Nano-MnFe2O4 particles were synthesized by co-precipitation phase inversion method and low-temperature combustion method respectively, using MnCl2, FeCl3, Mn(NO3)(2), Fe(NO3)(3), NaOH and C6H8O7. X-ray diffraction (XRD), transmission electron microscope (TEM), Fourier transform infrared spectroscopy (FT-IR), thermogravimetry-differential thermal analysis (TG-DTA) and differential scanning calorimetry (DSC) were used to characterize the structure, morphology, thermal stability of MnFe2O4 and its catalytic performance to ammonium perchlorate. Results showed that single-phased and uniform spinel MnFe2O4 was obtained. The average particle size was about 30 and 20 nm. The infrared absorption peaks appeared at about 420 and 574 cm(-1), and the particles were stable below 524 degrees C. Using the two prepared catalysts, the higher thermal decomposition temperature of ammonium perchlorate was decreased by 77.3 and 84.9 degrees C respectively, while the apparent decomposition heat was increased by 482.5 and 574.3 J.g(-1). The catalytic mechanism could be explained by the favorable electron transfer space provided by outer d orbit of transition metal ions and the high specific surface absorption effect of MnFe2O4 particles.