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Polyhedral Oligomeric Silsesquioxane-Phosphate Glass Matrix Nanocomposites with Additional Chapter on Phosphate Glass- Poly(Ethylene Terephthalate) Matrix Composites

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Polyhedral Oligomeric Silsesquioxane-Phosphate Glass Matrix Nanocomposites with Additional Chapter on Phosphate Glass- Poly(Ethylene Terephthalate) Matrix Composites The University of Southern Mississippi The Aquila Digital Community Dissertations Fall 12-1-2018 Polyhedral Oligomeric Silsesquioxane-phosphate Glass Matrix Nanocomposites with Additional Chapter on Phosphate Glass- Poly(ethylene terephthalate) Matrix Composites Kyoungtae Kim University of Southern Mississippi Follow this and additional works at: https://aquila.usm.edu/dissertations Part of the Ceramic Materials Commons, Inorganic Chemistry Commons, Polymer and Organic Materials Commons, and the Polymer Chemistry Commons Recommended Citation Kim, Kyoungtae, "Polyhedral Oligomeric Silsesquioxane-phosphate Glass Matrix Nanocomposites with Additional Chapter on Phosphate Glass-Poly(ethylene terephthalate) Matrix Composites" (2018). Dissertations. 1569. https://aquila.usm.edu/dissertations/1569 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]. POLYHEDRAL OLIGOMERIC SILSESQUIOXANE-PHOSPHATE GLASS MATRIX NANOCOMPOSITES WITH ADDITIONAL CHAPTER ON PHOSPHATE GLASS- POLY(ETHYLENE TEREPHTHALATE) MATRIX COMPOSITES by Kyoungtae Kim A Dissertation Submitted to the Graduate School, the College of Arts and Sciences and the School of Polymer Science and Engineering at The University of Southern Mississippi in Partial Fulfillment of the Requirements for the Degree of Doctor of Philosophy Approved by: Dr. Joshua U. Otaigbe, Committee Chair Dr. Sarah E. Morgan Dr. William L. Jarrett Dr. Derek L. Patton Dr. Joseph D. Lichtenhan ____________________ ____________________ ____________________ Dr. Joshua U. Otaigbe Dr. Jeffrey S. Wiggins Dr. Karen S. Coats Committee Chair Director of School Dean of the Graduate School December 2018 COPYRIGHT BY Kyoungtae Kim 2018 Published by the Graduate School ABSTRACT Preparation and characterization of tin fluorophosphate glass (Pglass) matrix nanocomposites incorporating polyhedral oligomeric silsesquioxane (POSS) were investigated on the structural, thermal, morphological, mechanical, and rheological properties. Various processes including synthesis, extrusion and sintering processes were applied to prepare the nanocomposite samples, and a series of characterizations were performed to enhance a comprehensive understanding of POSS/Pglass system. Another application of POSS with hydrophobic functional groups on the well-structured nanoscale silicate cage with three silanol groups was investigated to present the feasibility to use POSS molecule as a coating material on the surface of the hydrophilic inorganic glass. In addition, Poly(ethylene terephthalate) polymer matrix composites incorporating Pglass was studied to present the benefits of the Pglass with ultra-low glass transition temperature. Obtained nanocomposites via one pot synthesis method using Pglass and trisilanol phenyl POSS (TSP-POSS) showed significant increase of glass transition temperature (Tg) due to the bulky POSS molecules. The synthesized nanocomposites were effectively mixed in the carbon crucible by gases produced during the process, resulting in homogeneous dispersion of POSS in the Pglass matrix, showing transparent optical property and improved rheological, mechanical, and thermal properties. While during the extrusion process mechanical force was used to homogeneously mix the TSP-POSS in the Pglass matrix, determining highly porosity due to the function of a foaming agent of POSS. The studies revealed tunable morphology with respect to the amount of POSS and the extrusion conditions. 29Si Solid state NMR showed that after extrusion process silanol ii groups of TSP-POSS are all consumed by condensation reaction, consistent with the result of NMR analysis using the Pglass matrix nanocomposites prepared by sintering process. POSS molecules effectively were dispersed in the Pglass and chemically reacted with Pglass molecules lead to ingenerate the increase of Tg and increased chemical stability of nanocomposites compared to that of pure Pglass. The novel approach using POSS molecule which is grafting hydrophobic function groups on the core, are utilized to lead increased hydrophobicity of the glass surface. To mimick a lotus leaf with a combination of roughness and low surface energy, the micro- sized Pglass particle and hydrophobic POSS were used. Contact angle of the obtained surface-modified hydrophobic Pglass showed significant improvement compared to bulk pure Pglass. The umbrella effect of the long alkyl chains on bulky POSS core effectively covered the hydrophilic Pglass surface and significantly improved water repellency of the surface of bulk Pglass. In addition, Pglass/PET hybrids were successfully prepared using a mixing process. Various characterizations were performed to understand structure- property correlation in the hybrids with respect to amount of Pglass in the PET and experimental conditions. The investigation of morphological, structural, rheological, and crystallization properties revealed unique properties of Pglass/PET hybrids, attributed to the plasticizer and nucleation effects of polydispersed Pglass particles as well as the increased interfacial interaction between two components in the hybrids. iii ACKNOWLEDGMENTS I would like to thank my advisor, Dr Joshua Otaigbe for providing continuous guidance, support, and encouragement throughout my graduate study and research for PhD. Dr Otaigbe has intellectually inspired me with patience to improve my understanding of my research. Thank you for his whole-hearted mentorship. I would like to thank my other committee members, Dr Morgan, Dr Jarrett, Dr Patton, and Dr Lichtenhan for their valuable scientific discussions and support during my study and research. I am also thankful to Dr Todd Alam at the Sandia National Laboratory for his kind and valuable support at the scientific analysis. I would like to thank the Otaigbe research group, my classmates, friends, and the staff member of the School of Polymer Science and Engineering at University of Southern Mississippi for all of their kind aid and regards. Finally, I would like to thank financial supports from the National Science Foundation (NSF) and the School of Polymer Science and Engineering. iv DEDICATION First and foremost, I would like to thank my wife, Hyunjung, for her sacrifice, understanding, support and invaluable love during my study. I would like to thank my parents for their devotional love and support in the pursuit of my education. I am sure that my father be happy in the heaven. I would like to thank my sons, Kyuryeon and Euiryeon. Their love made me stronger and gave me motivation to go forward continuously. And I would like to thank my brothers, sisters, and their family. v TABLE OF CONTENTS ABSTRACT ........................................................................................................................ ii ACKNOWLEDGMENTS ................................................................................................. iv DEDICATION .................................................................................................................... v LIST OF TABLES ........................................................................................................... xiii LIST OF ILLUSTRATIONS ........................................................................................... xiv CHAPTER I - INTRODUCTION ...................................................................................... 1 1.1 Thesis Organization .................................................................................................. 1 1.2 Literature Review...................................................................................................... 2 1.3 References ............................................................................................................... 15 – SYNTHESIS AND CHARACTERIZATION ON NOVEL PHOSPHATE GLASS MATRIX NANOCOMPOSITES CONTAINING POLYHEDRAL OLIGOMERIC SILSESQUIOXANE WITH IMPROVED PROPERTIES .................... 36 2.1 Introduction ............................................................................................................. 37 2.2 Experimental methods ............................................................................................ 42 Materials and preparation of nanocomposites ................................................. 42 Measurements .................................................................................................. 43 2.2.2.1 Differential Scanning Calorimetry (DSC) ................................................ 43 2.2.2.2 Thermogravimetric analysis (TGA) .......................................................... 44 vi 2.2.2.3 Attenuated total reflectance Fourier transform infrared spectroscopy (ATR-FTIR) .......................................................................................................... 44 2.2.2.4 Atomic force microscopy (AFM) ............................................................. 44 2.2.2.5 X-ray photoelectron spectroscopy (XPS) ................................................. 45 2.2.2.6 Scanning electron microscopy (SEM) - Energy Dispersive X-ray spectroscopy (EDX) .............................................................................................. 45 2.2.2.7 Transmission electron microscopy (TEM) ............................................... 46 2.2.2.8 Melt rheology ...........................................................................................
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