An Eu 3ϩ -dibenzoylmethide (DBM) -oligoacrylic acid (OAA) composite was prepared in water, ethanol, and a glycerin mixed solvent. Influence of pH value on the synthesis was also given. A composite with pH of 10.0 was most suitable for the synthesis. It was confirmed by UV-VIS, Fourier transform infrared (FTIR), excitation spectra, and conductivity measurement that DBM, the second ligand, which had low molecular weight, coordinated with Eu 3ϩ in the ionomer chain, instead of dispersing in the OAA matrix. When the molar ratio of DBM-Eu 3ϩ was 2:1, which was found to be the best ratio to obtain the maximum intensity of fluorescence (due to the 5 D 0 3 7 F 2 transition), the fluorescence intensity of the Eu 3ϩ -DBM-OAA (emitted at 616 nm) increased logarithmically with the increase of the molar ratio of Eu 3ϩ -OAA in the range of 0 to 6 : 1. Energy transfer in the composite was also discussed.