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

Remoção de metais pesados em efluentes sintéticos utilizando vermiculita como adsorvente

Heavy metals are used in many industrial processestheirs discard can harm fel effects to the environment, becoming a serious problem. Many methods used for wastewater treatment have been reported in the literature, but many of them have high cost and low efficiency. The adsorption process has been used as effective for the metal remoal ions. This paper presents studies to evaluate the adsorption capacity of vermiculite as adsorbent for the heavy metals removal in a synthetic solution. The mineral vermiculite was characterized by differents techniques: specific surface area analysis by BET method, X-ray diffraction, raiosX fluorescence, spectroscopy in the infraredd region of, laser particle size analysis and specific gravity. The physical characteristics of the material presented was appropriate for the study of adsorption. The adsorption experiments weredriveal finite bath metod in synthetic solutions of copper, nickel, cadmium, lead and zinc. The results showed that the vermiculite has a high potential for adsorption, removing about 100% of ions and with removal capacity values about 85 ppm of metal in solution, 8.09 mg / g for cadmium, 8.39 mg/g for copper, 8.40 mg/g for lead, 8.26 mg/g for zinc and 8.38 mg/g of nickel. The experimental data fit in the Langmuir and Freundlich models. The kinetic datas showed a good correlation with the pseudo-second order model. It was conducteas a competition study among the metals using vermiculiti a adsorbent. Results showed that the presence of various metals in solution does not influence their removal at low concentrations, removing approximat wasely 100 % of all metals present in solutions

Síntese e caracterização de CuNb2O6 e CuNbC através de reação sólido- sólido e gás- sólido a baixa temperatura

The refractory metal carbides have proven important in the development of engineering materials due to their properties such as high hardness, high melting point, high thermal conductivity and high chemical stability. The niobium carbide presents these characteristics. The compounds of niobium impregnated with copper also have excellent dielectric and magnetic properties, and furthermore, the Cu doping increases the catalytic activity in the oxidation processes of hydrogen. This study aimed to the synthesis of nanostructured materials CuNbC and niobium and copper oxide from precursor tris(oxalate) oxiniobate ammonium hydrate through gas-solid and solid-solid reaction, respectively. Both reactions were carried out at low temperature (1000°C) and short reaction time (2 hours). The niobium carbide was produced with 5 % and 11% of copper, and the niobium oxide with 5% of copper. The materials were characterized by X-Ray Diffraction (XRD), Rietveld refinement, Scanning Electron Microscopy (SEM), X-Ray Fluorescence Spectroscopy (XRF), infrared spectroscopy (IR), thermogravimetric (TG) and differential thermal analysis (DTA , BET and particle size Laser. From the XRD analysis and Rietveld refinement of CuNbC with S = 1.23, we observed the formation of niobium carbide and metallic copper with cubic structure. For the synthesis of mixed oxide made of niobium and copper, the formation of two distinct phases was observed: CuNb2O6 and Nb2O5, although the latter was present in small amounts

Desenvolvimento de argamassa para restauração utilizando resíduo do polimento do porcelanato

The coatings mortars are essential elements of building structures because they execute an important role in protecting walls and are particularly exposed to aggressive action responsible for its degradation over time. The importance of wall coverings has been the subject of discussion and analysis in the conservation and rehabilitation of old buildings. Are sometimes removed and replaced with inappropriate solutions of constructive point of view or architecture. The most commonly used coatings on walls of old buildings is based on traditional hydraulic lime mortars. The present study aims at the formulation of new lime- based mortars and aerial fine aggregate, in order to contribute to a better field of conservation and restoration mortar coating of old buildings. Residue was used for polishing porcelain as fine aggregate, replacing the aggregate (sand), in percentages 05-30% by mass. We conducted a thorough evaluation of the mortar properties in fresh and hardened state by comparing the performance of the same with a reference mortar. The residue used was characterized as the density, bulk density, and particle size laser, scanning electron microscopy, X-ray diffraction and X-ray fluorescence. Formulations were produced 7, 6 with residue and one commonly used formulation, which served as a reference. In the formulations of lime mortars air (hydrated lime powder CH-I) has been adopted a stroke volume (1:3) with constant binder, was varied and the water / binder and aggregate and waste. For evaluation of mortars fresh, proceeded to consistency analysis, specific gravity, water retention and air content embedded. In the hardened state assays were performed in specific gravity, water retention, modulus of elasticity, tensile strength in bending, compressive strength, water absorption by capillary action, adhesion, tensile strength, resistance to shrinkage and salts by of crystallization trials with resources chloride solution, nitrate and sulfate all sodium in prismatic at 90 days of age, in addition to the micro structural analysis of mortars. Based on the results we can see that the mortar formulated with 10% content of waste and the reference free retraction feature more stable closer to neutrality. The composition of 10% was obtained better performance against the action of the salt crystallization. The mortar with 15% residue obtained better density, lower air content embedded and high capacity for water retention developing good workability. The replacement of 20% of waste generates a satisfactory utilization of resistance to compression, flexion and traction grip the base. And, finally, it can be seen that the mortar with 10, 15 and 20% residual show, in principle, good suitability as coatings, thus enabling a final result consistent with durability, workability and aesthetics developing therefore a material with better performance to repair or replace existing mortars in old buildings

Efeito da adição de fibras da palma do licuri (syagrus coronata) no comportamento físico e mecânico de compósitos de matriz cimentícia

This research was motivated by the requirement of asbestos s replacement in building systems and the need to generate jobs and income in the country side of the state of Bahia, Brazil. The project aimed at using fibers from licuri leaves (syagrus coronata), an abundant palm in the region, to produce composites appropriate for the sustainable production of cement fibre reinforced products in small plants. The composites were produced in laboratory using Portland cement CP-II-F32, sand, water, licuri palm fiber contents of 1.0, 1.5 and 2.0% by weight of binder (two different fiber length) and metakaolin. The latter was chosen as an additional binder for its efficiency to reduce the alkalinity of cementitious matrixes therefore preventing the degradation of vegetable fibers. The characterization of the composite components was carried out by sieving and laser particle size analyses, thermal analysis, fluorescence and X-ray diffraction. The composites performance was evaluated by 3- point-bending tests, compressive strength, ultrasound module of elasticity, free and restrained shrinkage, water capillarity absorption and apparent specific gravity. It has been found that the addition of fibers increased the time to onset of cracking over 200.00% and a 25% reduction in cracks opening in the restrained shrinkage test. The capillary absorption reduced about 25% when compared to fiber-free composites. It was also observed with regard to flexural strength, compressive strength and specific gravity, that the addiction of fibers did not affect the composite performance presenting similar results for compounds with and without fibers. In general it can be stated that the reinforced composite fibers of palm licuri presents physical and mechanical characteristics which enable them to be used in the intended proposals of this research

Redução aluminotérmica do óxido de tântalo usando uma tocha de plasma como ignitor

In this work was used a plasma torch of non transferred arc with argon as work gas, using a power supply with maximum DC current of 250 A and voltage of 30 V to activate the plasma and keep it switched on. The flame temperature was characterized by optical emission spectroscopy, through Boltzmann-plot-method. The torch has been used like igniter in the aluminothermic reduction of the mixture tantalum oxide and aluminum, seeking to obtain metallic tantalum. In heating of the reagents only one particle will be considered to study interactions between plasma-particle, seeking to determinate its fusion and residence time. The early powders were characterized by laser granulometry, scanning electron microscopy (SEM) and X-ray diffraction analysis. The final product of this reaction was characterized by SEM and X-ray diffraction. Crystallite size was calculated by the Scherrer equation and microdeformation was determined using Willamsom-Hall graph. With Rietveld method was possible to quantify the percentile in weight of the products obtained in the aluminothermic reaction. Semi-quantitative chemical analysis (EDS) confirmed the presence of metallic tantalum and Al2O3 as products of the reduction. As was waited the particle size of the metallic tantalum produced, presents values in nanometric scale due the short cooling time of those particles during the process

Influência da adição de cinza do bagaço de cana calcinada em sistemas de pastas para cimentação de poços petrolíferos

Cementing operation is one of the most important stages in the oil well drilling processes and has main function to form hydraulic seal between the various permeable zones traversed by the well. However, several problems may occur with the cement sheath, either during primary cementing or during the well production period. Cements low resistance can cause fissures in the cement sheath and compromise the mechanical integrity of the annular, resulting in contamination of groundwater and producing zones. Several researches show that biomass ash, in particular, those generated by the sugarcane industry have pozzolanic activity and can be added in the composition of the cementing slurries in diverse applications, providing improvements in mechanical properties, revenue and cement durability. Due to the importance of a low cost additive that increases the mechanical properties in a well cementing operations, this study aimed to potentiate the use of sugarcane bagasse ash as pozzolanic material, evaluate the mechanisms of action of this one on cement pastes properties and apply this material in systems slurries aimed to cementing a well with 800 m depth and geothermal gradient of 1.7 °F/100 ft, as much primary cementing operations as squeeze. To do this, the ash beneficiation methods were realized through the processes of grinding, sifting and reburning (calcination) and then characterization by X-ray fluorescence, XRD, TG / DTG, specific surface area, particle size distribution by laser diffraction and mass specific. Moreover, the ash pozzolanic activity added to the cement at concentrations of 0%, 20% and 40% BWOC was evaluated by pozzolanic activity index with lime and with Portland cement. The evaluation of the pozzolanic activity by XRD, TG / DTG and compressive strength confirmed the ash reactivity and indicated that the addition of 20% in the composition of cement slurries produces improvement 34% in the mechanical properties of the slurry cured. Cement slurries properties evaluated by rheological measurements, fluid loss, free fluid, slurry sedimentation, thickening time and sonic strength (UCA) were satisfactory and showed the viability of using the sugarcane ash in cement slurries composition for well cementing

Estudo do perfil térmico de fornos do tipo "caipira" utilizados pelo setor de cerâmica vermelha em parelhas na região Seridó-RN

The present study aimed to characterize the thermal profile of wood fired oven used by the red ceramic industry in Parelhas, in the Seridó region/RN, aiming to propose structural interventions that can contribute to increasing productivity and product quality, optimize wood consumption and mitigate existing losses during the burning process. The study was conducted at Cerâmica Esperança in the city of Parelhas -RN, Brazil, during the period from August 2012 to September 2013. Four treatments were performed with three replicates, ie, with, a total of 12 experimental units (burnings). In the first stage 4 treatments were performed with three replicates, totaling 12 experimental units (firings). In the second stage 2 treatments were performed with three replications, totaling 6 experimental units (firings). The physical characteristics of the wood were analyzed using standard NBR 11941 and NBR 7190 for basic density and moisture, respectively. The clay was used as a reference parameter for distinguishing treatments. For both the analysis and characterization was carried out using techniques of fluorescence X (XRF) rays, X-ray diffraction (XRD) analysis, particle size analysis (FA). In the first and second stages were monitored: the time during the firing process, the amount of wood used at each firing, the number of parts enfornadas for subsequent determination of the percentages of losses, but also product quality. To characterize the thermal profile of the oven, we measured the temperature at 15 points scored in the surface charge put into the oven. Measurements were taken every 30 minutes from preheat until the end of burning, using a pyrometer laser sight sighting from preheating until the end of burning. In the second step 12 metal cylinders distributed on the oven walls, and the cylinder end walls 8 of the furnace 2 and rollers on each side walls are installed equidistant to 17 cm from the soil and the surface 30 of the wall are installed. The cylinders distributed on the front were placed 50 cm above the furnace, and the base of the oven 20 cm distant from the ground. 10 also thermocouples were installed, and five thermocouples distributed 1.77 cm above the combustion chambers, and one thermocouple on each side, and three thermocouples in front of the oven. We carried out the measurements of the temperatures every 1 hour during the burning two hours in cooling the cylinders with a pyrometer and thermocouples for dattaloger. These were fixed with depth of 30 cm from the wall. After statistical analysis it was found that: the thermal profile of the furnace surface and at different heights was heterogeneous; and the ranges of density and moisture content of wood are within recommended for use as an energy source standards. We conclude that even at low temperatures reached during firing there was a significant production of good quality products, this is due to high concentrations of iron oxide and potassium oxide found in clay, which lowers the melting point of the piece. The average burn time for each step varied 650-2100 minutes wood consumption was on average 20 m3, product quality was on average 16% of first quality, 70% second, third and 5% to 10% loss . The distance between the wire and the surface of the oven was a significant parameter for all treatments, but with different variations, meaning that the wire should not be so generic and unique form, used as a criterion for completion of the burn process. The central part of the furnace was the area that reached higher temperature, and in a unified manner, with the highest concentration of top quality products. The ideal temperature curve, which provided the highest quality of ceramic products was achieved in the central part of the furnace

Obtenção de pós de Nb a partir da redução aluminotérmica com ignição por plasma

The aluminothermic reduction consists in an exothermic reaction between a metallic oxide and aluminum to produce the metal and the scum. The extracted melted metal of that reaction usually comes mixed with particles of Al2O3 resulting of the reduction, needing of subsequent refine to eliminate the residual impure as well as to eliminate porosities. Seeking to obtain a product in powder form with nanometric size or even submicrometric, the conventional heat source of the reaction aluminothermic , where a resistor is used (ignitor) as ignition source was substituted, for the plasma, that acts more efficient way in each particle of the sample. In that work it was used as metallic oxide the niobium pentoxide (Nb2O5) for the exothermal reaction Nb2O5 + Al. Amounts stoichiometric, substoichiometric and superestoichiometric of aluminum were used. The Nb2O5 powder was mixed with aluminum powder and milled in planetarium of high energy for a period of 6 hours. Those powders were immerged in plasm that acts in a punctual way in each particle, transfering heat, so that the reaction can be initiate and spread integrally for the whole volume of the particle. The mixture of Nb2O5 + Al was characterized through the particle size analysis by laser and X-ray diffraction (DRX) and the obtained product of reaction was characterized using the electronic microscopy of sweeping (MEV) and the formed phases were analyzed by DRX. Niobium powders with inferior sizes to 1 mm were obtained by that method. It is noticed, through the analysis of the obtained results, that is possible to accomplish the aluminothermic reduction process by plasma ignition with final particles with inferior sizes to the original oxide

Photoluminescence of Eu(3+) ion in SnO(2) obtained by sol-gel

Photoluminescence data of Eu-doped SnO(2) xerogels are presented, yielding information on the symmetry of Eu(3+) luminescent centers, which can be related to their location in the matrix: at lattice sites, substituting to Sn(4+), or segregated at particles surface. Influence of doping concentration and/or particle size on the photoluminescence spectra obtained by energy transfer from the matrix to Eu(3+) sites is investigated. Results show that a better efficiency in the energy transfer processes is obtained for high symmetry Eu(3+) sites and low doping levels. Emission intensity from (5)D(0) -> (7)F(1) transition increases as the temperature is raised from 10 to 240 K, under excitation at 266 nm laser line, because in this transition the multiphonon emission becomes significant only above 240 K. As an extension of this result, we predict high effectiveness for room temperature operation of Eu-based optical communication devices. X-ray diffraction data show that the impurity excess inhibits particle growth, which may influence the asymmetry ratio of luminescence spectra.

Hydroxyapatite deposition study through polymeric process on commercially pure Ti surfaces modified by laser beam irradiation

Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)

Estudo comparativo das argilas das olarias dos municípios de Alfenas e Areado, MG

Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)

Razão triglicérides/HDL-C e proteína C reativa de alta sensibilidade na avaliação do risco cardiovascular

Introduction: Calculated indexes from laboratory measurements and the determination of plasma markers are commonly used in cardiovascular risk assessment. Objective: To use triglycerides/high-density lipoprotein cholesterol (HDL-C) ratio, estimate of low-density lipoprotein (LDL) particle size and high sensitive C-reactive protein (hs-CRP) levels to the clinical and laboratorial assessment of coronary risk among patients with coronary disease. Material and methods: Sixty patients were chosen accordingly, 36 female (F) (65 ± 9 years of age) and 24 male (M) (55 ± 10 years of age) diagnosed with stable ischemic cardiopathy at Ana Neri Hospital, Salvador, Bahia, Brazil. The investigation was carried out at the Clinical Biochemistry Laboratory of the College of Pharmacy at Federal University of Bahia (UFBA). Blood samples were collected after a 12-hour fast to determine hs-CRP, lipid profile and risk indicators. All data were assessed through Syncron LX®20 Beckman Coulter. The inferential analysis results were considered significant when p ≤ 5%. Data analysis was carried out with GraphPad Prism® (4.03 version) software. Results: Data analysis showed a positive correlation between hs-CRP and triglycerides/HDL-C ratio only among women (r = 0.4; p = 0.0442), n = 36. The analysis of other parameters did not show any significance. Conclusion: The triglycerides/HDL-C ratio and hs-CRP may be used as indicators of increase in cardiovascular risk among women with coronary artery disease (CAD).

Air-particle abrasion on zirconia ceramic using different protocols: Effects on biaxial flexural strength after cyclic loading, phase transformation and surface topography

This study evaluated the effect of different air-particle abrasion protocols on the biaxial flexural strength and structural stability of zirconia ceramics. Zirconia ceramic specimens (ISO 6872) (Lava, 3M ESPE) were obtained (N=336). The specimens (N=118, n=20 per group) were randomly assigned to one of the air-abrasion protocols: Gr1: Control (as-sintered); Gr2: 50 μm Al2O3 (2.5 bar); Gr3: 50 μm Al2O3 (3.5 bar); Gr4: 110 μm Al2O3(2.5 bar); Gr5: 110 μm Al2O3 (3.5 bar); Gr6: 30 μm SiO2 (2.5 bar) (CoJet); Gr7: 30 μm SiO2(3.5 bar); Gr8: 110 μm SiO2 (2.5 bar) (Rocatec Plus); and Gr9: 110 μm SiO2 (3.5 bar) (duration: 20 s, distance: 10 mm). While half of the specimens were tested immediately, the other half was subjected to cyclic loading in water (100,000 cycles; 50 N, 4 Hz, 37 °°C) prior to biaxial flexural strength test (ISO 6872). Phase transformation (t→m), relative amount of transformed monoclinic zirconia (FM), transformed zone depth (TZD) and surface roughness were measured. Particle type (p=0.2746), pressure (p=0.5084) and cyclic loading (p=0.1610) did not influence the flexural strength. Except for the air-abraded group with 110 μm Al2O3 at 3.5 bar, all air-abrasion protocols increased the biaxial flexural strength (MPa) (Controlnon-aged: 1030±153, Controlaged: 1138±138; Experimentalnon-aged: 1307±184-1554±124; Experimentalaged: 1308±118-1451±135) in both non-aged and aged conditions, respectively. Surface roughness (Ra) was the highest with 110 μm Al2O3(0.84 μm. FM values ranged from 0% to 27.21%, higher value for the Rocatec Plus (110 μm SiO2) and 110 μm Al2O3 groups at 3.5 bar pressure. TZD ranged between 0 and 1.43 μm, with the highest values for Rocatec Plus and 110 μm Al2O3 groups at 3.5 bar pressure. © 2013 Elsevier Ltd.

Estudo das características de tamanho de gotas de bicos de pulverização de energia centrífuga e hidráulica na cultura do algodoeiro

Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)