The synthesis of yttria-stabilized zirconia nanoparticles with a fine control on the chemical composition and the distribution of yttrium cations is of major interest to master the mechanical, optical or ionic conduction properties of the final material. However, a fine control of this chemical homogeneity within the particles, especially above 5 mol.% of yttria (Y 2 O 3), is challenging with conventional synthesis routes. In the present study, for the first time the interest of using supercritical sol-gel like synthesis is demonstrated for the continuous production in a single step of high quality zirconia (ZrO 2) nanocrystals of 7 nm stabilized with Y 2 O 3 without post-treatment. Three compositions are investigated, i.e., 1.5, 3, and 8 mol.% of Y 2 O 3 and in-depth physico-chemical characterizations such as X-ray diffraction, total X-ray scattering, High-resolution electron microscopy, Raman and X-ray photoelectron spectroscopy are performed to asses and thus prove the successful synthesis of these different compositions while keeping a good chemical homogeneity. This enables to confirm that this original process leads to a unique and fine structural control for such small yttria-doped zirconia nanocrystals.< Leer menos