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Co-doped NiTiO₃/g-C₃N₄ composite photocatalysts were prepared by a modified Pechini method to improve their photocatalytic activity toward methylene blue photodegradation under visible light irradiation. The combination of Co-doped NiTiO₃ and g-C₃N₄ and Co-doping into the NiTiO₃ lattice synergistically enhanced the photocatalytic performance of the composite photocatalysts. X-ray photoelectron spectroscopy results for the Co-doped NiTiO₃/g-C₃N₄ composite photocatalysts confirmed Ti-N linkages between the Co-doped NiTiO₃ and g-C₃N₄. In addition, characteristic X-ray diffraction peaks for the NiTiO₃ lattice structure clearly indicated substitution of Co into the NiTiO₃ lattice structure. The composite structure and Co-doping of the C-<i>x</i> composite photocatalysts (<i>x</i> wt % Co-doped NiTiO₃/g-C₃N₄) not only decreased the emission intensity of the photoluminescence spectra but also the semicircle radius of the Nyquist plot in electrochemical impedance spectroscopy, giving the highest <i>k_app</i> value (7.15 × 10⁻³ min⁻¹) for the C-1 composite photocatalyst.