Mechanochemical synthesis of nanocrystalline TiO2 from liquid TiCl4

The synthesis of TiO2 by soft mechanochemical reaction and subsequent annealing of the products was studied. In the first series liquid TiCl4 and (NH4)2CO3 powder were used as reactants, while in the second one TiCl4 and (NH4)2CO3 were again used but with Na2SO4 · 10H2O and Na2SO4 employed as additives. The synthesis was almost complete after 5 min of milling. The NH4Cl by-product was removed by low-temperature heating. Annealing at 230–650 °C led to anatase TiO2 with a crystallite size calculated by X-ray diffraction to be in the range 10–50 nm.