Obtenção de nanopartículas de hexaferrita de bário pelo método pechini

In this study barium hexaferrite was (general formulae BaFe12O19) was synthesized by the Pechini method under different conditions of heat treatment. Precursors like barium carbonate and iron nitrate were used. These magnetic ceramic, with magnetoplumbite type structure, are widely used as permanent magnet because of its excellent magnetic properties, such as: high Curie temperature, good magnetic anisotropy, high coercivity and corrosion resistance. The samples were characterized by thermal analysis (DTA and TG), X- ray Diffraction (XRD), Fourier transform infrared spectroscopy (FTIR), Scanning Electron Microscopy (SEM) end Vibrating sample Magnetometer (VSM). The results confirm the expected phase, which was reinforced according to our analysis. A single phase powder at relatively high temperatures with particle sizes around 100 nm was obtained. The characteristic magnetic behavior one of the phases has been noted (probably superparamagnetic material), while another phase was identified as a ferrimagnetic material. The ferrimagnetic phase showed vortex configuration with two central and slightly inclined plateaus. In general, increase of heat treatment temperature and time, directly influenced the technological properties of the samples

Desenvolvimento de bloco de vedação com barita na composição de partida para blindagem de radiação X

This work main objective is to study the use of bricks in barium X-rays rooms in order to contribute to the optimization of shielding rooms diagnosis. The work was based on experimental measurements of X-ray attenuation (40 to 150 kV), using ceramic seal bearing the incorporation of barium sulfat (BaSO4). Different formulations were studied in three different firing temperatures and evaluated for incorporation in the ceramic body. The composition of 20% of barite processed at a temperature of 950 ° C showed better physical and mechanical properties, is considered the most suitable for the purpose of this work. Were produced bricks sealing composition formulated based on that presented the best technological features. These blocks were tested physically as a building material and wall protective barrier. Properties such as visual, deviation from the square, face flatness, water absorption and compressive strength were evaluated for all the blocks produced. The behavior of this material as attenuator for X-rays was investigated by experimental results which take into account mortar manufacturers barium through the different strains and compared with the reference material (Pb). The simulation results indicated that the ceramic block barium shows excellent properties of attenuation equivalence lead taking into account the energy used in diagnostic X-ray

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

Extração de metais (K, Mg, Ba, Ca, Cr, Mn, Li, Fe) de água produzida utilizando sistema microemulsionado

The produced water is a byproduct formed due to production of petroleum and carries with it a high amount of contaminants such as oil particles in suspension, organic compounds and metals. Thus, these latter pollutants are very difficult to treat because of its high solubility in water. The objective of this work is to use and evaluate a microemulsioned system to remove metals ( K , Mg , Ba , Ca , Cr , Mn , Li , Fe ) of synthetic produced water. For the extraction of metals, it was used a pseudoternary diagram containing the following phases: synthetic produced water as the aqueous phase (AP), hexane as organic phase (OP), and a cosurfactant/surfactant ratio equal to four (C/S = 4) as the third phase, where the OCS (saponified coconut oil) was used as surfactant and n-butanol as cosurfactant. The synthetic produced water was prepared in a bench scale and the region of interest in the diagram for the removal of metals was determined by experimental design called. Ten points located in the phase Winsor II were selected in an area with a large amount of water and small amounts of reagents. The samples were analyzed in atomic absorption spectrometer, and the results were evaluated through a statistical assesment, allowing the efficiency analysis of the effects and their interactions. The results showed percentages of extraction above 90% for the metals manganese, iron, chromium, calcium, barium and magnesium, and around 45% for metals lithium and potassium. The optimal point for the simultaneous removal of metals was calculated using statistical artifact multiple response function (MR). This calculation showed that the point of greatest extraction of metals occurs was the J point, with the composition [72% AP, 9% OP, 19% C/S], obtaining a global extraction percentage about 80%. Considering the aspects analyzed, the microemulsioned system has shown itself to be an effective alternative in the extraction of metals on synthetic produced water remediation

Estudo do efeito do óxido de bário no comportamento de massas para porcelanato

In this work, it is proposed the study of the effect of barium oxide acting as synthetic flow in the behavior of masses for stoneware from the use of raw materials found in the deposits of minerals of the Rio Grande do Norte that it makes use of a great natural potential for the industrialization of the product. The porcelanato is a sophisticated product with excellent final properties being applied as ceramic coating in buildings of high standard of engineering. The raw materials selected for the development of the study had been two types of argilas, two types of feldspatos, dolomita, talco, barium carbonate and silica, being characterized by X-ray fluorescence, X-ray diffraction, granulometric analysis, dilatometric analysis and thermal analysis. Thus, it is intended to define four formulations using the cited raw materials that will be processed, conformed and sintered in the temperatures of 1150 °C, 1175 °C, 1200 °C, 1225 °C e 1250 °C. From the physical characterizations, chemical and morphologic of the formed formulations, the effect of barium oxide is determined in the physical and mechanical properties of the studied system carrying water absorption tests, linear retraction, apparent porosity, apparent specific mass, compacting curve, flexural strength and microstructural analysis by XRD and SEM. After analyzing the results, indicated that barium oxide acts as a flux of high temperature and as the ordering of structure, where the embedded glass phase has the nucleating effect phase potassium silico-aluminum reacting with free silica which together with the high content of potassium concentrated form a new crystalline phase called microcline. The masses studied with the addition of barium oxide present physical-mechanical properties highly satisfactory in reduced firing temperatures, which implies a saving in energy given off in the production and increased productivity

Remoção conjugada de metais e óleo de água produzida

Petroleum can be associated or not with natural gas, but in both cases water is always present in its formation. The presence of water causes several problems, such as the difficulty of removing the petroleum from the reservoir rock and the formation of waterin-oil and oil-in-water emulsions. The produced water causes environmental problems, which should be solved to reduce the effect of petroleum industry in the environment. The main objective of this work is to remove simultaneously from the produced water the dispersed petroleum and dissolved metals. The process is made possible through the use of anionic surfactants that with its hydrophilic heads interacts with ionized metals and with its lipophilic tails interacts with the oil. The studied metals were: calcium, magnesium, barium, and cadmium. The surfactants used in this research were derived from: soy oil, sunflower oil, coconut oil, and a soap obtained from a mixture of 5wt.% coconut oil and 95wt.% animal fat. It was used a sample of produced water from Terminal de São Sebastião, São Paulo. As the concentration of the studied metals in produced water presented values close to 300 mg/L, it was decided to use this concentration as reference for the development of this research. Molecular absorption and atomic absorption spectroscopy were used to determine petroleum and metals concentrations in the water sample, respectively. A constant pressure filtration system was used to promote the separation of solid and liquid phases. To represent the behavior of the studied systems it was developed an equilibrium model and a mathematical one. The obtained results showed that all used surfactants presented similar behavior with relation to metals extraction, being selected the surfactant derived from soy oil for this purpose. The values of the partition coefficients between the solid and liquid phases " D " for the studied metals varied from 0.2 to 1.1, while the coefficients for equilibrium model " K " varied from 0.0002 and 0.0009. The removal percentile for oil with all metals associated was near 100%, showing the efficiency of the process

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

Tratamento de água de produção de petróleo visando o aproveitamento na obtenção de barrilha

The petroleum production is associated to the produced water, which has dispersed and dissolved materials that damage not only the environment, but also the petroleum processing units. This study aims at the treatment of produced water focusing mainly on the removal of metals and oil and using this treated water as raw material for the production of sodium carbonate. Initially, it was addressed the removal of the following divalent metals: calcium, magnesium, barium, zinc, copper, iron, and cadmium. For this purpose, surfactants derived from vegetable oils, such as coconut oil, soybean oil, and sunflower oil, were used. The investigation showed that there is a stoichiometric relationship between the metals removed from the produced water and the surfactants used in the process of metals removal. It was also developed a model that correlates the hydrolysis constant of saponified coconut oil with the metal distribution between the resulting stages of the proposed process, flocs and aqueous phases, and relating the results with the pH of the medium. The correlation coefficient obtained was 0.963. Next, the process of producing washing soda (prefiro soda ahs ou sodium carbonate) started. The resulting water from the various treatment approaches from petroleum production water was used. During this stage of the research, it was observed that the surfactant assisted in the produced water treatment, by removing some metals and the dispersed oil entirety. The yield of sodium carbonate production was approximately 80%, and its purity was around 95%. It was also assessed, in the production of sodium carbonate, the influence of the type of reactor, using a continuous reactor and a batch reactor. These tests showed that the process with continuous reactor was not as efficient as the batch process. In general, it can be concluded that the production of sodium carbonate from water of oil production is a feasible process, rendering an effluent that causes a great environmental impact a raw material with large scale industrial use

Caracterização estrutural de Perovskitas Lax-1AxCoO3 (x=0 e 0,2) ,dopadas com cálcio e bario, por espectroscopia de absorção de raios X (XAS).

In this work, the structures of LaCoO3, La0,8Ba0,2CoO3 and La0,8Ca0,2CoO3 perovskites were characterized as a function of temperature (LaCoO3 structure being analyzed only at room temperature). The characterization of these materials were made by X-Ray Absorption Spectroscopy (XAS), in the cobalt K-edge, taking into account the correlated Einstein model X-ray absorption fine structure (EXAFS). The first part of the absorption spectrum corresponded the X-ray absorption near edge structure (XANES) and extended X-ray absorption fine structure (EXAFS). These materials were prepared by the combustion method. The combustion products were calcinated at 900 0C, for 6 hours in air. Noted that the sample LaCoO3 at room temperature and samples doped with Calcium and Barium in the temperature range of 50 K to 298 K showed greater distortion to monoclinic symmetry with space group I2/a. However, the sample doped with barium at the temperatures 50 K, 220 K, and 260 K showed a slight distortion to rhombohedral symmetry with space group R-3c. The La0,8Ca0, 2CoO3 structure was few sensitive to temperature variation, showing a higher local distortion in the octahedron and a higher local thermal disorder. These interpretations were in agreement with the information electronic structural on the XANES region and geometric in the EXAFS region

Variação espacial e sazonal de elementos maiores e traços no estuários do Rio Curimataú (RN), através de dados geoquímicos e de sensoriamento remoto

The Curimataú estuary is located in the oriental coast of Rio Grande do Norte State in Brazil. Its importance resides in the fact that this region possesses one of the last portions of preserved mangrove in the Rio Grande do Norte State. Nevertheless, it has been severely affected by many anthropogenic activities, as sugarcane monoculture and shrimp farming. Former works demonstrated that an accumulation of heavy metals is occurring in oysters in this estuary, and perhaps it could be explained by the input of metals in this ecosystem deriving from the shrimp farming. To better understanding the origin of these metals, bottom sediment samples, cores and suspended particulate matter were collected for a characterization of metal concentrations (Al, Ba, Cd, Cu, Cr, Fe, Mn, Ni, Pb, Zn) and to determine the potentially bioavailable metals. Additionally, the enrichment ratio for each element analyzed was calculated. The mineralogical composition of sediment samples and cores were obtained by X-ray diffraction. Moreover, data of orbital remote sensing were used in order to detect and quantify suspended matter by applying a logarithmic algorithm. Geochemical data of bottom sediments and cores revealed that, excepting Ba and Pb, the elements analyzed presented concentrations characteristic of an unpolluted ecosystem (Al: 0,25 - 8,76 %; Ba: 3,03 - 870 µg.g-1; Cd: < 0,25 µg.g-1; Cr: 1,72 - 82,4 µg.g-1; Cu: 0,12 -25,3 µg.g-1; Pb: 0,38 - 23,7 µg.g-1; Fe: 0,10 - 5,82 %; Mn: 15,1 - 815 µg.g-1; Ni: 0,14 - 36,1 µg.g-1; Zn: 1,37 - 113 µg.g-1). During the dry season a distribution pattern was observed, with higher metal concentrations in the margins, decreasing toward the central portion of the channel. These metal concentrations were well correlated with mineralogical compositions, with clay minerals prevailing at the margins, and quartz and feldspar in the center. However, this pattern was not observed during the wet season, probably because of the high water flux that disturbed bottom sediments. But, as observed for the dry season, a good correlation between metal concentrations and mineralogical composition was also observed for the wet season, with high metal concentrations where there were high quantities of clay minerals. Low enrichment ratios were obtained for the majority of elements analyzed, excepting for Mn, Ba and Pb. Manganese presented the higher ratios downstream for both seasons, and it can be an evidence of anthropogenic impact by shrimp farming. As barium and lead concentrations in sediment samples presented analytical problems during the total sample digestion, one cannot be sure that the ratios obtained correspond to the reality. The highest metal concentrations in particulate matter were obtained in the portion dominated by fluvial transport for all metals analyzed, excepting for copper. Barium and zinc were the only elements that presented elevated concentrations that are not common of unpolluted ecosystems (Ba: 5730 - 8355 µg.g-1; Zn: 3899 - 4348 µg.g-1). However, these high concentrations could not be related to the shrimp farming and waste waters from the town of Canguaretama, once they were obtained from the fluvial particulate matter, that is upstream from the activities above mentioned. The application of the logarithmic algorithm to the processed LANDSAT image was well succeeded, although the acquired image does not correspond exactly to the field campaigns. The IKONOS image provided very detailed views of the suspended sediment concentration at the estuary, as the mixture of distinct water flows at the confluence of Cunhaú and Curimataú rivers, with more turbid waters from Cunhaú river, that is directly affected by effluents from shrimp farming and urban waste waters deriving from the town of Canguaretama

Síntese e caracterização de pós Ba(x)Sr(1-x)Co0,8Fe0,2O3- através do método de coprecipitação via oxalato

Ceramic powders based on oxides of perovskite-type structure is of fundamental interest nowadays, since they have important ionic-electronic conductivity in the use of materials with technological applications such as gas sensors, oxygen permeation membranes, catalysts and electrolytes for solid oxide fuel cells (SOFC). The main objective of the project is to develop nanostructured ceramic compounds quaternary-based oxide Barium (Br), Strontium (Sr), Cobalt (Co) and Iron (Fe). In this project were synthesized compounds BaxSr(1-x)Co0, 8Fe0,2O3- (x = 0.2, 0.5 and 0.8) through the oxalate co-precipitation method. The synthesized powders were characterized by thermogravimetric analysis and differential thermal analysis (TGADTA), X-ray diffraction (XRD) with the Rietveld refinement using the software MAUD and scanning electron microscopy (SEM). The results showed that the synthesis technique used was suitable for production of nanostructured ceramic solid solutions. The powders obtained had a crystalline phase with perovskite-type structure. The TGA-DTA results showed that the homogeneous phase of interest was obtained temperature above 1034°C. It was also observed that the heating rate of the calcination process did not affect the elimination of impurities present in the ceramic powder. The variation in the addition of barium dopant promoted changes in the average crystallite size in the nanometer range, the composition being BSCF(5582) obtained the lowest value (179.0nm). The results obtained by oxalate co-precipitation method were compared with those synthesis methods in solid state and EDTA-citrate method