Fundamentals of Thermal Analysis

1. Definition and types of thermal analysis

Thermal analysis (TA) is defined as the study of the relationship between a sample property and its temperature as the sample is heated or cooled in a controlled manner. Therefore, many thermal analysis techniques are defined and used depending on the physical properties of interest.

Thermal analysis techniques include:

Physical quantities of interest
Technique
Mass Thermogravimetry (TG)
 Evolved Gas Analysis (EGA)
Temperature difference Differential Thermal Analysis (DTA)
Heat flow rate difference Differential Scanning Calorimetry (DSC)
Dimensional properties Thermodilatometry (TD)
Mechanical properties Thermomechanical Analysis (TMA)
Dynamic Mechanical Analysis (DMA)
Electrical properties Thermally Stimulated Current Analysis (TSC)

 

The following physicochemical changes can be measured using commonly used thermal analysis instruments: STA(TG-DTA/DSC) (a simultaneous thermal analysis measurement instrument for TG and DTA/DSC), DSC, and TMA.

Device Temperature range Change
STA (TG-DTA/DSC) RT to 1500°C Decomposition, oxidation, reduction, transition, melting, solidification, crystallization, dehydration, sublimation, evaporation, adsorption, hardening, glass transition, etc.
DSC -180°C to 725°C
RT to 1500°C
Transition, melting, solidification, crystallization, glass transition, dehydration, etc.
TMA -150°C to 600°C
RT to 1500°C
Expansion, shrinkage, softening, coefficient of thermal expansion (CTE), etc

2. Thermal analysis model data

Let's look at a typical thermal analysis curve for the measurement results obtained with commonly used thermal analysis equipment. The measurement results of thermal analysis are shown with the target physical quantity on the vertical axis and temperature (or time) on the horizontal axis.

 

About-TA-TGABOUT-TA-DTA

ABOUT-TA-DSC

ABOUT-TA-TMA

Schematic diagram of thermal analysis curves obtained under linear heating conditions


3. Information obtained from thermal analysis results

The information obtained from the measurement results of STA(TG-DTA/DSC), DSC, and TMA is as follows:

Method Output Information gained
TG Mass change The temperature of weight loss or gain, and the magnitude of weight loss or gain (rate of change)
DTA Temperature difference with reference material Endothermic and exothermic reaction temperature
Changes in specific heat capacity (glass transition, etc.)
DSC Energy change Temperature and energy of endothermic and exothermic reactions (Enthalpy change)
TMA Length change Expansion and contraction amount, expansion rate, coefficient of thermal expansion, softening temperature

Both DTA and DSC are techniques for measuring the heat transfer that accompanies chemical and physical changes, but DSC can directly measure endothermic and exothermic energy by integrating endothermic and exothermic peaks over time (calculating the area), whereas DTA peak areas do not directly correspond to energy values, but are values proportional to the endothermic and exothermic energy. Therefore, DSC gives quantitative information on endothermic and exothermic energy, while DTA is limited to qualitative information.

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