Abstract

Metal–molybdenum sulfide (MMoSx)‐based catalysts exhibit good performance over a wide pH range toward hydrogen evolution with relatively low overvoltage requirements. Therefore, they are considered as suitable alternatives to Pt as catalysts for hydrogen evolution reaction. Herein, self‐supported amorphous CuMoSx and NiMoSx nanosheet arrays are prepared on copper foam (CF) and nickel foam (NF), respectively, through an anion‐exchange strategy. CF and NF are first converted into CuTCNQ and NiTCNQ nanowire arrays (TCNQ = tetracyanoquinodimethane), which are then in situ reacted with (NH4)2MoS4 solution to generate amorphous CuMoSx/CF and NiMoSx/NF nanosheets, respectively, as efficient electrocatalysts for H2 generation. NiMoSx/NF exhibits a superior catalytic activity to CuMoSx/CF in 0.5 m H2SO4 solution, as CuMoSx/CF requires overpotentials (η) of 213 and 275 mV to obtain current densities of 10 and 50 mA cm−2, respectively, whereas NiMoSx/NF only requires η of 174 and 248 mV to receive the same current densities, respectively. Furthermore, these electrodes exhibit considerable long‐term electrochemical durability. Herein, an effective and easy‐to‐operate strategy for the construction of self‐supported metal–molybdenum sulfide nanosheet arrays films toward a highly efficient electrochemical hydrogen generation reaction is provided.

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