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Nanosized ZrO2 powder was prepared by evaporative decomposition of solution (EDS). The particle size is from 50nm to 200nm. This process has such advantages as high purity, precise compositional control, simple procedure and successive auto-operating. In this process, mixed solution of zirconium acetate and yttrium nitrate was atomized to from a fine mist and blown into the hot zone from the bottom of face. The solution was rapidly decomposed at 900℃ and the powder was collected by a filter system. The powder characteristics can be controlled by adjusting the concentration, droplet volume and decomposition temperature of the solution.