【Abstract】 Co 3O 4 nanoparticles were prepared by mixing polyvinylalcohol(PVA) and Co(NO 3) 2 in a mole ratio of 1∶3~4, at 100~130 ℃ to evaporate and remove water, and calcining at 400 ℃ for 2 h. The structure, crystal type and surface appearance were characterized by IR, XRD and TEM. The results showed that metal carbonate was formed using the polymer combustion methods, and the Co 3O 4 gave a cubic polygon appearance. Agglomerate free, well dispersive Co 3O 4 nanoparticles with the cubic structure and the average size of ca. 33 nm could be obtained from carbonated precursor by this simple and economical methods.更多还原