Thermal Analysis of Polymers Fundamentals and

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.

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	p. ix
Introduction	p. 1
Differential Scanning Calorimetry (DSC)	p. 7
Introduction	p. 7
Elements of Thermodynamics in DSC	p. 9
The Basics of Differential Scanning Calorimetry	p. 18
Purity Determination of Low-Molecular-Mass Compounds by DSC	p. 37
Calibration of Differential Scanning Calorimeters	p. 41
Measurement of Heat Capacity	p. 52
Phase Transitions in Amorphous and Crystalline Polymers	p. 58
Fibers	p. 115
Films	p. 123
Thermosets	p. 130
Differential Photocalorimetry (DPC)	p. 154
Fast-Scan DSC	p. 162
Modulated Temperature Differential Scanning Calorimetry (MTDSC)	p. 168
How to Perform DSC Measurements	p. 208
Instrumentation	p. 217
Appendix	p. 225
Abbreviations	p. 225
References	p. 229
Thermogravimetric Analysis (TGA)	p. 241
Introduction	p. 241
Background Principles and Measurement Modes	p. 242
Calibration and Reference Materials	p. 251
Measurements and Analyses	p. 256
Kinetics	p. 277
Selected Applications	p. 295
Instrumentation	p. 308
Appendix	p. 311
Abbreviations	p. 312
References	p. 314
Thermomechanical Analysis (TMA) and Thermodilatometry (TD)	p. 319
Introduction	p. 319
Principles and Theory	p. 320
Instrumental	p. 326
Calibration	p. 332
How to Perform a TMA Experiment	p. 335
Key Applications	p. 340
Selected Industrial Applications (with Details of Experimental Conditions)	p. 363
Appendix	p. 378
Abbreviations	p. 380
References	p. 381
Dynamic Mechanical Analysis (DMA)	p. 387
Introduction	p. 387
Characterization of Viscoelastic Behavior	p. 394
The Relationship between Time, Temperature, and Frequency	p. 401
Applications of Dynamic Mechanical Analysis	p. 410
Examples of DMA Characterization for Thermoplastics	p. 424
Characteristics of Fibers and Thin Films	p. 432
DMA Characterization of Crosslinked Polymers	p. 438
Practical Aspects of Conducting DMA Experiments	p. 456
Commercial DMA Instrumentation	p. 477
Appendix	p. 488
Abbreviations	p. 489
References	p. 491
Dielectric Analysis (DEA)	p. 497
Introduction	p. 497
Theory and Background of Dielectric Analysis	p. 502
Dielectric Techniques	p. 520
Performing Dielectric Experiments	p. 528
Typical Measurements on Poly(Methyl Methacrylate) (PMMA)	p. 538
Dielectric Analysis of Thermoplastics	p. 553
Dielectric Analysis of Thermosets	p. 576
Instrumentation	p. 592
Appendix	p. 599
Abbreviations	p. 599
References	p. 603
Micro- And Nanoscale Local Thermal Analysis	p. 615
Introduction	p. 615
The Atomic Force Microscope	p. 616
Scanning Thermal Microscopy	p. 618
Thermal Probe Design and Spatial Resolution	p. 620
Measuring Thermal Conductivity and Thermal Force-Distance Curves	p. 624
Local Thermal Analysis	p. 628
Performing a Micro/Nanoscale Thermal Analysis Experiment	p. 633
Examples of Micro/Nanoscale Thermal Analysis Applications	p. 637
Overview of Local Thermal Analysis	p. 644
Abbreviation	p. 647
References	p. 648
Index	p. 651
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Thermal Analysis of Polymers Fundamentals and Applications

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