Abstract: The un-doped, single-doped and co-doped TiO2 nanopaticles have been synthesized by hydrothermal method at 150°C. The prepared samples were characterized by X-ray diffraction (XRD), field emission scanning electron microscopy (FE-SEM), Fourier transform infrared (FT-IR), Ultraviolet and visible spectroscopy (UV–vis), X-ray photoelectron spectroscopy (XPS) and BET method. The results showed that anatase was the predominant phase and specific surface area was about 201m2/g. for the N, Fe co-doped TiO2. Compared to un-doped TiO2, N-TiO2、Fe-TiO2 and P-25, the absorption edge of the N, Fe co-doped TiO2 shifted to longer wavelength and its photocatalytic activity for degradation of methyl orange (MO) under Xe-lamp (350W) was higher. [ABSTRACT FROM AUTHOR]