In this study, a novel MoS2/NiO nanoflower decorated with different concentrations NiO nanoparticles (0, 2, 5, 8, and 12 wt%) was synthesized via the hydrothermal method. The FESEM illustrated spherical flower-like morphology for three-dimensional structures of both MoS2 and MoS2/NiO nanocomposite. XRD analysis confirmed the formation of the MoS₂/NiO nanocomposite without any indication of a new phase. Raman spectroscopy of MoS₂/NiO nanoflowers exhibited a shift of the first-order peaks to lower frequencies, indicating n-type doping due to the incorporation of NiO. The electrochemical properties of the nanocomposite were found to be improved due to the incorporation of the NiO nanoparticle into it. The MoS₂/12 wt% NiO offers a specific capacitance of 154.45 F g-1, which is 6.5 times larger than that of the MoS₂ (23.48 F g-1) nanoflower. It exhibited remarkable energy storage capacity and maintained 85% capacitance even after 10,000 charge-discharge cycles. The electrochemical impedance spectroscopy showed that the incorporation of NiO nanoparticles reduced charge transfer resistance, enhancing ion intercalation and electronic conductivity which boosted charge carrier kinetics in the MoS₂/NiO nanocomposite, thereby improving its overall electrochemical performance. The nanostructured MoS₂/NiO, fabricated through a straightforward and low-cost method with enhanced specific capacitance and increased stability, holds promise for developing efficient, eco-friendly, and affordable energy storage devices.