Gd2-xEuxO3 powder materials doped with Eu3+ using different concentration from x = 0 to 2 were prepared by a new sol-lyophilization synthesis and fiber single crystal (Gd2O3-Gd2O3/Eu3+) oxides were grown using laser-heated pedestal growth (LHPG) technique. X-ray powder diffraction performed at room temperature showed that the materials obtained by lyophilization technique are cubic, lies in the nanometer range and different from bulk materials. The materials are a continued solid solution and the lattice parameter a-axis increases with Eu3+ concentration. The fibers grown by LHPG technique were single crystal, transparent, red in color when Eu3+ concentration is high, and the structure is monoclinic for Eu3+ < 15%. The luminescence of Eu3+ from C-2 crystallographic site was been detected. In the case of nano-particles oxide, an additional peak in emission spectral is obtained at lambda = 610 nm. The influence of Eu3+, particles sizes and the structure on the luminescence spectral of Eu3+ ions was been described. (C) 2004 Elsevier B.V. All rights reserved.