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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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Abstract  

The present work investigates the influence of milling and calcination atmosphere on the thermal decomposition of SrTiO3 powder precursors. Both pure and neodymium-modified SrTiO3 samples were studied. Milling did not significantly influence numerical mass loss value, but reduced the number of decomposition steps, modifying the profiles of the TG and DTA curves. On the other hand, milling increases the amount of energy liberated by the system upon combustion of organic matter. It was also observed that the milling process, associated to the calcination in an oxygen atmosphere, considerably decreases the amount of organic matter and increases the final mass loss temperature.

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Journal of Thermal Analysis and Calorimetry
Authors: Márcia Silva, Mary Alves, S. Lima, L. Soledade, Elaine Paris, E. Longo, A. Souza, and Iêda Santos

Abstract  

Sr(Ti,Nd)O3 was synthesized in order to evaluate the influence of the amount of neodymium on the thermal and structural properties of SrTiO3. The synthesis was carried out using the polymeric precursor method. A small mass gain was observed for the SrTiO3 and SrTi0.98Nd0.02O3 samples accompanied by an exothermic peak in the DTA curves. Other steps at higher temperatures are assigned to the combustion of the organic material and carbonate. Elimination of defects by previous calcination of the precursors is responsible by the short and long range ordering of the perovskite. Cubic phase was obtained for undoped and doped SrTiO3.

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Journal of Thermal Analysis and Calorimetry
Authors: A. de Oliveira, J. Ferreira, Márcia Silva, Soraia de Souza, F. Vieira, E. Longo, A. Souza, and Iêda Santos

Abstract  

NiWO4 and ZnWO4 were synthesized by the polymeric precursor method at low temperatures with zinc or nickel carbonate as secondary phase. The materials were characterized by thermal analysis (TG/DTA), infrared spectroscopy, UV–Vis spectroscopy and X-ray diffraction. NiWO4 was crystalline after calcination at 350 °C/12 h while ZnWO4 only crystallized after calcination at 400 °C for 2 h. Thermal decomposition of the powder precursor of NiWO4 heat treated for 12 h had one exothermic transition, while the precursor heat treated for 24 h had one more step between 600 and 800 °C with a small mass gain. Powder precursor of ZnWO4 presented three exothermic transitions, with peak temperatures and mass losses higher than NiWO4 has indicating that nickel made carbon elimination easier.

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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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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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