801 resultados para DRX e MEV


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Adsorption is a process that has become indispensable due to pollution caused by industrial activity. More economically viable adsorbents are being tested to replace the high cost of materials used. The clays can be used as adsorbents and are low cost materials, natural properties feasible for the application in the adsorption process, structural modifications are performed with ease promoting selective adsorption in these materials. The objective of this study was to synthesize and characterize adsorbents used in the adsorption of organic compounds. The adsorbents were characterized by the techniques of XRD, SEM, FTIR and TG. The results show that the studied materials have affinity to organic compounds and can be applied as adsorbents. The materials studied are viable and can be applied in the treatment of effluents contaminated in industrial scale.

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Ferroelectric ceramics with perovskite structure (ABO3) are widely used in solid state memories (FeRAM’s and DRAM's) as well as multilayered capacitors, especially as a thin films. When doped with zirconium ions, BaTiO3-based materials form a solid solution known as barium zirconate titanate (BaTi1-xZrxO3). Also called BZT, this material can undergo significant changes in their electrical properties for a small variation of zirconium content in the crystal lattice. The present work is the study of the effects of deposition parameters of BaTi0,75Zr0,25O3 thin films by spin-coating method on their morphology and physical properties, through an experimental design of the Box-Behnken type. The resin used in the process has been synthesized by the polymeric precursor method (Pechini) and subsequently split into three portions each of which has its viscosity adjusted to 10, 20 and 30 mPa∙s by means of a rotary viscometer. The resins were then deposited on Pt/Ti/SiO2/Si substrates by spin-coating method on 15 different combinations of viscosity, spin speed (3000, 5500 and 8000 rpm) and the number of deposited layers (5, 8 and 11 layers) and then calcined at 800 ° C for 1 h. The phase composition of the films was analyzed by X-ray diffraction (XRD) and indexed with the JCPDS 36-0019. Surface morphology and grain size were observed by atomic force microscopy (AFM) indicating uniform films and average grain size around 40 nm. Images of the cross section of the films were obtained by scanning electron microscopy field emission (SEM-FEG), indicating very uniform thicknesses ranging from 140-700 nm between samples. Capacitance measurements were performed at room temperature using an impedance analyzer. The films presented dielectric constant values of 55-305 at 100kHz and low dielectric loss. The design indicated no significant interaction effects between the deposition parameters on the thickness of the films. The response surface methodology enabled better observes the simultaneous effect of variables.

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This work presents a new ceramic material obtained through the incorporation of solid waste from the steel industry and known as dedusting powder PAE - in ceramic formulations based on clay, potassium and sodium feldspars, kaolin and talc. Formulations were prepared with ceramic residue levels of 0% (basic mass - MB), 2%, 4% and 8%, subjected to firing at temperatures of 1000 ° C, 1050ºC, 1100ºC and 1150ºC for periods of 15 min. and 120 min. The physicchemical and mechanical properties of these ceramic formulations were determined based on the firing temperature, residence time in the oven and the percentage of waste. Since the physicochemical and mechanical properties of the sintered materials were evaluated by chemical analysis techniques (fluorescence X-rays - FRX), particle size distribution, specific surface area, apparent density, structural analysis by diffraction of X-rays (DRX) and characterization of surface by scanning electron microscopy (SEM). The magnetic response characteristics and the pattern of magnetic ferrites of the samples were analyzed in the assay conditions, having noticed that the saturation magnetic susceptibility depend on the sintering temperature of the material and it is associated with its crystal structure. From the analysis results, it was concluded that the ceramic material with better physical and mechanical properties is obtained when the 8% from PAE residue is added to standard formulation under the burn time of 15 minutes and temperature of 1150ºC.

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This work shows that the synthesis by combustion is a prominent alternative to obtain ceramic powders of higher oxides, nanostructured and of high purity, as the ferrites of formulas Co(1-x)Zn(x)Fe2O4 e Ni(1-x)Zn(x)Fe2O4 with x ranging from 0.2 mols, in a range from 0.2 ≤ x ≥ 1.0 mol, that presents magnetic properties in coexistence of ferroelectric and ferrimagnetic states, which can be used in antennas of micro tapes and selective surfaces of low frequency in a range of miniaturized microwaves, without performance loss. The obtainment occurred through the combustion process, followed by appropriate physical processes and ordered to the utilization of the substrate sinterization process, it gave us a ceramic material, of high purity degree in a nanometric scale. The Vibrating Sample Magnetometer (VSM) analysis showed that those ferritic materials presents parameters, as materials hysteresis, that have own behavior of magnetic materials of good quality, in which the magnetization states can be suddenly changed with a relatively small variation of the field intensity, having large applications on the electronics field. The X-ray Diffraction (XRD) analysis of the ceramic powders synthesized at 900 °C, characterize its structural and geometrical properties, the crystallite size and the interplanar spacing. Other analysis were developed, as Scanning Electron Microscopy (SEM), X-ray Fluorescence (XRF), electric permittivity and the tangent loss, in high frequencies, through the equipment ZVB - 14 Vector Network Analyzer 10 MHz-14 GHz, of ROHDE & SCHWART.

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A Proteção Respiratória Ocupacional é atualmente uma exigência legal do Ministério do Trabalho e Emprego para garantia da saúde e segurança de milhares de trabalhadores que labutam com exposição habitual a substâncias nocivas que possam ocasionar doenças ocupacionais por inalação de ar contaminado no local de trabalho, cuja principal via de penetração no organismo humano é o Sistema Respiratório. Carvões ativados são materiais obtidos a partir de fontes carbonáceas e utilizados como elemento tecnológico filtrante nos equipamentos destinados a proteção respiratória individual. Fomentada por esse contexto, e visando potencializar conceitos de eco-eficiência e sustentabilidade em produção de materiais, este trabalho destina-se a produção de carvão ativado com potencial filtrante a partir de um rejeito agrícola abundante na região Nordeste do Brasil através de uma rota que favorece carbonização e ativação simultâneas, seguido de neutralização térmica. A biomassa precursora foi caracterizada por Ensaios padrões para determinação do teor de umidade e cinzas, Análise Química Elementar, Análises Térmicas (TG e DSC) e Distribuição Granulométrica por difração a laser. As amostras de carvões ativos sintetizadas foram caracterizadas por Difração de Raios X (DRX), Medidas de área específica por BET, Microscopia Eletrônica de Varredura (MEV), Análise assistida com ultravioleta visível e Redução à Temperatura Programada (TPR) por Amônia. A rota empregada favorece uma tecnologia alternativa para o aproveitamento de resíduos e aplicável para a Proteção Respiratória Ocupacional. A atmosfera de queima influencia diretamente na produção. A temperatura de carbonização variou conforme a estabilidade térmica da amostra. A cristalinidade, morfologia, teor mineralógico, área superficial específica e a adsorção em fase líquida e gasosa variaram em função da interação do resíduo precursor com o tipo e concentração de ácido utilizado. Os ensaios de adsorção demonstraram a efetividade da ativação segundo a rota experimental proposta. O potencial catalítico dos materiais produzidos para uso em máscaras respiratórias foi evidenciado pelo ensaio de TPR. O processo de produção estudado se mostrou eficaz para obtenção dos carvões promovendo processamentos e aplicações mais nobres para materiais cujo uso tem sido restrito a meras aplicações primárias ou descarte, mas cujo potencial tecnológico é amplo, empreendedor, sustentável, viável em escala industrial e de baixo custo.

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The Sustainability has been evidence in the world today; organizations have sought to be more and more into this philosophy in their processes, whether products or attendance. In the present work were manufactured eco-composites with animal fiber (dog wool) that is currently discarded into the environment without any use. Project phases consisted on the initial treatment of fibers with alkaline solution (NaOH) at 0.05 mols for removal of impurities, developing methods to convert these fibers (reinforcement) blended with castor oil polyurethane (matrix) in eco-composite with different proportions (5%, 10%, 15% and 20%). Fiber properties were evaluated by analysis of SEM, XRD and FTIR. The composites were produced by compression molding with dimensions 30x30x1cm. For characterization of the composites the following tests were performed: mechanical (tensile, compression, shore hardness A) according the standards and testing water absorption, moisture regain and biodegradation. The analysis of thermal properties on fibers and composites were by TG, DSC, thermal conductivity, resistivity, heat capacity and thermal resistance. Analyzing the results of these tests, it was observed that the composite reinforced with 20% showed a better thermal performance between others composites and dimensional stability when compared to commercial thermal insulation. Also is possible to observe a balance in moisture absorption of the composite being shown with its higher absorption rate in this same sample (20%). The micrographs show the fiber interaction regions with polyurethane to fill the empty spaces. In hardness and compression testing can identify that with increasing percentage of the fiber material acquires a greater stiffness by making a higher voltage is used for forming necessary. So by the tests performed in eco-composites, the highest percentage of fiber used as reinforcement in their composition obtained a better performance compared to the remaining eco-composites, reaching values very close to the PU.

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Pozzolanic materials such as rice husk ash are widely used to substitute part of cement, because they react with calcium hydroxide (CH) producing calcium silicate hydrate (C-S-H), which aggregate better physical, chemical and mechanical properties to the cement slurry. The usage of rice husk biomass ash from agribusiness in addition to or partially replacing cement is a noble purpose and a good way of sustainable development which currently is an obsession around the world. The ashes utilized in this study were characterized by: scanning electron microscopy technique (SEM), Fourier transform infrared spectroscopy (FTIR), Energy-dispersive X-ray spectroscopy (EDX) and BET method. The pozzolanic activity of RHA and WRHA in cement slurries was evaluated by: thermal-gravimetric technique and derivative thermogravimetry (TGA/DTG), X-ray diffraction (XRD) and Compressive Strength. The slurries formulated with additions of 10% and 20% of RHA and WRHA were cured for 28 days at 58 °C. The results of thermal analysis demonstrated that a 20% WRHA addition caused a reduction of approximately 73% of Portlandite (calcium hydroxide – CH) phase related to standard slurry (STD). The XRD scans also demonstrated the reduction of the Portlandite peaks’ intensity for each slurry compared with STD slurry. The RHA and WRHA react chemically with Portlandite producing calcium silicate hydrate (C-S-H), confirming their effect as a pozzolanic agent. The WRHA presented the best results as a pozzolanic material.

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This study aimed to evaluate the potential of oxidative electrochemical treatment coupled with adsorption process using expanded perlite as adsorbent in the removal of textile dyes, Red Remazol and Novacron Blue on synthetic effluent. Dyes and perlite were characterized by thermogravimetry techniques (TG), Differential Scanning Calorimetry (DSC), Spectroscopy infrared (IR), Scanning Electron Microscopy (SEM), X-ray diffraction (XRD) and X-ray fluorescence (XRF) techniques. Electrochemical treatments used as anodes, Ti/Pt and Pb/PbO2 under different conditions: 60 minutes, current density 20, 40 e 60 mAcm-2, pH 1, 4.5 e 8 and temperature variation 20, 40 e 60 ºC. In the case of adsorption tests, contact time of 30 minutes for the Remazol Red dye and 20 minutes for Novacron Blue were established, while pH 1, 4.5 e 8, 500 mg adsorbent and temperature variation 20, 40 e 60 ºC were used for both treatments. The results indicated that both treatments, electroxidation/adsorption and the adsorption/electroxidation, were effective for removing color from synthetic solutions. The consumption of electricity allowed to evaluate the applicability of the electrochemical process, providing very acceptable values, which allowed us to estimate the cost. Total organic carbon (TOC) and Gas Chromatography linked mass spectrometer (GC-MS) analyzes were performed, showing that the better combination for removing organic matter is by Pb/PbO2 and perlite. Meanwhile, GC-MS indicated that the by-products formed are benzoic acid, phthalic acid, thiocarbamic acid, benzene, chlorobenzene, phenol-2-ethyl and naphthalene when Remazol Red was degraded. Conversely, aniline, phthalic acid, 1, 6 - dimethylnaphthalene, naphthalene and ion hidroxobenzenosulfonat was detected when Novacron Blue was studied. Analyses obtained through atomic absorption spectrometry showed that there was release of lead in the electrochemical oxidation of analyzes that were performed with the anode Pb/PbO2, but these values are reduced by subjecting the effluent to adsorption analysis. According to these results, sequential techniques electroxidation/adsorption and adsorption/electroxidation are to treat solutions containing dyes.

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This study aimed to evaluate the potential of oxidative electrochemical treatment coupled with adsorption process using expanded perlite as adsorbent in the removal of textile dyes, Red Remazol and Novacron Blue on synthetic effluent. Dyes and perlite were characterized by thermogravimetry techniques (TG), Differential Scanning Calorimetry (DSC), Spectroscopy infrared (IR), Scanning Electron Microscopy (SEM), X-ray diffraction (XRD) and X-ray fluorescence (XRF) techniques. Electrochemical treatments used as anodes, Ti/Pt and Pb/PbO2 under different conditions: 60 minutes, current density 20, 40 e 60 mAcm-2, pH 1, 4.5 e 8 and temperature variation 20, 40 e 60 ºC. In the case of adsorption tests, contact time of 30 minutes for the Remazol Red dye and 20 minutes for Novacron Blue were established, while pH 1, 4.5 e 8, 500 mg adsorbent and temperature variation 20, 40 e 60 ºC were used for both treatments. The results indicated that both treatments, electroxidation/adsorption and the adsorption/electroxidation, were effective for removing color from synthetic solutions. The consumption of electricity allowed to evaluate the applicability of the electrochemical process, providing very acceptable values, which allowed us to estimate the cost. Total organic carbon (TOC) and Gas Chromatography linked mass spectrometer (GC-MS) analyzes were performed, showing that the better combination for removing organic matter is by Pb/PbO2 and perlite. Meanwhile, GC-MS indicated that the by-products formed are benzoic acid, phthalic acid, thiocarbamic acid, benzene, chlorobenzene, phenol-2-ethyl and naphthalene when Remazol Red was degraded. Conversely, aniline, phthalic acid, 1, 6 - dimethylnaphthalene, naphthalene and ion hidroxobenzenosulfonat was detected when Novacron Blue was studied. Analyses obtained through atomic absorption spectrometry showed that there was release of lead in the electrochemical oxidation of analyzes that were performed with the anode Pb/PbO2, but these values are reduced by subjecting the effluent to adsorption analysis. According to these results, sequential techniques electroxidation/adsorption and adsorption/electroxidation are to treat solutions containing dyes.

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Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)

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Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)

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Composites based on alumina (Al2O3), tungsten carbide (WC) and cobalt (Co) exhibit specific properties such as low density, high oxidation resistance, high melting point and high chemical inertia. That composite shows to be a promising material for application in various fields of engineering. In this work, the mechanical properties of the composite (Al2O3 – WC – Co), particularly density and hardness, were evaluated according to the effects of the variables of powder processing parameters, green compact and sintered. Powder composites with the composition of 80 wt% Al2O3, 18 wt% WC and 2 wt% Co were processed by high energy ball milling in a planetary mill for 50 hours as well as mixed by manual mixing in a glass vessel with the same proportion. Samples were collected (2, 10, 20, 30, 40 and 50 hours) during the milling process. Then, the powders were compacted in a cylindrical die with 5 mm in diameter in a uniaxial press with pressures of 200 and 400 MPa. The sintering was in two stages: first, the solid phase sintering was performed at 1126 and 1300 °C for 1 hour with a heating rate of 10 °C/min in a resistive furnace under argon atmosphere for green samples compacted in 200 and 400 MPa; the second sintering was performed on dilatometer in solid phase at 1300 °C for green sample compacted in 200 MPa, another sintering also was performed on dilatometer, this time in liquid phase at 1550 °C for green samples compacted in 200 and 400 MPa, with the same parameters used in resistive furnace. The raw materials were characterized by X – ray diffraction (XRD), X – ray fluorescence (XRF), scanning electron microscopy (SEM), energy dispersive spectroscopy (EDS) and laser particlemeter. The sintered samples were subjected to microhardness testing. The results showed that high energy milling achieved to the objectives regarding the particle size and the dispersion of composite phases. However, the hardness did not achieve to significant results, this is an indication that the composite has low fracture toughness.

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Composites based on alumina (Al2O3), tungsten carbide (WC) and cobalt (Co) exhibit specific properties such as low density, high oxidation resistance, high melting point and high chemical inertia. That composite shows to be a promising material for application in various fields of engineering. In this work, the mechanical properties of the composite (Al2O3 – WC – Co), particularly density and hardness, were evaluated according to the effects of the variables of powder processing parameters, green compact and sintered. Powder composites with the composition of 80 wt% Al2O3, 18 wt% WC and 2 wt% Co were processed by high energy ball milling in a planetary mill for 50 hours as well as mixed by manual mixing in a glass vessel with the same proportion. Samples were collected (2, 10, 20, 30, 40 and 50 hours) during the milling process. Then, the powders were compacted in a cylindrical die with 5 mm in diameter in a uniaxial press with pressures of 200 and 400 MPa. The sintering was in two stages: first, the solid phase sintering was performed at 1126 and 1300 °C for 1 hour with a heating rate of 10 °C/min in a resistive furnace under argon atmosphere for green samples compacted in 200 and 400 MPa; the second sintering was performed on dilatometer in solid phase at 1300 °C for green sample compacted in 200 MPa, another sintering also was performed on dilatometer, this time in liquid phase at 1550 °C for green samples compacted in 200 and 400 MPa, with the same parameters used in resistive furnace. The raw materials were characterized by X – ray diffraction (XRD), X – ray fluorescence (XRF), scanning electron microscopy (SEM), energy dispersive spectroscopy (EDS) and laser particlemeter. The sintered samples were subjected to microhardness testing. The results showed that high energy milling achieved to the objectives regarding the particle size and the dispersion of composite phases. However, the hardness did not achieve to significant results, this is an indication that the composite has low fracture toughness.

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Contamination of groundwater by BTX has been featured in recent decades. This type of contamination is due to small and continuous leaks at gas stations, causing serious problems to public health and the environment. Based on these antecedents, the search for new alternatives for treating contaminated water is shown to be essential. Therefore, this study aimed to evaluate the efficiency of removal of BTX by adsorption processes employing commercial alumina (Al2O3) and alumina supported with iron (Fe/Al2O3) as adsorbents. It was prepared by a in a synthetic gasoline solution and distilled water to simulate an actual sample. Initially, the adsorbents were characterized by techniques XRD, TG / DTG, XRF, FTIR and SEM/EDS, several trials, where he was placed synthetic solution to react in the presence of Al2O3 and Fe/Al2O3 in a closed, mechanical stirring system were performed varying the catalyst concentration 2, 4 and 6 g.L-1 every 0, 10, 30 60, 90 and 120 min, aliquots were taken and brought to analysis by gas chromatography flame ionization with headspace extraction. The results indicated that the absorbent which has higher BTX removal capacity was the Fe/Al2O3 at a concentration of 6 g.L-1, pH = 4 and time of 90 minutes reaction, resulting in an efficiency, resulting in a 86,5% efficiency for benzene removal, for the 95,4% toluene, 90,8% for ɱ,ρ- xylene and 93.7% for the θ-xylenes. Subsequently, we performed a kinetic study of the reactions, the values of experimental adsorption capacity (qe) showed agreement with the values of the theoretical adsorption capacity (qc) to the pseudo-second-order model in the adsorption tests using 2 and 6 gL-1 of Al2O3 and assays using 2, 4 and 6 g.L-1 of Fe/Al2O3. A fact corroborated by the R2 values, thus indicating that the chemical interactions are present in the adsorption mechanisms of BTX.

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Lubricants and cutting middle distillates typically have large amounts of n-paraffins to increase its freezing point and fluidity. Accordingly, the removal of n-paraffins of long chain lubricants oils and diesel is essential to get a product with good cold flow properties. The development of new catalysts, which exhibit thermal stability and catalytic activity for the hydroisomerization reaction is still a challenge. Thus, silicoaluminophosphates (SAPO) were synthesized by different routes. Have been used also post-synthesis treatment for obtaining hybrid structures and others synthesis have been carried out with mesoporous template (soft and hard-template). Therefore, SAPO have been impregnated with H2PtCl6 solution by the incipient wetness method. Then assessments of catalytic activities in hydroisomerization and hydrocracking reactions of hexadecane have been held. Besides SAPO, niobium phosphate - NbP - were also impregnated with platinum and evaluated in the same reaction. After impregnation, these catalysts have been characterized by X-ray diffraction (XRD), nitrogen adsorption, infrared spectroscopy with adsorbed pyridine (IV-PY), scanning electron microscopy (SEM) and resonance nuclear magnetic 29Si (29Si-NMR). The characterization results by XRD have shown that it has been possible to obtain mesoporous SAPOs. However, for the syntheses with soft template there was collapse of the structure after removal of the organic template. Even so, these catalysts have been actives. It was possible to obtain hybrid materials through the synthesis of SAPO-11 made with hard templates and by means of post-synthesis treatments samples of SAPO-11. Moreover, NbP has shown characteristic XRD of amorphous materials, with high acidity and were active in the conversion of hexadecane.