Nano-sized cobalt oxide powders were prepared by low pressure spray pyrolysis process. The precursor powders obtained by low pressure spray pyrolysis process from the spray solution with ethylene glycol had several microns size and hollow structure. The precursor powders obtained from the spray solution with optimum concentration of ethylene glycol formed the nano-sized cobalt oxide powders with regular morphology after post-treatment without milling process. On the other hand, the cobalt oxide powders obtained from the spray solution without ethylene glycol had submicron size and spherical shape before and after posttreatment. The mean size of the cobalt oxide powders formed from the spray solution with concentration of ethylene glycol of 0.7M was 180 nm after post-treatment at temperature of . The mean size of the powders could be controlled from several tens nanometer to micron sizes by changing the post-treatment temperatures in the preparation of cobalt oxide powders by low pressure spray pyrolysis process.