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An Investigation Into the Structural Design of Polymer Thin Films: from Stimuli Responsive Polyampholyte Brushes to Polymer- Grafted Nanocomposites

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An Investigation Into the Structural Design of Polymer Thin Films: from Stimuli Responsive Polyampholyte Brushes to Polymer- Grafted Nanocomposites University of Tennessee, Knoxville TRACE: Tennessee Research and Creative Exchange Doctoral Dissertations Graduate School 8-2018 An Investigation into the Structural Design of Polymer Thin Films: From Stimuli Responsive Polyampholyte Brushes to Polymer- Grafted Nanocomposites Rachel Irene Ramirez University of Tennessee, [email protected] Follow this and additional works at: https://trace.tennessee.edu/utk_graddiss Recommended Citation Ramirez, Rachel Irene, "An Investigation into the Structural Design of Polymer Thin Films: From Stimuli Responsive Polyampholyte Brushes to Polymer-Grafted Nanocomposites. " PhD diss., University of Tennessee, 2018. https://trace.tennessee.edu/utk_graddiss/5020 This Dissertation is brought to you for free and open access by the Graduate School at TRACE: Tennessee Research and Creative Exchange. It has been accepted for inclusion in Doctoral Dissertations by an authorized administrator of TRACE: Tennessee Research and Creative Exchange. For more information, please contact [email protected]. To the Graduate Council: I am submitting herewith a dissertation written by Rachel Irene Ramirez entitled "An Investigation into the Structural Design of Polymer Thin Films: From Stimuli Responsive Polyampholyte Brushes to Polymer-Grafted Nanocomposites." I have examined the final electronic copy of this dissertation for form and content and recommend that it be accepted in partial fulfillment of the equirr ements for the degree of Doctor of Philosophy, with a major in Chemistry. S. Micheal Kilbey II, Major Professor We have read this dissertation and recommend its acceptance: Ampofo K. Darko, Emmanouil Doxastakis, Bin Zhao Accepted for the Council: Dixie L. Thompson Vice Provost and Dean of the Graduate School (Original signatures are on file with official studentecor r ds.) An Investigation into the Structural Design of Polymer Thin Films: From Stimuli Responsive Polyampholyte Brushes to Polymer-Grafted Nanocomposites A Dissertation Presented for the Doctor of Philosophy Degree The University of Tennessee, Knoxville Rachel Irene Ramirez August 2018 Copyright © 2018 by Rachel I Ramirez ii Dedication This dissertation is dedicated to my loving parents, Ada Caro and Rafael Ramirez, my fiancée Joshua Moncada, my brothers, Luis and Miguel Santiago, and my dog, Maximus. iii Acknowledgements Firstly, I would like to extend my sincerest and everlasting gratitude to my advisor, Prof. S. Michael Kilbey II. His determination, guidance, and encouragement, have molded me into a responsible researcher that can express clear, concise ideas and results. My years in Dr. Kilbey’s lab have been instrumental in my development as a materials scientist, not only filled with professionalism but filled with laughter, as well, that has led to fostering friendships with my group members and with Dr. Kilbey. I will forever be grateful to Dr. Kilbey for his mentorship and friendship as I continue my career. I would also like to acknowledge my family, friends, and colleagues who have supported and encouraged me during my entire journey to receiving my Ph.D. in polymer chemistry at The University of Tennessee. First, I would like to thank my parents, Ada Caro and Rafael Ramirez, for their full support. Even when the road became rocky and I became very discouraged, their encouragement through the hard times and unconditional love are what kept me motivated to move forward. Both of you are not only fantastic parents but incredible people and I can honestly say that I would not be the person I am today without you. I would also like to thank my brothers Luis and Miguel, for offering both words of advice and a kick in the pants when I needed it. I would also like to thank my fiancé Joshua Moncada, who has kept me grounded during the most difficult times in graduate school. His love and support mean more to me than he will ever know. Special thanks go to Dr. Jeremiah Woodcock for providing insight and background on polyampholyte brushes. Dr. John Dunlap of the Advanced iv Microscopy and Imaging Center at The University of Tennessee-Knoxville is gratefully acknowledged for his assistance with atomic force microscopy studies. I truly thank Dr. Xu Wang for establishing the foundation for many polymeric synthetic techniques. Finally, I am grateful to all of the members (past and present) of the Kilbey research group for their friendship, support, advice, and engaging conversations. These members include Jesse Davis, Zach Seibers, Graham Collier, Kamlesh Bornani, Bethany Aden, Dayton Street, Elizabeth O’Connell, Will Ledford, Natalie Czarnecki, and Sina Sabury. This work would not be possible without the financial support from the National Science Foundation and Honeywell. Thank you all for your help. v Abstract Understanding how the structural design of polymer thin films impacts their response to stimuli, such as pH, is crucial for developing systems with targeted attributes to further expand the scope of their applications. These polymer systems can be modified based on the choice of monomers, composition, and structural design, which provides a tunable source for both functionality and tailorability. This tailorability in design gives rise to a wide array of molecular properties that have a significant impact on the macroscopic properties of thin films. This dissertation work aims to provide insight into how the structural design can impact properties on two categories of polymer thin films: copolymer-grafted nanocomposites and polymer brushes. Copolymer nanocomposites were investigated on how the miscibility of the copolymer-grafted nanoparticles can be tuned by using the enthalpic interactions between the graft and the polymer matrix. Changing the overall composition of the copolymer allowed us to drive dispersion of the resulting nanocomposites in the matrix. The copolymer-grafted nanoparticles were synthesized using surface- initiated activators regenerated via electron transfer atom transfer radical polymerization in which poly(methyl methacrylate-r-cyclohexyl methacrylate) was grown from the silica nanoparticle surface and dispersed in a chemically dissimilar polystyrene matrix. An investigation into how the thermomechanical properties of the resulting copolymer-grafted nanocomposites was conducted using fused deposition modeling. vi The second category of polymer thin films examined was polyampholyte brushes in which the impact of modifying the composition on swelling behavior was investigated. Polyampholytes are comprised of charge-positive and charge- negative repeat units, which directly contributes to trade-offs between charge which is externally regulated by solution pH and added salt, and structure. A series of swelling studies were performed to examine how copolymer composition affects structural response of random polyampholyte brushes as pH is changed and betaine, a zwitterion, is added. The work in this dissertation involves the investigation of several types of polymer thin films, the common theme is clarifying how the structural design and composition affects the properties of polymer brushes, both as copolymer-grafted nanocomposites and on planar surfaces. In total, this research provides insight into how polymer design, polymer structure, and behavior responses are associated. vii Table of Contents 1.1: Introduction .................................................................................................... 1 1.1 Universal Importance of Polymer Thin Films .................................................. 2 1.2 Research Objectives ....................................................................................... 4 1.3 Thin Film Copolymer-grafted Nanocomposites ............................................... 8 1.3.1 Miscibility of copolymer-grafted nanoparticles in a chemically dissimilar matrix .......................................................................................................... 8 1.3.2 Overview of fused deposition modeling ........................................... 12 1.3.3 Scaling of polymer grafted-nanoparticles via the grafting “through” approach .................................................................................................. 15 1.4 Polyampholyte Brushes Synthesized via ARGET ATRP .............................. 17 1.5 Organization of Dissertation .......................................................................... 19 Chapter 2: Dispersion of Polymer-grafted Nanoparticles Poly(methyl methacrylate- r-cyclohexyl methacrylate) Synthesized via Surface-initiated ARGET ATRP in a Chemically Dissimilar Matrix ............................................................................... 21 2.1 Abstract ......................................................................................................... 22 2.2 Introduction ................................................................................................... 23 2.3 Experimental Section .................................................................................... 28 2.3.1 Materials and preparations .............................................................. 28 2.3.2 General characterization ................................................................. 28 2.3.3 Synthesis of poly(methyl methacrylate-r-cyclohexyl methacrylate) (P(MMA-r-CHMA)) via ARGET ATRP ...................................................... 29 2.3.4 Synthesis of 3-(2-bromoisobutyramido)propyl(trimethoxy)silane ..... 30 viii 2.3.5 Activation of nanoparticles using 3-(2-bromoisobutyramido)propyl (trimethoxy)silane
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