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利用脉冲热分析技术(PulseTA)实现对热分析-质谱(TA-MS)联用系统中逸出气体质谱信号的定量,考察了多种实验参数如不同载气流速、温度以及分析样品量等因素对热分析-质谱联用系统中逸出气体质谱信号定量校正的影响.实验结果表明,利用PulseTA对TA-MS联用系统中逸出气体CO2定量结果与理论计算值的相对误差约2.85%.同时利用TG-DTG-MS联用技术对氮化铟(InN)粉体的热分解行为进行研究,在氩气气氛下InN粉体的热分解过程一步完成,InN粉体在550～750℃得到相应的正离子质谱峰:N2+(m/z=28),所释放的N非常接近InN中N的理论含量.利用PulseTA技术检测到InN粉体受热分解放出氮气质量的实验测量值与理论计算值的相对误差约为1.36%.
The quantitative analysis of escaped gas mass spectrometry signals in a thermal analysis-mass spectrometry (TA-MS) system was carried out using pulse thermal analysis (Pulse TA). Various experimental parameters such as different carrier gas flow rates, temperatures, and sample sizes On the quantitative analysis of escaped gas mass spectrometry signals in the thermal analysis-mass spectrometry system.The experimental results show that the relative error of the quantitative results of CO2 escaped from TA-MS system with the theoretical calculation of pulse TA is about 2.85%. At the same time, the thermal decomposition behavior of indium nitride (InN) powder was studied by TG-DTG-MS. The thermal decomposition of InN powder was completed in one step under argon atmosphere. InN powder was obtained at 550-750 ℃ The corresponding positive ion mass spectrum peak is N2 + (m / z = 28), and the released N is very close to the theoretical content of N in InN. The experimental measurement and theoretical calculation of the nitrogen mass of InN powder by pyrolysis are detected by PulseTA technique The relative error is about 1.36%.