Nanomaterials based on dark titanium dioxide are of considerable interest as promising photocatalysts. In this work, titanium dioxide initially obtained by pulsed laser ablation (Nd:YAG laser with 1064 nm, 7 ns, 20 Hz) was subjected to additional laser treatment. The thus obtained powder materials were annealed and study of the structure by X-ray diffraction, optical properties by diffuse reflection spectroscopy, and photocatalytic properties in the processes of decomposition of the Rhodamine B dye and evolution of hydrogen from an aqueous methanol solution are presente