Synthesis, characterization and particle size distribution of TiO2 colloidal nanoparticles

Nanoparticles of controlled size, well defined shape, pure phase and of clean surfaces are ideal model systems to investigate surface/interfacial reactions. In this study we have explored the possibility of synthesizing TiO2 nanoparticles in the size range of 7–20 nm under well controlled experimental conditions. A simple method based on the hydrolysis of TiCl4 was used to obtain particles having surfaces free from organics. Stable dispersions of TiO2 nanoparticles of various sizes were obtained by optimizing the reaction/dialysis time and temperature. The synthesized TiO2 particles were found to be predominantly of anatase phase and narrow particle size distributions were obtained. The TiO2 particles were characterized with respect to their phase, size and shape by X-ray diffraction (XRD) and transmission electron microscopy (TEM), respectively. Particle size distribution in a colloidal dispersion was obtained by the electrospray scanning mobility particle sizer (ES-SMPS) method and compared with an average particle size determined from dynamic light scattering (DLS). The average particle sizes obtained by the DLS and ES-SMPS methods were in good agreement, while a primary particle size of ∼4 nm was found in X-ray diffraction irrespective of the particle size in solution. Early stages of the nucleation process were monitored by the ES-SMPS method. These results show that small particles of 4–5 nm are initially formed and it is highly likely that large particles are formed due to aggregation of primary particles.