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The nitrogen and fluorine co-doped TiO2 polycrystalline powder was synthesized by calcinations of the hydrolysis product of tetrabutyl titanate with ammonium fluoride. Nitrogen and fluorine co-doping causes the absorption edge of TiO2 to shift to a lower energy region.The photocatalytic activity of co-doped TiO2 with anatase phases was found to be 2.4 times higher than that of the commercial TiO2photocatalyst Degussa P25 for phenol decomposition under visible light irradiation. The co-doped TiO2 powders only contain anatase phases even at 1000℃. Apparently, ammonium fluoride added retarded phase transformation of the TiO2 powders from anatase to rutile.The substitutional fluorine and interstitial nitrogen atoms in co-doped TiO2 polycrystalline powder were responsible for the vis light response and caused the absorption edge of TiO2 to shift to a lower energy region.