Caracterização de atapulgita visando aplicação para reforço de materiais poloméricos

The clay mineral attapulgite is a group of hormitas, which has its structures formed by microchannels, which give superior technological properties classified the industrial clays, clays of this group has a very versatile range of applications, ranging from the drilling fluid for wells oil has applications in the pharmaceutical industry. Such properties can be improved by activating acid and / or thermal activation. The attapulgite when activated can improve by up to 5-8 times some of its properties. The clay was characterized by X-ray diffraction, fluorescence, thermogravimetric analysis, differential thermal analysis, scanning electron microscopy and transmission electron microscopy before and after chemical activation. It can be seen through the results the efficiency of chemical treatment, which modified the clay without damaging its structure, as well as production of polymer matrix composites with particles dispersed atapugita

Influência dos parâmetros de processo na deposição de nitreto de titânio por plasma em gaiola catódica

Titanium nitride films were grown on glass using the Cathodic Cage Plasma Deposition technique in order to verify the influence of process parameters in optical and structural properties of the films. The plasma atmosphere used was a mixture of Ar, N2 and H2, setting the Ar and N2 gas flows at 4 and 3 sccm, respectively and H2 gas flow varied from 0, 1 to 2 sccm. The deposition process was monitored by Optical Emission Spectroscopy (OES) to investigate the influence of the active species in plasma. It was observed that increasing the H2 gas flow into the plasma the luminescent intensities associated to the species changed. In this case, the luminescence of N2 (391,4nm) species was not proportional to the increasing of the H2 gas into the reactor. Other parameters investigated were diameter and number of holes in the cage. The analysis by Grazing Incidence X-Ray Diffraction (GIXRD) confirmed that the obtained films are composed by TiN and they may have variations in the nitrogen amount into the crystal and in the crystallite size. The optical microscopy images provided information about the homogeneity of the films. The atomic force microscopy (AFM) results revealed some microstructural characteristics and surface roughness. The thickness was measured by ellipsometry. The optical properties such as transmittance and reflectance (they were measured by spectrophotometry) are very sensitive to changes in the crystal lattice of the material, chemical composition and film thicknesses. Therefore, such properties are appropriate tools for verification of this process control. In general, films obtained at 0 sccm of H2 gas flow present a higher transmittance. It can be attributed to the smaller crystalline size due to a higher amount of nitrogen in the TiN lattice. The films obtained at 1 and 2 sccm of H2 gas flow have a golden appearance and XRD pattern showed peaks characteristics of TiN with higher intensity and smaller FWHM (Full Width at Half Maximum) parameter. It suggests that the hydrogen presence in the plasma makes the films more stoichiometric and becomes it more crystalline. It was observed that with higher number of holes in the lid of the cage, close to the region between the lid and the sample and the smaller diameter of the hole, the deposited film is thicker, which is justified by the most probability of plasma species reach effectively the sample and it promotes the growth of the film

Obtenção e caracterização de dióxido de estanho nanoestruturado pelo método de síntese contínua por combustão em solução

Continuous Synthesis by Solution Combustion was employed in this work aiming to obtain tin dioxide nanostructured. Basically, a precursor solution is prepared and then be atomized and sprayed into the flame, where its combustion occurs, leading to the formation of particles. This is a recent technique that shows an enormous potential in oxides deposition, mainly by the low cost of equipment and precursors employed. The tin dioxide (SnO2) nanostructured has been widely used in various applications, especially as gas sensors and varistors. In the case of sensors based on semiconducting ceramics, where surface reactions are responsible for the detection of gases, the importance of surface area and particle size is even greater. The preference for a nanostructured material is based on its significant increase in surface area compared to conventional microcrystalline powders and small particle size, which may benefit certain properties such as high electrical conductivity, high thermal stability, mechanical and chemical. In this work, were employed as precursor solution tin chloride dehydrate diluted in anhydrous ethyl alcohol. Were utilized molar ratio chloride/solvent of 0,75 with the purpose of investigate its influence in the microstructure of produced powder. The solution precursor flux was 3 mL/min. Analysis with X-ray diffraction appointed that a solution precursor with molar ratio chloride/solvent of 0,75 leads to crystalline powder with single phase and all peaks are attributed to phase SnO2. Parameters as distance from the flame with atomizer distance from the capture system with the pilot, molar ratio and solution flux doesn t affect the presence of tin dioxide in the produced powder. In the characterization of the obtained powder techniques were used as thermogravimetric (TGA) and thermodiferential analysis (DTA), particle size by laser diffraction (GDL), crystallographic analysis by X-ray diffraction (XRD), morphology by scanning electron microscopy (SEM), transmission electron microscopy (TEM), specific surface area (BET) and electrical conductivity analysis. The techniques used revealed that the SnO2 exhibits behavior of a semiconductor material, and a potentially promising material for application as varistor and sensor systems for gas

Síntese de pigmentos cerâmicos inorgânicos nanométricos e encapsulados com estrutura core-shell pela rota dos precursores poliméricos

The present work has as objective the development of ceramic pigments based in iron oxides and cobalt through the polymeric precursor method, as well as study their characteristics and properties using methods of physical, chemical, morphological and optical characterizations.In this work was used iron nitrate, and cobalt citrate as precursor and nanometer silica as a matrix. The synthesis was based on dissolving the citric acid as complexing agent, addition of metal oxides, such as chromophores ions and polymerization with ethylene glycol. The powder obtained has undergone pre-ignition, breakdown and thermal treatments at different calcination temperatures (700 °C, 800 °C, 900 °C, 1000 °C and 1100 °C). Thermogravimetric analyzes were performed (BT) and Differential Thermal Analysis (DTA), in order to evaluate the term decomposition of samples, beyond characterization by techniques such as BET, which classified as microporous materials samples calcined at 700 ° C, 800 º C and 900 º C and non-porous when annealed at 1000 ° C and 1100 º C, X-ray diffraction (XRD), which identified the formation of two crystalline phases, the Cobalt Ferrite (CoFe2O4) and Cristobalite (SiO2), Scanning Electron Microscopy (SEM) revealed the formation of agglomerates of particles slightly rounded;and Analysis of Colorimetry, temperature of 700 °C, 800 °C and 900 °C showed a brown color and 1000 °C and 1100 °C violet

Estudo da sinterabilidade de ligas de níquel obtidas por meio dos portadores de liga sic, si3n4 ou si metálico com grafita

Nickel alloys are frequently used in applications that require resistance at high temperatures associated with resistance to corrosion. Alloys of Ni-Si-C can be obtained by means of powder metallurgy in which powder mixtures are made of metallic nickel powders with additions of various alloying carriers for such were used in this study SiC, Si3N4 or Si metal with graphite. Carbonyl Ni powder with mean particle size of 11 mM were mixed with 3 wt% of SiC powders with an average particle size of 15, 30 and 50 μm and further samples were obtained containing 4 to 5% by mass of SiC with average particle size of 15 μm. Samples were also obtained by varying the carrier alloy, these being Si3N4 powder with graphite, with average particle size of 1.5 and 5 μm, respectively. As a metallic Si graphite with average particle size of 12.5 and 5 μm, respectively. The reference material used was nickel carbonyl sintered without adding carriers. Microstructural characterization of the alloys was made by optical microscopy and scanning electron microscopy with semi-quantitative chemical analysis. We determined the densities of the samples and measurement of microhardness. We studied the dissociation of carriers alloy after sintering at 1200 ° C for 60 minutes. Was evaluated also in the same sintering conditions, the influence of the variation of average particle size of the SiC carrier to the proportion of 3% by mass. Finally, we studied the influence of variation of the temperatures of sintering at 950, 1080 and 1200 ° C without landing and also with heights of 30, 60, 120 and 240 minutes for sintering where the temperature was 950 °C. Dilatometry curves showed that the SiC sintered Ni favors more effectively than other carriers alloy analyzed. SiC with average particle size of 15 μm active sintering the alloy more effectively than other SiC used. However, with the chemical and morphological analyzes for all leagues, it was observed that there was dissociation of SiC and Si3N4, as well as diffusion of Si in Ni matrix and carbon cluster and dispersed in the matrix, which also occurred for the alloys with Si carriers and metallic graphite. So the league that was presented better results containing Si Ni with graphite metallic alloy as carriers, since this had dispersed graphite best in the league, reaching the microstructural model proposed, which is necessary for material characteristic of solid lubricant, so how we got the best results when the density and hardness of the alloy

Síntese e caracterização de cerâmicas nanométricas para produção de gás de síntese

In this work, ceramic powders belonging to the system Nd2-xSrxNiO4 (x = 0, 0.4, 0.8, 1.2 and 1.6) were synthesized for their use as catalysts to syngas production partial. It was used a synthesis route, relatively new, which makes use of gelatin as organic precursor. The powders were analyzed at several temperatures in order to obtain the perovskite phase and characterized by several techniques such as thermal analysis, X-rays diffraction, Rietveld refinement method, specific surface area, scanning electron microscopy, energy dispersive spectroscopy of X-rays and temperature programmed reduction. The results obtained using these techniques confirmed the feasibility of the synthesis method employed to obtain nanosized particles. The powders were tested in differential catalytic conditions for dry reforming of methane (DRM) and partial oxidation of methane (POM), then, some systems were chosen for catalytic integrals test for (POM) indicating that the system Nd2-xSrxNiO4 for x = 0, 0.4 and 1.2 calcined at 900 °C exhibit catalytic activity on the investigated experimental conditions in this work without showing signs of deactivation

Revestimentos a base de Ta/Al2O3 produzidos por aspersão térmica sobre substrato metálico

Metal substrates were coated by thermal spraying plasma torch, they were positioned at a distance of 4 and 5 cm from the nozzle exit of the plasma jet. The starting materials were used for deposition of tantalum oxide powder and aluminium. These two materials were mixed and ground into high-energy mill, then immersed in the torch for the production of alumina coating infused with particles of tantalum with nano and micrometric size. The spraying equipment used is a plasma torch arc not transferred, which operating in the range of 250 A and 80 V, was able to produce enough heat to ignite aluminothermic between Ta2O5 and aluminum. Upon reaching the plasma jet, the mixing powders react with the heat of the blaze, which provides sufficient energy for melting aluminum particles. This energy is transferred through mechanisms of self-propagating to the oxide, beginning a reduction reaction, which then hits on the surface of the substrate and forms a coating on which a composite is formed by a junction metal - ceramic (Ta +Al2O3). The phases and quantification of each were obtained respectively by X-ray diffraction and the Rietveld method. Morphology by scanning electron microscopy and chemical analysis by energy dispersive spectroscopy EDS. It was also performed measurements of the substrate roughness, Vickers microhardness measurements in sprays and determination of the electron temperature of the plasma jet by optical emission spectroscopy EEO. The results confirmed the expectation generated around the end product of spraying the mixture Ta2O5 + Al, both in the formation of nano-sized particles and in their final form. The electron excitation temperature was consistent with the purpose of work, in addition, the thermodynamic temperature was efficient for the reduction process of Ta2O5. The electron excitation temperature showed values of 3000, 4500 and 8000 K for flows10, 20 and 30 l / min respectively, these values were taken at the nozzle exit of the plasma jet. The thermodynamic temperature around 1200 ° C, was effective in the reduction process of Ta2O5

Utilização de nanosílica como aditivo estendedor para pastas cimentantes de baixa densidade destinadas à cimentação de poços petrolíferos

Cementing operations are conducted at different times of the well s life and they have high importance, because the functions are fundamental to keep good properties during a long life of the well, such as, maintain the mechanical stability of the well, to promote the isolation hydraulic and support the tubing. In some situations, the rocky zones have low fractures pressures and require the use of lightweight slurries to prevent the hydrostatic pressure in the formation is greater than the pressure of fracture. There are three ways to reduce the density of cement slurries: exterders water additives, microspheres and foamed slurries. The most used extender water additive is sodium bentonite, which is a clay with a good capacity of water absorption and expansion of its volume, the main disadvantage of this additive is the reduction of the strength. Currently, the use of nanoscale particles has received special attention, mainly because they get new functionalities. Following this trend, this paper aims to use a colloidal solution of nano-silica as an exterders water additives for use in oil wells. Slurries were designed with fixed 13lb/gal density and concentration of nano silica 0.1 gpc; 0.4 gpc; 0.7 and 1gpc, the influence of nano-silica was studied at these levels in isolation and combined varying concentrations of CaCl2,. Tests including rheology, stability, strength, thickening time, porosity and permeability. Besides the API tests, microstructural characterizations were performed after 28 days of the slurries, X-ray diffraction (XRD) and scanning electron microscopy (SEM)

Estudo sobre a redução aluminotérmica de Ta2O5 e TiO2 usando descarga de cátodo oco

In this study it was used two metallic oxides, Ta2O5 and TiO2, in order to obtain metallic powders of Ta and Ti through aluminothermic reduction ignited by plasma. Ta2O5 and TiO2 powders were mixed with Al in a planetary mill, using different milling times. A thermal analysis study (DTA and TG) was carried out, in order to know the temperature to react both the mixtures. Then, these mixtures were submitted to a hollow cathode discharge, where they were reacted using aluminothermic reduction ignited by plasma. The product obtained was characterized by XRD and SEM, where it was proven the possibility of producing these metallic particles, different from the conventional process, where metallic ingots are obtained. It was verified that the aluminothermic reduction ignited by plasma is able to produce metallic powders of Ta and Ti, and a higher efficiency was observed to the process with Ta2O5-Al mixtures. Among different microstructural aspects observed, it can be noted the presence of metallic nanoparticles trapped into an Al2O3 matrix, besides acicular structures (titanium) and dendritic structures (tantalum), which are a product characteristic from a fast cooling

Processamento e caracterização de compósitos Poli(METACRILATO DE METILA)/Sílica (PMMA/SiO2)

Currently the search for new materials with properties suitable for specific applications has increased the number of researches that aim to address market needs. The poly (methyl methacrylate) (PMMA) is one of the most important polymers of the family of polyacrylates and polymethacrylates, especially for its unique optical properties and weathering resistance, and exceptional hardness and gloss. The development of polymer composites by the addition of inorganic fillers to the PMMA matrix increases the potential use of this polymer in various fields of application. The most commonly used inorganic fillers are particles of silica (SiO2), modified clays, graphite and carbon nanotubes. The main objective of this work is the development of PMMA/SiO2 composites at different concentrations of SiO2, for new applications as engineering plastics. The composites were produced by extrusion of tubular film, and obtained via solution for application to commercial PMMA plates, and also by injection molding, for improved the abrasion and scratch resistance of PMMA without compromising transparency. The effects of the addition of silica particles in the polymer matrix properties were evaluated by the maximum tensile strength, hardness, abrasion and scratch resistance, in addition to preliminary characterization by torque rheometry and melt flow rate. The results indicated that it is possible to use silica particles in a PMMA matrix, and a higher silica concentration produced an increase of the abrasion and scratch resistance, hardness, and reduced tensile strength

Simulação computacional de medidas estereológicas em estruturas de metal duro (WC-Co)

This work focuses on the creation and applications of a dynamic simulation software in order to study the hard metal structure (WC-Co). The technological ground used to increase the GPU hardware capacity was Geforce 9600 GT along with the PhysX chip created to make games more realistic. The software simulates the three-dimensional carbide structure to the shape of a cubic box where tungsten carbide (WC) are modeled as triangular prisms and truncated triangular prisms. The program was proven effective regarding checking testes, ranging from calculations of parameter measures such as the capacity to increase the number of particles simulated dynamically. It was possible to make an investigation of both the mean parameters and distributions stereological parameters used to characterize the carbide structure through cutting plans. Grounded on the cutting plans concerning the analyzed structures, we have investigated the linear intercepts, the intercepts to the area, and the perimeter section of the intercepted grains as well as the binder phase to the structure by calculating the mean value and distribution of the free path. As literature shows almost consensually that the distribution of the linear intercepts is lognormal, this suggests that the grain distribution is also lognormal. Thus, a routine was developed regarding the program which made possible a more detailed research on this issue. We have observed that it is possible, under certain values for the parameters which define the shape and size of the Prismatic grain to find out the distribution to the linear intercepts that approach the lognormal shape. Regarding a number of developed simulations, we have observed that the distribution curves of the linear and area intercepts as well as the perimeter section are consistent with studies on static computer simulation to these parameters.

Estudo de massa cerâmica triaxial visando à otimização do ciclo de queima da indústria de cerâmica estrutural

Over recent years the structural ceramics industry in Brazil has found a very favorable market for growth. However, difficulties related to productivity and product quality are partially inhibiting this possible growth. An alternative for trying to solve these problems and, thus, provide the pottery industry the feasibility of full development, is the substitution of firewood used in the burning process by natural gas. In order to contribute to this process of technological innovation, this paper studies the effect of co-use of ceramic phyllite and kaolin waste on the properties of a clay matrix, verifying the possible benefits that these raw materials can give to the final product, as well as the possibility of such materials to reduce the heat load necessary to obtain products with equal or superior quality. The study was divided into two steps: characterization of materials and study of formulations. Two clays, a phyllite and a residue of kaolin were characterized by the following techniques: laser granulometry, plasticity index by Atterberg limits, X-ray fluorescence, X-ray diffraction, mineralogical composition by Rietveld, thermogravimetric and differential thermal analysis. To study the formulations, specifically for evaluation of technological properties of the parts, was performed an experimental model that combined planning involving a mixture of three components (standard mass x phyllite x kaolin waste) and a 23 factorial design with central point associated with thermal processing parameters. The experiment was performed with restricted strip-plot randomization. In total, 13 compositional points were investigated within the following constraints: phyllite ≤ 20% by weight, kaolin waste ≤ 40% by weight, and standard mass ≥ 60% by weight. The thermal parameters were used at the following levels: 750 and 950 °C to the firing temperature, 5 and 15 °C/min at the heating rate, 15 and 45min to the baseline. The results showed that the introduction of phyllite and/or kaolin waste in ceramic body produced a number of benefits in properties of the final product, such as: decreased absorption of water, apparent porosity and linear retraction at burn; besides the increase in apparent specific mass and mechanical properties of parts. The best results were obtained in the compositional points where the sum of the levels of kaolin waste and phyllite was maximal (40% by weight), as well as conditions which were used in firing temperatures of 950 °C. Regarding the prospect of savings in heat energy required to form the desired microstructure, the phyllite and the residue of kaolin, for having small particle sizes and constitutions mineralogical phases with the presence of fluxes, contributed to the optimization of the firing cycle.

Comportamento magnético de compósitos de matriz polimérica com adição de ferritas

Polymer matrix composites offer advantages for many applications due their combination of properties, which includes low density, high specific strength and modulus of elasticity and corrosion resistance. However, the application of non-destructive techniques using magnetic sensors for the evaluation these materials is not possible since the materials are non-magnetizable. Ferrites are materials with excellent magnetic properties, chemical stability and corrosion resistance. Due to these properties, these materials are promising for the development of polymer composites with magnetic properties. In this work, glass fiber / epoxy circular plates were produced with 10 wt% of cobalt or barium ferrite particles. The cobalt ferrite was synthesized by the Pechini method. The commercial barium ferrite was subjected to a milling process to study the effect of particle size on the magnetic properties of the material. The characterization of the ferrites was carried out by x-ray diffraction (XRD), field emission gun scanning electron microscopy (FEG-SEM) and vibrating sample magnetometry (VSM). Circular notches of 1, 5 and 10 mm diameter were introduced in the composite plates using a drill bit for the non-destructive evaluation by the technique of magnetic flux leakage (MFL). The results indicated that the magnetic signals measured in plates with barium ferrite without milling and cobalt ferrite showed good correlation with the presence of notches. The milling process for 12 h and 20 h did not contribute to improve the identification of smaller size notches (1 mm). However, the smaller particle size produced smoother magnetic curves, with fewer discontinuities and improved signal-to-noise ratio. In summary, the results suggest that the proposed approach has great potential for the detection of damage in polymer composites structures

Comportamento reológico de materiais cimentícios para poços de petróleo contendo naftaleno condensado ou policarboxilato

Pastas a base de cimento Portland são utilizadas na cimentação de poços de petróleo. Elas consistem de uma mistura de partículas sólidas de cimento dispersas em água e aditivos. Atualmente, diversos materiais alternativos são utilizados como aditivos, objetivando a modificação e a melhoria das propriedades das pastas de cimento, especialmente no aumento da fluidez. Novos aditivos plastificantes são capazes de suportar as diversas condições de poços, promovendo propriedades no estado fluido compatíveis às condições exigidas para cimentação.Dispersantes são os componentes da pasta que garantem fluidez, além de proporcionar controle na água perdida por filtração na formação porosa, garantindo o sucesso da operação de bombeio. Em deter minados campos, além do efeito da profundidade, as condições geológicas das formações promovemvariações do gradiente de pressão e temperatura ao longo da profundidade vertical do poço. Recentemente, diversos aditivos químicos da indústria da construção civil tem sido estudados em condições de cimentação de poços de petróleo. Vários produtos testados tem apresentado desempenho superior aos produtos normalmente empregados pela indústria de petróleo com boa relação custo/benefício em função do volume de mercado da construção civil. Resultados promissores na seleção de aditivos com função dispersante da construção civil para operações de cimentação de poços de petróleo onshore foram obtidos para temperaturas até 80°C. O potencial de uso desses aditivos permite estabelecer novas soluções para problemas encontrados na cimentação de poços de petróleo HPHT, poços sujeitos à injeção de vapor, poços depletados e poços produtores de gás. Na construção civil, os superplastificantes permitem reduzir o fator água/cimento das argamassas proporcionando melhoria de propriedades como resistência mecânica e fluidez. Assim, o objetivo deste trabalho foi o estudo e a caracterização reológica de pastas constituídas de cimento Portland, água e aditivos do tipo plastificante, com função dispersante a base de naftaleno condensado e policarboxilato, na faixa de temperaturas de 58°C e 70ºC. As condições utilizadas para a avaliação dos aditivos alternativos foram baseadas em uma cimentação primária para um poço hipotético de 2200 m de profundidade e gradientes geotérmicos de 1,7°F/100 pés e 2,1°F/100 pés. Os resultados demonstraram a grande eficiência e o poder dispersivo do policarboxilato para as temperaturas estudadas. O aditivo promoveu alta fluidez, sem efeitos de sedimentação da pasta. O dispersante à base de naftaleno reduziutant o a viscosidade plástica como o limite de escoamento acimada concentração a partir de 0,13%. O modelo de Bingham descreveu bem o comportamento reológico das pastas com policarboxilato para todas as concentrações

Comportamento da adição do carbeto de nióbio (nBC) na matriz metálica do aço ferrítico 15kH2mfa

The 15Kh2MFA steel is a kind of Cr-Mo-V family steels and can be used in turbines for energy generation, pressure vessels, nuclear reactors or applications where the range of temperature that the material works is between 250 to 450°C. To improve the properties of these steels increasing the service temperature and the thermal stability is add a second particle phase. These particles can be oxides, carbides, nitrites or even solid solution of some chemical elements. On this way, this work aim to study the effect of addition of 3wt% of niobium carbide in the metallic matrix of 15Kh2MFA steel. Powder metallurgy was the route employed to produce this metallic matrix composite. Two different milling conditions were performed. Condition 1: milling of pure 15Kh2MFA steel and condition 2: milling of 15Kh2MFA steel with addition of niobium carbide. A high energy milling was carried out during 5 hours. Then, these two powders were sintered in a vacuum furnace (10-4torr) at 1150 and 1250°C during 60 minutes. After sintering the samples were normalized at 950°C per 3 minutes followed by air cooling to obtain a desired microstructure. Results show that the addition of niobium carbide helps to mill faster the particles during the milling when compared with that steel without carbide. At the sintering, the niobium carbide helps to sinter increasing the density of the samples reaching a maximum density of 7.86g/cm³, better than the melted steel as received that was 7,81g/cm³. In spite this good densification, after normalizing, the niobium carbide don t contributed to increase the microhardness. The best microhardness obtained to the steel with niobium carbide was 156HV and to pure 15Kh2MFA steel was 212HV. It happened due when the niobium carbide is added to the steel a pearlitic structure was formed, and the steel without niobium carbide submitted to the same conditions reached a bainitic structure