Análise do efeito do tempo da moagem de alta energia no tamanho de cristalito e microdeformação da rede cristalina do WC-Co

Hard metals are the composite developed in 1923 by Karl Schröter, with wide application because high hardness, wear resistance and toughness. It is compound by a brittle phase WC and a ductile phase Co. Mechanical properties of hardmetals are strongly dependent on the microstructure of the WC Co, and additionally affected by the microstructure of WC powders before sintering. An important feature is that the toughness and the hardness increase simultaneously with the refining of WC. Therefore, development of nanostructured WC Co hardmetal has been extensively studied. There are many methods to manufacture WC-Co hard metals, including spraying conversion process, co-precipitation, displacement reaction process, mechanochemical synthesis and high energy ball milling. High energy ball milling is a simple and efficient way of manufacturing the fine powder with nanostructure. In this process, the continuous impacts on the powders promote pronounced changes and the brittle phase is refined until nanometric scale, bring into ductile matrix, and this ductile phase is deformed, re-welded and hardened. The goal of this work was investigate the effects of highenergy milling time in the micro structural changes in the WC-Co particulate composite, particularly in the refinement of the crystallite size and lattice strain. The starting powders were WC (average particle size D50 0.87 μm) supplied by Wolfram, Berglau-u. Hutten - GMBH and Co (average particle size D50 0.93 μm) supplied by H.C.Starck. Mixing 90% WC and 10% Co in planetary ball milling at 2, 10, 20, 50, 70, 100 and 150 hours, BPR 15:1, 400 rpm. The starting powders and the milled particulate composite samples were characterized by X-ray Diffraction (XRD) and Scanning Electron Microscopy (SEM) to identify phases and morphology. The crystallite size and lattice strain were measured by Rietveld s method. This procedure allowed obtaining more precise information about the influence of each one in the microstructure. The results show that high energy milling is efficient manufacturing process of WC-Co composite, and the milling time have great influence in the microstructure of the final particles, crushing and dispersing the finely WC nanometric order in the Co particles

Anodização para obtenção de membranas cerâmicas

This a study on the achievement of alumina membranes by the method of anodizing. From this method got up a layer of aluminum oxide on the anodic metal, who presented the basic properties necessary for the application as a support for the production and acquisition of nanomaterials, such as porosity nano and resistance to high temperature, and other properties, as resistance to corrosion, and chemical, high ranking of the structure and pore size of the pores. The latter, ranging from 10 to 100nm depended on the electrolyte used, which in this study was the H2SO4. To remove all remaining aluminum, it is a bath of dissolution with HCl and CuCl where the residual aluminum has been withdrawn, and the deep pores were opened after chemical treatment with NaOH. After the dissolution, the membranes were calcined at temperatures of 300, 600 and 900° C, and sintered at temperatures of 1200 and 1300º C to win mechanical strength, porosity and observe the desired crystallization. Then went through analyses of composition through X-ray diffraction and morphology of the microstructure through a scanning electron microscope. The method was effective for obtaining alumine membranes applied in the processes of production of materials in nano

Obtenção de cerâmicas à base de tricálcio fosfatos utilizando óxido de magnésio como aditivo

The tricalcium phosphate ceramics has been widely investigated in the last years due its bioresorbable behavior. The limiting factor of the application of these materials as temporary implants is its low strength resistance. The tricalcium phosphate presents an allotropic transformation β→α around 1250 ºC that degrades its resistance. Some studies have been developed in order to densify this material at this temperature range. The objective of this work is to study the influence of the addition of magnesium oxide (MgO) in the sintering of β-TCP. The processing route was uniaxial hot pressing and its objective was to obtain dense samples. The samples were physically characterized through density and porosity measurements. The thermal behavior was studied through dilatometric, thermal differential and thermogravimetric analysis. The mechanical properties were characterized by three point flexure test and Vickers microhardness measurements, analyzed of the microstructure. The addition of magnesium oxide doesn t cause an improvement of the mechanical strength in relation to material without additive.

Obtenção de cerâmicas à base de tricálcio fosfatos utilizando óxido de manganês como aditivo

The calcium phosphate ceramics have been very investigated as material for bone implants. The tricalcium phosphate (β-TCP) had a great potential for application in temporary implants like a resorbable bioceramic. This material presents a limitation in its sintering temperature due to occurrence of the allotropic transformation β → α at temperatures around 1200°C, not allowing the attainment of dense ceramic bodies. This transformation also causes cracks, what diminishes the mechanical strength, limiting its use to applications of low mechanical requests. This work studies the influence of the addition of manganese oxide in the sintering of β-TCP. Two processing routes were investigated. The first was the powder metallurgy conventional process. The test bodies (samples) were pressed and sintering at temperatures of 1200 and 1250°C. The second route was uniaxial hot pressing and its objective was to obtain samples with high relative density. The samples were physically characterized through density and porosity measurements. The thermal behavior was studied through dilatometric, thermal differential and thermogravimetric analysis. The mechanical properties were characterized by three point flexure test and Vickers microhardness measurements. The microstructure was analyzed by scanning electron microscopy. The addition of manganese oxide caused an improvement of the mechanical strength in relation to the material without additive and promoting the stabilization of β-TCP to greater temperatures

Efeito da introdução de resíduo de cinza de forno cerâmico em massa para cerâmica estrutural

The red ceramics and structural ceramics, as they are known, include ceramic materials made by blocks of seals and structures, bricks, tiles, smail flagstones manacles, rustic floors and ornamental materials. Their fabrication uses raw material such as clay and clay sites, with some content of impurity. It has good durability and mechanical strength to compression, low cost, making it one of the mainly used materials in civil engineering. The incorporation of many industrial activities residue to ceramic products is a technological alternative for reducing the environmental impact caused by its carefree disposal. This incorporation can promote chemical change and inertness of metals from residue, by fixation in the glassy phase of ceramic during the burning stage. The main aim of this project is to study the technical feasibility of the addition of ceramic oven ash into formulations of mass for structural ceramics. In this project two kinds of clay (plastic and non-plastic) were used, as well as the ash from firewood used in the process of burning of structural ceramics. A group of experiments was outlined, which permitted the evaluation of the influence of the burning cycle in different temperatures of the ash content in formulations for ceramic blocks through technological properties, mechanical behavior and microstructure. Five samples were processed of each one of the masses of plastic and non-plastic clay without addition of ash and with addition of ash on the percentages of 10 % and 20 %, for temperatures of 850 °C, 950 °C, 1050 °C and 1150 °C, obtained through sinterization process. Among the studied compositions, the one which presented best performance was the mass of clay with 10 % of ash, at temperature of 1150 °C, with the smallest absorption of water, the smallest apparent porosity, specific apparent mass a bit over the others and greatest mechanical resistance to flexion. The composition made confirmed the technical feasibility of the use of ash in the mass for structural ceramics with maintenance of its necessary characteristics for its purposes

Caracterização de cerâmicas porosas de alumina reforçada com zircônia produzidas pelo método da réplica

Porous ceramics have many applications: thermal insulation, catalytic support, materials to fire protection, filters, and others. There are many techniques to production of ceramic filters. One technique to obtain ceramic filters is the replication method. This method consists in the impregnation of polymeric foam with ceramic slurry followed by a heating treatment that will burn out the organic elements and sintering of the material, resulting of a replication of the original foam. To perform their functions ceramic filters must satisfy mechanical requirements and permeability parameters (darcian k1 and no-darcian k2). The permeability and the strength of the ceramic material are dependent of the pore size and pore distribution. To the use at high temperatures the evaluation of mechanical properties in these temperatures is necessary. In this work the mechanical behavior of two commercial porous ceramics (10 and 40 poros per inch) was studied these materials were submitted to compression and four-point flexure test (room temperature, at 1000 °C, after thermal shock). Density and porosity measurements, permeability tests and microstructural analysis by scanning electronic microscopy (SEM) were realized. The Results showed that the decrease of mechanical strength of these materials, when submitted to thermal shock, occur for propagation of new cracks from cracks pre-existing and the permeability depends of the pore size

Obtenção de compósitos cerâmicos baseados em Al2O3/TiC através dos precursores poliméricos

The obtaining of ceramic materials from polymeric precursors is subject of numerous studies due to lower energy costs compared to conventional processing. The aim of this study is to investigate and improve the mechanism for obtaining ceramic matrix composite (CMC) based on SiOC/Al2O3/TiC by pyrolysis of polysiloxane in the presence of an active filler and inert filler in the pyrolysis temperature lower than the usually adopted for this technique, with greater strength. It also investigates the influence of pyrolysis temperature, the content of Alas active filler, the presence of infiltrating agents (Al, glass and polymer) after pyrolysis, temperature and infiltration time on some physical and mechanical properties. Alumina is used as inert filler and Al and Ti as active filler in the pyrolysis. Aluminum, glass and polysiloxane are used as agents infiltrating the post-pyrolysis. The results are analyzed with respect to porosity and bulk density by the Archimedes method, the presence of crystalline phases by X-ray diffraction (XRD) and microstructure by scanning electron microscopy (SEM). The ceramic pyrolyzed between 850 °C 1400 °C contain porosity 15% to 33%, density 2.34 g/cm3 and flexural strength at 4 points from 30 to 42 MPa. The microstructure features are porous, with an array of Al2O3 reinforced by TiC particles and AlTi3. The infiltration post-pyrolysis reveals decrease in porosity and increase density and strength. The composites have potential applications where thermal stability is the main requirement

Otimização topológica de estruturas termoelásticas tridimensionais

This work presents an optimization technique based on structural topology optimization methods, TOM, designed to solve problems of thermoelasticity 3D. The presented approach is based on the adjoint method of sensitivity analysis unified design and is intended to loosely coupled thermomechanical problems. The technique makes use of analytical expressions of sensitivities, enabling a reduction in the computational cost through the use of a coupled field adjoint equation, defined in terms the of temperature and displacement fields. The TOM used is based on the material aproach. Thus, to make the domain is composed of a continuous distribution of material, enabling the use of classical models in nonlinear programming optimization problem, the microstructure is considered as a porous medium and its constitutive equation is a function only of the homogenized relative density of the material. In this approach, the actual properties of materials with intermediate densities are penalized based on an artificial microstructure model based on the SIMP (Solid Isotropic Material with Penalty). To circumvent problems chessboard and reduce dependence on layout in relation to the final optimal initial mesh, caused by problems of numerical instability, restrictions on components of the gradient of relative densities were applied. The optimization problem is solved by applying the augmented Lagrangian method, the solution being obtained by applying the finite element method of Galerkin, the process of approximation using the finite element Tetra4. This element has the ability to interpolate both the relative density and the displacement components and temperature. As for the definition of the problem, the heat load is assumed in steady state, i.e., the effects of conduction and convection of heat does not vary with time. The mechanical load is assumed static and distributed

Método de Otimização Topológica em Estruturas Tridimensionais

The topology optimization problem characterize and determine the optimum distribution of material into the domain. In other words, after the definition of the boundary conditions in a pre-established domain, the problem is how to distribute the material to solve the minimization problem. The objective of this work is to propose a competitive formulation for optimum structural topologies determination in 3D problems and able to provide high-resolution layouts. The procedure combines the Galerkin Finite Elements Method with the optimization method, looking for the best material distribution along the fixed domain of project. The layout topology optimization method is based on the material approach, proposed by Bendsoe & Kikuchi (1988), and considers a homogenized constitutive equation that depends only on the relative density of the material. The finite element used for the approach is a four nodes tetrahedron with a selective integration scheme, which interpolate not only the components of the displacement field but also the relative density field. The proposed procedure consists in the solution of a sequence of layout optimization problems applied to compliance minimization problems and mass minimization problems under local stress constraint. The microstructure used in this procedure was the SIMP (Solid Isotropic Material with Penalty). The approach reduces considerably the computational cost, showing to be efficient and robust. The results provided a well defined structural layout, with a sharpness distribution of the material and a boundary condition definition. The layout quality was proporcional to the medium size of the element and a considerable reduction of the project variables was observed due to the tetrahedrycal element

Síntese citrato-hidrotermal e caracterização eletroquímica de LSCF para aplicação como catodo em célula a combustível de temperatura intermediária

The lanthanum strontium cobalt iron oxide (La1-xSrxCo1-yFeyO3 LSCF) is the most commonly used material for application as cathode in Solid Oxide Fuel Cells (SOFCs), mainly due to their high mixed ionic electronic conductivity between 600 and 800ºC. In this study, LSCF powders with different compositions were synthesized via a combination between citrate and hydrothermal methods. As-prepared powders were calcined from 700 to 900°C and then characterized by X-ray fluorescence, X-ray diffraction, thermal analyses, particle size analyses, nitrogen adsorption (BET) and scanning electronic microscopy. Films of composition La0,6Sr0,4Co0,2Fe0,8O3 (LSCF6428), powders calcined at 900°C, were screen-printed on gadolinium doped ceria (CGO) substrates and sintered between 1150 and 1200°C. The effects of level of sintering on the microstructure and electrochemical performance of electrodes were evaluated by scanning electronic microscopy and impedance spectroscopy. Area specific resistance (ASR) exhibited strong relation with the microstructure of the electrodes. The best electrochemical performance (0.18 ohm.cm2 at 800°C) was obtained for the cathode sintered at 1200°C for 2 h. The electrochemical activity can be further improved through surface activation by impregnation with PrOx, in this case the electrode area specific resistance decreases to values as low as 0.12 ohm.cm2 (800°C), 0.17 ohm.cm2 (750°C) and 0.31 ohm.cm2 (700°C). The results indicate that the citrate-hydrothermal method is suitable for the attainment of LSCF particulates with potential application as cathode component in intermediate temperature solid oxide fuel cells (IT-SOFCs)

Estudo do aproveitamento do rejeito da mineração de esmeraldas na produção de refratários conformados isolantes

Emerald mining is an important area of the economy in Brazil, country which is in second place among the exporting nations of this gem. Due to the process of extraction, a great amount of reject is generated. Since there is no appropriate destination, the reject is abandoned around the mining industries, contributing to environment degradation. Nowadays, some of the most relevant things to an industry in general are: energy conservation, cost reduction, quality and productivity enhancement. The production of isolating, transformed refractory materials achieves the sustainability dimension when protection of the environment is incorporated to such process. This work investigates the use of emerald mining rejects in the ceramic body of refractory materials, aiming at obtaining a product whose characteristics are compatible with commercial products and, at the same time, allow the use of such rejects to solve the environmental issue caused by its disposal in nature. X-ray fluorescence analysis show that the emerald reject obtained after the flotation to extract molybdenum and mica has 70% of silica and alumina (SiO2+Al2O3) and 21% of a basic oxides and alkaline metals and earthy alkaline mixture (Na2O, K2O, CaO e MgO). Because of the significant amount of silica and alumina present in the reject, four refractory ceramic bodies were prepared. Samples with a rectangular shape and dimensions 100x50x10 mm were pressed in a steel mold at 27,5 MPa and sintered at 1200ºC for 40 min. under environment atmosphere in a resistive oven. The sintered samples were characterized in relation to the chemical composition (FRX), mineralogical composition (DRX), microstructure (MEV) and physical and mechanical properties. The results indicate that the mixture with 45% of reject, 45% of alumina and 10% of kaolin presents a refractory quality of 1420ºC, dimensional linear variation below 2.00%, apparent specific mass of 1,56 g/cm3 and porosity of 46,68%, which demonstrates the potential use of the reject as raw material for the industry of isolating transformed refractory materials

Desenvolvimento e teste de um protótipo de reator de plasma com gaiola catódica rotatória para nitretação em lote de pequenas peças

The technique of ion nitriding, despite being fully consolidated in the industry, has great limitations when applied to the treatment of small parts. This is because effects that occur due to non-uniformity of the electric field, generate localized heating in parts, damaging the uniformity of nitrided layer. In addition, because the samples are treated static parts thereof are untreated. To expand the use of plasma nitriding, this work presents the development, assembly and testing of a prototype plasma reactor with rotatory cathodic cage [patent pending], able to meet these needs, giving the material a uniform treatment and opening doors to industrial scale production. The samples tested with hexagonal nuts are 6.0 mm in diameter, made of stainless steel AISI 304 nitrided at a pressure of 1 mbar in an atmosphere of 20% H2 + 80% N2 for 1 h. After treatment, testing visual inspection, optical microscopy and microhardness were carried out to check the effectiveness of the process for uniformity and hardness of the parts. All samples exhibited uniform color, and matte brownish, unlike the untreated samples, silver color and gloss. The hardness of the surface (top and sides) was 65% and even higher than the original hardness. The nitrided layer showed great uniformity in microstructure and thickness. It is concluded, therefore, that the unit was effective constructed for the purposes for which it was designed

Caracterização morfológica e microestrutural da perovskita BaCexPr1-xO3 sintetizada a partir do método de complexação combinando EDTA/Citrato

In this study, binary perovskite (BaCexO3) were doped with praseodymium (Pr) to obtainment of the ternary material BaCexPr1-xO3. This material was synthesized by the complexation method combining EDTA/Citrate with the stoichiometric ratio of the element Praseodymium ranging from x = 0.1 to x = 0.9 in order to determine the influence of this rare earth element on the morphology and microstructure of the final powder. At first the material was synthesized based on the route proposed by literature (Santos, 2010), and then characterized by SEM and XRD, besides being refined by the Rietveld method. In the material that had lowest residual parameter, S, and lowest average size of crystal, pH variation of synthesis solution was made in order to identify the influence of this parameter on the morphology and microscopy of the final powder. The results show that addition of praseodymium did not directly influence the crystallographic and lattice parameters, keeping even the same orthorhombic structure of the binary material BaCexO3, according to Yamanaka et al (2003). Material type BaCe0,2Pr0,8O3 had lowest residual parameter (S=1.4) and lowest average size of crystallite (26.4 nm), being used as reference in the pH variation of synthesis solution for 9, 7, 5 and 3, respectively. Variation of this parameter showed that when the synthesis solution pH was decreased to below 11, there was an increase in the average size of crystals, for pH 9, about 58.3%, for pH 7 (30.3 %), for pH 2 (2.3%) and for pH 3 (42%), indicating that the value initially used and quoted by Santos (2010) was the most coherent

Síntese e caracterização de tungstatos de cério e estrôncio para fins catalíticos

The main goal of this work was to produce nanosized ceramic materials of the family of the tungstates (tungstates of cerium and strontium), and test them for their catalytic activity in processes involving the transformation of methane (CH4). The methodology used for the synthesis of the ceramic powders involved the complexation combining EDTA-citrate. The materials characterization was performed using simple and differential thermogravimetry, x-ray diffraction, transmission electron microscopy, and energy dispersive spectroscopy (EDS). The microstructure analysis was performed using the refinement by the Rietveld method, and the crystallite size and distribution of the materials was elucidate by the Scherrer and Williamson-Hall methods. The conditions of the synthesis process for the three envisaged materials (SrWO4, SrWO4 using tungsten oxide concentrate as raw material, and Ce2(WO4)3) were adjusted to obtain a single phase crystalline material. The catalytic tests were carried out in the presence of methane and synthetic air, which is composed of 21% O2 and 79% N2. The analysis of the conversion of the reaction was done with the aid of an fourier transform infrared device (FTIR). The analysis showed that, structurally, the SrWO4 produced using raw materials of high and poor purity (99% and 92%, respectively) are similar. The ideal parameters of calcination, in the tested range, are temperature of 1000 °C and time of calcination 5 hours. For the Ce2(WO4)3, the ideal calcination time and are temperature 15 hours and 1000°C, respectively. The Williamson-Hall method provided two different distributions for the crystallite size of each material, whose values ranged between the nanometer and micrometer scales. According to method of Scherrer, all materials produced were composed of nanometric crystallites. The analyses of transmission electron microscopy confirmed the results obtained from the Williamson- Hall method for the crystallite size. The EDS showed an atomic composition for the metals in the SrWO4 that was different of the theoretical composition. With respect to the catalytic tests, all materials were found to be catalytically active, but the reaction process should be further studied and optimized.

Em cantos de reis: a tradição discursiva em Autos de Natal

This study incorporates many areas of knowledge to the Linguistics field, as it centers the social historicity of Brazilian and autos potiguares on two analytical proposes: the presence of linguistic formulas - in its macrostructure - into the paradigm of discursive traditions, following Kabatek (2006), Koch and Oesterreicher (2007), besides the theory of Speech Acts, in its microstructure, proposed by Austin (1990) and Searle (1995). Under Zumthor (1993; 1997; 2000; 2005; 2010), the idea of textual variability (mouvance) was alluded, highlighting that the text is always modifying, according to the performance and reception of the language uses. Considering this theoretical framework, we focus on the trinomial linguistic formulas, orality and performance, in order to describe the dynamics of stability, variation and change, emphasizing yet how extra-linguistic social-historic cultural relations influence its composition. Such discuss is inherent more precisely to Textual Analysis in enhancing the orality tradition as a linguistic support. The text, in its turn, becomes effective as an evocation, motivated by the transmission, reception and variability from its conservation and reiteration. Naturally, a methodological support based on quali-quantitative research was chosen, based on Flick (2009), who justifies the corpus composed by Brazilian Folias de Reis chants and Bois de Reis potiguares . Thereby Language dynamics, subjacent to tradition which takes effect by the use of a common social memory, are observed from two dimensions: on the first, it evocates the sacralization (religious) in which they stand their devotion to biblical History; secondly, a dissacralization with identified and ideological values, inherent to a people culture. The chant shows, in this ludic impulse, a contextualized activity which results in the following conclusion: the changing and stability processes in textual macro and microstructures occur, at the same time, by the adjustment to the use of the text accomplishing a social-political function and an ethical-pedagogic one; supposedly, social relationships arise the tradition and it, on its turn, evocates the variability and the nomadism in the text