Polytypes of two-dimensional transition metal dichalcogenide can extend the architecture and application of nanostructures. Herein, NbVSe alloy nanosheets in the full composition range () were synthesized by a colloidal reaction. At = 0.1-0.3, a phase transition occurred from various hexagonal (three 2H and one 4H types) phase NbSe to an atomically homogeneous 1T phase VSe. Density functional theory calculations also revealed a polytypic phase transition at = 0.3, which was shifted close to 0 in the presence of Se vacancies. Furthermore, the calculations validate favorable formation of Se vacancies at the phase transition. The sample at = 0.3 exhibited enhanced electrocatalytic activity toward the hydrogen evolution reaction (HER) in 0.5 M HSO. The Gibbs free energy indicates that the catalytic HER performance is correlated with the active Se vacancy sites of polytypic structures.
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