This paper investigated the preparation of NiSb/NiSe nanomaterials using a microwave method and explored their electrochemical properties and potential applications in supercapacitors. The NiSb/NiSe nanomaterials were synthesized on nickel foam using microwave radiation, resulting in uniformly distributed flower-like nanostructures. This structure not only provided abundant electrochemical reaction sites, but also improved the electrical conductivity and ion diffusion, contributing to the overall performance of supercapacitors. Electrochemical tests showed that the NiSb/NiSe material exhibited a high specific capacity of 525 mAh g−1 at 1 A g−1 and maintained 65% capacity after 8000 cycles, demonstrating excellent cycling stability and battery-type charge storage capability. In addition, a hybrid supercapacitor assembled using NiSb/NiSe as the anode material and activated carbon (AC) as the cathode material achieved an energy density of 100.34 Wh kg−1 at a power density of 774.9Wkg−1, significantly enhancing energy storage efficiency. The effect of different microwave powers and reaction times on the morphology and electrochemical properties of the materials were further investigated, with the optimal preparation conditions found to be 800 W and 150 s. The NiSb/NiSe materials synthesized under this condition not only have the best electrochemical properties, but also exhibit low charge transfer impedance and excellent electrical conductivity. In summary, NiSb/NiSe flower-like nanomaterials as supercapacitor electrode materials demonstrate great potential for energy storage applications due to their high specific capacity, good cycling stability and high energy density.
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