Microwave radiation as heating method in the synthesis of titanium dioxide nanoparticles from hexafluorotitanate-organic salts

Nanocrystalline anatase was obtained from ionic liquid-like precursors containing hexafluorotitanate-organic salts and less than 25 wt.% of water, and using boric acid as fluoride scavenger. Two alternative heating methods were explored using either a conventional oven or a domestic microwave apparatus. A significant reduction in the reaction time from 24 h to only few minutes was obtained using the microwave route. The as-prepared materials were characterized by X-ray diffraction, transmission electron microscopy, nitrogen sorption analysis, and attenuated total reflectance Fourier transformed infrared, X-ray photoelectronic and Raman spectroscopes. The convenience of using the microwave heating option was a function of the organic cation present in the precursor. Thus, organic ammonium cations containing only hydrocarbon substituents, such as diethylammonium, phenylammonium and benzyltrimethylammonium led to the precipitation of nanocrystalline anatase powder with high specific surface area (up to 120 m² g⁻¹) in a short processing time (1-3 min). Otherwise, alcohol and carboxylate functionalized cations decomposed under microwave treatment. Moreover, the choice of the organic cation allowed tuning several properties of the end material, such as particle size and pore morphology.