The synthesis of Fe3+-stabilized zirconia by the nitrate/urea combustion route was investigated. Using several characterization techniques, including X-ray diffraction, field-emission-gun scanning electron microscopy and notably Mossbauer spectroscopy. it was possible to determine the appropriate amount of urea that allows to obtain a totally stabilized Zr0.9Fe0.1O1.95 solid solution. The nanocrystalline zirconia solid solution is mostly tetragonal. but the presence of the cubic phase could not be ruled out. An in-depth study of the thermal stability in air showed that the Fe3+ solubility in the stabilized solid solution starts to decrease at about 875 degrees C which results in the formation of hematite (possibly containing some Zr4+) at the surface of the zirconia grains and further provokes the progressive transformation into the monoclinic zirconia phase. (C) 2009 Elsevier Ltd. All rights reserved.