The development of bifunctional electrocatalysts with high performance for both hydrogen evolution reaction (HER) and oxygen evolution reaction (OER) with earth-abundant elements is still a challenge in electrochemical water splitting technology. Herein, we fabricated a free-standing electrocatalyst in the form of vertically oriented Fe-doped Ni3S2 nanosheet array grown on three-dimensional (3D) Ni foam (Fe-Ni3S2/NF), which presented a high activity and durability for both HER and OER in alkaline media. On the basis of systematic experiments and calculation, the Fe-doping was evidenced to increase the electrochemical surface area, improve the water adsorption ability, and optimize the hydrogen adsorption energy of Ni3S2, which resulted in the enhancement of HER activity on Fe-Ni3S2/NF. Moreover, metal sites of Fe-Ni3S2/NF were proved to play a significant role in the HER process. During the catalysis of OER, the formation of Ni–Fe (oxy)­hydroxide was observed on the near-surface section of Fe-Ni3S2/NF, and the introduction of the Fe element dramatically enhanced the OER activity of Ni3S2. The overall water splitting electrolyzer assembled by Fe-Ni3S2/NF exhibited a low cell voltage (1.54 V @ 10 mA cm–2) and a high durability in 1 M KOH. This work demonstrated a promising bifunctional electrocatalyst for water electrolysis in alkaline media with potential application in the future.

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It is a great challenge to fabricate electrode with simultaneous high activity for the hydrogen evolution reaction (HER) and the oxygen evolution reaction (OER). Herein, a high‐performance bifunctional electrode formed by vertically depositing a porous nanoplate array on the surface of nickel foam is provided, where the nanoplate is made up by the interconnection of trinary Ni–Fe–Mo suboxides and Ni nanoparticles. The amorphous Ni–Fe–Mo suboxide and its in situ transformed amorphous Ni–Fe–Mo (oxy)hydroxide acts as the main active species for HER and OER, respectively. The conductive network built by Ni nanoparticles provides rapid electron transfer to active sites. Moreover, the hydrophilic and aerophobic electrode surface together with the hierarchical pore structure facilitate mass transfer. The corresponding water electrolyzer demonstrates low cell voltage (1.50 V @ 10 mA cm−2 and 1.63 V @ 100 mA cm−2) with high durability at 500 mA cm−2 for at least 100 h in 1 m KOH.

The development of high-performance electrocatalyst with earth-abundant elements for water-splitting is a key factor to improve its cost efficiency. Herein, a noble metal-free bifunctional electrocatalyst was synthesized by a facile pyrolysis method using sucrose, urea, Co(NO) and sulfur powder as raw materials. During the fabrication process, Co, S co-doped graphitic carbon nitride (g-CN) was first produced, and then this in-situ-formed template further induced the generation of a Co, N, S tri-doped graphene coupled with Co nanoparticles (NPs) in the following pyrolysis process. The effect of pyrolysis temperature (700, 800, and 900 °C) on the physical properties and electrochemical performances of the final product was studied. Thanks to the increased number of graphene layer encapsulated Co NPs, higher graphitization degree of carbon matrix and the existence of hierarchical macro/meso pores, the composite electrocatalyst prepared under 900 °C presented the best activity for both hydrogen evolution reaction (HER) and oxygen evolution reaction (OER) with outstanding long-term durability. This work presented a facile method for the fabrication of non-noble-metal-based carbon composite from in-situ-formed template and also demonstrated a potential bifunctional electrocatalyst for the future investigation and application.

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