The development of advanced energy storage materials is crucial for the evolution of high-performance supercapacitors. Recently, nickel-cobalt layered double hydroxides (NiCo LDHs) stand out due to their synergistic effects and abundant redox-active sites, which contribute to superior electrochemical performance. Herein, we design simple cyclic voltammetry-assisted electrochemical synthesis of thin-film NiCo LDHs on stainless steel mesh as a binder-free electrode, which demonstrates enhanced redox-type charge storage and excellent durability. Specifically, the synthesized NiCo LDHs exhibits a porous, sheet-like architecture, confirmed through various structural characterization techniques. Electrochemical measurements in 1M KOH electrolyte showed significant diffusion-contributed capacity in the NiCo LDHs thin films, demonstrating high specific capacitance of 1406.7 F/g (633 C/g) and excellent cycling stability 83%. Moreover, the NiCo LDHs exhibited high energy density of 97.6 Wh/g at a power density of 1666.7 W/kg, respectively. Our work provides the facile cyclic voltammetry method for direct, scalable deposition, providing a straightforward route to optimize redox-active LDHs for efficient supercapacitor applications, highlighting the potential for advanced energy storage solutions.
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