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TiO2/Nb2O5 photocatalyst loaded with WO3 (WO3-TiO2/Nb2O5) was prepared by a modified hydrolysis process, and characterized by X-ray diffractometry, transmission electron microscopy, Raman spectra and UV-Vis diffuse refraction spectroscopy.The photocatalytic activity of WO3-TiO2/Nb2O5 was investigated by employing splitting of water for O2 evolution. The results indicate that WO3 loading can pronouncedly improve the photocatalytic activity of TiO2/Nb2O5 by using Fe3+ as an electron acceptor under UV irradiation. The optimum molar fraction of the loaded WO3 is 2%, and the largest speed of O2 evolution for 2%WO3-TiO2/Nb2O5 catalyst is 151.8 μmol/(L·h).