A Calcination-Free Sol-Gel Method to Prepare TiO -Based Hybrid Semiconductors for Enhanced Visible Light-Driven Hydrogen Production.

In recent years, the sol-gel method has been extensively utilized to develop efficient and stable organic semiconductor composite titanium dioxide (TiO ) photocatalysts. However, the high-temperature calcination requirements of this method consume energy during preparation and degrade encapsulated organic semiconductor molecules, resulting in decreased photocatalytic hydrogen production efficiency. In this study, we found that by selecting an appropriate organic semiconductor molecule, 1,4-naphthalene dicarboxylic acid (NA), high-temperature calcination can be avoided in the sol-gel process, yielding an organic-inorganic hybrid material with stable and effective photocatalytic properties. The uncalcined material displayed a hydrogen production rate of 2920±15 μmol g  h , which was approximately twice the maximum production rate observed in the calcined material. Likewise, the specific surface area of the uncalcined material, at 252.84 m  g , was significantly larger compared to the calcined material. Comprehensive analyses confirmed successful NA and TiO doping, while UV-vis and Mott-Schottky tests revealed a reduced energy bandgap (2.1 eV) and expanded light absorption range. Furthermore, the material maintained robust photocatalytic activity after a 40-hour cycle test. Our findings demonstrate that by using NA doping without calcination, excellent hydrogen production performance can be achieved, offering a novel approach for environmentally friendly and energy-saving production of organic semiconductor composite TiO materials.