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Nanoindentation Characterization of Clay Minerals and Clay-Based Louisiana State University LSU Digital Commons LSU Doctoral Dissertations Graduate School 2013 Nanoindentation characterization of clay minerals and clay-based hybrid bio-geomaterials Rohit Raj Pant Louisiana State University and Agricultural and Mechanical College Follow this and additional works at: https://digitalcommons.lsu.edu/gradschool_dissertations Part of the Civil and Environmental Engineering Commons Recommended Citation Pant, Rohit Raj, "Nanoindentation characterization of clay minerals and clay-based hybrid bio-geomaterials" (2013). LSU Doctoral Dissertations. 958. https://digitalcommons.lsu.edu/gradschool_dissertations/958 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]. NANOINDENTATION CHARACTERIZATION OF CLAY MINERALS AND CLAY-BASED HYBRID BIO-GEOMATERIALS A Dissertation Submitted to the Graduate Faculty of the Louisiana State University and Agricultural and Mechanical College in partial fulfillment of the requirements for the degree of Doctor of Philosophy in The Department of Civil and Environmental Engineering by Rohit Raj Pant B.E., National Institute of Technology Rourkela, 2002 M.S., Louisiana State University and A&M College, 2007 December 2013 i To My grandparents My parents My family My teachers and My alma mater ii Acknowledgements I would like to express my sincere gratitude to my advisor, Dr. Guoping Zhang, whose expertise, understanding and patience added considerably to my graduate experience. I cannot thank you enough for your guidance and continuous support throughout my Ph.D. journey. I also wish to express my deep appreciation to the members of my graduate committee: Dr. Murad Y. Abu-Farsakh, Dr. Jungwon Jung, Dr. Ying Wang and Dr. Steven G. Hall. Your encouragement, guidance, and valuable suggestions have highly benefited my PhD work. I would also like to acknowledge the elucidating discussions with Professor G. Byerly, LSU and Dr. V.P. Singh, CAMD-LSU. Technical support of Mr. Rick Young, Rock Preparations Laboratory lab, Ms. Wanda LeBlanc, X-Ray Diffraction & Geochemistry Lab, Dr. Dogmei Cao, Material Characterization Center and Ying Xiao, Biological Sciences, LSU in sample preparation and SEM/TEM imaging is greatly appreciated. I have greatly benefited from the collaboration with my fellow research group members, thank you for your time, patience and insightful discussions. I thank my grandparents, parents and my family for the support they provided me through my entire life. Your love and support has given me the strength and guidance to pursue my dreams and succeed in my career path. iii Table of Contents Acknowledgements............................................................................................................. iii List of Tables ....................................................................................................................... vii List of Figures .................................................................................................................... viii Abstract … .............................................................................................................................. x Chapter 1. Introduction ....................................................................................................... 1 1.1. Background ................................................................................................................. 1 1.2. Objective and Scope ................................................................................................... 2 1.3. Organization of the Dissertation ................................................................................. 3 1.4. References ................................................................................................................... 4 Chapter 2. Literature Review ............................................................................................ 5 2.1. Clay and Clay Minerals .............................................................................................. 5 2.1.1. General Structure and Classification of Clay Minerals ...................................... 5 2.1.2. Review of Mechanical Properties of Clay Minerals ........................................... 8 2.2. Clay Based Composites ............................................................................................ 10 2.2.1. Mechanism of Clay-polymer Interaction in Nanocomposites .......................... 10 2.2.2. Classification of Clay Based Composites ......................................................... 11 2.2.3. Clay Based Cementitious Binder ...................................................................... 12 2.3. Techniques for Chemical, Structural and Microstructural Characterization ............ 13 2.3.1. X-ray Diffraction ............................................................................................... 13 2.3.2. Scanning Electron Microscope (SEM).............................................................. 14 2.3.3. Transmission Electron Microscope (TEM) ....................................................... 16 2.4. Nanoindentation Technique ....................................................................................... 17 2.4.1. Indentation Modulus ......................................................................................... 19 2.4.2. Hardness ............................................................................................................ 20 2.4.3. A Grid Indentation Technique .......................................................................... 21 2.4.4. Continuous Stiffness Measurement .................................................................. 22 2.5. References ............................................................................................................ 24 Chapter 3. Elastic-Plastic Anisotropy of Muscovite Probed by Nanoindentation ............................................................................................ 32 3.1. Introduction ............................................................................................................... 32 3.2. Materials and Methods .............................................................................................. 33 3.3. Analysis of Results ................................................................................................... 34 3.3.1. Load Displacement Curves ............................................................................... 34 3.3.2. Indentation Modulus ......................................................................................... 38 3.3.3. Hardness ............................................................................................................ 39 3.3.4. Anisotropy ......................................................................................................... 41 3.3.5. Fracture Toughness ........................................................................................... 42 iv 3.4. Discussion ................................................................................................................. 43 3.5. Conclusions ............................................................................................................... 46 3.6. References ................................................................................................................. 46 Chapter 4. Indentation Size Effect in Muscovite Mica ............................................. 50 4.1. Introduction ............................................................................................................... 50 4.2. Review of ISE Models .............................................................................................. 51 4.2.1. Strain Gradient Theory and Physical Material Length Scale (Nix & Gao (1998)) .......................................................................................... 51 4.2.2. Non-linear Coupling of Flow Stress (Abu Al-Rub 2007, Abu Al-Rub and Voyiadzis 2004a, b) ......................................................................................... 53 4.2.3. Reverse Indentation Size Effect ........................................................................ 54 4.3. Indentation Size Effect in Muscovite Mica .............................................................. 55 4.3.1. Indentation Normal to Basal Plane ................................................................... 55 4.3.2. Indentation Parallel to Edge .............................................................................. 55 4.4. Discussion ................................................................................................................. 57 4.5. Conclusion ................................................................................................................ 58 4.6. References ................................................................................................................. 59 Chapter 5. Chemical and Microstructural Characterization of a Hybrid Clay-Lime-Starch Bio Nanocomposite ................................................... 61 5.1. Introduction ............................................................................................................... 61 5.2. Materials and Methods .............................................................................................
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