The Co 3 O 4 /ZnIn 2 S 4 p-n heterojunction photocatalyst was successfully prepared using the block stacked by Co 3 O 4 nanosheets as the carrier. Because the surface of the Co 3 O 4 nano-block is rough, it is easy to absorb more ZnIn 2 S 4 nanosheets, which leads to the tight coupling of composite Co 3 O 4 /ZnIn 2 S 4 . In addition, the interaction of the p-n heterojunction interface accelerates the separation of photogenerated carriers, thus increasing the rate of photocatalytic hydrogen evolution. In the photocatalytic hydrogen evolution test, the composite Co 3 O 4 /ZnIn 2 S 4 showed excellent hydrogen evolution performance, and the maximum hydrogen evolution capacity was up to 72.01 μmol, which was about 5.6 times that of pure Co 3 O 4 . Under the action of the built-in electric field, the accumulation of electrons and holes in the ZnIn 2 S 4 conduction band and Co 3 O 4 valence band is accelerated, thus higher separation efficiency is achieved. The addition of various characterizations also confirmed the excellent properties of the composites. This work provides a reference for the construction of photocatalytic heterojunction.