<p>This study investigates the synthesis and photocatalytic performance of pure and doped nickel titanium oxide (NiTiO₃) nanoparticles for efficient wastewater treatment. NiTiO₃-based nanoparticles have been synthesized by chemical route. The structural properties of synthesized nanoparticles are studied using Powder X-ray diffraction (XRD). Scanning electron microscopy (SEM) has been performed to investigate the morphological features. Purity and stoichiometry of synthesized materials have been studied using energy-dispersive spectroscopy (EDS). Optical characterizations confirm successful doping and a notable reduction in bandgap energy, with the Zn + Mg co-doped sample exhibiting the lowest bandgap of 1.68&#xa0;eV. Synthesized samples have been used in the intended application as photocatalysts. Under UV light irradiation, the doped samples demonstrate significantly improved photocatalytic activity in degrading methylene blue dye. The Zn + Mg-doped NiTiO₃ achieves a maximum degradation efficiency of approximately 97.41% within 180&#xa0;min, outperforming pristine NiTiO₃ by over ~ 37%. This enhanced performance is attributed to increased defect states and improved charge carrier separation. The values of the rate of reaction for the degradation process have been obtained using pseudo-first-order kinetic plots. The highest rate of reaction is obtained for the Zn and Mg co-doped NiTiO₃ sample, i.e., 0.01787&#xa0;min⁻¹. The recyclability and reproducibility tests are performed for five experimental cycles. These findings underscore the role of dopant engineering in optimizing photocatalytic materials and highlight the potential of NiTiO₃-based systems in sustainable wastewater remediation. The results contribute to advancing the field of photocatalysis by demonstrating a viable pathway for tuning material properties to achieve higher contaminant removal rates.</p>