The present work accentuates the aspects of electrochemical analysis determined by Cyclic Voltammeter(CV), especially enhancement in Supercapacitor's specific capacitance and energy density. In this work, Nickel Oxide (NiO) and Nickel Oxide @ reduced Graphene Oxide ([email protected]) nanocomposite materials using as electrodes synthesized by the Microwave irradiation method. Performance of the synthesized material further characterized using X-Ray diffraction (XRD), Fourier Transform Infrared Spectroscopy (FTIR), Field-Emission Scanning Electron Microscope (FE-SEM), BET(Brunauer–Emmett–Teller) specific surface-area, Thermo Gravimetric Analysis (TGA), and CV. Electrochemical performance of active material at three different molarities (2M, 4M & 6M) of potassium hydroxide (KOH) as an electrolyte is analyzed and observed decline in specific capacitance for synthesized nanocomposite materials in a lower state of electrolyte concentration. Accordingly, Specific capacitances at 1A/g are 270F/g, 395 F/g at 1A/g current density, and Energy densities of 10.2Wh/Kg, 17.55Wh/Kg are observed for NiO and [email protected] respectively at 6M KOH.