Large scale synthesis of nanostructured zirconia-based compounds from freeze-dried precursors

Nanocrystalline zirconia powders have been obtained at the multigram scale by thermal decomposition of precursors resulting from the freeze-drying of aqueous acetic solutions. This technique has equally made possible to synthesize a variety of nanostructured yttria or scandia doped zirconia compositions. SEM images, as well as the analysis of the XRD patterns, show the nanoparticulated character of those solids obtained at low temperature, with typical particle size in the 10–15 nm range when prepared at 673 K. The presence of the monoclinic, the tetragonal or both phases depends on the temperature of the thermal treatment, the doping concentration and the nature of the dopant. In addition, Rietveld refinement of the XRD profiles of selected samples allows detecting the coexistence of the tetragonal and the cubic phases for high doping concentration and high thermal treatment temperatures. Raman experiments suggest the presence of both phases also at relatively low treatment temperatures.

Graphical abstractZr1−xAxO2−x/2 (A=Y, Sc; 0≤x≤0.12) solid solutions have been prepared as nanostructured powders by thermal decomposition of precursors obtained by freeze-drying, and this synthetic procedure has been scaled up to the 100 g scale.Figure optionsDownload full-size imageDownload as PowerPoint slideHighlights► Zr1−xAxO2−x/2 (A=Y, Sc; 0≤x≤0.12) solid solutions have been prepared as nanostructured powders. ► The synthetic method involves the thermal decomposition of precursors obtained by freeze-drying. ► The temperature of the thermal treatment controls particle sizes. ► The preparation procedure has been scaled up to the 100 g scale. ► This method is appropriate for the large-scale industrial preparation of multimetallic systems.