POLYMER COMPOSITES From Nano- to Macro-Scale
POLYMER COMPOSITES From Nano- to Macro-Scale
POLYMER COMPOSITES From Nano- to Macro-Scale Klaus friedrich Stoyko Fakirov Zhong Zhan ringer
POLYMER COMPOSITES From Nano- to Macro-Scale Klaus Friedrich Stoyko Fakirov Zhong Zhang a - springer
Library of Congress Cataloging-in-Publication Data Friedrich. Klaus. 1945. Polymer composites: from nano-to macro-scale/Klaus Friedrich, Stoyko Fakirov, Zhong Zhang Includes bibliographical references and index. ISBN 10- ISBN10:0-387-26312X(e-book) ISBN13:9780387241760ISBN13:9780387262130 1. Polymeric composites. I. Fakirov, Stoyko Il. Zhang, Zhong, 1968-Ill. Title TA418.96F762005 620.192—dc22 2005050146 Printed on acid-free paper @2005 Springer Science+ Business Media, Inc all rights reserved. This work may not be translated or copied in whole or in part wi s, written permission of the publisher(Springer Science+Business Media, Inc, 233 Spring scholarly analysis. Use in connection with any form of information storage and retrieval electronic adaptation, computer software, or by similar or dissimilar The use in this publication of trade names, trademarks, service marks even if the are not identified as such, is not to be taken as an expression of opinion as to hether or not they are subject to proprietary rights Printed in the United States of America 987654321 SPIN11053842
Library of Congress Cataloging-in-Publication Data Friedrich, Klaus, 1945- Polymer composites: from nano-to-macro-scale/Klaus Friedrich, Stoyko Fakirov, Zhong Zhang. p. cm. Includes bibliographical references and index. ISBN 10: 0-387-24176-0 ISBN 10: 0-387-26312-X (e-book) ISBN 13: 9780387241760 ISBN 13: 9780387262130 1. Polymeric composites. I. Fakirov, Stoyko II. Zhang, Zhong, 1968- III. Title TA418.9.C6F762005 620.1’92—dc22 2005050146 Printed on acid-free paper. ¤ 2005 Springer Science+Business Media, Inc. All rights reserved. This work may not be translated or copied in whole or in part without the written permission of the publisher (Springer Science+Business Media, Inc., 233 Spring Street, New York, NY 10013, USA), except for brief excerpts in connection with reviews or scholarly analysis. Use in connection with any form of information storage and retrieval, electronic adaptation, computer software, or by similar or dissimilar methodology now know or hereafter developed is forbidden. The use in this publication of trade names, trademarks, service marks and similar terms, even if the are not identified as such, is not to be taken as an expression of opinion as to whether or not they are subject to proprietary rights. Printed in the United States of America. 9 8 7 6 5 4 3 2 1 SPIN 11053842 springeronline.com
Contents Preface Editors biographies XIX Part I Nanocomposites: Structure and properties Chapter 1 Carbon Nanotube-Reinforced Polymers: a State 4.1 Comparison of the Multiple-Wall Carbon Nanotubes d o-ootwu of the art review 1 Introduction 2 General Problems in Nanocomposite Technology 3 Experimental 3. 1 Manufacturing of Multiple-Wall Carbon 3.2 Treatment of Carbon Nanotubes 3.3 Matrix Polymers 3.4 Electron Microscopy .5 Dynamic-Mechanical Thermal Analysis 4 Results 4.2 Purification 4.3 CNT/Epoxy Composites: Dis Matrix Bonding, and Functionalization 4.3.1 Dispersion 4.3. 2 Nanotube- Matrix Interactio 4.3.3 Functionalization 4.4 Microscopy 4.4.1 Matrix Bonding to the Nanotubes 4.4.2 Crack Bridging and Telescopic Pull-Outs 4.5 Thermal and Mechanical Properties 4.6 Electrical Properties 011335561824 5 Conclusions 6 Acknowledgements 7 References
Contents Preface Editors Biographies xv xix Part I Nanocomposites: Structure and Properties 1 Chapter 1 Carbon Nanotube-Reinforced Polymers: a State of the Art Review 3 1 Introduction 3 2 General Problems in Nanocomposite Technology 4 3 Experimental 6 3.1 Manufacturing of Multiple-Wall Carbon Nanotubes 6 3.2 Treatment of Carbon Nanotubes 7 3.3 Matrix Polymers 7 3.4 Electron Microscopy 7 3.5 Dynamic-Mechanical Thermal Analysis 8 4 Results 8 4.1 Comparison of the Multiple-Wall Carbon Nanotubes Studied 8 4.2 Purification 10 4.3 CNWEpoxy Composites: Dispersion, Matrix Bonding, and Functionalization 11 4.3.1 Dispersion 11 4.3.2 Nanotube-Matrix Interaction 13 4.3.3 Functionalization 13 4.4 Microscopy 15 4.4.1 Matrix Bonding to the Nanotubes 15 4.4.2 Crack Bridging and Telescopic Pull-Outs 16 4.5 Thermal and Mechanical Properties 17 4.6 Electrical Properties 18 5 Conclusions 21 6 Acknowledgements 2 1 7 References 22
Chapter 2 Application of Non-Layered Nanoparticles in Polymer Modification 2 Surface Treatment and Compounding 2.1 Raw Materials 2.2 Regrafting of the Nanoparticles by Irradiation 2.3 Characterization of the Irradiation Products 8 2.4 Preparation of PP-Based Nanocom and Their Characterization 5 Preparation of Epoxy-Based Nanocomposites and Their Characterization 3 Thermoplastic Systems 3. 1 Effect of Irradiation Grafting Polymerization 3.2 Tensile Properties 3.3 Fractography Thermosetting Sys 4. 1 Interfacial Interactions in the Composites 4.2 Curing behavi riction and wear Performance 5 Conclusions 42 6 Acknowled 7 References Chapter 3 Reinforcement of Thermosetting Polymers by the Incorporation of Micro-and Nanoparticles 4 1 Introduction 2 Manufacturing of Thermosetting Nanocomposites 3 Properties of Nanocomposites 3. 1 Stress-Strain behavior 3.3 Stiffness-lmpact Energy Relationship 3.4 Dynamic Mechanical Properties 3.5 Wear Performance 4 Acknowledgements 670 5 References Chapter 4 Polyimides Reinforced by a Sol-Gel derived Organosilicon Nanophase: Synthesis and Structure-Property Relationships 1 Nanocomposites Based on Flexible-Chain Polymers 63 2 Nanocomposites Based on Semi-Rigid Chain
vi Contents Chapter 2 Application of Non-Layered Nanoparticles in Polymer Modification 1 Introduction 2 Surface Treatment and Compounding 2.1 Raw Materials 2.2 Pregrafting of the Nanoparticles by Irradiation 2.3 Characterization of the Irradiation Products 2.4 Preparation of PP-Based Nanocomposites and Their Characterization 2.5 Preparation of Epoxy-Based Nanocomposites and Their Characterization 3 Thermoplastic Systems 3.1 Effect of Irradiation Grafting Polymerization on the Nanoparticles 3.2 Tensile Properties 3.3 Fractography 4 Thermosetting Systems 4.1 Interfacial Interactions in the Composites 4.2 Curing Behavior 4.3 Friction and Wear Performance 5 Conclusions 6 Acknowledgements 7 References Chapter 3 Reinforcement of Thermosetting Polymers by the Incorporation of Micro- and Nanoparticles 1 Introduction 2 Manufacturing of Thermosetting Nanocomposites 3 Properties of Nanocomposites 3.1 Stress-Strain Behavior 3.2 Impact Behavior 3.3 Stiffness-Impact Energy Relationship 3.4 Dynamic Mechanical Properties 3.5 Wear Performance 4 Acknowledgements 5 References Chapter 4 Polyimides Reinforced by a Sol-Gel Derived Organosilicon Nanophase: Synthesis and Structure-Property Relationships 1 Nanocomposites Based on Flexible-Chain Polymers 2 Nanocomposites Based on Semi-Rigid Chain Polymers (Polyimides)
Content 2.1 In Situ Generation of an Organosilicon Nanophase 67 2.2 Structural Characterization 2.3 Water Uptake 69 2. 4 Thermomechanical Performance 2.5 Dielectric Properties 72 3 Conclusions 4 Acknowled 5 References 74 Chapter 5 Layered Silicate/Rubber Nanocomposites via latex and solution Intercalations I Concept of N 2 Production of Rubber/Clay Nanocomposites 2.1 Latex Intercalation 778 2. 1. 1 Nanocomposites from Rubber Latex 2. 1.2 Nanocomposites from Latex Blend 2.1.3 Radiation- Vulcanized nR La 2.2 Solvent-Assisted Intercalation 4 Acknowledgements 5 Referenc 7889 Chapter 6 Property Improvements of an Epoxy Resin by Nanosilica Particle Reinforcement 1 Introduction and State of the art 91 2 Preparation and Characterization Techniques 2.1 Basic Material Components 2.2 Preparation of Nanosilica-Filled Epoxy Composites 2.3 Structural and Mechanical analysis 3. 1 Microstructure 2.3.2 Viscosity Studies of the Unfilled and Filled Resin 2.3.3 Mechanical Properties 4449955% 2.3, 4 Tribological Properties 2.3.5 Failure Analysis 3 Microstructural and Rheological Details 3.1 Particle Distribution 6689 4 Mechanical Properties 4. 1 Three-Point Bending 4.2 Microhardness 4.3 Fracture Toughness 10l 4.4 Tribological Properties 101
Contents 2.1 In Situ Generation of an Organosilicon Nanophase 2.2 Structural Characterization 2.3 Water Uptake 2.4 Thermomechanical Performance 2.5 Dielectric Properties 3 Conclusions 4 Acknowledgements 5 References Chapter 5 Layered SilicateIRubber Nanocomposites via Latex and Solution Intercalations 1 Concept of Nanoreinforcement 2 Production of RubberIClay Nanocomposites 2.1 Latex Intercalation 2.1.1 Nanocomposites from Rubber Latex 2.1.2 Nanocomposites from Latex Blends 2.1.3 Radiation-Vulcanized NR Latex 2.2 Solvent-Assisted Intercalation 3 Future Issues 4 Acknowledgements 5 References Chapter 6 Property Improvements of an Epoxy Resin by Nanosilica Particle Reinforcement 1 Introduction and State of the Art 2 Preparation and Characterization Techniques 2.1 Basic Material Components 2.2 Preparation of Nanosilica-Filled Epoxy Composites 2.3 Structural and Mechanical Analysis 2.3.1 Microstructure 2.3.2 Viscosity Studies of the Unfilled and Filled Resin 2.3.3 Mechanical Properties 2.3.4 Tribological Properties 2.3.5 Failure Analysis 3 Microstructural and Rheological Details 3.1 Particle Distribution 3.2 Viscosity 4 Mechanical Properties 4.1 Three-Point Bending 4.2 Microhardness 4.3 Fracture Toughness 4.4 Tribological Properties vii 67 68 69 70 72 73 74 74 77 77 78 79 79 8 1 84 87 8 8 88 89 9 1 9 1 94 94 94 95 95 95 95 96 96 96 96 98 99 99 99 101 101 5 Conclusions 103
6 Acki 7 References Part II Special Characterization Methods and modeli 107 Chapter 7 Micro-Scratch Testing and Finite element Simulation of Wear Mechanisn of Polymer Composites 1 Introduction 2 Micro-Scratch Testin 110 The Representative Wear Mechanisms 113 4 Wear Considerations by Finite Element Contact Analysis 114 4. 1 Finite Element Macro/Micro-Contact Models l15 4.2 Normal Fiber Orientation 116 4.3 Parallel Fiber Orientation l18 4.4 Anti-Parallel Fiber Orientation 120 Finite Element Simulation of the Fiber/Matrix Debonding 121 5. 1 Debonding Model and Interface Element 12 22 5. 1.2 Conditions of Debonding 123 5.1.3 Unloading Considerations 125 5.1.4 The Debonding Algorithm 5.2 Calculations for N-Oriented Carbon Fibers in a peeK matrix 6 Conclusions 129 7 Acknowledgements 8 References Chapter 8 Determination of the Interface Strength of Polymer-Polymer Joints by a Curved Interface Tensile Test 133 2 Curved Interface Tensile Test 136 3 Stress Calculation by Finite-Element analysi 3. 1 Flat Interface 3.2 Curved interfac 38 4. 1 Materials and Specimen Preparati 4.2 Tensile Tests and Strain Estimation 4.3 Determination of the Adhesion Strength 5 Conclusions and Outlook
viii 6 Acknowledgements 7 References Contents Part I1 Special Characterization Methods and Modeling 107 Chapter 7 Micro-Scratch Testing and Finite Element Simulation of Wear Mechanisms of Polymer Composites 109 1 Introduction 109 2 Micro-Scratch Testing 110 3 The Representative Wear Mechanisms 113 4 Wear Considerations by Finite Element Contact Analysis 114 4.1 Finite Element Macromicro-Contact Models 115 4.2 Normal Fiber Orientation 116 4.3 Parallel Fiber Orientation 118 4.4 Anti-Parallel Fiber Orientation 120 5 Finite Element Simulation of the FiberMatrix Debonding 121 5.1 Debonding Model and Interface Elements 122 5.1.1 Interface Elements 122 5.1.2 Conditions of Debonding 123 5.1.3 Unloading Considerations 125 5.1.4 The Debonding Algorithm 125 5.2 Calculations for N-Oriented Carbon Fibers in a PEEK Matrix 126 6 Conclusions 129 7 Acknowledgements 130 8 References 130 Chapter 8 Determination of the Interface Strength of Polymer-Polymer Joints by a Curved Interface Tensile Test 1 Introduction 2 Curved Interface Tensile Test 3 Stress Calculation by Finite-Element Analysis 3.1 Flat Interface 3.2 Curved Interface 4 Experimental Observations 4.1 Materials and Specimen Preparation 4.2 Tensile Tests and Strain Estimation 4.3 Determination of the Adhesion Strength 5 Conclusions and Outlook 6 References
Contents Chapter 9 Manufacturing and characterization of Microfibrillar Reinforced Composites from Polymer Blends 1 Introduction 2 Materials, Processing, and Characterization Techniques 151 3 Structure and Properties of MFCs 153 I Structure and Properties of MFCs Based on Pet/PP blends 153 3.1.1 Morphology 3.1. 2 Mechanical Properties of the Drawn Blends After Processing l57 3. 2 Structure and Properties of MFCs Base on LCP/PPe blends 159 3. 2. 1 Morphology 3.2.2 Mechanical Properties of Injection Molded LCP/PPE Blends with MFC Structure 162 4 Conclusions 5 Acknowledgements 6 Refe Chapter 10 Tribological Characteristics of Micro-and Nanoparticle Filled Polymer Composites 169 1 Introductie 169 2 Influence of Particle Size: from Micro- to Nanometer 170 3 Influence of the Nanoparticle Volume Content 171 4 Particle-Filled Polytetrafluoroethylene 174 5 Integration of Inorganic Partic With Traditional Fillers 5. 1 Inorganic Particles and Other Fillers l75 5.2 Combinative Effect of Nanoparticles and Short Carbon Fibers 6 Conclusion 182 7 Acknowledgement 8 References 182 Part Ill Macrocomposite: Processing and Application 187 Chapter 11 Production of Thermoplastic Towpregs and Towpreg-Based Composites 189 1 Introduction 2 Raw Materials 190 3 Production of Towpregs 3. 1 Process and Equipment Description
Contents ix Chapter 9 Manufacturing and Characterization of Microfibrillar Reinforced Composites from Polymer Blends 1 Introduction 2 Materials, Processing, and Characterization Techniques 3 Structure and Properties of MFCs 3.1 Structure and Properties of MFCs Based on PETPP Blends 3.1.1 Morphology 3.1.2 Mechanical Properties of the Drawn Blends After Processing 3.2 Structure and Properties of MFCs Based on LCPIPPE Blends 3.2.1 Morphology 3.2.2 Mechanical Properties of Injection Molded LCPPPE Blends with MFC Structure 4 Conclusions 5 Acknowledgements 6 References Chapter 10 Tribological Characteristics of Micro- and Nanoparticle Filled Polymer Composites 1 Introduction 2 Influence of Particle Size: from Micro- to Nanometer 3 Influence of the Nanoparticle Volume Content 4 Particle-Filled Polytetrafluoroethylene 5 Integration of Inorganic Particles With Traditional Fillers 5.1 Inorganic Particles and Other Fillers 5.2 Combinative Effect of Nanoparticles and Short Carbon Fibers 6 Conclusion 7 Acknowledgement 8 References Part I11 Macrocomposites: Processing and Application Chapter 11 Production of Thermoplastic Towpregs and Towpreg-Based Composites 1 Introduction 2 Raw Materials 3 Production of Towpregs 3.1 Process and Equipment Description
Contents 3.2 Relationships Between Final Properties and Processing Conditions 3. 2.1 Parameters Affecting the Polymer Powder 3. 2.2 Influence of the Processing Conditions on the Final Composite Properties 4 Production of Towpreg-Based Composites 4. 1 Compression Molding 4. 1.1 Process Description 4.1.2 Molding Conditions 4.2 Process Modeling 4445 onso 4.2.2 Non-Isothermal Consolidation 197 4.2.3 Validation of the Consolidation model 200 4.3. 1 Process Description 200 4.3.2 Processing Conditio 4.3.3 Process Modeling 20l 4.4 Filament Winding 2 Processing Co 4.4.3 Relationships Between Final Properties and Processing Conditions 204 4.5 Long Fiber-Reinforced Composite Stamping 4.5.1 Process Description 4.5.2 Processing Conditions 5.1 Mechanical Properties of Continuous Fiber-Reinforced Composites 5.2 Mechanical Properties of Discontinuous Fiber-Reinforced Comp 7 Acknowledgements 211 Chapter 12 Manufacturing of Tailored Reinforcement for Liquid Composite Molding Processes 215 1 Introduction 215 2 Pre-selection of Sewing Thread 2.1 Selection Criteria 217 2.2 Polyester Thread in Global Preform Sewing 3 Tailored Reinforcements 4 Stitching Parameters and Their Influence on the Fiber-Reinforced Polymer Composites 221
Contents 3.2 Relationships Between Final Properties and Processing Conditions 3.2.1 Parameters Affecting the Polymer Powder Deposition 3.2.2 Influence of the Processing Conditions on the Final Composite Properties 4 Production of Towpreg-Based Composites 4.1 Compression Molding 4.1.1 Process Description 4.1.2 Molding Conditions 4.2 Process Modeling 4.2.1 Isothermal Consolidation 4.2.2 Non-Isothermal Consolidation 4.2.3 Validation of the Consolidation Model 4.3 Pultrusion 4.3.1 Process Description 4.3.2 Processing Conditions 4.3.3 Process Modeling 4.4 Filament Winding 4.4.1 Process Description 4.4.2 Processing Conditions 4.4.3 Relationships Between Final Properties and Processing Conditions 4.5 Long Fiber-Reinforced Composite Stamping 4.5.1 Process Description 4.5.2 Processing Conditions 5 Composite Properties 5.1 Mechanical Properties of Continuous Fiber-Reinforced Composites 5.2 Mechanical Properties of Discontinuous Fiber-Reinforced Composites 6 Conclusions 7 Acknowledgements 8 References Chapter 12 Manufacturing of Tailored Reinforcement for Liquid Composite Molding Processes 1 Introduction 2 Pre-selection of Sewing Thread 2.1 Selection Criteria 2.2 Polyester Thread in Global Preform Sewing 3 Tailored Reinforcements 4 Stitching Parameters and Their Influence on the Fiber-Reinforced Polymer Composites
Contents 4.1 Machine Parameters 4. 1. 2 Presser Foot Pressure 223 4.2 Stitching Pattern 224 5 Quality Secured Preforming 225 5. 1 Macro Preform Quality 5.2 Micro Preform Quality 5.3 Fiber Disturbance at seams 226 6 Liquid Composite Molding Process for Net-Shape Preforms 227 6. 1 Preform LCM Process Chain 2 Thermal Behavior of Seam in FrPc 8 Conclusions 9 Acknowledgements 10 References Chapter 13 Deconsolidation and Reconsolidation of Thermoplastic Composites During Processing 233 233 2 Experimental Observations 2. 1 Void growth 235 2.2Mi of Voids 2.3 Squeezed Flow of Resin During Reconsolidation 237 Mechanistic Model of the Void Growth 3. 1 Discussion of the Mechanism 38 3.2 Void-Growth Model 3.3 Theoretical Predictic 244 Thermal/Mechanistic Models of Migration of Voids 246 4.2 Thermal Analysis 246 4.3 Void Closure ueezed Creep Flow of Resin 253 Chapter 14 Long Fiber-Reinforced Thermoplastic Composites in Automotive Applications 255 55 Long Glass Fiber-Reinforced Poly with Mineral fillers 3 Long Fiber-Reinforced Polyamide 66 with Minimized
Contents xi 4.1 Machine Parameters 4.1.1 Thread Tension 4.1.2 Presser Foot Pressure 4.2 Stitching Pattern 5 Quality Secured Preforming 5.1 Macro Preform Quality 5.2 Micro Preform Quality 5.3 Fiber Disturbance at Seams 6 Liquid Composite Molding Process for Net-Shape Preforms 6.1 Preform LCM Process Chain 6.2 Thermal Behavior of Seam in FRPC 7 Quality Management 8 Conclusions 9 Acknowledgements 10 References Chapter 13 Deconsolidation and Reconsolidation of Thermoplastic Composites During Processing 233 1 Introduction 2 Experimental Observations 2.1 Void Growth 2.2 Migration of Voids 2.3 Squeezed Flow of Resin During Reconsolidation 3 Mechanistic Model of the Void Growth 3.1 Discussion of the Mechanism 3.2 Void-Growth Model 3.3 Theoretical Predictions 4 Thermalh4echanistic Models of Migration of Voids 4.1 Discussion of Mechanisms 4.2 Thermal Analysis 4.3 Void Closure 4.4 Squeezed Creep Flow of Resin 5 Conclusions 6 Acknowledgement 7 References Chapter 14 Long Fiber-Reinforced Thermoplastic Composites in Automotive Applications 1 Introduction 2 Long Glass Fiber-Reinforced Polypropylene with Mineral Fillers 3 Long Fiber-Reinforced Polyamide 66 with Minimized Water Absorption 259