High-performance supercapacitors (SCs) are becoming the preferred energy storage technology for future technological advancements. Techniques such as interfacial engineering and the use of dopants are being employed to improve their effectiveness. The hybridized nanostructure plays a crucial role in enhancing the overall electrochemical performance. Here, we propose an electrochemical method for the fabrication of the CuO@S-NiV LDH core−shell electrode for SC application. The initial investigation focuses on the effect of sulfur (S) doping in NiV LDH on its structural, morphological, and SC characteristics. The CuO@S-NiV LDH(1:1) core−shell electrode, fabricated with CuO as the core and S-doped NiV LDH as the shell, showed a maximum areal capacitance of 1072 mF cm −2 and maintained 93% stability over 5000 cycles. Besides, the fabricated aqueous CuO@S-NiV LDH(1,1)//NF@AC asymmetric supercapacitor (ASC) exhibited a maximum energy density of 26 Wh kg −1 and a power density of 1001 W kg −1 . It also demonstrated satisfactory cycling stability, retaining 93% of its capacitance over 5000 cycles, indicating a promising potential for a highperformance SC. This work paves the way for fabricating high-areal-capacitance electrodes for smart and wearable energy storage devices.