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Polyoxometalates (POMs) are ideal preassembled platforms for constructing transition metal catalysts because they are rich in oxygen and transition metal elements. In contrast to traditional methods for preparing V2O5/MoS2 composite catalysts, the method proposed in this study leverages the selective preference of vanadium for oxygen vs. sulfur. A MoS2-based electrocatalyst composited with a small amount of V2O5 was constructed in situ on a carbon cloth via a one-pot hydrothermal method using a Lindqvist-type POM, i.e., (C16H36N)2 Mo3V3O16(OCH2)3CCH2CH3 (Mo3V3), as a precursor. This catalyst was used for efficient electrocatalytic hydrogen evolution reaction. The experimental results reveal that the introduction of a small amount of V2O5 considerably increases the electrochemically active surface area of the catalyst, effectively enhancing the catalytic performance of the material. This study provides a new design strategy and synthetic pathway for precise construction of high-performance composite electrocatalysts based on POM precursors.

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