Heating　reflux　aging　technology　was　first　applied　to　obtain　a　series　of　ceria　zirconia　mixed　oxides　composed　of　0.6CeO(2)-0.4ZrO(2).　N-2　physical　adsorption,　FT-Raman,　and　UV-Vis　diffuse　spectroscopy　techniques　were　preformed　to　investigate　the　relationships　between　the　structure　and　oxygen　storage　capacity　of　ceria　zirconia　mixed　oxides　prepared　at　different　pH　value　of　precipitation.　The　composition　of　ceria　zirconia　mixed　oxides　fluctuated　with　the　pH　value　of　precipitation,　leading　to　the　variation　in　the　phase　ingredients,　defects,　crystallization　and　texture.　Controlling　the　pH　value　of　precipitation　at　10.5-11.0　can　avoid　the　introduction　of　Si,　improve　the　texture,　phase　homogeneity　and　defects　concentration,　decrease　the　degree　of　crystallization,　and　increase　the　oxygen　storage　capacity.