Herein, well‐crystallized ZnTiO3 particles are first prepared by hydrothermal method. A series of S‐scheme heterojunction photocatalysts of ZnTiO3/g‐C3N4 (referred to as ZTO/CN) with different mass ratios are synthesized by successfully doping ZnTiO3 in g‐C3N4 precursors and loading ZnTiO3 onto g‐C3N4 nanosheets by calcination. It is clearly found that the ZnTiO3 particles are successfully loaded on g‐C3N4 nanosheets by the X‐ray diffractometer, energy‐dispersive X‐ray spectra, and high‐resolution transmission electron microscopy images. Moreover, the specific surface area of 3.0% ZTO/CN is higher than that of pure g‐C3N4. Using triethanolamine as the hole sacrificial agent, the highest CO and H2 yields are achieved in the 3.0% ZTO/CN composite catalyst under the xenon lamp irradiation for 1 h. The generation rates of CO and H2 reach 15.19 and 5.77 μmol g−1 h−1, respectively, which are 2.9 and 4.1 times higher than that of pure g‐C3N4. The CO and H2 yields of the ZTO/CN composite catalyst show a trend of increasing and then decreasing with the increasing of ZnTiO3 content, which is due to the fact that excess ZnTiO3 can lead to a reduction of the effective heterojunction interface between ZnTiO3 and g‐C3N4, decreasing the transfer and separation efficiency of photogenerated electrons and holes and thus reducing the photocatalytic activity.
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