Thermal Analysis in Polymers Book

Preface ix

1 Introduction Joseph D. Menczel R. Bruce Prime Patrick K. Gallagher 1

2 Differential Scanning Calorimetry (DSC) Joseph D. Menczel Lawrence Judovits R. Bruce Prime Harvey E. Bair Mike Reading Steven Swier 7

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) R. Bruce Prime Harvey E. Bair Sergey Vyazovkin Patrick K. Gallagher Alan Riga 241

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) Harvey E. Bair Ali E. Akinay Joseph D. Menczel R. Bruce Prime Michael Jaffe 319

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

Appendix378

Abbreviations 380

References 381

5 Dynamic Mechanical Analysis (DMA) Richard P. Chartoff Joseph D. Menczel Steven H. Dillman 387

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) Aglaia Vassilikou-Dova Loannis M. Kalogeras 497

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 Valeriy V Gorbunov David Grandy Mike Reading Vladimir V. Tsukruk 615

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

Abbreviation 647

References 648

Index 651