generate the working cathode and anode of a small battery. Figure 7.2. demonstration of the battery elements Figure 7.3. 3D printed film electrodes for LIBs made of LFMP, LFP, LTO, LMO, and LCO-based materials. Figure 7.4. Interdigitated electrodes or LIBs printed in 3D Figure 7.5. Framework electrodes made of LFMP, LMO, LFP, LTO and LCO-based materials are 3D printed for LIBs. Figure 7.6. Solid-state electrolytes made of LLZ-based and LAGP materials are 3D printed for solid-state REBs. Figure 7.7. REBs are made by 3D printing metal-based and carbon film electrodes. Figure 7.8. The 3-D print battery elements of the spacecraft. Figure 7.9. representing the three-dimensional print battery utilized in the automobile. Figure 7.10. The 3-D print battery comprises (A) wearing bangle, (B) stretchy smartphone, and (C–D) elastic MEMS circuit setup Figure 7.11. 3 packing techniques for three-dimensional printed REBs. Figure 7.12. The battery’s Swelling. Figure 8.1. Diagram illustration of an electrolysis cell Figure 8.2. Computer-assisted design drawings of the (A) 3D published membrane and (B) anode Figure 8.3. Inkjet printing regarding fuel cell materials Figure 8.4. (a) Diagrammatic of a fundamental deposition MCED set-up made up of piezo levels and the electrolyte involving the dispensing nozzle and micropipette and (b) SEM photograph of 6 same microstructures that are fabricated with a copper-based electrolyte. (Han et al., 2016)

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LIST OF TABLES Table 2.1. Disadvantages and Advantages of 3D Printing, Nanoarchitectonics, and Photolithography in Comaprison to the Production of Electrodes for Applications using Electrochemical Energy Table 2.2. Modification Methods for Electrodes from 3D-Printing Table 6.1. Review of three-dimensional Printing Techniques. Table 8.1. The cell produced from SOFC is fabricated partially or totally through 3D printing. (Blue text was employed to show the layers deposited through technologies of 3D printing)

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PREFACE Electronics products are becoming increasingly common in the digital age. Electronic items such as televisions, smartphones, computers, and gaming cabinets have drastically revolutionized the way people live, interact, and work over the last few decades. Demands for personalization and miniaturization in consumer items are two significant trends that pose technical problems in designing and manufacturing future electronic products. Due to their effectiveness in permitting on-demand manufacture of highly customizable electronics on a broad range of conformal surfaces and substrates, 3D printed electronics have gotten much interest in recent years. This textbook explains 3D printed electronics, particularly energy devices, and provides readers with useful information. It does not necessitate any prior understanding of the subject on the part of the reader. This book contains eight chapters. Each chapter of the book explains the fundamental concept regarding a particular topic. Chapter 1 offers a detailed and thorough introduction of 3D printing technology, which contains additive manufacturing and its types along with its applications. Chapter 2 gives information on the application of 3D printing technology. Chapter 3 familiarizes the readers with the concept of Gas-Phase 3D printing of functional materials that contain a thorough background history so that readers can easily grasp these concepts. Chapter 4 discusses the 3D printing technology for the solar cell, including photovoltaic cell, solar concentrators, three-dimensional printing,3D printed solar cell and the Futuroscope. 3D printing, is also called additive manufacturing, is a technique for layering a threedimensional object employing a computer-generated design. Chapter 5 thoroughly explains the 3D printed components for flexible supercapacitors along with their synthesis methods and characterization. Chapter 6 provides a detailed explanation of three-dimensional printing of piezoelectric materials and their different types (ceramics, polymers, pottery polymers), plus the concept of poling is also explained in this chapter. Chapter 7 focuses on the three-dimensional printing of rechargeable Ed batteries and the required battery materials also; the Li-based 3D-printed materials for REBs are also explained thoroughly to understand readers and end with the applications. This ends with chapter 8 that provides information about the three-dimensional fuel cells, their efficiency, and future scope. This book is an excellent resource for anyone attracted to energy 3D printing. The book is also a valuable textbook for graduate and undergraduate courses that seek to provide students with a complete understanding of 3D printed electronics foundations.

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Author

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CHAPTER

1

INTRODUCTION 3D PRINTING TECHNOLOGY

CONTENTS

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1.1 Introduction ........................................................................................ 2 1.2 Additive Manufacturing and its Types ................................................... 4 1.3 Ingredients Utilized for Digital Fabrication Technology in Fabricating Industry ...................................................................... 8 1.4 Digital Fabrication’s Usage in Manufacturing Technology ................. 13 References .............................................................................................. 19

2

3D Printing for Energy Applications

1.1 INTRODUCTION Through the sequential adding of supplies, physical items from a geometric depiction are fashioned by additive manufacturing or 3D printing, also known as digital fabrication technology. High tech which is emerging quite quickly is 3D printing technology. It is high-tech which is extensively utilized everywhere. In the industry of locomotives, in healthcare, aviation industry, and agriculture for open-source designs manufacture, digital fabrication technology is utilized for bulk customization progressively (Saheb & Kumar, 2020). From the prototype of a CAD (computer-aided design), an item’s print can be taken in layers by the removal of material directly through additive manufacturing. In the industry of manufacturing, the constituents employed for additive manufacturing, its use, and its categories are presented in the paper. Through successively adding ingredients, physical items can be formed through geometric depiction by 3D printing (Shahrubudin et al., 2020). In the current time, remarkable growth has been delegated to this 3D procedure. Charles Hull initially marketed this additive manufacturing in 1980 (Gartner et al., 2015). Recently, its use is most popular in food as well as aviation industry for the production of the 3D printed cornea, artificial pumps for heart, bridges of steel in Amsterdam, collections of jewelry, and PGA rocket engine (azdozian et al., 2018; Mogy & Rabea, 2021). From the models of CAD (computer-aided design), 3D arrangements can be constructed through layering mechanization, which was created out of 3D printing (Tofail et al., 2018). It is quite multipurpose and being truly advanced are the qualities attributed to this technology. For the improvement of proficiency regarding production, corporations hope to uncover various potentials as well as exploring new prospects through additive manufacturing. Through its use, materials based on graphene, standard thermoplastics, metal, and ceramics can now be printed by employing digital fabrication technology (Low et al., 2017). The manufacturing line can be changed as well as many businesses may be revolutionalized through 3D printing. Prices will be reduced and the speed of manufacturing will be increased through the adoption of this technology. Similarly, manufacturing will be greatly influenced by the consumer’s request. The ultimate creation and demands for specifications will be greatly catered to the customer. Power over the value and an open and accomodating procedure of production will be allowed as the sites of digital fabrication technology will be nearer to the consumer. The reduction of international shipping will take place by adopting this

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Introduction 3D Printing Technology

3

technology. As location sites will be closer, time and energy could be saved through the technology of fleet-tracking. The business system can also be transformed through 3D printing technology. Beginning to ending and more complete facilities may be offered as well as the management of the whole activity (Rajan et al., 2016).

Figure 1.1. FDM additive manufacturing technology’s graphic diagram. (Source: https://www.researchgate.net/figure/A-schematic-illustration-of-theFDM-3D-printing-technology_fig1_333719097)

Recently, the use of 3D printing is done worldwide. In healthcare, the business of aerospace, the agricultural line of work, and the business of automotive, digital fabrication technology is utilized for bulk customization and production of open-source designs of all kinds progressively (Garg et al., 2017). However, many drawbacks in the industry of manufacturing also follow the high tech i.e., 3D printing. Countries relying on inexpert professions will be greatly affected economically as manufacturing labor will be reduced which is a negative result of additive manufacturing. Moreover, unsafe objects such as guns and knives may be printed by any user through this mechanism. Thus, to avoid the entrance of offenders and terrorists with weapons, access to this technology should be restricted to particular individuals. Also, individuals may forge items by attaining the blueprints somehow. As the 3D items can be generated just by printing them in the machine after drawing, it is quite easy to forge (Pîrjan & Petroşanu, 2013).

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4

3D Printing for Energy Applications

In the industry of progressive production, a prevailing and accomodating method in the shape of 3D printing has appeared in current times. Particularly in the industry of production, various countries have been using this mechanization. Thus in the production industry, the constituents utilized, their use, and an outline of the kinds of 3D printing are presented in this paper.

Figure 1.2. The procedure of an archetypal way of 3D printing. Source: https://3dprinting.com/what-is-3d-printing/

1.2 ADDITIVE MANUFACTURING AND ITS TYPES Through diverse functions, the development of many types of additive manufacturing has taken place. Material extrusion, binding jetting, vat photopolymerization, powder bed fusion, sheet lamination, material jetting, and directed energy deposition; are the 7 sets into which ASTM has categorized digital fabrication technology as stated by ASTM Standard F2792 (Frazier, 2014). Due to all of them having a specific use, no arguments about which technology works or machine is superior has taken place. An assortment of goods are being made by using 3D printing and its use is not restricted to just prototyping practice (Zaman et al., 2018).

1.2.1 Binder Jetting Powder elements are joined by a liquid uniting instrument that is selectively placed on it and is the method of binder jetting which is a type of 3D printing and is a speedy model. To create the layer, a jet chemical binder is used by

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Introduction 3D Printing Technology

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the mechanism of binder jetting on the scattered powder (Low et al., 2017). Great-capacity goods from sand or related goods of unprocessed sinters and casting designs are the results of the use of binding jetting. Hybrid, metals, ceramics, and polymers are some of the constituents that can be printed by binder jetting. Added treatment is not needed by some constituents such as sand. Powder goods are cemented with each other which is the reason why binder jetting is an inexpensive, rapid, and easy procedure. Huge goods can also be printed by binder jetting.

1.2.2 Directed Energy Deposition For the addition to present substituents of extra constituents that have to be repaired or added is an intricate printing procedure called directed energy deposition (Tofail et al., 2018). Items of decent worth are created by it and it has a grain arrangement’s great degree influence. The nozzle can shift in several directions and is not set to a precise axis is the only difference between directed energy deposition and material extrusion. Aside from that, they are alike in theory. In the shape of powder or wire, it is classically employed in hybrids based on metals, or metals but also utilized with polymers and ceramics. LENS (Laser engineered net shaping) and laser deposition are two samples of this high tech (Tofail et al., 2018). Fragments assessed in m’s (meters) or mm can be repaired or produced through a laser machine which is a developing technology. Various abilities in the solitary structure and scalability are offered by this technology which is why it is receiving praise in the oil, tooling, gas, transportation, and aerospace areas (Polonsky et al., 2019). Portions are achieved subsequently and at the time of casting, thermal power can be exploited for thawing by the laser LENS (Dilberoglu et al., 2017).

1.2.3 Materials Extrusion Alive cells, plastics, or food can be printed in multiple colors and multiple things can be printed by using additive manufacturing based on material extrusion (Tieber, 2019). The prices are cheap and this procedure is extensively employed. Plus, portions of goods that are wholly operational can be built by it (Tofail et al., 2018). The material extrusion system’s initial sample is FDM (fused deposition modeling). The chief substance is a polymer and the development of FDM took place in the early nineteen hundreds (Stansbury & Idacavage, 2016). By the extrusion of thermoplastic fiber and warming the fragments to their peak from the base in layers is way FDM works. Following are the functions of FDM:

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Further, in the extrusion track, the ultra-fine beads receive the deposition of thermoplastic which has been warmed to a condition of partly liquidness (Jiawang et al., 2014). A detachable substance that performs like scaffolding is added by the 3D printer wherever buffering or sustenance is required (Jiawang et al., 2014). For instance, the 3D bone prototype is produced by FDM at the time of the procedure by using plastic ingredients that are hard (Jiawang et al., 2014).

1.2.4 Materials Jetting Selective deposition of built constituents through drop by drop is a method of digital fabrication called material jetting as stated by ASTM Standards. UV light is utilized to build a portion that is layered after precipitations of a substance that is photosensitive is dispensed to solidify on it by a printhead in material jetting (Silbernagel et al., 2019). The precision of great dimensions and fragments with leveled surfaces are produced by material jetting. Material jetting contains an extensive assortment of ingredients like biologicals, ceramics, hybrid, composite, and polymers as well as printing of several substances (Tofail et al., 2018).

1.2.5 Powder Bed Fusion The methods included in the procedure of powder bed fusion are SLS (selective laser sintering), EBM (electron beam melting), and SHS (selective heat sintering). For the substance powder to thaw together, a laser or beam of electrons is employed in this technique. Composite, ceramics, metals, and polymers are the sample of ingredients utilized in this procedure. Additive manufacturing based on powder is the chief sample of SLS. 1987 was the year of the development of this mechanism by Carl Deckard. Varying surface finish, quick speed, and great precision are the functions of SLS (Tiwari et al., 2015). Ceramic items, metal, and plastic can be created by utilizing SLS (Ventola, 2014). For the generation of a 3D item, powders of polymer are sintered by a laser of great power. Whereas, for the creation of a 3D printed item in selective heat sintering, the powder of thermoplastic is liquefied by employing a head thermal print. Finally, for the heating up of a substance, an energy supply is enhanced by EBM (Ventola, 2014).

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1.2.6 Sheet Lamination For the production of an item’s segment, the bonding of sheets of substances is done in digital fabrication technology’s sheet lamination as stated by the ASTM description (Silbernagel et al., 2019). UAM i.e., ultrasound additive manufacturing, and LOM i.e., laminated object manufacturing are the samples of additive manufacturing that utilize this procedure (Tofail et al., 2018). Recycling of extra matter can be done, it is comparatively cheaper, the substance is simple to control and wholly colored prints can be taken which are the benefits of this procedure. A less functional period and production is low cost for the manufacturing of complex geometric segments in LOM (Vijayavenkataraman et al., 2017). From featureless foil supply, metal films are taken through the use of sound in the pioneering method called UAM.

1.2.7 Vat Photopolymerization The main 3D printing technique that is frequently used is photopolymerization, which in general refers to the curing of photo-reactive polymers by using a laser, light, or ultraviolet (UV) (Lee et al., 2016). The example of 3D printing technologies by using photopolymerization is stereolithography (SLA) and digital light processing (DLP). In the SLA, it was influenced by the photoinitiator and the irradiate exposure of particular conditions as well as any dyes, pigments, or other added UV absorbers (Stansbury & Idacavage, 2016). Meanwhile, digital light processing is a similar process to Stereolithography that works with photopolymers. The light source is a major difference. Digital Light Process uses a more conventional light source, such as an arc lamp with a liquid crystal display panel. It can apply to the whole surface of the vat of photopolymer resin in a single pass, generally making it faster than Stereolithography (Krkobabić et al., 2020). The important parameters of Vat Photopolymerization are the time of exposure, wavelength, and the amount of power supply. The materials used initially are liquid and they will harden when the liquid is exposed to ultraviolet light. Photopolymerization is suitable for making a premium product with good details and high quality of surface (Tieber, 2019). Through the use of UV (ultraviolet), laser or light, photo-reactive polymers are cured which is the digital fabrication procedure of photopolymerization (Lee et al., 2016). DLP (digital light processing) and SLA (stereolithography) are the samples of additive manufacturing that utilize this mechanism. Pigments, more absorbers, and dyes as well as certain circumstances being exposed and photoinitiator were the inspirations of

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SLA (Stansbury & Idacavage, 2016). Photopolymers are employed in DLP and are comparable to SLA. Their main dissimilarity is the light supply. A curved lamp containing a liquid crystal exhibition panel is a traditional light supply that is typically employed by DLP. It is quicker than SLS as it takes just a sole pass for the photopolymer resin’s entire surface to be applied on (Krkobabić et al., 2020). Power source quantity, contact time, and wavelength are the chief limits of vat photopolymerization. At exposure to UV light, the liquid which was originally in a liquid state is hardened. A creation containing a surface of great value and decent particulars can be made through photopolymerization (Tieber, 2019).

1.3 INGREDIENTS UTILIZED FOR DIGITAL FABRICATION TECHNOLOGY IN FABRICATING INDUSTRY For the production of constant first-rate gadgets, fixed conditions need to be met by first-class substituents needed for additive manufacturing like any other engineering procedure. Thus, the end-utilizers, buyers, and providers agree on the substance controls, necessities, and processes to guarantee superiority. Metallic, polymers, ceramic and their mixtures in the shape of composites, FGMs (functionally graded materials), or hybrids are materials whose wholly operational portions digital fabrication technology can manufacture (Tofail et al., 2018).

Figure 1.3. Market Segmentation of Additive Manufacturing Items. Source: https://www.alliedmarketresearch.com/3d-printing-material-market

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1.3.1 Metals Due to the benefits provided by metal digital fabrication technology, the fields of the appliance of medicine, aerospace, production industry, and automobile are quite interested in it (Horst et al., 2018). Intricate fabrication procedures can take place due it such as aerospace portions getting prints of humanoid organs due to metal’s outstanding physical characteristics. Stainless steels, cobalt-based alloys, titanium alloys, aluminum alloys, and nickel-based alloys are samples of this substance (Martin et al., 2017; DebRoy et al., 2018). In the additive manufacturing dental function, the most appropriate item is cobalt-based alloys. Elongation, elasticity, situations healed through heat, stiffness of great precision, and great recovery ability are its properties due to which it is suitable (Hitzler et al., 2017). Moreover, through the use of nickel-based alloys, aerospace portions can be produced by digital fabrication technology (Murr, 2016). In perilous settings, the items made from nickel-based alloys can be employed as the heat temperature of 1200.0 °C can be resisted by it and it possesses great endurance towards corrosion (Horst et al., 2018). Also, titanium alloys can be used to take prints of objects. Oxidation resistance, ductility, low density, and good corrosion are some selective features owned by titanium alloys. It can be utilized in the biomedical field and aerospace apparatuses i.e., in high operating and stresses temperatures (Trevisan et al., 2018).

Figure 1.4. A metal fragment that is digitally fabricated. Source: https://pick3dprinter.com/best-metal-3d-printer/

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1.3.2 Polymers The manufacture of operational edifices containing hard geometries to models involving elements of polymer is the use of additive manufacturing technology (Caminero et al., 2018). Extruded thermoplastic filament like PP (polypropylene), PLA (polylactic acid), PE (polyethylene), and ABS (acrylonitrile butadiene styrene) is deposited in sequential coatings and develop a 3D print by utilizing FDM (fused deposition modeling) (Caminero et al., 2018). For additive manufacturing, thermoplastic filaments like PMMA and PEEK with greater liquifying temperatures can be employed (Dizon et al., 2018). Because of the lower weight, flexibility in processing, and lower price, digital fabricating polymer substances with low liquifying points or in liquid condition are extensively utilized (Wang et al., 2017). By giving mechanical aid in orthopedic implantation and taking part in the gadget’s effective operation, the polymer substances had a significant function in medical gadgets items and biomaterials.

Figure 1.5. Items of polymer fashioned through digital fabrication. Source: https://www.3dprintingmedia.network/new-report-forecasts-polymer-3d-printing-to-generate-55-billion-yearly-by-2030/

1.3.3 Ceramics By setting up the decent mechanical features and the parameters’ enhancement, 3D printed items can be produced by utilizing concrete sans big pores and ceramics in additive manufacturing (Baldassarre & Ricciardi, 2017). Being sturdy, resistant to fire, and powerful are the properties of ceramics. It is very appropriate for the upcoming creation of buildings and construction as it can be put on in any form and geometry due to its flexible

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nature before setting (Gunatillake & Adhikari, 2016). In aerospace and dental usage, ceramics is quite valuable as stated by Owen et al, (2018). Zirconia, alumina, and bioactive glasses are its samples (Gmeiner et al., 2015). Through digital fabrication technology, alumina has the skill to be processed. Microelectronics, aerospace industry, catalyst, high-technology industry, chemicals, and absorbents are the numerous purposes of alumina which is a brilliant ceramic oxide. Curing complexity is owned by alumina. The printing of intricately formed alumina portions containing high green density and post sintering great density can be done by additive manufacturing (Zocca et al., 2017). The dance part was made by the processing of bioactive glass and glass-ceramic by SLA in experimentation. The bending power of this substance was drastically enhanced by it. Bone and scaffolds which are pertinent clinical edifices could be applied bioactive glass by the growth of the mechanical power. Solid mass ceramics owning very homogeneous microstructure, great densities, and great bending and compression power may be produced by employing SLCM (Stereolithographic Ceramic Manufacturing). Utilized for element tubing, nuclear power locations employ zirconia which is very appropriate for it. Due to lower thermal neutron absorption and radiation vulnerability, hafnium-free zirconium is very appropriate for this usage (Gmeiner et al., 2015).

Figure 1.6. Ceramic items made by additive manufacturing. Source: https://www.pinterest.com/pin/383157880803083640/

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1.3.4 Composites Pepped-up industries are being revolutionized by the tailorable features, lower weight, and excellent changeability of composite items. Glass fibers reinforced polymer composite and carbon fibers reinforced polymer composites are its samples (Amer et al., 2018; Hao et al., 2018). Due to decent resistance to corrosion, great definite stiffness, decent fatigue working and power, carbon fiber reinforced polymers composite formations are broadly employed in the aerospace industry (Hao et al., 2018). Because of the efficiency and price efficacy, glass fibers reinforced polymer composites has amazing likely usage and also extensively utilized for numerous uses in 3D printing application. Comparatively lower coefficient of thermal increase and a great thermal conductivity are owned by fiberglass. It is very appropriate for usage in additive manufacturing applications as it is not influenced by curing temperatures employed in manufacturing procedures and it cannot burn (Liu et al., 2015).

1.3.5 Smart Materials The items whose shape and geometry can be changed through the effect of the external environment like water and heat are called smart materials (Lee et al., 2017). Soft robotic structure and soft evolving system are samples of additive manufactured items fashioned by smart materials. 4D printed things is another name given to smart materials. Shape memory polymers and shape memory alloys are samples of group smart materials (Yang et al., 2016). For microelectromechanical gadgets appliances and biomedical implantations, the usage of nickel-titanium which is a shape-memory alloy can be done (Singh & Raghav, 2018). Density, alteration temperature and reproducibility is the significant problem in the manufacture of digitally fabricated objects by the use of nickel-titanium. Some kinds of chemical, light, and electricity heat receive a response from SMP i.e., shape memory polymer which is a type of operational substance. It can be convenient and easy to manufacture the shape memory polymer’s complex form by employing additive manufacturing. Part density, dimensional precision, and surface irregularity are the basis of the object’s value assessment (Yang et al., 2016).

1.3.6 Specials Materials Some special material samples are:

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Through the progression of additive textile manufacturing, the industry of clothes and accessories will gleam. Reduced price of the supply chain, packing’s decreased price, and item’s short manufacturing period are a few benefits in the fashion industry provided by digital fabrication technology. • Lunar dust For moon colonization in the time to come usage, the skill to develop layer upon layer from lunar dust rests with a 3D printing procedure (Joshi & Sheikh, 2015). • Food For foods such as meat, sauce, chocolate, pizza, candy, spaghetti, etc., the wanted geometry and form can be processed and produced through additive manufacturing. The constituent’s taste and the nutrients need not be reduced according to 3D food printing and yet it permits the consumers to change the components which result in the production of nutritious food (Joshi & Sheikh, 2015).

1.4 DIGITAL FABRICATION’S USAGE IN MANUFACTURING TECHNOLOGY 14.1 Aerospace Industry For construction and component, unmatched liberty plans are provided by additive manufacturing. The reduction of the need for supplies and energy can be done due to the digital fabrication technology’s ability to create intricate and enhanced geometries and portions that are light in weight in the field of aerospace (Wang et al., 2019). Also, for the production of segments of aerospace, fewer items will be used which will lead to fuel being saved by the use of additive manufacturing. For objects like engines or any aerospace machinery, their production is made possible broadly by applying digital fabrication technology. Consistent changing is required by the engine’s segment as it is impaired with ease. Thus, for the obtaining of these kinds of extra segments, a decent answer lies in the form of additive manufacturing (Ahn, 2016). The harm tolerance, tensile characteristics, and corrosion/oxidation resistance make alloys based on nickels more desirable in the field of aerospace (Razumov et al., 2017).

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1.4.2 Automotive Industry The development, manufacturing, and designing of innovative materials have taken a new turn and altered the industry due to additive manufacturing. More intricate and agiler structures in less period are made possible due to the digital printing method in the field of automobiles. For instance, in 2014, the initial digitally printed electrical car was printed by Local Motor. A digitally printed bus named OLLI was also developed by Local Motors who did not limit themselves to cars and spread additive manufacturing’s extensive scale of usage. Recyclable, without a driver, very clever, and electrical are the properties of OLLI. Ford applies digital printing to develop segments of engines and models and is the front-runner in its usage (Maghnani., 2015). For assembly and examining automobiles, hand devices have been produced by BMW using the same technology. For the production of models and extra segments, SLM Solution Group AG joined forces with AUDI in 2017 (Sreehitha, 2017). Successful and perfect automobile models are encouraged by emphasizing and trying several substitutes right at the enhancement levels in the field of automobiles which has been enabled by additive manufacturing. Moreover, excess and utilization of resources can be reduced by it. Plus, innovative plans can be tested very quickly as it requires reduced time and price (Maghnani., 2015).

1.4.3 Industry of Food The food business also opened up to many possibilities through additive manufacturing, not just the field of aerospace. The enhancement of the existence of nutritious components while the reduction of pointless components is required due to the rising request of personalized foods for specialized nutritional requirements like pregnant women, athletes, patients, and children, etc (Dankar et al., 2018). The implementation of additive manufacturing took place because personalized foods need to be produced in an imaginative and thorough way. Based on CAD i.e., computer-aided design information, the discharge of sequential layers is done in 3D-food printing also known as food layer manufacture. Numerous complex forms and structures are made by mixing and processing precise substances through their use (Fateri & Gebhardt, 2015). Innovative foodstuff containing fascinating and intricate forms and designs can be created by using flat foods like crackers, pasta, and pizza or food like pureed food, sugar, and chocolate.

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Possessing lower price, ecologically welcoming, and decent regulation overvalue, digital printing technology is a high-power proficiency technology for food development. As it can adapt to separate requirements and likings, and innovative procedures can be created for customization of food, additive food printing can provide an advantage and be nutritious for individuals. Without the requirement to workout, diets would be able to impose themselves as customer’s data will help adapt food components and preparation (Fateri & Gebhardt, 2015).

1.4.4 Industry of Medicine and Healthcare Communication, visualization, and education, as well as prints of replacement tissues, cartilage and bone, research for cancer, pharmaceutical, and drug research, organ, and skin through digital printing technology (Ventola, 2014). Biomedical creations contain many 3D printing technology benefits that are listed below:

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At a very low price, the skin’s original configuration can be replicated by 3D printing technology. Chemical, pharmaceutical, and cosmetic items can be tested through their use. Thus, testing the items by using the skins of animals is pointless. Through the use of replications of the skin, precise outcomes will be acquired by the scientist. The production of dosage systems with intricate drug-release reports, exact regulation of dropped prescription and size, increased effectiveness, and great reproducibility can be achieved through employing digital printing for the printing of drugs (Ventola, 2014). 3D printing technology can print cartilage and bone to replace bony voids in the cartilage or bone that are caused by trauma or disease. This treatment is different options from using auto-grafts and allografts because this treatment focuses on generating bone, maintain, or improve its function by using in vivo. Bony spaces due to illness or shock in the bone or cartilage can be replaced by printing bone and cartilage through 3D printing high-tech. As this remedy emphasizes maintaining, improving, and generating bone by the use of in vivo, diverse choices like allografts and auto-grafts can be used. The maintenance, restoration, improvement, and replacement of the tissue function can be done through digital fabrication

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technology. Suitable surface chemistry, interlinked pore system, decent mechanical features, and biocompatibility are possessed by the replacement tissues (Low et al., 2017). Accidents, defects at birth, and disease-causing organs to fail can be printed by this technology. Cancer exploration can be accelerated by this technology as it can create a model of greatly regulated cancer tissues. Precise and dependable information can be provided to the patients by additive manufacturing. Surgical methods can be practiced by neurosurgeons with the help of digital fabrication technology which can be used in the studying procedure. As the digital prototype is an imitation of the pathological state of a true patient, chances can be provided for hands-on teaching to the doctors, precision can be improved and clinical processes can be done in fewer periods by trainers.

1.4.5 The Construction Industry, Architecture, and Building Geometrical intricacy realization is given limitless potentials by digital printing technology which is an ecologically welcoming derivative. Machinery for construction and complete buildings can be printed through additive manufacturing. Digital printing technology will be facilitated in an improved way through the appearance of BIM (Building Information Modelling). Understanding and data about digital buildings are given by BIM which is a physical and operational features’ digital depiction Designing, constructing and demolition of the building can be decided by it as it is a dependable foundation for decision at the time of its ongoing life cycle (Maghnani., 2015). Sustaining, making, and fabricating will be made more effective by this cooperative and ground-breaking technology. Zones of issues can be highlighted and suspensions can be avoided with the use of additive manufacturing, as well as the structures’ pictorial can be created and designed quickly in a cheaper way by the companies. Plus, the communication between customers and the engineer of a building can flow more smoothly and plainly. Leaving the old-fashioned technique of making an idea on pencil and paper in the past, 3D printed buildings go beyond it as a consumer’s anticipation comes more from the formation of a design. Amsterdam’s Canal House and Russia’s Apis Cor Printed House are its samples (Sreehitha, 2017).

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1.4.6 Industry of Fashion and Fabric Customer clothes and items, 3D printed shoes, and ornaments emerge in the marketplace when digital fabrication technology arrives at the retail field (Saheb & Kumar, 2021). It is beginning to turn into reality globally even though the mixture of digital printing and fashion does not look like a genuine match. For instance, the mass manufacture of 3D printed shoes is being developed by huge corporations such as Adidas, Nike, and New Balance. Sneakers, customized shoes, and shoes for sportspersons are made through digital fabrication. Moreover, artistic potentials related to fashion design can be broadened through additive manufacturing. The creation of shapes sans molds is made likely by it. The conventional textile can get embellishments and the employment of mesh scheme can develop clothes that are produced and designed by digital fabrication technology. Decorations and leather items can also be made by this technology and are not just beneficial for the field of fashion. For example, decorations, making of watches and ornaments, etc., (Wang et al., 2017). Exclusive and tailored items are offered to the consumer for the improvement of the design of the item through the use of digital fabrication technology and are not meant to replicate existing items according to designers and sellers. The demanded custom designing and fitting of the item can be done by the technology which is a huge benefit of it. Plus, the price of the supply network can be reduced by it. Concludingly, items in little amounts require less time to be created and delivered (Dizon et al., 2018).

1.4.7 Industry of Electronics and Electric Digital fabrication technology’s real aptitude is being recognized as it is becoming increasingly available to different fields such as technology and science etc. The creation of mechanical electric gadgets such as bulk customized gadgets, active electrical substances, electrodes, and the embedment of conductors in the digital printing gadgets for adaptive planning is already being done. Electrode matters can be developed in bulk quantities by a time-effective and cheap price tactic provided by digital fabrication’s method of FDM. Specific applications can be used to create 3D electrodes whose surface

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area and pattern are tailored for them in comparison to carbon, copper, and aluminum electrodes which are marketable. 8.0 electrons can be printed in just thirty minutes by the digital fabrication procedure as it has a great extent of accuracy and is wholly mechanical (Tofail et al., 2018). The ability to regulate and increase electronic current charges resting with any electric constituents and gadgets is called active electronic constituents. Moreover, gadgets capable of generating energy are also included in it. LEDs (light-emitting diodes), transistors, operational amplifiers, batteries, rectifiers controlled by silicon and diodes are its instances. The intricate operations of these components make it different from passive constituents which do not require a greatly detailed manufacturing procedure but these do. The electronics of the item, as well as its administering, are given benefits by digital fabrication technology. In a single procedure, various items will be capable of being made through the adoption of the electric method in Industry Revolution 4.00 with the advent of printing machinery for multiple substances (Baldassarre & Ricciardi, 2017). The ecological contamination in the current world needs to be rapidly addressed which instigated the production of an electric gadget with reliable safety, fast development, great dependency, and cheap price of manufacturing (Pîrjan & Petroşanu, 2013).

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Ahn, D. G. (2016). Direct metal additive manufacturing processes and their sustainable applications for green technology: A review. International Journal of Precision Engineering and Manufacturing-Green Technology, 3(4), 381-395. 2. Amer, A. A. R., Abdullah, M. M. A. B., Ming, L. Y., & Tahir, M. F. M. (2018). Performance and properties of glass fiber and its utilization in concrete-A review. In AIP Conference Proceedings, 2030(1), 20296. 3. Baldassarre, F., & Ricciardi, F. (2017). The additive manufacturing in the Industry 4.0 Era: the case of an Italian FabLab. Journal of Emerging Trends in Marketing and Management, 1(1), 105-115. 4. Caminero, M. A., Chacón, J. M., García-Moreno, I., & Rodríguez, G. P. (2018). Impact damage resistance of 3D printed continuous fibre reinforced thermoplastic composites using fused deposition modelling. Composites Part B: Engineering, 148, 93-103. 5. Dankar, I., Pujolà, M., El Omar, F., Sepulcre, F., & Haddarah, A. (2018). Impact of mechanical and microstructural properties of potato puree-food additive complexes on extrusion-based 3D printing. Food and Bioprocess Technology, 11(11), 2021-2031. 6. DebRoy, T., Wei, H. L., Zuback, J. S., Mukherjee, T., Elmer, J. W., Milewski, J. O., ... & Zhang, W. (2018). Additive manufacturing of metallic components–process, structure and properties. Progress in Materials Science, 92, 112-224. 7. Dilberoglu, U. M., Gharehpapagh, B., Yaman, U., & Dolen, M. (2017). The role of additive manufacturing in the era of industry 4.0. Procedia Manufacturing, 11, 545-554. 8. Dizon, J. R. C., Espera Jr, A. H., Chen, Q., & Advincula, R. C. (2018). Mechanical characterization of 3D-printed polymers. Additive Manufacturing, 20, 44-67. 9. El Mogy, T., & Rabea, D. (2021). An overview of 3D printing technology effect on improving solar photovoltaic systems efficiency of renewable energy. Proceedings of the International Academy of Ecology and Environmental Sciences, 11(2), 52-67. 10. Fateri, M., & Gebhardt, A. (2015). Process parameters development of selective laser melting of lunar regolith for on‐site manufacturing applications. International Journal of Applied Ceramic Technology, 12(1), 46-52.

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11. Frazier, W. E. (2014). Metal additive manufacturing: a review. Journal of Materials Engineering and performance, 23(6), 1917-1928. 12. Garg, A., Bhattacharya, A., & Batish, A. (2017). Failure investigation of fused deposition modelling parts fabricated at different raster angles under tensile and flexural loading. Proceedings of the Institution of Mechanical Engineers, Part B: Journal of Engineering Manufacture, 231(11), 2031-2039. 13. Gartner, J., Maresch, D., & Fink, M. (2015). The potential of additive manufacturing for technology entrepreneurship: an integrative technology assessment. Creativity and Innovation Management, 24(4), 585-600. 14. Gmeiner, R., Deisinger, U., Schönherr, J., Lechner, B., Detsch, R., Boccaccini, A. R., & Stampfl, J. (2015). Additive manufacturing of bioactive glasses and silicate bioceramics. J. Ceram. Sci. Technol, 6(2), 75-86. 15. Gunatillake, P. A., & Adhikari, R. (2016). Nondegradable synthetic polymers for medical devices and implants. In Biosynthetic Polymers for Medical Applications, 23(5), 33-62. 16. Hao, W., Liu, Y., Zhou, H., Chen, H., & Fang, D. (2018). Preparation and characterization of 3D printed continuous carbon fiber reinforced thermosetting composites. Polymer Testing, 65, 29-34. 17. Hitzler, L., Williams, P., Merkel, M., Hall, W., & Öchsner, A. (2017). Correlation between the energy input and the microstructure of additively manufactured cobalt-chromium. In Defect and Diffusion Forum, 379, 157-165. 18. Horst, D. J., Duvoisin, C. A., & de Almeida Vieira, R. (2018). Additive manufacturing at Industry 4.0: a review. International journal of engineering and technical research, 8(8), 1-16. 19. Ianko, T., Panov, S., Sushchyns’ky, O., Pylypenko, M., & Dmytrenko, O. (2018). Zirconium alloy powders for manufacture of 3d printed articles used in nuclear power industry. Problems of Atomic Science and Technolog, 1(133), 147-153. 20. Jiawang, Y., Linshuang, Z., Zhiming, D., Qifeng, X., & Zhihua, Z. (2014). Study on combustion heat of pyrotechnics. Procedia Engineering, 84, 849-853.

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21. Joshi, S. C., & Sheikh, A. A. (2015). 3D printing in aerospace and its long-term sustainability. Virtual and Physical Prototyping, 10(4), 175185. 22. Khazdozian, H. A., Manzano, J. S., Gandha, K., Slowing, I. I., & Nlebedim, I. C. (2018). Recycled Sm-Co bonded magnet filaments for 3D printing of magnets. AIP Advances, 8(5), 056722. 23. Krkobabić, M., Medarević, D., Pešić, N., Vasiljević, D., Ivković, B., & Ibrić, S. (2020). Digital light processing (DLP) 3D printing of atomoxetine hydrochloride tablets using photoreactive suspensions. Pharmaceutics, 12(9), 833. 24. Lee, J. Y., An, J., & Chua, C. K. (2017). Fundamentals and applications of 3D printing for novel materials. Applied materials today, 7, 120133. 25. Lee, J. Y., Tan, W. S., An, J., Chua, C. K., Tang, C. Y., Fane, A. G., & Chong, T. H. (2016). The potential to enhance membrane module design with 3D printing technology. Journal of Membrane Science, 499, 480490. 26. Liu, Z., Zhang, L., Yu, E., Ying, Z., Zhang, Y., Liu, X., & Eli, W. (2015). Modification of glass fiber surface and glass fiber reinforced polymer composites challenges and opportunities: from organic chemistry perspective. Current organic chemistry, 19(11), 991-1010. 27. Low, Z. X., Chua, Y. T., Ray, B. M., Mattia, D., Metcalfe, I. S., & Patterson, D. A. (2017). Perspective on 3D printing of separation membranes and comparison to related unconventional fabrication techniques. Journal of membrane science, 523, 596-613. 28. Maghnani, R. (2015). An exploratory study: the impact of additive manufacturing on the automobile industry. International Journal of Current Engineering and Technology, 5(5), 1-4. 29. Martin, J. H., Yahata, B. D., Hundley, J. M., Mayer, J. A., Schaedler, T. A., & Pollock, T. M. (2017). 3D printing of high-strength aluminium alloys. Nature, 549(7672), 365-369. 30. Murr, L. E. (2016). Frontiers of 3D printing/additive manufacturing: from human organs to aircraft fabrication. Journal of Materials Science & Technology, 32(10), 987-995. 31. Owen, D., Hickey, J., Cusson, A., Ayeni, O. I., Rhoades, J., Deng, Y., ... & Zhang, J. (2018). 3D printing of ceramic components using a customized 3D ceramic printer. Progress in additive manufacturing, 3(1), 3-9.

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32. Pîrjan, A., & Petroşanu, D. M. (2013). The impact of 3D printing technology on the society and economy. Journal of Information Systems and Operations Management, 7(2), 360-370. 33. Polonsky, A. T., Lang, C. A., Kvilekval, K. G., Latypov, M. I., Echlin, M. P., Manjunath, B. S., & Pollock, T. M. (2019). Three-dimensional analysis and reconstruction of additively manufactured materials in the cloud-based BisQue infrastructure. Integrating Materials and Manufacturing Innovation, 8(1), 37-51. 34. Rajan, V., Sniderman, B., & Baum, P. (2016). 3D opportunity for life: Additive manufacturing takes humanitarian action. Delight Insight, 1(19), 1-8. 35. Razumov, n., popovich, a., & eng, s. (2017). Production of highnitrogen steel spherical powder by mechanical alloying and plasma spheroidization. Scientific and technical journal, 3 (91), 2017, 69, 6589. 36. Saheb, S. H., & Kumar, J. V. (2020). A comprehensive review on additive manufacturing applications. In AIP Conference Proceedings (2281), 20024. 37. Shahrubudin, N., Koshy, P., Alipal, J., Kadir, M. H. A., & Lee, T. C. (2020). Challenges of 3D printing technology for manufacturing biomedical products: A case study of Malaysian manufacturing firms. Heliyon, 6(4), 03734. 38. Shahrubudin, N., Lee, T. C., & Ramlan, R. (2019). An overview on 3D printing technology: Technological, materials, and applications. Procedia Manufacturing, 35, 1286-1296. 39. Silbernagel, C., Gargalis, L., Ashcroft, I., Hague, R., Galea, M., & Dickens, P. (2019). Electrical resistivity of pure copper processed by medium-powered laser powder bed fusion additive manufacturing for use in electromagnetic applications. Additive Manufacturing, 29, 100831. 40. Singh, P., & Raghav, A. (2018). 3D food printing: a revolution in food technology. Acta Scientific Nutritional Health, 2(2), 11-12. 41. Sreehitha, V. (2017). Impact of 3D printing in automotive industry. International Journal of Mechanical and Production Engineering, 5(2), 91-94. 42. Stansbury, J. W., & Idacavage, M. J. (2016). 3D printing with polymers: Challenges among expanding options and opportunities. Dental materials, 32(1), 54-64.

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43. Tang, X., & Yu, Y. (2015). Electrospinning preparation and characterization of alumina nanofibers with high aspect ratio. Ceramics International, 41(8), 9232-9238. 44. Tieber, A. (2019). Market, sales and marketing key performance indicators for products of additive manufacturing processes. Academic Journal of Economic Studies, 5(1), 42-46. 45. Tiwari, S. K., Pande, S., Agrawal, S., & Bobade, S. M. (2015). Selection of selective laser sintering materials for different applications. Rapid prototyping journal, 21(6), 630-648. 46. Tofail, S. A., Koumoulos, E. P., Bandyopadhyay, A., Bose, S., O’Donoghue, L., & Charitidis, C. (2018). Additive manufacturing: scientific and technological challenges, market uptake and opportunities. Materials today, 21(1), 22-37. 47. Trevisan, F., Calignano, F., Aversa, A., Marchese, G., Lombardi, M., Biamino, S., ... & Manfredi, D. (2018). Additive manufacturing of titanium alloys in the biomedical field: processes, properties and applications. Journal of applied biomaterials & functional materials, 16(2), 57-67. 48. Uhlmann, E., Kersting, R., Klein, T. B., Cruz, M. F., & Borille, A. V. (2015). Additive manufacturing of titanium alloy for aircraft components. Procedia Cirp, 35, 55-60. 49. Uz Zaman, U. K., Rivette, M., Siadat, A., & Mousavi, S. M. (2018). Integrated product-process design: Material and manufacturing process selection for additive manufacturing using multi-criteria decision making. Robotics and Computer-Integrated Manufacturing, 51, 169180. 50. Ventola, C. L. (2014). Medical applications for 3D printing: current and projected uses. Pharmacy and Therapeutics, 39(10), 704. 51. Vijayavenkataraman, S., Fuh, J. Y., & Lu, W. F. (2017). 3D printing and 3D bioprinting in pediatrics. Bioengineering, 4(3), 63. 52. Wang, X., Jiang, M., Zhou, Z., Gou, J., & Hui, D. (2017). 3D printing of polymer matrix composites: A review and prospective. Composites Part B: Engineering, 110, 442-458. 53. Wang, Y. C., Chen, T., & Yeh, Y. L. (2019). Advanced 3D printing technologies for the aircraft industry: a fuzzy systematic approach for assessing the critical factors. International Journal of Advanced Manufacturing Technology, 105(10).

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54. Lin, Y. C., & Chen, T. (2020). A multibelief analytic hierarchy process and nonlinear programming approach for diversifying product designs: Smart backpack design as an example. Proceedings of the Institution of Mechanical Engineers, Part B: Journal of Engineering Manufacture, 234(6-7), 1044-1056. 55. Yang, Y., Chen, Y., Wei, Y., & Li, Y. (2016). 3D printing of shape memory polymer for functional part fabrication. The International Journal of Advanced Manufacturing Technology, 84(9), 2079-2095. 56. Yeung, C. M., Yu, K. M. K., Fu, Q. J., Thompsett, D., Petch, M. I., & Tsang, S. C. (2005). Engineering Pt in ceria for a maximum metal− support interaction in catalysis. Journal of the American Chemical Society, 127(51), 18010-18011. 57. Zocca, A., Lima, P., & Günster, J. (2017). LSD-based 3D printing of alumina ceramics. Journal of Ceramic Science and Technology, 8(1), 141-148.

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CHAPTER

2

APPLICATIONS OF 3D PRINTING IN ELECTROCHEMICAL ENERGY DEVICES

CONTENTS

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2.1 Introduction ....................................................................................... 26 2.2 3D-Printing Electrodes for Applications Using Electrochemical Energy ........................................................................................... 29 2.3 Structure of the Support of 3D-Printed .............................................. 32 2.4 3D-Printed Electrolyzer Devices ........................................................ 42 2.5 Electrochemical Energy Storage and 3D Printing ............................... 45 References ............................................................................................... 61

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2.1 INTRODUCTION The globe is currently experiencing an climate and energy emergency. Manhood is producing greater greenhouse gas productions and rapidly depleting our present stock of fossil fuels, like gas, coal, and oil. According to the International Energy Agency’s (IEA) latest “Key World Energy Statistics” paper, the consumption of the energy of the world based on fossil fuels in 2015 was around 8 Gtoe. Use of the world’s use of fossil fuel-based resources has doubled since the IEA published the first “Key World Energy Statistics” bulletin. Through the year 2112, the earth’s remaining reserves of fossil fuel are projected to be depleted at the current rate of depletion (Wang & Domen, 2019). In the last half-century, international and (EU) measures have been applied in an attempt to fight the aforementioned challenges. Overall, these policies advocate for a reduction in the use of carbon-based fossil fuels, an increase in the usage of sources of renewable energy, and a decrease in releases of greenhouse gases. Numerous research paths can be pursued to attain these objectives, including the development for storage and electrochemical energy conversion applications of next-generation materials/electrodes. Water splitting, commonly known as electrolysis, is currently the subject of extensive research in the field of energy conversion. Water intense is the process of contravention down H2O into O2 and H2as a outcome of an electric charge being applied. A variety of renewable energy mehtods, such as wind farms or solar panels, can provide the outside electric charge required to divide the water. For buildings The H2 can then be routed to restricted fuel cells to generate electricity (Roy et al., 2019). Otherwise, H2 gas formed by electrolysis process of water may be injected from fueling places in a vehicle and used in the interior fuel cell in a vehicle to power the electric motor. Because H2O is the only consequence, this method of generating power is considered to be environmentally friendly. Unfortunately, because the currently used catalysts employed in the mechanism of electrolyzers are dependent on the luxurious and scarce group of platinum metals, especially Pt, RuO2 and IrO2, water electrolysis accounts for just 4% of global H2 production. These platinum group metals catalysts must be substituted with cost efficient materials which can compete or outdo the act of the modern catalysts to enhance the electrolysis efficiency of water, and therefore the total energy generation way. As a result, researchers throughout the world

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have been attempting to build electrodes and devices using more costeffective manufacturing methods to decrease the cost of water splitting technology (Shafiee & Topal, 2009; Elliott et al., 2017). If the world is to be free of the detrimental effects of fossil fuel combustion, other substitute technologies of energy must be more researched and pushed out in combination with the water electrocatalysis electricity approach.As a result, it’s not unexpected that research into battery and supercapacitor technologies is exploding, as indicated by the growing number of articles published in these fields over the last time (Godwin et al., 2018). Despite the fact that battery and supercapacitor technologies are well established, materials of next-generation are required to extend the useable time of these devices such as to prevent material degradation throughout the cycle of charging and discharging, to control at a quicker degree than is now possible. Batteries and supercapacitors store energy in very different ways. Supercapacitors store charge using electrostatic principles, whereas batteries store charge through redox reactions. Nevertheless, similar to water electrolysis, both of these technologies are receiving extensive investigation in attempt to change how people convert and store energy (Strickler et al., 2019).

Figure 2.1. 3D printing, photolithography, and nanoarchitectonics are examples of electrochemical energy electrode creation and modification processes. Source: https://pubs.acs.org/doi/abs/10.1021/acs.chemrev.9b00783

Recently, there has been a lot of research into (3D) printing, a way to make devices and electrodes for the applications of electrochemical energy conversion and storage. 3D printing, or additive manufacturing, is a process

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which permits for the rapid prototyping of sophisticated and simple 3D objects from a variety of raw materials (Zhang et al., 2018; King et al., 2019). Over a deposition process in layer-by-layer assembly managed by (CAD) software, a photogrammetry, or3D printing, 3D scanner permits the consumer to produce a 3D assembly. Nowadays, 3D printing is a versatile manufacturing process, since it can be utilized with a variety of precursor materials to create both insulating and conducting goods. Charles Hull invented 3D printing in 1986, using an UV laser to promote polymerization in resin materials. Stereolithography is the name for this 3D printing method (SLA). Other 3D-printing methods have swiftly emerged since the development of SLA, selective laser sintering, selective laser melting, binder jetting (BJ), direct ink writing, fused deposition modelling and digital light methods are just a few of the 3D-printing techniques now accessible (DLP). As a result, 3D printing, in comparison to alternative electrode-fabrication technologies like nanoarchitectonics or photolithography, provides a unique platform because it is a versatile and adaptive technology (Stauss & Honma, 2018; Pang et al., 2019). 3D printing of devices and electrodes provides for a wide range of geometry, rigidity, size, and porosity features. Controlling these attributes depends on the precursor materials used and the 3Dprinting technology used. The size of 3D-printed objects can range from the mm scale to well past the m scale, reliant on the 3D-printing technology. In the production of instruments for electrochemical energy uses, this adaptability is critical. Furthermore, 3D printing can be used to create conductive substrates and electrodes. Nanoarchitectonics is the coherent materials strategy of using nanotechnology and other domains of chemistry including electrochemistry, self-assembly and supramolecular chemistry. Photolithography is the alteration of an previously present technology. These two procedures can be used to modify 3Dprinted electrodes after they’ve been printed, but they can’t be utilized to make the electrode and the structures of the devics (Cao et al., 2019).

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Table 2.1. Disadvantages and Advantages of 3D Printing, Nanoarchitectonics, and Photolithography in Comaprison to the Production of Electrodes for Applications using Electrochemical Energy Techniques

Disadvantage

Advantage

3D printing

requires postfabrication methods

Electrodes may be fully manufactured via 3D printing, requiring no clean room or specialised workers, and are scalable for energy applications.

photolithography

a long lead time is required Personnel with high levels of expertise are required. There are numerous steps to the final electrode in a clean room, and you’ll need separate support to get started.

complex designs can be formed

nanoarchitectonics

Many steps to the finished electrode require highly skilled workers, and distinct support is required to begin.

conductive and complex materials can be synthesized

For electrochemical energy-conversion methods the efficiency of 3D-printed devices, such as the OER and HER is all about printing modification of the parts (HER).

2.2 3D-PRINTING ELECTRODES FOR APPLICATIONS USING ELECTROCHEMICAL ENERGY For water splitting applications there are a variety of 3Dprinting processes that may be used to build 3D printed electrode supports, as described earlier in this Review. Furthermore, there are a number of precursor materials that can be utilized in each of these procedures. As a result, the 3D-printing technique utilized is dictated by the material from which the electrode must be manufactured. FDM, for example, would be the 3D-printing method of excellent for fabricating an electrode through thermoplastic materials including polyurethane, acrylonitrile butadiene styrene and. polylactic acid (Pascuzzi et al., 2020). Various groups have used FDM 3D printing to make electrodes used in OER and HER. Foster and his colleagues were the first to use FDM to print graphene and PLA based electrodes for the HER.

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They used a viable filament named “Black Magic.” Regrettably, the printed electrode of graphene has weak HER performance due to conductivity difficulties with the commercial filament. Post fabrication adjustments to these graphene/PLA electrodes are required to obtain greater conductivity and, as a result, a very common electrode support for water splitting (Yan et al., 2016). Other merhods such as SLA is another choice to make a device from nonconductive polymers; nevertheless, electrode supports must be conductive for this production method to work. As a result, in case where SLA is used to make support structures, an additional phase to bond a conductive coating is required. Ding and coworkers, for example, used a commercially available PlasClear resin to 3D print a rectangular-shaped interlocked electrode for the OER. Because the electrode from 3D-printing was constructed from the insulating substance, a series of procedures were required to create a conductive device for catalyst to be deposited in active OER method. 1st , the electrode surface was sensitized and activated by dipping the electrodes in two commercially available electroless solutions for 5 minutes each: “copper solution electroless C,” which contains 5 wt percent HCl along with 5 wt percent SnCl2, finally, “copper solution electroless D,” It comprises 5 percent HCl and 5 percent PdCl2, along with sodium. After drying in a 60°C oven, the electrode was dipped in 5% H2SO4 for 5 minutes before being washed with DW. The electrode was immersed in a viable solution of electroless comprising of C4H4, Na2O4, , NaPO2H2, HF, and NiCl2 for 30 minutes at 97 °C to generate a NiP conductive layer. Ding and colleagues showed that at a current density of 10 mA cm2, the conductive NiP/PlasClear electrode from 3D-printing had an OER of 1.53 V vs relative hydrogen electrode (RHE) (Browne et al., 2019). The performance of OER is now quite strong, since a potential of 1.53 V vs RHE equates to an OER overpotential of 300 mV, that is comparable to that of current-generation OER catalysts; the most wellknown OER catalysts, RuO2 and IrO2, have overpotential values of around 300 mV at 10 mA cm -2.

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Figure 2.2. In the literature, there are numerous structures of electrodes 3Dprinted created for splitting of water. Basket shape (A) [Ambrosi & Pumera, 2018]. Mesh shape (B) [Ambrosi & Pumera, 2018]. [Ambrosi et al., 2016] Ribbon form (C). [Foster et al., 2017] (D) Circular form. Springer Nature, 2017. All rights reserved. (E) A void-shaped circular. With permission from ref Browne et al. (2018), reproduced/adapted. American Chemical Society. All rights reserved. (F) The form is square. [Browne et al., 2019] Wiley and Sons, Inc., Wiley and Sons, Inc., Wiley & Sons, Inc (G) Mesh with a square shape. [Su et al., 2019]. Source: https://pubs.acs.org/doi/abs/10.1021/acssuschemeng.8b04327

Finally, because SLM uses just raw materials from metal powder, this sort of three dimensional printing is required if a conductive-based electrode needs to be created in a single step. This sort of metal three dimensional printing is, without a doubt, the most common choice for water splitting electrodes. This is most probable due to the fact that, unlike FDM and SLM, SLM electrodes do not require any extra treatments to become conductive devices. Inappropriately, because none of the SLM printing precursor materials are especially dynamic for the HER or the OER ingredients are frequently put on the SLM devices to provide active splitting of water catalysts (Zhu et al., 2019). The water splitting capacities of these electrodes were tested after they were immersed in 1 M KOH. At current densities of 10 and 10 mA cm2, the HER and OER potentials were 0.45 and 1.6V, respectively. As a result, any three dimensional printing process, such as

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SLM, SLA, and FDM, must take additional measures to adapt the electrode surface to these reactions in order to develop a highly active electrode for water splitting applications. Changes to the electrode support’s structure to allow water splitting or post printing changes like ALD to cover active HER or OER electrode on the electrode to advance activity are examples of such steps. The following sections will go over both of these options (Maeda & Mallouk, 2019).

2.3 STRUCTURE OF THE SUPPORT OF 3D-PRINTED The geometry of the HER and OER is critical, Because it has the potential to aid or obstruct the evolution and separation of gases from the electrode surface. Bubbles can form and passivate the electrode’s surface if the O2 and H2 gases are not evacuated, resulting in a reduction in activity assessed by galvanostatic or potentiostatic methodshe experimentalist may conclude that the placed catalyst is not active for the OER/HER because of this dropin activity, when it is actually because of the to a poor design of the electrode . Gas can be trapped at the base of a electrode of glassy carbon with the active zone of located on the corner of a polytetrafluoroethylene rodlike arrangement, resulting in the accumulation of gaseous products like H2 or O2 (Kumar & Himabindu, 2019; Yang et al., 2019).

This difficulty can be easily handled by 3D printing electrode supports that are intended to avoid gaseous product accumulation, enabling for effective analysis of conversion of electrochemical energy catalysts. A variety of complicated structures, such as meshes, ribbons, baskets, and upright circular plates, have been printed for the HER and the OER, according to the literature (Figure 2. 2). For instance, similar assembly has described on employing SLM to construct stainless steel, ribbons, baskets and meshes using 316L stainless steel particles from Concept Laser GmbH, allowing for a evaluation of various structures as a function of HER and OER action. At 5 mA, the electrode of basket has a potential of 1.7 V versus RHE, the electrode of ribbon-like has a potential of 1.55 V versus RHE at 10 mA cm2, and electrodes of mesh-structured have a potential of 1.6 V versus RHE (10 mA cm2).As a result of these OER measurements, the ribbon is the best base electrode geometry, trailed by a mesh, and then the basket design. Surprisingly, the no holes electrode is the best electrode, suggesting that permeable assemblies obstruct oxygen development by preventing bubbles from cracking. Additionally, the mesh electrodes and stainless-steel basket

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were used as functioning electrodes, with potentials of 0.55 V against RHE at 0.45 V and5 mA at 10 mA cm2, respectively. According to a comparison of HER action with the shape of the electrodes of 3D-printing, the electrode of basket is a least operative assembly for splitting of water (Fu et al., 2019). Enhancing the roughness of the surface of the active region, threedimensional electrodes printing of metal with varied surface microstructures has been researched to improve applications of conversion of electrochemical energy. SLM was used in one experiment to make TiO2Ti-centered electrodes for photoelectrochemical oxidation of water (Figure 2. 3) (Le et al., 2019).

Figure 2.3. Influence of 3D-printed electrode structure on efficiency of photoelectrochemical. (A) 0 conical arrays, (B) 216 conical arrays, and (C) 407 conical arrays on TiO2Ti electrodes. (D) At the same voltage, photoelectrochemical performance of TiO2Ti-centered electrodes with 0 (black), 217 (blue), and 407 (red) conical arrays. (Gannarapu et al., 2016). Source: https://onlinelibrary.wiley.com/doi/abs/10.1002/aenm.201770122

The TiO2Ti-based electrodes all had the similar geometric area, though, a flat surface was observed in one electrode, another contain 216 conical arrays, the last electrode contain 407 conical arrays. The idea in the conical arrays is to enhance the electrode’s deceptive surface area, which would increase the absorption, parting of hole and electron pairs and irradiation light, the later being a main stumbling barrier in the field of PEC oxidation of water (Browne et al., 2020). The flat electrode, the 407 conical array electrode all had photocurrent densities of around 0.19, 0.25, and 0.31 mA cm2 at

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a potential of 1.23 V vs RHE, suggesting that the conical microstructures promote PEC water oxidation. Because micro sized features may be constructed to enhance flat-based metal electrodes, this reading reveals that SLM 3D printing may be utilized to tailor metal-centered electrodes for PEC oxidation of water. Unfortunately, due to device limitations, SLM is unable to yield nanosized structures that can develop PEC oxidation of water features even further; though, given the rapid step of advancement in the 3D-printing arena in terms of the development of improved printers, nanostructure fabrication by 3D printing is on the perspective (Santos et al., 2019). Table 2.2. Modification Methods for Electrodes from 3D-Printing Revision Techniques

Limitations

Benefits

electrodeposition

Semi-uniform deposition and electrodeposition solutions may cause environmental damage.

low cost, facile, vari- ( Mallik & Ray, ous metal oxides and 2011) metals can be placed

ALD

luxurious equipment needed, require a skilled consumer to do the ALD

Adapts the surface, uniform, various metal oxides and metals are placed

potentiostat polishing

procedure and may be affluent; materials utilized in the refining may change the metal

increases the smooth- ( Huang et al., 2017) ness l, increases the lifetime of the meta and reductions brittleness related with the metal, metal can convert eroding free

electrochemical activation

semireproducible

low cost, quick

( Foster et al., 2017)

anodization

semiuniform alteration, only a some of materials can experience anodization

facile, low cost

( Chitrada et al., 2015)

enzyme activation

semireproducible

ecologically pleasant, ( Wirth et al., 2019) manageable

solvent activation some solvents can become injurious to health, e.g., DMF in women

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low cost, quick

ref

( George, 2010)

( Gusmão et al., 2019)

Applications of 3D Printing in Electrochemical Energy Devices thermal activation

After thermal activation, PLA-based electrodes become exceedingly brittle; thermal activation shloud be performed in a controlled environment or the electrode will turn to powder.

for graphene centered electrodes the thermoplastic is carbonized

35

( Novotný et al., 2019)

Electrodes for electrochemical energy conversion applications were constructed using a commercial graphene/PLA filament and FDM 3D printing, as previously mentioned (Figure 2. 2D and E). Electrodes with diverse structures have been described, just like 3D-printed metal electrodes. The HER was tested on spherical electrodes having a hole in the centre. Lacking any alteration of the graphene electrodes, only spherical electrode and the spherical electrode having a hole in the middle demonstrated HER current densities of 0 and 1.5 mA cm2 at an overpotential of 1 V vs RHE (Foo et al., 2018) . When the two 3D-printed structures are compared, it appears that the spherical construction having the hole performs superior in terms of HER.

Figure 2.4. (A) Diagram of the 3D-printing procedure, from design of electrode to printed electrode modification. (B) IrO2 metal is electrodeposited on the electrode from 3D-printing. (C) Pt metal is electroplated onto the electrode from 3D-printing. (D) Ni metal is electroplated onto the 3 electrode from 3Dprinting. (E) LSV curves for water splitting for modified 3D-printed electrodes.

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(Ambrosi & Pumera, 2018) ALD onto a stainless steel 3D-printed electrode and (G) the ALD procedure. (Browne et al., 2019) (F, G). (H) Microconical arrays electrode design and (I) anodization procedure (Gannarapu et al., 2016). Source: https://onlinelibrary.wiley.com/doi/abs/10.1002/adfm.201700655

The recognized conductivity difficulties through the electrodes made with this viable graphene/ PLA could explain this improvement in HER performanceThe electrode design is essential as the filament merely holds 8 percent graphene by weight. When more filament is utilised to 3D print, the chance of the electrode to be least conductive increases, which could explain why the complete spherical electrode is least active as a HER electrode when associated to the spherical electrode having a hole. When paired with FDM, this commercial filament creates a cost efficient substitute to 3D printing of metal for the production of parts from 3D-printing; nevertheless, these pieces when employed as electrodes, PLA has drawbacks. Because PLA disintegrates in aqueous solutions with the passage of time because of PLA chain cleavage, and because the HER is done in aqueous solutions i.e., NaOH, over time use of these graphene electrodes is a problematic as the electrode’s reliability might be in problem (Manzanares et al., 2018; Ngo et al., 2018). Post modification printing techniques must be carried out on electrodes from 3D-printing, irrespective of the fact that the electrodes were manufactured using SLM, SLA, or FDM 3D printing. This is to advance the electrodes for the electrochemical reaction.

2.3.1 Metal Electrodes from 3D-Printing Making electrodes with 3D printed metal is simple and quick. However, the presently offered precursor 3D-printing metal powders are not known to be effective in water splitting; thus, metal-printed electrodes must be adjusted to contest with current state-of-the-art water splitting catalysts. Low-cost post modification procedures, like solvent, heat, and enzyme treatments, can be used on PLA-based electrodes (Manzanares et al., 2018).

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Modifying metal electrodes manufactured in 3D for water splitting applications can be done using a variety of approaches. Electrodeposition, ALD, and anodization are examples of these, each with its own set of benefits and drawbacks. Electrochemical techniques such as electrodeposition and anodization outcomes in the formation of a semi uniform metal oxide or metal coating. Anodization causes the development of the natural oxide of the metal. Electrodeposition creates a layer of material from a solution comprising of precursors of a metal salt, whereas anodization causes the development of the natural and inherent oxide of the metal. These two methods are cost effective and straightforward to use, but ALD may provide you more regulation over the uniformity of the layer (Parra et al., 2018). When it comes to depositing metals or metal oxides onto electrodes from 3D-printing, ALD has some limitations. ALD is a costly technology that requires the expertise of a trained professional to use. The most common application of electrodeposition has been for the placement of active materials for electrodes from 3D-printing. Every shape or form electrode may be adjusted with a variety of active materials for splitting of water like Ni, NiP, Pt, IrO2, NiFe oxide, NiMoS2, and MoS2 by electrodeposition. This approach was utilized by Ambrosi and colleagues onto a 3D stainless steel basket-shaped electrode to place Ni and Pt for the HER and Ni and IrO2 for the OER and. Multiple cycling 3D stainless steel basket-shaped electrode in a handmade iridium chloride solution within the voltage limits of 0.6 and +0.6 V versus Ag/AgCl was used to deposit the IrO2 (Figure 2. 4B). Using a chrono potentiometric regime, In a viable platinum coating solution, the Pt was plated on the basket 3D electrodes by using a decreasing current of 2 mA cm2 for 30 minutes. Finally, under chronoamperometry control, the Ni was electrodeposited in a nickel chloride-based solution by using a voltage of 1 V versus Ag/AgCl for 1 hour. (Figure 2. 4D) (Hughes et al., 2017)

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Figure 2.5. (A) Diagram of the 3D-printing procedure, from design of electrode to printed electrode modification. (B) IrO2 metal is electrodeposited on the electrode from 3D-printing. (C) Pt metal is electroplated onto the electrode from 3D-printing. (D) Ni metal is electroplated onto the 3 electrode from 3Dprinting. (E) LSV curves for water splitting for modified 3D-printed electrodes. (Ambrosi & Pumera, 2018) ALD onto a stainless steel 3D-printed electrode and (G) the ALD procedure. (Browne et al., 2019) (F, G). (H) Microconical arrays electrode design and (I) anodization procedure (Lee et al., 2017). Source: https://pubs.rsc.org/en/content/articlelanding/2020/se/c9se00679f

The OER catalysts were tested using improved 3D stainless steel basketshaped electrode with IrO2 and Ni layers. The IrO2-modified basket electrode outperformed the Ni-modified electrode in terms of OER, as represented in Figure 2. 4E. Furthermore, the 3D-printed Pt-modified basket electrode

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outperformed the Ni-modified electrode as the best electrode for the HER. Furthermore, this group has demonstrated that electrodeposition of IrO2 can increase when equated to the printed electrode of stainless-steel, the OER efficiency of 3D ribbon-shaped stainless-steel electrodes (Ariga et al., 2012; Hughes et al., 2017). SLM has previously been used in combination with ALD and anodization to tune the PEC water oxidation surfaces of metal three-dimensionalprinted electrodes. In a research, SLM has been used to manufacture square electrodes of stainless-steel; however, because to stainless steel’s lack of PEC water oxidation characteristics, the surfaces of the 3Dprinted electrodes were customized with TiO2 with the help of ALD (Figure 2.4FG) (Browne et al., 2020). TiCl4 was used as a precursor and H2O was used as a reactive in the ALD process. The number of cycles performed determined the width of the TiO2 layer placed on the electrode from 3D-printing. Quantifiable TiO2 films of varying widths were placed and analyzed as PEC oxidation of water catalysts in this research. The thicknesses of the layers of TiO2 were measured using ellipsometry before the electrochemical evaluation and found to be 77, 54 and 28 nm for the ALD cycle numbers of 1200, 800,and 400 respectively. The performance of the TiO2 layer rose with growing TiO2 thickness, which was connected to the crystallinity of the layer, according to the PEC water oxidation investigations (Mayorga et al., 2018). Wallace and coworkers used SLM printing to create another study used electrodes from 3D-printing for PEC oxidation of water, though the SLM printing technique was done with precursor of Ti metal powder. Wallace and his colleagues constructed several electrodes having a flat base including microconical arrays, which were different from those used in the prior PEC water oxidation investigation (Figure 2. 4H). As a result, three electrodes with 0, 216, and 407 microconicals were made for this study (Kim et al., 2017).

2.3.2 Polymer-Based Electrodes from 3D-Printing Because FDM 3D printers are substantially fewer expensive than SLM 3D printers, FDM is a preferred substitute to SLM. In addition, even inexperienced users can utilize FDM 3D printers. As a result, there have been a slew of recent reports on the “Black Magic” graphene/PLA filament, which is commercially accessible,being utilized in FDM 3D printing to make electrodes. This commercial filament’s electrodes have been employed in

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a variety of electrochemical applications, such as sensors, supercapacitors, and water splitting (Huang et al., 2019). Various post modification procedures have been carried out to increase the conductive properties of these 3D-printed graphene and PLA electrodes. Conductive materials having electrodeposition like electrochemical activation, Au, enzyme activation, solvent activation, and heat activation are examples of these treatments. The development of the post modification stages in connection to this filament for splitting of water will be discussed in this section (Su et al., 2005). The initial study on the printed and post-modification handling for “Black Magic” filament for splitting of water was published in 2017, specifically for the HER. The primary HER activity of the electrodes printed from 3D was boosted by the electrodes cycling in acidic fluid between voltage of 0 to 1.5 V against SCE. The HER efficiency of the 3D-printed electrodes improved after 100 cycles and even more after 1000 cycles (Figure 2. 5A) (Vernardou et al., 2017). The rise in HER activity, according to the scientists, is related to the hydrolysis of PLA in the acidic solutions, that removes the PLA from the electrode. Moreover, the researcher used energydispersive X-ray (EDX) spectroscopy to detect Ti metal in the filament, and they the consistent improvement in HER performance throughout cycling was connected to the comparative rise of Ti metal in the electrode from 3D-printing because of the decline in PLA (Maurel et al., 2019). Other researches show phosphatebuffered saline (PBS) solution for electrochemical activation in combination with activation with solvent for asprinted “Black Magic” graphene and PLA electrodes from 3D was carried out and evaluated on HER electrodes. In PBS solution, electrochemical activation for 150 s at a voltage of 1.5 V vs Ag/AgCl increased the HER efficiency of viable raphene and PLA electrodes from 3D when equated to the printed electrode. A rise in oxygenated graphitic material on the electrode’s surface was connected to an increase in HER activity.Moreover, electrochemical impedance spectroscopy (EIS) studies revealed that the electrochemically activated electrodes had a small decrease in resistive behavior (Lee et al., 2019; Su et al., 2019). The HER performance of the electrodes from 3D improves after solvent activation in N,N-dimethylformamide (DMF) for 10 minutes, compared to the electrochemically activated and as-printed electrodes, the physical spalling of the PLA from the electrode increases the availability of active graphene-based materials throughout the system. Surprisingly, in

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this study, the optimum post manufacturing treatment for HER performance was a mixture of the two previous activation approaches, namely, first DMF activation, then electrochemical activation. The increased development in the HER for the DMF/electrochemical activation 3D-printed electrode was explained by the decrease of PLA in the electrode and thus the improved conductivity determined by EIS, as well as the oxidation of the graphene at the electrode’s surface to functionalized graphene observed by X-ray photoelectron spectroscopy (XPS) (Gannarapu et al., 2017). The filament contains a variety of impurities, according to a latest research into the nature of the improved splitting of water capability of these electrodes from 3D-printing generated from the marketable “Black Magic” filament. Before any printing is done, an EDX study revealed that the filament has metal impurities of Al, Fe, and Ti. Furthermore, the printed electrodes were activated via DMF in this study, and both activated with DMF and printed electrodes from 3D-printing were assessed as OER electrodes (Figure 2. 5D) (Gannarapu et al., 2016). due to the larger comparative ratio of impurities from metal because of the elimination of the PLA polymer by treatment with DMF, the electrode from DMF 3D printing was found to be the better electrode for the reaction in OER. Contaminations in such electrodes created by the filament “Black Magic” were discovered in the real filament from the manufacturing procedure, according to a follow-up research (Ambrosi & Pumera , 2018; Cheng et al., 2019).

Figure 2.6. Electrolyzer devices made with PEM 3D printing. (A) The PEM electrolyzer device is depicted schematically. (B) Images of a bipolar plate asprinted, (C) a bipolar plate that has been changed with silver paint (D) formation of other silver layer by electrodeposited. (E) I.V. arcs of an electrolyzer with the bipolar plates displayed in panel (D). (AE) (Chisholm et al., 2014) (AE) (AE) (AE) (AE) (FH) Channel structure for bipolar plates from 3D-printing, and (I)

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IV arcs of electrolyzer devices from 3D-printing constructed with the bipolar plates depicted in panes (FH). (F−I) (Yang et al., 2018). [Source: https://ideas.repec.org/a/eee/appene/215y2018icp202-210.html]

2.4 3D-PRINTED ELECTROLYZER DEVICES The production of numerous pieces that make up electrolyzer devices, such as bipolar plates, current collectors, and electrodes, has also been done via 3D printing. In theory, additive manufacturing might reduce the cost of producing these components, creating electrolyzer skills a more costeffective and environmentally friendly way to manufacture hydrogen for a hydrogen economy. Reliant on the situation if the electrolyzer is constructed on alkaline-exchange membrane or else proton-exchange membrane tehcnique, the mechanisms which maye be 3D-printed intended for devices of electrolyzer shall be dissimilar (Browne et al., 2019). For example, it is not possible to 3D-print electrodes for PEM electrolyzers, but electrodes for AEM electrolyzers may be 3D-printed using a variety of 3D-printing methods like SLM, SLA, and FDM. The bipolar plates, on the other hand, are one of the most expensive components of a PEM electrolyzer since they must be resilient to acidic medium and simply adjusted to permit for the creation of various routes so that the reactants can get to the catalysts. As a result, expensive methods and materials, such as graphite or metals, are used to make these plates, resulting in the bipolar plates adding a substantial price to the fabrication of devices of PEM electrolyzer. According to reports, for PEM electrolyzers, bipolar plates add to 23-48 percent of the device’s price; thus, if the bipolar plates’s price might be reduced through the overall economic cost of novel fabrication ways, including 3D printing, would be reduced, dvelopin a more feasible method for energy conversion (Huang et al., 2017). For the case of PEM electrolyzers, couple of researches have created prototypes from 3D-printing utilising various techniques of 3D-printing, demonstrating the flexibility of 3D printing for these complicated structures and prototypes in large-scale. (Chisholm et al., 2014; Yang et al., 2018) Chisholm et al. demonstrated that for a PEM electrolyzer flow plates may be developed and 3D-printed by the use of cost efficient additive making technique in the first investigation (Figure 2. 6A) .

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A polypropylene polymer filament was used to make the flow plates in a 3D printer of FDM. Since conductive flow plates must be used, a coating of silver paint was applied to the flow plates and left to dry for one hour. The movement plates coated with the silver paint were then dried for twenty minutes at 120 degrees Celsius. After that, another layer of silver paint was applied, followed by electrodepositing another Ag layer for 1000 seconds at a voltage of 1 V vs Ag wire from a solution comprising 0.3 M AgNO3 in 1 M NH3. A membrane electrode assembly (MEA) was created to test the flow plates’ efficiency, employing modern cathodic and anodic PEM splitting of water catalysts Pt and IrO2, respectively, as well as a Nafion membrane. Between the the flow plates and MEA, gaskets were positioned, and the cell was sealed with a 7.5 N m compression to finish the electrolyzer device (Browne et al., 2018). To see if the 3Dprinted plates might be used as a substitute to typical viable electrolyzer plates, device was put through a current potential (IV) analysis with DW as an electrolyte, which was driven to the device at 10 mL min1 at different temperatures. The device using the electrolyte at temperatures of 70, 50, and 30 °C attained current densities of 1.09 and 1.04 A cm2 at a potential of 2.5 V, according to the IV curves (Figure 2. 6E). These findings suggest that the device as a entire could operate in an electrolyzer, although not to the same amount as other organisations who used the similar modern catalysts in profitable devices of electrolyzer. Because the thermal expansion coefficient of polypropylene is 510 times greater than that of silver at various temperatures, the authors believe for the 3D-printed device, the loss of activity is because of ohmic losses between the first layer of silver paint and the flow plate polypropylene coating. As a result, a alteration in the silver coating may occur, lowering coating coverage and causing flow plate resistance. In spite of the ohmic losses, PEM electrolyzer prototype demonstrated that working and cost efficient flow plates may be made to exchange viable flow plates (Foster et al., 2017; Ambrosi et al., 2018). Yang et al. utilized a costly additive making technique to develop diverse variants of combined bipolar plates with incorporation and without addition of a liquid and gas-diffusion layer to gain understanding of the different channel flow systems which may be made by the use of 3D printing. Stainless steel 316L powder was used to 3D print the integrated bipolar plates. During the comparison investigations, the plates from 3D-printing were exclusively used for the cathodic flank of the electrolyzer as flow plates due to the metal powder precursor choice. The writers supposed that stainless steel would be a more cost-effective alternative to

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titanium for the anodic plate, however, that it can be susceptible to anodic decomposition if used as a water oxidation plate. In this investigation, the SLM produced three different channel patterns: (1) similar flow passage, (2) a pin flow passage having an LGDL, and (3) a pin flow passage (Figure 2. 6). The electrolyzer instruments were built by the use of a bipolar plate of graphite on the anodic flank and plate from 3D-printing on the cathodic flank with aluminium plates at the end to test the performance of the bipolar plates from 3D-printing in function (Tanzi et al., 2019). A viable Toray paper gas-diffusion layer was used in place of the two bipolar plates that did not have the LGDL from 3D-printing joined into the plate. A catalyst-layered membrane , for the cathodic and anodic materials, with PtB and IrRuOx was created and in every electrolyzers introduced as the catalytic layers As a result, excluding the cathodic bipolar plate from 3D-printing, every component of electrolyzer was retained constant and any changes in the device’s efficiency can be traced back to the cathodic bipolar plate from 3D-printing. The IV arcs (Figure 2. 6I) demonstrated the performance might be improved by altering the cathodic bipolar design. At a voltage of 1.715 V, the current densities of the electrolyzer with parallel passages, pin passages, and pin passages having the LGDL were 1.579, 1.619, and 2.000 A cm2, respectively (Benck et al., 2014; Browne & Mills, 2018). The plate haiving least ohmic resistance from the measurements of EIS was found to have the highest activity of the pin channel bipolar plate with the LGDL. Comparing the the bipolar plate from 3D-printing and Toray paper GDL, the removal of the resistance from interfacial contact between the hybrid bipolar plate from 3D-printing and the LGDL arrangement resulted in least ohmic resistance for the pin passage bipolar plate having the LGDL. Furthermore, the IV curve was used to compare the 3D-printed plates to a traditional electrolyzer, revealing that every 3D-printed devices outperform the conventional electrolyzer. Intriguingly, cells from 3D-printing are lighter in volume and mass than traditional cells, which may outcomes in substantial maintenance and assembly, savings if the plates were utilized in stacks (Shi et al., 2019).

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Figure 2.7. Alkaline electrolyzer devices manufactured in 3D. (A-C) FDM and SLM 3D printed alkaline electrolyzer device; (D) LSV arcs in panels for for the electrolyzer device (A-C). (Ambrosi & Pumera, 2018) (A.D.) (E) A FDM-based alkaline electrolyzer device. Electrodes for the electrolyzer in panel (E) made of SLA (F). (G) Electrolyzer device LSV with without and with electrodeposited Ni, the Ti electrodes from panels (E and F). (Hornés et al., 2021). Source: https://onlinelibrary.wiley.com/oi/abs/10.1002/admt.201900433

In this regard, it is crucial to mention that the bipolar plate electrolyzer from 3D-printing manufactured from viable conductive PLA thermoplastic may not be a candidate for electrolyzer devices with next-generation bipolar plate for future bipolar plate electrolyzer from 3D-printing. Relating the low ohmic resistances of the substitute electrolyzers in the research (0.1), the significant potentials displayed by a C-CGPLA electrolyzer are linked to the large ohmic resistance. The C-CGPLA electrolyzer’s poor performance is linked to earlier researches stated before in this Analysis that used this viable PLA conductive thermoplastic for 3-electrode-cell splitting of water analysis, as such researches found that electrodes from 3D-printing made from this easily accessible filament yield poor electrodes, which is linked to the C-CGPLA electrolyzer’s poor performance (Hornés et al., 2021).

2.5 ELECTROCHEMICAL ENERGY STORAGE AND 3D PRINTING In the field of energy storage, 3D printing is gaining popularity since it permits for the quick production of complicated geometric objects with

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high accuracy. Because it allows for precise control over the thickness and geometry of the electrodes, 3D printing is an excellent method for constructing 3D designed electrochemical energy structures. It is also possible to present porosity into 3D-printed items using 3D-printing processes (Rodriguez et al., 2016). First, the density of the infill could be made to favour electrolyte ingestion and hence boost conductivity in the printed items. Next, modifying a 3D-printed object after it has been produced can increase its porosity. Freeze-drying after ink writing, for example, will vaporize the solvent from the ink, resulting in macroporosity. It is unclear whether 3D printing has a favourable effect on microporosity (pores smaller than 2 nm). Some preliminary investigations revealed that to support microporous carbons by the use of a polymeric matrix can clog micropores, and for EES, reducing the electrodes’ active surface area, that will be examined more in this portion of the analysis (Walsh & Ponce, 2014). We will look at the efficiency of electrodes from 3D-printing for electrochemical storage of eneergy, such as batteries and supercapacitors, employing a variety of 3D-printing precursor for 3D-printing and after 3D-printing alterations of the printed components in this section of the Review.

2.5.1 Supercapacitors 2.5.1.1 3D-Printed Electrodes for Electrochemical Storage Applications: Methods and Precursor Materials Up to the present time, a variety of 3D-printing methods and, as a result, precursor are being used to build supercapacitor-associated electrodes and devices, including SLM, FDM systems. PES is one of the most basic and extensively used 3D printing processes for printing multi-component structures for supercapacitor electrodes; nevertheless, the slurries of precursor should be adjusted. The rheologic parameters of the slurries utilzied to make 3D-printed supercapacitor electrodes have a significant impact on the printability and structure (Yang et al., 2018). The visco-elastic behavior of the slurry should permit coaring at a definite rate of feeding, keeping the printed product’s shape. Areir and colleagues investigated this link by creating extrusion 3D printing pastes with different concentrations of activated carbon and polyvinyl alcohol in a solution. Suitable blend of these constituents is critical in dispersions as the PVA can pass through the nozzle faster than the particles of activated carbon, keeping a grade of activated carbon particle concentration, that will certainly result in an electrode that

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is not homogeneous. While by the use of a gel PVA/H2SO4 electrolyte, the supercapacitor device from 3D-printingcan offer 0.121 F g1.118. The device’s greatest electrochemical efficiency is tied to the visco-elastic behavior of the paste of electrolyte and electrode, as well as their capacity to be 3D printed. This 3D-printing technology permits the current collector, electrode, and electrolyte to be printed one after the other, which is ideal for supercapacitor device fabrication. PVA and activated carbon based slurry was created in water and used as the precursor of 3D-printing, as in the prior study. In a 2 M H3PO4 electrolyte, the 3D printed supercapacitor had a capacitance of 0.2 F g1, and a specific power of 57.60 W kg1, with 56 percent of the capacitance remaining after 500 cycles. The energy-storage characteristics of the 3D-printed supercapacitor demonstrated good consistency; thus, this feasible and cost efficient approach might be employed to create even complicated devices for wearable devices (Chitrada et al., 2015Mebed et al., 2019).When compared to other supercapacitor devices printed using alternate 3D-printing processes, including SLM, the cycle stability of these PES-produced devices is substantially lower; thus, more advances in this 3D-printing field are required. Multilayer supercapacitor components can be 3D printed using a dual-nozzle technique. In one case, water was used to prepare carbon and a PVA-based slurry. In 1.6 M PVA/ H2SO4 electrolyte, a 3D-printed supercapacitor cell delivered 38.5 mF g-1 at 0.136 mA g1. The conductivity and specific capacitance decreased as the electrode thickness was raised, probably due to reduced ion diffusion across the extremely viscid electrode (Wirth et al., 2019). Two distinct systems of 3D printing can work together to create numerous constituents of a supercapacitor that require different sorts of precursors. The multimaterial system of 3D printing has a benefit above distinct FDM and paste-extrusion systems of3D-printing in that the supercapacitor from 3D-printing can be created lacking any removal from the printing bed and moving it to alternative bed, resulting in great dimensional precision. A pasteextrusion and FDM printer system were utilised in a study by Tanwilaisiri and colleagues to build a system of 3D-printing to print a supercapacitor device by the use of different precurors using an paste-extrusion and FDM printer system. The supercapacitor device’s packaging frames were 3D-printed utilising FDM printing and PLA in the production procedure. The system of paste-extrusion was utilised to print the electrode, current collector during the same process (Gusmão et al., 2019). Activated carbon was combined with sodium carboxymethyl cellulose in ethanol/water to make the slurries used to print the electrode material. In 1.5 M PVA/H3PO4 electrolyte, the 3D

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printed supercapacitor cell can supply 238.42 mF g1 at 0.0159 A g1. It has an energy density of 76.26 mW s g-1. Unfortunately, because of the hindering diffusion of ions through the activated carbon electrodes of 3D-printing, this multimaterial 3D-printing technology produces a very resistive cell of supercapacitor. To increase the energy-storage qualities of the devices created from this multimaterial system, the viscosity of the slurry and the 3D-printing process must be tuned (Novotný et al., 2019). Supercapacitors have also been manufactured using FDM. Various kinds of filaments could be utilzied, even though PLA filaments are the most common for EES. Because PLA is an insulating substance, the conductivity of the filaments and therefore the items from 3D-printing composed of PLA must be increased before they can be used as EES components. Extruding mixes of PLA and further conductive constituents, that can eventually act as active constituents on the electrodes, is one way to give the filaments conductivity. The procedures for producing bespoke filaments for FDM are shown in Figure 2. 8AD. For the active materials to be fully utilised, the shape of the printed items must be optimised. If the finishing electrical or ionic conductivity does not meet the specifications, dissolving or pyrolysis can be used to reduce the amount of PLAq. Foster et al. employed FDM 3D printing to produce electrodes for solid-state supercapacitors using a widely available filament made comprised of graphene and PLA. The specific capacitance of these supercapacitor cells in electrolyte of 1 M PVA/H2SO4 is 17.17 F g-1. While equated to non-3D-printed supercapacitors, however, these are very low capacitance values (Germscheidt et al., 2021). Direct ink writing is a new type of additive fabrication which has been used to make graphene and graphite oxide supercapacitors by several organisations. The supercapacitor performance of devices 3D-printed using DIW outperforms that of supercapacitors manufactured using FDM 3D printing in general. Figure 2EH displays the procedures of 3D printing with DIW. Zhu et al. (2019) constructed a symmetric capacitor with a gravimetric capacitance of 4.76 F g-1 and 95.5 percent afterr 10,000 cycles capacitance retention on the basis of a graphene aerogel from 3D-printed and DIW in 3 M KOH. The composite of graphene aerogel was made by direct ink writing to make a porous graphene architecture. The printable ink was made with GO, a solution of resorcinol, hydrophilic fumed silica, formaldehyde in 2,2,4-trimethylpentane and graphene nanoplatelets as the solvent (Wei et al.,

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2015). The mass stacking of GO and graphene nanoplatelets in the 3D-printed supercapacitor was adjusted to obtain a favourable balance of capacitance and conductivity. Figure2.9A depicts the rate capability of 3D-printed electrodes of various configurations. The incorporation of graphene nanoplatelets to the GO solution enhances the composite’s conductivity while reducing the final composite’s specific surface area. The inclusion of hydrophilic fumed silica functions as a viscosifier, giving a shear thinning behaviour and high shear yield stress, while increasing the concentration of graphene oxide boosts the printability. Finally, organic sol gel chemistry causes a postprinting gelation when resorcinol and formaldehyde are mixed. As a result, this ink has the potential to be a shear thinning non-Newtonian fluid with a high yield stress and storage modulus. Supercritical drying, Gelation, carbonization, and hydrofluoric acid etching of the silica transform the printed electrodes into aerogels (Santos et al., 2019). Yun et al. demonstrated that DIW can make 3D-printed GO hydrogels. To get acceptable inks for printing, the rheological qualities of the inks were also carefully altered. The 3D-printed electrodes were chilled to 80 degrees Celsius for 2 hours, then freeze-dried for 12 hours before being condensed with hydrazine hydrate steam in a hydrothermal process at 100 degrees Celsius for 5 hours. These electrodes were subsequently used to make supercapacitors in a 1 M PVA/H3PO4 electrolyte, which produced a gravimetric capacitance of 20.2 F g-1 . Irregular supercapacitors can also be made using 3D-printing methods. DIW created the first 3D printed asymmetric supercapacitor with Shen and coworkers. The negative or positive electrodes in this work were made of vanadium nitride/graphene or vanadium pentoxide quantum dots respectively, with extremely concentrated GO dispersions (Hashemi et al., 2020; Kang et al., 2020). Mixing quantum dots of vanadium nitride/ graphene or vanadium pentoxide with highly concentrated graphene oxide dispersions offers the inks excellent shear-thinning and visco-elastic behavior rheological characteristics, making them appropriate for extrusion 3D printing. The irregular supercapacitor has a gravimetric capacitance of 67.1 F g-1, having 65 percent capacitance retention of percent at 6.0 mA cm2 after 8 000 cycles. This irregular supercapacitor can also generate 3.77 mW cm2 of power and 73.9 Wh cm2 of areal energy density. Zhu et al. (2019) published another study focused on the construction of unequal supercapacitors employing mixed inorganic and graphene materials like V2O5, Co3V2O8, and ZnV2O6 to create printable inks. DIW, chemical

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reduction, and freeze-drying were utilized to produce the 3D-printed aerogel electrodes. The conductivity of the graphene ink is increased by adding inorganic compounds such as V2O5, Co3V2O8, and ZnV2O6 (Carmo et al., 2013).

Figure 2.8. (A) Slurry recipe, (B) tape casting, (C) extrusion, and (D) 3D printing are the stages for energy-storage devices from 3D printing using FDM. (Maurel et al., 2020) (E) formulation of materials, (F) generation of printable inks by modifying the rheology, (G) 3D printing, and (H) post-processing are the stages for DIW 3D printing. (EH) (Yang et al., 2019). Source: https://onlinelibrary.wiley.com/doi/abs/10.102/adma.201902725

Figure 2.9. (A) Rate capability of electrodes from 3D printing made up of numerous active materials [106]. (B) Rate capability of electrodes from 3D printing with numerous MnO2 load stackingings. (Zhang et al., 2020). Source: https://www.sciencedirect.com/science/article/pii/S2542435118304586

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2.5.1.2 Modification of components after 3D-Printing The supercapacitor electrodes developed did not show adequate capacitance activity due to the insulating characteristics of the easily accessible PLA/ graphene filament utilised in combination with FDM 3D printing. Gusmao et al. examined the consequence of treatment in solvent on the areal capacitance of the graphene/PLA commercial filament’s as-printed electrodes. A number of polar aprotic and polar protic solvents were utilised to break down the PLA and produce the electrodes from 3D-printing further conductive. When polar aprotic solvents were compared to polar solvents, the results revealed that considerably improved values of areal capacitance are observed by polar aprotic solvents (Carmo et al., 2013). Other groups have improved the characteristics of supercapacitor of the printed electrodes generated from this viable filament using postmodifications such as electrodeposition.. Foo et al. electrodeposited a tinny coating of Au onto an electrode from 3D-printing and used in solid-state supercapacitor devices as the cathode, comparing it to a device without any electrodeposited coating onto the cathode. The enhanced performance of the Au-based supercapacitor was explained by the Au layer enhancing ionic transport and electrical conductivity during operation. Yao and colleagues revealed a new case of employing electrodeposition as a post modification procedure to construct effectual supercapacitors from 3D-printing.The 3D-printed graphene aerogels were employed as supports for the MnO2 electrodeposition to generate electrodes with pseudocapacitive properties in this study, which were made via DIW of a GO ink. The electrodeposition time utilized to make the 3D-printed GO/MnO2 electrodes employ as a big impact on the mass stacking of MnO2, which modifies the areal and volumetric capacitances these electrodes can give. The specific capacitance as a function of MnO2 loading is shown in Figure 2. 9B (Tanwilaisiri et al., 2018). The electrode with the maximum MnO2 stacking had good volumetric and areal capacitances of 115.5 and 11.55 F cm3, respectively, as well as a 73.2 percent rate capability from 0.5 to 10 mA cm2. Moreover, the mass loading of the MnO2 was increased to 182.2 mg cm2 by increasing the thickness of the naked 3Dprinted graphene aerogel electrode from 1 to 4 mm. Because ion diffusion is not limited, increasing the mass loading linearly rises the areal capacitance while maintaining the gravimetric and volumetric capacitances. High areal, gravimetric, and volumetric capacitances can be achieved using graphene aerogels from 3D-printing. This research shows ways in which 3D printing could be used to make high-surface-area supports for the coating of massive amounts of active

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supercapacitor constituents. According to Wang and colleagues, RGO-based 3D-printed scaffolds could be utilzied as a substrate for electrodepositing manganese oxide and nickel oxide to build micropseudocapacitors (Wang et al., 2019). Extrusion-based 3D printing was used to construct interdigitated electrodes using a concentrated graphene oxide ink. The interdigitated electrodes were then ice-covered in liquid nitrogen, freeze-dried for 12 hours, then decreased in Ar/H2 gas flow for 6 hours. A voltage of 1 V was applied for 400 seconds to electrodeposit nickel oxide. The electrodes were then calcined in air for 2 hours at 300°C. Mn oxide was electrodeposited on the RGO substrate by the use of a solution of sodium nitrate and manganese nitrate and a voltage of 1 V for 1000 seconds. The majority of postmodification treatment investigations currently in the literature are conducted FDM and direct ink writing were used to produce supercapacitor-based 3D-printed electronics. SLM and DLP have developed some patterns of post-modification cures on supports from 3D-printing for supercapacitor applications (Azhari et al., 2017). Chang and colleagues used a Porcelite ceramic resin and DLP at 400 nm to 3D print a nonconductive latticestructured electrode support. To make a ceramic lattice substrate, the lattice scaffold was dehydrated and heated at 1500 degree celcius for 4 hours. The ceramic substrate was then roughened by immersing it in an 8 M HNO3 solution for 10 minutes before being washed in water. After that, the support was immersed in a HCl and SnCl2solution for 5 minutes to activate the surface. A solution of silver ammonia was used to submerge the substrate. Lastly, in a solution, electrodeposition was done on the substrate to generate a Cu metal layer. CuSO45H2O, EDTA, HCHO, and NaOH are some of the chemicals used. Finally, cyclic voltammetry was used to electro-oxidize the electrode. The 6 M KOH electrolyte was used to make symmetric supercapacitors, which had 849 F g-1 gravimetric capacitance at 5 mA cm3 and 70.2 percent capacitance retention after five thousand cycles. Because of the electroless copper plating, the produced electrodes had a good conductivity, demonstrating the modest and inexpensive electrodeposition could be advantageous in the field of electrodes for supercapacitors from 3D-printed (Rocha et al., 2017). Zhao et al. utilzied SLM 3D printing to create a titanium-based matrix that was coated in polypyrrole and used as a supercapacitor electrode. Using a Ti6AI4V metal powder, SLM was first utilised to create titanium interdigitated electrodes. After that, the electrodes were electropolymerized at 0.75 V for 40 minutes in 0.1 M sodium p-toluene sulfonate and an aqueous

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solution of 0.1 M pyrrole to coat the titanium structures with polypyrrole coating. After that, the electrodes were evaluated as supercapacitors in an PVA/H3PO4 electrolyte. At 5 mV s1, the electrode brought a volumetric capacitance of 10.1 F cm3. It produced 213.5 Wh m3 of energy and 15.0 kW m3 of power. After 1000 cycles, the capacitance retention was 78 percent. This research also revealed that the actual device’s footprint may be reduced, allowing 3D-printing techniques like SLM to be employed for tiny power sources (Yu et al., 2019).

Figure 2.10. Battery constituents 3D-printed in many forms: Ink Writing 3Dprinted (A) a current collector, (B) an anode, (C) a cathode, and (D) finished device, as well as (E) the electrochemical response. [123] (AE) (AE) (AE) (AE) (AE) 3D-printed fibre cathode and anode (F), installation on a cell with fibre shape (G), and electrochemical performance (H). (FH) (FH) (FH) (FH) (FH) (FH (I) A comparison of the rate capabilities of three different types of 3Dprinted batteries. (Liu et al., 2018). FDM 3D-printed components for a (K) coin cell (J). (L) The electrochemical efficiency of the FDM battery.

3D-printing skill provides a fantastic opening to construct battery constituents, in not-too-distant future, it can enable for the uninterrupted production of fully 3D-printed batteries. calendaring, electrolyte infilling, Drying, heatsealing, and clamping are just a few of the standard battery production steps that will be abolished. There have already been numerous advancements in 3D printers that can print multiple inks or fibers one after the other (Chang et al., 2019).

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Figure 2.11. 3-D printed electrodes of lithium-ion battery with a lattice offers passages for lithium to travel into the electrode efficiently. Source: https://www.asme.org/topics-resources/content/3dprint-lithiumionbattery-could-power-electric

However, due to the difficulties of 3D printing electrochemically active and structurally stable things at the same time, the creation of filaments and inks for printing in 3D rests a task. In order to print high-quality structures which are burdened with active elements electrochemically, the mix of the filaments and inks must be adjusted. Batteries have an iondiffusion control device, which means that the capability of ions to infuse to the surface of the electrode limits their electrochemical performance. Because it enables for the inclusion of texture to printed things, 3D printing skill can play a major role in assisting kinetics. Hierarchical pores can be designed into electrodes 3D printing, increasing the surface area of the interphase where electrodes and electrolyte interact and thus enhancing active material use and rate performance (Shen et al., 2018). To put it another way, 3D printing has the potential to improve present battery technology just by utilising this new manufacturing method. There have been a few researches on battery components and batteries from 3D printing so far. Though, because this is a relatively new sector, more study and advance is required before it can be used in industrial battery manufacturing. In this part, we’ll look at the several types of active materials which are being utilised to demonstrate the

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idea of 3D-printed batteries, as well as the results. Grouping of the materials will take place by the sort of battery knowledge in which these are being used, with a concentration on Liion batteries but also LiO2, LiS, and Na-ion batteries discussed concisely. The goal is to increase consciousness of the wider difficulties that 3D-printed active materials are being used to address (Zhao et al., 2020).

Figure 2.12. Schematic of the process to 3D-print solid electrolyte structures. Source: https://www.semanticscholar.org/paper/3D-Printing-Electrolytes-forSolid-State-Batteries.-McOwen-Xu/ec969570480b5b676466a476df397b06e65a07c2/figure/0

By developing concentrated inks of Li4Ti5O12 (LTO) and LiFePO4 (LFP), which act as the anode and cathode materials, inkjet printing was used to create electrodes for Li-ion batteries. The technique for fabricating these batteries via direct ink writing is shown in Figure 2. 10AD. Ethylene glycol, glycerol, deionized water, and cellulose-based viscosifiers were utilized in the first inks, coupled with active ingredients. To eliminate the organic additives and sinter the nanoparticles of the active materials, the electrodes from 3D-printing were calcinated at 600 °C in an environment of inert gas. The specific capacities of these 3D-printed electrodes were 160 and 131 mAh g1, respectively, for LTO and LFP, which are anode and cathode materials. It had a 1.5 mAg cm2 areal capacity when built in an interdigitated battery, as represented in Figure 2. 10E. Another research for Li-ion batteries into 3D-printed inks made of LTO and LFP has been conducted by using GO in the electrode recipie. The addition of GO

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increases the rheological behaviour of the inks, which makes them easier to print. The amount of GO in the aqueous dispersion has a big impact. The dispersals of GO have a liquid-like behaviour when the concentration is low, that is not acceptable for printing in 3D; yet, as the concentration is increased, the dispersals of GO have a gel-like behaviour, that is good for printing in 3D (Shen et al., 2018; Zhao et al., 2020). GO has the ability to increase shear-thinning and viscosity behaviour while also improving electrochemical efficiency. GO bring into line under the shear stress created by the nozzle of 3D-printing, resulting in improved electrical conductivity for the electrodes. It also serves as a useful matrix for 3D-printed battery inks. Printable cathode and anode battery inks are made by mixing LTO and LFP into extremely concentrated GO solutions. Furthermore, the graphene oxide flakes growth of the surface area of the electrodes, allowing LFP and LTO to be accommodated. Freeze-drying and a heat treatment at 600 °C can be applied after the 3D printing process. The first aids in the removal of the solvent from the printed structures, while the second reduces graphene oxide. The specific capacity values of the 3D-printed RGO/LFP and RGO/ LTO are 164 and 185 mAh g1, respectively. The electrochemical cell offers 100 mAh g-1 when fully built. Key benefit of 3D printing is its abilility to enable for the creation of electrodes in a variety of forms. As demonstrated in Figure 2F and G, LTO and LFP-centered electrode materials can also be 3D-printed as fibres. LFP or LTO, carbon nanotubes, and PVDF were used to create the inks. LFP wire electrode had a 165 mAh g1 specific capacity, while an LTO wire electrode had an 189 mAh g-1 specific capacity. Both fibre electrodes were assembled into a cell with a specific capacity of 110 mAh g-1 by the use of PVDF-co-HFP gel saturated with LiPF6 DEC as gel electrolyte, as displayed in Figure 2. 10H, having the benefit of decent elasticity and a possible use for handy electronics (Chang et al., 2019). Liu and colleagues compared the manufacturing of LFP electrodes for Li-ion batteries by the use of low temperature 3D printing, DIW, and traditional roller covering. Different ink characteristics are required for each of these electrode manufacturing techniques. The structure, gemoetry, and porosity structure of the produced electrodes are all influenced by the solid concentration of the inks. LFP, carboxymethyl cellulose and Super P were mixed in 1,4-dioxane and water to make slurries. The 3D-printing mechanism at low-temperature included a apparatus with a low-temperature compartment that allowed the ink to be frozen at 30 degrees Celsius as it was created. The freeze-driying of electrodes was dine at 60 degrees Celsius. As the line breadth of electrodes manufactured by DI writing inclines to grow

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in association to that of 3D printing electrodes at low-temperature, by the use of 3D printing electrodes at low-temperature aids to retain the structure and shape of the product more accurately (Rymansaib et al., 2016). The printing procedure as well as the solid composition of the slurry might affect the electrode thickness. Thick electrodes are produced using 3D printing electrodes at low-temperature. To allow for optimal stable structural and printability, the solid content of the inks must be adjusted. The printing precision improves as the solid component of the slurries increases. Because of the the enormous amounts of solvent existing in the slurry when inks with less solid content are utilised, significant flaws can form, causing electrodes with higher porosity. But, if the inks have an excessive amount of solid content, cracks can form on the electrodes following the freeze drying process due to the electrodes’ higher thickness. The conductive network is hampered when the electrodes have an too much amount of big pores and cracks, resulting in low specific capacity and poor electrical conductivity. Additionally, if the porosity falls to too less amount, the ionic conductivity decreases as well, resulting in decreased capacity values. As a result, inks with low solid concentration are constrained by their electrical conductivity, whereas high solid content inks are constrained by their ionic conductivity (Areir et al., 2017). Medium solid concentration in inks, on the other hand, were tuned for enhanced electrode integrity. The electrochemical performance of several Li-ion battery manufacturing processes is compared in Figure 2. 10I. The electrodes made with electrodes from 3D printing electrodes at low-temperature had the maximum capacity, delivering 163 mAh g. Inkjet printing is being utilised to devise 3D printing electrodes from other forms of inorganic resources utilized as cathode in Li-ion batteries, including LiMn1xFexPO4. 129 The polarisation electrodes with thick block-shape is often substantially greater than of tiny electrodes. Though, because of the line in which they are printed, the electrodes created by 3D printing contain extra space than those made by the traditional blade-casting approach. As a result, the electrolyte’s diffusion path has been enhanced, allowing it to perform at a high rate capability. The specific capacity of such electrodes from 3D printing is enhanced to 161 mAh g-1 (Areir et al., 2017). Li-ion batteries could be totally manufactured using sequential printing of the battery constituents and stereolithography and such as the electrodes, separator, casing, and electrolyte, in addition to inkjet printing. The active ingredients Ketjenblack, LiTFSI in propylene carbonate, and polymer were used to make the inks for the LFP and LTO electrodes (vinilpyrrolidone).

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As a result, the as-printed design can be treated uby the use of UV to create batteries with a capacity of 4.45 mAh cm2. Aerosol Jet 3D printing can also be used to make Ag electrodes for Liion batteries. The ability of Ag to produce AgLi alloys have been exploited to show the advantages of producing a hierarchical permeable microlattice. Because of the increased electrolyte ions movement, the formation of cavities in the electrodes via 3D printing increases the electrochemical efficiency of Li-ion batteries. By allowing the electrode to deform, it condenses ion diffusion routes, expands the space between the phases, and decreases intercalation-prompted stress. In comparison to a block electrode, the active material usage is improved overall, resulting in a specific capacity rate of 210 mAh g-1 (Maurel et al., 2018) Further 3D-printing processes, including FDM, are also being used to make Li-ion batteries with LTO and LMO as anode and cathode ingredients, as presented in Figure 2. Though, filaments for this type of printing technology are mostly designed of polymers with poor ionic and electrical conductivities, such as PLA. To enable the production of electrochemical devices, specialised filament advancements are required (Maurel et al., 2018). Electrical conductivity needs to be enhanced in the electrode filaments, consequently additives with conductive properties like, Super P, multiwalled nanotubes, or graphene can be combined with PLA liquefied in dichloromethane. The printability and conductivity of the resultant filaments is affected by the size of the combinations produced within the PLA matrix. To make cathode and anode filaments, LMO and LTO can be inserted to the PLA and additive with conductive properties solutions, respectively. PLA can be filled with a mixture of LiClO4, ethyl methyl carbonate, LiTFMS, LiPF6, or propylene carbonate to improve the electrolyte filaments (Skylar et al., 2019). The best electrolyte filament was LiClO4 because it had strong ionic conductivity and could be printed in ambient settings without degrading. With a capacity of 9.74 mAh cm3, LMO/PLA/MWNT gives the maximum capacity for the cathode, and LTO/PLA/graphene provides the best capacity for the anode with a capacity of 9.48 mAh cm3. The electrochemical reaction of the entire cell, that had a capacity of 22.96 mAh cm3, is shown in Figure 2. 10L. Anodes for Li-ion batteries were also created using graphene nanoplatelets and PLA filaments. The graphene nanoplatelet composition was tweaked to achieve a good balance of conductivity and printability. This process produced 3D-printed electrodes with low specific

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capacities. However, a chemical treatment that improves porosity can be used to improve performance during postmanufacturing. The filaments lack percolation and have a high resistance where a modest proportion of nanoplatelets of graphene is incorporated to them. As a result, to boost electrochemical activity and conductivity, the proportion of nanoplatelets of graphene should be enhanced to 15–20%. It did, however, contain a low capacity of 20 mAh g-1. The capacity of the electrodes from 3D-printing could be raised to 500 mAh g-1 by postprinting treatment of soaking them in 1 M NaOH (Fu et al., 2016).

Figure 2.13. Different 3D printed forms of batteries (a) Construction strategies, (b) electrode architecture, (c) battery conewfiguration. Source: https://www.sciencedirect.com/science/article/abs/pii/ S2542435120305183

Anodes in Li-ion batteries are optimised utilizing graphite and PLA filaments. The addition of plasticizers improves the electrochemical performance, whereas increasing the loading of active material improves the efficiency of electrochemical. To be utilised as 3Dprinting filaments, materials with a less quantity of plasticizers are excessively brittle, and ones with a high number of plasticizers are excessively soft. The graphite grains separate effortlessly from the matrix of the polymer, indicating

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that the components have a weak connection (Sajadi et al., 2021). The incorporation of conductive substances makes the electronic conductivity better of composite layers, but due to the segregation of the additives inside the matrix of the polymer, it cannot add to a improved flexible capacity loss. The capacity of these 3D-printed anodes is 200 mAh g-1. Various other batteries, such as LiO2, LiS, and Na-ion batteries, have been proved to be produced using 3D printing. A 3D-printable aqueous ink on the basis of holey graphene oxide which is binder and additive-free and has been proposed for the fabrication of cathodes for LiO2 batteries. The holey graphene oxide’s hydrophilicity enables for constant, extremely concentrated dispersals in water. The water was removed from the 3D-printed electrodes by freezing them and then thermally reducing them at 1000 degrees Celsius. Such electrodes have a capacity of 3879 mAh g-1 when used as cathodes for LiO2 batteries. Vacuumfiltrated sheets made of the same decreased holey graphene material were also constructed for comparison, providing just 92 mAh g1. The use of 3D printing trailed by a freeze-drying technique can surely deliver a beneficial design for increased LiO2 electrode efficiency, benefitting cyclability and capacity retention (Gao et al., 2019). The precursor used to make graphene had a distinct nanoporosity and, as a result, a varied electrochemical efficiency. Electrodes from 3D-printing made of RGO from natural graphite have a capacity of 600 mAh g-1, whereas those made of RGO from Vor-X graphene have a capacity of 2 471 mAh g−1 (Down et al., 2019).

Figure 2.14. Imminent suggestion in the area of electrochemical energy storage and conversion and 3D printing. Source: https://pubmed.ncbi.nlm.nih.gov/32049499/

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54. Hughes, R. A., Menumerov, E., & Neretina, S. (2017). When lithography meets self-assembly: a review of recent advances in the directed assembly of complex metal nanostructures on planar and textured surfaces. Nanotechnology, 28(28), 282002. 55. Jiang, Q., Kurra, N., Alhabeb, M., Gogotsi, Y., & Alshareef, H. N. (2018). All pseudocapacitive MXene‐RuO2 asymmetric supercapacitors. Advanced Energy Materials, 8(13), 1703043. 56. Jiang, Y., Xu, Z., Huang, T., Liu, Y., Guo, F., Xi, J., ... & Gao, C. (2018). Direct 3D printing of ultralight graphene oxide aerogel microlattices. Advanced Functional Materials, 28(16), 1707024. 57. Jun, J., Kim, H., Choi, H. J., Lee, T. W., Ju, S., Baik, J. M., & Lee, H. (2019). A large-area fabrication of moth-eye patterned Au/TiO2 gap-plasmon structure and its application to plasmonic solar water splitting. Solar Energy Materials and Solar Cells, 201, 110033. 58. Kang, Z., Alia, S. M., Young, J. L., & Bender, G. (2020). Effects of various parameters of different porous transport layers in proton exchange membrane water electrolysis. Electrochimica Acta, 354, 136641. 59. Kim, J., Kim, J. H., & Ariga, K. (2017). Redox-active polymers for energy storage nanoarchitectonics. Joule, 1(4), 739-768. 60. Kim, M. J., Cruz, M. A., Ye, S., Gray, A. L., Smith, G. L., Lazarus, N., ... & Wiley, B. J. (2019). One-step electrodeposition of copper on conductive 3D printed objects. Additive Manufacturing, 27, 318-326. 61. King, L. A., Hubert, M. A., Capuano, C., Manco, J., Danilovic, N., Valle, E., ... & Jaramillo, T. F. (2019). A non-precious metal hydrogen catalyst in a commercial polymer electrolyte membrane electrolyser. Nature nanotechnology, 14(11), 1071-1074. 62. Kumar, S. S., & Himabindu, V. (2019). Hydrogen production by PEM water electrolysis–A review. Materials Science for Energy Technologies, 2(3), 442-454. 63. Lacey, S. D., Kirsch, D. J., Li, Y., Morgenstern, J. T., Zarket, B. C., Yao, Y., ... & Hu, L. (2018). Extrusion‐based 3D printing of hierarchically porous advanced battery electrodes. Advanced Materials, 30(12), 1705651. 64. Le Fevre, L. W., Fields, R., Redondo, E., Todd, R., Forsyth, A. J., & Dryfe, R. A. (2019). Cell optimisation of supercapacitors using a

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75. Mayorga-Martinez, C. C., Sofer, Z., Sedmidubský, D., Luxa, J., Kherzi, B., & Pumera, M. (2018). Metallic impurities in black phosphorus nanoflakes prepared by different synthetic routes. Nanoscale, 10(3), 1540-1546. 76. Mebed, A. M., Abd-Elnaiem, A. M., El-Said, W. A., & Asafa, T. B. (2019). Review on the Formation of Anodic Metal Oxides and their Sensing Applications. Current Nanoscience, 15(1), 6-26. 77. Ngo, T. D., Kashani, A., Imbalzano, G., Nguyen, K. T., & Hui, D. (2018). Additive manufacturing (3D printing): A review of materials, methods, applications and challenges. Composites Part B: Engineering, 143, 172-196. 78. Novotný, F., Urbanová, V., Plutnar, J., & Pumera, M. (2019). Preserving fine structure details and dramatically enhancing electron transfer rates in graphene 3D-printed electrodes via thermal annealing: toward nitroaromatic explosives sensing. ACS applied materials & interfaces, 11(38), 35371-35375. 79. O’Neil, G. D., Ahmed, S., Halloran, K., Janusz, J. N., Rodríguez, A., & Rodríguez, I. M. T. (2019). Single-step fabrication of electrochemical flow cells utilizing multi-material 3D printing. Electrochemistry Communications, 99, 56-60. 80. Palenzuela, C. L. M., & Pumera, M. (2018). (Bio) Analytical chemistry enabled by 3D printing: Sensors and biosensors. TrAC Trends in Analytical Chemistry, 103, 110-118. 81. Pang, J., Mendes, R. G., Bachmatiuk, A., Zhao, L., Ta, H. Q., Gemming, T., ... & Rummeli, M. H. (2019). Applications of 2D MXenes in energy conversion and storage systems. Chemical Society Reviews, 48(1), 72133. 82. Parra-Cabrera, C., Achille, C., Kuhn, S., & Ameloot, R. (2018). 3D printing in chemical engineering and catalytic technology: structured catalysts, mixers and reactors. Chemical Society Reviews, 47(1), 209230. 83. Pascuzzi, M. E. C., Goryachev, A., Hofmann, J. P., & Hensen, E. J. (2020). Mn promotion of rutile TiO2-RuO2 anodes for water oxidation in acidic media. Applied Catalysis B: Environmental, 261, 118225. 84. Pomerantseva, E., Bonaccorso, F., Feng, X., Cui, Y., & Gogotsi, Y. (2019). Energy storage: The future enabled by nanomaterials. Science, 366(6468).

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85. Redondo, E., Ségalini, J., Carretero-González, J., Goikolea, E., & Mysyk, R. (2019). Relation between texture and high-rate capacitance of oppositely charged microporous carbons from biomass waste in acetonitrile-based supercapacitors. Electrochimica Acta, 293, 496-503. 86. Reyes, C., Somogyi, R., Niu, S., Cruz, M. A., Yang, F., Catenacci, M. J., ... & Wiley, B. J. (2018). Three-dimensional printing of a complete lithium ion battery with fused filament fabrication. ACS Applied Energy Materials, 1(10), 5268-5279. 87. Rocha, V. G., Garcia-Tunon, E., Botas, C., Markoulidis, F., Feilden, E., D’Elia, E., ... & Saiz, E. (2017). Multimaterial 3D printing of graphene-based electrodes for electrochemical energy storage using thermoresponsive inks. ACS applied materials & interfaces, 9(42), 37136-37145. 88. Rodriguez, E. J., Marcos, B., & Huneault, M. A. (2016). Hydrolysis of polylactide in aqueous media. Journal of Applied Polymer Science, 133(44). 89. Roger, I., Shipman, M. A., & Symes, M. D. (2017). Earth-abundant catalysts for electrochemical and photoelectrochemical water splitting. Nature Reviews Chemistry, 1(1), 1-13. 90. Roy, N., Suzuki, N., Terashima, C., & Fujishima, A. (2019). Recent improvements in the production of solar fuels: from CO2 reduction to water splitting and artificial photosynthesis. Bulletin of the Chemical Society of Japan, 92(1), 178-192. 91. Rymansaib, Z., Iravani, P., Emslie, E., Medvidović‐Kosanović, M., Sak‐Bosnar, M., Verdejo, R., & Marken, F. (2016). All‐Polystyrene 3D‐ Printed Electrochemical Device with Embedded Carbon Nanofiber‐ Graphite‐Polystyrene Composite Conductor. Electroanalysis, 28(7), 1517-1523. 92. Sajadi, S. M., Enayat, S., Vásárhelyi, L., Alabastri, A., Lou, M., Sassi, L. M., ... & Ajayan, P. M. (2021). Three-dimensional printing of complex graphite structures. Carbon, 181, 260-269. 93. Saleh, M. S., Li, J., Park, J., & Panat, R. (2018). 3D printed hierarchically-porous microlattice electrode materials for exceptionally high specific capacity and areal capacity lithium ion batteries. Additive Manufacturing, 23, 70-78. 94. Shafiee, S., & Topal, E. (2009). When will fossil fuel reserves be diminished?. Energy policy, 37(1), 181-189.

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GAS-PHASE 3D PRINTING OF FUNCTIONAL MATERIALS

CONTENTS

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3.1 Introduction ....................................................................................... 76 3.2 Background and History ................................................................... 78 3.3 Deposition Manifold Head ............................................................... 80 3.4 Sald Aided Digital Fabrication’s Features ............................................ 86 3.5 Future Possibilities and Summary ...................................................... 88 References ............................................................................................... 89

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3.1 INTRODUCTION A developing fabrication technique that permits the formation of freeform parts without the requirement of casting or machining is 3D printing (also known as additive manufacturing (Guo and Leu, 2013; Vallat et al., 2017). In beginning it established for the purpose of prototyping, 3D printing is a layer-by-layer production method in which computeraided design (CAD) is used to produce a structure. In past few year, this method is developing more quickly, and is already used by many companies and institutions such as Airbus ,NASA or Boeing, the last one having gained the Federal Aviation Administration (FAA) certification for the first metallic components’ 3D printed (Joshi and Sheikh, 2015). As it was established in 1984, now the print of metallic components at the industrial and laboratory level from the initial polymeric material at customer level become feasible. Glass, ceramics, and even Teflon are the latest typical materials that come in this list (Eckel et al., 2016). During several years, numerous 3D printing methods have been established that are certainly linked with the material nature being printed. So for the design of customer-based complex parts made from several unlike materials, from chemically resistant polymers to metals, 3D printing is a magician box contributing in approximately limitless options. Also, for the degradation of modern functional materials, such as porous silica or quartz, hybrid materials, hydrogels, sugar scaffolds, or biomaterials, 3D printing has been used related to others techniques (Kim et al., 2017; Yan et al., 2021). In this work, to show a modern method for functional materials’ printing, we integrate the capability of 3D printing with the exclusive resources of SALD. Specifically, for our outdoor SALD system ,we exploit 3D printing to make customer-based monolithic adjacent heads. At the hour of need, the attained heads are manufactured. They are easier and of low cost to tune than standard heads manufactured by traditional methods. To manufacture plastic heads with different sizes and shapes, we used a cheaper tabletop 3D printer. For instance, 3D printing permits the combination of the full gas distribution system inside the head body,making the assembly of the head simple. As they can be simply manufactured if damaged and blocked at the time of degradation, so they can be assumed as disposable parts because they are less expansive. Heads may also be printed in different materials or metal at the time of need. We can simply modify different sizes of substrate and with no need of preceding patterning or masking steps, execute patterns and ASD on a surface and all this is presented by simple alterations of the head designs. At the end, gas-phase chemical manufacturing and freeform motives

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of functional materials can be understood by joining a 3D printed reduced SALD head with a table of XYZ. Great applicability is offered by this type of easy open-air method for 3D printing and the patterning of functional materials with nanometer resolution in the Z axis and great conformality, for many operations (Li et al., 2020). Spatial atomic layer deposition (SALD) is a new method 100 times quicker ,even at pressure of atmosphere, than traditional atomic layer deposition (ALD). Recent works utilized these resourses concentrating on greater-rate, big area of storage for scaling-up into mass creation. Contrarywise, this chapter presents that SALD certainly shows a perfect stage for area-selective removal of functional materials by proper design and reduction of close-proximity heads of SALD. Specifically, the low-priced customer-based close-proximity heads, which can be simply altered and designed to gain different free-form patterns and deposition areas, and even multimaterial complex structures are manufactured by the function given by 3D printing . At the end, functional materials’ 3D printing can be executed with nanometric resolution in Z by designing a reduced head with round concentric gas channels. This establishes a new gas-phase method of 3D printing. Continuous and conformal thin films of functional materials may be printed with high deposition rate and at low temperatures in outdoors, as the procedure is depend on ALD reactions. A new multipurpose method of printing devices and functional materials with topological and spatial control is presented by this new method, therefore overall expanding the ability of ALD and SALD ,and in the areaselective deposition’ field of functional materials, a new path is opened (Bandyopadhyay et al., 2015). Moreover patterning and lithography are frequently executed in cleanrooms, therefore increase the cost of the end products. In this situation, to take the resolution of inkjet printing to the micrometer level, there has been considerable development (An et al., 2015). And other new bottom side-up techniques are being established, for instance, depend on interfacial convective and microfluidics assemblage (Li et al., 2021). In the past few years ,in the atomic layer deposition (ALD) field, one new method known as area-selective deposition (ASD) has been establised In ALD, surfacelimited, selfterminating reactions, solid-gas occur (Leskelä and Ritala, 2003). This leads to very continuous and compacted thin films with an exceptional conformality and thickness control of sub-nanometer, main resources for surfaces of different functional gadgets and materials and interfaces of engineering. Various approaches can be applied to control the responsiveness of ALD precursors for different surfaces to produce

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selectivity are specified by ALD’ surface-limited nature and leads to ASD (Wen et al., 2016; Guan et al., 2017).

3.2 BACKGROUND AND HISTORY For several technologies and applications, the main role is the opportunity to pattern functional materials in an easy and inexpensive way (Barth et al., 2010; Yang et al., 2015). At large scale, there is the opportunity of of functional materials’ direct printing with different methods, inkjet printing is one of the most famous technique. Standard methods depend on lithography are efficient and mature while regarding the micro and nano level, they include many steps the production and design of masks, and high-priced apparatus (Chung et al., 2019). These include the usage of self-assembled monolayers to hindren the growth in specific components of the surface or the usage of a substrate with dissimilar materials (growth hindration or postponement occuring in one of them) as previously studied by Mackus et al. (2018) Whereas these methods are very attractive and have verified to be effective, but there is requirement to have a surface with dissimilar materials, and in maximum cases a prepatterning step is essential. Similarly, transitional etching steps are required for few of the ASD methods (Vallat et al., 2017). Lastly, the usage of costly vacuum apparatus and the integral low storage rate of ALD are the drawbacks of these methods .

Figure 3.1. a) Closeness spatial atomic layer deposition (SALD) system (b) In a normal close-proximity SALD head, the 3D arrangement of the different parts

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(c) On substrate top, Close view of the deposition head bottom (d) Image of a traditional head fixed in our SALD system, presenting pipes and connections’ complex set. Source:

Note: a) SALD system depend on a gas manifold injector employed in the open air (no storage chamber used). An inert gas (Ar or N2) is bubbled throught the precusors which is deposited in bubbler to carry out the instable molecules. b) The different flows carrying the precursors and inert gas stored in separated channels are carried out by different flows.Through the corresponding channels, the different flows are needed to be distributed by numerous connections and parts. c) Precursors are inoculated through their corresponding channels and after that exhausted through next exhaust channels, so typical atomic layer deposition (ALD) cycles are reproduced by being exposed to moving substrate. The arrangement presented the deposition of ZnO from water and diethyl zinc (DEZ). d) Image of a conventional in our SALD system, the picture of installed traditional head, presenting the complex set of connections and pipes Spatial ALD (SALD) has developed itself as cheaper alternative and great-throughput to traditional ALD, in past few years. SALD is depend on precursors’ spatial separation, opposite to sequential (temporal) separation in ALD (Poodt et al., 2012; Nguyen et al., 2017). So, precursors are unceasingly inoculated in different locations, which are spatially detached by an inert gas area. The typical ALD cycle is repeated, as model is exposed to different areas . Because, SALD can be two times quicker than ALD as no elimination steps are needed (Muñoz et al., 2016).. Moreover at the pressure of atmosphere (AP-SALD), SALD can performed, leading to more suitable for scalingup than vacuum-based ALD. But different conformality, control of thickness to the sub-nanometer scale of ALD and the low temperature processing are sustained in SALD as SALD is depend on the self-terminating chemistry than ALD and similar surface-limited. Because of the powerful application to photovoltaics, the value of thin films put on by SALD has been presented (Muñoz et al., 2017). Though AP-SALD can be applied in various different ways the primarily established method of the close-proximity proposed by Levi et al. is worth interesting (Figure 3. 1a). It depends on a multifold injection head

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(Figure 3. 1b) in which on a moving substrate, the inert gas and different precursors are spread along corresponding slits. By inserting the surface of the substrate and the substrate sufficiently close (normally in the series of hundreds micrometers), only on the substrate particularly of ALD ,the gas−solid reactions can occur and there is prevention of cross-talk between precursor (Figure 3. 1c). Opposite to other SALD methods, the process occur in open air and there is no use of reaction chamber , so efficiently similar to a functional materials printer (Levy et al., 2008).

3.3 DEPOSITION MANIFOLD HEAD The deposition multifold head is the main part of such SALD systems, and therefore size of the sample can easily adopt this principle in order to scale down (for patterning or ASD) or up (for huge-area deposition) the process. The deposition head has been conventionally manufacture in metal by many different methods. In the unique patent by Levy et al. (2008) inside the head gas distribution was carried out over channels that were gained by putting a sequence of plates together with engraved grooves or cut channels. Whenever a channel gets choked by the undissolved materials if the polishing, reassembly and disassembly of head is required then this head is not ideal. Lately, by traditional machining methods, easy heads have been manufactured , for instance, to obtain the channels of the gas distribution, water jet cutting with welding of different pieces (Figure 3. 1b) (Muñoz et al., 2017). But, in both cases the processes for manufacturing the heads are complex and costly and and/or time taking. Moreover, the use of conventional limits the complexity and flexibility of the head design is limited by the usage of traditional fabrication methods. Lastly, many pipes and connections are vital for different flows distribution, increasing the probability of contamination and leakage(Figure 3. 1d). SALD system is providing in Movie S1, Supporting Information, in which deposition executed.

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Figure 3.2. (a) For the different types of gases, 3D arrangement of the internal distribution channels:green shows metallic precursor, blacks represents exhaust in black ,red shows co-reactant,and blue shows inert gas. (b) Clear resin prints head. Distribution channels can be noticed. (c) With fittings, printed head which is ready to plug and show in the system of spatial atomic layer deposition (SALD). (d) Bottommost view ,with dissimilar outlet designs, of two different heads. e) Heads’ in-situ printing from Formlabs in a Form 2 in clear resin(f) The head design similar to 3D printed in metal.

Note: Design with respect to the head showed in (a) is on left. Design with wider exhaust channels and just one metal precursor outlet and and parting between different outlets is on right. By using 3D CAD methods, the design of customized heads is carried out and it is shown in Figure 3.2. Through computational fluid dynamics (CFD) simulations, the optimization of dimensions and shape of different channels could be performed . For the different gas ,the 3D structure of the inner distribution channel like inert gas for a monolithic and reactive precursors, customize head design is shown in Figure3.2 .The heads 3D print permits the usage of such curved, bell-like shaped patterns that are more designated than the rectangular ones used in our traditional head to get a homogeneous flow leaving the head (Munoz et al., 2014). How the circulation of the three main flows, i.e., inert gas metallic precursor, and co-reactant (an oxidizer or water to deposite oxides), are simply circulated inside the head with different channels is also presented by the scheme. Figure 3. 2b presents a head whn get printed in the Formlabs clear resin, integrating the distribution channels presented in design in Figure 3. 2a.

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(The with the shapes, different internal channels are visible). Countrary to complex head presented in Figure 3. 1, 3D printing therefore permits the manufacturing of monolithic heads where the of the channels shape can be simply altered (though printing in Movie S2, Supporting Information, a head is presented) and in which the application of the gas distribution is carried out. Figure 3. 2c represents the printed head which added some fitting so by just joining the exhaust line and three flow lines, it readily used by SALD system. (In Movie S3 (Supporting Information) A movie can find where to execute a deposition, the install printed head in the SALD system is used). As presented, the usage of customized design channel arrangements and shapes is allowed by 3D printing .To select the gasses from specific exhaust channels (as head case presented in Figure 3. 1a−c, ), or to alter the quantity of metallic outlets in head , so it is very simple to alter and improve them, or for instance for improving the process or in situ classification (Huerta et al., 2020). Certainly, considering the close-proximity SALD nature, the control of efficient separation of precursors on substrate top to confirm a proper ALD reaction is very important (Masse et al., 2019).This is generally measured by regulating different flows and by regulating the gap between the substrate and the head. With the availability of low-cost 3D printed heads, another parameter that can be easily modified and tuned which directly affects the exposure time of precursors to the substrate surface is for instance the gap between the different outlets (i.e., the head design). The lowest part of two different head designs are shown by Figure3.2d. From Figure 3. 2a the outlets in the design are presented to the left. To the right, the outlets with respect to the design in which, the exhausts (gray) are broader and the gap between the different outlets is larger and only one precursor channel (green) has been involved. This is suitable because the cross-talk of precursor is prevented more efficiently by bigger gap, and therefore there is less importance of the value of opening and the head is properly arrange parallel with substrate, easing the process of the system and enhancing reproducibility. However, if both the righr and left designs are improved, then because of the variation in quantity of channels of precursor the heads’left part is two times faster in growth rate related to right part . When get printed in clear resin, where the internal conducts are visible, this variant of head is showed by the picture in Figure3.2e. So for prototyping and optimization, plastic heads are very suitable, and as a low cost, even non reusable, varient to tradition heads (Bandyopadhyay et al., 2015). Nevertheless, the use of There could be a problem on the usage of plastic heads for depositions when chemical

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unsuitability may present with the precursors or at high temperatures (>200 °C). In this case, with the advance technologies of different 3D printing, heads with intricate internal patterns like the ones presented here can also be printed harder and thermally more stable materials, namely, ceramics or metals. With the same design shown in Figure 3. 2e (a deposition is shown by movie, executed with the metallic head is presented in Movie S4, Supporting Information), 3D printed metallic head is showed by Figure3.2. The flexibility of this simple method is extended by printing heads with intricate patterns in different materials. Figure 3. 3 presents other cases of the options presented by applying the 3D printing of SALD heads. Figure 3. 3a presents two varieties of the head shown in Figure 3. 2e having variety of lengths of outlet, therefore producing a smaller area of deposition. No doubt, when using the standard, non-easily modifiable head, the deposition region always remains same, irrespect the sample size to be coated. This has two major disadvantages. On one side, when depositing on prototype smaller than deposition head, a huge amount of precursor waste. Contrary to this ,by consecutive coating the different parts of the substrate for prototypes bigger than the head, it is almost impossible to get a unifoem continuous layer (Huerta et al., 2020). So, the adjustment of outlet size with the coated prototype is very stimulating. By using the head with standard outlet length of (5 cm) and 2.5 cm , Cu2O thin films deposited is shown in Figure3.3a. In both cases, ahomogeneous film can be attained by proper channels design inside the head and the modification of the deposition parameters. The first case existing in this work of simple direct ASD is shown by the smaller film, without the etching steps or prepatterning needs.

3.3.1 Gap Between Head and Substrate To confirm effective precursor separation and therefore reaction of ALD mode, it is important to regulate the gap between substrate and head. But the deposition regime between ALD and CVD (where above the substrate, precursors react in the gas phase) needs to be tuned to mechanically regulate the gap (Masse et al., 2019). Since there is greater rate of deposition, when dealing with featureless, flat substrates ,deposition in spatial CVD (SCVD) mode could be suitable (Hoye et al., 2013). Moreover, when nanostructures coats, SCVD has presented to be conformal. Lastly, the usage of precursors that would not respond in the ALD mode is allowed by SCVD mode (i.e., selective reaction shows with the substrate). Moreover, we have presented in the past that when doing a static deposition then do a selective deposition

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of lines, SCVD mode can be used (i.e., meanwhile if the deposition is static, precursors can just meet in specific areas under the head with a static substrate) (Masse et al., 2019). By joining this static deposition mode with greater flexibility in manufacturing the injection head according to 3D printing, SCVD heads can be simply manufactured to deposit freeform patterns. The head with round outlets in the place of straight outlets usually used in SALD, showed in Figure3.3b. Round patterns can be printed straightly, by doing static deposition in CVD mode with this kind of head. The flows used and time of deposition can control the thickness of the films, producing different colors.

3.3.2 Multi-Materials’ Concurrent Deposition The simultaneous placing of various constituents in several sites is a likelihood presented by additive manufacturing SALD deposition heads. An example of this is of various constituents being concurrently patterned (once the procedure is improved, the head has been modeled and printed, this could pave the way for immediate placement of gadgets comprising of several layers without the need for any patterning stages). In the deposition space, a digital head intersects only in the middle area and has been made to displace 2 diverse substances. The 2 diverse precursors are supplied by 2 autonomous precursors outlets made of metal which are then incorporated by the head. Sideways to the outlets, these precursors can be found at the head’s very opposite’s edges and are shorter than others (exhaust, oxidizer, and inert gas). A small opening of inert gas is at the end of the outlet. A lot more networks would be implied and it will be quite difficult or maybe impossible to create such a head with orthodox machinery. In a single block, a head like this could be created through digital fabrication. As illustrated in Figure3. 3c, a ZnO/Cu2O/ZnO multilayer has been examined to be placed by the head. Through the copper precursor passage, only nitrogen was placed even though originally, ZnO was deposited. Nitrogen alone was inserted from the outlet after switching off the zinc precursor after the performance of a particular number of cycles. Cu2O started to deposit after the nitrogen bubbling was started from the precursor and it turned on the copper precursor. Figure 3.3d shows an SEM cross-sectional picture of the intersection in the middle part of the deposition which contains various layers of substances. Figure 3.3d ((≈75.0 nm vs. ≈475.0 nm) shows an SEM closeup picture of a slim layer of Cu2O which was placed for the demo as the deposition amount of ZnO is higher than Cu2O (0.020 nm s−1 vs. 1.0 nm s−1, correspondingly) (Muñoz et al., 2012; Hoye et al., 2015). The diverse layers can be seen through the EDS

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analysis performed, even though sufficient resolution cannot be provided as the SEM probe is too huge. Two diverse patterns can be deposited in diverse areas through customized patterns of the head used to inject, as displayed in Figure 3, but through the reproducible and regulated thickness, various layers can also be placed (provided ALD is included).

Figure 3.3. a) 3D illustration of 2 printed heads having diverse outlet measurements (5.0 cm vs. 2.50 cm). b) 3D illustration of a head intended for round shape placement in stationary spatial SCVD (CVD) manner. ZnO circles having dissimilar thickness are displayed (coordinating with depositions of 1.0, 1.50, and 2.0 min). c) 3D illustration of a custom head having 2 unlike precursor outlets made of metal intersecting on the middle area of the deposition location and 3D outlook of the consequential multilayer design that can be attained through a head like this. d) EDS analyses and paralleling SEM images of a ZnO/Cu2O/ ZnO pile placed through a 2-metal precursor head presented in (c).

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3.4 SALD AIDED DIGITAL FABRICATION’S FEATURES The achievement of operational substances’ particular deposition having customized designs can be done by additive manufacturing of the custom heads and their designing as shown in the examples above. A manufacturing and designing stage for every case is needed if the substances are directly and selectively deposited though it is a huge leap ahead. Moreover, whether the head is used in SCVD or SALD method, its features will affect the form of the conclusive deposition in each case. The probability of having topologic manufacturing and the ability to make patterns that are freeform in the 3 aspects is required for specific functions (Poodt et al., 2012). By properly designing the SALD heads, this can be done again. Particular deposition can be achieved by the miniaturing of SALD heads in addition to its suitability due to the great rate of deposition and atmospherically processing in upscaling. A SALD pen’s imagined look is illustrated in Figure 3.4a. Digitally fabricated in pure resin is a SALD pen shown in Figure 3.4b. The round gas passages are set up concentrically while the head is in a cylinder shape as shown in Figure 3.4c. The substrate is revealed to the various precursors as the movement of the head is freeform which leads to the achievement of freeform deposition. The SALD pen’s manufacture and designing are very practical as additive manufacturing offers a lot of flexibility. As presented in Figure 3.4d, the personal printing with the freeform design of operational substances can be simply done in a digital table. The method based on SALD is exceptional even though inkjet printing proposes some similar features. First of all, procedures and applications that cannot work with solvents and require gas deposition will perfectly work with SALD as it is based on it. Also, inkjet printing does not allow the resolution Z to be regulated to the degree of the sub-nanometer which is allowed by SALD as it is based on the method of ALD. Plus, ALD cannot reach the thicknesses which SALD can because of its great degree of deposition. Some advantages provided by various resources of ALD are deposited films’ density, conformality, and lower deposition temperature providing great substance value. CVD reaction-based plasma aerosol or spray coating jets on which other deposition structures are grounded produce thinner films that are less uniform, but it is important when likening them (Vaezi et al., 2013). Sans a pattern stage, a ZnO circle is printed by the SALD pen as drawn in Figure 3.4e, and it is fitted in a 3D table. (Movie S5.0, Supporting Information shows a circle being written by the SALD pen). Using the SALD pen in Figure 3.4f, a

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circle of ZnO on a substrate made of silicon is printed with the thickness of 50.0 nm and was done in four minutes.

Figure 3.4. a) Scheme of a customized design spatial atomic layer deposition (SALD) pen. b) Image of a SALD pen following a 3D print. c) Observation from the base of the SALD pen approach where the concentric circular gas outlets permitting deposition in every direction can be seen. d) Scheme of the SALD pen situated in a 3D table. e) Picture of the printed SALD pen mounted in the 3D table and designing a ZnO circle. f) ZnO circle and g) LMGP initials on a Si wafer composed with the 3D printed SALD pen.

The diameter of the SALD pen is greater than the lateral thickness of the circle. This is because the reaction occurs where the metallic precursor is unsealed under the pen (i.e., beneath the metal precursor outlet and adjoining exhaust outlet). The formation of the head, specifically the diameter of the opening for the metallic precursor as well as the distance among the latter and the adjoining exhaust outlet describes the minimal lateral resolution of the system. However, the deposition parameters (i.e., whether the system is managed in SALD or SCVD mode) can affect the lateral resolution. Figure 3. 4g, is also an example of freeform direct printing with a SALD pen illustrating the lab initials (LMGP) being written with a ZnO film which was 120 nm thick. Although prior techniques allowed a miniaturized plasma gun to exclusively transform the substrate before a conventional ALD

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deposition, this method permits the direct deposition of efficient materials at a reduced temperature with complex designs in the open air (Matter et al., 2021). Never before has a gas-based 3D printing technique been suggested, additionally it is the first time that ALD, with its entire assets, is put into operation as an open-air 3D printing method.

3.5 FUTURE POSSIBILITIES AND SUMMARY Centered on an open-air close-proximity SALD technique, the latest approach has been introduced for the 2D and 3D printing of operational materials, with nanometric resolution in Z. Customized SALD heads, can be prepared and printed without any difficulty at lower prices than standard heads formulated by conventional methods since additive manufacturing provides digital fabrication. Intricate multi-material devices can be printed without requiring patterning procedures and it is simpler to modify the area of the deposition due to these customized heads. Through the execution of depositions in static SCVD mode, complicated designs can be simply prepared with custom printed heads. Lastly, a SALD pen has been created and printed that permits the open-air printing of functional materials through the decrease in the SALD head in size and employing concentric circular gas outlets. According to the concepts evidence, there are few to numerous millimeters in lateral resolution, utilizing optimized engineering additional miniaturization of the SALD pen should give way to a finer lateral resolution, as far as the micron scale, hence permitting the deposition of patterns with more related scales in the three dimensions (Babu et al., 2015; Klein et al., 2015). The same goes for the rest of the ASD approaches put forward. The introduced approach signifies a breakthrough in the area of functional materials, leading the route to easier manufacture of complex and custom devices. For example, the outlets can be planned to have a shape that is not uniform so that non-homogenous films are developed on purpose so that combinatorial studies can be carried out effortlessly (George et al., 2017).

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43. Sanchez, C., Belleville, P., Popall, M., & Nicole, L. (2011). Applications of advanced hybrid organic–inorganic nanomaterials: from laboratory to market. Chemical Society Reviews, 40(2), 696-753. 44. Sevim, S., Franco, C., Liu, H., Roussel, H., Rapenne, L., Rubio‐Zuazo, J., ... & Puigmartí‐Luis, J. (2019). In‐Flow MOF Lithography. Advanced Materials Technologies, 4(6), 1800666. 45. Tan, M. J., Owh, C., Chee, P. L., Kyaw, A. K. K., Kai, D., & Loh, X. J. (2016). Biodegradable electronics: cornerstone for sustainable electronics and transient applications. Journal of Materials Chemistry C, 4(24), 5531-5558. 46. Vaezi, M., Seitz, H., & Yang, S. (2013). A review on 3D micro-additive manufacturing technologies. The International Journal of Advanced Manufacturing Technology, 67(5-8), 1721-1754. 47. Vallat, R., Gassilloud, R., Eychenne, B., & Vallée, C. (2017). Selective deposition of Ta2O5 by adding plasma etching super-cycles in plasma enhanced atomic layer deposition steps. Journal of Vacuum Science & Technology A: Vacuum, Surfaces, and Films, 35(1), 01B104. 48. Wen, L., Zhou, M., Wang, C., Mi, Y., & Lei, Y. (2016). Nanoengineering energy conversion and storage devices via atomic layer deposition. Advanced Energy Materials, 6(23), 1600468. 49. Yan, C., Zhang, X., Ji, Z., Wang, X., & Zhou, F. (2021). 3D-Printed Electromagnetic Actuator for Bionic Swimming Robot. Journal of Materials Engineering and Performance,1, 1-9. 50. Yang, S. M., Lee, S., Jian, J., Zhang, W., Lu, P., Jia, Q., ... & MacManus‐ Driscoll, J. L. (2015). Strongly enhanced oxygen ion transport through samarium-doped CeO 2 nanopillars in nanocomposite films. Nature communications, 6(1), 1-8. 51. Zhu, S., Kherbeche, A., Feng, Y., & Thoraval, M. J. (2020). Impact of an air-in-liquid compound drop onto a liquid surface. Physics of Fluids, 32(4), 041705.

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CHAPTER

4

3D PRINTING TECHNOLOGY FOR SOLAR CELLS

CONTENTS

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4.1 Introduction ....................................................................................... 96 4.2 Printing Technologies History for Photovoltaic Cells........................... 96 4.3 Three-Dimensional Printing ............................................................... 97 4.4 Photovoltaic Cells Flexibility and There Modules ............................... 98 4.5 Solar Concentrators ......................................................................... 100 4.6 3D Printed Solar Panels.................................................................... 102 4.7 Future Prospects .............................................................................. 105 References ............................................................................................. 107

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4.1 INTRODUCTION From the recent several years, photovoltaics (PV) have seen significant expansion in the US and around all of the globe (Haegel et al., 2019; Kustatscher et al., 2019). Global PV shipments, for example, have surged elevenfold in the last decade. PV installations have already totaled 509 GW globally. The accessibility of the resources as well as the available markets, changing technologies of the solar cells, and policies of the domestic government policies all contribute to this adexpansion. With a market share of 96 percent, crystalline silicon has been the most popular PV technology. Solar cells use the photovoltaic effect to develop energy in the existence of the sun. Photons generates electron hole pairs based on their energy. For charge separation, photovoltaic cells include integrated junctions of the p-n. Different types of the metal based contacts are integrated on the facade and back sides of traditional photovoltaic cells to remove such charges. Thus several metal based contacts are just available on the rear side of some advanced gadget architectures (Kaydanova et al., 2004; Hörteis & Glunz, 2008). Now a days In energy sector 3D printing is rapidly becoming a appreciated asset. The effect of 3D farication on renewable energy, in particular, might be very essential. Green energy is one of the most significant challenges of our century in terms of climate change. We are seeing the expansion of electric motors, solar panels as fossil fuels become increasingly scarce. However, the several of these strategies are still fairly costly so must be enhanced. Several researches are employed on three-dimensional printing of photovoltaic panels by hoping that a large amount of sun is used, which is an infinite resource. Researchers said that thanks to additive manufacturing, solar panel production costs might be cut in half. They might even outperform standard solar panels in terms of efficiency. In this blog post, we’ll look at how 3D printing technology is assisting the renewable energy business, notably solar energy (Koval’, 2002; Sopori et al., 2008).

4.2 PRINTING TECHNOLOGIES HISTORY FOR PHOTOVOLTAIC CELLS Ni plating based on electroless process was employed to fabricate metal based contacts on space photovoltaic cells in the 1950s (Iles, 1993). Vacuum evaporation with a metal shadow mask was used to metallize Si solar cells in the 1960s (Green, 1993). Titanium and Silver layers were initially employed

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to collect charges, while Titanium platinum and silver was later on utilized for the metal based contacts. When titanium joins with silicon, a less resistance contact is formed. As a barrier to diffusion, Pd was employed. Pd also improves resistance to corrosion, preventing the contacts from flaking during temperature–humidity testing. As a conductor, silver (about 4 m thick) is employed. The numerous photovoltaic cells were manufactured for space uses until the mid-1970s, while terrestrial solar cells remained too exclusive for the domestic population. The approaches were prolonged, and expensive metallic elements were used . Photovoltaic cells of silicon that has the metal of screen printed based associates with façade of Silver and complete region of Aluminum back links were presented in 1975 (Ralph, 1975). Thus these screen developed contacts were very costly to produce because of their selfaligning nature. During the 1970s and 1980s, individual solar cells were 4 cm2. Drwabacks associated with screen developed photo voltaic cells grew more noticeable as photovoltaic cell sizes increases to hundred cm2 and photovoltaic cells enhanced. Contact metallization became a technological obstacle when solar cell efficiency climbed from 4% to 16.5 percent.

4.3 THREE-DIMENSIONAL PRINTING Additive manufacturing (AM), often known as fast prototyping or 3-D printing, is a rapidly expanding technique utilized in the creation of solar cells. Thus the solid works as well as computer aided drafting of the object to be placed is created using this technique. After that, the structure is used in Slicer programmed. So partilcauly this programme distributes the diagram into layers and carries the guidelines to an imprinter. Then the particular structure is then printed layer by layer on a substrate by utilizing a head of the printer. The procedure can be utlized to deposit solar cell elements directly on the active device or to produce exterior structures (such as light trapping structures). 3D printing has been used to make photovoltaic cells such as copper zinc tin sulphide dye-sensitized solar cells etc. Fused Deposition Modelling (FDM) was utilised by James and Contractor (James & Contractor, 2018) to construct a cost-effective counter electrode on the basis of fractal for cells of DSSC (Figure. 4.1) Dijk et al. (2015) used 3D printing to create external light trapping structures. An organic solar cell module was topped with a reflector array (Fig. 4.2). A number of papers

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(Ruiz et al., 2017; Saengchairat et al., 2017) have focused on the emergence of 3D for electronic components.

Figure 4.1. (a) Illustration using FDM technique of three dimensional printing (b) schematic of nature-influenced fractal electrode in printed. Source: https://link.springer.com/chapter/10.1007/978-3-030-36296-6_178

4.4 PHOTOVOLTAIC CELLS FLEXIBILITY AND THERE MODULES From the recent years 3D printing is utilized for the fabrication of solar applications, having ability of transforming the manufacturing and efficacy of photovoltaic (PV) cells and solar panels. Low-cost production of malleable solar panels for use on housing, and transportable electronics will be possible thanks to 3D printing (Jean et al., 2019).

Figure 4.2. (a) A lab-to-fab translation instrument used for solution-processed solar cells based on a slot-die coater of 3D-printer (b) roll-to-roll printing of

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perovskite solar cells, designed with ability to use at large-scale. Source: https://pubs.rsc.org/en/content/articlelanding/2010/cc/ c0cc01691h

Vack and colleagues used rigid substrates, but there can be an extension of such low-temperature machineries to flexible substrates, generating three dimensional printing a feasible lab-to-fab technique for solution-processed solar cells. Extremly thin semitransparent solar microcells arrays, that can achieve a similar efficiency to traditional solar panels, are a substitute to flexible organic cells. Flexible interconnects, such as flexible front electrodes, are required for this type of display. Front electrodes are one of the most difficult aspects of Si photovoltaic cells in general (Conings et al., 2015). Using a stage of three axes micropositioning attached to a small-nozzle, Ahn et al. were capable to create, spanning, stretchy, and elastic microelectrodes of silver. By the use of the same 3D printing process, similar connecting capabilities were demonstrated for indium oxide doped with Sn, common translucent conductor. These flexible microelectrodes’ remarkable omnidirectionality gives up new possibilities for building complicated threedimensional solar systems. In this regard, Massachusetts Institute of Technology (MIT) researchers used a genetic algorithm to optimise 3D photovoltaic structures with random shapes to maximise energy generation, by greatly enhance the quantity of solar radia, demonstrating solar panels that designed properly may be more useful than flat solar panels of flat shape . Bernardi et al. positioned Si solar cells that exist in market onto three dimensional printed plastic settings with optimum geometries, revealing densities of energy single area of projection that were two to twenty times greater than flat stationary panels and a 1.5 to four times increase in energy density (Hwang et al., 2015; Giacomo et al., 2016). Beyond three dimensional printed plastic settings, these easy or more complicated and effective origami such as three dimensional geometries necessitate the usage of less expensive and customised cells elastic and stretchy intersects, that, as previously shown in this section, are presently under progress by the group of three dimensional printing. In result, three dimensional printing is a good contender for enabling a changing in the 3DPV-based PV-sector

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Figure 4.3. (a) Attachment of an unplanarized array of Si solar micro-cell by spanning silver microelectrodes put in by 3D printing ; (b) response of current (I)–voltage (V) of and an array of 14-microcell linked by silver microelectrodes and a single silicon solar microcell; (c) Si ribbons printed by spanning ITO microelectrodes; and (d) three dimenional structure of ITO strips. Source: https://pubmed.ncbi.nlm.nih.gov/19213878/

4.5 SOLAR CONCENTRATORS The recent demonstration in external light traping using 3D-printed concentration arrays on thin film solar cells has piqued intrigue in 3D-printed fabrication of functional devices and parts in photovoltaic application. This mechanism works by sunlight focus via parabolic concentrator sperture (small) before it reaches the solar cell, and then diverts photons which are reflected upwards by the cell using a spacer. Light travels through the photovoltaic cell numerous times as a result of the retro-reflection, resulting in a considerable band absorption improvement and greater PCE (Giacomo et al., 2016). ELT via parabolic mirrors preserves the photovoltaic cell’s attributes because it doesn’t alter the cellfrom core, allowing thin film solar cells to benefit from its high quality. In this regard, van Dijk and colleagues just published an ELT optimization analysis using 3D-printed WLT with

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hexagonal, square, and round compound parabolical concentrator arrays (PCAs). They showed the placing silver-coated smoothened, silver-coated thermoplastic traps on organic solar cell top increased the External Quantum Efficiency (EQE) by Fifteen to twenty seven percent for tinny layer nanocrystalline silicon, crystalline silicon, and natural solar cells (Yoon et al., 2011). A 3D-printed CSC installed on a organic flat solar cell has been claimed to boost the EQE by up to 16 percent.

Figure 4.4. (a) Before and after chemical smoothening of a three dimensional-printed compound parabolic solar concentrator (CPC); the larger surface is showed by insets . (b) Main focal ring of sunlight of a silver-coated CPC (c) A CPC and separate enclosure that can be used to form an exterior trap of light. (d) from the entering side, the reflection in the parabolic curve is seen in this perspective of the CPC. The red encircles two wrinkles in the concentrator. Source: https://www.osapublishing.org/oe/fulltext.cfm?uri=oe-24-14A1158&id=345203

Furthermore, the same concentration integrated optics that were developed to maximise the PCE of PV technology like discussed can be used to achieve high energy densities required for solar radiation modification to attain a better match with the dependent wavelength transformation efficacy of the PV device in known as ‘‘Third Generation Solar Cells,” also called upconversion solar cells (UC-PV). Luminescence procedures of Up-conversion

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(UC) combine two photons of low-energy (sub-band gap) into one photon of high-energy. The composed solar spectrum can be extended in existing solar cells by enhancing the solar cell and spectral up-converter materials separately (transition metals, actinides and lanthanides). This direction of research has seen Arnaoutakis and others successfully integrate focusing optics into up-conversion PV tools (Gizachew et al., 2011; Galagan et al., 2012). Films based on and polymer-based coatings and focusing optics have been an achievement since they were first introduced Such a sophisticated device technology, which has been done in past few years with the usage of multi-material stereo-lithography, is very useful for using 3D-printing technologies (SLA). High-quality plastic optics with high quality has been produced by printing technology (Printopticalr118). Price et al. Such a sophisticated device technology, which has been done in past year with the help of multi-material stereo-lithography, is particularly advantageous for employing 3D-printing technologies (SLA). To generate high-quality plastic optics, new UV-inkjet printing technology (Printopticalr118) has been established. Organic resins doped with SLA printable rare-earth developed for spectral converting enables for the direct manufacture of combined upconversion plus focusing optics for a new production of improved solar cells via 3D printing (Jiang et al., 2016).

4.6 3D PRINTED SOLAR PANELS Solar panels are photovoltaic modules that generate heat or electricity from the sun. Solar cells make these devices. The solar cells’ job is using physical and chemical processes to convert light into electricity. The majority of these solar elements are composed of crystall-like silicon, but scientists are rapidly developing other materials, such as thin-film solar cells (Jiang et al., 2016). The development of that fascinating device of energy is yet ongoing. In terms of efficacy and quality, conventional solar panels can be improved yet. As a result, three dimensional printing aficionados are responsible for their particular research for the formation of amazing three dimensional printed solar panels.

4.6.1 Best Solution to Make Solar Panels- 3D Printing Over prices are certainly impeding the formation of renewable energy. These technologies are of high costs and not available to the general public yet. Solar panels are a great illustration of how 3D printing can be used to develop new projects.

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To begin, developing good solar panels involves extensive research and development. These panels require solar cells, which are a type of technology that turns light into power and was previously made with expensive materials (Ruiz et al., 2017). A huge number of experiments and prototypes are required to develop an entirely new solar panel based on new materials with revolutionary technological capabilities. These are the projects in discussion which require clarity, and you’ll need good miniatures to show your team, investors, or potential clients the entire project. Here, three dimensional printing may be your partner, as it will authorize you to produce samples with high-quality and perform all of the necessary iterations. However, if you desire to employ additive production to make something, you’ll have to make the materials’ print. For solar panels, like, a certain material must be used to absorb the sunlight. (Ahn et al., 2009)

4.6.2 The Cost is reduced by 50 Percent using 3D Printed Solar Panels Solar panel production costs could be cut in half thanks to additive printing, according to MIT researchers. Expensive materials like glass, polysilicon, and indium aren’t required for these novel structures. The new constituents that could now be three dimensional printed are, of course, what makes these projects possible. Synthetic perovskite, for example, is now recognized as a less expensive material for solar devices (Ahn et al., 2009).

4.6.3 Easy Implanation in Deveopling Countires Solar panels can be 3D printed, and they are less expensive than regular glass panels. Because procedures for printing ultra-thin solar strips have been discovered, the 3D printed panels are indeed lighter. It also decreases the problems associated with their transportation by reducing their weight. Because this technology is getting more affordable, it is now a viable option for making renewable energy accessible and transportable to anybody, everywhere, even underdeveloped countries with limited access to electricity (Ahn et al., 2010).

4.6.4 Efficiency is enanced by20 Percent using 3D Printed Solar Panels These panels are also twenty percent more effective than traditional panels in terms of quality, as 3D printing has enabled the development of new processes, 3D printing materials, and new designs. The solar industry

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need a fresh innovation, and more importantly, a strategy to become more inexpensive. In this discipline, 3D printing appears to be the new revolution (Ryu et al., 2012).

4.6.5 Making Solar Panels owes to 3D Printing There is already a new technology of three dimensional printed solar cell. This invention has the potential to revolutionise the market of renewable energy. For example there are few companies that use three dimensional printing to manufacture solar panels, as well as scientists who are searching best ways to manufacture better solar cells. CSIRO is printing solar cell rolls using industrial 3D printers. These Australian researchers were successful in making A3 solar cell sheets that may be applied to some surface, like buildings or windows (Bernardi, 2012). Those solar panels are both efficient and functional. Those are the largest solar cells, and they are made of a lightweight flexible plastic. The researchers created an ink that is photovoltaic in nature that is applied to the flexible plastic strip. Screen printing, gravure coating, and slot-die coating are all part of this process. They were able to construct a precise system thanks to additive manufacturing.

Figure 4.6. Solar cell created at the CSIRO. Source: https://www.csiro.au/en/Research/MF/Areas/Innovation/Flex-Electronics/Printed-Solar-Cells

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4.6.6 The Future of Solar Panels by 3D Printing In this industry, three dimensional printing may fast make a valuable asset. It may, for instance, enable bulk customisation in that industry. People will be capable to order personalised 3D printed solar panels that are tailored to their specific needs, with the proper form and size. The newly created 3D printing material has the potential to revolutionise the solar energy industry. Furthermore, these cheap and effective structures will be ideal for creating solar-powered gadgets that might supply electricity to rural locations world-wide (Ruiz et al., 2017). The 3D printing and business of energy and are becoming excellent collaborators. They could certainly work together to produce a slew of reasonable green energy projects to combat climate fluctuation.

4.7 FUTURE PROSPECTS Solar cells of flexible multi-layer and complicated three dimensional solar collectors are among the more complex uses of printed electronics. This large-area, low-cost 3D printing method will likely enable the anticipated revolution of 3D solar systems that are greatly effective even without sun monitoring. Major advancements in three dimensional printing of high-quality optics and flexible (contact) materials, as well as the development of novel printable active materials inks for constructing multilayer devices, are still required before this can happen (Sha et al., 2015). Finally, it’s worth keeping an eye on the formation of ecologically sensitive materials that can dynamically change arrangements in response to external stimuli with time, because shape-memory polymers used in known as 4D printing may be particularly useful for evolving adaptable harvesting, dynamic, and self-configurable tools like solar cells (Sha et al., 2015).

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Figure 4.7. Behind the solar cell ,(UC-PV) tool schematic with combined optics. (b) a bifacial silicon solar cell ,one of the parabolic concentrators connected is shown in detail. The UC phosphor is linked to the parabolic concentrator’s exit aperture. (c) A CPC optics’ 2D array of integrated with a standard two-dimensional array of the UC-SC. The spaces between the layers are merely there to show how they work. Source: https://www.osapublishing.org/oe/abstract.cfm?uri=oe-22102-A452

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Ahn, B. Y., Duoss, E. B., Motala, M. J., Guo, X., Park, S. I., Xiong, Y., ... & Lewis, J. A. (2009). Omnidirectional printing of flexible, stretchable, and spanning silver microelectrodes. Science, 323(5921), 1590-1593. 2. Ahn, B. Y., Lorang, D. J., Duoss, E. B., & Lewis, J. A. (2010). Direct-write assembly of microperiodic planar and spanning ITO microelectrodes. Chemical communications, 46(38), 7118-7120. 3. Allison, J. L. J. (1973). The violet cell: an improved silicon solar cell. Comsat technology Review, 3, 1-22. 4. Bag, M., Jiang, Z., Renna, L. A., Jeong, S. P., Rotello, V. M., & Venkataraman, D. (2016). Rapid combinatorial screening of inkjetprinted alkyl-ammonium cations in perovskite solar cells. Materials Letters, 164, 472-475. 5. Bernardi, M. (2012). N. Ferralis, JH Wan, R. Villalon. J. Grossman. Solar energy generation in three dimensions. Energy & Environmental Science, 5, 6880-6884. 6. Conings, B., Drijkoningen, J., Gauquelin, N., Babayigit, A., D’Haen, J., D’Olieslaeger, L., ... & Boyen, H. G. (2015). Intrinsic thermal instability of methylammonium lead trihalide perovskite. Advanced Energy Materials, 5(15), 1500477. 7. Di Giacomo, F., Fakharuddin, A., Jose, R., & Brown, T. M. (2016). Progress, challenges and perspectives in flexible perovskite solar cells. Energy & Environmental Science, 9(10), 3007-3035. 8. Dijk, L. V., Paetzold, U. W., Blab, G. A., Schropp, R. E., & Di Vece, M. (2016). 3D‐printed external light trap for solar cells. Progress in Photovoltaics: Research and Applications, 24(5), 623-633. 9. Doshi, P., Mejia, J., Tate, K., & Rohatgi, A. (1997). Modeling and characterization of high-efficiency silicon solar cells fabricated by rapid thermal processing, screen printing, and plasma-enhanced chemical vapor deposition. IEEE Transactions on Electron Devices, 44(9), 1417-1424. 10. Fischer, M. (2018, March). ITRPV 9th edition 2018 report release and key findings. In PV CellTech conference, 14, 6-19. 11. Galagan, Y., Coenen, E. W., Sabik, S., Gorter, H. H., Barink, M., Veenstra, S. C., ... & Blom, P. W. (2012). Evaluation of ink-jet

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printed current collecting grids and busbars for ITO-free organic solar cells. Solar Energy Materials and Solar Cells, 104, 32-38. Gizachew, Y. T., Escoubas, L., Simon, J. J., Pasquinelli, M., Loiret, J., Leguen, P. Y., ... & Aguerre, J. P. (2011). Towards ink-jet printed fine line front side metallization of crystalline silicon solar cells. Solar Energy Materials and Solar Cells, 95, 70-82. Granek, F., Hermle, M., Huljić, D. M., Schultz‐Wittmann, O., & Glunz, S. W. (2009). Enhanced lateral current transport via the front N+ diffused layer of n‐type high‐efficiency back‐junction back‐ contact silicon solar cells. Progress in photovoltaics: research and applications, 17(1), 47-56. Green, M. A. (1993). Silicon solar cells: evolution, high-efficiency design and efficiency enhancements. Semiconductor science and technology, 8(1), 1. Haegel, N. M., Atwater, H., Barnes, T., Breyer, C., Burrell, A., Chiang, Y. M., ... & Bett, A. W. (2019). Terawatt-scale photovoltaics: Transform global energy. Science, 364(6443), 836-838. Hahn, G., & Schönecker, A. (2004). New crystalline silicon ribbon materials for photovoltaics. Journal of Physics: Condensed Matter, 16(50), R1615. Hörteis, M., & Glunz, S. W. (2008). Fine line printed silicon solar cells exceeding 20% efficiency. Progress in Photovoltaics: Research and Applications, 16(7), 555-560. Hwang, K., Jung, Y. S., Heo, Y. J., Scholes, F. H., Watkins, S. E., Subbiah, J., ... & Vak, D. (2015). Toward large scale roll‐to‐roll production of fully printed perovskite solar cells. Advanced materials, 27(7), 12411247. Iles, P. A. (2001). Evolution of space solar cells. Solar Energy Materials and Solar Cells, 68(1), 1-13. James, S., & Contractor, R. (2018). Study on nature-inspired fractal design-based flexible counter electrodes for dye-sensitized solar cells fabricated using additive manufacturing. Scientific reports, 8(1), 1-12. Jean, J., Woodhouse, M., & Bulović, V. (2019). Accelerating photovoltaic market entry with module replacement. Joule, 3(11), 2824-2841. Jiang, Y., Chen, Y., Zhang, M., Qiu, Y., Lin, Y., & Pan, F. (2016). 3D-printing Ag-line of front-electrodes with optimized size and

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interface to enhance performance of Si solar cells. RSC advances, 6(57), 51871-51876. Kaydanova, T., Miedaner, A., Curtis, C., Alleman, J., Perkins, J. D., Ginley, D. S., ... & Chiu, L. (2003). Direct inkjet printing of composite thin barium strontium titanate films. Journal of materials research, 18(12), 2820-2825. King, B. H., O’Reilly, M. J., & Barnes, S. M. (2009). Characterzing aerosol Jet® multi-nozzle process parameters for non-contact front side metallization of silicon solar cells. In 2009 34th IEEE Photovoltaic Specialists Conference (PVSC), 16, 1107-1111. Koval’, I. V. (2002). N-halo reagents. N-halosuccinimides in organic synthesis and in chemistry of natural compounds. Russian journal of organic chemistry, 38, 301-337. Kustatscher, E., Plesker, R., Philipps, S., & Franz, M. (2019). First record of plant fossils from the Upper Muschelkalk (late Anisian, Middle Triassic) at Bruchsal (Baden-Württemberg, Germany). Zeitschrift der Deutschen Gesellschaft für Geowissenschaften, 4 (56), 321-338. Prudenziati, M., Moro, L., Morten, B., Sirotti, F., & Sardi, L. (1989). Ag-based thick-film front metallization of silicon solar cells. Active and passive electronic components, 13(3), 133-150. Ralph, E. L. (1975, May). Recent advancements in low cost solar cell processing. In 11th Photovoltaic Specialists Conference, 2 (6), 315. Ruiz-Morales, J. C., Tarancón, A., Canales-Vázquez, J., MéndezRamos, J., Hernández-Afonso, L., Acosta-Mora, P., ... & FernándezGonzález, R. (2017). Three dimensional printing of components and functional devices for energy and environmental applications. Energy & Environmental Science, 10(4), 846-859. Ryu, J., D’Amato, M., Cui, X., Long, K. N., Jerry Qi, H., & Dunn, M. L. (2012). Photo-origami—Bending and folding polymers with light. Applied Physics Letters, 100(16), 161908. Saengchairat, N., Tran, T., & Chua, C. K. (2017). A review: Additive manufacturing for active electronic components. Virtual and Physical Prototyping, 12(1), 31-46. Schubert, G., Beaucarne, G., Tous, L., & Hoornstra, J. (2019, September). Trends in metallization and interconnection–Results of the survey conducted during the 8th Metallization and Interconnection Workshop. In AIP Conference Proceedings, 2156 (1), 20002.

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33. Sha, W. E., Ren, X., Chen, L., & Choy, W. C. (2015). The efficiency limit of CH3NH3PbI3 perovskite solar cells. Applied Physics Letters, 106(22), 221104. 34. Shanmugam, V., Wong, J., Peters, I. M., Cunnusamy, J., Zahn, M., Zhou, A., ... & Mueller, T. (2015). Analysis of fine-line screen and stencil-printed metal contacts for silicon wafer solar cells. IEEE Journal of Photovoltaics, 5(2), 525-533. 35. Sopori, B., Rupnowski, P., Appel, J., Mehta, V., Li, C., & Johnston, S. (2008). Wafer preparation and iodine-ethanol passivation procedure for reproducible minority-carrier lifetime measurement. In 2008 33rd IEEE Photovoltaic Specialists Conference, 14, 1-4. 36. Teng, K. F., & Vest, R. W. (1988). Metallization of solar cells with ink jet printing and silver metallo-organic inks. IEEE Transactions on components, hybrids, and Manufacturing Technology, 11(3), 291-297. 37. Untch, M., Rezai, M., Loibl, S., Fasching, P. A., Huober, J., Tesch, H., ... & von Minckwitz, G. (2010). Neoadjuvant treatment with trastuzumab in HER2-positive breast cancer: results from the GeparQuattro study. Journal of Clinical Oncology, 28(12), 2024-2031. 38. van Dijk, L., Marcus, E. P., Oostra, A. J., Schropp, R. E., & Di Vece, M. (2015). 3D-printed concentrator arrays for external light trapping on thin film solar cells. Solar Energy Materials and Solar Cells, 139, 19-26. 39. Yoon, J., Baca, A. J., Park, S. I., Elvikis, P., GEDDES III, J. B., Li, L., ... & Rogers, J. A. (2011). Ultrathin silicon solar microcells for semitransparent, mechanically flexible and microconcentrator module designs. In Materials for Sustainable Energy: A Collection of PeerReviewed Research and Review Articles from Nature Publishing Group, 13 (5), 38-46.

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3D PRINTED COMPONENTS FOR FLEXIBLE SUPERCAPACITORS

CONTENTS

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5.1 Introduction ..................................................................................... 112 5.2 Synthesis Techniques of 3D Printed Capacitor .................................. 114 5.3 3D Printed Supercapacitors Characterization ................................... 115 References ............................................................................................. 123

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5.1 INTRODUCTION The miniaturised energy storage systems research significantly stimulate the increasing demand for wearable and portable electronics, e.g., wearable sensors and implantable medical devices (Yu et al. 2020; Zheng et al. 2020). The perfect candidate is Micro-supercapacitors (MSCs), where charges can be accumulated by redox reactions or reversible electrostatic ion adsorption at the interface within the electrolytes and electrodes (Hu et al., 2015; Lu et al., 2019). Substantial attention is received because of their long-term cycle life, high-rate capability, and high power density (Tahir et al. 2019). Crafting in-plane MSCs by situating electrodes in an interdigitated model fully inflated the benefits of the electrode materials (Kyeremateng, et al., 2017; Zhang, Cao, et al. 2019). Several patterning mechanisms are used to found patterned electrodes, e.g., spray-masking, photolithography, and laser scribing (Liu et al. 2016; Brousse et al. 2018). Nevertheless, few leading restraints like complex processing, present in the large-scale MSCs production. To reduce such drawbacks, the progress of high-performance MSCs is needed urgently that are created in a more effective but simple way. For broad applications, being a disruptive technology, threedimensional (3D) printing, recognized as additive manufacturing (AM) as well appeared. This approach is able to pattern electrode (or electrolyte) materials for the purpose of energy storage, within three dimensions by employing a computer-aided design (Zhang & McKeon, 2019; Pang et al. 2020). For the creation of 3D patterned structures, within recent 3D printing mechanisms, direct ink writing (DIW) is generally used that depends upon the ink extrusion by an ensuing layer-by-layer deposition of the extruded ink and a nozzle (Sun et al. 2015; Ambrosi & Pumera, 2016). Because of the association of material flexibility properties and low cost, DIW has evolved into progressively powerful in applications of miniaturised energy storage (Zhang et al. 2017; Tian & Zhou 2020). One of the research frontiers is 3D printed MSCs; pervasive endeavours have been committed to obtaining effective energy storage. Still, these researches are in their inception. The adjustment of electrode materials is proven to be significant to boost more the electrochemical nature of 3D printed MSCs. For MSCs, there has been the development of two leading electrode materials. The first as carbon materials, like two-dimensional (2D) graphene nanosheets (NSs) and one-dimensional (1D) carbon nanotubes, are broadly used in micro-electric double-layer capacitors (m-EDLCs), where high-rate proficiency is found and ion adsorption takes place (Sun et al. 2015; Liu et al.

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2017). Whereas, the higher capacitances are offered by the common usage of pseudocapacitive materials e.g., transition metal oxides. Nevertheless, as compared to m-EDLC materials, they offer lower-rate capacity owing to the existence of micro-pseudocapacitors (MPCs) Faradic redox reactions (Kurra et al. 2015; Tian et al. 2015).

Figure 5.1. A capacitor - 3D printed. Source: https://www.nano-di.com/blog/dragonfly-3d-printed-pcb-with-6-capacitors-and-soldered-components

There are attracted broad attention of a classical transition metal oxide, Fe2O3. Its increased theoretical capacitance is the reason that makes it an auspicious pseudocapacitive material. Nevertheless, its decreased electrical conductivity impedes its usage in energy storage prospects (Zhou et al. 2018; Kumar et al. 2020). The assimilation of pseudocapacitive materials and conductive carbon into printable inks is known as an auspicious approach to make better the electrical conductivity by constituting an optimized structure of electrode with abundant redox-active sites and agile kinetic channels for electrodes, which necessarily stimulates the thorough electrochemical nature of 3D printed MSCs (Zhu et al. 2014; Gu et al. 2016). One of the principal hurdles for finding alike printable inks places in the scrupulous control of the formulations of ink. Furthermore, to keep a superior electrochemical role at hard conditions, there is an expectation of reliable mechanical flexibility, which, for wearable MSCs, turns into a principal challenge. Hither, there is a discussion of 3D printed Ag electrodes/graphene/ Fe2O3 with a cost-effective DIW approach for solid-state flexible MSCs. With the mixture of 2D graphene NSs, 1D Ag nanowires (NWs), and Fe2O3

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nanoparticles (NPs) using binder, the immensely concentrated printable electrode ink is developed well. For 3D printed MSCs, high energy density, high device areal capacitance, and promising cycling stability are found using the improvement in synergistic structure. At the same time, reliable flexibility is shown at different cycles and bending angles (Tan et al. 2019). Their enormous potential in applications of wearable and portable electronics is indicated by the promising flexibility and superior performance of electrochemical of the 3D printed MSCs (Yang et al. 2020).

5.2 SYNTHESIS TECHNIQUES OF 3D PRINTED CAPACITOR 5.2.1 Formation of Fe2O3 NPs 1.212 g Fe(NO3)3–9H2O is supplemented into 60 ml deionized water by following the classical Fe2O3 NP synthesis method (Owusu et al. 2017). After getting a clear solution, after that, the mixture is stirred for 2 hours. Subsequently, the formed solution is moved to a Teflon-lined stainlesssteel autoclave and stored for 24 hours at 120°C. Later, tempered to room temperature, the commodity is centrifuged for 10 minutes at 11,000 rpm and ished many times with ethanol and deionized water. At last, it is dried for 12 hours at 70°C to attain Fe2O3 NPs.

5.2.2 Formation of Fe2O3/graphene/Ag ink Firstly, graphene NSs and Fe2O3 NPs (by Ashine Advanced Carbon Materials Co., Ltd) and the aqueous solution of Ag NWs (10 mg mL−1, by Zhejiang Kechuang Advanced Materials Co., Ltd) are added to compose a mixture having 6 : 2 : 1 mass ratio (i.e., Fe2O3 : graphene : Ag). After that, for the removal of the remaining moisture, the composite dispersion is maintained for 12 hours at 70°C. Polyvinylidene fluoride (PVDF) binder having 1 : 9 mass ratio is inserted into the fully dried mixture. It is then blended uniformly and prepared. Ultimately, a suitable quantity of N-Methyl pyrrolidone (NMP) solvent is supplemented into the composition to make printable Fe2O3/graphene/Ag ink through a high-speed mixer (5 minutes, 3500 rpm). For the purpose of contrasting, Fe2O3/Ag ink (having a mass ratio among Ag, Fe2O3, and PVDF being 1 : 6 : 1) and the bare Fe2O3 ink (having a mass ratio between PVDF and Fe2O3 being 1 : 6) are achieved by the same scheme.

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5.2.3 Device Fabrication On the PET substrate, being a current collector, a silver paste is printed before electrodes printing. There is an insertion of prepared ink into a 5 ml syringe using a nozzle (whose inner diameter is about 330 μm) and is printed on the current collector as interdigital electrodes with the help of the 3-axis extrusion system. Subsequently, there is an immersion of the as-printed electrodes in deionized water and after that freeze-dried for 8 hours. For the formation of LiCl-polyvinyl alcohol (PVA) gel electrolyte, classical methods are followed. In deionised water of 10 ml, PVA of 1 g and LiCl of 0.85 g are added which is kept being mixed up at 95°C till the solution clarify. At last, to get a solid-state micro-supercapacitors, using LiCl-PVA gel electrolyte, the electrodes are covered uniformly and dried for 30 minutes at 70°C (Gu et al. 2016).

5.2.4 Electrochemical Measurements and Structural Characterization X-ray diffraction (XRD) analyzes the crystal structure on an X-ray diffractometer (Discovery of Bruker D8) using Cu Kα radiation (i.e., λ = 1.5418 Å). There is a record of a 2θ angle of diffraction spectra from 10–90°, at a rate of 5° min−1 and 0.02°step size. A field-emission scanning electron microscopy (SEM, JEOL-7100F) provided with energy dispersive spectrum (EDS) collects the morphologies of all devices and materials. With a Raman spectroscope, Raman spectra are gathered (i.e., Horiba Scientific LabRAM HR Evolution). Galvanostatic charge-discharge (GCD) measurements, electrochemical impedance spectroscopy (EIS), and cyclic voltammetry (CV) tests evaluate the electrochemical performance of every MSCs in a two-electrode system with an electrochemical workstation (CHI 760E). Anton Paar MCR102 identifies the rheological characteristics of Fe2O3/graphene/Ag composite ink. Agilent B1500A Semiconductor Device Analyzer measures the electrical transport characteristics of the printed wired electrodes (Li et al. 2019).

5.3 3D PRINTED SUPERCAPACITORS CHARACTERIZATION There are two main phases of the DIW procedure of the hybrid-dimensional electrodes, as shown in Figure 5. 2(a).

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In the initial phase, for the construction of the current collector, there is an implementation of the DIW of silver paste onto the PET substrate. The fixed pneumatic pressure drives the ink extrusion. There are many interdigitated fingers that are involved in the composition of the designed pattern. A roundtrip printing routine is used for each finger (Haider et al. 2020). It is worth observing that the DIW process has the capacity of scripting MSC arrays in one single operation, as illustrating in Figure 5. 2(b), exhibiting its benefit.

Figure. 5.2. (a) Diagram of the process of DIW of 3D printed adaptable MSCs having Fe2O3/graphene/Ag electrodes. Images of (b) interdigitated silver pattern arrays - 3D printed, (c) hybrid-dimensional electrode arrays - 3D printed and (d) a 3D printed MSC in a bending.

In the second phase, there is a subsequent performance of the Fe2O3/ graphene/Ag electrode ink DIW after regulating the previous interdigitated silver pattern. The Fe2O3 NPs respond being the active material; the 1D silver nanowires (NWs) and 2D graphene NSs are acted being the conductive additives. With the hydrothermal procedure, Fe2O3 NPs are found prior to the preparation of electrode ink (Owusu et al. 2017). It is found that the spherical morphology is dispersed uniformly, where the diameters of the particle are primarily distributed in the range of 30 nm - 60 nm. Typically, Fe2O3-based materials are recognized as pseudocapacitive and are broadly utilized for the applications of symmetric supercapacitors (Li et al. 2019; Serrapede et al. 2019). The weak transportation of electrons during the processes of discharge and charge is the main barrier for such applications. Thus, 1D Ag

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NWs and 2D graphene NSs are made known to synergistically improve the transportation of electrons of Fe2O3 NPs in the hybrid-dimensional electrode ink. Direct evidence is presented by the electrical transport characterization of different printed electrodes that there is a significantly higher electrical conductivity concerning Fe2O3/graphene/Ag composite as compared to that of the Fe2O3/Ag composite and bare Fe2O3 nanoparticles. An appropriate amount of solvent rigorously regulates the mass ratio of 2D graphene NSs, 1D Ag NWs, and Fe2O3 NPs. A slight amount of binder is added further to make highly concentrated Fe2O3/graphene/Ag electrode ink to make sure the good printability of electrode ink. 3D printed MSCs are attained subsequent to the post drying method, as illustrated in Figure 5. 2(c and d), where initially good flexibility is noticed.

5.3.1 Viscosity Measurements For the study of the printability of the as-prepared electrode ink, its fluidity behaviour is noticed. A smooth extrusion out of the micronozzle is enabled by the found electrode ink as shown in the inlay of Figure 5. 3(a). If the bottle having the electrode ink at its bottom is reversed, the ink is not moved down towards the wall of the bottle and remained at the bottom firmly even after 24 hours (refers to Figure 5. 3a), which shows its high viscosity and also the solid-like rheological behaviour. As anticipated, high apparent viscosity (>107 mPa s) and good shear-thinning property are shown by such highly concentrated ink, as illustrated in Figure 5. S4. Hence, there will be stable and continuous printing with this ink (Zhang, Shi, et al. 2019). For the study of the crystallographic characterization of the materials and the steps of the electrode ink, XRD is used. All the peaks attained for Fe2O3 NPs relate to the Fe2O3 stages (JCPDS card no. 33-0664) as shown in Figure 5. 3(b); there is no clue of other characteristic impurity peaks, showing the sample’s high purity. In contrast, the presence of Ag NWs is disclosed clearly by the characteristic peaks of the 3D printed MSC electrode. For the investigation of the variations of the attained electrode inks, Raman spectroscopy is performed further. Raman spectra (refer to Figure 5. S5a) having bands at 274, 214, 583, 383 cm−1 are attributed to the existence of Fe2O3 NPs in the uncovered Fe2O3 electrodes (Yin et al. 2019; Zhang, Shi, et al. 2019). The G band and D band are indicated by the newly arose peaks at 1590 and 1350 cm−1, respectively, approving the presence of graphene within the Fe2O3/graphene/Ag electrode ink (Li et al. 2017; Wang et al. 2019). For the Fe2O3/graphene/Ag electrodes, EDS analysis is

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performed as well employing the silicon substrate, where the C, Fe, O, and Ag components are obtained and the presence of graphene NSs, Ag NWs, and Fe2O3 NPs is approved further.

Figure 5.3. (a) Images of the found electrode ink at various time periods (the inset illustrating the ink extrusion state out of a micronozzle). (b) MSC electrodes and XRD patterns of Fe2O3 NPs. (c) Image and (d, e) SEM photographs of MSC electrodes - 3D printed.

5.3.2 Microstructural Investigation Figure 5. 3(c) shows the 3D printed MSC’s size with details. Further, the microstructure of 3D printed electrodes is investigated with the help of SEM. No link within neighbouring electrodes is attained in the interdigitated symmetric electrodes being a good pattern is led by using the method of DIW. With respect to the SEM photographs of the printed MSC electrodes ( refers to Figure 5. 3(d)), the finger’s thickness is around 320 μm and the breadth of each finger is erected to be greater than two times of the internal nozzle’s diameter (Sun et al. 2018). The MSC electrodes’ inner structure is further disclosed by the higher-magnification SEM photograph (refers to Figure 5. 3e), where the 1D Ag interwoven NWs are entered within the graphene layers and the 2D graphene NSs serves to be the supporter. Fe2O3 NPs are strongly connected to 1D Ag NWs and dispersed well. It could be concluded that the promising electrode ink’s printability is partly associated with its favourable internal distribution.

5.3.3 Electrochemical Characterization GCD measurements and CV tests are operated in a two-electrode system with LiCl-PVA gel electrolyte to determine the electrochemical nature of the

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printed symmetrical MSCs. In the MSCs, the contribution of the capacitance of the silver current collector is disclosed to be negligible at the start. In Figure 5. 4(a), the CV plots show that redox reaction-based spikes are noticed for uncovered Fe2O3/ Ag, Fe2O3/graphene/Ag, and Fe2O3 dependent MSCs. Such spikes may be referred to as the Li+ addition in Fe2O3 (Sun et al. 2018). In contrast, there are too higher peak current values of Fe2O3/ graphene/Ag MSCs as compared to those of the uncovered Fe2O3 MSCs, signifying greater charge-discharge capacitances of the prior. In Figure 5. 4(b), the GCD plots represent similar discharge and charge behaviours; where an extreme 1.3 V voltage window is viable for every symmetrical MSC device. Figure 5. 4(c) present the relevant discharge capacitances. The 412.3 mF cm−2 maximal areal capacitance is shown by the Fe2O3/graphene/ Ag MSCs at 2 mA cm−2 current density which is much greater than that of the Fe2O3/Ag MSCs (i.e., 224.1 mF cm−2) and uncovered Fe2O3 MSCs (i.e., 19.9 mF cm−2). This is direct evidence that there is a structural benefit of Fe2O3/graphene/Ag MSC electrodes comparable to uncovered Fe2O3 and Fe2O3/Ag MSC electrodes (Zhang & McKeon, 2019).

Figure 5.4. (a) CV plots at 10 mV s−1 scan rate, (b) GCD plots at 2 mA cm−2 current density, and (c) device areal capacitances of different 3D printed MSCs. (d) CV plots, (e) GCD plots, (f) Nyquist curve and (g) protracted cycling stability of Fe2O3/graphene/Ag MSCs comparable to those of formerly recorded MSCs.

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As illustrated in Figure 5. 4(d), for Fe2O3/graphene/Ag MSCs, with the increase of scan rates, in CV plot the increase in current densities are noticed; for the scan rates less than 50 mV s−1, redox current peaks can be obtained, demonstrating discharge processes and good pseudocapacitive charge. The maximum of 336.5 mF cm−2 device areal capacitance is yielded by Fe2O3/graphene/Ag MSCs at the 5 mV s−1 scan rate, which is too greater than that of the uncovered Fe2O3 MSCs and Fe2O3/Ag MSCs. For the hybriddimensional MSCs, the Nyquist curve (see Figure 5. 4f) and the GCD plots found at different current densities (see Figure 5. 4e) further approve the speedy electrolyte ions diffusion, and the promising pseudocapacitive behaviours, respectively (Bellani et al. 2019). For the study of the MSCs cycling stability, a protracted cycling test is administered. Exceptionally 89% of high capacitance retention is exhibited as illustrated in Figure 5. 4g, for above 5000 discharge and charge cycles, recommending the processes of charge storage are highly stable. The Ragone curve of the Fe2O3/graphene/Ag MSCs is shown in Figure 5. 4h, where the estimated power densities and areal energies are 1.07 mW cm−2 and 65.4 μWh cm−2, respectively, over 2 mA cm−2 current density (refers to Table S1). This Ragone curve is clear evidence that the power density and energy density values of the MSCs are necessarily beneficial when compared with prior recorded MSCs like NiCo2O4 MSCs, SWCNTs MSCs, Ti3C2Tx MSCs, and activated graphene (AG) sodium-ion micro capacitors (NIMCs)//sodium titanate (NTO) (Lu et al., 2019; Zheng et al. 2019). For the MSC devices, the remarkable electrochemical performance is chiefly associated with the optimal 3D printed hybrid-dimensional electrode structure, which supports the ionic transport and swift electron transport while the processes of discharge and charge. Ion migration occurs within two electrodes during the processes of discharge and charge, where there is an abundantly different electrical transport in different electrodes. Less electrical transport is indicated by the elemental low electrical conductivity of the arid Fe2O3 MSCs. The electrical transport is improved to some extent while introducing Ag NWs. There is a creation of a highly conductive 3D network using 2D graphene NSs and 1D Ag NWs in Fe2O3/graphene/Ag electrodes, where there is a significant boost of electrical transport. Hence, effective ionic transport can also be carried out in electrodes. The improvement of the electrochemical performance of the device has resulted from the exceptional transport of ions and electrons (An et al. 2017).

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Figure 5.5. (a) 3D printed Fe2O3/graphene/Ag MSCs Bending test showing great flexibility. (b) CV plots at various bending angles and (c) capacitance retention all along the cyclic bending of 3D printed Fe2O3/graphene/Ag MSCs. (d) Image, (e) CV plots and (f) GCD plots of MSC units linked in parallel and series.

Inclusive of the better electrochemical performance of 3D printed graphene/ Fe2O3/Ag MSCs, the MSC devices’ flexibility is also studied using the bending of MSCs at various angles (see Figure 5. 5a). There is a specification of the bending angle which is demonstrating in the inset of Figure 5. 5(b). The CV plots almost stay unaltered at various bending angles (180°, 90°, 45°, and 0°) as shown in the same Figure 5., showing the promising MSCs mechanical flexibility during the processes of discharge and charge. The MSCs cyclic bending is administered to approve the durability of flex. A significantly 90.2% of high capacitance retention is reported subsequent to 500 bending cycles (see Figure 5. 5c), illustrating that the 3D printed MSCs firmly connected to the PET substrate and at the same time reliable flexibility is shown (Lee et al., 2017). MSC units can be associated with parallel and series to obtain the requirement for higher working current and voltage, respectively. These integrations of MSC are obtained as illustrated in Figure 5. 5(d), where two similar MSCs are clearly associated with silver paste. The delivered voltage of MSC units in a sequence is twice that of a lone MSC, as signified by the GCD plots (Figure 5. 5f) and CV plots (Figure 5. 5e). Same as, if the connection of the MSCs is parallel, then the delivered current is doubled

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approximately. The capability of MSCs to be organized in parallel and series to provide higher operating current and voltage is representing their potential in realistic applications.

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Ambrosi, A., & Pumera, M. (2016). 3D-printing technologies for electrochemical applications. Chemical Society Reviews, 45(10), 2740-2755. An, J., Le, T. S. D., Lim, C. H. J., Tran, V. T., Zhan, Z., Gao, Y., ... & Kim, Y. J. (2018). Single‐step selective laser writing of flexible photodetectors for wearable optoelectronics. Advanced Science, 5(8), 1800496. Beidaghi, M., & Gogotsi, Y. (2014). Capacitive energy storage in micro-scale devices: recent advances in design and fabrication of micro-supercapacitors. Energy & Environmental Science, 7(3), 867884. Bellani, S., Petroni, E., Del Rio Castillo, A. E., Curreli, N., Martín‐ García, B., Oropesa‐Nuñez, R., ... & Bonaccorso, F. (2019). Scalable production of graphene inks via wet‐jet milling exfoliation for screen‐ printed micro‐supercapacitors. Advanced Functional Materials, 29(14), 1807659. Brousse, K., Nguyen, S., Gillet, A., Pinaud, S., Tan, R., Meffre, A., ... & Simon, P. (2018). Laser-scribed Ru organometallic complex for the preparation of RuO2 micro-supercapacitor electrodes on flexible substrate. Electrochimica Acta, 281, 816-821. Gu, S., Lou, Z., Li, L., Chen, Z., Ma, X., & Shen, G. (2016). Fabrication of flexible reduced graphene oxide/Fe 2 O 3 hollow nanospheres based on-chip micro-supercapacitors for integrated photodetecting applications. Nano Research, 9(2), 424-434. Haider, W. A., Tahir, M., He, L., Yang, W., Minhas-khan, A., Owusu, K. A., ... & Mai, L. (2020). Integration of VS2 nanosheets into carbon for high energy density micro-supercapacitor. Journal of Alloys and Compounds, 823, 151769. Hu, H., Pei, Z., & Ye, C. (2015). Recent advances in designing and fabrication of planar micro-supercapacitors for on-chip energy storage. Energy Storage Materials, 1, 82-102. Kim, C., Kang, D. Y., & Moon, J. H. (2018). Full lithographic fabrication of boron-doped 3D porous carbon patterns for high volumetric energy density microsupercapacitors. Nano Energy, 53, 182-188.

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10. Kumar, S., Telpande, S., Manikandan, V., Kumar, P., & Misra, A. (2020). Novel electrode geometry for high performance CF/Fe 2 O 3 based planar solid state micro-electrochemical capacitors. Nanoscale, 12(37), 19438-19449. 11. Kurra, N., Xia, C., Hedhili, M. N., & Alshareef, H. N. (2015). Ternary chalcogenide micro-pseudocapacitors for on-chip energy storage. Chemical Communications, 51(52), 10494-10497. 12. Lee, J. Y., An, J., & Chua, C. K. (2017). Fundamentals and applications of 3D printing for novel materials. Applied materials today, 7, 120-133. 13. Li, H., & Liang, J. (2020). Recent development of printed micro‐ supercapacitors: printable materials, printing technologies, and perspectives. Advanced Materials, 32(3), 1805864. 14. Li, J., Wang, Y., Xu, W., Wang, Y., Zhang, B., Luo, S., ... & Hu, C. (2019). Porous Fe2O3 nanospheres anchored on activated carbon cloth for high-performance symmetric supercapacitors. Nano Energy, 57, 379-387. 15. Li, J., Zhang, G., Fu, C., Deng, L., Sun, R., & Wong, C. P. (2017). Facile preparation of nitrogen/sulfur co-doped and hierarchical porous graphene hydrogel for high-performance electrochemical capacitor. Journal of Power Sources, 345, 146-155. 16. Liu, L., Ye, D., Yu, Y., Liu, L., & Wu, Y. (2017). Carbon-based flexible micro-supercapacitor fabrication via mask-free ambient micro-plasmajet etching. Carbon, 111, 121-127. 17. Liu, Z., Wu, Z. S., Yang, S., Dong, R., Feng, X., & Müllen, K. (2016). Ultraflexible in‐plane micro‐supercapacitors by direct printing of solution‐processable electrochemically exfoliated graphene. Advanced Materials, 28(11), 2217-2222. 18. Lu, Y., Jiang, K., Chen, D., & Shen, G. (2019). Wearable sweat monitoring system with integrated micro-supercapacitors. Nano Energy, 58, 624-632. 19. Owusu, K. A., Qu, L., Li, J., Wang, Z., Zhao, K., Yang, C., ... & Mai, L. (2017). Low-crystalline iron oxide hydroxide nanoparticle anode for high-performance supercapacitors. Nature communications, 8(1), 1-11. 20. Pang, Y., Cao, Y., Chu, Y., Liu, M., Snyder, K., MacKenzie, D., & Cao, C. (2020). Additive manufacturing of batteries. Advanced Functional Materials, 30(1), 1906244.

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21. Serrapede, M., Rafique, A., Fontana, M., Zine, A., Rivolo, P., Bianco, S., ... & Lamberti, A. (2019). Fiber-shaped asymmetric supercapacitor exploiting rGO/Fe2O3 aerogel and electrodeposited MnOx nanosheets on carbon fibers. Carbon, 144, 91-100. 22. Sun, G., An, J., Chua, C. K., Pang, H., Zhang, J., & Chen, P. (2015). Layer-by-layer printing of laminated graphenebased interdigitated microelectrodes for flexible planar microsupercapacitors. Electrochemistry Communications, 51, 33-36. 23. Sun, S., Zhai, T., Liang, C., Savilov, S. V., & Xia, H. (2018). Boosted crystalline/amorphous Fe2O3-δ core/shell heterostructure for flexible solid-state pseudocapacitors in large scale. Nano Energy, 45, 390-397. 24. Tahir, M., He, L., Haider, W. A., Yang, W., Hong, X., Guo, Y., ... & Mai, L. (2019). Co-electrodeposited porous PEDOT–CNT microelectrodes for integrated micro-supercapacitors with high energy density, high rate capability, and long cycling life. Nanoscale, 11(16), 7761-7770. 25. Tan, D. Q. (2020). Review of polymer‐based nanodielectric exploration and film scale‐up for advanced capacitors. Advanced Functional Materials, 30(18), 1808567. 26. Tan, H. W., An, J., Chua, C. K., & Tran, T. (2019). Metallic nanoparticle inks for 3D printing of electronics. Advanced Electronic Materials, 5(5), 1800831. 27. Tian, X., Shi, M., Xu, X., Yan, M., Xu, L., Minhas‐Khan, A., ... & Mai, L. (2015). Arbitrary shape engineerable spiral micropseudocapacitors with ultrahigh energy and power densities. Advanced Materials, 27(45), 7476-7482. 28. Wang, R., Zhao, Q., Zheng, W., Ren, Z., Hu, X., Li, J., ... & Xu, C. (2019). Achieving high energy density in a 4.5 V all nitrogen-doped graphene based lithium-ion capacitor. Journal of Materials Chemistry A, 7(34), 19909-19921. 29. Xue, J., Zhao, Z., Zhang, L., Xue, L., Shen, S., Wen, Y., ... & Zhang, C. (2017). Neutrophil-mediated anticancer drug delivery for suppression of postoperative malignant glioma recurrence. Nature nanotechnology, 12(7), 692-700. 30. Yang, X., Li, Y., Zhang, P., Sun, L., Ren, X., & Mi, H. (2020). Hierarchical hollow carbon spheres: Novel synthesis strategy, pore structure engineering and application for micro-supercapacitor. Carbon, 157, 70-79.

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31. Yin, L., Gao, Y. J., Jeon, I., Yang, H., Kim, J. P., Jeong, S. Y., & Cho, C. R. (2019). Rice-panicle-like γ-Fe2O3@ C nanofibers as highrate anodes for superior lithium-ion batteries. Chemical Engineering Journal, 356, 60-68. 32. Yu, C., An, J., Chen, Q., Zhou, J., Huang, W., Kim, Y. J., & Sun, G. (2020). Recent advances in design of flexible electrodes for miniaturized supercapacitors. Small Methods, 4(6), 1900824. 33. Zhang, C. J., McKeon, L., Kremer, M. P., Park, S. H., Ronan, O., Seral‐ Ascaso, A., ... & Nicolosi, V. (2019). Additive-free MXene inks and direct printing of micro-supercapacitors. Nature communications, 10(1), 1-9. 34. Zhang, G., Shi, Y., Wang, H., Jiang, L., Yu, X., Jing, S., ... & Tsiakaras, P. (2019). A facile route to achieve ultrafine Fe2O3 nanorods anchored on graphene oxide for application in lithium-ion battery. Journal of Power Sources, 416, 118-124. 35. Zhang, H., Cao, Y., Chee, M. O. L., Dong, P., Ye, M., & Shen, J. (2019). Recent advances in micro-supercapacitors. Nanoscale, 11(13), 58075821. 36. Zhang, P., Wang, F., Yu, M., Zhuang, X., & Feng, X. (2018). Twodimensional materials for miniaturized energy storage devices: from individual devices to smart integrated systems. Chemical Society Reviews, 47(19), 7426-7451. 37. Zheng, S., Huang, H., Dong, Y., Wang, S., Zhou, F., Qin, J., ... & Bao, X. (2020). Ionogel-based sodium ion micro-batteries with a 3D Naion diffusion mechanism enable ultrahigh rate capability. Energy & Environmental Science, 13(3), 821-829. 38. Zheng, Y., Ouyang, M., Han, X., Lu, L., & Li, J. (2018). Investigating the error sources of the online state of charge estimation methods for lithium-ion batteries in electric vehicles. Journal of Power Sources, 377, 161-188. 39. Zhou, Z., Zhang, Q., Sun, J., He, B., Guo, J., Li, Q., ... & Yao, Y. (2018). Metal–organic framework derived spindle-like carbon incorporated α-Fe2O3 grown on carbon nanotube fiber as anodes for highperformance wearable asymmetric supercapacitors. ACS nano, 12(9), 9333-9341.

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CHAPTER

6

THREE-DIMENSIONAL PRINTING OF PIEZOELECTRIC MATERIALS

CONTENTS

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6.1 Introduction .................................................................................... 128 6.2 Piezoelectric Materials .................................................................... 128 6.3 Poling ............................................................................................. 132 6.4 Mathematical Representation of the Charge Piezoelectric Constant ...................................................................................... 153 6.5 Summary ......................................................................................... 154 Reference ............................................................................................. 155

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6.1 INTRODUCTION The chapter provides a summary of three-dimensional printing techniques for Piezoelectric matters (PEM) by utilising different methods including coronal poling, interface poling, as well as additional poling processes, The technique of combining poling and three-Dimensional printing allows for the printing of every category of the complicated sized sensor by one step, whereas many traditional methods need complex and time utilizing procedures. However, three-Dimensional printing combined with poling technique and substance limitations, and stages to reduce the engineering hurdles are currently being researched (Tay et al., 2017). We were capable to create personalized components having complicated forms out of metals ceramics, and polymers using an additional production process, also known as three-dimensional printing, having no requirement for moulds or processing, which is required in traditional formative and manufacturing of the material. Building of industries, manufacturing of medicine, foodstuff preparation, aerospace, soft detectors and controller applications have all attracted the interest of individuals all over the world (Liaw & Guvendiren, 2017). The three-dimensional printing of piezoelectric matters is accomplished in many ways, based on the kind of matter like polymers, materials of ceramic, and polymeric materials. When piezoelectric matters are threedimensional printed, poling occurs during the printing process, which is termed in-situ poling, and poling occurs after the piezoelectric matter is three-dimensional printed. Ultrasound transducers, nano-generators, mobile phones, Sensors, the automobile industry, and further common uses are only a few of the uses for piezoelectric matters (Komorowski et al., 2021).

6.2 PIEZOELECTRIC MATERIALS The material of Piezoelectric is non-centrosymmetric insulator substances that produce an electric charge around the lattice once the stress is applied to them, This is known as the effect of straight piezoelectric, and it occurs when +ve & -ve charges are created on contrary sides of the lattice because of the positioning of dipoles of electricity in the crystal that is noticed by Pierri and Jaques in 1880 (Yamada et al., 1982). Whenever an exterior electric current is supplied to a lattice, the irregular separations of anions and actions cause significant net distortion of a lattice; the strain in piezo-electric substances is either substantial or hardness, based upon the polarisation of the supplied field; this concept is called «indirect piezoelectric effect.” The

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indirect piezoelectric effect (Dias & Das, 1996) is expressed by utilizing the concepts of basic thermodynamic, and the formulas for the indirect and direct piezoelectric effects are provided below(Dias & Das, 1996). Indirect piezoelectric effect = X = sT + dE

(1)

Direct piezoelectric effect = D = dT + εE

(2)

In the above equations (1) and (2) the abbreviation is T (stress), X ( Strain), ε ( material permittivity), d(coefficient of piezoelectric), s ( mechanical observance), E ( field of electricity), D (electric displacement). Certain piezoelectric matters, known as pyroelectric matters, have spontaneous type polarisation which diminishes as the temperature increases, the spontaneous type of polarisation of certain pyroelectric matters may be reshaped through adding a field of electricity, and these matters are called ferroelectric matters, consequently, the matters of Ferroelectric have the properties of both piezoelectric and pyroelectric, and such piezoelectric matters come in a variety of shapes and sizes, e.g., amorphous or crystalline appearance, polymer appearance and the combination of both matters are known as polymer- ceramic appearance, these are clarified in the followings (Valentine et al., 2017):

6.2.1 Ceramic Materials Organic or Artificial matters may be used to make the materials piezoelectric. Crystalline substances such as a salt of Rochelle, quartz (SiO2), topaz, crystals of Tourmaline-group, and biological things ( such as wood, dentin, hair, enamel, bone, rubber and silk ) are examples of natural PEM. Artificial piezoelectric matters are crystalline which are polymers & their composites, analogues of quartz, ceramic objects, and several kinds of artificial ceramics having a perovskite crystalline structure such as (Pb(Zrx Ti1−x )O3, 1 > x > 0 ) Lead zirconate titanate is also called PZT, (LiNbO3)Lithium niobate, (PbTiO3)lead titanate, (BaTiO3)Barium titanate, (LiTaO3)Lithium tantalate, Potassium niobate (KNbO3) etc. and further piezoceramics having no lead. ABO3 is a common chemical formula for perovskite crystalline structure, in Which A is a bigger ion of metal, generally lead Pb/barium Ba is utilized, and B is a tiny ion of metal, generally titanium Tier zirconium Zr is utilized (Zhou et al., 2008; Zhou et al., 2011) Ceramics have a wide range of electrical characteristics. Certain materials limit the flow of electricity in the presence of a quite high electric field, and finally making them good insulator material. Other materials

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are used as conductive materials because they enable an electrical current to flow through them. The 3rd type of material, which are beneficial semiconductors, allows electricity to flow only under certain circumstances or when an energy criterion is met. Certain ceramics, on the other hand, don’t carry electric current but experience interior polarisation of charge, allowing them to be used as capacitors to store electric charge. Barium titanate(BT) for capacitors, tin oxide for gas sensors, zinc oxide for varistors, (lead(P), zirconium(Z), titanate(T)) for piezoelectrics, (lead(P) lanthanum(L) zirconium(Z) titanate(T) for electro-optic devices, & also lithium niobate for electro-optic devices are all instances of electro-ceramics (Wang et al., 2007).

6.2.2 Polymer PVDF (Polyvinylidene fluoride) and its composites are the most well-known piezoelectric polymers. Polyvinylidene fluoride has the chemical formula (C2H2F2)n and available in 3 various stages such as α,β, and γ stages. β and γ stages of polyvinylidene fluoride have polarity, but the α stage has no polarity. In the high polarity stage, slight layers of Polyvinylidene fluoride are utilised for piezoelectric uses. The slight layers of polyvinylidene fluoride may be made by a solvent or from a melt (Cholleti, 2018 Curie & Curie, 1880). The procedure utilized for hardening the liquid or the kind of solution utilised determines the stage of the layer created, and the α and β stages are generated when the melt (temp. is greater than 167 degrees Celcius) is cooled to 80 degrees Celcius. If the stage of polyvinylidene fluoride layer is extended to three hundred per cent strain, it changes into a high polarity stage. Due to its limited conduction of heat, limited density, and strong heat and chemical tolerance, the α-stage of the layer of polyvinylidene fluoride is commonly used as an insulation matter (Cid et al., 2020). The technique of solvent cast is utilized to make polyvinylidene fluoride from solvents. Di-methylacetamide or dimethylformamide has employed as solvents. In stretching circumstances, the layers of polyvinylidene fluoride are whipped through providing a strong electric current of the average 20 kiloVolt per mm. The layer of polyvinylidene fluoride has a piezoelectric coefficient between 20 pC/N and 30 pC/N, and that is 10x less than ((Lead(P) zirconate(Z) titanate(T)). Compared to pure Polyvinylidene fluoride, composites of polyvinylidenefluoride containing tetrafluoroethylene, and tetrafluoroethylene have superior piezoelectric characteristics. The composite polymer of polyvinylidene

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fluoride-tetrafluoroethylene has a piezoelectric coefficient and its value is above 100 pC/N. Due to its lower constant of stiffness, such polymer is utilised as presser detectors instead of actuators. The severe operating temp. for the β-stage polyvinylidene fluoride layer is 80 degrees Celcius, while 110 degrees Celcius for the β-phase polyvinylidene fluoride-tetrafluoroethylene layer (Cid et al., 2020). Due to their good impedance similarity with liquid, the polymers are much more suitable for hydrophones production (inside water acoustic sensors) over ((Lead(P) zirconate(Z) titanate(T)). Pressure detectors in the injection lines of diesel and shock wave detectors are two more common uses.

6.2.3 Pottery Polymer Polymer-based composite materials of pottery have been made through mixing the characteristics including minimum 2 matters, based on the uses, they are commonly utilized in a variety of commercial processes, ranging from detectors and actuators to smart devices for such uses, composites with zero to three connectivity, which means that a 3-D associated polymer stage is packed to segregated pottery particles have got attention for such applications, owing to their design flexibility and low cost (Sebastian & Jantunen,, 2012; Cid et al., 2020). Based on the particular blend of piezoelectric characteristics & elasticity of polymer medium, nanocomposites incorporating piezoelectric pottery fillers inside a polymer medium have significant attention. The characteristics of the piezo-polymer compound are enhanced since the characteristics of the component stages interact to boost the compound’s application range and mechanical characteristics (Venkatragavaraj et al., 2001). So the medium of the polymer has low piezoelectric coefficients and dielectric constants than the inserted piezoelectric pottery, the characteristics of the effective dielectric & piezoelectric of 2-stage compounds have no comparison to those of mono phased equivalents. As a result, numerous studies have shown that including electrical conductor materials into the polymer medium improves the polarity of the implanted piezoelectric fillers, therefore improving its characteristics of electricity conduction (Dang et al., 2010). Carbon nanotubes (CNTs) having currently gained popularity as fillers owing to their electric conduction behavior (Dang et al., 2010). The connection among the processing method of compounds, the shape, and characteristics of the electric conduction particulates, particularly

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determines the dielectric & piezoelectric characteristics of composites, is, although, relatively poorly understood. Barium titanate-Polyvinylidene fluoride and Barium titanate–PEGDA are two leading three-dimensional printed pottery-polymer piezoelectric compounds (Kim et al., 2014; Kim et al., 2018).

6.3 POLING Poling would be a process that starts piezoelectrically in ferroelectric pottery by supplying electricity to turn the polar orientation of crystals to the pattern paths closest to the applied electricity (Liaw & Guvendiren, 2017). Poling is the practice of providing an exterior electric field to tiny molecule dipoles to align molecules across the direction of the field. This integrating technique was developed by Kim et al. (2018). Inert pottery would be converted to electromechanically active matters by Poling (Haertling, 1999). Poling is a critical stage in achieving the compound’s specific piezoelectric characteristics. The polymer containing compounds are poled at their glass transition temp. by progressively warming them and exposing them to a high static exterior electric field (McKenna et al., 2007; Dietze & Souni, 2008). The temp. over which polling occurs, as well as the imposed strength of the electric field, are important factors in determining the electro-mechanical characteristics of poling compounds. To arrange the areas in the applied field direction, both temp and imposed electric fields are utilized to reduce the electricity shortage. The procedure of arrangement and the selected actual polling temp are dependent on the interior arrangement of the polymer compounds, for example, whether it is shapeless or semicrystalline. Mechanical extending of the polymer layer among the poling procedure improves the crystal arrangement quality in certain polymers, such as Polyvinylidene fluoride. By expanding the polymer, arranges the unstructured strands in the layer plane and allows for homogeneous crystal rotation via an electric current. Inside the surface of the polymeric material, the mechanical and electrical characteristics (and thus the transmission reaction) either are extremely anisotropy or isotropy, based upon whether extending is biaxial or uniaxial. The porous structure strengthens the crystalline alignment in semicrystalline polymers, and the polarity is steady up to the Curie point

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(TC ). Many phasic compounds have been conventionally poled by utilizing the contacts poling technique. The substance is now in close touch with the poling electrode in such poling process. This method, although, has significant drawbacks, as it might produce dielectric malfunction of the composite matters, particularly whenever the composite contains extra conductivity (McKenna et al., 2007; Dietze & Souni, 2008). Within that procedure, the specimens should also be placed into a silicone oil bath to provide consistent heat. Investigators (Waller & Safari, 1988) made the poling technique of corona release to solve the technique’s difficulties. within such an approach, a strong poling voltage is given to molecules of the air over the specimen, eradicating bodily touch. Investigators have also proven that the corona poling approach may achieve greater voltages than the conventional contact poling technique (McKenna et al., 2007; Huang et al., 2012).

6.3.1 Corona Poling A current from the corona point is showered upon the surface which contains no electrode within the corona poling method, generating an electric current among the specimen surface. Because of no electrodes, there is no leakage of current in the specimen at fragile areas, a greater voltage at poles may be obtained. This approach also allows for the poling of bigger specimens and may be converted to constant procedures for commercial processing. As illustrated in Figure 1, the live wire is linked to the corona release electrode, and the primary plate upon which the specimen is resting is earthed. The corona electrodes tiny point guarantees that neighbouring molecules of air are ionized. A protected shell surrounds the entire poling equipment. This prevents ionised molecules of air from coming into touch with nearby things. The separation between the electrode and the specimen is an important experimental variable, and research has shown that differing lengths may have a substantial impact on the polling method (Waller & Safari, 1988). To make sure experiment reproducibility and remove experiment variation, the remoteness of corona electrode from the specimen remained constant at ten millimetres for such tests.

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Figure 6.1. Corona release method, the live wire ionizes the nearby molecules of air over the specimen surface having no needle. There is no bodily touch between the corona electrode and the specimen surface. Source: https://www.researchgate.net/figure/Corona-discharge-technique-thelive-wire-ionizes-the-surrounding-air-molecules-onto-the_fig1_329791287/ amp

6.3.1.1 Additive Manufacturing with the help of Electric Poling (EPAM) Additive Manufacturing with the help of electric Poling (EPAM) is a poling while printing approach that uses the corona poling technique to integrate Additive Manufacturing (AM) and electric poling procedures to create unrestricted shape piezoelectric appliances constantly (Yen et al., 2013; Lee & Tarbutton, 2015). The dipoles of Polyvinylidene fluoride polymer stay homogeneous and perfectly arranged upon a broad area in this technique, which involves only one layout, manufacture, and production process. The liquid Polyvinylidene fluoride polymer is mechanically strained & electrically poled inside the suit via the front tip in the EPAM (Additive Manufacturing with the help of electric Poling ) process under the circumstances of high electric current and greater temp. The system of EPAM manufactures piezoelectric appliances by directly printing piezoelectric objects from Polyvinylidene fluoride polymeric thread using a strong electric current among the printing bed & the nozzle tip in an AM machine.

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Polyvinylidene fluoride polymer appliances of one hundred millimetres mm in length are printing is done using 4 different electric field conditions such as 3.0 MV/m,2.0 MV/m, 1MV/m, and 0.0MV/m. The printing margin b/w the surface area of the printing and point of the nozzle is 0.3 millimetres. While poling, there has burned in the primary film of the printing, as well as an electrical failure happened at 3 MV/m electric fields. The job of sustaining the electric field stayed difficult, limiting the operational limitations of the below configuration to 3.0 MV/m as shown in Figure 2. (e). Sharper spikes at the poles β-crystal wavelength of Polyvinylidene fluoride polymer are caused by a strong electric field. The findings demonstrate that supplying a high electric current during printing similarly transforms the α phasing to the β phasing of Polyvinylidene fluoride polymer owing to the synchronization of molecular chain and synchronisation of dipole (Lee et al., 2014; Lee & Tarbutton, 2015).

Figure 6.2. Piezoelectric Polyvinylidene fluoride printing arrangements. Source: pdf

https://iopscience.iop.org/article/10.1088/1757-899X/455/1/012046/

Notice following:

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(a) An experimental model that blends the procedure of electric poling and the procedure of additive production, (b) The mathematical model of the EPAM technique, (c) Extraction outcome of strand category of Polyvinylidene fluoride polymer. The Polyvinylidene fluoride polymer is fed inside the extruder at 230 degrees Celcius and is managed via an extraction motor,

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(d) In the technique of electric poling-assisted additive manufacturing, testing findings of mechanical extension and electrical poling, (e) f) A smouldering area (f) Corona ejection damage to the plane of printing, (Lee et al., 2014; Lee & Tarbutton, 2015).

6.3.1.2 Incorporated three-dimensional printing and poling of Corona (IPC) Incorporated three-dimensional Printing & Poling of Corona (IPC) is a poling while printing procedure, also known as in-situ poling among the threedimensional printing method that combines three-dimensional printing and poling of the corona to enable the production of piezoelectric Polyvinylidene fluoride detectors with no need a final procedure of poling (Teske et al., 2002). In such a method, poling is done in a controlled warming atmosphere with a strong electric field applied to the jet-like anode and the warming surface like a cathode. A set gap between the jet point and the upper surface specimen allows the nozzle to follow the specified route. The dipole moment alignment of Polyvinylidene fluoride molecular chains is advanced by the concurrent electric field among the bottom heating pad and jet. Incorporated three-dimensional Printing & Poling of Corona is an improved EPAM technique by applying a stronger electric field among three-dimensional prints. Greater More than 2 MV/m electric fields was discovered to induce electric failure, resulting in a temporary electromagnetic disruption that might induce the loose connection of the printer with the computer (Kim et al., 2017). An additional drawback of the Additive Manufacturing with the help of the electric Poling approach was restricted that it could only make a single film of a piezoelectric appliance. As a result, the Additive Manufacturing with the help of the electric Poling technique was improved to allow for a stronger electric field (40 MV/m) use and the printing of several films, as illustrated in Figure 3.

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Figure 6.3. Graphic of IPC procedure model: (a) three-dimensional printing of Polyvinylidene fluoride film, (b) Corona poling procedure(51). Source: https://iopscience.iop.org/article/10.1088/1361-665X/aa738e/meta

The 0.9 millimetres distance b/w the bed surface and the jet are secured to prevent the jet from contacting the specimen and preventing the printing of the primary film blockage, as well as to provide an adequate gap for supplying elevated electric power. The printing temperature ranges from 230-260 degrees Celcius, and the speed of the printing is below 10 mm/s, along with the constraints of at least 1 mm/s through the software of a threedimensional printer (Richards & Odegard, 2010). The highest operating electric voltage is 12 kV that does not obstruct the printing procedure. Due to the safety procedures involved in running high voltage uses, the user running the three-dimensional printer throughout the incorporated 3D Printing & Poling of Corona procedure is advised to keep a security gap. In the Incorporated 3D Printing & Poling of Corona approach, this was discovered that raising the heating temperature of the surface minimizes the piezoelectricity of the Polyvinylidene fluoride layer (Teske et al., 2002) and that by supplying 12 kV electric power, piezoelectric resultant current of about 0.106 nA may be produced.

6.3.2 Contact Poling That’s the traditional poling method, where a high DC power is used to pole the piezoelectric pottery and compounds. Such poling technique needs bodily touch b/w the specimen electrode & the active electrode, as well as by using a high electric field the specimen would be poled. Although, the use of high Dc power to the polymer medium compounds, frequently

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causes the dielectric malfunction of the specimen. As illustrated in Figure 4, the specimens are put in the oil bath of silicone and even warmed up to their glass transition temp. For such an approach, the specimens must be covered with the upper electrode in contrast to a lower electrode, and poling is generally confined to smaller samples (Waller & Safari, 1988). The benefit of such poling arrangement is based on the poling field’s uniformity and total control. The poling of the electrode is less complicated than the poling of the corona. There are several laboratory settings for contact poling, including contact poling at ambient conditions, contact poling through a temp cycle (heated poling), and Bauer’s cyclic poling technique (Lim et al., 2012; Zhang et al., 2012). We may select one or more depending on our requirements. Localized failure in feeble areas, like prohibits more poling, circuit leakage of the electrodes, and perforations are the main disadvantages of such technique, in contrast to the dielectric failure. That’s why the polling procedure is carried out in a sealed container or while submerged in a liquid that acts as an electrical insulator (Wang et al., 2014; Tabatabaei & Mehdipour, 2015). Furthermore, charge inoculation procedures close to pointed electrode tips or interior gaps might limit it, thus a safe map of electrode structure is required. The corona ejection technique was intended to enhance this type of poling (Waller & Safari, 1988).

Figure 6.4. Contact poling configures the electrical arrangement of the specimen. The upper electrode of the specimen seems to be in connection with the electrode of poling. The base plate (on which the specimen is rested) is grounded. Source: https://www.semanticscholar.org/paper/A-Review-on-3D-printingof-piezoelectric-materials-Cholleti/4c1c12fcf119b30cdbd3453f3353a8b75df1 3c13

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6.3.3 Three-Dimensional Optical Printing of Piezoelectric Nanoparticle Three-dimensional Optic Printing of Piezoelectric nano-particles (Kim et al., 2014) is a printing technology that employs a final procedure of contact poling, that’s the poling following printing process, In such methods, the polymer compounds matters are optically printed into the 3-D nanostructures by utilizing digital projected printing, in such procedures, Piezoelectric polymers are made through combining barium titanate nanoparticles along with photo-labile polymeric solvents like polyethene glycol diacrylate and subjecting them to digital optical filters that might be continuously changed to create user-defined three-dimensional nano-structures. The barium titanate nanoparticles are treated with acrylate surface functional groups, whereby established straight covalent bonds with the polymer medium under direct sunlight, increasing the mechanical to electrical alteration effectiveness of the compounds. Through ten per cent mass loading of chemically processed Barium titanate microparticles, the 40 pC/N value of piezoelectric coefficients (d33) is observed, which is above 10x than compounds synthesised through unprocessed barium titanate microparticles more than two times greater than compounds having unprocessed barium titanate microparticles and carbon microtubes to enhance mechanical force transport efficiency gains. Such findings assist in to manufacture of effective three-dimensional piezoelectric polymers via micro surface modification (Waller & Safari, 1988).

Figure 6.5. Printing using Digital Projection. Source: https://pubmed.ncbi.nlm.nih.gov/25046646/

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Notice following: • Figure(a) shows the digital projection printing system, which displays vital digital filters upon the photo-labile piezoelectric microparticle polymer matrix liquid, which is depicted in the diagram. Any design may be digitilized, and the images are projected into the polymeric solvent using the digital mirror appliance. • Figure (b) Scanning electron micrograph of Barium titanate nanoparticles produced by a hydrothermal method. • Figure(c) the piezoelectric polymer compound matters with Barium titanate nanoparticles (orange circles in the figure) bonded on a PEGDA substrate are depicted in this cartoon (black lines in the figure). The TMSPM linkage is covalently attached to the nanoparticle facet and cross-linked with the PEGDA substrate in this zoomed-in view.

Figure 6.6. The patchwork of piezoelectric microstructures printed utilizing Digital Printing Projection. Source: https://pubmed.ncbi.nlm.nih.gov/25046646/

Notice following:

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• Figure (a) shows an array of the dot, • Figure (b, c) shows arrays of a square having various sized void gaps, • Figure (d) shows an array of honeycombs. All formations were made up in less than two seconds by utilizing a PEGDA solvent laden having one per cent of the TMSPM-customized Barium titanate nanoparticles, • Figure (e) shows an array of mushroom-like, • Figure (f) shows an array of the cross,

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• Figure (g) shows an array of tapered cantilevers (cantilever; dark area, light area, hold up), • Figure (h) shows the Microtubule structure formed through discharging an array of honeycomb from the substance. The layer folds up after discharge because of small pressure inclines in the layer (19). The printing cell may be utilised to ignite the polymer upon photo producing the compound matters. It demands employing a poling field that is greater than the coercive field (equivalent to ten V/m) of the Barium titanate nanoparticles to arrange the dipoles in the perovskite crystal lattice. The upper and lower electrodes that also functioned as the upper and lower surfaces of the photo manufacturing cell were made of indium tin oxide (ITO)-coated crystal plates. The most height of the photogenerated frameworks may be set by using an elastomeric spacer (such as Copper foil layer) during the conductive glass substance, and specific electric fields might be used to polarise the Barium titanate nanoparticles. The produced layers may be kept on the glass plates for evaluation and classification, discarded to construct independent devices, or transported to certain other materials for more incorporation after the piezoelectric compound has been activated (Kim et al., 2014).

6.3.4 Single-Step Solution Evaporation three-dimensional printing of Supported Piezoelectric Polyvinylidene Fluoride Nanoparticles The poling earlier than printing technique is single-step Solution evaporationsupported three-dimensional Printing of Piezoelectric Polyvinylidene fluoride nanoparticles designs, but there is no poling concerned in this procedure because the intrinsic piezoelectric β-phase of Polyvinylidene fluoride is utilized, that is often poled, so such method is regarded poling earlier than printing (Bodkhe et al., 2017). By using solution evaporationsupported three-dimensional printing at ambient temperature, β-phase Polyvinylidene fluoride and BTO are utilised to construct self-supporting piezoelectric devices on micro to millimetres scale. The nanoparticle is dissolved in an extremely volatile solution and then extruded via a tiny jet under given pressure in this method (Guo et al., 2013; Guo et al., 2014). Because the solution evaporates quickly, the required forms are retained: film-by-film, self-assisting, and even independent designs . A prepared millimetre size three-dimensional touch detector created in one printing phase is an example of such work’s applicability.

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Figure 6.7. Solution evaporation dependent three-dimensional printing. Source: https://pubs.acs.org/doi/abs/10.1021/acsami.7b04095

Notice following: • (Figure (a) shows that polyvinylidene fluoride nanoparticle-depended three-dimensional designs are printed using a solution evaporation-supported three-dimensional printing method. • Figure (b) elaborates that during a finger-tap test, a snapshot of the three-dimensional cylindrical detector was taken. • Figure (c) shows that the piezoelectric power yield of a three-dimensional cylindrical detector after 5 successive taps of the finger. • Figure (d) shows that filler addition increases the β-phase percentage in polyvinylidene fluoride, as shown in a diagram of the suggested technique (Bodkhe et al., 2017). Ball-milling dynamically stimulates the BaTiO3 NPs (BT) in Picture 7, which supplies polyvinylidene fluoride chains with attachment locations. Expansion through the injector causes the polymer chains to consolidate into an ordered β-phase. When the NP precipitates solidify, the polyvinylidene fluoride chains are arrested in the β-phase, resulting in enhanced piezoelectric characteristics. The effectiveness of the manufacturing process is demonstrated by a three-dimensional touch detector that produces about four volts from mild taps of a finger. The single-step three-dimensional printing of piezoelectric nanoparticles allows for the creation of fully prepared, complicated, light and

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elastic piezoelectric appliances. They might be used as settled or implanted sensors in aviation, biomedical, and robotics uses when coupled with certain other three-dimensional printed matters (Guo et al., 2014).

6.3.5 Piezoelectric Photocurable for Three-dimensional Printing Adhesive Depended Entirely on Polymers Piezoelectric photocurable for three-dimensional printing adhesive depended entirely on polymers (Chen et al., 2017) is the poling later than printing technique, such method resulted in the development of V-Ink, a polymerdepended piezoelectric photocurable adhesive (V-Ink) that may be used in additive manufacturing methods that use light-managed polymerization methods. The improved V-Ink comprises 35 weight per cent of polyvinylidene fluoride composites embedded in the photocurable adhesive, keeping into mind the barter among ability of manufacturing and piezoelectric properties. This method produces a thick piezoelectrically activated three-dimensional printed material through a piezoelectric power coefficient (g33) of 105.12 × 10 to 3 Vm/N. Such fresh stuff would open up new possibilities for additive manufacture of elastic functional appliances, particularly for monitoring and biosensors uses (Jiang et al., 2017).

Figure 6.8. (a) Diagramatic demonstration of the PμSL system & the threedimensional printing procedure flow is depicted from figure (b) to figure (g)( Chen et al., 2017). Source: https://www.researchgate.net/publication/318604324_The_Development_of_an_All-polymer-based_Piezoelectric_Photocurable_Resin_for_Additive_Manufacturing

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Figure 6.9. Three-dimensional printing of piezoelectric detectors. Source: https://www.researchgate.net/publication/318604324_The_Development_of_an_All-polymer-based_Piezoelectric_Photocurable_Resin_for_Additive_Manufacturing

Notice following: • Figure (a) shows that a piezoelectric detector with a three-dimensional printed polyvinylidene fluoride film, • Figure (a) shows that a diagrammatic depiction of the polyvinylidene fluoride feeble layer poling system having Al electrodes, • Figure (a) shows that when the polyvinylidene fluoride feeble layer having electrodes is exposed to transmitted stress, a diagrammatic example of the system monitoring the power output is shown (Chen et al., 2017). During the 1st stage, the V-Ink is manufactured for three-dimensional printed piezoelectric appliances; the polyvinylidene fluoride composites must be evenly distributed inside the V-Ink among the manufacturing technique, during the 2nd stage, a lengthy wait time is required for associated with elevated viscosity adhesive among the recoating step. As a result, the adhesive viscosity must be adjusted to manage the rest period while maintaining manufacturing output. During the 3rd stage, the piezoelectric improves the efficiency of V-Ink. The piezoelectric properties of the adhesive, which are reliant on the content of polyvinylidene fluoride and a poling electric current, are assessed in the laboratory based on the manufacturing capability of V-Ink (Chen et al., 2017). Quantitative techniques would be used in the coming years to optimise the concentration of various constituents of V-Ink, such as dimethyl fumarate (DEF) as a solution, polyvinylidene fluoride & 1,6-hexanediol diacrylate

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monomer (HDDA), in addition to enhancing the ability of manufacturing, piezoelectric properties, and mechanical characteristics. Further research would be conducted to improve the manufacturing ability of V-Ink and piezoelectric efficiency. Heat Treatment, for instance, may be used in threedimensional printing procedures since heat treatment reduces the efficient viscosity of the V-Ink (Richards & Odegard, 2010), allowing for the printing of V-Ink with a higher concentration of polyvinylidene fluoride. Furthermore, since the manufacturing velocity is significantly quicker than PμSL, the addition of a non-stop solution interface manufacturing setup provides for greater elasticity because the polyvinylidene fluoride may be thoroughly disseminated throughout the manufacturing procedure (Hennig et al., 1982). Furthermore, the mechanical characteristics of the printed gadgets would be classified and improved for use in elastic operational appliances, particularly bending & tension properties. This job is a first step toward developing an efficient all-polymer oriented piezoelectric photocurable adhesive for three-dimensional printing methods, and it introduces new possibilities for operational appliances, particularly biomedical detecting appliances, to be manufactured quickly and cheaply by utilizing emerging three-dimensional printing methods.

6.3.6 Three-dimensional Printing of Piezo Nanoparticles and Thermal Poling Throughout this approach, polyvinylidene fluoride or a Barium titanate particle is three-dimensional printed accompanied via thermal poling (Kim et al., 2018), which falls under the poling technique following the printing technique. Throughout this procedure, 9 wt. per cent Barium titanate or polyvinylidene fluoride layers had been produced via solvent-casting, and the film was sliced into numerous 5 centimetres squares pieces. At a temp of 200 degrees Celcius, the sliced specimens were supplied to a filaments extrusion (known as Filabot). The produced polyvinylidene fluoride or Barium titanate nanoparticles strand was then loaded into an FDM threedimensional printer, commonly referred to as an extrusion dependent technique, that dumps matters in the state of a consistent flowing film by the film to construct a three-dimensional design (Ackerman et al., 1988). At a tip temp of 250 degrees Celcius, the speed of printing was adjusted at 5 millimetres per second, and the thermal bed temp. was adjusted at 80 degrees Celcius, an FDM three-dimensional printing equipment (LulzbotTaz 5) was utilized to manufacture feeble layers of 0.33 millimetres thickness having dimensions of 11.5x37 millimetres. It’s crucial to keep in mind that printing

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at elevated temperatures might cause Barium titanate to flare and jam the jet. Reducing the quantity of duration the filament stays inside the heated jet solves this problem.

Figure 6.10. Schematic representation of (a) Experimental system for piezoelectric resultant current calculation & (b) specimen and electrode structure (18). Source: https://journals.sagepub.com/doi/full/10.1177/0021998317704709

Upon manufacturing the 2 layers using a casting of solution and threedimensional printing techniques, the specimens were ready to use for a thermal poling procedure, which has been shown to convert PVDF into the β-phase(Jiang et al., 2007). A diagram of the system is given in Figure 11(b) which shows that Copper painted electrodes were connected to specimens, linked to a high power supply, and subjected to a strong electric field of 35 MV/m, which was determined to be the highest electric field before undergoing an electric failure. Polyvinylidene fluoride, for example, needs about 50 MV/m to be polarised because of a large restrictive electric current, whereas Barium titanate only needs around 35 KV/m (Nagata & Kiyota, 1989). Upon immersing specimens in oil of silicon at 90 degrees Celcius, the electric failure was prevented, as well as it supports the acceleration of polarisation throughout the procedure. Both three-dimensional printed and solution-casted layers were thermally poled for 2 hours (Kim et al., 2018). According to the uniform dispersion and improvement of agglomeration for Barium titanate composites, and also the removal of densities and fractures caused by the extrusion of filament and three-dimensional printing method, the piezoelectric outputs in the three-dimensional printed layer exhibit greater output current over solution-casted layer. The three-dimensional printing method not just to enhances piezoelectric characteristics, and allows

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for the manufacturing of various forms of activated nanoparticles (Kim et al., 2018).

6.3.7 Three-dimensional Printing of Piezoelectric Element for Energy Concentrating and Ultrasonic Detection Three-dimensional printing of a piezoelectric material for energy focussing and acoustic detection is a poling after three-dimensional printing approach, in which a piezoelectric elements slurry containing BaTiO3 nanoparticles (100 nanometres) may be three-dimensional printed utilizing Mask-ImageProjection-based Stereolithography (MIP-SL) technique (Chen et al., 2016). The density of 5.64 grams per centimetres cube was achieved after a final procedure, which is 93.7 per cent of the density of material Barium titanate (6.02 grammes per centimetres cube). The relative permittivity and the constant of piezoelectric of the printed pottery are 1350 and 160 pC/N, correspondingly. To accomplish energy concentrating & acoustic detection, an acoustic transducer having a printed concentrated piezoelectric material was constructed. The transducer effectively visualised the anatomy of the pig eyeball with a 6.28MHz ultrasonic scan.

Figure 6.11. Three-dimensional printing utilizing Mask-Image-Projectionbased Stereolithography (MIP-SL). Source: https://www.infona.pl/resource/bwmeta1.element.elsevier-0748991fe4c8-37fc-bbaf-668f036fda80

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Notice following : • Figure (a) shows the demonstration of the Mask-Image-Projectionbased Stereolithography setup. • Figure (b) shows the Image pattern managed through the projection. • Figure (c) shows the three-dimensional geometry structured via Solid job. • Figure (d) shows the Interface to control the projector and motor. • Figure (e) shows the Optical picturing of Green-part made-up through the Mask-Image-Projection-based Stereolithography setup. • Figure (f) shows the 6.28 megahertz ultrasonic inspection by pig eyeball utilizing the printing concentrated transducer. • Figure (g) shows the Ultrasonic picturing of a pig eyeball.( Chen et al., 2016) The Mask-Image-Projection-based Stereolithography setup was used to generate a series of tubular piezoelectric specimens (width is 10 millimetres, thickness is 390 millimetres) utilizing a poling field of 30 kilovolts per centimetre at 100 degrees Celcius for 30 minutes. The loss of dielectric ( noted as tanδ) for standard Barium titanate is generally below 0.1, and the residual polarization (noted as Pr) is greater than 2μC/cm2. The less loss of dielectric of the printed pottery (tan= 0.018) shows that such specimen has a less loss of energy when used in a piezoelectric appliance. The piezoelectric characteristics of the printed piezoelectric elements may be utilized in biological imaging as well as additional uses (Chen et al., 2016).

6.3.8 3D Printing of PVDF with Near-field Electrospinning (NFES) The poling during printing technique is three-dimensional printing of polyvinylidene fluoride having NFES (Near-field electrospinning), in which wavy-substrate self-powered sensors (WSS) are created in an insitu & direct-write poling way via three-dimensional printed structurally customised material (Fuh et al., 2017). Additive manufacturing of a threedimensional printed elastic and cyclical curvy substance, coating, and Nearfield electrospinning filaments in a three-dimensional architect are among the production stages. Such three-dimensional design may significantly boost piezoelectric production and may be used to make self-powered detectors for detecting the pressure of the foot, human motion tracking, and finger-induced voltage production. The proposed technique improves on established electrospinning innovations, which are a conventional

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technique for synthesising three-dimensional designs and other dependable devices for biomedicine and electronics wearing devices by electrically driving the polymer nozzles and manufacturing nanomaterials from the Taylor cones of already blended solvent. Substances with diameters ranging from micrometres to nanometers, like plastics, polymeric compounds, and pottery. The conventional electrospinning process has inherent limitations in terms of anatomically and geometrically managed (DeWitt & Incropera, 1988).

Figure 6.12. Near-field electrospinning method. Source: https://pubmed.ncbi.nlm.nih.gov/28754916/

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Notice following: a) On the upper side of the curvy material, near-field electrospinning was used to create direct-write polyvinylidene fluoride filaments. b) Mechanical attachment of a curvy material to a conducting electrode made of copper foil. c) Polyvinylidene fluoride filaments are electrospun on the upper edge of a Cu-resin curvy substance using Near-field electrospinning. d) Completely enclosed by PDMS . Scale block is 200micrometres (Fuh et al., 2017).

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Figure 6.13. The three-dimensional printed automatic foot pressure detector. Source: https://pubmed.ncbi.nlm.nih.gov/28754916/

Note: (a) The illustration of self-powered sensors incorporated an automatic foot pressure detector arrangement (3×3; 4.5 cm×3 cm of measurement for every single cell) for sensing the pressure of the foot. (b) and (c) shows a 2-D shape design of pressure perspective from the subject of (b) standard foot, (c)smooth foot. (d) In a tiptoe pose and the related 2-D shape design of pressure potential (Fuh et al., 2017). Figure 13 presents the four steps of fabrication of piezoelectric generator with fibres of wavy and threedimensional (3D) topology. In the first step Cu foil is mechanically stuck to the thermoplastic elastomer (TPE) substrate with a 3D printed wavy surface (Figure. 13a, TPE substrate thickness is around 2 mm). Figure 13 b shows a tightly attached curvy substance with polyvinylidene fluoride piezoelectric filaments constantly formed on the copper foil electrode using an in-situ poled Near-field electrospinning method (Figure 13c, Near-field electrospinning processing system): The electrospinning procedure variables under such circumstance were 16 wt per cent polyvinylidene fluoride, solution (Dimethylformamide: acetone having a one to one weight ratio), and 4 wt per cent fluoro-surfactant (Capstone FS- 66 Near-field electrospinning has the capacity to implant a quite fine

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design of filaments onto the substance with remarkable precision. PDMS is then utilised to segregate and enclose the atmospheric disruption in the last stage (Fuh et al., 2017). This method is unique in that it presents geometrically three-dimensional curvy formations with enhanced electrical and piezoelectric characteristics. The piezoelectric production of the abovementioned three-dimensional design can be increased, and the reason for this could be due to the longer filament length electrospun through the Near-field electrospinning method. Following that, the wearing device and smart button programs benefit from the location accessible ability of piezoelectrically incorporated three-dimensional architecture, allowing the button-hitting action to be operationally identifiable towards any particular remotely controlled characteristics in an automatic mode. The approach described above has the potential to improve current electrospinning techniques for threedimensional composition for portable devices and medicinal uses (Fuh et al., 2017). Table 6.1. Review of three-dimensional Printing Techniques Three-dimensional Printing method

Material characteristics & Operating circumstances

Material effectively printed

Poling technique

Incorporated three-dimensional Printing

The temperature of Nozzle is 230℃

Polyvinylidene fluoride polymer thread-like structures

poling of Corona

Additive Manufacturing with the help of Electric Poling (EPAM), (2014) (Lee et al., 2014).

Extruder Temperature is 230degrees Celcius, Bed Temperature is 100 degrees Celcius, Extruder feed is 200 (mm/min) Electric field is 0.0 MV/m, 1.0 MV/m, 2.0 MV/m or 3.0 (MV/m)

Polyvinylidene fluoride polymer thread like structures (diameter is about 3.0 millimetres)

poling of Corona during printing technique

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Three-dimensional Optical Printing of Piezoelectric Nano-particle, (2014) (Kim et al., 2014).

Electric field strength is 12MV/m & Operating temperature -120℃

Barium titanate, nanoparticles incorporated in polyethene glycol diacrylate photolabile polymer.

Contact poling after printing technique

Incorporated three-dimensional Printing & Corona poling (IPC), (2017 )(Kim et al., 2017).

Bed Temperature 23,60,100 or 140 degrees Celcius & functional Voltage is 3kV ,6 kV ,9 kV or 12 kV

(diameter is about 2.7 millimetres)

Contact poling during printing technique

All-Polymeric-dependent piezoelectric photocurable resin for three-dimensional Printing (2017 )( Chen et al., 2017).

Ultraviolet light is 405nm & The electric field is 1.33 MV/m

Piezoelectric photocurable resin consisting of 35wt per cent of Polyvinylidene fluoride

Contact poling after printing technique

Piezoelectric constituent Three-dimensional Printing for energy focusing and ultrasonic sensing (2016) (Chen et al., 2017).

Electric field 10 kV/ cm, 20 kV/cm or 30 kV/cm Operating temp. is 122 degrees Celcius

BaTiO3 nanoparticles blended with Triton x-100 dispersant.

Contact poling after printing technique

Single-step Solution evaporation-supported three-dimensional Printing of Piezoelectric Polyvinylidene fluoride Nano polymers (2017 )( Bodkhe et al., 2017).

The diameter of Nozzle 100 μm Speed is 0.5 mm/s The time of Printing is 120 seconds

intrinsic piezoelectric β- phase Polyvinylidene fluoride and BaTiO3 blended in a volatile solution.

Poling before printing technique

three-dimensional Printing of Polyvinylidene fluoride with Near-field electrospinning(NFES),(2017) (Fuh et al., 2017).

Output power is 1V.1.5V or 2V & Output current is 50nA, 80nA or 110nA

Encapsulation of Polyvinylidene fluoride fibres on the peak with PDMS and base with Cu- adhesive curly substance.

Poling during printing technique

three-dimensional of Piezoelectric nano compounds and Thermal poling (2017) (Kim et al., 2017).

Extruder Temperature is 220 degrees Celcius Bed Temperature is 80 degrees Celcius The electric field is 35MV/m

9wt. per cent Barium titanate or Polyvinylidene fluoride filament (diameter is 2.7 millimetres)

Thermal poling after printing technique

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6.4 MATHEMATICAL REPRESENTATION OF THE CHARGE PIEZOELECTRIC CONSTANT The piezoelectric nanoparticles allow for the fabrication of elastic responsive Microelectromechanical systems (MEMS) for a variety of commercial uses. The piezoelectric characteristics of polymer–ceramic compounds are anticipated as follows by the Furukawa and Yamada representations:

6.4.1 Furukawa Model Furukawa investigated a 2-stage system consisting of cylindrical inclusions (such as pottery filler) fixed in a polymer medium, which is then enveloped by a homogenous matrix having characteristics that are similar to those of the ordinary compound. For the piezoelectric & dielectric coefficients of zero to three composites, Furukawa proposed the following formulae (Domínguez et al., 2019).

Where the volume per cent of pottery filler, d33 and g33 are piezoelectric charge constants and piezoelectric voltage constants and is the dielectric constant is noted by f and m referring to the pottery and polymer phases, correspondingly. The primary disadvantage of the Furukawa concept is that it ignores connections among component stages when generating equations as it assumes the compound is electrically homogenous. However, due to impacts of space charge (such as the Maxwell-Wagner impact), this can not be valid in the context of a 2-phase compound setup (Venkatragavaraj et al., 2001).

6.4.2 Yamada Model Yamada investigated both systems of PZT particles dust combined with polyvinylidene fluoride polymer and presented a framework to describe the manner of the compound’s characteristics depending on the characteristics of its component matters. The model is made up of ellipsoidal constituents distributed in a consistent polymer matrix, with the compound’s permittivity

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constant (εc) and piezoelectric charge constant (d33,c) calculated as following(Yamada et al., 1982; Dias & Das, 1996).

where is the shape factor (dependent on the topology of the filler constituents and their alignment for the compound’s surface), is the ceramic poling proportion, is the filler particle’s volume fraction, and ε is the coefficient of dielectric, with the subscripts m, c and f correlating to the compound, ceramic filler, and polymer medium characteristics.

6.5 SUMMARY The 1st technique is poling before printing, the 2nd technique is poling during printing, also defined as in-situ poling, and the 3rd technique is poling later than printing. The majority of such 3 techniques utilise contact poling or corona poling as its matter and structure technique to pole the material, Ceramic polymer nanocomposite’s three-dimensional printing gives elasticity owing to the polymer component and greater piezoelectric characteristics owing to the piezoelectric very small particles of ceramic, The piezoelectric charge constant (d33) is used to measure this piezoelectric characteristic and the Furukawa and Yamada approach compute this, with the Yamada model providing better highly supportive finding owing to the inclusion of the interplay of the ceramic constituents and polymer through utilising the variable (n), which connects the form and relative or alignment of the filler) (Venkatragavaraj et al., 2001).

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69. Yamada, T., Ueda, T., & Kitayama, T. (1982). Piezoelectricity of a high‐content lead zirconate titanate/polymer composite. Journal of Applied Physics, 53(6), 4328-4332 70. Yen, H. J., Chen, C. J., & Liou, G. S. (2013). Flexible multi‐colored electrochromic and volatile polymer memory devices derived from starburst triarylamine‐based electroactive polyimide. Advanced Functional Materials, 23(42), 5307-5316. 71. Yen, H. J., Wu, J. H., Wang, W. C., & Liou, G. S. (2013). High‐Efficiency Photoluminescence Wholly Aromatic Triarylamine‐Based Polyimide Nanofiber with Aggregation‐Induced Emission Enhancement. Advanced Optical Materials, 1(9), 668-676. 72. Zhang, K., Niu, H., Wang, C., Bai, X., Lian, Y., & Wang, W. (2012). Novel aromatic polyimides with pendent triphenylamine units: synthesis, photophysical, electrochromic properties. Journal of Electroanalytical Chemistry, 682, 101-109. 73. Zhang, S., Li, F., Jiang, X., Kim, J., Luo, J., & Geng, X. (2015). Advantages and challenges of relaxor-PbTiO3 ferroelectric crystals for electroacoustic transducers–A review. Progress in materials science, 68, 1-66. 74. Zhou, J., Gu, Y., Fei, P., Mai, W., Gao, Y., Yang, R., ... & Wang, Z. L. (2008). Flexible piezotronic strain sensor. Nano letters, 8(9), 30353040. 75. Zhou, Q., Lau, S., Wu, D., & Shung, K. K. (2011). Piezoelectric films for high frequency ultrasonic transducers in biomedical applications. Progress in materials science, 56(2), 139-174.

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CHAPTER

7

3-D PRINTING OF RECHARGABLE ED BATTERIES

CONTENTS

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7.1 Introduction ..................................................................................... 164 7.2 Three-Dimensional Printing Technology ........................................... 165 7.3 Battery Materials .............................................................................. 169 7.4 Li-Based 3D-Printed Materials For Rebs ........................................... 173 7.5 Mtal-Based 3D Printed Materials For Rebs ....................................... 184 7.6 Application of Three-Dimensional Printing Battery ........................... 187 7.7 Package Approaches of Three-Dimensional Printed Rebs ................. 191 7.8 Benefits of Three-Dimensional Print Battery ..................................... 193 7.9 Disadvantages of Three-Dimensional Print Battery ........................... 194 References ............................................................................................. 195

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7.1 INTRODUCTION An essential component of electric operating setups is the storage of energy and there is a rising demand for extremely high-powered batteries these days. Attempts are made throughout the years to investigate cell topologies, novel electrode matters, electrolytes, minimize production costs, new manufacturing methods to enhance the electrochemical efficiency of batteries, and extend its usage. The formation of various types of complicated designs via three-dimensional printing is extensively documented in the nineteenth century (Das et al., 2016; Dertinger et al., 2020). Such additive manufacturing represents a significant advancement in the realm of battery tech manufacturing. Three-dimensional printing has been used by scientists from Carnegie Mellon University (CMU) and Missouri University of Science and Technology to create elevated capability batteries of lithiumion (Farrell & Wood, 2018). Health-care equipment, robotics, electric automobiles, Cellphones, remote detectors & computers can be powered and operated. The inventors of batteries of lithium-ion were given the Nobel Prize in Chemistry early this year (6). Matters experts, on the other hand, are in serious requirement of improved batteries for the Internet appliance, the next era of smart gadgets, and other applications (Chang et al., 2018). For the stowing of energy from reuseable, variable sources such as wind and solar, strong batteries are required. Material jetting process (MJP), matter extrusion, Powder bed fusion (PBF), lamination of layer, directed energy deposition (DED), (aerosol jet printing (AJP), Container lightpolymerization, binder jetting process (BJP), and lithography-based process (LBP) are the significant three-dimensional printing methods for battery production. The most latest result of the CMU company’s efforts with AJP tech is 3-D batteries (Porter et al., 2017; Deiner et al., 2019). The potential for three-dimensional batteries to revolutionize all moveable electronic appliances, from cell phones to notebooks and game systems, has been generated by customer needs and the necessity for substantial advances in three-dimensional batteries. Scientists may use AJP to create the electrodes of the battery in a ventral shape, increasing their permeability. When compared to a solid-form battery frame, enhancing the permeability of the cathode allows for a greater volume to be employed for stock of energy. Electrodes with permeable design may increase the charging capability of lithium-ion batteries (Choi et al., 2012). This is due to a certain design that permits Li to permeate the volume of the electrode, leading to an elevated degree of electrode occupancy, which enhances the capability of energy stocking (20). In standard batteries, thirty to fifty per cent of the entire volume of

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the electrode is unused. And, contrary to injection printing, which may only generate one stream of matter, three-dimensional printing may now achieve the needed permeability with accurate and complicated shapes (Vickers, 2017). The silver three-dimensional printed electrode is lithium plated to get the requisite lithium concentration. Three-dimensional printed systems outperform silver-plated electrodes by 400 per cent in precise capacity (relatively to electrode mass) and 100 per cent in surface capacity (relatively to stored energy) inside the electrode region (above area) (Xiao et al., 2011). 3-D printing may create the latest three-dimensional structured electrodes with such a greater surface region and greater density of charge, enabling for small dissemination lanes and low confrontation among transfer of ion, resulting in increased density of power and density of battery in the forms of durability and atmospheric footprint. Because of low sophisticated manufacturing methods, 3-D printing considerably minimizes wastage of matter and accelerates manufacturing (Vickers, 2017). Numerous electrochemical variables (electrolyte uptake, ionic & electronic conductivity, and thickness,) and three-dimensional parameters ( filling sequence, filling concentration, extra extrusion, circumference, contraction, & subtype of extrusion) are solved by the fusion battery and three-dimensional printing tech for improved three-dimensional printed lithium-ion batteries (Zhu et al., 2017). Companies should build their gadgets dependent on the shape & size of current batteries, which take up the majority of the area in current electronic equipment. The majorities of them are spherical or square form and are designed to work with buttons and pouch batteries. As a result, companies should define a certain form & size for the battery when developing goods, which consumes area and limits pattern possibilities. For the next era of elastic electronics, this is rapidly becoming a structure issue (Kim et al., 2015). Power density, the capability to keep charges without releasing them, the capability to recharging hundreds or thousands of times, and security are all aspects that go into determining a battery’s efficiency. When experimenting with novel techniques, battery makers take great effort to guarantee that the battery’s efficiency does not suffer.

7.2 THREE-DIMENSIONAL PRINTING TECHNOLOGY Three-dimensional printing is rapidly utilised to manufacture complicated three-dimensional things using digitally controlled phase transition

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deposition and solution-dependent reactive matters and dyes as an innovative manufacturing process. To manufacture the three-dimensional battery, this manufacturing approach usually starts with film-by-film processing, as illustrated in Figure 7. 1 (Javey et al., 2007). Certain industrial procedures on three-dimensional print processes have been described in the following content to manufacture the battery, among many forms of three-dimensional printing.

7.2.1 Powder bed fusion (PBF) Powder bed fusion is a three-dimensional printing technique that uses a dusty bed to bond components. To effectively combine components into a dusty bed, several resources, like electron/lasers beams, are utilised. A roller is used to distribute a fine powder coating across a consistent layer. The nonmelted powder is extracted once the required form is achieved and reused in the subsequent manufacturing step. Selective laser melting (SLM), selective laser sintering (SLS), selective heat sintering (SHS), and electron beam melting (EBM), direct metal laser sintering (DMLS), are all part of the Powder bed fusion procedure (Vickers et al., 2017; Espera et al., 2019).

7.2.2 Directed Energy Deposition (DED) Three-dimensional laser coating (LC), direct metal deposition (DMD), Laser engineering mesh formation (LENS), and directional light production (DLF) are some of the directed energy deposition technologies. Directed energy deposition is a very complicated printing method that is frequently utilized for restorations and modifications.

Figure 7.1. 3-D printed film by film to generate the working cathode and anode of a small battery. Source: https://www.sciencedirect.com/science/article/pii/ B9780128215487000026

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Further matters are added using the components. A basic directed energy deposition machine has a jet positioned on multiaxis arms which distribute melted matters and solidify them on a particular surface. The technique is comparable to matter extrusion, however, the jet may move in any orientation and is not fixed to a single axis. Matters that may be deposited at an angle using machines having 4 & 5 axes are combined with an electron/laser beam while deposition. Polymers and pottery may be utilised in such a process, although metals in the state of wire/powder are the most common (Gaikwad et al., 2015).

7.2.3 Material Jetting Process Material jetting procedure uses a consistent placement method to shower matters onto a building platform. The substance is showered upon the base or constructing surface, in which it is repaired and the design is constructed film by film. The matter travels straight on the building base from the jet. The machine’s design and the mechanism for regulating matter deposition differ. Ultraviolet light is used to repair the material layer. The quantity of matters that may be utilized is restricted since the staff should settle. Due to their fluidity and capability to make droplets, waxes and polymers are ideal materials (Azhari et al., 2017).

7.2.4 Binder Jetting Process (BJP) BJP uses a powder-dependent material and an adhesive. The adhesive acts as a binding material among the films of dirt. Resins are frequently fluid, whereas construction materials are usually a powder. The printing head moves straight along the X-axes and Y-axes of the machine, laying sheets of building and adhesive matters in alternating directions. After every sheet, the things to be printed are placed on the respective construction platform. Because of the binding method used, the matter’s properties are often not suitable for structural components, and while the printing rate is fairly fast, further final processing may increase the whole production duration (Choi et al., 2017).

7.2.5 Material Extrusion Fused deposition modelling (FDM) is a popular method of matter extrusion. The matter is drawn into a jet and warmed before being placed film by film. The jet may be travelled straight after every fresh film is applied, and the platform may be adjusted vertically upper and lower sides. Several

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elements impact the final model’s performance, however, if such variables are effectively controlled, they offer a lot of power and practicality. Temp control or chemical methods may be used to bind the matter films. Using Fused deposition modelling, French scientists studied a better technique for manufacturing LiFePO4/graphite batteries (Ying, 2016). Direct induction (DIW) is an extrusion-dependent additive manufacturing technique that is commonly utilized on both the micro-scale & the macro-scale. In Direct induction, fluid-phase ink is extruded having a regulated flow speed through a tiny jet and deposited across a digitally specified route to produce a threedimensional film by film design (Wei et al., 2017).

7.2.6 Vat Photopolymerization Vat polymerization creates a film by film design using a vat of liquid photopolymer adhesive. If required, UV is utilized to fix the adhesive, as well as the platform transfers the manufactured object below after every successive film has repaired. Since such a technique, unlike dirt-dependent methods, employs fluids to build things, the matter has no design support throughout the manufacturing stage, whereas the powder technique relies on loose matters. In these circumstances, additional support structures will almost always be required (Carve & Wlodkowic, 2018).

7.2.7 Lithography-based Process Stereolithography is another name for the Lithography-based process. The lithography-based process is a layer-based manufacturing process that uses UV, infrared, and optical light to fix a fluid photo-polymerizable adhesive. Photopolymers may be uncovered to design elements having a predetermined shape utilizing a system dependent on a digital mirror appliance. Despite the high viscosity of such adhesives, modifications to the system utilizing a revolving building platform may still process emulsions with high solid material ceramic powder (Schwarzer et al., 2017).

7.2.8 Sheet Lamination The LOM (manufacture of laminates) & UAM (manufacture of ultrasonic additives) are both parts of the sheet-laminating procedure. Metal bars & Metal sheets are used in the manufacture of acoustic additives, and they are joined through acoustic welding. This method necessitates extra Tooling and frequently results in the removal of free metals while the welding procedure. Manufacture of Laminates procedure has a comparable film by film method,

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except rather than welding, it employs paper like a matter and adhesive. The Manufacture of Laminates procedure employs a cross-shadowing technique while printing to facilitate extraction (Hu & Sun, 2014). Stainless steel, Aluminum, titanium, and copper are among the metals used by the manufacture of ultrasonic additives process. The procedure is cryogenic and allows for the creation of interior designs. Since the metal doesn’t melt, such a technique may mix a variety of matters and uses a small amount of energy.

7.2.9 Aerosol Jet Printing Aerosol jet printing is a new direct contactless writing technology for producing precise characteristics on a variety of substances. Threedimensional 3-D-printed electronics are supported through Aerosol jet printing. Passive and active electronic elements (resistors, capacitors, antennas, detectors, and thin-film transistors), controllers, detectors, and a range of specific biochemical procedures have all been explored using this technique. Loose deposition and reasonably wide separating gaps enable scientists to build gadgets with more complicated structures than conventional manufacturing or the most generally utilised direct writing techniques. The extensive comparability of substances, high resolution, and directional autonomy of the Aerosol jet printing technique, when implemented as a digitally managed interconnected manufacturing technique, provide innovation for various utilizations. The spray may procedure sports printing on a range of materials, like pottery, plastic, and metallic geometry. Most available materials in the market, like fine particle inks, are being tuned for the aerosol jet procedure however they may be printed on plastic substance (and afterwards sintered using ink) under reduced deformation temperatures (Cao et al., 2017; Deiner et al., 2019).

7.3 BATTERY MATERIALS As seen in Figure 7.2, battery elements include electrodes, separators, solid polymer electrolytes, and current collectors. An anode having a -ve charge and a cathode having a +ve charge is found in every battery, segregated through an electrolyte. Lithium-ion batteries are energy storage devices wherein lithium ions flow from the -ve electrode to the +ve electrode while discharging as well as from the +ve electrode to the -ve electrode while charging. It’s difficult to find an ink substance that fulfils the operating needs of every element in a three-dimensional printed battery. The majority

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of current investigation on three-dimensional printed batteries is centred on electrolyte and electrode matters.

Figure 7.2. demonstration of the battery elements. Source: https://www.sciencedirect.com/science/article/pii/ B9780128215487000026

The complication of batteries is significantly higher since the electroactive matters employed in them are reactive, and geometries like anodes and cathodes are physiologically complicated. It may be hard to generate versions of such matters for three-dimensional printing, and once even printed, they should retain electrical links, manage chemical interactions among elements, and enable the battery to have been discharged and charged repeatedly. Furthermore, the batteries should be secure, this indicates that all batteries should fulfil strong safety requirements before being utilised in planes, houses, automobiles and other similar structures (Pop et al., 2008; Cice et al., 2010). To accommodate for new structures which are continuously evolving, testing requirements might have to be updated. We studied the acceptability of different three-dimensional printing matters having common liquid electrolytes in a preliminary investigation of the matters acceptability of three-dimensional printing matters utilized for the fabrication of containers for electrical and chemical energy-storing appliances such as lithium-ion batteries. For instance, three-dimensional printing polymers (like polylactic acid (PLA)) are not ionic conductors, posing a significant challenge for printed batteries (Yazdi et al., 2016). The researchers enhanced ionic conductibility by adding PLA to the electrolyte solvents. They also improved the conduction ability of the battery by using graphite or multilayer carbon nanotubes in the cathode and anode. However,

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just pottery batteries may endure high temp as compared to lithium-ion batteries in a hot area. Lithium-ion batteries employ fluid or gels electrolytes and are ineffective at higher temp (Chen et al., 2007). Due to the usual metals (like cobalt) included in lithium-ion batteries, there would be issues with matters delivery as the atmospheric catastrophe advances. They’re limitless. Lithium and cobalt are expected to be insufficient to fulfil the need for sustainable tech (Diouf & Pode, 2015). Lithium-ion batteries have grown popular in recent years. You may simply print full lithium-ion batteries in either form, like discs, squares, logos in our lab, and even great cats, using additive manufacturing tech. The difficulty with three-dimensional printed lithium-ion batteries is that the polymers utilized to build them are conductors of ions. The goal was to figure out a way to manufacture lithiumion batteries at a reasonable price using common three-dimensional printers. To keep the battery conductive, the inject polylactic acid into the electrolyte widely utilized in three-dimensional printing (Cardoso et al., 2017). To increase electrical conduction ability, scientists used graphite and carbon nanotubes in residential buildings. Various kinds of batteries, like ZnMnO2 with zinc anode from cathode MnO2, and ionic gel electrolyte (PVDFhexafluoropropylene), consisting of alkali Ag-gel electrolyte-Zn, graphene/ PLA /Li4Ti5O12, carbon/Li4Ti5O12 carbon/additive/PLA-LiFePO4 PLA/ additive, polyethylene/graphite/PLA glycol dimethyl ether average Mn500, PLA/LiMn2O4/MWNT, Mg-Zn, SiO2/PLA/LiFePO4, metal hydride-nickel (MH- Ni), Zn-AgO, alkaline NiZn, PLA/ graphene( are utilized. To enhance electrochemical efficiency put further matters during sustaining adequate mechanical strength for printing (Ren et al., 2018; Maurel et al., 2021)

7.3.1 Materials for Electrode The most widely utilized cathode and anode matters in three-dimensional printed batteries are lithium titanate (LTO) and lithium iron phosphate (LFP), which has a low expansion by volume, the ability of high speed, excellent stability, and safety. A further interesting matter category for electrode matters in three-dimensional printed batteries is carbon nanomaterials (carbon nanofiber, graphene and carbon nanotube,) (Liang et al., 2010). Condensed graphene and graphene oxide, for example, have been utilized to three-dimensional print superfast ultracapacitors. Because of its great mechanical strength, chemical stability, huge precise surface region, and outstanding electrothermal characteristics, carbon nanotubes and carbon nanofibers are also desirable substrates for printing inks. By comparing to a solid block Ag-electrode, the Ag micro lattice employed as lithium-

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ion battery electrodes improved battery efficiency in numerous respects, including a fourfold, enhances the precise capacity and a twofold enhances the areal capacity (Zia et al., 2021). A further advantage of the new method is that electrodes may now be made through common matters such as oxide and silicone that may store five to ten times extra energy as compared to the batteries of recent graphite lithium-ion. However, this presents a unique set of issues. Silicon swells substantially when charged as it may contain ten times extra lithium atoms (Liao et al., 2019). The silicon-electrode battery within the test car will grow to 3 times its initial volume and break during the 1st charging cycle. It’s the fact that certain matters may store extra lithium that causes them to fracture. It’s a bit of a slap in the face. As a result, stress reduction is critical. The researchers worked around this by adding channels and pillars to the electrodes, which prevent the battery from spreading. Because the electrode is saturated with lithium, it doesn’t have to enlarge. Reduced volumetric capacitance in threedimensional printed graphene aerogel electrodes is currently accomplished via “filling” the permeable graphene scaffold with additional nanomaterials and increasing their densities. The volumetric capacitances of their threedimensional printed graphene aerogel electrodes were 100 times greater than those of pure graphene aerogel electrodes (Aravindan et al., 2014). This appeared to come to a head in 2015 when South Korean scientists reported having reached an energy-density of 131 W-h per Kilogram for an ultracapacitor containing graphene electrodes. Such graphene-dependent ultracapacitor density-energy competition arose in part as a result of the belief that ultracapacitors might be recharged considerably faster than Li-ion batteries, making them a viable alternative. 1st, widespread manufacturing of such electrodes will need a large amount of graphene or graphene oxide matters, which are currently scarce. 2nd, the expensive cost of graphene oxide and graphene nanosheets with few sheets prevents them from being widely used in industry (Li & Li, 2004). The sodium-ion battery is the 2nd most common battery. 3-D printed of h Composite MoS2-graphene aerogels as extremely permeable electrode matters for Na-ion battery anodes. During the printing method, a thick liquid ink containing graphene oxide and a molecular MoS2 precursor (ammonium thiomolybdate) nanosheet is employed. The conversion process is inhibited at high speed, and rapid sodium ion intercalation with excellent stability dominates the electrode (Aravindan et al., 2014). This shows how threedimensional printing may be utilized as a processing tool to manipulate the characteristics of matters for the storage of energy.

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7.3.2 Electrolyte Materials Electrolyte is the battery’s key significant component, acting like a catalyst to keep them conductive by stimulating ion flow out from cathode toword anode while charging as well as the inverse movement while discharging. B attery longevity, battery safety, and electrochemical performance are all influenced by the electrolyte (Sun et al., 2013). With the advancement of 3-D printing, the electrolyte of a battery can now be produced directly, cutting down on the manufacturing prices, process, and time. In rechargeable lithium-ion batteries, there are ethylene carbonate electrolyte, HFP/Pyr13TFSI ionic liquid, Li + conductive glass-ceramic electrolyte (GCE), KOH liquid electrolyte, LiTFSI salt and Li7La3Zr2O12 (LLZ) electrolyte (Zhang et al., 2017; Zhang et al., 2020). To avoid the liquid electrolyte against moisture absorption and evaporation, it needs the airtight sealing (for lithium-ion batteries). The feature that perhaps the electrolyte is not formed of a gel or liquid material is what renders such batteries solid. Rather, the firm employs ceramics, that implies that, despite conventional batteries, no liquid could be raised to the point of exploding. Solid materials seem to be the best path to just go, as per the battery industry scientists, ceramics are now the metal to employ. Electrolytic ink compatibility to separators and electrodes within 3-D printing continues a serious concern (Rocha et al., 2020)

7.4 LI-BASED 3D-PRINTED MATERIALS FOR REBS 7.4.1 Li-based Structured electrodes Due to their validated preparation procedures and outstanding electrochemical efficiency LFMP, LFP, LTO, LMO and LCO are commonly utilised in 3D printed LIBs. Such materials are typically manufactured and incorporated with inks having excellent rheological properties. Then, utilizing IJP or DIW processes, inks are manufactured into electrodes with various designs. Even though these materials contain channels within for ion movement, but still poor conductivity is a key disadvantage (Kim et al., 2007). Traditional electrodes having coating improve electrochemical performance by enhancing the electrode conduction by introducing acetylene black or active carbon. A conductive component, like acetylene black or active carbon, is effectively incorporated within the inks as an additive for the electrodes having 3D printing. The ink was then extruded and formed into a predetermined structure, enhancing the stability ,3D electrode structure’s,

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and conductivity. Furthermore, from a structural standpoint, 3D electrodes are advantageous in terms of enhancing the capability of ionic conduction among electrolytes and electrode materials. Complicated electrode architectures may be destroyed after numerous cycles owing to ion movement in the electrode. Electrochemical efficiency could be affected as a result of the electrode deformation. Therefore, f or printing electrodes utilizing above materials, structural stability, electrode architectures, structured surface area, ink additives, and other aspects should all be carefully examined (Zhang et al., 2020).

7.4.1.1 Film Li-based electrodes The 3D designed micro-batteries, that can be utilised in microelectromechanical systems, biomedical sensors, and actuator drivers have received a lot of interest in academia since they can increase energy density while taking up less space. Based on the benefits of extended life cycle and good specific capacity, LMO/LCO has been researched in the past to create LIBs film cathodes. First 100 μm thick cathode film was produced using microbattery+LCO for Li in SLS process in 2007. The performance of this film electrode was about an order of magnitude better than those of thin-film micro-batteries by sputter-deposition. SLS is a widely used technology for fabricating 3D objects by sintering solid powdered substance particularly metal powder with a laser as the source of power (Zhang et al., 2020). It’s a common powder based 3D-printing process for producing 3D functional and long-lasting items. However, selective laser melting (SLM), an SLS-derived technology, is an effective way to produce tailored metals 65 and thermoplastics Their cheap cost, simple process and robust powder processing capabilities offer them a viable option for fabricating REBs delicate and complicated architecture (Khoo et al., 2018). Because of the increasing concentration of LCO with no substantial rise in resistances, they found that discharge capabilities is proportionate to cathode thickness (117 m) in this investigation (Figure 7. 2(a)). This is the first time someone has tried to control the functionality of a 3D-printed batteries by actively adjusting the electrode configuration. Following that, in a work according to the same group, the structured electrode having laser surface treatment that has improved cycling efficiency was proposed. This research showed that the film electrode’s surface structure has an impact on its efficiency. Thin-film electrodes are films having a thickness of a few tens of microns or less. Thinfilm electrodes too have recently garnered the interest of researchers. The IJP approach was used by Huang et al. (2019) to produce the LCO cathode

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of LIBs (Izumi et al., 2014). Because of its excellent printing resolution that is greater that is 80 percent LHV) with lesser electric energy and higher generation yields than contending electrolysis technologies (>5 kW h Nm−3 for alkaline, however >6 kW h Nm−3 for PEM and 800 °C) (Young et al., 2008; Sukeshini et al., 2011). However huge efforts had been devoted in the previous decades to form novel materials only some approaches had been discovered to take benefit of a straightforward rise of the performance of the cells through amendment of its geometry, probably because of the strict restrictions in manufacturing complicated ceramic shapes (Doreau et al., 2000). For example, a rise of the cell’s active area through electrolyte corrugation would directly minimize the cell interior resistance, for instance. its (ASR

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= R/A) area specific resistance, proportionately per projected area rises their performance. Through this way, Li et al. (2013) showed a double fold rise of power density in silicon-founded micro solid oxide fuel cells corrugated yttria-stabilized zirconia electrolytes of tinny film. Regardless of this effective experience, to the writers’ best knowledge, the same approaches had not been utilized in conventional solid oxide fuel cells through the gain of regulatory the cell geometry at the microscale could be easily predicted. It is possibly due to free-form development methods like 3D printing had revealed only lately their appropriateness for producing highly complicated dense ceramic portions with good mechanical features (Esposito et al., 2015). Through this way, Ruiz-Morales et al. (2017) recently reviewed the usage of 3D printing for applications of energy proposing the SLA (stereolithography) printing interest for producing high feature ratio SOFCs which are greatly performing. As per the Ruiz-Morales, the distinct works dedicated to the SOFCs development through 3D printing were concentrated on the fabrication of the planar cell with the only exclusion of the one lately published in the authors in which structures of honeycomb were utilized to expand the mechanical firmness of 3D printed membranes of yttriastabilized zirconia (El‐Toni et al., 2008; Daʹas et al., 2017). The stacks and solid oxide electrolysis/fuel cells are complicated geometrically multi-material devices founded on useful ceramics. As per the latest report additional than 100 steps are needed to fabricate a whole Solid oxide fuel cells stack utilizing traditional manufacturing procedures (punching, tape casting, laminating,screen-printing, firing, or stacking) (Wang et al., 2011). A large amount of steps, few of them need manual inputting, creates the fabrication of the devices a very complicated task with complex design and low dependability for directly producing related to market having a long time. Furthermore, the utilization of these multi-phase ceramic producing methods strongly disturbs the durability and reliability of solid oxide fuel cells structures as multiple seals and joints are existing in the last device. Because of these intrinsic restrictions, the solid oxide fuel cells industry stopped following highly necessary customized designed products to encourage a concept of cost-effective termed “mass customization” founded on the mixture of typical mass formed core planar solid oxide fuel cells units (United States Department of Energy’s Solid State Energy Conversion Alliance, SECA),which, in the last delayed commercialization in heterogeneous segments like as the marketable segment (Gibson et al., 2021).

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Having this perspective, the execution of inventive single-stage fabrication methods like ceramics 3D printing would be critical to overwhelmed major restrictions and reliability concerns of conventional producing of solid oxide fuel cells however enhancing their durability and precise power per unit volume and mass. More precisely, 3D printing of solid oxide fuel cells would permit simplification of the fabrication procedure, a rise of the solid oxide fuel cells design elasticity (permitting high pressure joint-less massive structures with inserted fluidics and present collection), a decrease in the early investment and cost of fabrication collectively with a little time-to-market and, lastly a decrease in consumption of energy and (waste) material. Regardless of the obvious interest of these preservative manufacturing methods for solid oxide fuel cells applications, the subject remained nearly unknown until the latest publication of a series of earlier studies completely attentive on addressing the deficiency of knowledge in 3D printing of operational ceramics of attention for solid oxide fuel cells (Sukeshini et al., 2009). They comprise comprehensive details on the electrochemical and fabrication performance of the SoA materials for solid oxide fuel cells electrolytes and fuel electrodes and oxygen specifically, ceriabased and zirconia-based electrolytes and diverse NiO-founded and LSM (lanthanum strontium manganite), and LSCF (lanthanum strontium cobalt ferrite), founded electrodes, also different approaches for enhancing their corresponding interfaces (Han et al., 2016). Table 8.1. The cell produced from SOFC is fabricated partially or totally through 3D printing. (Blue text was employed to show the layers deposited through technologies of 3D printing) Support/ printing technique

OCV (V); PPD (W cm−2)

Anode/inkjet

0.95; 710

Anode/inkjet

1.06; 860

Multilayer solid oxide fuel cells structure

NiO-YSZ/YSZ/LSM

Temperature (°C)

Reference.

600

(Hernández et al., 2014)

800

(Taylor et al., 2018)

1.10; 1040

750

Anode/inkjet

1.10; 940

750

(Jiang et al., 2012)

Anode/inkjet

1.10; 500

850

(Ruiz-Morales et al., 2017)

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Anode/inkjet

1.10; 460

850

(Kirubaharan et al., 2019)

Electrolyte/ inkjet

1.13; 790

900

(Sha et al., 2018)

Anode/inkjet

1.16; 1500

800

(Shah et al., 2019)

Anode/AJP

1.10; 440

850

1.19; 610

800

(Shimada et al., 2012)

1.05; 378

600

Anode/inkjet

(Sukeshini et al., 2015)

8.2 DENSE THIN ELECTROLYTES The dense electrolytes functioning at transitional temperatures (