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FTIR Results for the Binary Blends of P2VP and Pvph

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FTIR Results for the Binary Blends of P2VP and Pvph MORPHOLOGICAL STUDY OF COMPATIBILIZATION OF IMMISCIBLE POLYMER BLENDS USING A FUNCTIONALIZED BLOCK COPOLYMER A Thesis Presented to The Graduate Faculty of The University of Akron In Partial Fulfillment of the Requirements for the Degree Master of Science Roungrong Thongtan December, 2006 MORPHOLOGICAL STUDY OF COMPATIBILIZATION OF IMMISCIBLE POLYMER BLENDS USING A FUNCTIONALIZED BLOCK COPOLYMER Roungrong Thongtan Thesis Approved: Accepted: ______________________________ ______________________________ Advisor Department Chair Chang Dae Han Sadhan C. Jana ______________________________ ______________________________ Faculty Reader Dean of the College Thein Kyu Frank N. Kelley ______________________________ ______________________________ Faculty Reader Dean of the Graduate School Mark D. Soucek George R. Newkome ______________________________ Date ii ABSTRACT The effectiveness of a functional diblock copolymer in compatibilization of two immiscible homopolymers was investigated. For this study, polystyrene (PS) and poly(2- hydroxyethyl methacrylate) (PHEMA) were used as a pair of immiscible homopolymers, and polystyrene-block-poly(2-vinylpyridine) (S2VP diblock) copolymer was used as a functionalized compatibilizer. The rationale behind the choice of the ternary blend system lies in that the hydroxyl groups in PHEMA and the pyridine groups in the poly(2- vinylpyridine) (P2VP) block of S2VP diblock copolymer are expected to form hydrogen bonds, enhancing the miscibility between the PS and the PHEMA in the ternary blends. Indeed, the presence of specific interactions (hydrogen bonding) between PHEMA and S2VP diblock copolymer was observed via Fourier transform infrared spectroscopy, inducing a diffuse interphase between PS and PHEMA in the ternary blend during melt blending above the order-disorder transition temperature of the diblock copolymer. However, the interphase was not thermally stable. The diblock copolymer in the interphase was driven into the PHEMA-rich phase due to the specific interactions. Micelles of the diblock copolymer formed when its local concentration exceed the critical micelle concentration threshold. iii ACKNOWLEDGEMENTS I would like to express my deepest gratitude to my advisor, Professor Chang Dae Han, for his patience, his never-ending encouragements, and numerous philosophical lessons I have received during the course of my study. I would like to thank Professor Thein Kyu for kind advices and generosity allowing me to use some of his equipments. Also, I want to acknowledge Dr. Weibin Zha for synthesizing the block copolymer used in this research and for his time spent on training me polymer synthesis and microtoming skills. Thanks also go to Cameron Fraser for always be available and promptly helpful on equipment repair and trouble-shooting. Lastly, I would like to thank my family, especially my mother Kunya Thongton, and my dear friends both in Akron and in Thailand for their love and inexhaustible encouragement during the time of happiness and the moment of despair. iv TABLE OF CONTENTS Page LIST OF TABLES ........................................................................................................... vii LIST OF FIGURES ........................................................................................................ viii CHAPTER I. INTRODUCTION ........................................................................................................1 II. BACKGROUND 2.1 Polymer Thermodynamics of Binary Systems ................................................4 2.2 Microphases of Block Copolymers ..................................................................7 2.3 Assessment of Miscibility in Polymer Blend Systems ....................................8 2.4 Compatibilizers ..............................................................................................14 III. LITERATURE REVIEW 3.1 Glass Transition Temperature of Blends with Specific Interactions .............16 3.2 Diblock Copolymer as an Emulsifier .............................................................17 3.3 Nonfunctionalized Diblock Copolymer as a Compatibilizer .........................19 3.4 Functionalized Diblock Copolymer as a Compatibilizer ...............................21 3.5 Characteristics of Block Copolymer/Homopolymer Blends .........................22 3.6 Theories of Phase Structure of Homopolymers/Diblock Copolymer Blends ..........................................................................................................24 IV. EXPERIMENTAL METHODS 4.1 Materials ........................................................................................................32 4.2 Sample Preparation ........................................................................................33 4.3 Characterizations ............................................................................................34 v V. RESULTS AND DISCUSSION 5.1 Phase Behavior of Binary Blends of Homopolymers ....................................37 5.2 Morphology of Binary Blends of Homopolymer and Block Copolymer ......48 5.3 Morphology of PS/PHEMA/S2VP Ternary Blend System ...........................58 VI. CONCLUSIONS AND RECOMMENDATIONS ..................................................69 REFERENCES .................................................................................................................71 APPENDIX .......................................................................................................................78 vi LIST OF TABLES Table Page 1 The sensitivity limit of various polymer characterization techniques for phase separation detection. .........................................................................................9 2 Summary of the molecular characteristics of the polymers investigated in this study characterized by GPC method in THF solvent. Note that PHEMA is insoluble in THF solvent; its Mv is characterized by Aldrich.................34 3 List of blend samples prepared by melt-blending investigated in this study. ...........35 4 List of the thermal properties of the homopolymers measured by DSC and TGA. ..........................................................................................................................35 5 The characteristic interlamellar domain distance of neat S2VP diblock copolymer and the S2VP diblock copolymer in 30/70 PHEMA/S2VP blend...........57 6 List of dimensions: average domain size of PHEMA-rich phase, the average micelle size of the S2VP diblock copolymer, and average thickness of S2VP accumulated on the interfacial region along PHEMA-rich phase measured from TEM images via an image analysis program. ...................................................64 vii LIST OF FIGURES Figure Page 1 Chemical structures of the polymer components in the ternary polymer blend studied in this research.......................................................................................3 2 TGA analysis of materials in air at a heating rate 10 ºC/min without antioxidant..................................................................................................................35 3 DSC thermograms of PS20/PHEMA binary blends during the second heating scan. The tick marks indicate the values of the initial points, midpoints, and the final points of the glass transition. ..............................................38 4 Optical micrograph of 30/70 PS20/PHEMA blend at 23 – 245 °C. There was no change of morphology in such temperature range.........................................38 5 (a) Optical micrograph of 20/80 PS1.5/PHEMA blend at 245 ºC, and (b) TEM micrograph of 70/30 PS20/PHEMA blend prepared by solvent casting. .......................................................................................................................39 6 A schematic representing a formation of an aggregate in the binary blend of PS and PHEMA homopolymers, when PHEMA is a minor component...............40 7 Optical micrograph of 50/50 PS20/P2VP20 blend at 245 ºC. ...................................41 8 The turbidity curve of PS3/P2VP3 blend system observed under 500x using an optical microscope.......................................................................................42 9 Thermal analysis results of P2VP20/PHEMA blends. (a) Thermograms of the blends, (b) Plot of midpoint Tg as a function of weight composition of P2VP20. .....................................................................................................................44 10 IR spectra between 3800 – 2600 cm-1 of P2VP/PHEMA blends measured at 27 °C. Samples prepared by powder method.........................................................46 11 IR spectra between 3800 – 2600 cm−1 of P2VP/PHEMA blends measured at 180 °C. Samples prepared by powder method......................................................47 viii 12 IR spectra showing carbonyl stretching region between 1790 – 1650 cm−1 of P2VP/PHEMA blends measured at 27 °C. Samples prepared by powder method........................................................................................................................48 13 An optical micrograph showing the bicontinuous structure for the blend of PS20 and S2VP block copolymer at the composition 30/70 after being dried. The micrograph was taken at room temperature. The dark area represents S2VP block copolymer, and the white area represents PS20. ..................49 14 TEM image of 30/70 PS20/S2VP blend prepared by solution blending. The dark area represents P2VP block component, and the
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