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In order to study the luminescent properties of tary rare earth complexes with fl-diketone ligand,three new β-diketone ligands,1-phenyl-3-(p-phenylethynylphenyl)-1,3-propanedione(HPPP), 1-(2-thienyl)-3-(p-phenylethynylphenyl)-l,3-propanedione (HTPP) and 1-(2-furyl)-3-(p-phenylethynylphenyl)-1,3-propanedione (HFPP),were synthesized by Sonogashira coupling reaction and Claisen condensation.Three new tary rare earth complexes,TbL3phen (L = PPP,TPP,or FPP),were synthesized by the reaction of rare earth chloride TbCl3,1,10-phenanthroline (phen) with HPPP,HTPP,or HFPP respectively,in alcohol solution.The compositions were characterized by means of elental analysis,chemical analysis,and IR spectra.Luminescent properties of the three new complexes have been studied.The results show that the tary Tb(Ⅲ) complexes only emit the weak fluorescence of the Tb(Ⅲ) ion,which reveals the triplet state energy of the ligands does not match well with the excited state vibrating energy of Tb3+ ion.