Abstract: CeO2 nanometer powders of different sizes were prepared at low temperature by pyrolysis of amorphous citrate. XRD patterns show that CeO2 is cubic in structure, space group Oh5-FM3M·TEM indicates that the prepared CeO2 is spherical in shape, and the particle size distribution is in narrow range. It was found that calcination temperature is a more important factor affecting the crystallite size of CeO2 than calcining time, the smaller the particle. the bigger the crystallattice distortion, the worse the crystal growth. Solubility test of CeO2 in nitric acid reveals that the surface activity of CeO2 decreases with the increasing particle sizes. IR spectra analysis shows that the absorption of Ce-O bond is shifted to higher energy with the decrease of CeO2 particle sizes.