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Abstract  

With the aim of obtaining materials with applications in pigments, CoxZn7-xSb2O12 spinels were synthesized using the Pechini method. This method consists in the formation of a polymeric net, where the metallic cations are homogeneously distributed. In this work, two types of alcohol (ethyl glycol and ethylene glycol) were used for the synthesis of a zinc antimoniate spinel, CoxZn7-xSb2O12 (x=0-7). The materials were characterized by termogravimetry (TG) and differential thermal analysis (DTA). TG results indicated a decrease in total mass loss when cobalt was added to the solution substituting zinc, for samples prepared using the two different alcohols. Decomposition temperatures, obtained by TG and DTA, presented a decreasing behavior as cobalt was added to the material. In relation to the alcohols, all results indicated a better polymerization of the resin when ethylene glycol was used, being the most indicated one for cation immobilization. X-ray diffraction did not show differences between the two alcohols - both presented the spinel phase (Co, Zn)2.33Sb0.67O4. Samples with higher quantity of cobalt also presented ilmenite phase (Co, Zn)Sb2O6.

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Ln PO 4 producing. A derivative of the sol–gel methods is the synthesis route and patented by Pechini [ 24 ]. In this method carboxylic acids (e.g., citric acid) are used as the reagents chelating metal ions in the solution, glycols are used

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Abstract  

Effect of the synthesis conditions of Pechini technique on crystallinity and purity of Na3Ce(PO4)2 compound was investigated. Nano-sized cerium-sodium phosphate obtained when EDTA was used as an additional chelating agent for Ln3+. The total enthalpy change of Na3Ce(PO4)2 phase transition was determined as 14.2±0.7 kJ mol−1 for sample synthesized by conventional solid-solid reaction. The phase transition process was confirmed to occur at 1060°C or in temperature range 920–1060°C depending on thermal treatment of powders.

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Journal of Thermal Analysis and Calorimetry
Authors: M. Bernardi, E. Antonelli, A. Lourenço, C. Feitosa, L. Maia, and A. Hernandes

Abstract  

The results reported here based on a study of BaTi1–xZrxO3 (x=0, 0.2 and 1) nanometric powders prepared by the modified Pechini method. The powder samples annealed from 600 to 1000C/2 h were characterized by thermogravimetric analysis (TG), differential scanning calorimetry (DSC), X-ray diffraction (XRD) and scanning electron microscopy (SEM) techniques. The decomposition reactions of resins were studied using thermal analysis measurements. The barium titanate zirconate system presented just one orthorhombic phase. Furthermore, this study produced BaTiO3 powders with a tetragonal structure using shorter heat treatments and less expensive precursor materials than those required by the traditional methods.

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Abstract  

TiO2–CeO2 oxides for application as ceramic pigments were synthesized by the Pechini method. In the present work the polymeric network of the pigment precursor was studied using thermal analysis. Results obtained using TG and DTA showed the occurrence of three main mass loss stages and profiles associated to the decomposition of the organic matter and crystallization. The kinetics of the degradation was evaluated by means of TG applying different heating rates. The activation energies (E a) and reaction order (n) for each stage were determined using Horowitz–Metzger, Coats–Redfern, Kissinger and Broido methods. Values of E a varying between 257–267 kJ mol–1 and n=0–1 were found. According to the kinetic analysis the decomposition reactions were diffusion controlled.

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Journal of Thermal Analysis and Calorimetry
Authors: F. Vieira, Soraia Souza, A. Oliveira, S. Lima, E. Longo, C. Paskocimas, L. Soledade, A. Souza, and Iêda Santos

Abstract  

In this study undoped and Cr, Sb or Mo doped TiO2 were synthesized by polymeric precursor method and characterized by X-ray diffraction, UV–VIS spectroscopy, infrared spectroscopy and thermogravimetry (TG). The TG curves showed a continuous mass loss assigned to the hydroxyl elimination and Cr6+ reduction. Doped TiO2 samples showed a higher mass loss assigned to water and gas elimination at lower temperatures. In these doped materials a decrease in the anatase–rutile phase transition temperature was observed. After calcination at 1,000 °C, rutile was obtained as a single phase material without the presence of Cr6+.

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Journal of Thermal Analysis and Calorimetry
Authors: M. A. F. Souza, R. A. Candeia, S. J. G. Lima, M. R. Cassia-Santos, I. M. G. Santos, E. Longo, and A. G. Souza
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Journal of Thermal Analysis and Calorimetry
Authors: Camila Xavier, R. Candeia, M. Bernardi, S. Lima, E. Longo, C. Paskocimas, L. Soledade, A. Souza, and Iêda Santos

Abstract  

Magnesium and zinc ferrites have been prepared by the polymeric precursor method. The organic material decomposition was studied by thermogravimetry (TG) and differential thermal analysis (DTA). The variation of crystalline phases and particle morphology with calcination temperature were investigated using X-ray diffraction (XRD) and scanning electronic microscopy (SEM), respectively. The colors of the ferrites were evaluated using colorimetry. Magnesium ferrite crystallizes above 800°C, presenting a yellow- orange color with a reflectance peak at the 600–650 nm range, while zinc ferrite crystallizes at 600°C, with a reflectance peak between 650–700 nm, corresponding to the red-brick color.

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Journal of Thermal Analysis and Calorimetry
Authors: Mary Alves, Soraia Souza, Márcia Silva, Elaine Paris, S. Lima, R. Gomes, E. Longo, A. de Souza, and Iêda Garcia dos Santos

Abstract  

SrSnO3 was synthesized by the polymeric precursor method with elimination of carbon in oxygen atmosphere at 250 °C for 24 h. The powder precursors were characterized by TG/DTA and high temperature X-ray diffraction (HTXRD). After calcination at 500, 600 and 700 °C for 2 h, samples were evaluated by X-ray diffraction (XRD), infrared spectroscopy (IR) and Rietveld refinement of the XRD patterns for samples calcined at 900, 1,000 and 1,100 °C. During thermal treatment of the powder precursor ester combustion was followed by carbonate decomposition and perovskite crystallization. No phase transition was observed as usually presented in literature for SrSnO3 that had only a rearrangement of SnO6 polyhedra.

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Journal of Thermal Analysis and Calorimetry
Authors: Márcia Silva, Lydianne de O. Miranda, Maria Cassia-Santos, S. Lima, L. Soledade, E. Longo, C. Paskocimas, A. Souza, and Iêda Santos

Abstract  

Undoped and/or doped with 1 mol% of Co2+ Mg2TiO4 andMg2SnO4 powders were synthesized by the polymeric precursor method. The influence of the network former (Sn4+ or Ti4+) on the thermal, structural and optical properties was investigated. The recorded mass losses are due to the escape of water and adsorbed gases and to the elimination of the organic matter. Mg2TiO4 crystallizes at lower temperatures and also presents more ordered structure with a smaller unit call and having more intense green color than Mg2SnO4 has.

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