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The preparation of composite carbon nanomaterials is one of the methods for improving the electrochemical performance of carbon-based electrode materials for supercapacitors. However, traditional preparation methods are complicated and time-consuming, and the binder also leads to an increase in impedance and a decrease in specific capacitance. Therefore, in this work, we reduced Ni-Cu nanoparticles on the surface of nitrogen-doped carbon nanofibers (CNFs) by employing an electrostatic spinning method combined with pre-oxidation and annealing treatments. At the same time, Ni-Cu nanoparticles were vulcanized to Ni–Cu–S nanoparticles without destroying the structure of the CNFs. The area-specific capacitance of the CNFs/Ni–Cu–S–300 electrode reaches 1208 mF cm−2 at a current density of 1 mA cm−2, and the electrode has a good cycling stability with a capacitance retention rate of 76.5% after 5000 cycles. As a self-supporting electrode, this electrode can avoid the problem of the poor adhesion of electrode materials and the low utilization of active materials due to the inactivity of the binder and conductive agent in conventional collector electrodes, so it has excellent potential for application. [ABSTRACT FROM AUTHOR]