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A hybrid photocatalyst was constructed based on twin crystal Cd0.5Zn0.5S with a homojunction containing M-CoO as the co-catalyst. The homojunction containing M-CoO is proved to be a more efficient co-catalyst than its pure phase counterparts.

Heterojunction strategy has proven to be an effective approach for overcoming the quick photoexcited charge carrier recombination of graphitic carbon nitride (g‐C3N4) and facilitating its photocatalytic performances. Bearing the merits of transition metal dichalcogenides (TMDs) in mind, in this work, a novel flower‐like ReS2 coupled with layered g‐C3N4 was constructed via a facile hydrothermal route. The hybrid ReS2/g‐C3N4 catalysts create excellent photocatalytic hydrogen evolution without any additional co‐catalyst. Under visible‐light irradiation, the optimized 3 wt % ReS2/g‐C3N4 heterojunction exhibited a hydrogen evolution rate 8 times that of pristine g‐C3N4, maintaining a stable heterojunction after multiple photocatalytic cycles. ReS2/g‐C3N4 integrates the merits of both the configuration of a heterojunction and the formation of spatially conductive network, which effectively accelerate the transfer of photoinduced carrier. This work not only presents a marked ReS2/g‐C3N4 heterojunction photocatalyst, but provides more possibility for expanding applications in electrocatalysis, photothermal catalysis and energy storage.

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