Chapter
1.9. Transpiration Method
1.10. UV Spectroscopy for Vaporization Studies of Low-Volatile Compounds
1.11. Correlation Gas Chromatography
1.12. How to Adjust ∆lgHmo(T) Values to the Reference Temperature 298.15K Properly?
1.13. Indirect Determination of Molar Enthalpies of Vaporization of ILs from Calorimetric Results
1.14. Conclusions and Outlook
Chapter 2: Fast Scanning Chip Calorimetry
2.2.1. Fast Scanning Sensors
2.2.2. Temperature Calibration
2.2.2.1. The Thermometer and Thermal Lag
2.2.2.2. Static Temperature Gradients
2.2.2.3. Lateral Temperature Profile in Membrane Based Calorimeters
2.2.3. Heat Capacity Determination
2.3. Selected Applications of FSC
2.3.1. Polymer Crystallization
2.3.2. Crystal Nucleation in Polymers by Tammann's Nuclei Development Method
2.3.3. Enthalpy Relaxation and Homogeneous Crystal Nucleation in Polymer Glasses
2.3.4. Polymer Crystal Reorganization
2.3.6. Analysis of Chemically Unstable Materials
2.3.7. Analysis of Phase Transitions in Metals
2.3.9. Combination of FSC With Other Analytical Techniques
3.1.1. Thermal Strain and Phase Transitions in General
3.1.2. Methodology of Dilatometric Assessment of Phase Transformation
3.1.3. Dilatometry Applications in the Field of Materials
3.3. Analysis of Dilatometer Curves
3.4.1. Thermal Expansion Coefficient of an Austenitic Steel
3.4.2. Continuous Cooling Behavior of a Steel With Different Carbon Contents
3.4.3. Effect of Segregation on Isothermal Transformation Kinetics of Lower Bainite
3.6. Future Trends in Dilatometry
Chapter 4: Modern Isoconversional Kinetics: From Misconceptions to Advances
4.2.1. Preexponential Factor and Reaction Model
4.2.2. Single-Step Approximation
4.2.3. Meaning of Isoconversional Activation Energy
4.2.4. Application to Processes on Cooling
4.3.1. Crystallization and Melting of Polymers
4.3.2. Solid-Solid Transition
4.3.3. Crystallization From Solution
4.3.4. Thermal Decomposition During Continuous Cooling
4.3.6. Deconvolution of Overlapped Processes
Chapter 5: Kinetics and Mechanisms of Solid-Gas Reactions
5.2. Kinetic Concepts and Background
5.2.1. Pseudo-Steady-State Approximation
5.2.2. Fundamental Processes
5.2.3. Rate-Determining Step Approximation
5.2.4. General Rate Equation
5.3. Experimental Methods
5.3.1. Isothermal and Isobaric TG
5.3.2. Conditions for Collecting Reliable Kinetic Data
5.3.3. Sudden Jump Method
5.3.4. Hyphenated Techniques
5.4. Kinetic Geometrical Models and Elementary Mechanisms
5.4.1. Kinetic Geometrical Models
5.4.1.1. One-Process Models
5.4.1.2. Two-Process Models
5.4.1.3. Validation Tests
5.4.1.3.1. Pseudo-Steady-State Assumption
5.4.1.3.2. Rate-Determining Step of Growth Assumption
5.4.2. Elementary Mechanisms
5.4.2.1. Nucleation Elementary Mechanisms
5.4.2.2. Growth Elementary Mechanisms
5.5. Other Applications of the Jump Method
5.5.2. No-Reproducible Experiments
5.5.3. Validation of the Geometrical Model
5.6. Nonisothermal, Nonisobaric Conditions (Case of a Reacting Bed): CIN4 Approach
Chapter 6: Physico-Geometric Approach to the Kinetics of Overlapping Solid-State Reactions
6.2. Phenomenology of Overlapping Reactions in the Solid State
6.2.1. Overlapping Processes of a Mixture of Different Substances and a Substance With Different Reactivities
6.2.2. Overlapping Processes Controlled by Physico-Geometric Events
6.2.3. Consecutive and Concurrent Chemical Processes
6.3. Experimental Approach to Overlapping Processes
6.3.1. Characterization of Sample and Tracking of Reaction Process
6.3.2. Experimental Separation of Overlapping TA Peaks
6.4. Kinetic Approach to Overlapping Processes
6.4.1. Kinetic Data of Overlapping Processes
6.4.2. Preliminary Kinetic Approach to Overlapping Processes
6.4.3. Kinetic Deconvolution Analysis
6.4.4. Kinetic Modeling of the Overlapping Processes in the Solid State
Chapter 7: Analysis of Polymer Crystallization by Calorimetry
7.2. General Aspects of Polymer Crystallization
7.3. Analysis of Polymer Crystallization by Differential Scanning Calorimetry
7.3.1. Isothermal Crystallization
7.3.2. Critical Issues in DSC Analysis of Isothermal Polymer Crystallization
7.3.3. Nonisothermal Crystallization by DSC
7.4. Analysis of Polymer Crystallization by Fast Scanning Calorimetry
7.4.1. Nonisothermal Crystallization
7.4.2. Nonisothermal Crystal Nuclei Formation
7.4.3. Nonisothermal Cold-Crystallization
7.4.4. Isothermal Crystallization
7.4.5. Crystal Nucleation in Glassy Polymers
7.5. Analysis of Polymer Crystallization by Temperature-Modulated Calorimetry
7.5.1. Quasi-isothermal Crystallization of Polymers Investigated by TMDSC
7.5.2. Nonisothermal Crystallization of Polymers Investigated by TMDSC
7.6. Flow-Induced Crystallization
7.7. Combined Calorimetric+Complementary Analytical Techniques
7.7.2. In Situ Imaging and DSC
7.7.3. In Situ Rheology and DSC
Chapter 8: Glass Transition and Physical Aging of Confined Polymers Investigated by Calorimetric Techniques
8.2. Equilibrium vs. Nonequilibrium Dynamics
8.3. The Glass Transition
8.4. Recent Developments in Thermodynamic and Dynamic Aspects of Glasses Below Tg
8.4.1. Thermodynamics Below Tg
8.5. Glass Dynamics in Confinement
8.5.1. Nonequilibrium Dynamics: Tg and Physical Aging
8.5.2. Relation to the Rate of Spontaneous Fluctuations
8.5.3. Factors Affecting Tg Depression: Free Interface and Adsorption
8.5.4. Theoretical Description
8.6. Accessing Low-Energy Glassy States by Aging Nanostructured Glasses
Chapter 9: Decomposition of Organic Wastes: Thermal Analysis and Evolution of Volatiles
9.4. Analysis of the Volatiles Evolved and Kinetics
9.5. Evolution of Compounds
Chapter 10: Thermal Analysis of Biobased Polymers and Composites
10.1.1. Thermal Analysis and Calorimetry
10.2.1. Protein Denaturation and Gelation
10.2.2. Polymerization and Curing of Biobased Thermosets
10.2.2.1. Polycondensation of FA
10.2.2.2. Polyepoxides-Based Thermosets
10.2.3. Crystallization of Biobased Polyesters
10.2.6. Relaxation Process of Lignin
10.2.7. Degradation, Thermal, and Thermo-Oxidative Degradation
Chapter 11: Polymer Nanocomposites
11.3. Nano-Effects in PNCs
11.3.1. Confinement Effects
11.3.2. Entanglement Effects
11.3.3. The Influence of Nanoparticles on Glass Transition
11.3.4. The Influence of Nanoparticles on Polymer Melting and Crystallization
11.4. Thermal Analysis Methods in PNCs Characterization
11.4.1.1. Melting and Crystallization
11.4.1.2. Exfoliation and Intercalation
11.4.1.3. Glass Transition, Relaxation, and Fictive Temperature
11.4.1.5. Crystalline Fraction (CF), Rigid Amorphous Fraction (RAF), and Mobile Amorphous Fraction (MAF)
11.4.2.1. Glass Transition
11.4.2.2. Confinement Effect
11.4.2.3. Activation Energy of Glass Transition
11.4.3. Fast Scanning Calorimetry
11.4.5. Thermogravimetry (TG)
11.4.5.1. Thermal Stability
11.4.5.2. Thermal Degradation Kinetics
11.4.6. Thermoanalytical Methods (TG/MS, TG/FTIR)
11.4.8. Laser Flash Analysis (LFA)
Chapter 12: Thermal Behavior of Chalcogenide Glasses
12.2. Glass Transition Behavior
12.2.1. Enthalpy Relaxation Studied by DSC/DTA
12.2.2. Volume Relaxation Studied by TMA/DIL
12.2.3. Viscosity Measurements
12.3. Crystallization Behavior
12.3.1. Crystallization Studied by DSC/DTA
12.3.2. Crystallization Studied by TMA
12.3.3. Crystal Growth Rate Studied by Microscopy
Chapter 13: Applications of Thermal Analysis to the Study of Phase-Change Materials
13.2. Types of PCM and Their Applications
13.2.1. Latent Thermal Energy Storage Using PCMs
13.2.2. Classifications of PCMs and Their Applications
13.3. Thermal Analysis Methods on PCMs
13.3.1. Differential Scanning Calorimetry (DSC)
13.3.2. DSC-Dynamic Method
13.3.5. Specific Heat Measurement Using the DSC
13.3.6. Thermogravimetric Analysis (TGA)
13.4. DSC Applications on PCMs
13.5. TGA Applications on PCMs
13.6. TGA Applications on Nanomaterial-Based PCMs
13.7. Merits and Challenges
Appendix. Thermal Properties of Various Heat Storage Materials
Chapter 14: Characteristics of Thermal Decomposition of Energetic Materials in a Study of Their Initiation Reactivity
14.2. The Main Sources of Thermal Decomposition Data
14.3. Strategy and Reasons for the Various Approaches
14.3.1. Approach Based on Primary Fission Similarity
14.3.1.1.1. Generalization of Validity of the Relationships Found
14.3.1.1.2. Thermal Reactivity as a Kissinger Slope Relationship
14.3.1.2. Impact Reactivity (Sensitivity)
14.3.1.3. Friction Reactivity (Sensitivity)
14.3.1.4. Sensitivity to Electric Spark
14.3.1.5. Note Concerning the Use of the Czech Vacuum Stability Test
14.3.2. Approach on the Basis of Electron Structure in the Reaction Center
14.3.2.1. NMR Chemical Shifts—Specification of the Reaction Center in the Molecule
14.3.2.2. Correlation of Reaction Characteristics With Electron Charges
14.4.1. Why Are Low-Temperature Thermal Decomposition Data Important?
14.4.2. Primary Fission—Reaction Center of the Molecule
14.4.3. Relationships Between Decomposition Activation Energies and Performance of EMs
14.4.4. Mechanical and Electric Spark Sensitivities in Connection With Thermal Decomposition
14.4.4.1. Toward the Initiation Reactivity of 2,4,6,8,10,12-Hexanitro-2,4,6,8,10,12-Hexaazaisowurtzitane (HNIW)
Chapter 15: Pharmaceutical Applications of Thermal Analysis
15.2. Physical Characterization of Crystalline Drugs
15.2.2. Solid-Solid Transition Temperature
15.2.5. Unusual Melting Behavior
15.3. Evaluation of Amorphous Properties
15.3.1. Glass Transition and Relaxation
15.3.2. Specific Heat Capacity
15.3.4. Crystallization Tendency
Chapter 16: Thermoanalytical Characterization Techniques for Multiferroic Materials
16.1.1. Multiferroic Materials
16.1.2. Perovskite Oxide BiFeO3
16.1.2.1. Crystal Structure and Multiferroism in BiFeO3
16.1.2.2. Challenges of Bulk BiFeO3 Preparation
16.2. Thermoanalytic Characterization Techniques in BiFeO3 and Related Materials
16.2.1. Differential Scanning Calorimetry (DSC) and Differential Thermal Analysis (DTA)
16.2.2. Thermomechanical Analysis (TMA) and Thermodilatometry (TD)
16.2.3. Temperature-Dependent Structural Characterization Techniques (Thermodiffraction): X-Ray, Synchrotron, Neutron, an ...
16.2.4. Raman Thermospectroscopy
16.2.5. Impedance Thermospectroscopy
16.2.6. Dielectric Thermal Analysis (DEA)
Chapter 17: Chalcogenides for Phase-Change Memory
17.2. Glass-Forming Ability
17.3. Crystallization in Phase-Change Chalcogenides
17.3.3. Size-Dependent Crystallization
17.3.4. Uncertainty Over Tg in Fast Phase-Change Chalcogenides
17.3.5. Measurements of Crystal Growth Rate
17.3.6. Ultrafast DSC Measurements on Phase-Change Chalcogenides
17.3.6.1. The Kissinger Analysis
17.3.6.2. Johnson-Mehl-Avrami Kinetics
17.3.6.3. Regimes Revealed by Ultrafast DSC and the Influence of Mobility
17.3.7. Fragile-to-Strong Crossover
17.3.7.1. Effect of FSC on Crystallization Kinetics
Chapter 18: Recent Advances in Thermal Analysis and Calorimetry of Aluminum Alloys
18.1.1. Application of Aluminum Alloys for Structural Components
18.1.2. Heat Treatment Precipitation Hardening
18.1.3. Kinetics of Solid-Solid Phase Transformations and Its Measurement
18.2. Analysis of Solid-Solid Phase Transformations Kinetics in Metallic Alloys in a Wide Dynamic Range
18.2.2. Basics for Calorimetric Measurements of Solid-Solid Phase Transitions in (Al-) Alloys
18.2.3. Basics for Dilatometric Measurement of Solid-Solid Phase Transitions in (Al-) Alloys
18.2.4. Possible Reasons for the Remaining Zero-Level Curvature and its Elimination
18.2.5. Physical, Alloy-Specific Requirements on the Scanning Rate Range
18.2.6. DSC Devices, Quenching Dilatometer, and Sample Geometries Utilized to Achieve Nine Orders of Magnitude in Cooling ...
18.2.7. Some Peculiarities of Cooling Experiments—Temperature Control Limitations and Determination of the uCCR
18.3. Recent Developments
18.3.1. Brief Review on Sophisticated and Established DSC Methods—Their Field of Action and Limitations
18.3.2. Dilatometric Measurements of Solid-Solid Phase Transformations in Al Alloys
18.3.3. Analysis of Solid-Solid Phase Transformations at Fast Cooling Rates by FSC
18.4. Outlook and Future Prospective
Chapter 19: Metals and Alloys
19.1.1.1. Initial Metallurgical State of Alloy Samples
19.1.1.2. Temperature Calibration: Choice of Onset Temperature
19.1.1.3. Quantitative Enthalpy and Heat Capacity Calibration
19.1.1.4. Determination of Liquidus Temperature
19.1.5. Dynamic Mechanical Analysis (DMA)
19.2. Phase Diagram Characterization
19.2.1.1. Determination of Type of Reaction
19.2.1.2. Li-Sb-Potential Anode Material in Li-Ion Batteries
19.2.2. Thermal Analysis of Ternary Alloys
19.2.2.1. Ternary Systems—Validation of Model Predictions
19.3.2. Stability of Metallic Glass—Isothermal Annealing
19.3.3. Structural Relaxation of BMGs
19.4. Oxidation of Alloys
19.4.1. Determining Rate Laws for High-Temperature Kinetics
19.4.2. Active/Passive Oxidation
19.5. Transient Liquid-Phase Bonding
19.5.2. DSC Analysis of TLPB
19.6. Shape Memory Alloys (SMAs)
19.7. Kinetic Studies of Melting, Crystallization, and Glass Formation by Fast Scanning Calorimetry
19.7.1. Nonequilibrium Melting of Binary Alloys
19.7.2. Kinetic Competition in a Au55Pb22.5Sb22.5 Metallic Glass [148]
A.2. Terms and Definitions
A.3. Calibration and Sensitivity
Handbook of Thermal Analysis and Calorimetry
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