In order to prepare electrode materials with high specific capacitance and good cycling stability, spinel-type NiCo2O4 microspheres were prepared by surfactant-assisted co-precipitation using polyvinylpyrrolidone (PVP) as a surfactant, and the effects of surfactant dosage and alkali source on the electrochemical performances of NiCo2O4 materials were explored. The results show that the prepared NiCo2O4 electrode material has the best capacitance performance when the dosage of polyvinylpyrrolidone is 1.5 g and the alkali source is NaOH, and the specific capacitance reaches 642.8 F/g at a current density of 1 A/g. Meanwhile, the capacity retention rate of 73.6% is achieved after 1000 cycles of constant-current charging/discharging, showing a good cycling stability.