The thermal evolution of positron annihilation parameters in nanosized 10 mol % Y 2 O 3 doped ZrO 2 powders is presented. Three positron lifetimes have been determined up to 900 ºC annealing temperature. The two major ones have been interpreted, one as a mean between positron annihilation in the bulk and in vacancy-like open volume defects and the other, as due to annihilation in higher sized volume defects. The intensity ratio between the two defect structures depends on temperature and could be reflecting the thermal t"-to cubic metastable transformation known to occur in the studied system.1 Introduction Zirconia-based ceramic systems have been widely studied due to their excellent mechanical and electrical properties. Three equilibrium polymorphs are known for pure zirconia: monoclinic (up to 1200 ºC), tetragonal (up to 2400 ºC) and cubic (up to melting point) [1,2]. One of the main objectives in zirconia ceramics research is the stabilization of the tetragonal phase at RT, often achieved by the addition of a trivalent oxide as Y 2 O 3 is. As this situation provokes a certain amount of oxygen vacancies in the ZrO 2 host lattice for charge balance, the characterization and identification of the generated defects becomes most relevant since the electrical properties of yttria doped zirconias (YSZ) depend on the defect structure. Positron annihilation spectroscopy has proved to be an excellent tool for defect identification [3,4]. In particular, it was applied to the study of generated defects in ZrO 2 oxides upon doping with different trivalent oxides [5][6][7]. In the present work we present PALS results obtained on a 10 mol % Y 2 O 3 -stabilized ZrO 2 system (10YSZ) whose hyperfine interaction had been already determined [1]. The nanocrystalline powder synthesized by a nitrate-citrate gel-combustion process and stabilized in the metastable t"-form of the tetragonal phase, was characterized at the nanoscopic level using mainly the Perturbed Angular Correlations technique. Oxygen vacancy movement is revealed as a slow diffusion process involving a very small activation energy. As the powder was heated, a t"-to-cubic transformation occurred around 600 °C. Here, the evolution of the positron annihilation parameters with annealing temperature is analyzed in order to determine the existing different defect structures and correlate them with the phase evolution observed by PAC.