To promote the stable production and wide application of silver acetylide-silver nitrate （Ag₂C₂·AgNO₃）， the structural morphology and thermal decomposition characteristics were systematically studied by X-ray powder diffractometry， Fourier tranform infrared spectrometer， scanning electron microscopy， differential scanning calorimeter and thermogravimetric-mass-infrar- ed spectrometry techniques. The results indicate that the prepared Ag₂C₂·AgNO₃ sample is in the form of nanospheres with particle sizes ranging from 400 to 500 nm. There is only one exothermal decomposition process of Ag₂C₂·AgNO₃ with a peak temperature of 234.9 ℃， a weight loss of 8.72%， and a heat release of 1449 J·g^-1，at a heating rate of 10 ℃·min^-1. The apparent activation energy and pre-exponential constant of decomposition process are obtained as 108.9 kJ·mol^-1 and10^8.94 s^-1， respectively. Moreover， the gaseous decomposition products of Ag₂C₂·AgNO₃ were NO， NO₂ and CO₂.