The efficient and controllable synthesis method of high-performance energy storage electrode materials is crucial for advancing the development of energy storage technologies. Herein, by leveraging microwave heating technology in the sulfidation of nickel cobalt MOF, we effectively enhanced the efficiency of the synthesis process. Notably, sulfidation time emerged as a pivotal factor in tuning the crystalline phase structure and conductive properties of the material, leading to the successful development of NCS2 electrode material with a unique structure through optimized sulfidation conditions. Electrochemical performance tests of the NCS2 material revealed exceptional results; it exhibited a specific capacity of 1311 Fg[Formula: see text] at a current density of 1 Ag[Formula: see text] and retained 73.4% of its initial capacity when the current density increased to 10 Ag[Formula: see text], demonstrating outstanding rate performance. The composite NCS2//AC supercapacitor exhibits an energy density of 24.2 Whkg[Formula: see text] at power density of 800 Wkg[Formula: see text], even though after 1000 consecutive charge-discharge cycles, the capacity retention rate remained high at 77.1%, validating the exceptional stability and reliability of the NCS2 material during cycling. This work employs microwave sulfidation for the rapid and controlled synthesis of nickel cobalt sulfides, providing a green and efficient synthetic strategy for metal sulfide active materials.