Metal

Vacancy defect

Quantum mechanics

Catalysis

Phase (matter)

Engineering

Electrochemistry

Metallurgy

Materials science

Transition metal

Ammonia borane

Biochemistry

Chemical engineering

Electrocatalyst

Physical chemistry

Quenching (fluorescence)

Hydrogen

Physics

Organic chemistry

Fluorescence

Crystallography

Chemistry

Electrode

Hydrogen production

Overpotential

Advanced Energy Materials

For most Mo‐based electrocatalysts, the hydrogen evolution reaction (HER) activity depends on their own active structural defects or extrinsic transition metal centers. In this work, in order to combine the advantages of these two different active centers, a solid‐phase interface reaction (SPIR) strategy is proposed, which simultaneously introduces oxygen vacancies (V O ) and metal centers (Ru) into the 2D Mo‐based catalyst. Briefly, this SPIR occurs at the interface between MoS 2 and RuO 2 nanoparticles of the RuO 2 /MoS 2 precursor when overcoming the kinetic barriers at a suitable temperature under an Ar atmosphere. Since the adjacent parts of RuO 2 and MoS 2 are converted to Ru and MoO 2 in situ, a composite system MiSC‐1 containing a large amount of active Ru and V O on MoO 2 plane is obtained. Furthermore, theoretical calculations confirm the proposed mechanism of SPIR. MiSC‐1 shows excellent stability and catalytic performance in the HER, with an overpotential value of 12 mV at 10 mA cm −2 in 1.0 M KOH. Additionally, MiSC‐1 exhibits excellent performance in the hydrolysis of ammonia borane. This report will provide a versatile platform for the preparation of a multi‐component catalyst with high total activity as well as the identification of the structural details of the catalysts.

Coupling of Ru and O‐Vacancy on 2D Mo‐Based Electrocatalyst Via a Solid‐Phase Interface Reaction Strategy for Hydrogen Evolution Reaction