In this work, Nickel (Ni) and sulfur (S) codoped TiO2 nanoparticles were prepared by a sol-gel technique. The as-prepared catalyst was characterized using X-ray diffraction (XRD), Fourier transforms infrared spectroscopy (FTIR), FT-Raman spectroscopy, scanning electron microscopy (SEM), energy dispersive spectrometer (EDS), transmission electron microscopy (TEM), UV-Vis diffuse reflectance spectra (DRS) for investigating crystal structure, crystal phase, particle size and bandgap energy of these samples. The photocatalytic performances of all the prepared catalysts have been investigated for the degradation of methylene blue (MB) under visible light irradiation. It was noticed that Ni-S codoped TiO2(Ni-S/TiO2) nanoparticles exhibited much higher photocatalytic activity compared with pure, Ni and S doped TiO2 due to higher visible light absorption and probable decrease in the recombination of photo-generated charges. It was decided that the great visible light absorption was created for codoped TiO2 by the formation of impurity energy states near both the edges of the collection, which works as trapping sites for both the photogenerated charges to decrease the recombination process.