In the study the mechanochemical synthesis in the planetary ball mill was used to prepare photocatalytic materials obtained on the basis of TiO2 and nickel(II) acetylacetonate as a Ni²⁺ source. Three materials with different contents of Ni²⁺: 5, 10 and 20% wt. were prepared. The obtained materials were calcinated at 800°C for 1 h. Their physicochemical properties were investigated using the N₂ adsorption/desorption, FT-IR/PAS, XRD, UV-Vis/DRS and SEM methods. Additionally, thermal stability of the obtained materials was examined (TGA/DTG/DTA). Photocatalytic activity of the samples was tested in relation to the aqueous solution of Safranin T (initial concentration C₀ = 1×10^-5 mol L^-1) at the visible light (Vis). The results indicate that the mechanochemical synthesis is an effective and simple method for preparing materials with photocatalytic properties. All obtained materials were characterized by greater photocatalytic activity compared to the initial TiO₂.