Two binuclear complexes were successfully synthesized by ultrasound method:[Ln(2-Cl-6-FBA)3(5,5′-DM-2,2′-bipy)(H2O)]2, (Ln=Tb(1), Dy(2); 2-Cl-6-FBA=2‑chloro-6-fluorobenzoicacid; 5,5′-DM-2,2′-bipy=5,5′-dimethyl-2,2′-bipyridine). The crystal structure analysis showed that the two complexes were isomorphic. And they were characterized by IR spectra, Raman spectra and XRD. The fluorescence properties of complex 1 were studied and its luminescence lifetime was calculated. Subsequently, the heat capacity of the two complexes were measured and their thermodynamic functions were obtained. TG-DTG/FTIR/MS technique was used to test the thermal decomposition of the complex in order to better understand the thermal decomposition behavior. Complex 1 was tested at different heating rates to study its non-isothermal kinetics. The relationship between activation energy E and conversion rate α was calculated by M. J. Starink method and NL-INT method. The mechanism functions in the third step decomposition process were determined by double equal-double steps method as G(α) = 1-(1-α)1/2 and f(α) = 2(1-α)1/2. The activation energy E and the pre-exponential factor A were calculated, a series of thermodynamic parameter of the complex were obtained by the equations.
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