Nitrogen doped TiO2 (N/TiO2) photocatalysts were prepared using a mechanochemica1 method with raw amorphous TiO2 as precursors and various nitrogenous compounds doses (NH4F, NH4HCO3, NH3·H2O, NH4COOCH3, and CH4N2O). The photocatalysts were characterized by X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), and UV-Vis diffuse reflection spectra (UV-Vis-DRS). Their photocatalytical activities were evaluated with the degradation of p-nitrophenol and methyl orange under UV or sunlight irradiation. The catalysts had a strong visible light absorption which corresponding to doped nitrogen and consequent oxygen deficient. Concentration of the nitrogen substances also affected the visible light adsorption of the TiO2. The XPS results indicated the doped nitrogen in the TiO2 may exist in the formation of O2Ti−N−H and/or O2Ti−N, nitrogen was in form of interstitial atom. The results of photocatalytic activity showed the visible light adsorption mechanisms, as the doped nitrogen species gave rise to a mid-gap level slightly above the top of the (O-2p) valence band, but not from the mixed band gap of the N-2p and O-2p electronic levels.