904 resultados para solid-state-reaction technique
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Hydrogenated bulk Zn1-xCoxO samples were synthesized via standard solid-state reaction route with Co molar concentrations up to 15 at.%. Magnetic characterization demonstrates a room temperature ferromagnetic behavior associated to a paramagnetic Curie-Weiss component. Detailed microstructural analysis was carried out to exclude the presence of extrinsic sources of ferromagnetism. The magnetization increases linearly as a function of Co concentration. Hall measurements reveal an insulating character for the whole set of samples. In this context, the defect mediated magnetic coupling between the Co atoms under the scope of the bound magnetic polarons model is used to interpret the observed room temperature ferromagnetism. © 2012 Elsevier B.V. All rights reserved.
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Lead-free solid solutions (1-x)Bi0.5Na0.5TiO 3 (BNT)-xBaZr0.25Ti0.75O3 (BZT) (x=0, 0.01, 0.03, 0.05, and 0.07) were prepared by the solid state reaction method. X-ray diffraction (XRD) and Rietveld refinement analyses of 1-x(BNT)-x(BZT) solid solution ceramic were employed to study the structure of these systems. A morphotropic phase boundary (MPB) between rhombohedral and cubic structures occured at the composition x=0.05. Raman spectroscopy exhibited a splitting of the (TO3) mode at x=0.05 and confirmed the presence of MPB region. Scanning electron microcopy (SEM) images showed a change in the grain shape with the increase of BZT into the BNT matrix lattice. The temperature dependent dielectric study showed a gradual increase in dielectric constant up to x=0.05 and then decrease with further increase in BZT content. Maximum coercive field, remanent polarization and high piezoelectric constant were observed at x=0.05. Both the structural and electrical properties show that the solid solution has an MPB around x=0.05. © 2012 Elsevier Ltd and Techna Group S.r.l.
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In this work, the electrochemical behavior of Cu-16(wt.%)Zn-6.5(wt.%)Al alloy containing the β'-phase (martensite) was studied in borate buffer solution (pH 8.4) by means of open-circuit potential (EOC), electrochemical impedance spectroscopy (EIS) and cyclic voltammetry (CV). The alloy EOC was -0.29 V vs. Hg/HgO/OH-, similar to that of pure copper in this medium, indicating that the processes which occur on the alloy surface are mainly governed by copper. EIS response was related to the dielectric and transmission properties of the complex oxide layer. The CVs showed peaks concerning the redox reactions for copper and zinc. These peaks were assigned to the formation and reduction of copper and zinc species. Furthermore, they showed that the copper oxidation was suppressed by the presence of zinc and aluminum in the alloy composition. The copper and zinc oxidation to form complex oxide layers and the reduction of the different metallic oxides generated in the anodic potential scan suggest that a solid state reaction could determine the metallic oxide formation. © 2013 Elsevier Ltd. All rights reserved.
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In the current article, we studied the effect of yttrium [Y3+] ions' substitution on the structure and electric behavior of barium zirconate titanate (BZT) ceramics with a general formula [Ba1-x Y 2x/3](Zr0.25Ti0.75)O3 (BYZT) with [x = 0, 0.025, 0.05] which were prepared by the solid-state reaction method. X-ray diffraction patterns indicate that these ceramics have a single phase with a perovskite-type cubic structure. Rietveld refinement data confirmed [BaO 12], [ZrO6], [TiO6], [YO6] clusters in the cubic lattice. The Y3+ ions' effects on the electric conductivity behavior of BZT ceramics as a function of temperature and frequency are described, which are based on impedance spectroscopy analyses. The complex impedance plots display a double semicircle which highlights the influences of grain and grain boundary on the ceramics. Impedance analyses showed that the resistance decreased with the increasing temperature and resulted in a negative temperature coefficient of the resistance property in all compositions. Modulus plots represent a non-Debye-type dielectric relaxation which is related to the grain and grain boundary as well as temperature-dependent electric relaxation phenomenon and an enhancement in the mobility barrier by Y3+ ions. Moreover, the electric conductivity increases with the replacement of Ba 2+ by Y3+ ions may be due to the rise in oxygen vacancies. © 2013 The Minerals, Metals & Materials Society and ASM International.
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This paper reports on the structural characterization of Pb 1-xLaxZr0.40Ti0.60O3 (PLZT) ferroelectric ceramic compositions prepared by the conventional solid state reaction method. X-ray absorption spectroscopy (XAS) and Raman spectroscopy were used to probe the local structure of PLZT samples that exhibits a normal and relaxor ferroelectric behavior. From the Zr K-edge and Pb LIII-edge EXAFS spectra, a considerable dissymmetry of Zr and Pb sites was observed in all samples, including those showing a long-range order cubic symmetry and a relaxor behavior. The Raman spectroscopy results confirmed the existence of a local disorder in all PLZT samples through the observation of Raman active vibrational modes. The variation in the intensity of the E(TO 3) mode in the PLZT relaxor samples indicates that the process of correlation between nanodomains stabilizes at temperatures lower than T m. © 2013 Elsevier B.V. All rights reserved.
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Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)
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Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)
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Pós-graduação em Ciência e Tecnologia de Materiais - FC
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Pós-graduação em Ciência e Tecnologia de Materiais - FC
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Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)
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The processing of ferroelectric BaBi4Ti4O15 (BBT) ceramics from powders prepared by conventional solid state reaction (SSR) and mechanochemical activation (MA) has been investigated. It was shown that MA synthesis reduces the synthesis temperature of BBT powders, leading to smaller particles with reduced anisotropy and consequently to smaller grain size of ceramics. Dielectric properties were investigated in a wide range of temperatures (20-800 degrees C) and frequencies (1.21 kHz to 1 MHz). The relative dielectric permittivity at Curie temperature was higher for solid state obtained ceramics than for the mechanically treated ones. The conductivity of sintered samples was studied, suggesting decreasing of conductivity of BBT-MA in comparison with BBT-SS ceramics. The influence of the grain and the grain boundaries contribution to the dielectric behavior in both ceramics was analyzed through impedance spectroscopy. A well-defined ferroelectric hysteresis loop was obtained for both samples. (C) 2014 Elsevier Ltd and Techna Group S.r.l. All rights reserved.
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The study of ceramic materials is constantly evolving, especially in research related to advanced ceramics. Once these have many applications, this paper relates to synthesis by solid state reaction of calcium copper titanate (CCTO) ceramic material means doping with strontium. The powders were characterized using thermal analysis techniques such as TG (thermogravimetry), DTA (differencial thermal analysis), dilatometry, X-ray diffraction (XRD) and scanning electron microscopy (SEM). The compositions have submitted weight loss at around 6% with respect to carbonates used, and was attributed a temperature of 950° C to perform the calcination according to thermogravimetric analysis. After the process of calcination and milling, the particles presented approximately spherical shapes and high percentages of substitution Ca2+ with Sr2+ was evident by the presence of necks between to particles due to the milling calcination. Analyses with Energy Dispersive Spectroscopy (EDS) showed stoichiometries in different samples very similar to the theoretical stoichiometry
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The synthesis of calcium titanate, CaTiO3, was performed by mechanical activation and thermal treatment. Milling for up to 360 minutes in a planetary ball mill mechanically activated an equimolar mixture of CaCO 3 and TiO2 powders. A small amount of mechanically activated mixtures was pressed into briquettes and calcined at 850°C for two hours. The effect of mechanical activation on the solid-state reaction was studied using X-ray powder diffraction and differential thermal analysis. The change of morphology and size of powder particles due to milling, were determined by SEM, while BET analysis was used to determine the specific surface area of the powder. The sintering process was followed by a dilatometer during thermal treatment up to 1300°C. The main conclusion of the analysis of conducted investigations is that CaTiO3 ceramics can be obtained from an activated mixture at a much lower temperature than reported in the literature owing to acceleration of the chemical reaction and sintering.
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Since the discovery of YBaCuO, experiments have shown that its superconducting properties are strongly affected by the oxygen content. More recently, anelastic relaxation measurements in La2CuO4+δ, showed that the decrease in the oxygen content can be related to two events. One is the decrease in mobility between two adjacent CuO planes, and the other is the increase in the number of tilting patterns of the CuO6 octahedra. In the case of the bismuth-based ceramic, it is known that the oxygen content, within some limits, does not affect its superconducting properties. In order to evaluate the mobility and the effect of the oxygen content on this material we have prepared BSCCO ceramic and tested regarding its internal friction and electrical resistivity as a function of the temperature while the oxygen content was being reduced by a sequence of vacuum annelaing at 620 K. The samples were prepared in the Bi:Sr:Ca:Cu = 2212 and 2223 proportion, using powder obtained by the sol-gel route and conventional solid state reaction. The anelastic relaxation measurements were performed using a torsion pendulum operating with frequency about 15-35 Hz between 77 to 700 K. The diffraction pattern of the as sintered and the vacuum annealed material were also presented. The results have shown complex anelastic relaxation structures that were associated to the jump of interstitial oxygen atoms between two adjacent CuO planes. The vacuum annealing showed to be deleterious to the critical temperature of the superconducting ceramic.
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Pós-graduação em Ciência dos Materiais - FEIS