Metal‐organic frameworks (MOFs) have been considered as potential oxygen evolution reaction (OER) electrocatalysts owning to their ultra‐thin structure, adjustable composition, high surface area, and high porosity. Here, we designed and fabricated a vanadium‐doped nickel organic framework (V1−x−NixMOF) system by using a facile two‐step solvothermal method on nickel foam (NF). The doping of vanadium remarkably elevates the OER activity of V1−x−NixMOF, thus demonstrating better performance than the corresponding single metallic Ni‐MOF, NiV‐MOF and RuO2 catalysts at high current density (>400 mA cm−2). V0.09−Ni0.91MOF/NF provides a low overpotential of 235 mV and a small Tafel slope of 30.3 mV dec−1 at a current density of 10 mA cm−2. More importantly, a water‐splitting device assembled with Pt/C/NF and V0.09−Ni0.91MOF/NF as cathode and anode yielded a cell voltage of 1.96 V@1000 mA cm−2, thereby outperforming the‐state‐of‐the‐art RuO2(+)||Pt/C(−). Our work sheds new insight on preparing stable, efficient OER electrocatalysts and a promising method for designing various MOF‐based materials.

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Developing low-cost, efficient, and stable oxygen reduction reaction (ORR) electrocatalysts is crucial for the commercialization of energy conversion devices such as metal–air batteries. In this study, we report a Mn-doped Zn metal–organic framework-derived porous N-doped carbon composite (30-ZnMn-NC) as a high-performance ORR catalyst. 30-ZnMn-NC exhibits excellent electrocatalytic activity, demonstrating a kinetic current density of 9.58 mA cm–2 (0.8 V) and a half-wave potential of 0.83 V, surpassing the benchmark Pt/C and most of the recently reported non-noble metal-based catalysts. Moreover, the assembled zinc–air battery with 30-ZnMn-NC demonstrates high peak power densities of 207 and 66.3 mW cm–2 in liquid and flexible batteries, respectively, highlighting its potential for practical applications. The excellent electrocatalytic activity of 30-ZnMn-NC is attributed to its unique porous structure, the strong electronic interaction between metal Zn/Mn and adjacent N-doped carbon, as well as the bimetallic Mn/Zn–N active sites, which synergistically promote faster reaction kinetics. This work offers a controllable design strategy for efficient electrocatalysts with porous structures and bimetallic active sites, which can significantly enhance the performance of energy conversion devices.

Developing a highly efficient bifunctional catalyst for hydrolysis of metal hydrides and spontaneous hydrogen evolution reaction (HER) is essential for substituting conventional fuels for H2 production. Herein, Ru‐cluster‐modified Co3B−Co(OH)2 supported on nickel foam (Ru/Co3B−Co(OH)2@NF) is constructed by electroless deposition, calcination and chemical reduction. The catalyst exhibits an excellent hydrogen generation rate (HGR) of 4989 mL min−1 normalgcatalyst-1 ${{{\rm g}}_{catalyst}^{-1}}$ and good reusability, superior to most previously reported catalysts. Besides, Ru/Co3B−Co(OH)2@NF displays a prominent hydrogen evolution reaction catalytic capability with a low overpotential of 153.0 mV at 100 mA cm−2 (50.5 mV at 10 mA cm−2), a small Tafel slope of 40.0 mV dec−1 and long‐term stability (100 h@10 mA cm−2) in 1.0 M KOH. The excellent catalytic H2 generation capacity benefits from the rapid charge transfer promoted by metallic Co3B, the synergistic catalytic effect of Co3B−Co(OH)2 and Ru clusters, and the unique composite structure favorable for solute transport and gas emission.