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Although NiSx has a high storage advantage in ion battery as the anode material, the shortcomings such as poor conductivity and volume expansion seriously affect the performance. In this work, NiSx nanoparticles with an S/N-doped carbon layer (NiSx@S/N–C) are prepared by a simple hydrothermal reaction combined with heat treatment. At 2 A g−1, the discharge-specific capacity of the NiSx@S/N–C electrode can achieve at 609 mAh g−1 at the 400th cycle for lithium-ion batteries. Meanwhile, it shows the 270 mAh g−1 discharge capacity in the initial cycle and obtains a high specific capacity of 232 mAh g−1 after 250 cycles at 0.5 A g−1 for Na storage. In this research, a simple and reliable method is adopted to improve the capacity and performance of transition metal sulfide. [ABSTRACT FROM AUTHOR]