Abstract: One-step solvothermal method is employed to synthesize spinel-type NiCo₂O₄ electrode materials with various microstructures. The synthesis method is facile and efficient, and the final samples can be directly obtained without the subsequent calcination process, which is feasible to realize the large-scale fabrication. The composition and microstructures of NiCo₂O₄ are investigated by Raman, XRD, FT-IR and FE-SEM, and electrochemical performance is studied by cyclic voltammetry (CV), galvanostatic charge and discharge (GCD) and electrochemical impedance spectroscopy (EIS). It turns out that reaction time of the solvothermal has effect on the microstructure and electrochemical properties of NiCo₂O₄. NiCo₂O₄ microspheres can be obtained when the solvothermal reaction is at 120℃ for 12 h. Moreover, the NiCo₂O₄ microspheres have superior reversibility. The specific capacitance of 504.58 F/g is obatined at a current density of 0.5 A/g. Additionally, the NiCo₂O₄ microspheres deliver an outstanding cycling stability with about 82% of the capacitance retention after 1000 GCD cycles.