Modulated Temperature Differential Scanning Calorimetry: Theoretical and Practical Applications in Polymer Characterisation (Hot Topics in Thermal Analysis and Calorimetry)

Cover Page......Page 1
Title Page......Page 4
ISBN 140203749X......Page 5
Contents......Page 6
Foreword......Page 12
1 Introduction......Page 15
2.1 Some Preliminary Observations on Heat Capacity......Page 16
2.2 The MTDSC Experiment and Deconvolution Procedure......Page 18
3.2 Selection of Experimental Parameters......Page 27
3.4 Chemical Reactions and Related Processes......Page 30
3.5 The Glass Transition......Page 37
3.6 Melting......Page 52
3.7 Calibration......Page 64
3.8 Overview......Page 68
4.2 Modulation and Deconvolution......Page 69
4.3 Chemical Reactions and Related Processes......Page 70
4.4 Frequency Dependent Heat Capacity and the Glass Transition......Page 75
4.5 Melting......Page 80
4.6 Calibration......Page 83
References......Page 94
1 Introduction......Page 97
2.1 General Aspects of Polymer Network Formation......Page 99
2.2 Cure Reaction Mechanism......Page 101
2.3 Mechanistic Versus Empirical Cure Rate Law......Page 105
2.4 Specific Versus Overall Diffusion Control......Page 107
3.1 Gelation......Page 108
3.2 Vitrification and the Glass Transition......Page 109
3.3 Conversion and Conversion Rate......Page 110
3.4 Diffusion Effects During Cure......Page 111
4.1 General Considerations for Accurate Kinetic Analysis......Page 112
4.2 MTDSC Parameters......Page 115
5.1 Experimental Systems......Page 116
5.2 Remarks Concerning MTDSC Signals......Page 117
5.3 Isothermal Cure with Vitrification......Page 119
5.4 Non-Isothermal Cure with Vitrification and Devitrification......Page 126
5.5 Combined Cure Paths......Page 130
5.6 Slow Isothermal Cure......Page 132
5.7 Partial Vitrification......Page 135
5.8 Mobility Factor to Quantify Degree of Vitrification......Page 137
5.9 Heat Capacity Change as a Result of Reaction Before Vitrification......Page 138
5.10 Reaction-Induced Phase Separation......Page 141
6.1 Proposed Model......Page 143
6.2 Optimised Cure Rate Law......Page 147
6.3 Remarks Concerning the Proposed Model and Literature Models......Page 153
6.4 Remarks Concerning the Frequency Dependence of Heat Capacity During Cure......Page 154
7.1 Validation of the T[sub(g)] – x Model......Page 156
7.2 ΔC[sub(p)] and ΔT[sub(g)] at T[sub(g)] as a Function of Conversion......Page 158
8.1 MTDSC Calculation Procedure......Page 159
8.2 Influence of Chemical Structure on the (De)vitrification Behaviour of the Thermosetting Systems......Page 167
9 Conclusions and Future Developments......Page 168
References......Page 170
1 Introduction......Page 175
2 Heat Capacity and its Differential with Temperature Signal Over the Glass Transition Region......Page 179
3 Measurements of the Glass Transition Temperature and Increment of Heat Capacity......Page 180
4.1 Improvement in the Measurement of Polymer–Polymer Miscibility......Page 187
4.2 Interface Development Between Compatible Polymer Films......Page 197
4.3 Structured Latex Films......Page 209
4.4 Morphology Analysis of Interpenetrating Polymer Networks......Page 217
5 Conclusions......Page 225
References......Page 226
1 Introduction......Page 231
2.1 Equilibrium Melting......Page 233
2.2 Nucleation of Crystals and Molecules......Page 238
2.3 Irreversible Melting......Page 241
2.4 Local Equilibria......Page 247
2.5 Summary of Thermal Effects......Page 249
3.1 Evaluation of Heat Capacity by MTDSC as a Baseline for the Study of Melting......Page 251
3.2 Melting and Crystallisation by Standard DSC......Page 259
3.3 Types of Modulation of Temperature......Page 264
3.4 Deconvolution of the Reversing Heat Capacity......Page 266
4.1 Qualitative and Semi-quantitative Analysis of Polymer Melting by MTDSC......Page 272
4.2 Determination of Heat Capacity of Solids and Melts......Page 283
4.3 Determination of Heat of Fusion, Crystallinity and Kinetics......Page 289
4.4 Determination of Annealing and Reorganisation......Page 308
4.5 Reversible Melting......Page 323
5 Recommendations......Page 328
References......Page 330
C......Page 335
D......Page 336
G......Page 337
K......Page 338
M......Page 339
P......Page 340
S......Page 341
Z......Page 342