Two step, hydrolytic-solvothermal synthesis of redispersible titania nanocrystals and their gas-sensing properties

Abstract

A titanium chloromethoxide solution was prepared by reacting TiCl4 with methanol, followed by water addition. The starting solutions were characterized by Fourier Transform Infrared (FTIR) spectroscopy, evidencing that the in situ generated water results in early hydrolysis of the chloroalkoxide. The solution was reacted with molten dodecylamine at room temperature, obtaining a white slurry of amorphous titania nanoparticles. Stable, redispersible TiO2 nanocrystals could be prepared by subsequent solvothermal treatment in oleic acid at 250 °C. The use of oleic acid was essential for obtaining crystalline structures, while other surfactants prevented crystallization. The nanocrystals were characterized by X-ray Diffraction and Transmission Electron Microscopy, confirming the formation of anatase TiO2 nanocrystals with a mean size of 3.3 nm. The TiO2 nanocrystals were used for fabricating gas-sensing devices, which were tested towards ethanol vapors. The initial small size of the nanocrystals, and the limited size growth during the high-temperature sensor operation, result in remarkable sensing performances if compared with bulk titania sensors.