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Fe3+-doped TiO2 composite nanoparticles with different doping amounts were successfully synthesized using sol-gel method and characterized by X-ray diffraction (XRD),transmission electron microscopy (TEM) and ultraviolet-visible spectroscopy (UV-Vis) diffuse reflectance spectra (DRS). The photocatalytic degradation of methylene blue was used as a model reaction to evaluate the photocatalytic activity of Fe3+/TiO2 nanoparticles under visible light irradia-tion. The influence of doping amount of Fe3+ (ω: 0.00%-3.00%) on photocatalytic activities of TiO2 was investigated.Results show that the size of Fe3+/TiO2 particles decreases with the increase of the amount of Fe3+ and their absorptionspectra are broaden and absorption intensities are also increased. Doping Fe3+ can control the conversion of TiO2 from anatase to rutile. The doping amount of Fe3+ remarkably affects the activity of the catalyst, and the optimum efficiency occurs at about the doping amount of 0.3%. The appropriate doping of Fe3+ can markedly increase the catalytic activity of TiO2 under visible light irradiation.