Abstract: Several new binary complexes which were composed of europium(terbium,dysprosium) and tert-butylbenzoicacid have been synthesized.Such photoactive complexes with different concentrations were introduced into inorganic host tetrethoxysilane(TEOS) to prepare solid powder materials through hydrolysis and polycondensation processes(sol-gel method).Ultra-violet abs orption,fluorescence excitation and emission spectra and scanning electronic microscope were applied to characterize the sample materials,which shows that the hybrid composites are of high efficiency and strong luminescence of rare earthions is obtained.In the range of composite concentration of luminescent species(0.02,0.05,0.08,0.1mmol),emission intensities increase with the corresponding composite concentration and the concentration quenching effect has not occurred.