Yttria doped nanocrystalline zirconia powder was prepared by spray-pyrolysis technique. Powder crystallized into tetragonal form, as dense and compositionally homogeneous polycrystalline spheres. X-Ray diffraction (XRD) and high resolution transmission electron microscopy (HRTEM) have been used in order to characterize the mean size and the size distribution of crystalline domains. An average size of 6 nm was calculated by Scherrer formula from X-Ray diffraction pattern. The domain size, determined by analysis method developed by Hytch from HRTEM observations, ranges from 5 to 22 nm with a main population around the value 12 nm. Limits and complementary nature of XRD and HRTEM methods are discussed.