X-ray powder diffraction, transmission electron microscopy, and field-emission scanning electron microscopy were adopted to investigate the evolution process of Dy2O3 precursor microspheres and tripod-like structures, and a possible self-assembled process was identified during the morphology evolution. The same Dy2O3 microspheres and tripod-like structures were obtained by the calcination of the Dy2O3 precursors. The Dy2O3 microspheres with the diameter of 200-300 nm are consisted of the nanoparticles, while tripod-like Structures were assembled from variform bulky particles that were evolved from microspheres, the lengths of three arms are nearly the same about 10 mu m, and the angle between two arms is about 120 degrees. Photoluminescence measurement shows that Dy2O3 microspheres and tripod-like structures have one broad emission peak centered at 430 nm with the 341 nm excitation. (C) 2008 Elsevier B.V. All rights reserved.