Nano-Co3O4 with different morphologies was successfully synthesized by annealing CoC2O4·2H2O precursors. The as-obtained samples were characterized by powder X-ray diffraction (XRD), scanning electron microscopy (SEM), and low-temperature nitrogen adsorption-desorption. It was found that the volume ratio of N,N-dimethylformamide (DMF) and water played an important role in the formation of cobalt oxalate precursors with different morphologies. After calcination in air, cobalt oxalate precursors converted to Co3O4 nanomaterials while their original morphologies were maintained. The catalytic effect was investigated for nano-Co3O4 with different morphologies on the thermal decomposition of ammonium perchlorate (AP) by differential scanning calorimeter (DSC). The results indicated that all products showed excellent catalytic activity for thermal decomposition of AP and the Co3O4 nanorods with larger BET surface area and pore volume had the highest catalytic activity.
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