In this work, a facile one-pot sol-gel/hydrothermal two-step (SH II) process was developed to synthesize the P/Ag/Ag₂O/Ag₃PO₄/TiO₂ composite photocatalyst with superior H₂ evolution ability under solar light. Compared with the one-step sol-gel method, a negative shift of the conduction band edge (−0.51 eV vs. NHE) over H⁺/H₂ evolution potential was successfully achieved in SH II process by controlling the amount of metallic Ag formation under optimal conditions, which subsequently enabled the SH II–generated electrons to react with H⁺ to produce H₂. Moreover, the smaller crystal size, bigger specific surface area, faster charge carrier movability, and lower recombination rate in the SH II material played a critical role in increasing H₂ evolution. In addition, the H₂ generation rate of the SH II composite was further promoted by coupling with photocatalytic oxidation of alcohols, more specifically with methanol to efficiently consume photogenerated holes. Furthermore, higher H₂ yield was sustainably maintained even after ten recycling runs. Therefore, based on the advantages of simple operation and high efficiency, the SH II method could be a promising strategy to further improve the ability of composite photocatalysts for practical application in wastewater treatment and the water splitting field in the future.

在这项工作中，开发了一种简便的一锅溶胶-凝胶/水热两步法（SH II），以合成具有优异H ₂释放能力的P / Ag / Ag ₂ O / Ag ₃ PO ₄ / TiO ₂复合光催化剂。在太阳光下。与一步法溶胶-凝胶法相比，通过控制金属Ag的形成量，在SH II过程中成功实现了导带边沿H ⁺ / H ₂演化电势的负移（-0.51 eV对NHE）在最佳条件下，随后使由SH II生成的电子与H ⁺反应生成H ₂。此外，SH II材料中较小的晶体尺寸，较大的比表面积，较快的电荷载流子运动性和较低的复合率在增加H ₂逸出方面起着关键作用。另外，通过与醇的光催化氧化，更具体地与甲醇的光催化氧化偶联，进一步提高了SH II复合材料的H ₂生成速率，以有效地消耗光生空穴。此外，H ₂更高即使经过十次回收运行，产量仍可持续保持。因此，基于操作简便，效率高的优点，SH II方法可能是进一步提高复合光催化剂在废水处理和水分解领域的实际应用能力的有前途的策略。