Herein, FeS 2 @TiO 2 nanotubes photocatalyst was prepared by electrochemical anodization method followed by successive ionic layer adsorption and reaction method, and then finally annealed in a tube furnace for homogenous crystallization. The surface morphology, elemental composition, optical properties, and crystalline structure of the prepared FeS 2 @TiO 2 nanocomposite were found out by performing scanning electron microscopy, energy dispersive X-ray spectroscopy, X-ray diffraction, UV-Vis diffuse reflectance spectroscopy, and fluorescence spectroscopy, respectively, while bonds vibrations and various functional groups' presence were analyzed using Raman and Fourier transform infrared spectroscopy. A higher photocurrent density of 1.59 mA/cm 2 at 0.3 V versus reference electrode of Ag/AgCl (1.23 V versus reversible hydrogen electrode) using 100 mW/cm 2 intensive light source was shown by 15-FeS 2 @TiO 2 nanotubes (uniformly loaded photoanode) while donor density (N D ) of 3.68 Â 10 À13 cm À3 as compared to pure TiO 2 NTs (0.09 mA/cm 2 ), 05-FeS 2 @TiO 2 NTs (0.19 mA/cm 2 ), 10-FeS 2 @TiO 2 NTs (0.53 mA/cm 2 ) and 20-FeS 2 @TiO 2 NTs (0.61 mA/cm 2 ), respectively. The exceptional photoelectrochemical activity results were attributed to the homogenous integration of FeS 2 that not only increase the charge separation but also, intensively interacted with the substrate (TiO 2 nanotubes), which results in an excellent photoelectrochemical activity.