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Subramanian Udel 006 OPERANDO LIQUID-CELL ELECTRON MICROSCOPY OF THE ELECTROCHEMICAL POLYMERIZATION OF BEAM-SENSITIVE CONJUGATED POLYMERS by Vivek Subramanian A dissertation submitted to the Faculty of the University of Delaware in partial fulfillment of the requirements for the degree of Doctor of Philosophy in Materials Science and Engineering Fall 2020 © 2020 Vivek Subramanian All Rights Reserved OPERANDO LIQUID-CELL ELECTRON MICROSCOPY OF THE ELECTROCHEMICAL POLYMERIZATION OF BEAM-SENSITIVE CONJUGATED POLYMERS by Vivek Subramanian Approved: __________________________________________________________ Darrin J. Pochan, Ph.D. Chair of the Department of Materials Science and Engineering Approved: __________________________________________________________ Levi T. Thompson, Ph.D. Dean of the College of Engineering Approved: Louis F. Rossi, Ph.D. Vice Provost for Graduate & Professional Education and Dean of the Graduate College I certify that I have read this dissertation and that in my opinion it meets the academic and professional standard required by the University as a dissertation for the degree of Doctor of Philosophy. Signed: David C. Martin, Ph.D. Professor in charge of dissertation I certify that I have read this dissertation and that in my opinion it meets the academic and professional standard required by the University as a dissertation for the degree of Doctor of Philosophy. Signed: __________________________________________________________ Darrin J. Pochan, Ph.D. Member of dissertation committee I certify that I have read this dissertation and that in my opinion it meets the academic and professional standard required by the University as a dissertation for the degree of Doctor of Philosophy. Signed: ________________________________________________________ Chaoying Ni, Ph.D. Member of dissertation committee I certify that I have read this dissertation and that in my opinion it meets the academic and professional standard required by the University as a dissertation for the degree of Doctor of Philosophy. Signed: ___________________________________________________________ Karl S. Booksh, Ph.D. Member of dissertation committee ACKNOWLEDGEMENTS First and foremost, I would like to thank you Dr. Martin for helping me evolve as a scientist during my time in the lab. I think you deserve this whole paragraph to yourself. I am grateful for your unwavering support and guidance throughout my Ph.D. Thanks for always having the answers to all my questions especially when I started out. I still vividly remember the days when you came with me to the Talos room to teach me low-dose electron microscopy. Those moments have made my grad school life much more unique and memorable. Honestly, I would not have been able to achieve whatever I have until this point without your continuous support throughout my Ph.D. In the future, I truly hope to see PEDOT being used in our bodies someday (maybe Elon Musk would help us do that) and that your relentless quest for playing with “expensive toys” never ends. Next, this thesis would definitely not have been complete without the consistent feedback from my Ph.D. committee. Dr. Ni, Dr. Pochan and Dr. Booksh (and Dr. Kloxin for being on my qualifying committee), a special thank you to all of you for being available from time to time and for coming up with valuable suggestions about my work. Those suggestions and questions challenged me and made me think about my dissertation from a totally different perspective. Jen, I also owe you a debt of gratitude for all the help you have done. After the senior students graduated, you were a great mentor to me. Thanks for the time you iv invested in training me on the TEM and for all the suggestions and inputs you had in general on my experiments. Yong, thanks to you as well for helping me understand SEM and FIB. I would also like to thank my current lab members Shrirang, Peter, Quintin, Junghyun, Dr. Samadhan Nagane and Yuhang for their support. Likewise, I would also like to extend a vote of thanks to my previous group members Dr. Jinglin Liu, Dr. Bin Wei, Dr. Jing Qu and Dr. Chin-Chen Kuo for guiding me during the initial years of my Ph.D. Furthermore, Prof. Glenn Yap and Casey, thank you to both of you as well for teaching me the art of single crystal growth and of course for all the help with single crystal x-ray diffraction. Finally, this would not have been possible without the continuous emotional and moral support of my parents, relatives and friends both here in the USA, India and residing elsewhere in the world. Together, you all have made this journey so much fun for me and full of growth, happiness and scientific discoveries. v TABLE OF CONTENTS LIST OF TABLES ......................................................................................................... x LIST OF FIGURES ....................................................................................................... xi ABSTRACT .............................................................................................................. xviii Chapter 1 INTRODUCTION .............................................................................................. 1 1.1 Motivation: Elucidating the mechanistic details of the electrochemical polymerization reaction of poly(3,4-thylenedioxythiophene)(PEDOT) ... 1 1.2 The Technique: Operando Liquid-cell Transmission Electron Microscopy ................................................................................................ 2 1.3 Organization of the chapters ...................................................................... 4 1.3.1 Chapter 1: ...................................................................................... 4 1.3.2 Chapter 2: ...................................................................................... 4 1.3.3 Chapter 3: ...................................................................................... 5 1.3.4 Chapter 4: ...................................................................................... 5 1.3.5 Chapter 5: ...................................................................................... 6 1.3.6 Chapter 6: ...................................................................................... 6 REFERENCES ............................................................................................................... 8 2 MOLECULAR MOVIES: A REVIEW OF RECENT WORK, CURRENT CHALLENGES AND FUTURE OPPORTUNITIES IN LIQUID-PHASE TRANSMISSION ELECTRON MICROSCOPY (LPTEM) OF BEAM- SENSITIVE ORGANIC MATERIALS ........................................................... 11 2.1 Introduction ............................................................................................. 11 2.2 Considerations and challenges during imaging beam-sensitive materials in LPTEM ................................................................................ 14 2.2.1 Electron-water interactions .......................................................... 14 2.2.2 Beam-specimen interactions ........................................................ 16 vi 2.2.3 The “bowing effect” of viewing windows ................................... 19 2.2.4 Gas bubbles in the feed solution .................................................. 21 2.2.5 Dewetting due to hydrophobicity ................................................ 22 2.2.6 Irregular flow ............................................................................... 22 2.2.7 Finding the right focal plane ........................................................ 23 2.2.8 Voltage spikes in the potentiostat ................................................ 24 2.3 Recent applications of LPTEM in Materials Science .............................. 24 2.3.1 Soft materials ............................................................................... 24 2.3.2 Crystal Growth ............................................................................ 31 2.3.3 Batteries ....................................................................................... 33 2.3.4 Metal Organic Frameworks (MOFs) ........................................... 36 2.3.5 Nanowires .................................................................................... 38 2.3.6 Nanoparticles ............................................................................... 39 2.4 Future Opportunities ................................................................................ 39 2.4.1 Machine Learning ........................................................................ 39 2.4.2 Vibrational spectroscopy in liquid-phase electron microscopy ... 40 REFERENCES ............................................................................................................. 42 3 IN-SITU TRANSMISSION ELECTRON MICROSCOPY (TEM) OF THE ELECTROCHEMICALLY-DRIVEN NUCLEATION, GROWTH, AND SOLIDIFICATION OF POLY(3,4-ETHYLENEDIOXYTHIOPHENE) (PEDOT) ........................................................................................................... 54 3.1 Introduction ............................................................................................. 54 3.2 Materials and Methods ............................................................................ 58 3.2.1 Monomer solution: ...................................................................... 58 3.2.2 Liquid flow cell and electrochemistry chips: .............................. 58 3.2.3 Transmission Electron Microscopy: ............................................ 59 3.2.4 Electrochemistry: ........................................................................
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