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Polymer Reinforcement-Chemtec Copyright <91995 by ChemTec Publishing ISBN 1-895198-08-9 All rights reserved. No part of this publication may be reproduced, stored or transmitted in any form or by any means without written permission of copyright owner. No responsibility is assumed by the Author and the Publisher for any injury or/and damage to persons or properties as a matter of products liability, negligence, use, or operation of any methods, product ideas, or instructions published or suggested in this book. Printed in Canada ChemTec Publishing 38 Earswick Drive Toronto-Scarborough Ontario MlE lC6 Canada Canadian Cataloguing in Publication Data Lipatov, Yu. S. (Yuri Sergeevich), 1927 Polymer reinforcement Includes bibliographical references and index. ISBN 1-895198-08-9 I. Polymer--Additives. 2. Fillers (Materials). 3. Polymeric composites. I. Title. TP1120.L56 1994 668'.9 C95-900001-1 v To my wife Yuri S. Lipatov i Table of Contents INTRODUCTION 1 References 7 1 THE BASIC THEORIES OF POLYMER ADSORPTION 9 1.1 The main principles of polymer adsorption from dilute solution 10 1.2 Isotherms of polymer adsorption from dilute solutions 13 1.3Thermodynamicinteractionbetweenpolymerandsurface17 1.4TheStructureofadsorptionlayersofpolymers21 1.5Experimentalestimationofthethicknessoflayers30 1.6Adsorptionofpolymersfromsemi-dilutesolutions35 1.7Molecular-aggregativemechanismofadsorption40 1.8 Adsorption from solutions of polymer mixtures 42 1.9Adsorptionofpolymersfrommelts54 References58 2 ADHESION OF POLYMERS AT THE INTERFACE WITH SOLIDS 63 2.1Thermodynamictheoriesofadhesion64 2.2Theoriesofadhesion80 2.3Thetheoryofweakboundarylayers83 2.4Mechanismofadhesionjointformation85 2.5Thestrengthofadhesionjoints90 2.6Howtheadhesionattheinterfacemaybeenhanced?106 References113 ii 3 SURFACE LAYERS OF POLYMERS AT THE INTERFACE WITH SOLIDS 117 3.1 Definitions 117 3.2 Conformations of macromolecules at the polymer-solid interface 121 3.3Molecularpackinginsurfacelayers127 3.4 Methods of evaluation of the fraction of surface layers in filled polymers 134 3.5 Molecular mobility of macromolecules near the interface 136 3.6 Physico-chemical criterion of polymers highly loaded with fillers 144 3.7Microheterogeneityofsurfacelayers148 References 151 4 THERMODYNAMIC AND KINETIC ASPECTS OF REINFORCEMENT 153 4.1 Thermodynamic interaction between polymer and filler 153 4.2 Glass transitions in filled polymers 163 4.2.1 Influence of filler on the glass transition of filled polymers 163 4.2.2 Theoretical approach to glass transition phenomena in filled polymers 165 4.2.3 Structural relaxation in filled polymers near Tg170 4.3 Reinforcement of crystalline polymers 174 4.3.1 Kinetics of crystallization in the filler presence 175 4.3.2 Crystallization in thin layers on the surface 180 4.3.3Meltingoffilledcrystallinepolymers190 4.3.4 Influence of fillers on the morphology and structure of filled crystallizingpolymers192 4.4 Influence of the interface on the reactions of synthesis and mechanismofformationoflinearandnetworkpolymers194 4.4.1 Linear polymers 194 4.4.2 Crosslinked polymers 197 References200 iii 5 VISCOELASTIC PROPERTIES OF REINFORCED POLYMERS 203 5.1 Dependence of the elasticity modulus of particulate-filled polymers on the amount of filler 203 5.2Contributionofinterphaselayerstoviscoelasticproperties215 5.2.1Theoreticalapproach215 5.2.2Resolutionofrelaxationmaximaintwo-phasepolymeric system 219 5.2.3Experimentalevidence223 5.3 Basic principle of temperature-frequency-concentration superposition in reinforced polymers 228 5.4 Influence of the interphase layers on viscoelastic properties 533 5.5 Relaxation spectra of filled polymers 539 5.6 Rheological properties of filled polymers 245 References 251 6 POLYMER ALLOYS AS COMPOSITES 255 6.1 Polymer blends and alloys 255 6.2Thermodynamicsofthemixingofpolymers259 6.3Themechanismsoftheinterphaseformation268 6.3.1Thermodynamicgrounds268 6.3.2 Theories of polymer-polymer interface 273 6.3.3 Experimental data on the thickness and fraction of theinterphaseregions280 6.4 The degree of segregation in polymer alloys with incomplete phaseseparation285 6.5Interpenetratingpolymernetworks288 6.5.1MicrophaseseparationinthecourseofIPNformation291 6.5.2Non-equilibriumstructuresinIPNs295 6.5.3MechanicalpropertiesofIPNs301 6.6 The formation of the phase structure in oligomer-oligomer andoligomer-polymersystems308 References309 iv 7 FILLED POLYMER ALLOYS 313 7.1 Thermodynamic background 313 7.2 Phase state of binary polymer mixtures in presence of fillers 317 7.2.1 Phase diagrams of the systems polymer-polymer-solid 318 7.2.2Thermodynamicinteractionparametersinfilledpolymeralloys324 7.2.3 On kinetics of the phase separation of filled polymer alloys 331 7.2.4 On equilibrium and non-equilibrium compatibilization of polymer alloys 333 7.3 Model representation of a filled polymer alloy 335 7.4 Some properties of filled polymer alloys 339 7.4.1Mechanicalproperties339 7.4.2 Rheological properties 344 7.4.3Adhesion345 7.5 Filled interpenetrating polymer networks 346 7.5.1 Thermodynamic state of filled IPNs 346 7.5.2 Viscoelastic properties of filled LPNs 352 References 357 8 CONCLUDING REMARKS ON THE MECHANISM OF REINFORCING ACTION OF FILLERS IN POLYMERS 361 8.1 Role of polymer-filler bonds in reinforcement 362 8.2 Mechanism of reinforcement of rubber-like polymers 365 8.3 Reinforcement of thermoplastics and thermosets 373 8.4 Non-equilibrium state of polymer composite materials 380 References387 EPILOGUE390 NOMENCLATURE 391 INDEX 403 vii No one scientific truth is given in direct experiment. The direct experiment itself is the result of speculation. Vladimir Solovjev FOREWORD Polymeric composite materials have been known since ancient times. To create modern composites, it is necessary to use the fundamental principles of organic and inorganic chemistry, polymer chemistry, physical chemistry, phys- ics and mechanics of solid and polymers. In this monograph the author presents only one aspect of the problem, namely a physico-chemical one, as being the most general and typical of all the variety of modern composites. The materials included are polymers filled with particulate fillers, fiber-reinforced plastics, and polymer alloys and blends. The most common feature of all these materials is that they are heterogeneous multicomponent systems whose properties are not a sum of properties of constituent components. For more than 35 years, the author of this monograph has developed and attempted to prove experimentally the ideas according to which the main role in properties of composite materials belongs to the surface phenomena at the poly- mer-solid interface. Author believes that all the development of the physical chemistry of filled polymers confirms this idea. This book is dedicated chiefly to the analysis of surface and interphase phenomena in filled polymers and their contribution to the physical and mechanical properties of composites. The ad- vantage of such an approach is in its ability to describe the properties of all types of composites, namely those filled with disperse organic and inorganic fillers, re- inforced by organic and inorganic, including metallic fibers, where the matrix is viii formed by rubbers, thermoplasts, elastoplasts and reactoplasts. The details of the mechanisms of reinforcement may be different in each case but the physico-chemical principles remain valid, since they are based on the analysis of the interfacial phenomena. The above principles predetermined the structure of this book. Separate chapters are dedicated to the most fundamental principles of surface phenom- ena in polymers and to properties of the surface polymer layers at the interface with a solid. One can assert with confidence that fundamental principles of physico-chemical theory of filling of polymers include the theory of adsorption at the polymer-solid interface, adhesion to the surface, and the theory of behavior of surface or border polymer layers at the interface. In this monograph, I have used both theoretical and experimental data pre- sented in literature and experimental data and approaches developed by this author and his coworkers. Clearly, the development of any branch of science leads to the necessity to renounce some points of view developed earlier in order to formulate new, more precise theories. “In science, the only statements that have value are those which allow us to doubt their validity” - Valery Bryusov (1873 -1924). “For us, the freedom of the search of truth is the greatest value, even if it may lead to the collapse of all our ideals and beliefs”. Citing these words I would like to emphasize that other approaches and opinions are always wel- come. Finally, I wish to express my thanks and appreciation to many without whom this book could not be written. First to my wife, who, despite her own ac- tivity in polymer chemistry, helped, supported, and inspired me with her love and tenderness. Her advice to me has always been very fruitful and full of good- will. My warmest thanks to my collaborators at the Institute of Macromolecular Chemistry, Prof. Valery Privalko, Dr. Anatoly Nesterov, Dr. Tamara Todosiychuk, Dr. Valentin Babich, and Dr. Valery Rosovitsky for numerous dis- cussions. They provided many ideas, as well as the results, that are incorporated in this book. My sincere thanks to Dr. S. Lipatov (Kiev) and Mr. P. M. Oleshkevych (To- ronto) for their helpful assistance in preparing the computer version of this book. Yuri S. Lipatov Kiev, 1989-1994 Y. Lipatov 1 INTRODUCTION The reinforcement of linear and crosslinked polymers is
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