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Dispersion States and Surface Characteristics of Physically Blended Polyhedral Oligomeric Silsesquioxane/Polymer Hybrid Nanocomposites

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Dispersion States and Surface Characteristics of Physically Blended Polyhedral Oligomeric Silsesquioxane/Polymer Hybrid Nanocomposites The University of Southern Mississippi The Aquila Digital Community Dissertations Fall 12-2008 Dispersion States and Surface Characteristics of Physically Blended Polyhedral Oligomeric Silsesquioxane/Polymer Hybrid Nanocomposites Rahul Misra University of Southern Mississippi Follow this and additional works at: https://aquila.usm.edu/dissertations Part of the Materials Chemistry Commons, and the Polymer Chemistry Commons Recommended Citation Misra, Rahul, "Dispersion States and Surface Characteristics of Physically Blended Polyhedral Oligomeric Silsesquioxane/Polymer Hybrid Nanocomposites" (2008). Dissertations. 1154. https://aquila.usm.edu/dissertations/1154 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 DISPERSION STATES AND SURFACE CHARACTERISTICS OF PHYSICALLY BLENDED POLYHEDRAL OLIGOMERIC SILSESQUIOXANE/POLYMER HYBRID NANOCOMPOSITES by Rahul Misra Abstract of a Dissertation Submitted to the Graduate Studies Office of The University of Southern Mississippi in Partial Fulfillment of the Requirements for the Degree of Doctor of Philosophy December 2008 COPYRIGHT BY RAHUL MISRA 2008 The University of Southern Mississippi DISPERSION STATES AND SURFACE CHARACTERISTICS OF PHYSICALLY BLENDED POLYHEDRAL OLIGOMERIC SILSESQUIOXANE/POLYMER HYBRID NANOCOMPOSITES by Rahul Misra A Dissertation Submitted to the Graduate Studies Office of The University of Southern Mississippi in Partial Fulfillment of the Requirements for the Degree of Doctor of Philosophy Approved: December 2008 ABSTRACT DISPERSION STATES AND SURFACE CHARACTERISTICS OF PHYSICALLY BLENDED POLYHEDRAL OLIGOMERIC SILSESQUIOXANE/POLYMER HYBRID NANOCOMPOSITES by Rahul Misra December 2008 Control of dispersion and segregation states of nanostructured additives is one of the biggest challenges in realizing the optimum potential of high performance hybrid polymer nanocomposites. Polyhedral oligomeric silsesquioxane (POSS) nanostructured chemicals, with their hybrid organic-inorganic nature and flexible functionalization with a variety of organic substituents, yield possibilities to control dispersion and tune compatibility in a wide range of polymer systems. The overall goal of this research is to investigate the fundamental parameters that influence the dispersion and segregation states of POSS nanostructured chemicals, and to understand chain dynamics and conformations in physically blended POSS hybrid polymer nanocomposites (HPNC's). Multiple structural and mechanical factors influencing macro to nano scale surface and bulk properties were successfully investigated and correlated. A strategy based on thermodynamic principles for selective control of POSS dispersion states in a given polymer matrix is developed and discussed. This dissertation consists of eight chapters. Chapter 1 provides a detailed introduction about the development and current research interest in POSS/polymer nanocomposites. This chapter also discusses limitations of current advanced nanoprobe techniques. Chapter 2 establishes the overall goal of this research and specific research ii objectives. Chapter 3 establishes the preferential surface migration behavior of physically dispersed, non-reactive, closed cage octaisobutyl POSS (Oib-POSS) in a non- polar polypropylene matrix. Furthermore, influence of POSS surface segregation on the surface properties, especially nano-tribomechanical behavior is also discussed. Chapter 4 expands the studies by melt blending two different types of POSS molecules, a non- reactive, closed cage Oib-POSS and an open cage trisilanolphenyl POSS (Tsp-POSS), in a nylon 6 matrix. This chapter discusses the morphology, nano-dispersion and macro- to nanoscale tribomechanical characteristics in relation to the POSS structures. Chapter 5 probes the molecular miscibility, solution and solid-state chain dynamics in polystyrene solution blended with Oib- and Tsp-POSS based on classical thermodynamic principles. Chapter 6 extends the learnings from chapter 5 to utilize POSS as a dispersion aid to disperse Ti02 nanoparticles in polypropylene. Chapter 7 explores the surface properties of fluorinated and non-fluorinated POSS coated fabrics. Finally, chapter 8 explores a nature-inspired route to modify polymer surfaces utilizing hydrophobin proteins and their impact on surface morphology and nanotribological characteristics. in DEDICATION This dissertation is dedicated to my parents, especially my mother who has been a great source of motivation and inspiration from the beginning of my studies. My father always inspires me to follow my dreams and work hard to realize them. Also, this dissertation is dedicated to my wife who always stood by me and kept my spirit up during my toughest moments. Finally, this dissertation is also dedicated to my beautiful daughter Ayusha who means a world to me. IV ACKNOWLEDGEMENTS I would like to take this opportunity to thank my research advisor Dr. Sarah E. Morgan for her support, guidance, and encouragement throughout my graduate career. I would also like to thank the members of my graduate committee, Dr. Charles E. Hoyle, Dr. Robert Y. Lochhead, Dr. James Rawlins, Dr. Bruce X. Fu, and Dr. Sergei Magonov, for their guidance and valuable suggestions. I am thankful to the entire Morgan research group for their friendship and help throughout my studies, in particular, Alp Alidedeoglu, Chris Harris, Paul Jones, Kristin Hamilton, Brandon Drescher, Bobby Cook, and Chris Collins. I would also like to thank Dr. William Jarrett, Dr. Andreas Plagge, and Sara Bayley who helped me during these studies. In addition, I would like to acknowledge Velda Moore, Heatherly Edgar, Kim Wingo, and Erin Prince for their help. I am also thankful to Dr. Joe Lichtenhan for valuable discussions throughout my research. I am forever grateful to my parents, my wife, and my entire family, all of whom have provided encouragement and support throughout my life. The author also gratefully acknowledges the financial and material support for this research by National Science Foundation and Hybrid Plastics Inc., MS respectively. v TABLE OF CONTENTS ABSTRACT ii DEDICATION iv ACKNOWLEDGEMENTS v LIST OF ILLUSTRATIONS ix LIST OF TABLES xiv CHAPTER I. INTRODUCTION 1 Hybrid Polymer Nanocomposites Classification of Polymer Composites: Advantages and Challenges Polyhedral Oligomeric Silsesquioxane (POSS) Nanostructured Materials Developments in POSS/Polymer HPNC's Current Research Interests in POSS/Polymer HPNC's Thermodynamics of POSS Dispersion Tribology: Friction, Wear, and Adhesion Properties Friction Measurements for Polymeric Surfaces Quasi-static and Dynamic Nanomechanical Properties Motivation and Contribution of Current Research References II. OBJECTIVES OF RESEARCH 38 III. SURFACE ENERGETICS, DISPERSION AND NANOTRIBOMECHANICAL BEHAVIOR OF POSS/PP HYBRID NANOCOMPOSITES 40 Abstract Introduction Experimental Results and Discussion Conclusions Acknowledgements References VI IV. POSS-NYLON 6 NANOCOMPOSITES: INFLUENCE OF POSS STRUCTURE ON SURFACE AND BULK PROPERTIES 80 Abstract Introduction Experimental Results and Discussion Conclusions Acknowledgements References V. TAILORING MOLECULAR MISCIBILITY AND CHAIN DYNAMICS OF POSS/POLYSTYRENE BLENDS: CONTROL OF POSS PREFERENTIAL DISPERSION STATES 119 Abstract Introduction Experimental Results and Discussion Conclusions Acknowledgements References VI. POLYHEDRAL OLIGOMERIC SILSESQUIOXANE (POSS) TRISILANOLS AS DISPERSANTS FOR TITANIUM OXIDE NANOPOWDER 158 Abstract Introduction Experimental Results and Discussion Conclusions Acknowledgements References VII. NON-WETTING, NON-ROLLING, STAIN RESISTANT POLYHEDRAL OLIGOMERIC SILSESQUIOXANE COATED TEXTILES 176 Abstract Introduction Experimental Results and Discussion Conclusions Acknowledgements References vu VIII. NANOSCALE REDUCTION IS SURFACE FRICTION OF POLYMER SURFACES MODIFIED WITH SC3 HYDROPHOBIN FROM SCHIZOPHYLLUM COMMUNE 199 Abstract Introduction Experimental Results and Discussion Conclusions Acknowledgements References CONCLUSIONS AND RECOMMENDED FUTURE WORK 227 vm LIST OF ILLUSTRATIONS Figure I-1. Schematic representation of various hybrid plastics networks 4 1-2. Molecular structure of POSS 7 1-3. Generalized POSS structure: A) open cage, B) closed (condensed) cage 8 1-4. Various molecular architectures obtained via covalent attachment of POSS.... 10 III-l. Schematic structure of Octaisobutyl POSS 45 III-2. Three dimensional AFM tapping mode height images and surface roughness analysis of melt pressed (A) Neat PP (B) 5% Oib-POSS/PP (C) 10% Oib- POSS/PP (Z Scale: 150 nm, Rq: Root mean square roughness, Ra: Mean roughness, Hmax: maximum height) 51 III-3. AFM phase images of melt pressed (A) Neat PP surface (B) 10% Oib-POSS/PP surface, and microtomed (C) Neat PP bulk (D) 10% Oib-POSS/PP bulk 52 III- 4. SEM/EDAX mapping of melt pressed (A) Neat PP surface (B) 10% Oib- POSS/PP Surface and microtomed (C) 10% Oib-POSS/PP Bulk Nanocomposite 54 III-5. TEM-EDAX elemental surface mapping of a microtomed 10% Oib-POSS/PP sample (A) Carbon (B) Oxygen (C) Silicon (D) Silicon Overlap 55 III-6. ATR-FTIR spectra of (A) Oib-POSS (B) Neat PP (C) 5% Oib-POSS/PP (D) 10% Oib-POSS/PP 56 III-7. Variable angle ATR-FTIR spectra of Oib-POSS/PP HPNC 58 III-8. Relative concentration as a function of depth in Oib-POSS/PP HPNC 58 III-9. Friction loops obtained via
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