Mesoporous Ce1-x Zr (x) O-2 with high surface area was synthesized using a modified evaporation-induced self-assembly method that combined citric acid as complexing agent and cetyltrimethyl ammonium bromide as surfactant. The samples with different Ce/Zr molar ratio were characterized by thermogravimetry and differential thermal analysis, X-ray diffraction, transmission electron microscopy, selected area electron diffraction, Brunauer-Emmett-Teller (BET), and Barrett-Joyner-Halenda methods. It was found that when the Zr molar fraction was larger than 0.3, a mixture of cubic phase and tetragonal phase was formed. Ce0.7Zr0.3O2 solid solution had the largest BET surface area (217 m(2) g(-1)) and mesoporous structure. The catalytic performances of mesoporous Ce1-x Zr (x) O-2 for CO oxidation were examined. Mesoporous Ce0.7Zr0.3O2 solid solution demonstrated the best catalytic activity due to the high surface area and an enhanced redox property caused by appropriate Zr4+ incorporation.