Characterization Techniques for Polymer Nanocomposites

The book series "Polymer Nano–, Micro– and Macrocomposites" provides complete and comprehensive information on all important aspects of polymer composite research and development, including, but not limited to synthesis, filler modification, modeling, characterization as well as application and commercialization issues. Each book focuses on a particular topic and gives a balanced in–depth overview of the respective subfield of polymer composite science and its relation to industrial applications. With the books the readers obtain dedicated resources with information relevant to their research, thereby helping to save time and money. With its focus on the characterization of nanocomposites using such techniques as x–ray diffraction and spectrometry, light and electron microscopy, thermogravimetric analysis, as well as nuclear magnetic resonance and mass spectroscopy, this book helps to correctly interpret the recorded data. Each chapter introduces a particular characterization method, along with its foundations, and makes the user aware of its benefits, but also of its drawbacks. As a result, the reader will be able to reliably predict the microstructure of the synthesized polymer nanocomposite and its thermal and mechanical properties, and so assess its suitability for a particular application.

Preface XIII List of Contributors XV 1 Characterization of Nanocomposite Materials: An Overview 1 Vikas Mittal 1.1 Introduction 1 1.2 Characterization of Morphology and Properties 2 1.3 Examples of Characterization Techniques 5 References 12 2 Thermal Characterization of Fillers and Polymer Nanocomposites 13 Vikas Mittal 2.1 Introduction 13 2.2 TGA of Fillers 13 2.3 TGA of Polymer Nanocomposites 23 2.4 DSC of Fillers 25 2.5 DSC of Composites 26 3 Flame–Retardancy Characterization of Polymer Nanocomposites 33 Joseph H. Koo, Si Chon Lao, and Jason C. Lee 3.1 Introduction 33 3.2 Types of Flame–Retardant Nanoadditives 33 3.3 Thermal, Flammability, and Smoke Characterization Techniques 42 3.4 Thermal and Flame Retardancy of Polymer Nanocomposites 46 3.5 Flame Retardant Mechanisms of Polymer Nanocomposites 66 3.6 Concluding Remarks and Trends of Polymer Nanocomposites 68 Acknowledgments 69 References 69 4 PVT Characterization of Polymeric Nanocomposites 75 Leszek A. Utracki 4.1 Introduction 75 4.2 Components of Polymeric Nanocomposites 76 4.3 Pressure–Volume–Temperature ( PVT ) Measurements 79 4.4 Derivatives, Compressibility, and Thermal Expansion Coeffi cient 83 4.5 Thermodynamic Theories 89 4.6 Thermodynamic Interaction Coefficients 100 4.7 Theoretical Predictions 105 4.8 Summary and Conclusions 106 References 109 5 Following the Nanocomposites Synthesis by Raman Spectroscopy and X–Ray Photoelectron Spectroscopy (XPS) 115 Sorina Alexandra Garea and Horia Iovu 5.1 Nanocomposites Based on POSS and Polymer Matrix 115 5.2 Raman and XPS Applied in Synthesis of Nanocomposites Based on Carbon Nanotubes and Polymers 129 Acknowledgments 138 References 138 6 Tribological Characterization of Polymer Nanocomposites 143 Markus Englert and Alois K. Schlarb 6.1 Introduction 143 6.2 Tribological Fundamentals 144 6.3 Wear Experiments 149 6.4 Selection Criteria 152 6.5 Design of Polymer Nanocomposites and Multiscale Composites 153 6.6 Selected Experimental Results 153 References 165 7 Dielectric Relaxation Spectroscopy for Polymer Nanocomposites 167 Chetan Chanmal and Jyoti Jog 7.1 Introduction 167 7.2 Theory of Dielectric Relaxation Spectroscopy 168 7.3 PVDF/Clay Nanocomposites 171 7.4 PVDF/BaTiO3 Nanocomposites 175 7.5 PVDF/Fe3O4 Nanocomposites 177 7.6 Comparative Analysis of PVDF Nanocomposites 181 7.7 Conclusions 182 Acknowledgment 182 Nomenclature 182 References 183 8 AFM Characterization of Polymer Nanocomposites 185 Ken Nakajima, Dong Wang, and Toshio Nishi 8.1 Atomic Force Microscope (AFM) 185 8.2 Elasticity Measured by AFM 193 8.3 Example Studies 201 8.4 Conclusion 225 References 225 9 Electron Paramagnetic Resonance and Solid–State NMR Studies of the Surfactant Interphase in Polymer–Clay Nanocomposites 229 Gunnar Jeschke 9.1 Introduction 229 9.2 NMR, EPR, and Spin Labeling Techniques 230 9.3 Characterization of Organically Modified Layered Silicates 237 9.4 Characterization of Nanocomposites 242 9.5 Conclusion 247 Acknowledgments 248 References 248 10 Characterization of Rheological Properties of Polymer Nanocomposites 251 Mo Song and Jie Jin 10.1 Introduction 251 10.2 Fundamental Rheological Theory for Studying Polymer Nanocomposites 252 10.3 Characterization of Rheological Properties of Polymer Nanocomposites 257 10.4 Conclusions 279 References 280 11 Segmental Dynamics of Polymers in Polymer/Clay Nanocomposites Studied by Spin–Labeling ESR 283 Yohei Miwa, Shulamith Schlick, and Andrew R. Drews 11.1 Introduction 283 11.2 Spin Labeling: Basic Principles 284 11.3 Exfoliated Poly(methyl acrylate) (PMA)/Clay Nanocomposites 286 11.4 Intercalated Poly(ethylene oxide) (PEO)/Clay Nanocomposites 293 11.5 Conclusions 300 Acknowledgments 301 References 301 12 Characterization of Polymer Nanocomposite Colloids by Sedimentation Analysis 303 Vikas Mittal 12.1 Introduction 303 12.2 Materials and Experimental Methods 305 12.3 Results and Discussion 307 12.4 Conclusions 319 Acknowledgments 320 References 320 13 Biodegradability Characterization of Polymer Nanocomposites 323 Katherine M. Dean, Parveen Sangwan, Cameron Way, and Melissa A.L. Nikolic 13.1 Introduction 323 13.2 Methods of Measuring Biodegradation 323 13.3 Standards for Biodegradation 331 13.4 Biodegradable Nanocomposites 331 13.5 Starch Nanocomposites 336 13.6 PCL Nanocomposites 337 13.7 PHA/PHB Nanocomposites 339 13.8 Nanocomposites of Petrochemical–Based Polymer 342 13.9 Conclusions 343 References 343 Index 347

Vikas Mittal is an Assistant Professor at the Chemical Engineering Department of The Petroleum Institute, Abu Dhabi. He obtained his PhD in 2006 in Polymer and Materials Engineering from the Swiss Federal Institute of Technology in Zurich, Switzerland. Later, he worked as Materials Scientist in the Active and Intelligent Coatings section of SunChemical in London, UK and as Polymer Engineer at BASF Polymer Research in Ludwigshafen, Germany. His research interests include polymer nanocomposites, novel filler surface modifications, thermal stability enhancements, polymer latexes with functionalized surfaces etc. He has authored over 40 scientific publications, book chapters and patents on these subjects.