In the present work, nano-sized CuO, Co3O4 and CuCo2O4 powders were prepared via different methods such as co-precipitation, thermal decomposition of oxalate precursor and sol-gel and their catalytic activities towards thermal decomposition of ammonium perchlorate were investigated using DSC technique. CuCo2O4 showed better catalytic activity than others and the thermal decomposition temperature of ammonium perchlorate shift downward about 103 degrees C. The catalytic mechanism was also briefly discussed. TG-DSC, FT-IR, XRD, SEM, TEM and BET techniques were applied for studying of thermal behavior, examination of catalytic activity, spectroscopic, structural, morphological characterization and determination of specific surface area of synthesized powders, respectively. (C) 2011 Elsevier B.V. All rights reserved.