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Manufacturing Nanocomposites with Highly-Aligned Carbon Nanotubes

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Manufacturing Nanocomposites with Highly-Aligned Carbon Nanotubes ABSTRACT Novel Material Behavior in Carbon Nanotube/Elastomer Composites by Brent J. Carey Composites are multiphasic materials with individual constituent parts that work cooperatively to produce some desired result. For the common case of structural composites, the use of nanoscale additives does not always yield a predictable outcome due to the complex interactions that occur in the interfacial region where a reinforcing filler meets the supporting matrix. It stands to reason, however, that the thoughtful and deliberate exploitation of unusual effects in this region could lead to the development of nanocomposite materials with extraordinary properties. In this thesis work, I will introduce two such responses in a compliant nanocomposite consisting of highly-aligned carbon nanotubes (CNTs) encased within a poly(dimethylsiloxane) (PDMS) matrix. It is first demonstrated that the material exhibits extremely anisotropic dynamic mechanical behavior. The composite will behave in a way that is evocative of the neat polymer when deformed orthogonal to the CNT alignment direction, yet will exhibit strain softening when cyclically compressed along their axis due to the collective buckling of the nanotube struts. Next, it is shown that this nanocomposite material has the ability to respond and adapt to applied loads. Independent, yet complimentary tests reveal that the structure of the polymer in the presence of nanoscale interstitials will evolve during dynamic stressing, an effect that was predicted nearly 50 years ago. With support from both recent and established literature, an updated mechanism is proposed. Collectively, these results provide insight into the complicated mechanics between polymer matrices and embedded nanoparticles, and assist in the design of advanced synthetic materials with unique physical properties . Acknowledgments The path to PhD has been a strenuous, yet enriching experience. I’ve grown tremendously over the past 5 years, and never would have reached this point without the help of everyone mentioned below. I’d first like to show gratitude to my advisor, Prof. Pulickel M. Ajayan, for providing the driving force behind my research. In addition to his scientific expertise, he has constantly encouraged me to explore my interests, both academic and extracurricular. He is a patient and approachable mentor, and has treated me with the utmost respect during my time in his group, a reality that not all graduate students share. I’d also like to thank the other members of my committee, Prof. Enrique V. Barrera and Prof. Carl Rau, for their thoughtful feedback on my research. I am indebted to the numerous researchers with whom I have collaborated along the way, including Dr. Lijie Ci. Dr. Kevin Yager, Prof. Glaura Silva, Dr. Shashi Karna, Dr. Jerome Tzeng, Dr. Myung Gwan Hahm, Prof. Andrew Gouldstone, and Dr. Meng Qu. Appreciation is also shown to Prof. Rafael Verduzco, Dr. Mary Jane O’Rourke, and Prof. Edwin Thomas for meaningful discussions. I’d like to specifically mention Prof. Prabir Patra, as he had the foresight to procure the DMA for our group, and has gone out of his way over the years to maintain contact with me and encourage my progress. His dedication to my growth as a scientist is deeply appreciated. v Of course, this research would not be possible without the financial support of the NASA Graduate Student Researchers Program (GSRP). I owe many thanks to the nanomaterials group at the Johnson Space Center, including Dr. Brad Files, Dr. Ed Sosa, Dr. Rodrigo Devivar, and Mr. Eric Malroy, for their support and hospitality. The support staff of both the Applied Physics degree program and the Mechanical Engineering and Materials Science department have played a pivotal role in helping me navigate formalities, and Dr. Bruce Johnson, Ms. Yvonne Kambourelis, Ms. Carolyn Aresu, Ms. Sherry Vanderslice, and Ms. Linda Lerma are thanked for their assistance. Also, gratitude is shown to Dr. Jan Hewitt for her help in scientific writing and presenting, as well as the unsung heroes of the Fondren Library, who hunted down all of the obscure journal articles I requested. Not to be forgotten is the incredible social structure for graduate students at Rice University. This whole process would have been much more wearisome had there not been a place to hang my hat and commiserate with other burgeoning (read: struggling) researchers. Viva Valhalla. Finally, I owe the most to my incredible family. My parents have always encouraged me to reach higher, and their support has given me the confidence to achieve this life-long goal. My wife, Sarah, deserves recognition for her unwavering support over the years, and particularly for relocating to Houston so that I could pursue my degree. She has been my rock, and is a saint for tolerating the long (and often miserable) hours that graduate study requires. For these and many other reasons, I wouldn’t be where I am today without her. Contents Acknowledgments ..............................................................................................................iv Contents..............................................................................................................................vi List of Figures ......................................................................................................................ix List of Tables ..................................................................................................................... xvi List of Equations .............................................................................................................. xvii Nomenclature ................................................................................................................. xviii Introduction ........................................................................................................................ 1 1.1. Introduction to Carbon Nanotubes .......................................................................... 1 1.1.1. A Brief History of Carbon Nanotube Synthesis .................................................. 3 1.1.2. Growing Vertically-Aligned Arrays of Carbon Nanotubes ................................. 8 1.2. Introduction to Nanocomposite Materials ............................................................ 13 1.2.1. Comparing Various Matrices and Fillers .......................................................... 15 1.2.2. Managing Aggregation and Dispersion............................................................ 17 1.2.3. Understanding the Interface and Interphase .................................................. 19 1.3. Carbon Nanotube/Polymer Composites ................................................................ 23 1.4. Research Motivations ............................................................................................. 25 Manufacturing Nanocomposites with Highly-Aligned Carbon Nanotubes .................... 27 2.1. Composite Preparation through Forest Impregnation .......................................... 28 2.1.1. Poly(dimethylsiloxane) .................................................................................... 30 2.2. Preparing Composites with Vapor-Phase-Grown CNTs ......................................... 32 2.2.1. Synthesizing Many-Walled CNT Forests via Vapor Phase CVD........................ 32 2.2.2. Impregnation of Robust MWNT Forests .......................................................... 39 2.3. Preparing Composites with Few-Walled CNTs ....................................................... 40 2.3.1. Synthesizing Few-Walled CNT Forests via Pre-Deposited Catalyst CVD ......... 40 2.3.2. Impregnating Delicate FWNT Forests via “Sandwich” Preparation ................ 42 2.4. Comparing MWNTs and FWNTs in PDMS Composites .......................................... 48 2.4.1. Sample Preparation ......................................................................................... 49 Dynamic Mechanical Properties of Highly-Anisotropic Nanocomposites ..................... 50 vii 3.1. Unusual Behavior in Elastomer Composites and Nanotubes................................. 50 3.1.1. Nonlinear Viscoelasticity in Filled Elastomers ................................................. 51 3.1.2. Buckling, Kinking, and Negative Stiffness in Carbon Nanotubes ..................... 55 3.1.3. A Combination of These Unique Materials...................................................... 58 3.1.4. Dynamic Mechanical Analysis .......................................................................... 59 3.2. Cyclically Stressing Highly Anisotropic Nanocomposites ....................................... 60 3.2.1. Unfilled PDMS .................................................................................................. 60 3.2.2. Radial Deformation: Reminiscent of the Neat Polymer .................................. 62 3.2.3. Axial Deformation: Dynamic Strain Softening ................................................. 74 3.3. Determining the Mechanics of Deformation ......................................................... 76 3.3.1. Radial Loading .................................................................................................. 76 3.3.2. Axial Loading .................................................................................................... 78 Self-Stiffening in Nanocomposites: Isolating the Effect ................................................. 84 4.1. Conventional Responses to Cyclic Stressing..........................................................
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