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Information to Users INFORMATION TO USERS This m anuscrit has been reproduced from âie mîcrofîlin master. UMI fflms the text directfy from the original or copy submitted. Thus, some thesis and dissertation croies are in ^pewiiter face, while others may be from axQr type of conqmter printer. The qualify o f this reproduction is dqwmdent upon the quali^ o f the copy submitted. Broken or indistinct print, colored or poor quali^ illustrations and photographs, print bleedthrough, substandard marginq, and inqnoper alignment can adverse^ affect rqxroduction. In the unlikefy event that the author did not send UMI a complete manuscr^’t and there are missing pages, these wûl be noted. Also, if unauthorized copytigiit material had to be removed, a note win indicate the deletiorL Oversize materials (e.g., nuq)s, drawings, charts) are rq»roduced by sectioning the original, beginnmg at the uR)er left-hand comer and continuing from left to i^ it in eqpal sections with small o v erly Eadi original is also photogr^hed in one eqmsure and is included in reduced form at die back of the book. Photographs induded in the original manusoqit have been reproduced xerographically in this copy. Ifigher quality 6" x 9" black and white photogr^hic prints are available for aiy photographs or illustrations appearing in dus copy for an additional charge. Contact UMI directh^ to order. UMI A Bell & Howell information Company 300 North 2 e e b Road. Ann Arbor. Ml 48106-1346 USA 313.'76l-4700 800.521-0600 TRANSIENT SORPTION AND PERMEATION IN FLUOROPOLYMERS DISSERTATION Presented in Partial Fulfillment of the Requirements for the Degree Doctor of Philosophy in the Graduate School of The Ohio State University By Sangwha Lee, B.S., M.S. ***** The Ohio State University 1995 Dissertation Committee: Approved by K. S. Knaebel S. T. Yang Advisôr J. Charmers Department of Chemical Engineering DMI Number: 9526055 UMI Microform 9526055 Copyright 1995, by DMI Company. All rights reserved. This microform edition is protected against unauthorized copying under Title 17, United States Code. UMI 300 North Zeeb Road Ann Arbor, MI 48103 Copyright by Sangwha Lee 1995 (Dedication) To My Parents ACKNOWLEDGEMENTS I express sincere appreciation to Dr. Knaebel for his coherent guidance, patience, and insight throughout the research. Thanks to the other members of my advisory committee, Drs. Yang and Charmers, for their suggestions and comments. To my parents, I thank you for understanding and supporting me all the time. DuPont should be recognized for their financial support, and donation of fluoropolymer resins and other materials. Appreciation is also extended to Mr. D. Roy Groldsbeny, Dr. L. W. Buxton, and Dr. Sina Ebnesajiad for their sincere help and advice. Thanks to God ! in VITA April 26, 1963 .................Bom - Seoul, Korea 1986 .................................. B. S., Seoul National University, Seoul, Korea 1988 .................................. M. S., Seoul National University, Seoul, Korea 1989 -1990 ...................... Researcher, Korean Institute of Science and Technology Seoul, Korea PUBLICATIONS AND CONFERENCE PRESENTATIONS Lee, S. W.. Study on Paraffin Dehvdrocvclization. M.S. Thesis, Seoul National University, Seoul, Korea, 1988. Lee, S. W. and H. I. Lee, Paraffin Dehvdrocvclization over Bimetallic Catalyst (Pu Sn) SuvDorted by y-Alumina. Chemical Engineering Society of Korea, Fall Symposium, Pusan, Korea, Oct.1987. FIELDS OF STUDY Major Field: Chemical Engineering Studies in mass transfer phenomena in fluoropolymer-penetrant system under Dr. Kent S. Knaebel. IV TABLE OF CONTENTS ACKNOWLEDGMENTS.................................................................................................. üi VITA ....................................................................................................................................... iv LIST OF TABLES...............................................................................................................ix LIST OF FIGURES.............................................................................................................xi ABSTRACT........................................................................................................................ xvi CHAPTER PAGE I. INTRODUCTION.................................................................................................... 1 II. TRANSPORT THEORIES IN POLYMER MEMBRANES........................... 8 A. TRANSPORT PROPERTIES................................................................... 8 1. Diffusivity ..................................................................................................... 11 1.1. Activated state theory ................................... 11 1.2. Molecular m odels ............................................................................ 12 1.3. Free volume theory .......................................................................... 14 2. Solubility ....................................................................................................... 20 2.1. Energetic viewpoint ......................................................................... 20 2.2. Thermodynamic sense .....................................................................22 3. Physicochemical nature of components .....................................................25 3.1. Geometric effects of components .................................................. 25 3.2. Electronic factors affecting to penetrants and polymers ..............28 B. FICKIAN DIFFUSION.............................................................................30 1. Diffusion process ......................................................................................... 30 2. General solutions ......................................................................................... 32 2.1. Initial value problem .......................................................................32 2.2. Boundary value problem .................................................................36 2.3. Fickian characteristics......................................................................38 C. NON-FICKIAN DIFFUSION....................................................................40 1. Permeation anomalies ....................................................................................40 2. Sorption anomalies ........................................................................................43 3. Prior mathematical models ........................................................................... 51 3.1. Model equations for continuous morphological change ................52 3.2. Model equations for discontinuous morphological change .......... 57 D. KINETIC TH E O R Y ................................................................................... 63 1. Assumptions and preliminary information .................................................63 2. Development of model equations ................................................................66 2.1. Exponential dependence of rate equation ...................................... 68 2.2. Quadratic dependence of rate equation ..........................................69 3. The characteristic of kinetic model ............................................................. 72 4. Justification of the theory and its limitations ............................................ 80 m . FLUOROPOLYMERS............................................................................................82 A. GENERAL PHYSICAL AND CHEMICAL PROPERTIES 82 B. MOLECULAR STRUCTURE................................................................. 88 C. PROCESSING PROPERTIES................................................................. 94 1. Orientation ...................................................................................................... 94 2. General effects of processing .......................................................................96 D. SPECIFIC APPLICATIONS.....................................................................97 IV. EXPERIMENTAL METHODOLOGY............................................................. 100 A. ORGANIC SOLVENT SELECTIONS................................................ 101 B. EXPERIMENTAL METHODS, APPARATUS AND CONDITIONS................................................................................104 C. ANALYSIS METHODS.......................................................................... 114 1. Computer spreadsheet ................................................................................. 114 2. Statistical analysis ....................................................................................... 115 V. RESULTS AND DISCUSSION...........................................................................116 A. EXPERIMENTAL RESULTS................................................................ 116 1. Sorption characteristic ................................................................................116 1.1. Polymer ty p e ...................................................................................116 1.2. Solvent type ....................................................................................120 VI 1.3. Repeated exposure .........................................................................123 1.4. Orientation ......................................................................................123 1.5. Non-isotropic expansion ............................................................... 127 1.6. Solubility .......................................................................................
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