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Nanodiamond Composites Nanodiamond–Polymer Composites A thesis submitted to the faculty of Drexel University by Ioannis Neitzel In partial fulfillment of the requirements for the degree of Doctor of Philosophy July 2012 i © Copyright 2012 Ioannis Neitzel. All rights reserved. ii Dedications To my family, who has always supported and believed in me. Thank you for being understanding, challenging, inspiring and loving. iii ACKNOWLEDGEMENTS First and foremost I would like to thank my advisor, Dr. Yury Gogotsi and co-advisor Dr. Vadym Mochalin, who dedicated time and patience to teach me how to be a successful researcher. Their encouragement, inspiration and support enabled me to proceed through my doctorate studies and complete my dissertation. Also, I would like to thank my committee members Dr. Giuseppe R. Palmese, Dr. Caroline Schauer, Dr. Mark Vanlandingham and Dr. Steven May for their thoughtful advice and time. I am also thankful to Dr. Chris Li who took part in my Ph.D. candidacy exam. Working with Dr. Bastian Etzold was a great pleasure and I am thankful for his inspiration and support. Special thanks go to Dr. Isabel Knoke, Dr. JunJie Niu, Dr. Antonios Kontsos and Dr. Qingwei Zhang, for showing me the value of collaboration. Thanks go to the Nanomaterials and Palmese research group at Drexel University, especially to Riju Singhal, Amanda Pentecost, Amy Peterson and James Throckmorton for their help with experimental work and to Danielle Tadros and Jill Buckley for their help with administrative work. I also wish to thank our collaborators at the University of Pennsylvania and the Argonne National Labs, Dr. Jason Bares, Dr. Robert Carpick and Dr. Ali Erdemir as well as Dr. Senli Guo and Dr. Sergei Kalinin from the Oak Ridge National Laboratories for their help with AFM measurements. Thanks to Dr.Shahram Amini from the United Technology Research Center for establishing and cultivating a productive collaboration. I would also like to thank the faculty and staff of the Materials Science and Engineering Department and College of Engineering, especially Yenneeka Long, Dorilona Rose, Keiko Nakazawa, Sarit Kunz and Andrew Marx, who were always helpful. iv TABLE OF CONTENTS List of tables ........................................................................................................................... viii List of Figures ............................................................................................................................ ix Abstract .................................................................................................................................. xxii 1 Introduction ..................................................................................................................... 1 2 Literature review .............................................................................................................. 3 2.1 Introduction to polymer nanocomposites – Potential & Challenges .......................... 3 2.1.1 Polymer nanocomposite - theories and models .................................................. 6 2.1.1.1 Theories and modeling of polymer nanocomposites ..................................... 7 2.1.1.2 Predicting Young’s modulus of polymer nanocomposites ............................. 9 2.1.1.2.1 Predicting composite Young’s modulus using different models ............. 9 2.1.1.2.2 Young’s modulus in dependence of dispersion and agglomeration ..... 13 2.1.2 Recent developments in polymer nanocomposites .......................................... 16 2.2 Polymer matrices ....................................................................................................... 17 2.2.1 Thermoplastic and elastomeric polymer matrices ............................................ 17 2.2.2 Thermosetting polymer matrices ...................................................................... 18 2.3 Nanofillers for polymer composites .......................................................................... 19 2.3.1 Carbon nanomaterials as fillers ......................................................................... 20 2.3.1.1 Carbon Nanotubes (CNTs) ............................................................................ 20 2.3.1.2 Graphene ...................................................................................................... 21 2.3.1.3 Nanodiamond ............................................................................................... 21 2.3.1.3.1 Surface treatments for nanodiamond ................................................... 23 2.3.1.4 Other carbon nanomaterials ........................................................................ 30 2.3.2 Strategies for nanofiller dispersion .................................................................... 30 2.4 Polymer-nanodiamond composites ........................................................................... 32 2.4.1 Mechanical properties ....................................................................................... 33 2.4.1.1 Thermoplast-nanodiamond composites ...................................................... 33 2.4.1.1.1 Thermoplastic-ND composites for biomedical applications ................. 38 2.4.1.1.2 Synergetic effects of ND in reinforcing thermoplastic co-polymers ..... 43 2.4.1.2 Thermoset-nanodiamond composites ......................................................... 44 2.4.1.3 Elastomer-nanodiamond composites .......................................................... 45 2.4.2 Thermal properties of polymer-nanodiamond composites .............................. 46 v 2.4.2.1 Thermal stability of polymer-ND composites .............................................. 46 2.4.2.2 Thermal conductivity of polymer-ND composites ....................................... 47 2.4.3 Optical properties of polymer-nanodiamond composites ................................ 48 2.4.4 Electromagnetic shielding of polymer-ND composites ...................................... 50 2.4.5 Other applications for polymer-ND composites ................................................ 51 2.5 Summary .................................................................................................................... 52 2.6 Objectives................................................................................................................... 53 3 Materials and Methods .................................................................................................. 54 3.1 Materials .................................................................................................................... 54 3.1.1 Polymer matrices ............................................................................................... 54 3.1.1.1 The epoxy system Epon828/PACM .............................................................. 54 3.1.1.2 The thermoplastic polymer matrix Poly(L-lactic acid) .................................. 56 3.1.2 Nanodiamond .................................................................................................... 57 3.1.2.1 As received nanodiamond ............................................................................ 57 3.1.2.2 Purification of nanodiamond ....................................................................... 58 3.1.2.3 Aminated nanodiamond............................................................................... 58 3.1.2.4 Octadecylamine functionalized nanodiamond ............................................ 63 3.1.3 Manufacturing polymer-ND composites ........................................................... 65 3.1.3.1 Epoxy-nanodiamond composites ................................................................. 65 3.1.3.1.1 Epoxy-nanodiamond (as received) composites .................................... 65 3.1.3.1.2 Epoxy-nanodiamond (aminated) composites ....................................... 66 3.1.3.2 PLLA-ND composites .................................................................................... 67 3.2 Methods ..................................................................................................................... 67 3.2.1 Characterization of nanodiamond and nanodiamond-composites ................... 67 3.2.2 Mechanical characterization .............................................................................. 68 3.2.2.1 Mechanical testing of macroscale samples .................................................. 68 3.2.2.1.1 Compression and tensile testing ........................................................... 68 3.2.2.1.2 Fracture toughness tests using compact tension specimen ................. 69 3.2.2.1.3 Vickers indentation ............................................................................... 70 3.2.2.1.4 Pin-on-disk tribology tests ..................................................................... 70 3.2.2.2 Microscale mechanical testing ..................................................................... 71 3.2.2.2.1 Nanoindentation ................................................................................... 71 3.2.2.3 Nanoscale characterization using Atomic Force Microscopy....................... 78 vi 3.2.2.3.1 Probing octadecylamine functionalized nanodiamond ........................ 78 3.2.2.3.2 Probing epoxy-nanodiamond composites ............................................ 79 3.2.3 Other characterization techniques .................................................................... 80 3.2.3.1 Differential Scanning Calorimetry ................................................................ 80 3.2.3.2 Thermogravimetric
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