| Summary: | The exploration of high-efficiency bifunctional electrocatalysts for hydrogen evolution reaction (HER) and oxygen evolution reaction (OER) has long been challenging. The rational design of a catalyst by constructing heterostructures and a doping element are possibly expected to achieve it. Herein, the utilization of flower-like Fe/C-doped-MoS<sub>2</sub>/Ni<sub>3</sub>S<sub>2</sub>-450 spherical structural materials for electrocatalytic HER and OER is introduced in this study. The carboxyferrocene-incorporated molybdenum sulfide/nickel sulfide (Mo<sub>y</sub>S<sub>x</sub>/NiS) nanostructures were prepared by solvothermal method. After annealing, the iron and carbon elements derived from ferrocenecarboxylic acid enhanced the electrical transport performance and provided rich electronic sites for HER and OER in alkaline media. Specifically, the optimized flower-like Fe/C-doped-MoS<sub>2</sub>/Ni<sub>3</sub>S<sub>2</sub>-450 exhibited efficient bifunctional performance in alkaline electrolyte, with low overpotentials of 188 and 270 mV required to deliver a current density of 10 mA cm<sup>−2</sup> for HER and OER, respectively. This work provides valuable insights for the rational design of energy storage and conversion materials by the incorporation of transition metal and carbon elements into metal sulfide structures utilizing metallocene.
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