| Summary: | The rational fabrication of composite structures made of mixed components has shown great potential for boosting the energy density of supercapacitors. Herein, an elaborate hierarchical MOF-derived NiCo<sub>2</sub>S<sub>4</sub>@Mo-doped Co-LDH arrays hybrid electrode was fabricated through a step-wise method. By leveraging the synergistic effects of a uniform array of NiCo<sub>2</sub>S<sub>4</sub> nanowires as the core and an MOF-derived porous shell, the NiCo<sub>2</sub>S<sub>4</sub>@Mo-doped Co-LDH hybrid electrode demonstrates an exceptional specific capacitance of 3049.3 F g<sup>−1</sup> at 1 A g<sup>−1</sup>. Even at a higher current density of 20 A g<sup>−1</sup>, the capacitance remains high at 2458.8 F g<sup>−1</sup>. Moreover, the electrode exhibits remarkable cycling stability, with 91% of the initial capacitance maintained after 10,000 cycles at 10 A g<sup>−1</sup>. Additionally, the as-fabricated asymmetric supercapacitor (ASC) based on the NiCo<sub>2</sub>S<sub>4</sub>@Mo-doped Co-LDH electrode achieves an impressive energy density of 97.5 Wh kg<sup>−1</sup> at a power density of 835.6 W kg<sup>−1</sup>. These findings provide a promising approach for the development of hybrid-structured electrodes, enabling the realization of high-energy-density asymmetric supercapacitors.
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