Energy storage methods have been studied in-depth with regard to supercapacitors (SCs). Accelerating the electron/ ion transport rate is crucial for enhancing the electrochemical properties of electrodes. In particular, layered double hydroxides (LDHs) have made significant consideration caused by the high theoretical charge-storage capacitance and the ability to tune the microstructure. In this work, a simple two-step hydrothermal process is successfully used to sulfurize NiFe-LDH/CB nanocomposite, and the impact of sulfurization concentration on the capacitive characteristic was carefully investigated. Carbon black (CB) is supported on the NiFe-LDH which accelerates the electron transport rate to improve conductivity. Additionally, the sulfidation process boosts the free electron density of NiFe-LDH/CB while decreasing the electrode's charge transfer resistance. Hence, the specific capacitance of NiFe-LDH/CB/S(10) materials, which exhibit appealing electrochemical function, was 1397.9 F g −1 at 1 A g −1 . Obviously, it successfully enhances the reactive sites while maintaining the layered structure of LDHs to raise the material's rate of electron/ion transport. Furthermore, activated carbon (AC) was used as the cathode and NiFe-LDH/CB/S(10) as the anode to make the asymmetric supercapacitor. An impressive energy density of 38.22 Wh kg −1 at a power density of 799.95 W kg −1 is provided by the NiFe-LDH/CB/S(10)//AC asymmetric supercapacitor (ASC), which also boasts a strong retention of 63.86% after 5000 cycles. For the electrodes utilized in the energy storage components, it presents a workable alternative.