Porous NiCo 2 S 4 networks have been successfully synthesized by a facile one-pot solvothermal method without the use of any surfactant or template. Crystal structure, morphology, composition and surface area of the as-synthesized samples were characterized by X-ray di®raction, eld-emission scanning electron microscopy, X-ray photoelectron spectroscopy and BrunauerEmmet-Teller techniques. Owing to their porous nature and small crystalline size, the as-prepared NiCo 2 S 4 networks based supercapacitor electrodes showed a high speci¯c capacitance of 1250 FÁg À1 at 1 AÁg À1 , and excellent cycling stability with the retention capacity of 70.3% after 5000 cycles in the KOH aqueous solution electrolyte.