Using xylol as the oil phase, span-80 as the surfactant, and an aqueous solution containing zirconium (3 mol% Y2O3) and urea as the water phase, tetragonal phase ZrO2 nano-powders have been prepared via the coupling route of w/o emulsion with urea homogenous precipitation. The effects of the zirconium concentration, the reaction temperature and the urea content on the average size of the products have been examined. The as-prepared ZrO2 powders and the precursor powders were characterized by TGA-DTA, XRD, TEM and BET. Experimental results indicate that ZrO2 powders prepared via the coupling route of w/o emulsion with urea homogenous precipitation possess some excellent characteristics, such as well-rounded spherical shape and excellent dispersing. (C) 2012 Elsevier Ltd. All rights reserved.