Síntese de óxidos metálicos binários suportados em carbono amorfo (printex 6L) para a produção eletroquímica de peróxido de hidrogênio (H2O2)

O presente trabalho visa o estudo da eletrossíntese de H2O2 a partir da reação de redução de oxigênio (RRO) utilizando carbono Printex 6L modificado com óxidos binários compostos de nióbio, molibdênio e paládio, síntetizados pelo método dos precursores poliméricos. A análise dos materiais preparados foi feita a partir de experimentos de análise termogravimétrica (do inglês, TGA), fluorescência de raios X (FRX) e também de difração de raios X (DRX). As temperaturas de síntese foram escolhidas a partir dos resultados de TGA e tendo como temperatura máxima de 400 °C. As análises dos espectros de emissão de FRX mostraram a eficiência na incorporação dos materiais na matriz de carbono. Experimentos de DRX mostraram a presença de fases cristalinas de MoO2 e Nb2 O5 e PdO, e em comparação aos resultados da técnica de voltametria cíclica, existem pares redox que podem ser associados as transições dos metais nos estados de oxidação de +4 e +5, para molibdênio e nióbio, respectivamente e do estado +2 para o paládio. Nos experimentos de voltametria de varredura linear pode-se observar a tendência de maior geração de H2O2 pelo material com teor de 1% NbMo quando comparado com o carbono Printex 6L, de modo que foram calculadas as eficiências de geração de H2O2 , obtendo um resultado de 55,5% para o modificador de 1% NbMo comparado com 47,4% para o Printex 6L, e também de número de elétrons envolvidos na reação com um valor de 2,9 para o material de 1% e 3,1 para o carbono Printex. As análises das curvas de Koutechy-Levich confirmam os resultados anteriores. Análises em condições reduzidas na síntese orgânica corroboraram a melhor eficiência do material de 1% para o material com nióbio e molibdênio e revelaram a também a melhora eletrocatalítica do carbono quando incorporado com óxidos mistos de nióbio e paládio, sendo o melhor resultado expresso no material contendo 5% de nióbio e paládio, na proporção molar de 95 para 5% de cada elemento, respectivamente.

Memoria sobre la elaboración del agua clorurada y de los cloruros de los óxidos de los metales alcalinos calcio y sodio... seguida de una noticia sobre los medios fumigatorios, incluso el de Guyton-Morveau... /

Mode of access: Internet.

Vida de la bendita madre Isabel de Santo Domingo, compañera de Santa Teresa de Iesus, coadjutora de la santa en la nueua reforma de la Orden ..., fundadora del Monasterio de S. Iosef de Çaragoça, i relacion de la compañeras que traxo i de las hijas que crio en este monasterio /

Mode of access: Internet.

“Num só crio pra vender, não” : etnicidade, gênero e saberes domésticos em Moita Verde (Parnamirim, RN)

O presente trabalho consiste em etnografia realizada na comunidade quilombola de Moita Verde, Parnamirim (RN). Pensada a partir do processo de emergência étnica, tendo como campo de analise o espaço doméstico para pensar a relação entre as mulheres e as distintas arenas políticas, das relações entre famílias, com o entorno e agentes de Estado. Em especial, o envolvimento das mulheres com a criação de porcos vinculada a um sistema que se relaciona com outros saberes do sítio que vão para além da dimensão técnica, levando em consideração os saberes e práticas do grupo. Além disso, este saber, associado com outros saberes políticos, em contexto de relações étnico-raciais, pode ser usado dos debates sobre identidade e especificidade de direitos.

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

Obtenção de óxidos a base de níquel e cobalto para reação de oxidação parcial do metano

Nickel-based catalysts supported on alumina have been widely used in various reactions to obtain synthesis gas or hydrogen. Usually, higher conversion levels are obtained by these catalysts, however, the deactivation by coke formation and sintering of metal particles are still problems to be solved. Several approaches have been employed in order to minimize these problems, among which stands out in recent years the use of additives such as oxides of alkali metals and rare earths. Similarly, the use of methodologies for the synthesis faster, easier, applicable on an industrial scale and to allow control of the microstructural characteristics of these catalysts, can together provide the solution to this problem. In this work, oxides with spinel type structure AB2O4, where A represents divalent cation and B represents trivalent cations are an important class of ceramic materials investigated worldwide in different fields of applications. The nickel cobaltite (NiCo2O4) was oxides of spinel type which has attracted considerable interest due to its applicability in several areas, such as chemical sensors, flat panel displays, optical limiters, electrode materials, pigments, electrocatalysis, electronic ceramics, among others. The catalyst precursor NiCo2O4 was prepared by a new chemical synthesis route using gelatine as directing agent. The polymer resin obtained was calcined at 350°C. The samples were calcined at different temperatures (550, 750 and 950°C) and characterized by X ray diffraction, measurements of specific surface area, temperature programmed reduction and scanning electron microscopy. The materials heat treated at 550 and 750°C were tested in the partial oxidation of methane. The set of techniques revealed, for solid preparations, the presence of the phase of spinel-type structure with the NiCo2O4 NixCo1-xO solid solution. This solid solution was identified by Rietveld refinement at all temperatures of heat treatment. The catalyst precursors calcined at 550 and 750°C showed conversion levels around 25 and 75%, respectively. The reason H2/CO was around 2 to the precursor treated at 750°C, proposed reason for the reaction of partial oxidation of methane, one can conclude that this material can be shown to produce synthesis gas suitable for use in the synthesis Fischer-Tropsch process

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

Degradação do PMMA através da reação despolimerização uitlizando catalisadores de óxidos mistos

In this work, mixed oxides were synthesized by two methods: polymeric precursor and gel-combustion. The oxides, Niquelate of Lanthanum, Cobaltate of Lanthanum and Cuprate of Lanthanum were synthesized by the polymeric precursor method, and treated at 300 º C for 2 hours, calcined at 800 º C for 6h in air atmosphere. In gel-combustion method were produced and oxides using urea and citric acid as fuel, forming for each fuel the following oxides Ferrate of Lanthanum, Cobaltato of Lanthanum and Ferrato of Cobalt and Lanthanum, which were submitted to the combustion process assisted by microwave power maximum of 10min. The samples were characterized by: thermogravimetric analysis, X-ray diffraction; fisisorção of N2 (BET method) and scanning electron microscopy. The reactions catalytic of depolymerization of poly (methyl methacrylate), were performed in a reactor of silica, with catalytic and heating system equipped with a data acquisition system and the gas chromatograph. For the catalysts synthesized using the polymeric precursor method, the cuprate of lanthanum was best for the depolymerization of the recycled polymer, obtaining 100% conversion in less time 554 (min), and the pure polymer, was the Niquelate of Lanthanum, with 100% conversion in less time 314 (min). By gel-combustion method using urea as fuel which was the best result obtained Ferrate of Lanthanum for the pure polymer with 100% conversion in less time 657 (min), and the recycled polymer was Cobaltate of Lanthanum with 100 % conversion in less time 779 (min). And using citric acid to obtain the best result for the pure polymer, was Ferrate of Lanthanum with 100% conversion in less time 821 (min and) for the recycled polymer, was Ferrate of Lanthanum with 98.28% conversion in less time 635 (min)

Preparação de óxidos mistos de níquel e zinco nanoparticulados a partir de combustíveis alternativos

The field of "Materials Chemistry" has been developing in recent years and there has been a great increase of interest in the synthesis and chemical and physical properties of new inorganic solids. New routes of synthesis and synthesis modified has been developed with the aim not only to optimize the processes in laboratory scale, but also on an industrial scale, and make them acceptable by current environmental legislation. The phenomenology of current solid state chemistry properties coupled with the high temperature superconductivity, ferromagnetism, porosity molecular and colors are evidence affected by the synthesis method, which in turn can influence the technological application of these materials. From this understanding, mixed oxides of nickel and zinc nanoparticulate were synthesized by microwave-assisted combustion route using three specific types of organic fuels employing the weight ratios 1:1/2 and 1:1 of cation metallic/fuel, in order to investigate the influence of such proportions to obtain the solids. The new fuels were chosen to replace, for example, urea or glycine that are the fuels most commonly preferred in this kind of synthesis. The powders without heat treatment were studied by Thermogravimetric analysis (TGA), X-Ray Diffraction (XRD) and then calcined at 900°C. After heat treatment, the samples were characterized by analysis of X Ray Diffraction (XRD) and Scanning Electron Microscopy (SEM). The modified synthesis route porposed was effective for obtaining powders. Both the alternative fuels chosen as the different weight ratios employed, influenced in the morphology and obtaining oxides

Fabricación y caracterización de películas delgadas de óxidos transparentes con aplicaciones ópticas.

Los óxidos transparentes conductores (TCO′ s) son materiales compuestos conformados por oxígeno y un metal, que presentan una combinación única de alta estabilidad química, alta concentración electrónica y alta transparencia óptica. Por esta razón, el procesamiento de TCO′ s en película delgada va orientado hacia aplicaciones específicas tales como ventanas ópticas en celdas solares, sensores de gases, electrodos en dispositivos de pantallas planas, ventanas inteligentes. En este proyecto se trabajó en la síntesis experimental de dos TCO′ s relevantes tanto en investigación fundamental como en aplicaciones tecnológicas: el óxido de indio (In2O3) y el óxido de estaño (SnO2). Ambos TCO′ s se depositaron por la técnica de erosión iónica reactiva por corriente directa (DC). Para el análisis de las películas se utilizaron varias técnicas de caracterización: difracción de rayos X, espectroscopia UV-Visible, resistividad eléctrica, efecto Hall, así como microscopías electrónica de barrido y de fuerza atómica. Se fabricó también una bicapa de In2O3/SnO2, la cual se caracterizó además con espectroscopia de fotoemisión de rayos X (XPS).En esta tesis se reporta por primera vez la síntesis y caracterización de esta bicapa, la cual abre una línea de investigación en el área de interfaces. Asimismo, se desarrolló e implementó un procedimiento, basado en los modelos ópticos, tal que permite obtener parámetros que se utilizan para evaluar a cualquier película delgada TCO como potencial metamaterial. Las propiedades de las muestras se analizaron en función de la temperatura aplicada post-depósito: temperatura ambiente (TA), 100oC, 200oC, 300oC, bajo una atmósfera de argón o argón-oxígeno. Los resultados confirman que las películas presentan un crecimiento de tipo poli cristalino. Además, la calidad cristalina tiende a incrementarse como función del incremento de la temperatura. El In2O3 creció con estructura cúbica bcc (a=10.11 ˚A, ICDD #71-2195). A partir de 200C, se detectaron trazas de la fase romboédrica (a=5.490 ˚A, c=14.520 ˚A, ICDD #73-1809). Asimismo, el SnO2 creció con estructura tetragonal (a = 4.737 ˚A, c = 3.186 ˚A, ICDD #88-0287). Las películas de In2O3 poseen una transparencia promedio del 90 % en una ventana de 500 nm a 1100 nm. El borde de absorción se recorre al azul como función de la temperatura, de Eg=3.3 eV a Eg=3.7 eV por el efecto Burstein-Moss. Por otra parte, la bicapa presentó una interfaz claramente definida, sin difusión de especies metálicas. Al incrementarse la temperatura, de TA a 400oC, se detectaron dos fases de óxido de estaño: SnO2 y SnO, en un porcentaje atómico de ≈70 %:30 %, respectivamente. Se concluye que los parámetros y valores obtenidos de las películas como son el texturizado y espesor homogéneo, alta transparencia, crecimiento preferencial, ancho prohibido y resistividad eléctrica, son comparables a los que se requieren del In2O3 y SnO2 en película delgada para aplicaciones optoelectrónicas.