[en] Mesoporous titanium–zirconium and titanium- cerium oxide materials with different composition (Ce(Zr)=25, 50 and 80 mol %) were prepared by homogeneous precipitation with urea and further calcination at 773 K. The obtained materials were characterized by low temperature nitrogen physisorption, XRD, UV–Vis, FTIR and Raman spectroscopy. Their catalytic activity was tested in methanol decomposition to CO and hydrogen with a potential application as alternative fuel. All binary oxides possess higher specific surface area and higher dispersion as compared to the individual oxides. For the Ti-Zr binary materials the BET surface area passed through a maximum for the sample with equimolar Zr/Ti ratio, while it permanently increased with the decreased of Ce content in Ti-Ce samples. The Raman and XRD data indicated significant structure and morphology changes with the variation of Ce and Zr content due to the formation of mixed oxides. The catalytic behavior of the binary materials in methanol decomposition was in a complex relation with the improved textural characteristics of binary materials and to the specific interaction between the individual oxides, which could be successfully controlled by their composition.