A supercapacitor (SC) is a device that possesses outstanding potential to impart significant breakthroughs in energy storage. The current study deals with an experimental investigation in developing NiCo layered double hydroxides/reduced graphene oxide (rGO)/ Bismuth sulfide ( \(NiCo - LDHs/rGO/Bi_{2} S_{3}\) ) nanocomposites and exploring its characterization as well as electrochemical measurement. A simple and facile hydrothermal synthesis process was used to prepare \(NiCo - LDHs/rGO/Bi_{2} S_{3}\) nanocomposite. Efficient straightforward and adaptable synthetic approach is implemented to prepare the nanocomposite. In the present investigation X-ray diffraction(XRD), Scanning Electron Microscope (SEM), Energy Dispersive Spectroscopy(EDS), Transmission electron microscopy (TEM), Raman spectroscopy are applied for the characterization while cyclic voltammetry (CV), galvanic charge discharge (GCD), and electrochemical impedance spectroscopy (EIS) are used for electrochemical measurement of the nanocomposite. In the present study, the as-prepared \(NiCo - LDHs/rGO/Bi_{2} S_{3}\) nanocomposite exhibits rod type structure. The nanocomposite exhibits a decreased band gap and greater free electrons, suggesting that the nanocomposite favors electron transport. The \(NiCo - LDHs/rGO/Bi_{2} S_{3}\) nanocomposite possesses significantly high specific capacitance \(\left( {S_{c} } \right)\) value of 1139 F/g at current density (CD) of 1 A/g compared to that of NiCo-LDHs/rGO and \(Bi_{2} S_{3} /rGO\) . Further, the nanocomposite exhibits energy density (ED) of 36.86 Wh/kg and power density (PD) of 919 W/kg at a current density of 1 A/g. Because of its non-toxicity, plentiful availability, environment friendly and cost effectiveness, the as-developed nanocomposite finds significant real-world applications in SCs.