In this work the synthesis of ZrO₂-CeO₂ and ZrO₂-CeO₂/SiO₂ were developed, based on the process to form ordered mesoporous materials such as SBA-15 silica. The triblock copolymer Pluronic P-123 was used as template, aiming to obtain crystalline single phase walls and larger specific surface area, for future applications in catalysis. SAXS and XRD results showed a relationship between ordered pores and the material crystallization. 90% of CeO₂ leaded to single phase homogeneous ceria-zirconia solid solution of cubic fluorite structure (Fm3¯m). The SiO₂ addition improved structural and textural properties as well as the reduction behavior at lower temperatures, investigated by XANES measurements under H₂ atmosphere.