Abstract: In this research, novel visible light–induced Fe₂O₃–carbon nitride intercalation compound (CNIC) composite photocatalyst with different content of α–Fe₂O₃ were synthesized through simple mixing and heat treatment. The composite photocatalyst was characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), UV–vis diffuse reflection spectroscopy, Fourier transform infrared (FT–IR) spectroscopy and BET surface area measurements. The photocatalytic oxidation ability of the novel composite photocatalyst was evaluated employing methyl orange (MO) as a target pollutant. The experimental results show that Fe₂O₃–CNIC composites with 20% or 30% α–Fe₂O₃ exhibited the higher photocatalytic activity than either single–phase α–Fe₂O₃ or CNIC under visible-light irradiation. The as–prepared composite photocatalyst exhibitedan improved photocatalytic activity due to enhancement of photo-generated electron-hole separations at the interface.