Ultrafine Powder CuO was prepared by direct-heating Cu2(OH)2CO3 in differe nt calcination temperatures. XRD, FT-IR, SEM and surface area measurement tech niques were used to investigate the properties of the CuO powder. The results sh ow that the decomposition temperature has remarkably effect on crystallite size, morphology, surface structure, IR behavior and activity of the powder for H2O2 decomposition. The major morphology of the particle is fluffy-sphered in the l ower temperature, which is consists of small sheets of crystallite. With the inc reasing of calcination temperature, crystal of CuO grows up, the fluffy-sphere d particle reduces and catalytic activity decreases. FT-IR patterns revealed t hat the absorption of Cu-O and -OH bond in CuO ultrafine powder were red-s hifted.