Preparation of Nanosize Anatase TiO2 Powders by Hydrothermal Synthesis
Nanosize anatase TiO2 powders have been synthesized by hydrothermal synthesis by using technical grade TiOSO4 as precursor and urea as precipitating agent. The initial pressure of the reaction system was set at 6 MPa. Stirring speed was fixed at 300r/min. The reaction system reacted at the temperature ranged from 110 to 150°C for holding 2hrs to 8hrs and the concentration of the precursor was ranged from 0.25M to1.5M. XRD patterns show that the synthesized powders are in the form of anatase phase. Calculated grain size is ranged from 6.7 to 8.9nm by Scherrer method from the line broadening of the (101) diffraction peak of anatase. The specific surface area of the powders synthesized under different conditions is ranged from 124 to 240m2/g. The grain size of the powders increases with the increase of the reaction temperature, holding time and precursor concentration, respectively. The specific surface area decreases with the increase of reaction temperature and holding time, and does not obviously change with the change of precursor concentration when the concentration of the precursor is less than 1M. However, when the concentration is higher than 1M, the specific surface area will decrease quickly with the increase of the precursor concentration. XRD and DSC-TG analysis shows that the synthesized anatase TiO2 will begin to transform to rutile TiO2 at about 840°C. When heated to 1000°C for holding 1h, the anatase powders will transform to rutile completely.
Wei Pan and Jianghong Gong
F. Y. Ran et al., "Preparation of Nanosize Anatase TiO2 Powders by Hydrothermal Synthesis", Key Engineering Materials, Vols. 336-338, pp. 2017-2020, 2007