In recent years, catalysis and photocatalysis processes using TiO₂ nanoparticles (TNPs) have received great attention due to their effectiveness in degrading and mineralizing organic and inorganic compounds. Nanocrystalline TiO₂ powder with different crystallinity and phase structures were synthesized using a Ti alloy as anode and stainless steel as cathode by the galvanostatic anodization method in alcoholic solution of chloride. Sodium dodecyl sulphate (SDS) surfactant was used as additive for to control the particle size. The X-ray diffraction (XRD), RAMAN spectroscopy and transmission electron microscopy (TEM) results, showed that a 50:50 anatase and brookite mixture phase was obtained with crystal sizes 7.2 nm and 7.5 nm respectively without any annealing. The size of the particles and the material purity are measured using scanning electron microscopy (SEM), dynamic light scattering (DLS) and energy dispersive X-ray analysis (EDX) indicated that a particle size smaller than 40 nm and a free impurity materials. The Brunauer–Emmett–Teller (BET) results show a specific surface area bigger than 200 m²/g. The band gap energy of the resulting TNPs were determined by diffuse reflectance measurements according to the Kubelka Munk theory, revealing a value of 3.24 eV. Therefore, the results indicate the success of this method to create TiO₂ nanoparticles in aqueous medium with a good properties to be use like photocatalyst in a very economical and environmentally benign way.