Nanocrystals of uniform dysprosium oxide (Dy2O3) particles have been prepared by homogeneous precipitation technique. The particles were produced by aging DyCl(3)solution in presence of urea at elevated temperature. The particles were characterized with respect to their size, shape, and thermal decomposition behavior. It was found that the precipitated particles were spherical, uniform in size, and amorphous in nature. Upon heating in air, these particles decomposed into oxide and no change in morphology was observed. The dysprosium ion concentration was found to have significant effect on the particle size and its distribution.