Zirconia nano-particles have been produced by the hydrolysis of ZrOGl2 solution in the reverse micelles of a liquid-liquid two-phase system, in which sodium bis(2-ethylhexyl) sulfosuccinite (AOT) and toluene were chosen as the surfactant and organic phase, respectively. The reverse micelles prevented the aggregation of primary particles and reduced the diameters of zirconia nanoparticles. Superfine zirconia powders soft-aggregated by the zirconia nano-particles were obtained. The diameters of zirconia nanoparticles were influenced by the quantity of the surfactant.