Thermal Analysis of Polymers

Joseph D. Menczel, PhD, a recognized expert in thermal analysis of polymers with some thirty years of industrial and academic experience, is Assistant Technical Director at Alcon Laboratories. He has researched more than 120 polymeric systems in which he studied calibration of DSCs, glass transition, nucleation, crystallization, melting, stability, mechanical and micro-mechanical properties of polymers, and polymer-water interactions. Dr. Menczel holds six patents and is the author of seventy scholarly papers. He is the author of two chapters in the bookThermal Characterization of Polymeric Materials. In conducting DSC experiments, Dr. Menczel found a crystal/amorphous interface in semicrystalline polymers, which later became known as the rigid amorphous phase. He is also credited with developing the temperature calibration of DSCs for cooling experiments.R. Bruce Prime, PhD, is a consultant to industry and government and a recognized authority on the cure and properties of cross-linked polymer systems. During his thirty-year career with IBM, he led teams responsible for developing and implementing polymer applications for printer and information storage technologies. He holds four patents and is the author of more than fifty technical papers and the chapter on thermosets in Thermal Characterization of Polymeric Materials. Dr. Prime is a Fellow of SPE and NATAS and was the 1989 recipient of the Mettler-Toledo Award in Thermal Analysis. He maintains the Web site www.primethermosets.com.

• Preface ix1 Introduction 1Joseph D. Menczel, R. Bruce Prime and Patrick K. Gallagher2 Differential Scanning Calorimetry (DSC) 7Joseph D. Menczel, Lawrence Judovits, R. Bruce Prime, Harvey E. Bair, Mike Reading, and Steven Swier2.1. Introduction 72.2. Elements of Thermodynamics in DSC 92.3. The Basics of Differential Scanning Calorimetry 182.4. Purity Determination of Low-Molecular-Mass Compounds by DSC 372.5. Calibration of Differential Scanning Calorimeters 412.6. Measurement of Heat Capacity 522.7. Phase Transitions in Amorphous and Crystalline Polymers 582.8. Fibers 1152.9. Films 1232.10. Thermosets 1302.11. Differential Photocalorimetry (DPC) 1542.12. Fast-Scan DSC 1622.13. Modulated Temperature Differential Scanning Calorimetry (MTDSC) 1682.14. How to Perform DSC Measurements 2082.15. Instrumentation 217Appendix 225Abbreviations 225References 2293 Thermogravimetric Analysis (TGA) 241R. Bruce Prime, Harvey E. Bair, Sergey Vyazovkin, Patrick K. Gallagher, and Alan Riga3.1. Introduction 2413.2. Background Principles and Measurement Modes 2423.3. Calibration and Reference Materials 2513.4. Measurements and Analyses 2563.5. Kinetics 2773.6. Selected Applications 2953.7. Instrumentation 308Appendix 311Abbreviations 312References 3144 Thermomechanical Analysis (TMA) and Thermodilatometry (TD) 319Harvey E. Bair, Ali E. Akinay, Joseph D. Menczel, R. Bruce Prime, and Michael Jaffe4.1. Introduction 3194.2. Principles and Theory 3204.3. Instrumental 3264.4. Calibration 3324.5. How to Perform a TMA Experiment 3354.6. Key Applications 3404.7. Selected Industrial Applications (with Details of Experimental Conditions) 363Appendix 378Abbreviations 380References 3815 Dynamic Mechanical Analysis (DMA) 387Richard P. Chartoff, Joseph D. Menczel, and Steven H. Dillman5.1. Introduction 3875.2. Characterization of Viscoelastic Behavior 3945.3. The Relationship between Time, Temperature, and Frequency 4015.4. Applications of Dynamic Mechanical Analysis 4105.5. Examples of DMA Characterization for Thermoplastics 4245.6. Characteristics of Fibers and Thin Films 4325.7. DMA Characterization of Crosslinked Polymers 4385.8. Practical Aspects of Conducting DMA Experiments 4565.9. Commercial DMA Instrumentation 477Appendix 488Abbreviations 489References 4916 Dielectric Analysis (DEA) 497Aglaia Vassilikou-Dova and Ioannis M. Kalogeras6.1. Introduction 4976.2. Theory and Background of Dielectric Analysis 5026.3. Dielectric Techniques 5206.4. Performing Dielectric Experiments 5286.5. Typical Measurements on Poly(Methyl Methacrylate) (PMMA) 5386.6. Dielectric Analysis of Thermoplastics 5536.7. Dielectric Analysis of Thermosets 5766.8. Instrumentation 592Appendix 599Abbreviations 599References 6037 Micro- And Nanoscale Local Thermal Analysis 615Valeriy V Gorbunov, David Grandy, Mike Reading, and Vladimir V. Tsukruk7.1. Introduction 6157.2. The Atomic Force Microscope 6167.3. Scanning Thermal Microscopy 6187.4. Thermal Probe Design and Spatial Resolution 6207.5. Measuring Thermal Conductivity and Thermal Force-Distance Curves 6247.6. Local Thermal Analysis 6287.7. Performing a Micro/Nanoscale Thermal Analysis Experiment 6337.8. Examples of Micro/Nanoscale Thermal Analysis Applications 6377.9. Overview of Local Thermal Analysis 644Abbreviations 647References 648Index 651

"I have read it with great pleasure and it is my honor to provide this short review. Let me congratulate the editors on the concept of this book. They managed to tune the balance between basic principles and practical information finely . . .In conclusion I think that this book is very useful for students, PhDs, and researchers who are dealing or intended to deal with thermal analysis of polymers." (J Therm Anal Calorim, 2010)