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Ordered mesoporous Zr-Al composite oxide materials (denoted as OMZA-x) with different Zr contents have been synthesized by a solvent evaporation-inducing self-assembly procedure associated with a thermal treatment at 100 °C. A cooperative co-assembly process of amphiphilic triblock copolymer F127 molecules and inorganic hydroxyl species originated from the hydrolysis of Zr and Al precursors was proposed to explain the synthesis of OMZA-x. Compared to ordered mesoporous alumina prepared without introducing Zr species, the resultant OMZA-x exhibited a much more ordered mesostructure combined with a distinct increase in the pore volume and specific surface area. The highly homogenous doping of Zr into the mesopore walls together with the formation of Zr-O-Al bonds can effectively enhance the thermal and hydrothermal stability of OMZA-x. For instance, the ordered mesostructure and excellent textural properties of OMZA-6 prepared with the optimum atomic ratio of Al to Zr of 6 could be well maintained even after a high-temperature treatment at 1000 °C for 1 h or a hydrothermal treatment at 100 °C for 6 h. [ABSTRACT FROM AUTHOR]