Nickel-cobalt layered double hydroxides (LDHs) are promising materials for supercapacitor electrodes; however, they face challenges in terms of cycling stability and rate capability owing to agglomeration and low conductivity. In this study, Ni(III)CoAlx-LDH/GO with an extended layer spacing and excellent electronic conductivity was synthesized by one-step glow discharge electrolysis. A nickel–cobalt alloy was used as the anode, a graphite rod as the cathode, and sodium chloride as the electrolyte. In addition, incorporating an appropriate amount of aluminum chloride into the electrolyte can alter the microstructure of the electrode material, leading to enhanced electrochemical performance. Ni(III)CoAl0.2-LDH/GO, synthesized using 0.2 g AlCl3, demonstrated exceptional electrochemical performance of 1014C g−1 at 2 A/g. At a current density of 5 A/g, the capacitance retention rate was 85.3 % after 10,000 cycles, indicating strong cyclic stability. Moreover, an asymmetric supercapacitor built with Ni(III)CoAl0.2-LDH/GO as the anode and commercial activated carbon as the cathode achieved a specific capacitance of 146.2F/g at a current density of 1 A/g. This device demonstrated outstanding circular stability, retaining 85.07 % of its capacitance after 10,000 cycles. In addition, the device achieves relatively high energy density and power density (energy density of 66.63 Wh kg−1 at a power density of 1022.23 W kg−1). This study introduces a novel synthesis method for the preparation of high-performance electrode materials aimed at advancing energy storage devices.
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