| Summary: | Developing the large-scale preparation of non-noble metal catalysts with high performance is crucial for promoting the electrochemical production of hydrogen from water. In this work, a novel TiO<sub>2</sub>@FeNi<sub>2</sub>S<sub>4</sub> (TiO<sub>2</sub>@FNS) branch nanoflake array on Ni foam can be prepared at a large scale (50 cm<sup>2</sup>) by combining an atomic-layer-deposited (ALD) TiO<sub>2</sub> skeleton with one-step facile low-temperature (<100 °C) sulfurization method. As-prepared TiO<sub>2</sub>@FNS arrays exhibit excellent hydrogen evolution reaction (HER) performance with an overpotential of 97 mV at 10 mA cm<sup>−2</sup>, superior to the FNS counterpart (without TiO<sub>2</sub> coating) and other reported catalysts. The enhanced HER catalytic performance of TiO<sub>2</sub>@FNS is attributed to the increased specific surface area and improved structural stability due to the introduction of TiO<sub>2</sub> coating. Moreover, theoretical calculations also show that the bimetallic NFS structure is more favorable to the dissociation of water molecule and the desorption of H than the monometallic Ni<sub>3</sub>S<sub>2</sub> counterpart. With the combination of experimental results and theoretical calculations, this work has enlightened a new way of exploring high-efficient catalysts for HER.
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