A series of ZnO/Fe
2
O
3
/g-C
3
N
4
photocatalysts were synthetized by impregnation of g-C
3
N
4
with Zn(NO
3
)
2
·6H
2
O, and Fe(NO
3
)
2
·9H
2
O followed by calcination. The morphology, chemical composition, and structure of the resulted materials were carefully analyzed by various characterization techniques. The photocatalytic performance of ZnO/Fe
2
O
3
/g-C
3
N
4
composites was evaluated based on the H
2
evolution from water splitting reaction. The results showed that the ZnO/Fe
2
O
3
/g-C
3
N
4
composite can effectively produce more H
2
than pure g-C
3
N
4
when irradiated under visible-light. H
2
production rate over 3-ZnO/Fe
2
O
3
/g-C
3
N
4
composite was of 25 μmol·h
−1
, which is 4 times higher than that obtained in the presence of pure g-C
3
N
4
, clearly showing a significant improvement of the photocatalytic activity of the prepared nanocomposite. This result was attributed to the formation of a heterojunction between g-C
3
N
4
and ZnO/Fe
2
O
3
, which delayed the recombination of holes-electrons pairs and resulted in a remarkable increase in photocatalytic performance.