V-TiO2 photocatalyst with 0 ≤ V ≤ 20 mol% was prepared via the sol–gel method based on mixed oxide titanium–vanadium nanoparticles with size and composition control. The mixed oxide vanadium–titanium oxo-alkoxy nanonoparticles were generated in a chemical micromixing reactor, coated on glass beads via liquid colloid deposition method and underwent to an appropriate thermal treatment forming crystallized nanocoatings. X-ray diffraction, Raman, thermogravimetric and differential thermal analyses confirmed anatase crystalline structure at vanadium content ≤ 10 mol%, with the cell parameters identical to those of pure TiO2. At a higher vanadium content of ~20 mol%, the material segregation began and orthorhombic phase of V2O5 appeared. The crystallization onset temperature of V-TiO2 smoothly changed with an increase in vanadium content. The best photocatalytic performance towards methylene blue decomposition in aqueous solutions under UVA and visible light illuminations was observed in V-TiO2 nanocoatings with, respectively, 2 mol% and 10 mol% vanadium.

The mixed vanadium-titanium oxo-alkoxy (VTOA) nanoparticles were synthesized via sol-gel method in a chemical reactor with ultra-rapid micromixing. The nucleation and growth kinetics and particles size, followed by the static/dynamic light scattering methods, were quite different from those of pure oxo-alkoxy titanium (TOA) and vanadium (VOA) species. It was shown that the TOA species appear first and serve to be centres of attraction for hydrolysed VOA species at the nucleation stage. However, at the vanadium content above 20 mol% large VOA species imprison sub-nucleus TOA species prohibiting the nucleus appearance. The model analysis of the VTOA induction kinetics validated a significant increase of the nucleus size with an increase of the precursor concentration. The results support a new paradigm of the sol-gel process describing profound restructuring of the oxometallic species during assembling at the nucleation stage.