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Journal of Thermal Analysis and Calorimetry
Authors: F. M. Aquino, D. M. A. Melo, R. C. Santiago, M. A. F. Melo, A. E. Martinelli, J. C. O. Freitas, and L. C. B. Araújo

Abstract

Thermogravimetric data using the non-isothermal kinetic models of Flynn and Wall and “Model-free Kinetics” were used to determine the activation energy to study the decomposition kinetics of the ligand groups with system’s metallic ions that takes part in the synthesis of PrMO3 (M = Ni or Co). This activation energy was determined for the stage of highest decomposition of the organic matter to establish parameters in synthesis condition optimization and application of the proposed material.

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Journal of Thermal Analysis and Calorimetry
Authors: D. Melo, G. Vicentini, L. Zinner, K. Zinner, H. de Souza, M. Batista, A. Garrido Pedrosa, and R. Bezerra

Abstract  

Complexes of neodymium and europium with amides and aminoxides were synthesized and characterized by complexometric analyses with EDTA, CHN microanalytical procedures, IR absorption spectra, absorption spectra of neodymium complexes, emission spectrum of europium compounds at 77 K, thermogravimetric analyses in N2 and differential scanning calorimetry (DSC) in N2. Infrared spectroscopy results revealed that the nitrate molecules are bound to the central ions as bidentate. Thermogravimetric plots indicated that the decomposition of the complexes occurs in the range 363-1163 K and resulted in the formation of Ln2O3 residues.

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Journal of Thermal Analysis and Calorimetry
Authors: A. Garrido Pedrosa, M. Câmara, F. Borges, H. de Souza, H. Scatena Jr, D. Melo, and L. Zinner

Abstract  

Complexes of rare earth trifluoroacetates (TFA) with 4-methylmorpholine-N-oxide (MMNO) of composition Ln(TFA)33MMNO (Ln=Eu, Dy, Ho, Er, Yb and Y) were synthesized and characterized by elemental analysis data, complexometric titration with EDTA, IR absorption spectra, thermogravimetric analyses and differential scanning calorimetry (DSC) in N2 atmosphere. Infrared spectroscopy data revealed that the MMNO molecules are bound to the central ion through the oxygen of NO groups. These data suggest that the trifluoracetate groups are also coordinated. Thermogravimetric curves indicate that the decomposition of MMNO begins at approximately 350 K and results in Ln2O3 residue at around 1170 K. A theoretical kinetic study was carried out using a QBASIC program with the TG input data for the Dy complex.

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Journal of Thermal Analysis and Calorimetry
Authors: F. T. G. Vieira, A. L. M. Oliveira, D. S. Melo, S. J. G. Lima, E. Longo, A. S. Maia, A. G. Souza, and I. M. G. Santos

Abstract

Alkaline earth stannates have recently become important materials in ceramic technology due to its application as humidity sensor. In this work, alkaline earth stannates doped with Fe3+ were synthesized by the polymeric precursor method, with calcination at 300 °C/7 h and between 400 and 1100 °C/4 h. The powder precursors were characterized by TG/DTA after partial elimination of carbon. Characterization after the second calcination step was done by X-ray diffraction, infrared spectroscopy, and UV–vis spectroscopy. Results confirmed the formation of the SrSnO3:Fe with orthorhombic perovskite structure, besides SrCO3 as secondary phase. Crystallization occurred at 600 °C, being much lower than the crystallization temperature of perovskites synthesized by solid state reaction. The analysis of TG curves indicated that the phase crystallization was preceded by two thermal decomposition steps. Carbonate elimination occurred at two different temperatures, around 800 °C and above 1000 °C.

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Journal of Thermal Analysis and Calorimetry
Authors: D. Melo, R. M. M. Marinho, F. T. G. Vieira, S. J. G. Lima, E. Longo, A. G. Souza, A. S. Maia, and I. M. G. Santos

Abstract

Perovskite type oxides have been intensively studied due to their interesting optical, electrical, and catalytic properties. Among perovskites the alkaline earth stannates stand out, being strontium stannates (SrSnO3) the most important material in ceramic technology among them due to their wide application as dielectric component. SrSnO3 has also been applied as stable capacitor and humidity sensor. In the present work, SrSnO3:Cu was synthesized by polymeric precursor method and heat treated at 700, 800, and 900 °C for 4 h. After that, the material was characterized by thermal analysis (TG/DTA), X-ray diffraction (XRD), infrared spectroscopy, and UV–vis spectroscopy. Results indicated three thermal decomposition steps and confirmed the presence of strontium carbonate and Cu2+ reduction to Cu+ at higher dopant amounts. XRD patterns indicated that the perovskite crystallization started at 700 °C with strontiatite (SrCO3) and cassiterite (SnO2) as intermediate phases, disappearing at higher temperatures. The amount of secondary phase was reduced with the increase in the Cu concentration.

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Journal of Thermal Analysis and Calorimetry
Authors: Edjane F. B. Silva, Marcílio P. Ribeiro, Ana C. F. Coriolano, Ana C. R. Melo, Anne G. D. Santos, Valter J. Fernandes Jr., and Antonio S. Araujo

Abstract

Thermogravimetry was applied in order to investigate the catalytic degradation of heavy oil (15.4oAPI) over silica-based MCM-41 mesoporous molecular sieve. This material was synthesised by the hydrothermal method, using cetyltrimethylammonium bromide as organic template. The physicochemical characterization by nitrogen adsorption, X-ray diffraction, and thermogravimetry, showed that the obtained material presents well-defined structure, with a uniform hexagonal arrangement. The thermal and catalytic degradation of heavy oil was performed by thermogravimetric measurements, in the temperature range from 30 to 900 °C, at heating rates of 5, 10, and 20 °C min−1. By using the model-free kinetics, proposed by Vyazovkin, it was determined that the activation energy to degrade the heavy oil was ca. 128 kJ mol−1, and for degradation of oil in presence of MCM-41, this value decreased to 69 kJ mol−1, indicating the performance of the mesoporores catalyst for the degradation process.

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Journal of Thermal Analysis and Calorimetry
Authors: M. A. F. de Souza, A. G. Souza, R. A. Candeia, D. M. A. Melo, L. E. B. Soledade, M. R. C. Santos, I. M. G. Santos, S. J. G. Lima, and E. Longo
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