Abstract: T-jump/FTIR spectroscopy was used to study thermal decomposition of energetic material [Co(CHZ)3](ClO4)2 and [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 lnA=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.

Key words: Cobalt perchlorate, Nickel perchlorate, Carbohydrazide, Thermal kinetics, Flash pyrolysis, T-jump /FTIR spectroscopy