Abstract: By one-step in situ synthesis at low temperature, NiCo₂S₄ nanoarray, hierarchical three-dimensional network structured and with the nickel foam as base, was obtained.The product was characterized by SEM amd XRD, and its electrochemical properties were investigated.The results showed that due to the unique layered network structure, the NiCo₂S₄ nanoarray could not only provide a large number of electrochemical active sites, but had good electron transfer capacity.The area specific capacitance of the electrochemical properties of NiCo₂S₄@ foam nickel electrode could reach 10.15 F/cm² when the current density was 20 m A/cm², and when the current density increased to 100 m A/cm², the area specific capacitance was 7.29 F/cm², showing excellent capacitance retention; when the load of NiCo₂S₄ was 14.8 mg, the current density was 20 m A/cm², and the electrode was charged and discharged for 5 000 times, the capacitance retention rate was 72.5%, demonstrating good cycling stability of the NiCo₂S₄@ foam nickel electrode.