Franz Legrand

Chemical control in precipitation of spherical zirconia particles

Monodisperse spherical zirconia particles are precipitated by hydrolysis of alcoholic solutions of zirconium alkoxides in the presence of long-chain carboxylic acids. The particle size can be finely tuned from 0.1 to 2.5 Μm by controlling the concentration of zirconium alkoxide, the water/zirconium ratio, the nature of alcohol from ethanol to butanol, the nature of carboxylic acid from caproic to oleic acid and its concentration. The relationships between the induction time before nucleation, the particle size and all the above parameters are tentatively explained on the grounds of the solubility of the carboxy-alkoxide derivatives and their tendency to form micelles. Calcination of precipitated powders between 300 and 600 ‡C produces mixtures of varying composition from cubic to monoclinic phases of small crystallite sizes, and brings out the loss of surface area and organic content. Different conditions of drying powders lead to variously ordered microstructures.