136 resultados para Organic Chemical Synthesis (030503)
em Repositório Institucional UNESP - Universidade Estadual Paulista "Julio de Mesquita Filho"
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Nanosized and highly reactive magnesium mobate (MgNb2O6) powders were successfully synthesized by a new wet-chemical method by means of the dissolution of Nb2O5 center dot 5H(2)O and in a solution of oxalic acid followed by the addition of stoichiometric amounts of magnesium carbonate. The Nb-Mg-oxalic acid solution was evaporated resulting in a dry and amorphous powder that was calcined in the temperature range from 200 to 900 degrees C for 2 h. The crystallization process from the amorphous state to the crystalline MgNb2O6 was followed by thermal analysis. The calcined powders characterized by FT-Raman spectroscopy, X-ray diffraction (XRD) and their morphology examined by high resolution scanning electron microscopy (HR-SEM). Pure MgNb2O6, free from the second phases and obtained at 800 degrees C was confirmed by a combined analysis using XRD and FT-Raman. The average diameter of the particles was calculated from the HR-SEM image as 70 urn approximately. This technique allows a better mixing of the constituent elements and thus a better reactivity of the mixture to obtain pre-reaction products with high purity at lower temperatures and reducing cost. It can offer a great advantage in the PMN-PT formation with respect to the solid-state synthesis. (c) 2006 Elsevier Ltd and Techna Group S.r.l. All rights reserved.
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Ultra-fine powders of Na1-xLixNbO3 (x=0; 0.06; 0.09; 0.12) were synthesized by the Polymeric Precursors Method. Such powders had their orthorhombic structures determined by X-ray diffraction and their surface area determined by BET isotherms (less than 10 m(2) g(-1)). Densification was followed by dilatometric study. The powders, calcined at 700 degrees C for 5 h, were sintered at 1290 degrees C during 2 h under ambient atmosphere with no application of extra pressure. The samples with relative densities higher than 95% were analyzed by impedance spectroscopy at room temperature, under a signal amplitude of 1 V-rms. Dielectric constants of about 180 and dielectric loss factor of about 0.03 were measured showing small dependence with frequency. The electrical properties were similar to those obtained for samples sintered by hot pressing. (C) 1999 Elsevier B.V. Limited and Techna S.r.l. All rights reserved.
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Tungsten oxide/titania (WO3/TiO2) nanopowders were synthesized by the polymeric precursor method which varied the WO3 content between 0 and 10 mol%. The powders were thermally treated in a conventional furnace and their structural, microstructural and electric properties were evaluated by X-ray diffraction (XRD), Raman spectrometry, N 2 physisorption, NH3 chemisorption, temperature-programmed reduction (TPR), X-ray absorption near-edge spectroscopy (XANES) in situ XANES and extended X-ray absorption fine structure spectroscopy (EXAFS) and transmission electron microscopy (TEM). XRD and Raman spectrometry confirmed the homogeneous distribution of an amorphous WO3 phase in the TiO 2 matrix which stabilized the anatase phase through the generation of [TiO5·V0] or [TiO5·V 0] complex sites. Conventional TPR-H2 (temperature programmed reduction) along with XANES TPR-H2 and XANES TPR-EtOH showed that WO3/TiO2 sample reduction occurs through the formation of these complex clusters. Moreover, the addition of WO3 promoted an increase in the surface acidity of doped samples as revealed by NH3 chemisorption. The WO3/TiO2 bulk-ceramic samples were further used to estimate their potential application in a humidity sensor in the range of 15-85% relative humidity. Probable reasons that lead to the different humidity sensor responses of samples were given based on the structural and surface characterizations. Correlation between the sensing performance of the sensor and its structural features are also discussed. Although all samples responded as a humidity sensor, the W2T sample (2 mol% added WO3) excelled for sensitivity due to the increase in acid sites, optimum mean pore size and pore size distribution. © 2013 Elsevier B.V.
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Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)
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The one-dimensional coordination polymer of palladium(II) with pyrazolato (Pz -) and azide (N 3 -) as bridging ligands, of formula [Pd 3(μ-N 3)(μ-Pz) 5] n, has been prepared. From IR and Raman studies it was evidenced the exobidentate nature of pyrazole ligands as well the μ-1,1-bridging coordination of azido groups. NMR experiments showed two sets of broadened signals with different intensities indicating the presence of pyrazolato groups in distinct chemical environments. The proposed structure of [Pd 3(μ-N 3)(μ-Pz) 5] n consists of a zigzag ribbon in which each (Pz) 2Pd(Pz) 2 entity is bound to two stacked planar units [Pd(μ-Pz)(μ-N 3)Pd core] with very weak Pd-Pd interaction, based on UV-Vis spectroscopy.
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This paper describes research on a simple low-temperature synthesis route to prepare bismuth ferrite nanopowders by the polymeric precursor method using bismuth and iron nitrates. BiFeO 3 (BFO) nanopowders were characterized by means of X-ray diffraction analyses, (XRD), Fourier transform infrared (FT-IR) spectroscopy, Raman spectroscopy (Raman), thermogravimnetric analyses (TG-DTA), ultra-violet/vis (UV/Vis) and field emission scanning electron microscopy (FE-SEM). XRD patterns confirmed that a pure perovskite BiFeO 3 structure with a rhombohedral distorted perovskite structure was obtained by heating at 850 °C for 4 hours. Typical FT-IR spectra for BFO powders revealed the formation of a perovskite structure at high temperatures due to a metal-oxygen bond while Raman modes indicated oxygen octahedral tilts induced by structural distortion. A homogeneous size distribution of BFO powders obtained at 850 °C for 4 hours was verified by FE-SEM analyses. © 2012 Elsevier Ltd and Techna Group S.r.l.
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Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)
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Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)
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Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)
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Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)
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Slightly < 111 >-oriented 0.65Pb(Mg1/3Nb2/3)03-0.35PbTiO(3) ceramic was prepared using fine powders obtained by means of an alternative and promising chemical oxide precursor method. High quality samples with improved structural, microstructural, dielectric and ferroelectric properties were obtained. The dielectric constant value (epsilon similar to 2577) measured at 1 kHz is compared to unpoled < 112 > grain-oriented ceramics while the remanent polarization (P-r similar to 19-1 mu cm(-2)) is compared with random grain-oriented ceramics. These results point out the viability to produce ferroelectric PMN-PT ceramics of very good quality using powder precursors prepared from this chemical method. (c) 2007 Elsevier B.V. All rights reserved.
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O trabalho teve por objetivo estudar as modificações de atributos químicos de um Latossolo Vermelho após dois anos de manejo com adubação orgânica e/ou mineral com diferentes sistemas de cultivo. O experimento foi realizado na área experimental da Universidade Estadual Paulista - UNESP, localizada no município de Selvíria, Estado do Mato Grosso do Sul, no ano agrícola 2004/2005 e 2005/2006. Os tratamentos foram: cultivo convencional; cultivo mínimo e semeadura direta. As adubações foram: testemunha (sem adubação); adubação mineral (300 kg ha-1 da fórmula 20-00-20); adubação orgânica (esterco bovino - 20 Mg ha-1); adubação orgânica (esterco bovino) + ½ adubação mineral recomendada para a cultura utilizada; 20 e 30 Mg ha-1 de lodo de esgoto. em um ano foi utilizada a soja como cultura e no seguinte o sorgo. Avaliaram-se os atributos químicos do solo em quatro camadas. Os atributos químicos do Latossolo Vermelho foram modificados no primeiro ano após as adubações; a adubação com esterco, lodo de esgoto e a combinação do esterco+adubação mineral foram eficazes em modificar os atributos químicos do solo estudado; o lodo de esgoto foi mais eficaz na recuperação do P do solo e, a semeadura direta contribuiu para o aumento de K no solo
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Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)
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Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)
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Synthesis and characterization of antimony tartrate used as a precursor of ceramic powders obtained by Pechini's method were carried out. Antimony tartrate was chosen as a substitute for the antimony citrate commonly used in this chemical processing, because of difficulties in preparing the citrate. FTIR and TGA/DTA analysis showed that antimony tartrate, H-2[Sb-2(C4H2O6)(2)]. forms a polymeric structure. The procedure described indicates that the antimony chelate obtained is adequate for Pechini's method.