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Synthesis of Polyhedral Oligomeric Silsesquioxane (POSS) Functionalized Carbon Nanotubes for Improved Dispersion in Polyurethane Films

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Synthesis of Polyhedral Oligomeric Silsesquioxane (POSS) Functionalized Carbon Nanotubes for Improved Dispersion in Polyurethane Films The University of Southern Mississippi The Aquila Digital Community Dissertations Spring 5-2013 Synthesis of Polyhedral Oligomeric Silsesquioxane (POSS) Functionalized Carbon Nanotubes for Improved Dispersion in Polyurethane Films Xiaonan Kou University of Southern Mississippi Follow this and additional works at: https://aquila.usm.edu/dissertations Part of the Polymer Chemistry Commons Recommended Citation Kou, Xiaonan, "Synthesis of Polyhedral Oligomeric Silsesquioxane (POSS) Functionalized Carbon Nanotubes for Improved Dispersion in Polyurethane Films" (2013). Dissertations. 705. https://aquila.usm.edu/dissertations/705 This Dissertation is brought to you for free and open access by The Aquila Digital Community. It has been accepted for inclusion in Dissertations by an authorized administrator of The Aquila Digital Community. For more information, please contact [email protected]. The University of Southern Mississippi SYNTHESIS OF POLYHEDRAL OLIGOMERIC SILSESQUIOXANE (POSS) FUNCTIONALIZED CARBON NANOTUBES FOR IMPROVED DISPERSION IN POLYURETHANE FILMS by Xiaonan Kou Abstract of a Dissertation Submitted to the Graduate School of The University of Southern Mississippi in Partial Fulfillment of the Requirements for the Degree of Doctor of Philosophy May 2013 ABSTRACT SYNTHESIS OF POLYHEDRAL OLIGOMERIC SILSESQUIOXANE (POSS) FUNCTIONALIZED CARBON NANOTUBES FOR IMPROVED DISPERSION IN POLYURETHANE FILMS by Xiaonan Kou May 2013 Carbon nanotube (CNT) polymer nanocomposites are promising advanced materials. These materials exhibit the advantages of traditional polymeric materials, such as being light weight and easy to process, combined with the potential to exhibit enhanced mechanical, thermal and electrical properties compared to pure polymers. To achieve substantial improvement of composite properties at low CNT loading, uniform dispersion of CNTs in the polymer matrix and strong CNT-polymer interfacial interaction are needed. However, it is difficult to achieve adequate dispersion and interfacial interactions due to the inert nature of CNTs. In this project, polyhedral oligomeric silsequioxane (POSS) will be used as a dispersing agent for multi-walled carbon nanotubes (MWNTs) in polyurethane (PU) matrices. This dissertation consists of six chapters. Chapter I provides a detailed introduction of the fundamental knowledge of CNTs, PU, and POSS. At the end of this chapter, the motivation and rationale of this research are given. Chapter II establishes the overall goal and specific objectives of this research. Chapter III describes the synthesis and characterization of three POSS modified CNTs and one organosilane modified CNT. Grafting efficiency of the different grafted molecules are calculated and compared. Chapter IV discusses the dispersion behavior of four covalently modified CNTs in both ii solvents and PU matrices. Differences in dispersion behaviors of the modified CNTs are correlated to the solubility parameters of the grafting molecules and the surface structures of modified CNTs. Chapter V provides further discussion of the dispersion of POSS and silane modified CNTs by reviewing the assessment of the physical properties of PU composites containing the modified CNTs. Morphological, thermal, mechanical and electrical properties are used to estimate the interactions of the modified CNTs with the PU matrix. Chapter VI explores the function of the trisilanolphenyl POSS lithium salt (TSPLi) as a dispersant for CNTs in thermoplastic polyurethane (TPU) during melt extrusion. The dispersion of CNTs and TSPLi modified CNTs are estimated by mechanical and electrical property measurement of the PU/CNT and PU/CNT-POSS composites. iii COPYRIGHT BY XIAONAN KOU 2013 The University of Southern Mississippi SYNTHESIS OF POLYHEDRAL OLIGOMERIC SILSESQUIOXANE (POSS) FUNCTIONALIZED CARBON NANOTUBES FOR IMPROVED DISPERSION IN POLYURETHANE FILMS by Xiaonan Kou A Dissertation Submitted to the Graduate School of The University of Southern Mississippi in Partial Fulfillment of the Requirements for the Degree of Doctor of Philosophy Approved: _Sarah E. Morgan______________________ Director _Robert Y. Lochhead____________________ _Derek L. Patton________________________ _James W. Rawlins______________________ _J. Paige Buchanan______________________ _Susan A. Siltanen______________________ Dean of the Graduate School May 2013 ACKNOWLEDGMENTS First I would like to express my greatest gratitude to my two advisors, Dr. Morgan and Dr. Lochhead, for their consistent encouragement and support. I also want to acknowledge my other committee members, Dr. Rawlins, Dr. Buchanan and Dr. Patton for their guidance. I would like to thank everyone in both Morgan’s group and Lochhead’s group for their valuable friendship, in particular, Dr. Chris Sahagun, Dr. Bobby Cook, Dr. Mithun Bhattacharya, Lea Paslay, Sarah Exley, Elana Lewis, Yuhong Wei, Yan Zong, Qi Wu, Katrina Knauer, Matthew Williams, Robert Boswell, Vipul Padman, and Tylor Bryd. I would also like to give my gratitude to other people who helped me with my research, especially Yingji Wu, Lawrence LaBeaud, Jinhai Yang, Amber Windham, Jessica Douglas, and Dr. Ken Curry. I’m grateful to Hybrid Plastics. Inc. for the helpful discussions on my research and use of their laboratory facilities. In particular, I would like to thank Dr. Joe Lichtenhan, Dr. Joe Schwab, Dr. Gregory Brust, Zack Kemp and Mike Carr. I want to acknowledge the coating lab in polymer science for their help in coating formulation and testing. I would also like to acknowledge Bayer Corporation, Lubrizol Corporation for providing free samples for this project. Finally I want to give thanks to my family and all the great friends I made here, for having faith in me during my hardest time. iv TABLE OF CONTENTS ABSTRACT ............................................................................................................................... ii ACKNOWLEDGMENTS .......................................................................................................... iv LIST OF TABLES .................................................................................................................... vii LIST OF ILLUSTRATIONS ................................................................................................... viii LIST OF EQUATIONS ............................................................................................................ xii LIST OF ABBREVIATIONS .................................................................................................. xiv CHAPTER I. INTRODUCTION .............................................................................................. 1 Carbon Nanotubes (CNTs) Polyurethane (PU) Polyhedral Oligomeric Silsesquioxane (POSS) Motivation and Contribution of the Research References II. OBJECTIVES OF RESEARCH ....................................................................... 29 III. SYNTHESIS AND CHARACTERIZATION OF POSS MODIFED CARBON NANOTUBES ................................................................................................. 30 Abstract Introduction Experimental Results and Discussion Conclusions Acknowledgments References IV. DISPERSION OF POSS MODIFED CARBON NANOTUBES IN SOLVENTS AND POLYURETHANE FILMS ................................................ 54 Abstract Introduction Experimental Results and Discussion Conclusions Acknowledgments References v V. PROPERTIES OF THERMOPLASTIC POLYURETHANE COMPOSITES WITH POSS MODIFIED CARBON NANOTUBES ........................................ 84 Abstract Introduction Experimental Results and Discussion Conclusions Acknowledgments References VI. TRISILANOLPHENYL POSS LITHIUM SALT (TSPLI) AS A DISPERSANT FOR CARBON NANOTUBES IN THERMOPLASTIC POLYURETHANE ........................................................................................ 112 Abstract Introduction Experimental Results and Discussion Conclusions Acknowledgments References VII. CONCLUSIONS AND RECOMMENDED FUTURE WORK ....................... 134 vi LIST OF TABLES Table 1. Structure Parameters of POSS and APTS Measured in MD Simulation (in nm) ............................................................................................................ 38 2. POSS Grafting Density Calculation of CNT-g-POSS and CNT-g-silane Based on TGA ................................................................................................. 42 3. Successive Procedure for AC Energy Minimization ......................................... 58 4. Hildebrand Solubility Parameter Calculation of POSS and Silane (in (J/cm3)1/2) Used in This Project ................................................................... 62 5. Hansen Solubility Parameters of Good and Poor Solvents of POSS Molecules in This Project ((J/cm3)1/2) ............................................................... 63 6. Peak Analysis of DTGA Traces of Neat PU, PU/CNT and PU/CNT-g-APIB Composites ...................................................................................................... 77 7. Calculation of Degree of Phase Separation of TPU/CNT-g-POSS by IR Results ............................................................................................................. 92 8. DSC Results of the Heat-Cool-Heat Ramp of TPU/CNT-g-POSS samples ....... 98 vii LIST OF ILLUSTRATIONS Figure 1. Various Allotropes of Carbon (A) Graphene Sheet, (B) C60 Fullerene, (C) Open-ended SWNT, and (D) MWNT ........................................................... 2 2. A Schematic of the Percolation Phenomenon and
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