The goal of the present work is to create ZnO/NiO nanocomposites (NCs) for the photocatalytic destruction of organic contaminants using the co-precipitation technique. To investigate physiochemical characteristics, FT-IR, UV visible spectroscopy, SEM, and XRD were used. The ZnO hexagonal phase and the NiO cubic phase in the ZnO/NiO NCs were verified by the diffraction pattern. NCs were discovered to have larger average crystallite sizes. The bandgap energy calculated from the Tauc plot for the ZnO is 3.02 and 2.74 eV for the ZnO/NiO NC's. SEM analysis revealed the morphological study and particle size was calculated using the histogram technique and found to be 124.5 nm for the ZnO and 49.2 nm for the ZnO/NiO NCs. Photocatalytic degradation in the presence of sunlight showed 72.8% degradation of Methylene blue (MB) for the ZnO and 79.2% for the ZnO/NiO NCs. The increase in the photocatalytic capablity for the NCs is attributed to the synergistic effect between ZnO and NiO which effectively separated charge carriers preventing greater recombination rate. The robustness of ZnO/NiO NCs as a catalyst option was shown by their exceptional performance.