采用溶胶 -凝胶法和有机溶剂分解法 ,制备了 Ce- Zr固溶体 .应用 XRD和 L RS谱测试 ,详细研究了经不同温度焙烧后固溶体的结构、晶相和热稳定性 ,并进行了储氧量、比表面积的测定和催化活性评价 .结果表明 ,XRD和 L RS相结合 ,可以较好地表征固溶体的结构和纯度 ;固溶体的纯度、晶相和储氧量与制备方法有直接关系 ,溶胶 -凝胶法能制得纯度高的萤石型富铈固溶体 ,并且储氧量高 ,但热稳定性较有机溶剂分解法制得的固溶体差 ;含富铈固溶体的三效催化剂老化后的催化活性明显高于含纯 Ce O2 的三效催化剂 Ce-Zr solid solution was prepared by sol-gel method and organic solvent decomposition method. The structure, crystal phase and thermal stability of the solid solution after calcination at different temperatures were studied in detail by XRD and LRS spectroscopy. The results showed that the structure and purity of the solid solution can be well characterized by the combination of XRD and L RS. The purity, crystal phase and oxygen storage capacity of the solid solution are directly related to the preparation method. The sol-gel method can produce fluorite-type cerium-rich solid solution with high purity and high oxygen storage capacity, but its thermal stability is worse than that obtained by organic solvent decomposition. The three-way catalyst with cerium-containing solid solution Activity was significantly higher than the pure Ce O2 containing three-way catalyst