microspheres have been synthesized via a rapid microwave route followed by annealing process. Diverse morphologies of samples can be easily realized by changing the volume ratio of H 2 O/EtOH. The samples were characterized by scanning electron microscopy (SEM), X-ray diffraction (XRD), fourier transform infrared spectroscopy (FT-IR), thermogravimetry analysis (TGA). Under the excitation of UV light, Lu 2 O 3 :Ln 3 + exhibited the characteristic transitions of Ln 3 + , and green (Tb 3 + ), blue (Tm 3 + ), red (Eu 3 + ), yellow (Dy 3 + ) light can be obtained. Under 360 nm irradiation ( 1 D 2 -3 F 4 transition of Tm 3 + ), both characteristic transitions of Tm 3 + and Dy 3 + can be observed in Lu 2 O 3 :1%Tm 3 + ,x%Dy 3 + samples. Furthermore, the critical distance between Tm 3 + and Dy 3 + was calculated, and the energy transfer process from Tm 3 + to Dy 3 + was dipole-dipole interaction. This synthetic method may be useful for preparing other inorganic materials with multi-color emitting.