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Structure, Characterization and Exploration of Synthesis of Conical and Polyhedral Crystals of Graphite

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Structure, Characterization and Exploration of Synthesis of Conical and Polyhedral Crystals of Graphite Structure, Characterization and Exploration of Synthesis of Conical and Polyhedral Crystals of Graphite A Thesis Submitted to the Faculty of Drexel University by Svetlana Dimovski in partial fulfillment of the requirements for the degree of Doctor of Philosophy January 2006 © Copyright 2006 Svetlana Dimovski. All Rights Reserved. iii DEDICATIONS To my family and the divine circle of my friends, for shaping and enriching my life with their love and dedication, and To the memory of my beloved step-father, Antonije Djuric, for a legacy of love, courage, humor, independence, and freedom of choice. iv ACKNOWLEDGEMENTS This work would not be accomplished without the genuine support of a large number of people. First and foremost, I would like to thank my graduate advisor, Prof. Yury Gogotsi, for his support, coaching, encouragement and guidance throughout my PhD studies. His vision, trust, enthusiasm and an extraordinary abundance of energy were a large source of motivation and a major driving force that kept me on this path. As a teacher, Prof. Gogotsi showed me how to look outside the box and how to define, analyze and solve problems. As a leader and manager, he taught me the importance of setting high goals, developing personal mastery, and staying firm and enthusiastic during the process. I am grateful that under his tutelage and his enduring optimism I had plenty of opportunities to practice and develop new skills and apply these learnings towards my professional and personal development. Thanks are further due to my thesis committee members; Prof. Frank Ko, Prof. Richard Knight and Prof. Alexander Fridman from Drexel University, and Prof. John E. Fischer from the University of Pennsylvania. Their constructive criticism, challenging questions and stimulating discussions were of crucial importance towards completion of this work. They helped me address the problem from various directions and establish clear boundaries for my work. During the course of my research I had an opportunity to collaborate with Prof. Slava V. Rotkin from Lehigh University, Prof. John Jaszczak, Prof. Stephen Hackney and v Prof. George W. Robinson from Michigan Technological University, and Prof. Pin-Heng Tan from the Chinese Academy of Sciences. Prof. Rotkin’s expertise in modeling of the energetics of carbon nanostructures was very instructional in understanding the mechanism of formation of graphite polyhedral crystals. Prof. John Jaszczak and the team from MTU shared their insights, knowledge, expertise and some data about naturally occurring counterparts of carbon cones. Working with Prof. Jaszczak has been a greatly rewarding experience for me and I owe him my sincere special thanks for the past few years of productive collaboration. Prof. Ping-Heng Tan provided his valuable insights in the analysis of Raman spectra of graphite single crystal edge planes and graphite polyhedral crystals. These collaborations contributed to the research in providing various pieces of the puzzle that brought me closer to the solution of problem. I would like to thank Mr. David von Rohr for introducing me to the world of microscopy and for kindly sharing his knowledge and experience of this analytical technique. I am thankful to Mr. Davide Mattia for his experimental help with hydrothermal experiments and Dr. Haihui Ye and Dr. Joseph Libera for help with transmission electron microscopy. J. Libera started the research on polyhedral crystals and cones in glassy carbon that I continued. Dr. L. Rotkina and Dr. D. Ge helped me with FIB work. Mr. Jay Bhatt, Hagerty library information services librarian, provided an excellent support in getting access to literature material utilized in the present study. On a number of occasions Beth Carroll, Maria Pia Rossi, Holly Burnside and Kristopher Behler proof-read my manuscripts, presentations or posters and helped me say what I really meant to say. I am grateful for their kind support. Members of the vi Nanomaterials Group at Drexel University have always been supportive colleagues and friends, and for that I owe them greatest respect. My new colleagues and great management team at Procter & Gamble Miami Valley Information Center have been very supportive and understanding during the writing of this thesis. Mr. Matthew H. Chestnut kindly helped with proof-reading many of pages that follow. His input and suggestions were of a great value for me. Thanks are further due to my undergraduate mentor, Prof. Leposava Sidjanin from the University of Novi Sad, Serbia and Montenegro, a person with charismatic energy, integrity and optimism. It was her professional expertise, guidance and coaching craftsmanship that had a vital influence in forming my desire to study materials science and engineering. The Department of Materials Science and Engineering at Drexel University has been a venue of a tremendous change over the last few years. It was an exciting period of time for both faculty and students, and it was a valuable experience for me to participate in this growth process. I greatly enjoyed the friendliness and supportive atmosphere at the department. Mr. Bill Jones from Solar Atmospheres, Inc. helped me run my initial experiments on their production site. Solar Atmospheres, Inc. built and donated a customized furnace for our experimental needs. Mr. Jones’s generosity and support are indeed far beyond ordinary, and I owe him my sincere thanks. I am very grateful for getting to know every person that life had brought to me so far, but I would like to mention an inner circle of special friends whose presence had the vii greatest impact on me since I came to the USA. They are: Riad, Korhan, Goknur, Mesut, Alexei and Eda. Some of these people I’ve known for years and some of them I happened to meet recently, nevertheless, they all amaze me over and over with their compassion, strength, wisdom, passion and balance. As a mentor and a friend, Prof. Riad Gobran truly enlightened my life with his wisdom, an interesting outlook on life, unlimited encouragement and support. I thank him for always going out of his way in helping me and guiding me through my trying times. I am thankful beyond words for his joie-de-vivre and the way he affected my perception of life. Finally, my dear family, I thank them for their compassion, love, patience and strength. Unfortunately, the time spent away from each other can never be restored. This research has been sponsored by the Department of Energy grant DE-FJ02- 01ER45932. The purchase of the Raman spectrometer and environmental SEM was supported by NSF grants DMR-0116645 and BES-0216343. Kind thanks go to Zonta International and Nikolich Trust for financial support through the Amelia Earhart and Studenica Foundation scholarships. viii TABLE OF CONTENTS LIST OF TABLES............................................................................................................. xi LIST OF FIGURES .......................................................................................................... xii ABSTRACT..................................................................................................................... xxi CHAPTER 1: INTRODUCTION........................................................................................1 CHAPTER 2: LITERATURE REVIEW.............................................................................5 2.1 Graphite....................................................................................................................7 2.2 Carbon nanotubes...................................................................................................11 2.3 Observation of multi-shell non-planar graphitic materials ....................................18 2.3.1 Carbon whiskers and cones...................................................................19 2.3.2 Carbon nanotubes with polygonal cross-section...................................28 2.3.3 Properties of carbon cones and polygonal tubes: theoretical considerations........................................................................................31 2.4 Nanotubes and cones made of inorganic compounds............................................35 2.5 Summary, motivation and study objectives...........................................................41 CHAPTER 3: MATERIALS AND METHODS ...............................................................45 3.1 Materials ................................................................................................................45 3.1.1 Glassy carbon........................................................................................46 3.1.2 Carbon cones in natural graphite samples ............................................51 3.2 Materials characterization techniques....................................................................55 3.2.1 Scanning electron microscopy .............................................................57 ix 3.2.2 Transmission electron microscopy ......................................................65 3.2.3 Micro-Raman spectroscopy .................................................................76 CHAPTER 4: RESULTS AND DISCUSSION ................................................................88 4.1 Carbon cones..........................................................................................................88 4.1.1 Occurrence of cones in glassy carbon....................................................88 4.1.2 Naturally occurring carbon cones ........................................................101 4.1.3 Carbon cones
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