Dysprosium carbonates nanoparticles were synthesized by the reaction of dysprosium acetate and NaHCO 3 by a sonochemical method. Dysprosium oxide nanoparticles with average size about 17 nm were prepared from calcination of Dy 2(CO 3) 3·1.7H 2O nanoparticles. Dy(OH) 3 nanotubes were synthesized by sonication of Dy(OAC) 3·6H 2O and N 2H 4. The as-synthesized nanostructures were characterized by scanning electron microscopy (SEM), X-ray powder diffraction (XRD), transmission electron microscopy (TEM), and Fourier transform infrared spectroscopy (FT-IR). Photoluminescence measurement shows that the nanoparticles have two emission peaks around 17,540 cm −1 and 20,700 cm −1, which should come from the electron transition from 4F 9 / 2 → 6H 15 / 2 levels and 4F 9 / 2 → 6H 13 / 2 levels, respectively. The effect of calcination temperature and sonication time was investigated on the morphology and particle size of the products. The sizes could be controlled by the feeding rate of the precipitating agent (NaHCO 3 and N 2H 4) and slower feeding rate lead to smaller nanoparticles.