The abundant active sites, high theoretical capacitance, and cost-effective synthesis of transition metal oxides@sulfides (TMOs@TMSs) have made them a highly desirable choice as active electrode materials for supercapacitors. This study demonstrated the successful fabrication of a CuCo2O4@CdS nanoheterostructure electrode using a simple and economical co-precipitation method The morphology, physicochemical properties, and electrochemical behavior of this electrode were subsequently studied. The synthesized CuCo2O4@CdS nanoheterostructure was characterized using Infrared Fourier-transform spectroscopy, X-ray diffraction, Raman spectroscopy, energy dispersive X-ray spectroscopy, X-ray photoelectron spectroscopy, scanning electron microscopy, High-resolution transmission electron microscopy, N2 adsorption/desorption isotherms and atomic force microscopy. The electrochemical performance was studied using cyclic voltammetry, impedance spectroscopy, and galvanostatic charge-discharge (GCD) measurements with a 6 Molar KOH aqueous electrolytic solution. Results from powder X-ray diffraction pattern and energy dispersive X-ray revealed the formation of CuCo2O4@CdS nanoheterostructure. Furthermore, SEM images showed the formation of more spherical structures in nanoheterostructure. The results of optical measurements of thin films were analyzed, which showed an increase in the energy gap (Eg) of CuCo2O4 nanoparticles when combined with cadmium sulfide (CdS). Additionally, the intensity of photoluminescence of the CuCo2O4@CdS nanoheterostructure was lower compared to the pure nanoparticles. Moreover, the newly synthesized CuCo2O4@CdS nanoheterostructure showed a specific capacitance of 257.5 F g−1 at a current density of 0.5 A g−1 via a three-electrode galvanostatic charge-discharge system, respectively. In the asymmetric device, the supercapacitor yielded an optimum energy density and power density of 19.6 Wh kg−1 and 700 W kg−1 at 1 A g−1 current density, respectively. Although the capacitance retention was maintained at nearly 85.2 % after 4000 cycles at a current density of 3 A g−1.
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