Nanocrystals of four transition metal oxides (TMOs) were prepared by a novel quick precipitation method and characterized by X-ray diffraction (XRD) and transmission electron microscopy (TEM). From the XRD patterns, average particle sizes for CuO, NiO, Co 2 O 3 , MnO 2 are calculated to be 15 nm, 4 nm, 13 nm, 40 nm, respectively. The TEM study revealed that the majority of CuO particles are of 6–8 nm in size. Catalytic activities of the TMO nanocrystals for thermal decomposition of ammonium perchlorate (AP) were investigated using differential thermal analysis (DTA), thermogravimetric analysis (TGA) and ignition delay measurements. The order of catalytic activity of these oxide nanocrystals on thermal decomposition of AP was found to be: Co 2 O 3 > CuO > NiO > MnO 2 .