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We reported a facile self-generated sacrificial template method for fabricating mesoporous three dimension NiCo2O4/graphene electrode material. Nickel, cobalt, and zinc ions dissolved in ethylene glycol reacted with potassium hydroxide solution to co-deposit onto graphene at 140 °C under atmospheric environment. With further addition of potassium hydroxide, zinc hydroxide as a self-generated sacrificial template was dissolved in situ, leading to the formation of mesoporous morphology. Structure and morphology characteristics were determined by X-ray diffraction, scanning electron microscopy, high-resolution transmission electron microscopy, and N2 adsorption experiments. Electrochemical properties were analyzed by AC impedance spectroscopy, cycling voltammetry, and charge/discharge test in 2 M KOH. Results showed that the as—prepared NiCo2O4/graphene electrode possessed a large specific surface area of 281.4 m2 g−1, an ultrahigh specific capacity of 1024.99 and 662.12 C g−1 at current density of 1 and 50 A g−1 respectively, and a long-term cycling life of 10,000 charge/discharge tests.

A facile synthesis approach was successfully developed to synthesize mesoporous NiCo2S4 in ethylene glycol. X-ray diffraction, scanning electron microscopy, high-resolution transmission electron microscopy, and N2 adsorption–desorption experiment were conducted to examine the morphology and microstructure of the as-prepared NiCo2S4. Furthermore, electrochemical measurements, including cyclic voltammetry, galvanostatic charge–discharge tests, and electrochemical impedance spectroscopy, were carried out in a three-electrode system to evaluate the electrochemical properties of the mesoporous NiCo2S4. The as-prepared NiCo2S4 possessed a high specific surface area of 223.6 m2 g−1 with a high specific capacity of 406 C g−1 at 0.5 A g−1. In addition, only a 6.3 % loss of specific capacity was observed at 5 A g−1 after 20,000 GCD cycles, suggesting a long life cycle.