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Synthesis, Characterization and Surface Modification of Polydimethylsiloxane and Its Composites

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Synthesis, Characterization and Surface Modification of Polydimethylsiloxane and Its Composites University of Massachusetts Amherst ScholarWorks@UMass Amherst Doctoral Dissertations Dissertations and Theses March 2015 Synthesis, Characterization and Surface Modification of Polydimethylsiloxane and Its Composites Yan Wang University of Massachusetts Amherst Follow this and additional works at: https://scholarworks.umass.edu/dissertations_2 Part of the Polymer and Organic Materials Commons Recommended Citation Wang, Yan, "Synthesis, Characterization and Surface Modification of olyP dimethylsiloxane and Its Composites" (2015). Doctoral Dissertations. 332. https://doi.org/10.7275/6388175.0 https://scholarworks.umass.edu/dissertations_2/332 This Open Access Dissertation is brought to you for free and open access by the Dissertations and Theses at ScholarWorks@UMass Amherst. It has been accepted for inclusion in Doctoral Dissertations by an authorized administrator of ScholarWorks@UMass Amherst. For more information, please contact [email protected]. SYNTHESIS, CHARACTERIZATION AND SURFACE MODIFICATION OF POLYDIMETHYLSILOXANE AND ITS COMPOSITES A Dissertation Presented by YAN WANG Submitted to the Graduate School of the University of Massachusetts in partial fulfillment of the degree requirements for the degree of DOCTOR OF PHILOSOPHY February 2015 Polymer Science and Engineering Department 1 © Copyright by Yan Wang 2015 All Rights Reserved ii SYNTHESIS, CHARACTERIZATION AND SURFACE MODIFICATION OF POLYDIMETHYLSILOXANE AND ITS COMPOSITES A Dissertation Presented by YAN WANG Approved as to style and content by: ________________________________ Thomas J. McCarthy, Chair ________________________________ Maria M. Santore, Member ________________________________ Vincent M. Rotello, Member ___________________________ David A. Hoagland, Department Head Polymer Science and Engineering iii To my parents and Wei Zhao iv ACKNOWLEDGMENTS I would like to first thank my advisor, Prof. Thomas J. McCarthy, for all his help and support during the past several years. He is a great advisor and teacher, using both his words and actions to teach me how to become a creative, passionate, independent and collaborative researcher. He taught me how to get inspiration from other fields and generate innovative research ideas, how to systematically solve a problem, and when it is time to close the door on a project. He also provided me with the opportunity to work on both independent and collaborative projects, from which I continuously improve my critical thinking, communication and leadership skills. I acknowledge my two other committee members, Prof. Santore and Prof. Rotello for their valuable suggestions on my PhD thesis work. It is my honor to have such accomplished researchers on my committee. Thanks to all the past and current McCarthy group members, Pei, Peiwen, Joe, Dennis, Fang, Minchao, Connor, Dan, Liming, Satchel and Jack, I have plenty of great memories both inside and outside the lab. I grew a lot both academically and socially with their help. Particularly, I thank Peiwen and Joe, who gave me enormous advice and support at the beginning of my PhD life. I quickly got adapted to the research environment in Amherst, and learned from them how to become a productive researcher. I also want to thank Jack, for all the enjoyable conversations with him about research and life. I appreciate all the help from my collaborators and ‘great helpers’ inside and outside the Polymer Science and Engineering department, including Joe White, Dannielle Ryman, Jiaming Zhuang, Lei Zhang, Michael Beaulieu, Dan King, Yucheng Chen, Polina Ware, Brian Cromer, Connor Evans, Irem Kosif, Wenxu Zhang and Ying Zhou. I would also like to thank all my classmates, all my friends in v the department, and the great softball team members. My friendship with them is a much cherished part of my life in Amherst. I would like to thank MRSEC, CHM, CUMIRP, and Henkel for their financial support. I also thank the staff members including Lisa, Maria, Alyssa, Sekar, Greg and Dave for making my life in Amherst easier. Finally, I especially thank Wei Zhao and my parents. Their unconditional love and support help me overcome many obstacles in my personal and professional life. Therefore, I dedicate this thesis to them. vi ABSTRACT SYNTHESIS, CHARACTERIZATION, AND SURFACE MODIFICATION OF POLYDIMETHYLSILOXANE AND ITS COMPOSITES FEBRUARY 2015 YAN WANG, B.S., TSINGHUA UNIVERSITY M.S., UNIVERSITY OF MASSACHUSETTS AMHERST Ph.D., UNIVERSITY OF MASSACHUSETTS AMHERST Directed by: Professor Thomas J. McCarthy Silicone elastomers are widely employed in composite, coatings, biomedical, sealant and electronics applications. This dissertation highlights new methodologies and formulation approaches to improve the performance of siloxane polymers, including the mechanical properties, surface properties, optical properties and transport properties. It also provides an in-depth understanding about dip-coating deposition on chemically patterned surfaces. The first chapter presents the process of transforming sand into siloxane polymers of excellent mechanical strength. History, properties and applications of siloxane polymers are systematically discussed. Another focus of this chapter is wetting, including the concepts of contact angles and capillary bridge ruptures. Five interconnected projects are discussed following the introduction. Base- catalyzed siloxane equilibration is fully utilized in the first and second projects. First, extremely stretchable silicone elastomers are prepared by copolymerizing silica particles and octamethylcyclotetrasiloxane with siloxane equilibration. It is demonstrated that Stöber silica particles can actively participate in the chemical cross- linking of linear PDMS, serving as SiO4 linking group reservoirs. Second, vii permanently hydrophilic silicones are obtained by grafting PEO-PDMS copolymers to cross-linked silicones via siloxane equilibration. High power light-emitting diodes require a transparent encapsulant of high refractive index and low water permeability. The third project concerns the uniform incorporation of high refractive index inorganic fillers into siloxane polymers. Silicone composites with tailored refractive indices, different molecular structures, tunable mechanical properties and excellent transparency are achieved via sol-gel chemistry. In the fourth project, the high water transport rate in pure silicone is clarified, for both linear and cross-linked silicones. This high water transport rate results from the special structural features of silicone. Incorporation of water-resistant coating layers, silanized fillers and polyimide blocks are shown to be several effective approaches to decrease the water permeability of silicones. The fifth project deals with dip-coating deposition on chemically patterned surfaces. The mechanisms of capillary bridge deformation and rupture for dip-coating deposition on chemically and topographically patterned surfaces are compared. Ordered inorganic and organic individual crystal arrays are successfully patterned on smooth and chemically patterned surfaces prepared by photolithography. viii TABLE OF CONTENTS Page ACKNOWLEDGMENTS .............................................................................................v ABSTRACT ................................................................................................................ vii LIST OF TABLES ..................................................................................................... xiii LIST OF FIGURES .....................................................................................................xv CHAPTER 1 INTRODUCTION .............................................................................................1 1.1 Development of Organosilanes and Siloxane Polymers ..............................1 1.2 Preparation, Properties and Applications of Siloxane Polymers .................3 1.3 Cross-linking of Siloxane Polymers ............................................................6 1.4 Compounding of Siloxane Polymers ...........................................................8 1.5 Contact Angles ...........................................................................................10 1.6 Capillary Bridge Ruptures .........................................................................12 1.7 References ..................................................................................................13 2 SILICA CAN BE AN ACTIVE PARTICIPANT IN CROSS-LINKED SILICONE SYNTHESIS .............................................................................................17 2.1 Introduction ................................................................................................17 2.1.1 Background .................................................................................17 2.1.2 Objectives ...................................................................................19 2.2 Experimental Section .................................................................................19 2.2.1 Sample Preparation .....................................................................19 2.2.2 Fluorescence Microscopy Characterization and Calcination Tests ............................................................................20 2.2.3 Mechanical Properties Characterization .....................................21 2.3 Results and Discussion .............................................................................. 22 2.3.1 Silica Particles Actually Participate in the Cross-linked Silicone Synthesis ..........................................................................22
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