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Nitrogen‐Doped Hierarchical Heterostructured Aerophobic MoSx/Ni3S2 Nanowires by One‐pot Synthesis: System Engineering and Synergistic Effect in Electrocatalysis of Hydrogen Evolution Reaction

Non‐noble metal electrocatalysis has witnessed rapid and profound performance improvements owing to the emergence of advanced nanosynthetic techniques. Integration of these nanotechniques can lead to synergistic performance enhancement, but such system‐engineering strategies are difficult to achieve because of the lack of effective synthesis method. We hereby demonstrate an integrated approach that combines most of the existing nanotechniques in a facile one‐pot synthesis. Material characterization reveals that the product shows key features intended by techniques including morphological, structural, doping, heterointerface, and surface wetting engineering. The as‐obtained nitrogen‐doped hierarchical heterostructured MoSx/Ni3S2 nanowires show an overpotential that is only 50 mV higher than commercial Pt/C for hydrogen evolution reaction over current densities from 10 to 150 mA cm−2. Correlations between the adopted nanotechniques and the electrochemical reaction rates are established by evaluating the impacts of individual techniques on the activation energy, pre‐exponential factor, and transfer coefficient. This in‐depth analysis provides a full account of the synergistic effects and the overall improvement in electrocatalytic performance of hydrogen evolution reaction. This work manifests a generic strategy for multipurpose material design in non‐noble metal electrocatalysis.