In this work, TiO₂ 3D nanostructures (TF30) were prepared via a facile wet chemical process using ammonium hexafluorotitanate. The synthesized 3D TiO₂ nanostructures exhibited well-defined crystalline and hierarchical structures assembled from TiO₂ nanorods with different thicknesses and diameters, which comprised numerous small beads. Moreover, the maximum specific surface area of TiO₂ 3D nanostructures was observed to be 191 m²g^-1, with concentration of F ions on the surface being 2 at%. The TiO₂ 3D nanostructures were tested as photocatalysts under UV irradiation using Rhodamine B solution in order to determine their photocatalytic performance. The TiO₂ 3D nanostructures showed a higher photocatalytic activity than that of the other TiO₂ samples, which was likely associated with the combined effects of a high crystallinity, unique features of the hierarchical structure, a high specific surface area, and the advantage of adsorbing F ions.

A facile one-pot wet chemical process to prepare pure anatase TiO₂ hollow structures using ammonium hexafluorotitanate as a precursor is developed. By defining the formic acid ratio, we fabricate TiO₂ hollow structures containing fluorine on the surface. The TiO₂ hollow sphere is composed of an anatase phase containing fluorine by various analytical techniques. A possible formation mechanism for the obtained hollow samples by self-transformation and Ostwald ripening is proposed. The TiO₂ hollow structures containing fluorine exhibits 1.2 - 2.7 times higher performance than their counterparts in photocatalytic activity. The enhanced photocatalytic activity of the TiO₂ hollow structures is attributed to the combined effects of high crystallinity, specific surface area (62 m²g^-1), and the advantage of surface fluorine ions (at 8%) having strong electron-withdrawing ability of the surface ≡ Ti-F groups reduces the recombination of photogenerated electrons and holes.