In this study, a solvothermal method is used to synthesizes MOF-derived NiO/Ni composites and NiO samples at various calcination temperatures (350 °C, 450 °C, 550 °C, and 650 °C) and durations (4, 5, 6, and 7 h). The NiO/Ni sample calcined at 450 °C for 5 h (NiO/Ni-450) exhibits the highest specific capacitance (Cs) of 410 Fg⁻¹ at a scan rate of 5 mV s⁻¹. This superior performance results from the combined benefits of Ni's metallic conductivity and NiO's redox activity. In a 1 M KOH electrolyte, NiO/Ni-450 retains about 83 % of its initial capacitance after 2,000 cycles. The NiO sample formed by calcining NiO/Ni-450 for 5 h (H5) achieves a specific capacitance (Cs) of 371 Fg⁻¹ and retains 80 % of its capacitance after 2,000 cycles. NiO/Ni-450 and H5 demonstrate energy densities (Ed) of 8.58 and 5.48 Wh kg⁻¹, and power densities (Pd) of 608 and 500 W kg⁻¹, respectively. An asymmetric supercapacitor using NiO/Ni-450 and activated carbon (AC) shows an impressive 80 % capacitance retention after 9,000 cycles, with a Cs of 123 Fg⁻¹, and Ed and Pd values of 14.58 Wh kg⁻¹ and 4038 W kg⁻¹, respectively, highlighting the potential for industrial-scale production of these materials for energy storage.