It is of great importance to develop highly efficient electrocatalysts with low-cost, superior activity and good stability toward hydrogen production. The conductivity property and catalytic activity of transition metal electrocatalyst can be desirable optimized by metal doping for hydrogen evolution reaction (HER). Herein, a Co-doped MoS₂/NiS₂ nanosheet array was in-situ covered on the carbon cloth substrate (Co-MoS₂/NiS₂/CC) via facile successive three-step hydrothermal processes, in which Co-MoS₂ nanosheets were hierarchically integrated with NiS₂ nanosheets. Benefitting from the introduction of Co atom and numerous heterostructures, the as-obtained Co-MoS₂/NiS₂/CC allows high conductivity and plenty of accessible active sites, showing favorable synergistic effect for electrocatalytic HER properties. Specifically, the optimal Co-MoS₂/NiS₂/CC electrocatalyst requires low overpotentials of 92 and 122 mV to deliver current densities of 10 and 50 mA cm⁻² in 0.5 M H₂SO₄. It presents excellent electrocatalytic activity in 0.1 M KOH simultaneously. Moreover, such a Co-MoS₂/NiS₂/CC electrocatalyst shows a small Tafel slope of 47 mV dec⁻¹ and remarkable long-term stability. This work provides a novel strategy to synthesize transition metal-doped heterogeneous electrocatalysts for efficient hydrogen evolution reaction.

开发低成本、高活性和良好的制氢稳定性的高效电催化剂具有重要意义。过渡金属电催化剂的导电性能和催化活性可以通过金属掺杂用于析氢反应 (HER) 来优化。在此，Co掺杂的MoS ₂ /NiS ₂纳米片阵列通过简单的连续三步水热工艺原位覆盖在碳布基材（Co-MoS ₂ /NiS ₂ /CC）上，其中Co-MoS ₂纳米片与 NiS ₂分层集成纳米片。得益于Co原子和众多异质结构的引入，所获得的Co-MoS ₂ /NiS ₂ /CC具有高导电性和大量可接近的活性位点，对电催化HER性能显示出良好的协同效应。具体而言，最佳的 Co-MoS ₂ /NiS ₂ /CC 电催化剂需要 92 和 122 mV 的低过电位，以在 0.5 MH ₂ SO _{4 中}提供 10 和 50 mA cm ^{-2 的}电流密度。同时在 0.1 M KOH 中表现出优异的电催化活性。此外，这种 Co-MoS ₂ /NiS ₂ /CC 电催化剂显示出 47 mV dec ^-1的小塔菲尔斜率和显着的长期稳定性。这项工作为合成过渡金属掺杂的多相电催化剂以实现高效析氢反应提供了一种新策略。