Characterization of nanophase titania particles synthesized using in situ steric stabilization

Abstract

Ultrafine titania particles were synthesized from titanium tetraethoxide (TEOT) dissolved in ethanol. The concentration of water and of the soluble polymer hydroxypropylcellulose (HPC) were varied to control particle size. The HPC adsorbed onto the titania particles during growth, providing a steric barrier to aggregation. Electron microscopy showed that particles smaller than 70 nm were formed at high water concentrations (R > 120 where R is the molar ratio [H2O]/[TEOT]) and in the presence of HPC. The annealing-induced, phase-transformation behavior of these particles (amorphous → anatase → rutile) from 100 to 1000 °C was characterized by x-ray, Raman, and infrared techniques. The conversion of anatase to rutile occurred more readily for particles made at high water concentrations and with HPC. For particles formed by premixing TEOT with HPC prior to hydrolysis at R = 155, an 800 °C anneal yielded a rutile fraction exceeding 95%; particles made at R = 5.5 with no HPC showed negligible conversion at this temperature.