Synthesis and characterization of lanthanum- and yttrium-doped Fe2O3 pigments

MELO, D. M. A. et al. Synthesis and charactezarion of lanthanum and yttrium doped Fe2O3 pigments. Cerâmica, São Paulo, v. 53, p. 79-82, 2007.

Synthesis and characterization of lanthanum- and yttrium-doped Fe2O3 pigments

MELO, D. M. A. et al. Synthesis and charactezarion of lanthanum and yttrium doped Fe2O3 pigments. Cerâmica, São Paulo, v. 53, p. 79-82, 2007.

Síntese e caracterização de NiO-CGO para anodo e eletrólitos sólidos e base de Céria para SOFC

The direct use of natural gas makes the Solid Oxide Fuel Cell (SOFC) potentially more competitive with the current energy conversions technologies. The Intermediate Temperature SOFC (IT-SOFC) offer several advantages over the High Temperature SOFC (HT-SOFC), which includes better thermal compatibility among components, fast start with lower energy consumption, manufacture and operation cost reduction. The CeO2 based materials are alternatives to the Yttria Stabilized Zirconia (YSZ) to application in SOFC, as they have higher ionic conductivity and less ohmic losses comparing to YSZ, and they can operate at lower temperatures (500-800°C). Ceria has been doped with a variety of cations, although, the Gd3+ has the ionic radius closest to the ideal one to form solid solution. These electrolytes based in ceria require special electrodes with a higher performance and chemical and termomechanical compatibility. In this work compounds of gadolinia-doped ceria, Ce1-xGdxO2-δ (x = 0,1; 0,2 and 0,3), used as electrolytes, were synthesized by polymeric precursors method, Pechini, as well as the composite material NiO - Ce0,9Gd0,1O1,95, used as anode, also attained by oxide mixture method, mixturing the powders of the both phases calcinated already. The materials were characterized by X ray diffraction, dilatometry and scanning electronic microscopy. The refinement of the diffraction data indicated that all the Ce1-xGdxO2-δ powders were crystallized in a unique cubic phase with fluorite structure, and the composite synthesized by Pechini method produced smaller crystallite size in comparison with the same material attained by oxide mixture method. All the produced powders had nanometric characteristics. The composite produced by Pechini method has microstructural characteristics that can increase the triple phase boundaries (TPB) in the anode, improving the cell efficiency, as well as reducing the mass transport mechanism effect that provokes anode degradation

Síntese, caracterização e cinética da decomposição térmica dos materiais cerâmicos PrMO3 (M = Ni ou Co)

In this work have been studied the preparation, characterization and kinetic study of decomposition of the polymerizing agent used in the synthesis under non-isothermal condition ceramics PrMO3 of general formula (M = Co and Ni). These materials were obtained starting from the respective metal nitrates, as a cations source, and making use of gelatin as polymerizing agent. The powders were calcined at temperatures of 500°C, 700°C and 900°C and characterized by X-ray Diffraction (XRD), Thermogravimetric Analysis (TG / DTG/ DTA), Infrared Spectroscopy (FTIR), Temperature Programmed Reduction (TPR) and Scanning Electron Microscopy (SEM). The perovskite phase was detected in all the X-rays patterns. In the infrared spectroscopy observed the oxide formation as the calcination temperature increases with the appearance of the band metal - oxygen. The images of SEM revealed uniform distribution for the PrCoO3 and particles agglomerated as consequence of particle size for PrNiO3. From the data of thermal analysis, the kinetics of decomposition of organic matter was employed using the kinetics methods called Model Free Kinetics and Flynn and Wall, in the heating ratios 10, 20 and 30° C.min-1 between room temperature and 700°C. Finally, been obtained the values of activation energy for the region of greatest decomposition of organic matter in samples that were determined by the degree of conversion (α)

Síntese e caracterização de espinélios a base de Cu, Fe e Cr para pigmentos cerâmicos

Inorganic pigment comprises a host lattice, which is part of the chromophore component (usually a transition metal cation) and possible components modifiers, which stabilize, add or restate the properties pigments. Among the materials with spinel, ferrites, and the chromite stand out, because they have broad technological importance in the area of materials, applicability, pigments, catalytic hydrogenation, thin film, ceramic tiles, among others. The present work, pigments containing CuFe2O4, CuCr2O4,e CuFeCrO4, were synthesized by a method that makes use of gelatin as organic precursor using their application to ceramic pigments. The pigments were characterized by X-ray diffraction (XRD), Infrared spectroscopy, scanning electron microscopy (SEM) spectroscopy in the UV-visible and Colorimetry. The results confirmed the feasibility of the synthetic route used, with respect to powders synthesized, there is the formation of spinel phase from 500°C, with an increase in crystallinity and the formation of other phases. The pigments were shown to be crystalline and the desired phases were obtained. The copper chromite have hues ranging from green to black according to the calcination temperature, while the copper chromite doped with iron had brownish. The ferrites showed copper color and darker brown to black, which may indicate an interesting factor because of the importance of black pigment

Síntese, estudo cinético e análise microestrutural do sistema cério-níquel obtido pelo método pechini

The cerium oxide has a high potential for use in removing pollutants after combustion, removal of organic matter in waste water and the fuel-cell technology. The nickel oxide is an attractive material due to its excellent chemical stability and their optical properties, electrical and magnetic. In this work, CeO2-NiO- systems on molars reasons 1:1(I), 1:2(II) e 1:3(III) metal-citric acid were synthesized using the Pechini method. We used techniques of TG / DTG and ATD to monitor the degradation process of organic matter to the formation of the oxide. By thermogravimetric analysis and applying the dynamic method proposed by Coats-Redfern, it was possible to study the reactions of thermal decomposition in order to propose the possible mechanism by which the reaction takes place, as well as the determination of kinetic parameters as activation energy, Ea, pre-exponential factor and parameters of activation. It was observed that both variables exert a significant influence on the formation of complex polymeric precursor. The model that best fitted the experimental data in the dynamic mode was R3, which consists of nuclear growth, which formed the nuclei grow to a continuous reaction interface, it proposes a spherical symmetry (order 2 / 3). The values of enthalpy of activation of the system showed that the reaction in the state of transition is exothermic. The variables of composition, together with the variable temperature of calcination were studied by different techniques such as XRD, IV and SEM. Also a study was conducted microstructure by the Rietveld method, the calculation routine was developed to run the package program FullProf Suite, and analyzed by pseudo-Voigt function. It was found that the molar ratio of variable metal-citric acid in the system CeO2-NiO (I), (II), (III) has strong influence on the microstructural properties, size of crystallites and microstrain network, and can be used to control these properties

Otimização do processo de síntese do aluminato de cobalto via método de polimerização de complexos (MPC) através do planejamento fatorial fracionado

In the ceramics industry are becoming more predominantly inorganic nature pigments. Studies in this area allow you to develop pigments with more advanced properties and qualities to be used in the industrial context. Studies on synthesis and characterization of cobalt aluminate has been widely researched, cobalt aluminate behavior at different temperatures of calcinations, highlighting especially the temperatures of 700, 800 and 900° C that served as a basis in the development of this study, using the method of polymerization of complex (CPM), economic, and this method applied in ceramic pigment synthesis. The procedure was developed from a fractional factorial design 2 (5-2) in order to optimize the process of realization of the cobalt aluminate (CoAl2O4), having as response surfaces the batch analysis data of Uv-vis spectroscopy conducted from the statistic software 7.0, for this were chosen five factors as input variables: citric acid (stoichiometric manner), puff or pyrolysis time (h), temperature (° C), and calcinations (° C/min), at levels determined for this study. By applying statistics in the process of obtaining the CoAl2O4 is possible the study of these factors and which may have greater influence in getting the synthesis. The pigments characterized TG/DSC analyses, and x-ray diffraction (XRD) and scanning electron microscope (SEM/EDS) in order to establish the structural and morphological aspects of pigment CoAl2O4, among the factors studied it were found to statically with increasing calcinations temperature 700°< 800 <900 °C, the bands of Uv-vis decrease with increasing intensity of absorbance and that with increasing time of puff or pyrolysis (h) there is an increase in bands of Uv-vis proportionally, the generated model set for the conditions proposed in this study because the coefficient of determination can explain about 99.9% of the variance (R²), response surfaces generated were satisfactory, so it s possible applicability in the ceramics industry of pigments

Síntese e caracterização de catalisadores de LaNiO3 não suportados e suportados em Al2O3 e ZrO2 para a reforma a vapor do metano

Ionic oxides with ABO3 structure, where A represents a rare earth element or an alkaline metal and B is a transition metal from group VIII of the periodic table are potential catalysts for oxidation and good candidates for steam reforming reaction. Different methods have been considered for the synthesis of the oxide materials with perovskite structure to produce a high homogeneous material with low amount of impurities and low calcination temperatures. In the current work, oxides with the LaNiO3 formula had been synthesized using the method of the polymeric precursors. The thermal treatment of the materials took place at 300 ºC for 2h. The material supported in alumina and/or zirconia was calcined at 800 ºC temperature for 4h. The samples had been characterized by the following techniques: thermogravimetry; infrared spectroscopy; X-ray diffraction; specific surface area; distribution of particle size; scanning electron microscopy and thermo-programmed reduction. The steam reforming reaction was carried out in a pilot plant using reducing atmosphere in the reactor with a mixture of 10% H2-Argon, a mass about 5g of catalyst, flowing at 50 mL.min-1. The temperature range used was 50 - 1000 oC with a heating rate of 10 oC.min-1. A thermal conductivity detector was used to analyze the gas after the water trapping, in order to permit to quantify the consumption of hydrogen for the lanthanum nickelates (LaNiO3). The results showed that lanthanum nickelate were more efficient when supported in alumina than when supported in zirconia. It was observed that the methane conversion was approximately 100% and the selectivity to hydrogen was about 70%. In all cases were verified low selectivity to CO and CO2

Influência da temperatura de formação do íon de Keggin no processo de pilarização de esmectitas

As amostras de esmectita do estado do Pará, Amazônia, Brasil foram caracterizados utilizando XRD, FTIR e análise textural por curvas isotérmicas adsorpition-desorption nitrogênio. Na produção das argilas pilarizadas foi usado o íon Al13 (o íon de keggin), este íon foi obtido pela reação das soluções AlC(l3)6H2O / NaOH, com razão molar OH/Al=2, com intercalação em temperatura ambiente, durante as 3 horas e calcinada em 450ºC (temperatura adequada da calcinação). O material foi preparado utilizando soluções produzidas na faixa de temperatura de 25, 45, 65, 85, 105ºC, o Resultado mostrou que o processo de pilarização aumenta o espaçamento basal da argila natural de 14,02 para 19,74 Å e a área superficial de 44,30 para 198,03m²/g. a estabilidade térmica da argila natural foi melhorada pelo procedimento de pilarização.

Otimização do tempo e temperatura no processamento da gipsita oriunda dos cristalizadores da produção de sal para obter gesso de uso na construção civil

During the process of the salt production, the first the salt crystals formed are disposed of as industrial waste. This waste is formed basically by gypsum, composed of calcium sulfate dihydrate (CaSO4.2H2O), known as carago cru or malacacheta . After be submitted the process of calcination to produce gypsum (CaSO4.0,5H2O), can be made possible its application in cement industry. This work aims to optimize the time and temperature for the process of calcination of the gypsum (carago) for get beta plaster according to the specifications of the norms of civil construction. The experiments involved the chemical and mineralogical characterization of the gypsum (carago) from the crystallizers, and of the plaster that is produced in the salt industry located in Mossoró, through the following techniques: x-ray diffraction (XRD), x-ray fluorescence (FRX), thermogravimetric analysis (TG/DTG) and scanning electron microscopy (SEM) with EDS. For optimization of time and temperature of the process of calcination was used the planning three factorial with levels with response surfaces of compressive mechanical tests and setting time, according norms NBR-13207: Plasters for civil construction and x-ray diffraction of plasters (carago) beta obtained in calcination. The STATISTICA software 7.0 was used for the calculations to relate the experimental data for a statistical model. The process for optimization of calcination of gypsum (carago) occurred in the temperature range from 120° C to 160° C and the time in the range of 90 to 210 minutes in the oven at atmospheric pressure, it was found that with the increase of values of temperature of 160° C and time calcination of 210 minutes to get the results of tests of resistance to compression with values above 10 MPa which conform to the standard required (> 8.40) and that the X-ray diffractograms the predominance of the phase of hemidrato beta, getting a beta plaster of good quality and which is in accordance with the norms in force, giving a by-product of the salt industry employability in civil construction

Influência da temperatura de formação do íon de Keggin no processo de pilarização de esmectitas

As amostras de esmectita do estado do Pará, Amazônia, Brasil foram caracterizados utilizando XRD, FTIR e análise textural por curvas isotérmicas adsorpition-desorption nitrogênio. Na produção das argilas pilarizadas foi usado o íon Al,₁₃ (o íon de keggin), este íon foi obtido pela reação das soluções AlC_l36H₂O/aOH, com razão molar OH/Al=2, com intercalação em temperatura ambiente, durante as 3 horas e calcinada em 450ºC (temperatura adequada da calcinação). O material foi preparado utilizando soluções produzidas na faixa de temperatura de 25, 45, 65, 85, 105ºC, o Resultado mostrou que o processo de pilarização aumenta o espaçamento basal da argila natural de 14,02 para 19,74 Å e a área superficial de 44,30 para 198,03m,²/g. a estabilidade térmica da argila natural foi melhorada pelo procedimento de pilarização.

Possibilidades e limitações no uso da temperatura em cromatografia líquida de fase reversa

High-temperature liquid chromatography (HTLC) is a technique that presents a series of advantages in liquid phase separations, such as: reduced analysis time, reduced pressure drop, reduced asymmetry factors, modified retentions, controlled selectivities, better efficiencies and improved detectivities, as well as permitting green chromatography. The practical limitations that relate to instrumentation and to stationary phase instability are being resolved and this technique is now ready to be applied for routine determinations.

Caracterização reológica das diferentes fases de extrato de inulina de raízes de chicória, obtidas por abaixamento de temperatura

Inulin is a functional food ingredient, generally employed as sugar or fat substitute in food systems. This ingredient can be found in several vegetal products, including chicory roots. As the solubility of inulin is susceptible to temperature changes, the product suffers a fractionalization resulting in two phases when cooled, originating a precipitated phase, more viscose, and a liquid phase, of lesser viscosity. The study of rheological properties of different phases of inulin extract is important for equipment designing, such as mixer and bombs. In this work, rheological behavior at three different temperatures (25; 40 and 50 ºC) was determined for liquid and precipitated phases of inulin liquid extract, extracted from chicory roots by hot water diffusion and cooled at two different temperatures (8 and -10 ºC), suffering phases separation. The precipitated phase was analyzed in two conditions: pure and with the addition of microencapsulating agents (maltodextrin and hydrolized starch). All of them presented a linear behavior, similar to that of the Plastics of Bingham. Some of them, however, were not an adequate fit to this model.

Influência da embalagem de polietileno de baixa densidade e da temperatura na conservação do repolho minimamente processado

This research studied the effect of low density polyethylene packaging and storage temperature on the preservation of fresh-cut (minimally processed) cabbage. The cabbages, previously cooled to a temperature of 10 ºC, were selected, washed, cut in four parts (with the central stalk removed), sanitized, cut in strips, rinsed, put in the centrifuge, weighed and stored in plastic packaging of low density polyethylene (70 µm), and then stored in cold chambers at temperatures of 1 and 10 ºC for 20 days. The following aspects were evaluated: carbon dioxide, oxygen and ethylene in the internal atmosphere of the package as well as, pH, titratable acidity, total soluble solids, vitamin C, loss of fresh mass and the total soluble solids/acidity in the fresh-cut cabbage ratio. The experimental design was entirely casual, with three repetitions. The analysis parameters, except for the vitamin C, loss of fresh mass and ethylene, presented significant variation between the temperatures and days of storage. The cabbage stored at a temperature of 1 ºC presented a shelf life of around 15 days, significantly higher than that stored at 10 ºC. At this temperature, on the 8th day of storage, the product was completely decayed, unfit for commercialization or consumption.

Efeitos da temperatura do ar, linhagem e período do dia nas freqüências de ocorrências e tempos de expressão comportamental de matrizes pesadas

Behavioral adjustments may occur fast and with less cost than the physiological adaptations. Considering the social behavior is suggestive that the frequency and the intensity of aggressive interactions, the total social cohesion and the extent of vicious attitudes may be used to evaluate welfare. This research presents an analysis of the interactions between the experimental factors such as temperature, genetic and time of the day in the behavior of female broiler breeders under controlled environment in a climatic chamber in order to enhance the different reaction of the birds facing distinct environmental conditions. The results showed significant differences between the behaviors expressed by the studied genetics presenting the need of monitoring them in real-time in order to predict their welfare in commercial housing, due to the complexity of the environmental variables that interfere in the well being process. The research also concluded that the welfare evaluation of female broiler breeders needs to consider the time of the day during the observation of the behaviors.