Abstract: In this study, nickel sulfide (NiS), zinc sulfide (ZnS), and their composites have been synthesized by using surfactant driven hydrothermal method. Synthesized materials are investigated using X-ray diffraction (XRD), scanning electron microscopy (SEM), energy-dispersive X-ray spectroscopy (EDX), Fourier-transform infrared spectroscopy, UV–Vis and Photoluminescence spectroscopy. XRD results have shown the presence of corresponding structural planes. Crystallite size was much smaller (15 nm) in the case of ZnS nanomaterials, whereas, composite materials have shown size comparable to NiS nanomaterials. SEM images presented morphology of star-like, spherical, and mixture of two for NiS, ZnS, and NiS/ZnS nanocomposites respectively. EDX spectrum of composite materials showed Nickel, Zinc, and Sulfur, indicating the purity of the synthesized composite. Electrochemical measurements i.e. cyclic voltammetry and galvanostatic charge–discharge were determined for all three materials. Maximum specific capacitance is obtained as 1594.68 F g−1 at a scan rate of 5 mV S−1 for NiS/ZnS composite materials whereas a charging/discharging time of 461.97 s is observed. The composite materials have shown 95.4% retention for applied for 3000 charging–discharging cycles. The favorable behavior of NiS/ZnS composites indicated their potential as an electrode material for pseudo-capacitors.