Análise por difração de raios x de filmes de óxidos cerâmicos compostos por IrO2/TiO2/CeO2

Independent of the sample form (powder or film), XRD analysis of Ir0,3Ti(0,7-x)Ce xO2, (nominal) mixtures, for x=0, shows the formation of a solid solution phase between IrO2 and TiO2, as well as the rutile phases of IrO2 and TiO2. The presence of the anatase phase of TiO2 is also confirmed. The introduction of 30 mol% CeO2 in the mixture reveals the presence of the CeO2 and Ce2O3 phases, besides the already mentioned ones, in the powder. In the film form, however, an amorphous phase is identified. When all of the TiO2 is substituded by CeO2, for both sample forms, the only phases found are IrO2, CeO2 and Ce2O3. This result suggests cerium oxides are not capable of forming solid solutions with either IrO2 or (Ir,Ti)O2 acting solely as a dispersant matrix for these phases. These results are consistent with the much higher electrochemically active surface area when CeO2 is introduced in the binary Ti/Ir0,3Ti0,7O2 mixture. It was possible to establish a relationship between the electrochemical stability of the supported films and their crystalline structure. The unexpected presence of TiO2 and Ti2O3 in the Ti/Ir0,3Ce0,7O2 (film sample) is attributed to oxidation of the Ti support during the calcination step.

Reação de geração de oxigênio em eletrodos de Mn2O3 suportados em aço inoxidável

A study of the kinetics of oxygen evolution in alkaline conditions from ceramic films of Mn2O3 supported on stainless steel was carried out. This study has been done through the determination of transfer coefficients, Tafel slopes and exchange currents using potentiodynamic and quasi-potentiostatic measurements. The activation energy was determined as a function of the overpotential and, additionally, the electrode active surface was estimated. The results are consistent with data already published for other electrodes, implying that the methods used in this work were reliable and precise.

Preparação e caracterização de pós cerâmicos de aluminatos de lítio

The preparation of gamma-LiAlO2 by coprecipitation and sol-gel synthesis was investigated. Ceramic powders obtained by coprecipitation synthesis were prepared from aqueous solutions of aluminum and lithium nitrates using sodium hydroxide as precipitant agent. By sol-gel synthesis, the ceramic powders were prepared from hydrolysis of aluminum isopropoxide. The materials obtained by two routes of synthesis were dried at 80ºC and calcined at 550, 750, 950 and 1150ºC. The characterization was done by X-ray diffraction, infrared spectroscopy, emission and absorption atomic spectrometry, helium picnometry, specific surface area (BET method) and scanning electronic microscopy. Mixtures of crystalline phases were obtained by coprecipitation synthesis: 80ºC- LiAl2(OH)7.2H2O + Al(OH)3; 550 and 750ºC- alpha-LiAlO2 + eta-Al2O3; 950 and 1150ºC- gamma-LiAlO2 + LiAl5O8. Chemical analysis showed molar ration Al/Li @ 3. Crystalline single-phases were obtained by sol-gel synthesis above 550ºC: 550ºC-alpha-LiAlO2; 750, 950 and 1150ºC-gamma-LiAlO2. These powders presented molar ration Al/Li @ 1. Thus, gamma-LiAlO2 crystalline phase was obtained at 750ºC by sol-gel synthesis while by coprecipitation synthesis, a mixture of crystalline phases was obtained. These results showed the superiority of the sol-gel synthesis for the preparation of pure gamma-LiAlO2.

Caracterização de cinza de casca de arroz para uso como matéria-prima na fabricação de refratários de sílica

The characterization of rice husk ash, a deriving by-product of the burning of the rice husk during the rice processing is the object of this study. This by-product, for being rich in silica, can be an important raw material for the production of siliceous ceramics, such as thermal insulators and refractory. A combination of surface analysis, thermal analysis and microscopy analysis techniques was used for the characterization. The characterized by-product presented as main component the silica, under amorphous form, with a maximum content of alkalis around 1%, features that become it potentially interesting for the production of ceramic materials.

Resistência química de vitro-cerâmicos pertencentes a sistemas Li2O-ZrO2-BaO-SiO2 frente ao tratamento com soluções ácidas e básicas

The chemical durability of the Li2O-ZrO2-BaO-SiO2 system was examined by determination of the Vickers hardness. The dependence of hardness and of the chemical resistance with BaO addition was investigated. The experimental results indicate that the hardness increases with the BaO content. The samples surface's morphology submitted to the chemical treatment in acidic (H2SO4) and basic (KOH) solution was accompanied by scanning electron microscopy. The chemical durability of the materials with BaO showed better than the glass ceramic without this content. These materials treated with H2SO4 solution showed a preferential attack to the silica rich sites.

Células a combustível de baixa potência para aplicações estacionárias

A paradigmatic shift in developing fuel cell for stationary applications has been occurring in the last ten years. Previously, 100 kW class to a few MW class power plants were preferred but recently, the development has drifted towards units of only a few kW. The motivation is the present market situation, which favors disperse residential electric power generation from natural or liquefied gas. Membrane-type fuel cells are very promising for this application, due to their present state of development in the automobile industry. More recently, small ceramic fuel cells (SOFC) has also been found to be adequate for this application. Considering a family of 4 members, 1 kW (electric) units seem to be optimal for individual residences. This presentation discusses briefly the Brazilian scenario with respect to these units.

Fractionation of Wood Extracts

The aim of this thesis was to fractionate wood extracts into pure fractions using membrane technology, to observe membrane behaviour in solvents and to study the effect of conditioning on membrane performance. Four different wood extracts were used in the performed filtrations. In the literature part, the focus was on the effect of different solvent properties on polymeric membranes, especially on their retention and flux. Solute properties, such as shape, polarity and charge, were examined. Transport models, membrane stability and ways to improve the stability, when solvents were filtered, were also discussed. The experimental part consisted of a series of filtrations, where the effect of the wood extracts and solvent concentration on solute retention was observed. Polymeric and ceramic membranes were tested under different conditions and the solute analyses were performed with GC and GC-MS. It was discovered that it is possible to fractionate wood extracts using membrane technology to some extent, but more research must be done to understand the mechanisms behind the various interactions between the solvent and the membrane. Conditioning was also considered as an important part of the membrane pre-treatment.

Nano vitrocerâmica de escória de aciaria

The manufacture of glass-ceramics is an alternative route for the commercial use of metallurgical slags. Such types of glass-ceramics may find commercial applications owing to their low cost, good mechanical properties and superior visual aspect. Besides, due to the elimination of that industrial residue from the environment and also due to the possibility of replacement of natural stones such as marbles and granites, the use of slags is an activity with strong ecological appeal. While the use of blast-furnace slags for the production of glass-ceramics is well known, the utilization of steel making slags constitutes a challenge, because these materials possess low concentration of SiO2. In this work a novel composition for producing glasses and glass-ceramics from a steelmaking slag is presented. The crystal nucleation kinetics, the characterization of the resulting microstructures for two different thermal treatments and mechanical properties of the glass-ceramics are discussed. A glass-ceramic having a marble aspect, fine volumetric crystallization, high degree of crystallization and improved mechanical strength was obtained.

Estudo do efeito da quantidade de óxido de ferro em cinzas pesadas de carvão mineral na obtenção de vitrocerâmicos

Bottom ash has been used as raw material to glass and glass ceramic production because it is a source of SiO2 and Al2O3. However, the high concentration of iron (about 10% wt.) difficulty the control of the nucleation and the crystallization processes. The iron content was reduced by magnetic process, where the magnetite phase was mainly removed. In order to compare glass ceramics obtained from original and low iron bottom ashes, microstructural and dilatometric characterizations were performed.

Síntese, caracterização e estudo das propriedades catalíticas e magnéticas de nanopartículas de Ni dispersas em matriz mesoporosa de SiO2

Nickel nanoparticles supported on amorphous silica ceramic matrix were synthesized by the polymeric precursor method. The nanostructure was characterized by NMR, BET, XRD, SEM, TEM, and flame atomic absorption spectrometry techniques. It was observed a dependence of the crystallite size on the thermal annealing, under a N2 atmosphere. The materials presented a high catalytic activity and selectivity upon the beta-pinene hydrogenation reaction. The magnetic hystereses were also correlated with the morphology of the processed material.

Desenvolvimento de um dispositivo para obtenção de monocristais de ligas à base de cobre

This paper describes the drawing, construction and optimization of a device, which can be used to obtain single crystals of different metallic materials with melting point from 550 to 1050 ºC. Components of ease obtaining and of low cost were used. The device was based on the modified Bridgman technique and it was used to obtain single crystals of copper-based alloys. The temperature axial profiles and a difference less then 1% in the temperature between the wall and the center of the ceramic tube in the critical region for obtaining single crystals of good quality indicated that the oven presents a good thermal stability. Single crystals of CuZnAl and CuAlAg alloys of good quality were growth and characterized using optical microscopy and Laüe X-ray back reflection.

Fish colonization of artificial reefs in a large Neotropical reservoir: material type and successional changes

Artificial reefs have barely been used in Neotropical reservoirs (about five studies in three reservoirs), despite their potential as a fishery management tool to create new habitats and also to understand fish ecology. We experimentally assessed how reef material (ceramic, concrete, and PVC) and time modulated fish colonization of artificial reefs deployed in Itaipu Reservoir, a large reservoir of the mainstem Parana´ River, Brazil. Fish richness, abundance, and biomass were significantly greater in the reef treatments than at control sites. Among the experimental reefs, ceramic followed by the concrete treatments were the materials most effectively colonized, harboring the majority of the 13 fish species recorded. Although dependent on material type, many of the regularities of ecological successions were also observed in the artificial reefs, including decelerating increases in species richness, abundance, mean individual size, and species loss rates with time and decelerating decreases of species gain and turnover rates. Species composition also varied with material type and time, together with suites of life history traits: more equilibrium species (i.e., fishes of intermediate size that often exhibit parental care and produce fewer but larger offspring) of the Winemiller-Rose model of fish life histories prevailed in later successional stages. Overall, our study suggests that experimental reefs are a promising tool to understand ecological succession of fish assemblages, particularly in tropical ecosystems given their high species richness and low seasonality

Espectrofotometría de absorción atómica con tubo en la llama: aplicación en la determinación total de cadmio, plomo y zinc en aguas frescas, agua de mar y sedimentos marinos

Thermospray flame furnace Atomic Absorption Spectrometry (TS-FF-AAS) was used for the total determination of Cd, Pb and Zn in fresh water and seawater samples at µg L-1 levels, and in marine sediment samples at µg g-1 levels. Using a sample loop of 50 µL and a peristaltic pump the samples were transported into the metallic tube placed over an air/acetylene flame, through a ceramic capillary (o.d. = 3.2 mm) containing two parallel internal orifices (i.d = 0.5 mm). The detection limits determined for Cd, Pb and Zn using a synthetic water matrix (2.5% m/v NaCl, 0.5% m/v MgCl2 and 0.8% m/v CaCl2) were 0.32 µg L-1; 2.6 µg L-1 and 0.21 µg L-1 respectively. The methodology by TS-FF-AAS was validated by determination of Cd, Pb and Zn in certified reference materials of water and marine sediment, and the t-test for differences between means was applied. No statistically significant differences were established in fresh water and seawater (p>0.05), whereas differences became apparent in marine sediment (p<0.03).

NMR in Crystals and Powders of Topazes with Different Colours

The present work is a part of the large project with purpose to investigate microstructure and electronic structure of natural topazes using NMR method. To reach this task we determined the relative contents of fluorine and hydrogen in crystals blue, colorless, wine and wine irradiated topazes. Then we determined the electric field gradients in site of aluminium atoms by NMR method, calculated EFG using ab initio method, and measured relaxation time dependence on heating temperature for blue, colorless, Swiss blue and sky blue topazes. Nuclear magnetic resonance (NMR) is an effective method to investigate the local structure in the crystal. The NMR study of the single crystal gives detailed information especially about the local crystal structure. As a result of this work we have received practical data, which is possible to use in future for making personal dosimetry and for preparation of mullite, which is widely used in traditional and advanced ceramic materials.