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Graphitic carbon nitride (G-C3N4) and NiS-NiO/G-C3N4 nanocomposite have been synthesized via combustion and hydrothermal techniques, respectively. The chemical and morphological properties of these materials were confirmed using different analytical methods. SEM confirms the formation of G-C3N4 sheets containing additional petal-like shapes of NiS-NiO nanoparticles. The electrochemical testing of NiS-NiO/G-C3N4 symmetric supercapacitors is carried out from 0.6 M HCl electrolyte. Such testing includes charge/discharge, cyclic voltammetry, impedance, and supercapacitor stability. The charge/discharge time reaches 790 s at 0.3 A/g, while the cyclic voltammetry curve forms under a high surface area. The produced specific capacitance (C_S) and energy density values are 766 F/g and 23.55 W.h.kg⁻¹, correspondingly.