Mesoporous TiO2/ZrO2 nanocomposition was prepared by sol-gel method with Pluronic P123 and Macrogol 20000 as double templates. The structures and physicochemical properties of the composite were characterized by small-angle and wide-angle powder X-ray diffraction (XRD), Raman scattering studies, N-2 adsorption-desorption. The photocatalytic efficiencies of the products were assessed by monitoring the photodegradation of Rhodamine B (RhB). Compared with the samples prepared by single-template, the pore size of the sample prepared by double templates was larger, and their pore volume was increased. Furthermore, the employment of double templates retarded the crystal phase transformation from anatase-TiO2 to rutile-TiO2, and the obtained mesoporous composite showed high thermal stability. The photocatalytic reactions confirmed that the sample prepared by double templates (the concentration of RhB was 8.37%), showed higher photocatalytic activity than the sample prepared by single template (the concentrations of RhB were 10.31% and 8.96%, respectively). (C) 2012 Elsevier B.V. All rights reserved.