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A series of nickel sulfides derived from the hexagonal Ni-MOF are vulcanized through adjusting the hydrothermal time and the thiourea concentration. Among all the obtained nickel sulfides, one sample Ni-S2-3, which inherits the Ni-MOF’s morphology, shows the best electrochemical performance with a remarkable specific capacitance of 1128[Formula: see text]Fg[Formula: see text] at 1[Formula: see text]Ag[Formula: see text], a rate capacitance of 50% and a long cycle life of 74% retention after 5000 cycles. Furthermore, the asymmetrical supercapacitors (SCs) based on Ni-S2-3//AC exhibit a good supercapacitive performance with a maximum power density of 16.3[Formula: see text]Wh kg[Formula: see text] at a power density of 800[Formula: see text]Wkg[Formula: see text]. All these results indicate that vulcanizing Ni-MOF is an effective way to fabricate a superior electrode material with excellent electrochemical performance for SCs.