Characterization of nanostructured zirconia prepared by hydrolysis and reverse micelle synthesis by small-angle neutron and x-ray scattering

Low temperature techniques such as hydrolysis and reverse micelle syntheses provide the opportunity to determine the relationship between the structural properties and preparation conditions of zirconia powders as well as to tailor their physicochemical properties. We have performed small-angle neutron and synchrotron x-ray scattering (SANS and SAXS) experiments to study the nucleation and organization of zirconia nanoparticles via different preparation routes. First, the formation of reverse micelles in individual and mixed solutions of (ZrOCl₂+D₂O)/AOT/C₆D₅CD₃, and (NH₄OH+H₂O)/AOT/C₆D₅CD₃ systems at water/AOT molar ratio of 20 was characterized. Second, the aggregation of zirconia gels obtained from the reaction of the reverse micelle solutions after heat treatments was studied. Third, the nanostructure of zirconia powders prepared by the reverse micelle method is compared with the corresponding powders prepared by hydrolysis after different heat treatments.