Rational design of high-efficiency heterostructure photocatalyst is an effective strategy to realize photocatalytic H₂ evolution from pure water, but remains still a considerable challenge. Herein, an anatase/rutile TiO₂/g-C₃N₄ (A/R/CN) multi-heterostructure photocatalyst was prepared by a facile thermoset hybrid method. The combination of two type-II semiconductor heterostructures (i.e., A/R and R/CN) significantly improve the separation and transfer efficiency of photogenerated carriers of anatase TiO₂, rutile TiO₂ and g-C₃N₄, and A/R/CN photocatalyst with high activity is obtained. The optimal A/R/CN photocatalyst exhibits significantly increased photocatalytic overall water splitting activity with a rate of H₂ evolution of 374.2 μmol g⁻¹h⁻¹, which is about 8 and 4 times that of pure g-C₃N₄ and P25. Moreover, it is demonstrated to be stable and retained a high activity (ca. 91.2%) after the fourth recycling experiment. This work comes up with an innovative perspective on the construction of multi-heterostructure interfaces to improve the overall photocatalytic water splitting performance.

合理设计高效异质结构光催化剂是实现光催化从纯水中释放H ₂的有效策略，但仍然是一个巨大的挑战。在此，通过简便的热固性混合法制备了锐钛矿/金红石型TiO ₂ / gC ₃ N ₄（A / R / CN）多异质结构光催化剂。两种II型半导体异质结构（即A / R和R / CN）的组合显着提高了锐钛矿型TiO ₂，金红石型TiO ₂和gC ₃ N ₄的光生载流子的分离和转移效率。，得到具有高活性的A / R / CN光催化剂。最佳的A / R / CN光催化剂表现出显着提高的光催化总水分解活性，其H ₂释放速率为374.2μmolg ^-1 h ^-1，约为纯gC ₃ N ₄和P25的8倍和4倍。而且，在第四次循环实验后，它被证明是稳定的并保持了高活性（约91.2％）。这项工作提出了关于多异质结构界面构建的创新观点，以改善整体光催化水分解性能。