Ultrafine ZnO powder was synthesized by precipitation method, using zinc sulfate and aqueous ammonium carbonate as raw material and precipitant, respectively. The influence of the concentration of aqueous ammonium carbonate on the precipitation rate of Zn2+ was discussed and their relationship was also illustrated. The precipitation rate of Zn2+ increased gradually with the mol ratio of CO32-to Zn2+, which reached up to more than 96% when the mol ratio was 1.2. In addition, the crystal structure and morphology of the precursor and ZnO powder were also characterized using XRD and SEM. The results indicated that ZnO powder was hexagon wurtzite structure and spherical figure with high purity and regular crystal form.