In this work, mesoporous NiCo2O4 has been successfully synthesized by in situ removal of template method. The NiCo2O4 composite was precipitated by hydrolysis method using ethylene glycol as a high boiling point solvent at 140°C under atmospheric environment. Zinc hydroxide is used as the sacrificial template to construct the mesoporous structure with high specific surface area. The structure and morphology characteristics were carried out by X–ray diffraction, scanning electron microscopy, high resolution transmission electron microscopy, and N2 adsorption experiments. The electrochemical properties were investigated through AC impedance spectroscopy, cycling voltammetry and charge/discharge test in 7M KOH. The results exhibit that the as–prepared mesoporous NiCo2O4 shows a large specific surface area of 219.2m2 g−1, a high specific capacity of 660.53Cg−1 at current density of 1Ag−1. The mesoporous NiCo2O4 electrodes still remain 90% specific capacity retention compared with the first cycle over 32,000cycles, which exhibits the as–prepared electrode possess long–term stability.