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Graphene-Based Electrodes for High-Performance Electrochemical Energy Storage

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Graphene-Based Electrodes for High-Performance Electrochemical Energy Storage GRAPHENE-BASED ELECTRODES FOR HIGH-PERFORMANCE ELECTROCHEMICAL ENERGY STORAGE A Dissertation Presented to The Academic Faculty by Byeongyong Lee In Partial Fulfillment of the Requirements for the Degree Doctor of Philosophy in the George W. Woodruff School of Mechanical Engineering Georgia Institute of Technology December 2018 Copyright © 2018 by Byeongyong Lee GRAPHENE-BASED ELECTRODES FOR HIGH-PERFORMANCE ELECTROCHEMICAL ENERGY STORAGE Approved by: Dr. Seung Woo Lee, Advisor Dr. Hesketh Peter The George W. Woodruff School of The George W. Woodruff School of Mechanical Engineering Mechanical Engineering Georgia Institute of Technology Georgia Institute of Technology Dr. Hailong Chen Dr. Seung Soon Jang The George W. Woodruff School of School of Material Science and Mechanical Engineering Engineering Georgia Institute of Technology Georgia Institute of Technology Dr. Thomas Fuller School of Chemical & Biomolecular Engineering Georgia Institute of Technology Date Approved: July 30, 2018 ii ACKNOWLEDGEMENTS I would like to thank my advisor, Dr. Seung Woo Lee, for his advice and encouragement. I appreciate that I am one of his first graduate students. As a start-up member in his group, I could get valuable experiences for my future career. I would like to thank my committee members, prof. Peter J. Hesketh, prof. Hailong Chen, prof. Seung Soon Jang and prof. Thomas F. Fuller, for their comments on my research. I gratefully thank my collaborators, prof. Suguru Noda and prof. Zhongming Chen. They prepared few-walled carbon nonotube that was widely employed in my research. I thanks to prof. Hee Dong Jang and Dr. Sunkyung Kim for constructive discussion on the preparation of crumpled graphene and submicron Si particles. I appreciate prof. Kwangsup Eom for discussion on overall electrochemistry which helps me to analyze my experimental results. I truly thank Prof. Shuo Chen and Linxin Xie for their devotion to material characterization. I thank my collaborator, Dr. Seokjoon Kwon for collaborations on understanding the charge storage mechanism of graphene. I would also thank Prof. Maenghyo Cho for his advice on finding my research area. I would like to thank my collaborators and friends, Dr. Tianyuan Liu and Mr. Michael J. Lee, including all the group members in prof. Lee’s group. Above all things, I truly thank my wife, Hyunji Kim, and my sons, Eldor and Marvin for supporting me with their endless encouragement. I gratefully acknowledge financial support from prof. Lee’s Georgia Institute of Technology startup fund, Samsung Advanced Institute of Technology (SAIT)’s Global iii Research Outreach (GRO) program and Korea Institute of Geoscience and Mineral Resources (KIGAM). iv TABLE OF CONTENTS ACKNOWLEDGEMENTS iii LIST OF TABLES vii LIST OF FIGURES viii LIST OF SYMBOLS AND ABBREVIATIONS xvi SUMMARY xix CHAPTER 1. Introduction 1 1.1 Energy storage systems: Lithium-ion battery and electrochemical capacitor 1 1.2 Preparation of graphene 4 1.3 Graphene in energy storage applications 7 1.4 Chapter organization 10 CHAPTER 2. Confinement of silicon particles in graphene sheath 13 2.1 Overview 13 2.2 Approach 15 2.3 Experimental methods 16 2.3.1 Sample preparation 16 2.3.2 Material characterization 17 2.3.3 Electrochemical measurement 17 2.4 Results and discussion 18 2.5 Conclusions 32 CHAPTER 3. Graphene as a two-dimensional template 33 3.1 Overview 33 3.2 Approach 34 3.3 Experimental methods 35 3.3.1 Material preparation 35 3.3.2 Material characterization 36 3.3.3 Electrochemical measurement 37 3.4 Results and discussion 39 3.5 Conclusions 59 CHAPTER 4. Crumpled graphene oxide cathode for li-ion batteries 61 4.1 Overview 61 4.2 Approach 62 4.3 Experimental methods 62 4.3.1 Sample preparation 62 4.3.2 Material characterization 63 4.3.3 Electrochemical measurement 64 4.4 Results and discussion 65 4.5 Conclusions 79 v CHAPTER 5. Stacking-controlled assembly of cabbage-like graphene microsphere for charge storage application 80 5.1 Overview 80 5.2 Approach 81 5.3 Experimental methods 82 5.3.1 Sample preparation 82 5.3.2 Material characterization 83 5.3.3 Electrochemical measurement 83 5.4 Results and discussion 85 5.5 Conclusions 97 CHAPTER 6. Crumpled graphene anode for alkali-ion batteries 99 6.1 Overview 99 6.2 Approach 100 6.3 Experimental methods 102 6.3.1 Sample preparation 102 6.3.2 Material characterization 102 6.3.3 Electrochemical measurement 103 6.4 Results and discussion 104 6.5 Conclusions 121 CHAPTER 7. Conclusion and outlook 122 7.1 General conclusions 122 7.2 Perspective 124 REFERENCES 128 vi LIST OF TABLES Table 1.1 Properties of Graphene compared with other carbon materials. ........................ 3 Table 1.2 Summary of chapter organization .................................................................... 10 Table 2.1 Comparison of the electrochemical performances for the various Si-based electrodes. ......................................................................................................................... 28 Table 4.1 Capacity comparison of various free-standing carbon-based cathodes with f- FWNT/r-CGO ................................................................................................................... 77 Table 5.1 Atomic fraction of the functional groups on the C-GRs prepared at different urea concentrations with/without the heat treatment. ............................................................... 90 Table 6.1 Electrolytes and separators for Li-, Na- and K-cells ..................................... 104 Table 6.2 Discharge and charge capacities of the A-CGs. ............................................. 111 Table 6.3 Comparisons of graphene anodes for Na-Ion batteries .................................. 115 Table 7.1 Summaries of graphene as inactive component and active material in energy storage applications. ........................................................................................................ 124 vii LIST OF FIGURES Figure 1.1 Schematic illustration of (a) all carbon electrochemical double layer capacitor, (b) pseudocapacitor and (c) lithium ion battery. All devices have an active material, a current collector, a separator and electrolyte. Reprinted with permission from Ref#13 Copyright © 2014 Royal Society of Chemistry. ................................................................. 2 Figure 1.2 Schematic illustration of an ordinary electric double layer capacitor (EDLC) system and hybrid supercapacitor. Conventional EDLC has a symmetric cell configuration of activated carbon for both positive and negative electrodes. Hybrid supercapacitor, herein lithium ion capacitor, employs Li-intercalation negative electrode material (e.g., graphite and Li4Ti5O12) and capacitive positive electrode material. Reprinted with permission from Ref#18 Copyright © 2012 Royal Society of Chemistry. .................................................... 3 Figure 1.3 Schematic illustration of top-down and bottom-up graphene preparation. Reprinted with permission from Ref#25 Copyright © 2013 Royal Society of Chemistry. 6 Figure 1.4 Schematic illustration of aggregation-resistive graphene. Reprinted with permission from Ref#32 Copyright (2011) American Chemical Society. ......................... 6 Figure 1.5 Various methods to prepare graphene and their applications. Reprinted with permission from Ref#23 Copyright ©2012 Springer Nature.............................................. 7 Figure 1.6 (a) Preparation of graphene. (b) Galavanostatic discharge profile of graphene anode in Li-cell (Inset: charge/discharge profile at steady-state). (c) Cycling stability of graphene in Li-cell. Reprinted with permission from Ref#35 Copyright (2014) American Chemical Society. ............................................................................................................... 8 Figure 1.7 Schematic illustration of graphene-based composite electrodes. Reproduced from Ref#19 with permission of Springer Nature, Copyright ©2014. ............................. 10 Figure 2.1 Schematic procedure for the preparation of the recovered submicron Si coated with graphene and carbon (sm-Si@C/Gr). ....................................................................... 19 Figure 2.2 (a) As-prepared sm-Si colloid and its precipitation after a day. The color of the colloid was faded. (b) The mixture of the positively charged sm-Si and graphene oxide, showing stable dispersion over a week. ............................................................................ 20 Figure 2.3 (a) Low- and (b) high-magnification scanning electron microscopy (SEM) images of the sm-Si@C/Gr. (c) Low- and (d) high-magnification HRTEM images with the fast Fourier transformation analysis of the sm-Si@C/Gr. (e) SEM image of the sm- viii Si@C/Gr for energy-dispersive X-ray (EDX) analysis and corresponding elemental mapping of (f) silicon and (g) carbon. .............................................................................. 21 Figure 2.4 (a) X-ray diffraction (XRD) and (b) Raman spectra of the sm-Si, C@Gr and sm-Si@C/Gr. (c) XPS wide scan survey of the sm-Si@C/Gr. The inset shows high- resolution Si 2p spectra of the sm-Si@C/Gr and C@Gr. (d) Thermogravimetric measurements of the sm-Si@C/Gr and C@Gr electrodes in air at a heating rate of 5 °C min-1. ................................................................................................................................. 23 Figure 2.5 (a) CV scans of the sm-Si@C/Gr during 10 cycles at a scan rate of 0.1 mV s-1 (b) Galvanostatic discharge and charge profiles of the sm-Si@C/Gr
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