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The synthesis and characterisation of Ti–Zr mixed oxides containing 1 to 10 wt.% of Zr is herein reported. In addition, the samples were tested as photocatalysts in the generation of hydrogen from aqueous methanol solutions. The solids were prepared by sol-gel and then characterised by X-ray diffraction, high resolution electron microscopy, X-ray photoelectron spectroscopy, physisorption of nitrogen, scanning electron microscopy, UV-vis and Raman spectroscopies. The results show the presence of anatase as a predominant structure and the oxides present larger specific surface areas than that of pure titania. A maximum value of 168 m2/g was determined for the sample with 5 wt.% of zirconium. The calculated band gap energies varied from 3.05 to 3.15 eV. It was observed that the greater the zirconium content in the solid, the higher the generation rate of hydrogen when testing the Ti–Zr solids as photocatalysts. Under our experimental conditions, the best catalyst, Ti–Zr oxide with 10 wt.% Zr, showed a production rate of 2100 μmol of H2/h which was about tenfold higher than that observed for pure titania. [ABSTRACT FROM AUTHOR]