Synthesis and crystallization of titanium dioxide in supercritical carbon dioxide (scCO₂)

In this work, a simple and low-temperature method to synthesize titanium dioxide (TiO₂) particles with supercritical carbon dioxide is presented. The particles were synthesized by measuring 5 ml of tetra-n-butyl orthotitanate precursor to the supercritical chamber. The pressure was maintained at 15.0 MPafor all experiments. Reaction temperatures used were 50 °C or 70 °C. After reaching treatment parameters 10 ml of deionized water was introduced to the chamber with a co-solvent pump. A mixer was used inside the chamber to ensure proper mixing of water and precursor. Reaction times of 10, 60 and 300 min were used. Characterization of the particle crystal phase was determined by X-ray diffraction, differential scanning calorimetry and transmission electron microscopy. The specific surface areas were measured with nitrogen adsorption tests (BET). The results showed that the particles synthesized with reaction times of 10 and 60 min contained brookite as the crystalline phase. With longer reaction time of 300 min the phase shifted to anatase. In most experiments there was also significant amount of amorphous phase present. The specific surface areas varied between 274.3-566.6 m²/g.