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Investigation of Thin Film Materials for Next INVESTIGATION OF THIN FILM MATERIALS FOR NEXT GENERATION LITHIUM ION BATTERIES A Dissertation by CLEMENT JACOB Submitted to the Office of Graduate and Professional Studies of Texas A&M University in partial fulfillment of the requirements for the degree of DOCTOR OF PHILOSOPHY Chair of Committee, Haiyan Wang Committee Members, Arum Han Rusty Harris Xinghang Zhang Head of Department, Miroslav M. Begovic May 2016 Major Subject: Electrical Engineering Copyright 2016 Clement Jacob ABSTRACT Lithium ion battery is the dominant secondary storage technology for portable electronics, electric vehicles, medical devices and grid storage. While it has gained widespread acceptance, current generation battery materials are limited by the expensive and often toxic components, and safety concerns, and, still cannot meet projected storage requirements for future applications. A majority of studies rely on traditional synthesis techniques similar to those used for large scale manufacturing for development and investigation of new materials. Our work takes an alternate approach of harnessing thin film technology that has been extensively developed for semiconductor-related research. The thesis focuses on the investigation of the next generation environmentally friendly and low cost battery material using thin film- based studies. A better understanding and optimization using thin film techniques aids the development of traditional processes for bulk batteries and also paves a way for future all thin film-based battery for portable electronics. The work focuses on Mn-based materials because of its low cost and non-toxic nature. A unique one step deposition processes have been developed and demonstrated using the growth and analysis of epitaxial and highly textured Li(NixMnyCo1-x-y)O2 (NMC) thin film on stainless steel with a thin gold buffer layer. The NMC thin film cathodes gave a high capacity of 167 mAh.g-1 and 125 mAh.g-1 at 0.1 C and 0.5 C respectively. Another promising next generation material Li2MnO3 has also been investigated. An unique process to extract Li2O during synthesis has been developed to activate this material directly during deposition. -1 Li2MnO3 cathodes with capacity of 225 mAh.g were synthesized by tuning growth ii conditions appropriately. Another Mn based chemistry, commonly referred to as Li-rich oxide, has been investigated. Nano-domain and composite model structures have been developed to investigate unresolved questions about the microstructure of the films. It has been demonstrated that a nano-domain model best matches with the characteristic electrochemical properties of Li-rich cathodes with a demonstrated capacity of 293 mAh g-1 at 0.05 C. Further study has been carried out to explore optimum composition and structure for Li-rich based thin film cathodes.Composition variation experiments indicate that the 50:50 deposition schemes gave the highest capacity. Moreover, the results indicate a strong correlation between Li2MnO3 domain size on the capacity of the Li rich electrode. A study to investigate correlation between oxygen stoichiometry and microstructure on behavior of Li2MnO3 showed strong inter-correlation. It shows that Li rich cathodes performed the best when deposited at low oxygen partial pressure while Li2MnO3 required a moderate partial pressure for optimum capacity. Finally Li3PO4 and LiPON electrolytes have been investigated for all solid state battery development. An electrolyte coating on top of a NMC cathode film resulted in significant improvement to the observed capacity. Li3PO4 coated cathodes demonstrated a high capacity of ~ 80 µAh/µm.cm2 at 0.75 µA.cm-2, compared to 65 µAh/µm.cm2 that was observed in bare NMC. This work contributes to the implementation of all solid state batteries using thin film approaches with great potentials for various applications such as integrated circuits, portable medical devices and space applications. iii DEDICATION This work is dedicated to my mom‟s sacrifices, dad‟s patience and hard work, and brother‟s inspiration; invaluable lessons, love and support without which I wouldn‟t be here today. iv ACKNOWLEDGEMENTS I would like to thank my research advisor Dr.Haiyan Wang for all her insights, discussion and guidance through the course of my doctoral research. I am especially grateful for the independence, trust and latitude she gave me to explore new ideas. Dr.Wang‟s systematic approach, attention to detail and drive for results has lent strongly to both my professional and personal development. I would also like to thank my committee members, Dr. Arum Han, Dr. Rusty Harris and Dr. Xinghang Zhang for their time, advice and suggestions. I would also like to thank the faculty at Texas A&M University whose courses have been extremely informative. I am grateful to Dr. Xinghang Zhang and Dr. Haiyan Wang for introducing me to many of the fundamentals of Materials Science which has been extremely helpful through my research. I would also like to thank to Dr. Xing Cheng and Dr.Andreas Holzenburg for the many interesting discussions in their classes. I would also like to acknowledge my current and former colleagues. I would like to thank Tommy Lynch, Travis Neely, Alyaman Amer and Mitchell Underwood for their help with various projects through the years. I would also like to thank Dr. Michelle Myers,Jie Jian and Han Wang for their help with TEM imaging. I am also grateful for all the help and suggestions of my current and former colleagues, Dr.Sungmee Cho, Dr. Joon-Hwan Lee, Dr. Chen-Fong Tsai, Dr. Yuanyuan Zhu, Dr. Aiping Chen, Dr. Qing Su, Dr. Fauzia Khatkhatay, Dr.Liang Jiao, Wenrui Zhang, Leigang Li, Meng Fan and Jijie Huang. A special thanks to the Aggie Fab staff, Robert, Dennie and Jim for fixing broken equipments and setting up new ones v without which this research would not have been possible. Last but not the least, a big thanks to the electrical engineering staff especially, Tammy, Jeannie, Melissa, Anni and Henry. Finally, thanks to my parents and brother for their constant encouragement, patience and love all these years. Without their support, I would have not ventured into this time consuming but rewarding venture. vi NOMENCLATURE PLD Pulsed Laser Deposition PVD Physical Vapor Deposition TEM Transmission Electron Microscopy XRD X-ray Diffraction FWHM Full Width at Half Maximum SAED Selected Area Electron Diffraction FFT Fast Fourier Transformation SEM Scanning Electron Microscopy STEM Scanning Transmission Electron Microscopy HAADF High Angle Annular Dark Field Imaging WDS Wavelength Dispersive Spectroscopy SIMS Secondary Ion Mass Spectroscopy vii TABLE OF CONTENTS Page ABSTRACT ............................................................................................................................. ii DEDICATION ......................................................................................................................... iv ACKNOWLEDGEMENTS .......................................................................................................v NOMENCLATURE ............................................................................................................... vii TABLE OF CONTENTS ...................................................................................................... viii LIST OF FIGURES ................................................................................................................. xi LIST OF TABLES ................................................................................................................. xvi CHAPTER I INTRODUCTION AND LITERATURE REVIEW ............................................1 1.1 Fundamentals of Electrochemistry .................................................................2 1.2 Primary and Secondary Batteries ...................................................................8 1.3 Lithium Ion Batteries ...................................................................................16 1.4 Anode ...........................................................................................................20 1.5 Cathode ........................................................................................................23 1.6 Electrolyte ....................................................................................................36 1.7 Motivation for this Work .............................................................................42 1.8 Research Outline ..........................................................................................47 CHAPTER II RESEARCH METHODOLOGY .....................................................................54 2.1 Equipment Selection ....................................................................................55 2.2 Pulsed Laser Deposition ...............................................................................56 2.3 Sputter System .............................................................................................58 2.4 X-ray Diffraction (XRD) .............................................................................60 2.5 Wavelength Dispersive Spectroscopy (WDS) .............................................62 2.6 Secondary Ion Mass Spectroscopy (SIMS) .................................................64 2.7 Scanning Electron Microscopy (SEM) ........................................................65 2.8 Transmission Electron Microscopy (TEM) .................................................67 2.9 Thick Film Cathode Fabrication ..................................................................69
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