Pure NiO, N-doped, Fe-doped, N and Fe codoped NiO NPs were fabricated via a precipitation process. The powder X-ray diffraction (XRD) revealed the face centered cubic phase of NiO products. The full width at half maximum (FWHM) of the XRD peak was steadily enlarged with the order of elements N, Fe, N/Fe doped to NiO, and shifted towards a greater angle due to decrease in grain size, as shown by XRD. The average crystallite size of NiO products was calculated, ranging from 6.67 to 3.76 nm, according to the Debye Scherrer formula. The scanning electron microscopy (SEM) demonstrated considerable morphological changes in the produced nanoparticles, including those directed to rock-like geometries (NiO and Fe/NiO nanoparticles) while gas covered-nanocrystals (N/NiO and N/Fe/NiO nanoparticles) were formed using precipitation method. The particle size range of 10–50 nm was estimated using the bar scale in transmission electron microscopy (TEM) pictures. The elemental composition of Ni, O, Fe and N atoms in the respected samples was analyzed by Energy Dispersive X-Ray Analysis (EDX). Photoluminescence (PL) showed band edge emission at 370 nm. The band edge-absorption peak, which is caused by electronic transitions between energy levels, is determined to be in the range 314–325 nm. A UV–Vis analysis found an energy gap amid 3.2 eV and 2.5 eV. The chemical condition of the Fe and N doped NiO composites were validated using XPS. Using visible photo application of undoped and doped NiO NPs, the degradation of an azo dye termed methylene blue was examined. It was N/Fe/NiO (79.8%), Fe/NiO (76%), N/NiO (73%), and NiO (62%) throughout the 6 h irradiation duration. Increased production of OH• radicals was detected in fluorescence tests using terephthalic acid (TA) for N/Fe/NiO NPs, indicating the higher photo-degradation described. Furthermore, the degradation trends of both undoped and doped NiO NPs closely matched the pseudo first order kinetics, according to the kinetic analysis. There was also a suggestion for a thorough MB breakdown mechanism.