T-jump/FTIR spectroscopy was used to study thermal decomposition of energetic material [Co(CHZ)3](ClO4)2and [Ni(CHZ)3](ClO4)2 in thin film with rapid heating rate. During the exothermic decomposition process, the major gas products were identified as CO2, H2O, HCN, HNCO, and HONO. Time-to-exotherm (tx) kinetics method derived from the control voltage trace of T-jump/FTIR spectroscopy was introduced to resolve kinetics of the exothermic decomposition reaction of flash pyrolysis of the title compounds. In the temperature range of 613～653 K under 0.1 MPa Ar atmosphere the Arrhenius activation energy of the exothermic decomposition reaction of [Co(CHZ)3](ClO4)2 was determined to be Ea=39.42 kJ·mol-1 and InA=5.93. The Arrhenius activation energy of [Ni(CHZ)3](ClO4)2 was determined to be Ea=60.44 kJ·mol-1 and lnA=9.40 in the temperature range of 618～678 K under 0.1 MPa Ar atmosphere.%利用温度跃升傅立叶变换红外原位分析技术(T-jump/FTIR)对高氯酸碳酰肼钴和高氯酸碳酰肼镍的快速热分解反应进行了研究.研究表明,目标化合物快速热分解逸出的主要气相产物是CO2,H2O,HCN,HNCO和HONO.借助快速升温过程中Pt金属丝的控制电压变化曲线得到剧烈放热峰的诱导出现时间tx,利用tx值计算了两种目标化合物的快速热分解动力学参数.在0.1 MPa氩气气氛,613～653 K的实验温度范围内,高氯酸碳酰肼钴的活化能Ea=39.42 kJ·mol-1,lnA=5.93;在0.1 MPa氩气气氛,618～678 K的实验温度范围内,高氯酸碳酰肼镍的活化能Ea=60.44 kJ·mol-1,lnA=9.40.
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