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* Presents a solid introduction to thermal analysis, methods, instrumentation, calibration, and application along with the necessary theoretical background. * Useful to chemists, physicists, materials scientists, and engineers who are new to thermal analysis techniques, and to existing users of thermal analysis who wish expand their experience to new techniques and applications * Topics covered include Differential Scanning Calorimetry and Differential Thermal Analysis (DSC/DTA), Thermogravimetry, Thermomechanical Analysis and Dilatometry, Dynamic Mechanical Analysis, Micro-Thermal Analysis,…mehr
* Presents a solid introduction to thermal analysis, methods, instrumentation, calibration, and application along with the necessary theoretical background. * Useful to chemists, physicists, materials scientists, and engineers who are new to thermal analysis techniques, and to existing users of thermal analysis who wish expand their experience to new techniques and applications * Topics covered include Differential Scanning Calorimetry and Differential Thermal Analysis (DSC/DTA), Thermogravimetry, Thermomechanical Analysis and Dilatometry, Dynamic Mechanical Analysis, Micro-Thermal Analysis, Hot Stage Microscopy, and Instrumentation. * Written by experts in the various areas of thermal analysis * Relevant and detailed experiments and examples follow each chapter.
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Autorenporträt
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.
Inhaltsangabe
Preface ix 1 Introduction 1 Joseph D. Menczel, R. Bruce Prime and Patrick K. Gallagher 2 Differential Scanning Calorimetry (DSC) 7 Joseph D. Menczel, Lawrence Judovits, R. Bruce Prime, Harvey E. Bair, Mike Reading, and Steven Swier 2.1. Introduction 7 2.2. Elements of Thermodynamics in DSC 9 2.3. The Basics of Differential Scanning Calorimetry 18 2.4. Purity Determination of Low-Molecular-Mass Compounds by DSC 37 2.5. Calibration of Differential Scanning Calorimeters 41 2.6. Measurement of Heat Capacity 52 2.7. Phase Transitions in Amorphous and Crystalline Polymers 58 2.8. Fibers 115 2.9. Films 123 2.10. Thermosets 130 2.11. Differential Photocalorimetry (DPC) 154 2.12. Fast-Scan DSC 162 2.13. Modulated Temperature Differential Scanning Calorimetry (MTDSC) 168 2.14. How to Perform DSC Measurements 208 2.15. Instrumentation 217 Appendix 225 Abbreviations 225 References 229 3 Thermogravimetric Analysis (TGA) 241 R. Bruce Prime, Harvey E. Bair, Sergey Vyazovkin, Patrick K. Gallagher, and Alan Riga 3.1. Introduction 241 3.2. Background Principles and Measurement Modes 242 3.3. Calibration and Reference Materials 251 3.4. Measurements and Analyses 256 3.5. Kinetics 277 3.6. Selected Applications 295 3.7. Instrumentation 308 Appendix 311 Abbreviations 312 References 314 4 Thermomechanical Analysis (TMA) and Thermodilatometry (TD) 319 Harvey E. Bair, Ali E. Akinay, Joseph D. Menczel, R. Bruce Prime, and Michael Jaffe 4.1. Introduction 319 4.2. Principles and Theory 320 4.3. Instrumental 326 4.4. Calibration 332 4.5. How to Perform a TMA Experiment 335 4.6. Key Applications 340 4.7. Selected Industrial Applications (with Details of Experimental Conditions) 363 Appendix 378 Abbreviations 380 References 381 5 Dynamic Mechanical Analysis (DMA) 387 Richard P. Chartoff, Joseph D. Menczel, and Steven H. Dillman 5.1. Introduction 387 5.2. Characterization of Viscoelastic Behavior 394 5.3. The Relationship between Time, Temperature, and Frequency 401 5.4. Applications of Dynamic Mechanical Analysis 410 5.5. Examples of DMA Characterization for Thermoplastics 424 5.6. Characteristics of Fibers and Thin Films 432 5.7. DMA Characterization of Crosslinked Polymers 438 5.8. Practical Aspects of Conducting DMA Experiments 456 5.9. Commercial DMA Instrumentation 477 Appendix 488 Abbreviations 489 References 491 6 Dielectric Analysis (DEA) 497 Aglaia Vassilikou-Dova and Ioannis M. Kalogeras 6.1. Introduction 497 6.2. Theory and Background of Dielectric Analysis 502 6.3. Dielectric Techniques 520 6.4. Performing Dielectric Experiments 528 6.5. Typical Measurements on Poly(Methyl Methacrylate) (PMMA) 538 6.6. Dielectric Analysis of Thermoplastics 553 6.7. Dielectric Analysis of Thermosets 576 6.8. Instrumentation 592 Appendix 599 Abbreviations 599 References 603 7 Micro- And Nanoscale Local Thermal Analysis 615 Valeriy V Gorbunov, David Grandy, Mike Reading, and Vladimir V. Tsukruk 7.1. Introduction 615 7.2. The Atomic Force Microscope 616 7.3. Scanning Thermal Microscopy 618 7.4. Thermal Probe Design and Spatial Resolution 620 7.5. Measuring Thermal Conductivity and Thermal Force-Distance Curves 624 7.6. Local Thermal Analysis 628 7.7. Performing a Micro/Nanoscale Thermal Analysis Experiment 633 7.8. Examples of Micro/Nanoscale Thermal Analysis Applications 637 7.9. Overview of Local Thermal Analysis 644 Abbreviations 647 References 648 Index 651
Preface ix 1 Introduction 1 Joseph D. Menczel, R. Bruce Prime and Patrick K. Gallagher 2 Differential Scanning Calorimetry (DSC) 7 Joseph D. Menczel, Lawrence Judovits, R. Bruce Prime, Harvey E. Bair, Mike Reading, and Steven Swier 2.1. Introduction 7 2.2. Elements of Thermodynamics in DSC 9 2.3. The Basics of Differential Scanning Calorimetry 18 2.4. Purity Determination of Low-Molecular-Mass Compounds by DSC 37 2.5. Calibration of Differential Scanning Calorimeters 41 2.6. Measurement of Heat Capacity 52 2.7. Phase Transitions in Amorphous and Crystalline Polymers 58 2.8. Fibers 115 2.9. Films 123 2.10. Thermosets 130 2.11. Differential Photocalorimetry (DPC) 154 2.12. Fast-Scan DSC 162 2.13. Modulated Temperature Differential Scanning Calorimetry (MTDSC) 168 2.14. How to Perform DSC Measurements 208 2.15. Instrumentation 217 Appendix 225 Abbreviations 225 References 229 3 Thermogravimetric Analysis (TGA) 241 R. Bruce Prime, Harvey E. Bair, Sergey Vyazovkin, Patrick K. Gallagher, and Alan Riga 3.1. Introduction 241 3.2. Background Principles and Measurement Modes 242 3.3. Calibration and Reference Materials 251 3.4. Measurements and Analyses 256 3.5. Kinetics 277 3.6. Selected Applications 295 3.7. Instrumentation 308 Appendix 311 Abbreviations 312 References 314 4 Thermomechanical Analysis (TMA) and Thermodilatometry (TD) 319 Harvey E. Bair, Ali E. Akinay, Joseph D. Menczel, R. Bruce Prime, and Michael Jaffe 4.1. Introduction 319 4.2. Principles and Theory 320 4.3. Instrumental 326 4.4. Calibration 332 4.5. How to Perform a TMA Experiment 335 4.6. Key Applications 340 4.7. Selected Industrial Applications (with Details of Experimental Conditions) 363 Appendix 378 Abbreviations 380 References 381 5 Dynamic Mechanical Analysis (DMA) 387 Richard P. Chartoff, Joseph D. Menczel, and Steven H. Dillman 5.1. Introduction 387 5.2. Characterization of Viscoelastic Behavior 394 5.3. The Relationship between Time, Temperature, and Frequency 401 5.4. Applications of Dynamic Mechanical Analysis 410 5.5. Examples of DMA Characterization for Thermoplastics 424 5.6. Characteristics of Fibers and Thin Films 432 5.7. DMA Characterization of Crosslinked Polymers 438 5.8. Practical Aspects of Conducting DMA Experiments 456 5.9. Commercial DMA Instrumentation 477 Appendix 488 Abbreviations 489 References 491 6 Dielectric Analysis (DEA) 497 Aglaia Vassilikou-Dova and Ioannis M. Kalogeras 6.1. Introduction 497 6.2. Theory and Background of Dielectric Analysis 502 6.3. Dielectric Techniques 520 6.4. Performing Dielectric Experiments 528 6.5. Typical Measurements on Poly(Methyl Methacrylate) (PMMA) 538 6.6. Dielectric Analysis of Thermoplastics 553 6.7. Dielectric Analysis of Thermosets 576 6.8. Instrumentation 592 Appendix 599 Abbreviations 599 References 603 7 Micro- And Nanoscale Local Thermal Analysis 615 Valeriy V Gorbunov, David Grandy, Mike Reading, and Vladimir V. Tsukruk 7.1. Introduction 615 7.2. The Atomic Force Microscope 616 7.3. Scanning Thermal Microscopy 618 7.4. Thermal Probe Design and Spatial Resolution 620 7.5. Measuring Thermal Conductivity and Thermal Force-Distance Curves 624 7.6. Local Thermal Analysis 628 7.7. Performing a Micro/Nanoscale Thermal Analysis Experiment 633 7.8. Examples of Micro/Nanoscale Thermal Analysis Applications 637 7.9. Overview of Local Thermal Analysis 644 Abbreviations 647 References 648 Index 651
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