Synchronous thermal analyzer testing the thermal decomposition characteristics of ceramic materials

Ceramic materials, as excellent inorganic non-metallic materials, have a wide range of applications in various fields such as aerospace, electronic information, energy and environmental protection. It has excellent characteristics such as high strength, high temperature resistance, and corrosion resistance. However, in different usage environments, ceramic materials may undergo temperature changes, which may lead to physical or chemical changes. These changes directly affect the performance and service life of ceramic materials. Synchronous thermal analysis technology can simultaneously measure the thermogravimetric (TG) and differential thermal analysis (DTA) or differential scanning calorimetry (DSC) information of ceramic materials under the same experimental conditions, providing accurate data support for studying the changes of ceramic materials during heating.

1、 Measurement principle

Synchronous thermal analyzerMainly based on the principles of thermogravimetric analysis (TG) and differential thermal analysis (DTA) or differential scanning calorimetry (DSC), synchronous testing of ceramic materials is achieved.

Thermogravimetric analysis (TG) is a technique for measuring the relationship between the mass of a substance and temperature or time under program-controlled temperature. When ceramic materials are heated under a certain temperature program, if chemical reactions such as decomposition, oxidation, reduction occur, or physical changes such as dehydration and degassing occur, their quality will change.

Differential Scanning Calorimetry (DSC) is a technique that measures the temperature or time relationship between the required heat difference per unit mass of a sample and a reference substance at a programmed temperature. It can more directly reflect the energy changes of materials during thermal changes, providing more accurate data for studying the thermal stability and reaction kinetics of materials.

2、 Experimental steps

1. Measuring instrument: DZ-STA401 synchronous thermal analyzer

2. Measurement reference standard:

GB/T36402-2018 Test Method for Thermal Analysis Mass Spectrometry of Ceramic Materials

3. Measurement steps

3.1 Grind the tested ceramic material into a uniform powder form and screen the appropriate particle size sample through a sieve. First, place two empty crucibles above the sample rod and wait for TG to stabilize before inputting the mass.

3.2 Sample loading: Take out the crucible on the right side, place the appropriate amount of sample required for the experiment, and then place the experimental crucible inside the furnace body.

3.3 Setting experimental parameters: On the operating software of the instrument, set the atmosphere type of the experiment (such as nitrogen, air, etc.), gas flow rate generally between 50-100mL/min, heating rate generally between 5 and 20 ℃/min, termination temperature, and other parameters.

3.4 Starting the experiment: After confirming that the parameter settings are correct, start the experimental program, and the instrument will start heating up according to the set temperature program, while synchronously collecting TG or DSC data.

3.5 Data Processing: After the experiment is completed, use the data analysis software provided with the instrument to process the collected data, draw TG or DSC curves, and perform relevant analysis and calculations.

3、 Graph analysis

This is an experimental data chart of alumina ceramic material. The sample is heated to 1150 ℃ at a rate of 20 ℃/min, and the entire process is carried out under a nitrogen protected environment for programmed heating. The sample is very stable at around 900 ℃ without any quality changes. After 900 ℃, the internal high-temperature bonding meter and inorganic additives begin to rapidly react and decompose, resulting in weight loss. From the figure, it can be seen that the total weight loss of the sample from room temperature to 1150 ℃ is 11.95%, with a weight loss of 2.43mg. During the weight loss process, there is a significant exothermic reaction in the DSC spectrum, which is due to the presence of some residual energetic adhesives inside the tested ceramic material, resulting in exothermic reactions during high-temperature decomposition.

4、 Experimental conclusion

Synchronous thermal analysis technology can comprehensively and accurately reflect the quality changes and thermal effects of ceramic materials during heating, providing reliable experimental basis for studying the thermal properties of ceramic materials. For example, in the research and development of ceramic materials, the synthesis process can be optimized based on test results to improve material performance; In quality control, it is possible to quickly detect the purity and stability of materials to ensure product quality.