Control of the nanocrystalline zirconia structure through a colloidal sol-gel process

Abstract

A simple method to synthesize tetragonal zirconia stabilized at ambient temperature is developed and allows the monitoring of the tetragonal-monoclinic transition via a colloidal sol-gel process. By increasing the pH of an aqueous solution consisted of a zirconium precursor and a complexing agent (acetylacetone), a colloidal sol and then a gel can be formed under slightly acidic condition. After a drying step, tetragonal zirconia is easily obtained with an adequate thermal treatment at low temperature. The tetragonal-monoclinic transition occurs when the calcination temperature is increased. The relationship between the crystallite size, the crystallographic structure and the thermal treatment has been investigated by X-Ray Diffraction and the behaviour of the system from the gel state to the final powder has been studied by using Small Angle X-Ray Scattering and thermal analysis techniques. We demonstrate that compared to a chemical precipitation route, this colloidal sol-gel process allows the nanostructure of the material to be controlled due to the formation of primary nanoparticles. The presence of these nanoparticles makes possible the specific determination of the zirconia crystallographic phase through an accurate control of the nanostructure during the thermal treatment.