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A series of luminescent hybrid materials Eu (Phen)2Cl3/MCM-41 that the different assembled mass of Eu(Phen)2Cl3 included into the channels of MCM , have been synthesized by combining ultrasound technology. The properties of the hybrid materials were characterized by XRD(X-ray Diffraction), N2-adsorption-desorption, FT-IR and luminescence spectrum. The results show that the rare-earth compounds had been loaded into the holes of mesoporous material MCM-41. The luminescence intensities of the hybrid materials were improved as the increase of the loading concentration of the rare-earth complexes. The hybrid material has the maximal luminescence intensity when it reached the saturated loading concentration (7.17%). To compare with the pure rare-earth complex, the thermal stability of the hybrid materials were enhanced by about 100°C.