In this paper, F-TiO2 and TiN/F-TiO2 nanoparticle photocatalysts were prepared by ball milling. The photocatalysts were characterized by X-ray powder diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), terephthalic acid photoluminescence probing technique (TA-PL), X-ray photoelectron spectroscopy (XPS), and UV-vis diffuse reflection spectroscopy (DRS). The photocatalytic activity of the photocatalysts was evaluated by photocatalytic degradation of methylene blue (MB) and rhodamine B (RhB). The results showed that the photocatalytic activity of the F-TiO2 was much higher than that of TiO2, and the photocatalytic activity of the TiN/F-TiO2 was much higher than that of TiO2 and F-TiO2 under UV light irradiation. The optimum percentage of doped TiN is 0.2 wt.%. Compared with pure TiO2, the photoabsorption wavelength range of the TiN/F-TiO2 and F-TiO2 photocatalysts red shifts and improves the utilization of the total spectrum. The effect of ball milling time on the photocatalytic activity of the photocatalysts was also investigated. The optimum ball milling time is 12 h. The mechanisms of influence on the photocatalytic activity of the photocatalysts were also discussed. (C) 2010 Elsevier B.V. All rights reserved.