In this paper, it was demonstrated that Y2O3 microprisms could be prepared by a mixed-solvothermal method with triethylene tetramine as precipitator and sequent heat treatment process. X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopic (TEM) and high-resolution transmission electron microscopic (HRTEM) were used to characterize the products. The height of the Y4O(OH)(9)(NO3) microprisms is about 1.2 mu m and the length of the side of the bottom surface is about 0.6 mu m. It was found that the composition of solvent, dosage of triethylene tetramine, reaction time and reaction temperature had great effect on the morphologies of the final products. The as-obtained product via solvothermal process, monoclinic yttrium oxide hydroxide nitrate, Y4O(OH)(9)(NO3), could convert to Y2O3 with the same morphology after annealing at high temperatures. Eu3+ doped Y2O3 microprisms were also prepared and their photoluminescence (PL) properties were investigated. This method may be applied to prepare other rare earth oxides with complex structures. (C) 2012 Elsevier Ltd. All rights reserved.