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Journal of Thermal Analysis and Calorimetry
Authors: Gabriel de Araujo, Dalva de Faria, Márcio Zaim, Flávio de Souza Carvalho, Fabio de Andrade, and Jivaldo Matos

Abstract  

Tibolone polymorphic forms I (monoclinic) and II (triclinic) have been prepared by recrystallization from acetone and toluene, respectively, and characterized by different techniques sensitive to changes in solid state, such as polarized light microscopy, X-ray powder diffractometry, thermal analysis (TG/DTG/DSC), and vibrational spectroscopy (FTIR and Raman microscopy). The nonisothermal decomposition kinetics of the obtained polymorphs were studied using thermogravimetry. The activation energies were calculated through the Ozawa’s method for the first step of decomposition, the triclinic form showed a lower E a (91 kJ mol−1) than the monoclinic one (95 kJ mol−1). Furthermore, Raman microscopy and DSC at low heating rates were used to identify and follow the thermal decomposition of the triclinic form, showing the existence of three thermal events before the first mass loss.

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Journal of Thermal Analysis and Calorimetry
Authors: Mauro da Silva, Flávio de Souza Carvalho, Tereza da Silva Martins, Márcia de Abreu Fantini, and Paulo Isolani

Abstract

Two series of lanthanide oxides with different morphologies were synthesized through calcinations of two types of citrate polymeric precursors. These oxides were characterized by XRD patterns, SEM electronic microscopy, and N2 adsorption isotherms. SEM microscopy analysis showed that the calcination of crystalline fibrous precursors [Ln2(LH)3·2H2O] (L = citrate) originated fibrous shaped particles. On the other hand, the calcination of irregular shaped particles of precursors [LnL·xH2O] originated irregular shaped particles of oxide, pointing out a morphological template effect of precursors on the formation of the respective oxides.

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