We report on the synthesis of N-F-codoped TiO2 powders with a homogenous anatase structure via a thermal decomposition of the ammonium oxofluorotitanate ((NH4)(0.3)TiO1.1F2.1, NH4TiOF3 and (NH4)(2)TiOF4) precursors at 550 degrees C for 1 h in air. The ammonium oxofluorotitanate precursors were synthesized by a wet chemical method in the mixture of deionized water and absolute ethanol using titanium tetrachloride (TiCl4) and ammonium fluoride (NH4F) as reactants. The as-prepared samples were characterized by X-ray powder diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), thermogravimetry-differential scanning calorimetry (TG-DSC). Fourier transform infrared (FR) spectroscopy, X-ray photoelectron spectroscopy (XPS) and UV-vis spectroscopy. The results from XRD, TG-DSC and FTIR analyses confirmed a complete thermal conversion of the ammonium oxofluorotitanate precursors to N-F-codoped anatase TiO2 at a temperature of > 500 degrees C. The SEM and TEM observations exhibited that the morphologies of the precursors were not considerably affected by the thermal treatment at 550 degrees C for 1 h. The XPS data proved the presence of the nitrogen and fluorine atoms in the TiO2 structure. According to the resulting UV-vis spectra, the as-prepared samples demonstrated a strong visible-light absorbance in the wavelength range of 400-550 nm. The photocatalytic activity of the N-F-codoped anatase TiO2 was evaluated through a study of the decomposition of methyl orange under visible light irradiation. It was found that the sample derived from the (NH4)(0.3)TiO1.1F2.1 precursor by thermal treatment at 550 degrees C for 1 h showed much higher photocatalytic activity compared to the commercial undoped TiO2 (Degussa P25) due to the synergetic effects of a strong absorption in the visible-light region, red shift in absorption edge, good crystallinity, and porous structure. (C) 2011 Elsevier B.V. All rights reserved.