N–F‐codoped TiO2 materials were successfully fabricated by a hydrothermal method without any capping agent and further heat treatment. The results indicate interstitial N3− ion doping and the surface‐adsorbed F− ion on the TiO2 surface. By introducing N and F into the TiO2 lattice, the band gap of the obtained material is significantly reduced compared to the undoped TiO2. Moreover, the light absorption ability of the material was demonstrated to extend to visible light regions, contributing to the better photocatalytic activity. Furthermore, the sample with the NH4F/TiCl4 precursor molar ratio of 2:1 displayed the greatest photocatalytic activity with visible radiation. This study provides a new pathway to synthesize a novel photocatalyst having great potential for future applications.
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