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In this work, the sulfur vacancies were successfully introduced into the ZnIn 2 S 4 (ZIS) lattice through two facile approaches, plasma etching and annealing, for enhancing the photocatalytic performance. The optimized plasma-etched ZIS exhibited an enhanced H 2 generation rate of 706 lmol g -1 h -1 , which was 5 and 1.2 times higher than that of pure ZIS and annealed ZIS, respectively. Theoretical calculation demonstrated that surface S vacancy could arouse the catalytic activity of the adjacent S atoms in inert (001) basal plane, serving as the active site for hydrogen evolution reaction (HER). Although annealing could produce much more S vacancies than the plasma etching, a majority of bulk S vacancies usually acted as charge recombination center to lower the photocatalytic activity. Hence, even plasma-etched ZIS presented poor light absorption capacity, plasma etching showed a better effect on the HER improvement of ZIS than annealing. This work presents a simple and promising pathway for optimization of 3D ZIS photocatalysts to improve photocatalytic hydrogen evolution.

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