The composite photocatalyst, N-TiO 2 loaded with Ni 2 O 3 , was prepared by N 2 plasma treatment. X-ray diffraction, X-ray fluorescence, N 2 adsorption, UV-vis spectroscopy, photoluminescence, and X-ray photoelectron spectroscopy were used to characterize the prepared TiO 2 samples. The results indicated that the band gap energy was decreased obviously by nitrogen doping, whereas loading of Ni 2 O 3 did not influence the band gap and visible light absorption. The photocatalytic activities were tested in the degradation of 2,4,6-trichlorophenol (TCP) under visible light. The photocatalytic activity and stability of composite photocatalyst were much higher than that of catalyst modified with nitrogen or Ni 2 O 3 alone. The synergistic effect of doping nitrogen and Ni 2 O 3 over TiO 2 was investigated.