Rare earth complex Eu(phen)2Cl3·2H2O synthesized by precipitation method was incorporated into MCM-41 mesoporous molecular sieves which were synthesized via a hydrothermal method. Hybrid inorganic/organic mesoporous luminescent material Eu(phen)2/MCM-41 has been characterized by XRD, TEM, IR, UV-visible spectra and fluorescence spectra. Results indicated that the hybrid mesoporous material has typical structure of MCM-41 and retains the same pore structure as MCM-41 after the assembly process. The fluorescence spectra of these materials present a series of narrow lines assigned to 5D0 → 7F0,1,2,3,4 transitions. The high emission intensity observed is a promising property for application of the rare earth complex in technological luminescent devices.