The present work reports the synthesis of nanoparticles of nickel sulfide (NiS), zinc sulfide (ZnS), and NiS/ZnS nanocomposites using hydrothermal method followed by their analytical characterizations. Field emission scanning electron microscopic survey confirms the star-like, spherical and mixture of both shapes for the NiS, ZnS and NiS/ZnS nanocomposites, respectively, whereas EDX spectrum corroborates the chemical purity of as-synthesized nanomaterials. Optical band gap of NiS, ZnS and nanocomposite, as determined by the tauc’s plot method, were found 4 eV, 3.8 eV, and 4.2 eV, respectively. Cyclic voltammetry and galvanostatic charge-discharge have been measured and a maximum specific capacitance of 1594.68 F/g is observed at a scan rate of 5 mV/S for the composite material with a charging/discharging time of 461.97sec. Owing to Conducive performance and potential of the as-synthesized NiS/ZnS nanocomposite for electrochemical studies, suggests their appropriateness for pseudo-capacitor application