Using cetyltrimethy lammonium bromide (CTAB) as the template agent, cerium nitrate as the cerium resource, yttrium nitrate as the yttrium resource, and ammonium carbonate as the precipitating agent, mesoporous CeO 2 powders doped with different yttrium contents were successfully synthesized using a chemical precipitation method, under an alkalescent condition. Properties of the obtained samples were characterized and analyzed with X-ray diffraction (XRD), energy dispersive analysis of X-rays (EDAX), transmission electron microscopy (TEM), infrared (IR) absorbance, and the BET method. For the prepared samples with 20% (molar ratio) Y-doped content, a BET specific surface area of 106. 6 m 2 · g −1 , with an average pore size of 3.27 nm were obtained. XRD patterns showed that the doped samples were with a cubic fluorite structure. TEM micrographs revealed that the doped samples showed a spherical morphology with a diameter ranging from 20 to 30 nm and a round pore shape. IR results indicated that the Ce-O-Ce vibration intensity decreased as the Y-doped content increased. N 2 adsorption-desorption isotherms showed that the samples possessed typical mesopore characteristics. The average pore size of the samples decreased after mesoporous CeO 2 was doped with yttrium, and the average pore size decreased largely as the Y-doped content increased.