Nano Metal/C (Metal=Fe, Co) composite materials, in which nano iron and cobalt particles were uniformly distributed in carbon matrix, was prepared by pyrolysis of M-exchanged cation exchange resin(M-PAA). X-ray diffraction (XRD), Transmission Electron Microscope (TEM) results showed the particle size and morphology of nano iron and cobalt in M/C could be controlled by pyrolytic temperature. The particle size of Co and Fe in M/C obtained at 500 was respectively 15-40 nm and 10-35 nm. DTA was employed to test the thermal decomposition of ammonium perchlorate (AP) in the M/C and AP mixture. Results indicated the decomposition temperature at high-temperature decomposition of AP was lowered with the addition of amount of M/C-500, and the high temperature decomposition peaks of AP respectively lowered as much as 145.2°Cand 68.3°C with adding amount of 5% of Co/C and Fe/C obtained at 500 . The high and low temperature decomposition peaks of AP overlapped with addition of Co/C.