The development of highly efficient, inexpensive, abundant and non-precious metal electrocatalysts is the lifeblood of the hydrogen production industry, especially the hydrogen production industry by electrolysis of water. A Fe-Co-S/NF bifunctional electrocatalyst with nanoflower-like structure was synthesized on three-dimensional porous nickel foam through one-step hydrothermal and one-step hightemperature sulfuration operations, and the material displays high-efficiency electrocatalytic performance. As a catalyst for the hydrogen evolution reaction, Fe-Co-S/NF can drive a current density of 10 mA/cm 2 at an overpotential of 143 mV with a Tafel slope of 80.2 mV/dec. When it was used as an oxygen evolution reaction catalyst, it exhibits good OER reactivity with a low Tafel slope (82.6 mV/dec) and with requiring only 117 mV overpotential to drive current densities up to 50 mA/cm 2 . In addition, the Fe-Co-S/NF//Fe-Co-S/NF electrolytic cell was assembled, an electrolysis voltage of 1.64 V is required to drive a current density of 50 mA/cm 2 , which is one of the most active catalysts reported so far. This work indicates that the introduction of S, P and Se treating processes could effectively improve electrical conductivity of the material and enhance the catalytic activity of the material. This work offers an effective and convenient method for improving the morphology of the catalyst, increasing the surface area of the catalyst and developing high-efficiency and low-cost catalysts.