A β-diketonate-type ligand, N-(3-methoxyl–phenyl)ketoacetamide (L), and its complexes with europium (III) and terbium (III) were synthesized. The ligand and complexes were characterized by elemental analysis, IR spectra, 1HNMR spectra, mass spectra and luminescent spectra. The complexes were characterized by elemental analysis, IR spectra. The stoichiometry of metal-to-ligand in the complexes also was confirmed by the fluorescence behavior of the ligand and complexes in CH3CH2OH solution. In addition, the fluorescence properties of complexes in DMF, CH3OH, CH3CH2OH, acetone and CHCl3 were investigated. The characteristic fluorescence of terbium (III) was assigned.