Printing 3D Lithium-Ion Microbattery Using Stereolithography Qiming Chen Purdue University
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Purdue University Purdue e-Pubs Open Access Theses Theses and Dissertations 12-2016 Printing 3D lithium-ion microbattery using stereolithography Qiming Chen Purdue University Follow this and additional works at: https://docs.lib.purdue.edu/open_access_theses Part of the Engineering Commons Recommended Citation Chen, Qiming, "Printing 3D lithium-ion microbattery using stereolithography" (2016). Open Access Theses. 840. https://docs.lib.purdue.edu/open_access_theses/840 This document has been made available through Purdue e-Pubs, a service of the Purdue University Libraries. Please contact [email protected] for additional information. Graduate School Form 30 Updated PURDUE UNIVERSITY GRADUATE SCHOOL Thesis/Dissertation Acceptance This is to certify that the thesis/dissertation prepared By Qiming Chen Entitled Printing 3D Lithium-ion Battery Using Stereolithography For the degree of Master of Science in Mechanical Engineering Is approved by the final examining committee: Liang Pan Chair Kejie Zhao Justin Weibel To the best of my knowledge and as understood by the student in the Thesis/Dissertation Agreement, Publication Delay, and Certification Disclaimer (Graduate School Form 32), this thesis/dissertation adheres to the provisions of Purdue University’s “Policy of Integrity in Research” and the use of copyright material. Approved by Major Professor(s): Liang Pan Approved by: Jay P. Gore 12/1/2016 Head of the Departmental Graduate Program Date i PRINTING 3D LITHIUM‐ION MICROBATTERY USING STEREOLITHOGRAPHY A Thesis Submitted to the Faculty of Purdue University by Qiming Chen In Partial Fulfillment of the Requirements for the Degree of Master of Science in Mechanical Engineering December 2016 Purdue University West Lafayette, Indiana ii TABLE OF CONTENTS Page LIST OF FIGURES .................................................................................................................. iv ABSTRACT ............................................................................................................................ vi CHAPTER 1. BACKGROUND AND LITERATURE REVIEW .................................................. 1 1.1 Introduction .................................................................................................... 1 1.2 3D Lithium‐ion Microbattery .......................................................................... 2 1.2.1 3D Electrode .................................................................................................... 3 1.2.2 3D Solid Electrolyte ......................................................................................... 6 1.3 Solid Polymer Electrolyte (SPE) ....................................................................... 7 1.3.1 Lithium Salt ..................................................................................................... 8 1.3.2 Poly(ethylene oxide) (PEO) ............................................................................. 9 1.3.3 Gel Polymer Electrolyte (GPE) ...................................................................... 12 1.4 Flexible and Printable Battery ....................................................................... 13 1.5 Summary ....................................................................................................... 15 CHAPTER 2. MATERIALS AND METHODS ...................................................................... 16 2.1 Gel Polymer Electrolyte ................................................................................ 16 2.1.1 LiClO4 Electrolyte........................................................................................... 17 2.1.2 PEG Resin ...................................................................................................... 17 2.1.3 Preparation of GPE ........................................................................................ 18 2.2 Electrode Mixture ......................................................................................... 19 2.2.1 LFP and LTO ................................................................................................... 20 2.2.2 Mixture with GPE Resin ................................................................................ 20 iii Page 2.3 Microbattery Assembly ................................................................................. 21 2.3.1 Stereolithography System ............................................................................. 22 2.3.2 3D Microbattery Assembly ........................................................................... 23 2.4 Battery Testing .............................................................................................. 24 2.4.1 Ion Conductivity ............................................................................................ 24 2.4.2 GPE Characterization .................................................................................... 25 2.4.3 Mircobattery Cycle Test ................................................................................ 26 CHAPTER 3. RESULTS AND DISCUSSIONS ...................................................................... 28 3.1 Electrode Mixture ......................................................................................... 28 3.1.1 Rheology Control .......................................................................................... 28 3.1.2 Electrode Photo‐curing ................................................................................. 29 3.2 Gel Polymer Electrolyte Fabrication ............................................................. 30 3.2.1 Adding Al2O3 Nanoparticles .......................................................................... 30 3.2.2 Various 3D Structures ................................................................................... 31 3.3 Material Characterization ............................................................................. 35 3.3.1 Ionic Conductivity Measurement ................................................................. 35 3.3.2 GPE Cycle Test ............................................................................................... 37 3.3.3 Electrode Mixture ......................................................................................... 38 3.4 Cycling Test for Microbattery ....................................................................... 40 CHAPTER 4. CONCLUSIONS ........................................................................................... 42 LIST OF REFERENCES ......................................................................................................... 44 APPENDIX .......................................................................................................................... 49 iv LIST OF FIGURES Figure ............................................................................................................................. Page Figure 1‐1. 2D parallel plate and 3D interdigitated array batteries. .................................. 2 Figure 1‐2. Different 3D architectures for microbattery (a) 3D interdigitated, (b) 3D trench, (c) 3D concentric and (d) 3D aperiodic. .......................................... 3 Figure 1‐3. (a) Isometric view of the 3D microbattery; (b) cross‐section of a single‐pore battery; (c) schematic of alumina template based hybrid electrochemical device; (d) nanoporous microbattery electrodes coated on nickel scaffold. ................................................................................. 4 Figure 1‐4. (a) 3D interdigitated microbattery architecture fabricated by printing inks through 30m nozzle; (b) SEM images of C/PPYDBS post array. .............. 5 Figure 1‐5. LLT solid electrolyte in honeycomb structure: a) structure for half‐ cell; b) structure for full cell. ............................................................................. 6 Figure 1‐6. Conductivity of PEO with LiClO4 or LiBOB salt. ............................................... 10 Figure 1‐7. log versus 1/T plot on (PEO)8LIClO4 system with TiO4 and Al2O3 fillers. ...... 11 Figure 1‐8. Side view of the cable battery separated into component layers. ................ 14 Figure 1‐9. Bendable li‐ion battery turning on a blue LED in bend condition; inset shows the stacked layer in flexible battery. ................................................... 14 Figure 2‐1. Structure of PEGDA olimger. .......................................................................... 18 Figure 2‐2. UV‐polymerization for PEGDA. ....................................................................... 18 Figure 2‐3. Fabrication of GPE. ......................................................................................... 19 Figure 2‐4. Electrode mixture. .......................................................................................... 21 Figure 2‐5. Microbattery’s geometry and assembly: a) 3D geometry of GPE structure; b) microbattery assembly process: 1. fabrication of 3D GPE; 2. flow‐in of electrode mixture; 3. inserting current collectors). ........... 21 v Figure ............................................................................................................................. Page Figure 2‐6. Micro‐stereolithography system. ................................................................... 22 Figure 2‐7. Microbattery assmbly process: a) SEM picture of 3D GPE structure fabricated by stereolithography; b) after filling the trench with electrode mixture; c) SEM picture of Zigzag structure d) polymer matrix in 3D GPE. ...........................................................................................