CeO 2 -ZrO 2 solid solutions were prepared by means of thermal decomposition of cerium zirconyl oxalate in an argon flow at 1273 K followed by oxidation at 673-873 K in air. The reduction behavior of the obtained CeO 2 -ZrO 2 powders was investigated and compared with the samples prepared by the other methods already reported to yield CeO 2 -ZrO 2 powders with high redox activity. The CeO 2 -ZrO 2 samples prepared from the oxalate showed excellent reduction behavior, despite their very low surface areas. The reason for the excellent oxygen evolution behavior of the powders was discussed, from the viewpoints of the structure and the preparation process, and was attributed to both the appearance of a cubic phase with a different oxygen arrangement and the reduction by carbon formed in the sample preparation process.