Single-phase homogeneous Ce1- xZrxO2 solid solutions with various compositions were synthesized using the reversed microemulsion method. The structural properties and performance of Ce1- x ZrxO2 were studied using XRD, BET,SEM, HRTEM, TPR and CO oxidation measurements. The results show that in the range of x = 0.4 ～ 0.5 and x = 0.6 ～1.0, the solid solutions posses the cubic and the tetragonal phase structure, respectively. Solids obtained by the reversed microemulsion method were more homogeneous on the whole range of composition. XRD investigations of the prepared materials did not show segregation of cerium or zirconium oxides. Highly uniform nanosize solid solution particles of ceria-ziroxidation measurements indicate that the performance of the CeO2-ZrO2 mixed oxides is strongly related to the composition and structure of the oxides. Enhancement of the activity was found for the catalyst prepared by reversed microemulsion method as compared to the sample prepared by sol-gel method.