Ceria(CeO2) and Ce2(CO3)2·H2O microcube as a precursor of CeO2 were prepared by an ethanol-assisted homogeneous precipitation using cerium nitrate hexahydrate as a cerium source and urea as a precipitant. The synthesized CeO2 precursors were identified as orthorhombic Ce2(CO3)2·H2O. It was observed that the particle shape was controlled by the volume ratio of ethanol: water and reaction time. The precursor was calcined at 700 ℃ to obtain CeO2. The particle size distribution and morphology of synthesized CeO2 powder were similar to those of the precursors.