The design and synthesis of low-cost hydrogen evolution photocatalysts with high carrier separation capability and visible light responsiveness are key factors in increasing hydrogen production. In this work, zero-dimensional (0D) amorphous nickel boride (NixB) was synthesized using a reduction method. Subsequently, a 0D/2D amorphous NixB/ZnIn2S4 S-scheme heterojunction was fabricated through electrostatic attraction. This heterojunction exhibited stronger visible light responsiveness and enhanced photogenerated carrier separation performance. The morphology, composition, elemental, structural, and light absorption capacities of the as-synthesized composites were researched by SEM, TEM, XRD, XPS, and UV–vis DRS. The ability to separate photogenerated carriers were evaluated through photoelectrochemical experiments. The hydrogen evolution rate of NixB/ZnIn2S4 (2208 μmol h−1 g−1) increased 25 times than that of single ZnIn2S4 in sacrificial solution, and the apparent quantum yield (AQY) at 400 nm was 14.25 %. This study gives evidence of the great preponderance of S-scheme heterojunction and multidimensional material co-construction in improving hydrogen precipitation.
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