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 TiO2 photocatalyst Degussa P25 for phenol decomposition under visible light irradiation. The co-doped TiO2 powders only contain anatase phases even at 1000 degrees C. 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.

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