This work deals with the synthesis and thermal decomposition of complexes of general formula: Ln(ß-dik)3L (where Ln=Tb+3, ß-dik=4,4,4-trifluoro-1-phenyl-1,3- butanedione(btfa) and L=1,10-fenantroline(phen) or 2,2-bipiridine(bipy). The powders were characterized by melting point, FTIR spectroscopy, UV-visible, elemental analysis, scanning differential calorimeter(DSC) and thermogravimetry(TG). The TG/DSC curves were obtained simultaneously in a system DSC-TGA, under nitrogen atmosphere. The experimental conditions were: 0.83 ml.s-1 carrier gas flow, 2.0±0.5 mg samples and 10°C.min-1 heating rate. The CHN elemental analysis of the Tb(btfa)3bipy and Tb(btfa)3phen complexes, are in good agreement with the expected values. The IR spectra evinced that the metal ion is coordinated to the ligands via C=O and C-N groups. The TG/DTG/DSC curves of the complexes show that they decompose before melting. The profiles of the thermal decomposition of the Tb(btfa)3phen and Tb(btfa)3bipy showed six and five decomposition stages, respectively. Our data suggests that the thermal stability of the complexes under investigation followed the order: Tb(btfa)3phen < Tb(btfa)3bipy.