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Silicon Nanowire Anode for Lithium-Ion Batteries Louisiana State University LSU Digital Commons LSU Doctoral Dissertations Graduate School 2011 Silicon nanowire anode for lithium-ion batteries: fabrication, characterization and solid electrolyte interphase Wanli Xu Louisiana State University and Agricultural and Mechanical College Follow this and additional works at: https://digitalcommons.lsu.edu/gradschool_dissertations Part of the Chemical Engineering Commons Recommended Citation Xu, Wanli, "Silicon nanowire anode for lithium-ion batteries: fabrication, characterization and solid electrolyte interphase" (2011). LSU Doctoral Dissertations. 219. https://digitalcommons.lsu.edu/gradschool_dissertations/219 This Dissertation is brought to you for free and open access by the Graduate School at LSU Digital Commons. It has been accepted for inclusion in LSU Doctoral Dissertations by an authorized graduate school editor of LSU Digital Commons. For more information, please [email protected]. SILICON NANOWIRE ANODE FOR LITHIUM-ION BATTERIES: FABRICATION, CHARACTERIZATION AND SOLID ELECTROLYTE INTERPHASE A Dissertation Submitted to the Graduate Faculty of the Louisiana State University and Agriculture and Mechanical College in partial fulfillment of the requirements for the degree of Doctor of Philosophy in The Gordon A. and Mary Cain Department of Chemical Engineering by Wanli Xu B.S., Dalian University of Technology August 2011 DEDICATION To My Loving Parents, Grandparents, And Husband Zhe Nan 谨以此文 献给 我挚爱的父亲母亲 爷爷奶奶 和丈夫南哲 ii ACKNOWLEDGEMENTS First of all, my heartfelt gratitude goes out to my supervisor, Professor John C. Flake, for successful completion of my dissertation. I am so honored to join in his research group as the first graduate student, and worked with him to set up the lab and equipment from scratch. His untiring effort, encouragement, guidance and support helped me greatly in my graduate studies as well as successful completion of this dissertation. I will be benefiting from this valuable experience for my lifelong endeavors in academia. I also want to thank all of my committee members: Professor Gregory L. Griffin, Karsten E. Thomson, Jayne Garno and Richard L. Kurtz for their valuable suggestions and help in my academic research. I appreciate great help from Dr. Dongmei Cao from Material Characterization Center (MCC) and Dr. Vadim Palshin from Center for Advanced Microstructures and Devices (CAMD), and Dr. Ying Xiao from Department of Biology, LSU in material characterization training and expertise. My sincere thanks go to all the people who have contributed to my graduate studies in Louisiana State University, including Professor James J. Spivey, James E. Henry, and Kerry M. Dooley from Department of Chemical Engineering, and Professor Phillip T. Sprunger from Department of Physics, LSU. I am greatly appreciative of all the people who took part in my research, including other members from our research group: Sri Sai Vegunta, Joel Nino Bugayong, Purnima Narayanan, Minh Le, Johnpeter Ngunjiri and Maoming Ren; as well as Nitin Kumar, Nachal Devi Subramanian, Andrew Campos, and Mia Dvora from Department of Chemical Engineering; Golden Hwang, Wenyu Song and Xiaofeng Chang from Department of Electrical Engineering; Li Lu, Weiping Qiu, and Ranran Liu from Department of Mechanical Engineering for their generous help throughout these years. iii Many great thanks also go to all the supporting staff from Department of Chemical Engineering: Paul Rodriguez, Joe Bell, Darla Dao, Melanie McCandless, and Robert Willis for their generous help. Last but certainly not least, I cannot image to go through the past five years in graduate study and complete this dissertation without endless support from my family and friends. I want to thank my loving husband Zhe Nan for his unconditional love, support and caring for me wholeheartedly throughout this special time. Special thanks also go to my dear friends: Di, Limin, Yuan and Lingyan. iv TABLE OF CONTENTS DEDICATION ................................................................................................................................ ii ACKNOWLEDGEMENTS ........................................................................................................... iii LIST OF TABLES ........................................................................................................................ vii LIST OF FIGURES ..................................................................................................................... viii ABSTRACT ................................................................................................................................. xiv CHAPTER 1 INTRODUCTION .................................................................................................... 1 1.1 Context and Motivation ........................................................................................................ 1 1.2 This Work ............................................................................................................................. 3 CHAPTER 2 LITERATURE REVIEW ......................................................................................... 5 2.1 Lithium-Ion Battery .............................................................................................................. 5 2.1.1 Introduction .................................................................................................................... 5 2.1.2 Silicon Anodes: Advantages and Challenges ................................................................ 8 2.1.3 Solid Electrolyte Interphase ......................................................................................... 20 2.2 Silicon Nanowire: An Overview ......................................................................................... 29 2.2.1 Synthesis ...................................................................................................................... 29 2.2.2 Assembly and Integration ............................................................................................ 32 CHAPTER 3 SILICON NANOWIRE FABRICATION AND INTEGRATION VIA NICKEL MONOSILICIDE CONTACTS.................................................................................................... 35 3.1 Introduction ......................................................................................................................... 35 3.2 Material and Methods ......................................................................................................... 36 3.2.1 Silicon Nanowire Fabrication via Electroless Etching ................................................ 36 3.2.2 Silicon Nanowire Deposition ....................................................................................... 36 3.2.3 NiSi Formation via Thermal Annealing ...................................................................... 37 3.2.4 Electrical Resistance Measurement ............................................................................. 37 3.2.5 Material Characterization ............................................................................................. 38 3.3 Results and Discussion ....................................................................................................... 40 3.3.1 Silicon Nanowire Fabrication ...................................................................................... 40 3.3.2 Nickel Silicide Formation on Silicon Nanowires ........................................................ 47 3.4 Conclusions ......................................................................................................................... 58 CHAPTER 4 SILICON NANOWIRE COMPOSITE ANODES FOR LITHIUM-ION BATTERIES ................................................................................................................................. 59 4.1 Introduction ......................................................................................................................... 59 4.2 Material and Methods ......................................................................................................... 59 4.2.1 Silicon Nanowire Anode Preparation .......................................................................... 59 v 4.2.2 Anode Characterization ............................................................................................... 61 4.3 Results and Discussion ....................................................................................................... 71 4.3.1 Silicon Nanowire Array Anodes .................................................................................. 71 4.3.2 Silicon Nanowire Composite Anodes .......................................................................... 73 4.4 Conclusions ......................................................................................................................... 86 CHAPTER 5 SURFACE CHEMISTRY AND SOLID ELECTROLYTE INTERPHASE OF SILICON NANOWIRE ANODES ............................................................................................... 87 5.1 Introduction ......................................................................................................................... 87 5.2 Materials and Methods ........................................................................................................ 88 5.2.1 Anodes Preparation ...................................................................................................... 88 5.2.2 Electrochemical Measurements ..................................................................................
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