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The Perturbed Angular Correlations technique was used to determine the configurations around Zirconium ions and their thermal behavior in non-aggregated sub-micron zirconia spherical particles. Three residues containing- Zr surroundings were determined for the non-crystalline starting particles, which were identified under the assumption of a certain chemical reactions sequence during synthesis. While the one made up mainly by hydroxyl groups was common to both samples, the two involving mainly organic residues were particle size dependent. Upon crystallization, both sam-ples stabilized in the t´- and t- tetragonal forms and the Xc-cubic form but their amounts and temperatures of appearance were different. On heating, the structure of the smaller particles became gradually monoclinic achieving total degradation upon the subsequent cooling to RT.