Síntese de nanocristais coloidais de TiO2 via método solvotermal

Abstract

This work presents a systematic study about preparing titanium oxide nanoparticles by solvothermal method. TiO2 is a much studied material because its applications in areas like catalysis, sensors, energy conversion devices, and others. It is speculated that all this technologies can be promoted by using nanostructured oxide. In order to confirm this, it is necessary to develop synthetic routes that allow preparing the desired material with controlled size and shapes. The methodology utilized in this research work consists in dissolve titanium isopropoxide in a phenyl ether and oleic acid mixture. After the complete dissolution, a hydrogen peroxide aqueous solution is fast injected in the medium. Then, the resulting suspension is heated at 120oC and maintained by time intervals between 12 and 192 hours. It was analyzed the influence of Lewis bases addition at the reaction medium, using chloride, nitrate and sulfate in these experiments. The influence of different surfactants on the oxide properties was analized too. The powders were characterized by X-ray diffraction, Raman spectroscopy, infrared spectroscopy and scanning-transmission electron microscopy. It was verified that the addition of a Lewis bases is a key rule to obtain crystalline TiO2 by the proposed route. This could be observed by the addition of simple bases as well as by addition of basic surfactants. The synthesis methodology developed in this work allows the synthesis of nanostructured materials with narrow size distribution, with diameters between 7 and 4 nm and standard deviation of about 1 nm. It was observed that the materials have a hydrophobic character; this was attributed to the presence of surfactants bounded to the particles surface. Infrared spectroscopy allowed that confirmation. In summary, it was developed a synthetic methodology of TiO2 colloidal nanocrystals that allows a good control of the final material characteristics.