Estudo da síntese e sinterização de pós compósitos do sistema Ta-Cu

Ta-Cu bulk composites combine high mechanical resistance of the Ta with high electrical and thermal conductivity of the Cu. These are important characteristics to electrical contacts, microwave absorber and heat skinks. However, the low wettability of Ta under Cu liquid and insolubility mutual these elements come hard sintering this composite. High-energy milling (HEM) produces composite powders with high homogeneity and refines the grain size. This work focus to study Ta-20wt%Cu composite powders prepared by mechanical mixture and HEM with two different conditions of milling in a planetary ball mill and then their sintering using hydrogen plasma furnace and a resistive vacuum furnace. After milling, the powders were pressed in a steel dye at a pressure of 200 MPa. The cylindrical samples pressed were sintered by resistive vacuum furnace at 10-4torr with a sintering temperature at 1100ºC / 60 minutes and with heat rate at 10ºC/min and were sintered by plasma furnace with sintering temperatures at 550, 660 and 800ºC without isotherm under hydrogen atmosphere with heat rate at 80ºC/min. The characterizations of the powders produced were analyzed by scanning electron microscopy (SEM), x-ray diffraction (XRD) and laser granulometry. After the sintering the samples were analyzed by SEM, XRD and density and mass loss tests. The results had shown that to high intense milling condition produced composite particles with shorter milling time and amorphization of both phases after 50 hours of milling. The composite particles can produce denser structure than mixed powders, if heated above the Cu melting point. After the Cu to arrive in the melting point, liquid copper leaves the composite particles and fills the pores

Aproveitamento de resíduos minerais na formulação de argamassas para a construção civil

Current environmental concerns include the excessive consumption and inefficient use of non-renewable natural resources. The construction industry is considered one of the largest consumers of natural raw materials, significantly contributing to the environmental degradation of the planet. The use of calcareous quarry (RPPC) and porcelain tile polishing residues (RPP) as partial replacements of the cement in mortars is an interesting alternative to minimize the exploration of considerably large amounts of natural resources. The present study aimed at investigating the properties of fresh and hardened mortars produced using residues to replace cement. The residues used were fully characterized to determine their specific mass, unitary mass, particle size distribution and morphology, and composition. The performance of the mortars was compared to that of reference compositions, prepared without residues. A total of 18 compositions were prepared, 16 using residues and 2 reference ones. The mortars were prepared using Portland CP II F 32 cement, CH I hydrated lime, river sand and tap water. The compositions of the mortars were 1:1:6 and 1:0.5:4.5 (vol%), and water to cement ratios of 1.87 and 1.45 were used, respectively. The mortars in the fresh state were evaluated by consistency index, water retention, density of mass and incorporated air content tests. In their hardened state, the mortars were evaluated by apparent mass density, modulus of elasticity, flexural tensile strength, compressive strength and water absorption by capillarity. The mortars were also analyzed by scanning electron microscopy, energy dispersive spectroscopy, X-ray diffraction and fluorescence. Finally, they were classified according to NBR 13281 standards. The mortars prepared using residues partially replacing the cement exhibited lower modulus of elasticity compared to the reference compositions, thus improving the performance in their intended use. On the downside, the water absorption by capillarity was affected by the presence of residues and both the tensile and compressive strength were reduced. However, from the overall standpoint, the replacement of cement by calcareous quarry or porcelain tile polishing residues did not result in significant changes in the properties of the mortars. Therefore, compositions containing these residues can be used in the construction industry

Caracterização de compósitos Nb-20%cu obtidos por moagem de alta energia e sinterizados por fase líquida

In this work, was studied the formation of a composite of the refractory metal niobium with copper, through the process of high-energy milling and liquid phase sintering. The HEM can be used to synthesize composite powders with high homogeneity and fine size particle distribution. It may also produce the solid solubility in immiscible systems such as Nb-Cu, or extend the solubility of systems with limited solubility. Therefore, in the immiscible system Cu-Nb, the high-energy milling was successfully used to obtain the composite powder particles. Initially, the formation of composite particles during the HEM and the effect of preparation technique on the microstructure of the material was evaluated. Four loads of Nb and Cu powders containing 20%wt Cu were synthesized by MAE in a planetary type ball mill under different periods of grinding. The influence of grinding time on the metal particles is evaluated during the process by the withdrawal of samples at intermediate times of milling. After compaction under different forces, the samples were sintered in a vacuum furnace. The liquid phase sintering of these samples prepared by HEM produced a homogeneous and fine grained. The composite particles forming the sintered samples are the addition of a hard phase (Nb) with a high melting point, and a ductile phase (Cu) with low melting point and high thermal and electrical conductivities. Based on these properties, the Nb-Cu system is a potential material for many applications, such as electrical contacts, welding electrodes, coils for generating high magnetic fields, heat sinks and microwave absorbers, which are coupled to electronic devices. The characterization techniques used in this study, were laser granulometry, used to evaluate the homogeneity and particle size, and the X-ray diffraction, in the phase identification and to analyze the crystalline structure of the powders during milling. The morphology and dispersion of the phases in the composite powder particles, as well the microstructures of the sintered samples, were observed by scanning electron microscopy (SEM). Subsequently, the sintered samples are evaluated for density and densification. And finally, they were characterized by techniques of measuring the electrical conductivity and microhardness, whose properties are analyzed as a function of the parameters for obtaining the composite

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 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

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

Monitoramento da morfologia costeira em setores da bacia potiguar sob influência da indústria petrolífera utilizando geodésia de alta precisão e laser escâner terrestre

The objective of this Doctoral Thesis was monitoring, in trimestral scale, the coastal morphology of the Northeastern coast sections of Rio Grande do Norte State, in Brazil, which is an area of Potiguar Basin influenced by the oil industry activities. The studied sections compose coastal areas with intense sedimentary erosion and high environmental sensitivity to the oil spill. In order to achieve the general objective of this study, the work has been systematized in four steps. The first one refers to the evaluation of the geomorphological data acquisition methodologies used on Digital Elevation Model (DEM) of sandy beaches. The data has been obtained from Soledade beach, located on the Northeastern coast of Rio Grande Norte. The second step has been centered on the increasing of the reference geodetic infrastructure to accomplish the geodetic survey of the studied area by implanting a station in Corta Cachorro Barrier Island and by conducting monitoring geodetic surveys to understand the beach system based on the Coastline (CL) and on DEM multitemporal analysis. The third phase has been related to the usage of the methodology developed by Santos; Amaro (2011) and Santos et al. (2012) for the surveying, processing, representation, integration and analysis of Coastlines from sandy coast, which have been obtained through geodetic techniques of positioning, morphological change analysis and sediment transport. The fourth stage represents the innovation of surveys in coastal environment by using the Terrestrial Laser Scanning (TLS), based on Light Detection and Ranging (LiDAR), to evaluate a highly eroded section on Soledade beach where the oil industry structures are located. The evaluation has been achieved through high-precision DEM and accuracy during the modeling of the coast morphology changes. The result analysis of the integrated study about the spatial and temporal interrelations of the intense coastal processes in areas of building cycles and destruction of beaches has allowed identifying the causes and consequences of the intense coastal erosion in exposed beach sections and in barrier islands

Efetividade do clareamento dentário com peróxido de carbamida a 10% e avaliação dos efeitos adversos sobre o esmalte dentário

The aim of the present study was to assess the effectiveness and adverse effects on dental enamel caused by nightguard vital bleaching with 10% carbamide peroxide. This was accomplished through the interaction of researchers from different areas such as dentistry, materials engineering and physics. Fifty volunteers took part in the doubleblind randomized controlled clinical trial. They were allocated to an experimental group that used Opalescence PF 10% (OPA) and a control group that used a placebo gel (PLA). Fragments of human dental enamel from the vestibular surface of healthy premolars, extracted for orthodontic reasons, were fixed to the vestibular surface of the first upper molars of the volunteers for in situ observation. Bleaching was performed at night for 21 days. The observation periods included Baseline (BL), T0 (21 days), T30 (30 days after treatment) and T180 (180 days after treatment, only for the OPA group). Tooth color was assessed by comparing it with the Vita® scale and by the degree of satisfaction expressed by the volunteer. We also assessed adverse clinical effects, dental sensitivity and gingival bleeding. The study of adverse effects on enamel was conducted in vivo and in situ, using the DIAGNOdent® laser fluorescence device to detect mineral loss. Scanning electron microscopy (SEM) was used to check for superficial morphological alterations, energy dispersive spectrophotometry (EDS) to semiquantitatively assess chemical composition using the Ca/P ratio, and the x-ray diffraction (XRD) technique to observe alterations in enamel microstructure. The results showed that nightguard vital bleaching with 10% carbamide peroxide was effective in 96% of the cases, versus 8% for the PLA group. Dental sensitivity was present in 36% (9/25) of the cases. There was no significant association between gingival bleeding and the type of gel used (p = 1.00). In vivo laser fluorescence analysis showed no difference in values for the control group, whereas in the OPA group there was a statistically significant difference between baseline values in relation to the subsequent periods (p<0.01), with lower mean values for post-bleaching times. There was a significant difference between the groups for times T0 and T30. Micrographic analysis showed no enamel surface alterations related to the treatment performed. No significant alteration in Ca/P ratio was observed in the OPA group (p = 0.624) or in the PLA group (p = 0.462) for each of the observation periods, nor between the groups studied (p=0.102). The XRD pattern for both groups showed the presence of three-phase Hydroxyapatite according to JCPDS files (9-0432[Ca5(PO4)3(OH)], 18-0303[Ca3(PO4)2.xH2O] and 25-0166[Ca5(PO4)3(OH, Cl, F)]). No other peak associated to other phases was found, independent of the group analyzed, which reveals there was no disappearance, nucleation or phase transformation. Neither was there any alteration in peak pattern location. With the methodology and protocol used in this study, nightguard vital bleaching with 10% carbamide peroxide proved to be an effective and safe procedure for dental enamel

Desenvolvimento de um secador spray para obtenção de pós finos de precursores de nióbio

This work presents a spray-dryer designed to oxalate-niobate precursors and suitable for the production of Niobium Carbide. The dryer was intended to produce powders of controlled particle size. First, the precursor is dissolved in water to produce a solution of known concentration and then it is atomized on the spray-dryer to produce the powder. This equipment consists of a 304 stainless steel chamber, 0.48 m x 1.9 m (diameter x length), with a conical shape at the lower portion, which is assembled on a vertical platform. The chamber is heated by three 4 kW electrical resistances. In this process, drying air is heated as it flows inside a serpentine surrounding the chamber, in contrary to more traditional processes in which the hot drying air is used to heat the component. The air enters the chamber at the same temperature of the chamber, thus avoiding adherence of particles on the internal surface. The low speed flow is concurrent, directed from the top to the bottom portion of the chamber. Powders are deposited on a 0.4 m diameter tray, which separates the cylindrical portion from the conical portion of the chamber. The humid air is discharged though a plug placed underneath the collecting tray. A factorial experimental planning was prepared to study the influence of five parameters (concentration, input flow, operation temperature, drying air flow and spray air flow) on the characteristics of the powders produced. Particle size distribution and shape were measured by laser granulometry and scanning electronic microscopy. Then, the powders are submitted to reaction in a CH4 / H2 atmosphere to compare the characteristics of spray-dried powders with powders synthetizided by conventional methods

Extração automática de contornos de telhados usando dados de varredura a laser e campos randômicos de Markov

This paper proposes a methodology for automatic extraction of building roof contours from a Digital Elevation Model (DEM), which is generated through the regularization of an available laser point cloud. The methodology is based on two steps. First, in order to detect high objects (buildings, trees etc.), the DEM is segmented through a recursive splitting technique and a Bayesian merging technique. The recursive splitting technique uses the quadtree structure for subdividing the DEM into homogeneous regions. In order to minimize the fragmentation, which is commonly observed in the results of the recursive splitting segmentation, a region merging technique based on the Bayesian framework is applied to the previously segmented data. The high object polygons are extracted by using vectorization and polygonization techniques. Second, the building roof contours are identified among all high objects extracted previously. Taking into account some roof properties and some feature measurements (e. g., area, rectangularity, and angles between principal axes of the roofs), an energy function was developed based on the Markov Random Field (MRF) model. The solution of this function is a polygon set corresponding to building roof contours and is found by using a minimization technique, like the Simulated Annealing (SA) algorithm. Experiments carried out with laser scanning DEM's showed that the methodology works properly, as it delivered roof contours with approximately 90% shape accuracy and no false positive was verified.

Uso de dados fotogramétricos no refinamento geométrico de contornos de telhados de edifícios extraídos de dados laser

In this paper, a methodology is proposed for the geometric refinement of laser scanning building roof contours using high-resolution aerial images and Markov Random Field (MRF) models. The proposed methodology takes for granted that the 3D description of each building roof reconstructed from the laser scanning data (i.e., a polyhedron) is topologically correct and that it is only necessary to improve its accuracy. Since roof ridges are accurately extracted from laser scanning data, our main objective is to use high-resolution aerial images to improve the accuracy of roof outlines. In order to meet this goal, the available roof contours are first projected onto the image-space. After that, the projected polygons and the straight lines extracted from the image are used to establish an MRF description, which is based on relations ( relative length, proximity, and orientation) between the two sets of straight lines. The energy function associated with the MRF is minimized by using a modified version of the brute force algorithm, resulting in the grouping of straight lines for each roof object. Finally, each grouping of straight lines is topologically reconstructed based on the topology of the corresponding laser scanning polygon projected onto the image-space. The preliminary results showed that the proposed methodology is promising, since most sides of the refined polygons are geometrically better than corresponding projected laser scanning straight lines.

Effect of Ultrasonic Excitation on the Porosity of Glass Ionomer Cement: A Scanning Electron Microscope Evaluation

Background: Ultrasonic excitation (US) was applied to glass ionomer cement (GIC) during early set time to increase the advantageous properties of this material. Purpose: The aim of this in vitro study was to assess the inner porosity of GIC after US. Study design: A total of 16 specimens, for each material, were prepared from high-viscosity GIC Fuji IX GP, Ketac Molar, and Ketac Molar Easymix. Half of these specimens (n = 8) received 30 s of US during the initial cement setting. After completion of the material setting, specimens were fractured and observed by scanning electronic microscopy to quantitatively assay porosity inside the material using Image J software. Results: Statistical data analysis revealed that US reduced the porosity for all tested materials (P <= 0.05). The following reductions (expressed in percentages) were achieved: Fuji IX-from 3.9% to 2.8%; Ketac Molar Easy Mix-from 4.4% to 2.6%, and Ketac Molar-from 2.4% to 1.6%. Conclusion: Under the tested conditions, US was an effective method for porosity reduction inside the material. Microsc. Res. Tech. 74:54-57, 2011. (C) 2010 Wiley-Liss, Inc.

Effect of Er : YAG and diode lasers on the adhesion of blood components and on the morphology of irradiated root surfaces

Objectives: the aim of this study was to evaluate in vitro, by scanning electron microscopy (SEM), the adhesion of blood components on root surfaces irradiated with Er:YAG (2.94 mu m) and GaAlAs Diode (808 nm) lasers and the effects on the morphology of irradiated root surfaces.Methods: One hundred samples of human teeth were obtained. They were previously planed and scaled with manual instruments and divided into five groups of 20 samples each: G1 (control group) - absence of treatment; G2 - Er:YAG laser (7.6 J/cm(2)); G3 - Er:YAG laser (12.9 J/cm(2)); G4 - Diode laser (90 J/cm(2)) and G5 - Diode laser (108 J/cm(2)). After these treatments, 10 samples of each group received a blood tissue but the remaining 10 did not. After laboratory treatments, the samples were obtained by SEM, the photomicrographs were analysed by the score of adhesion of blood components and the results were statistically analysed (Kruskall-Wallis and Mann-Whitney test).Results: In relation to the adhesion of blood components, the study showed no significant differences between the control group and the groups treated with Er:YAG laser (p = 0.9633 and 0.6229). Diode laser radiation was less effective than control group and Er:YAG laser radiation (p < 0.01).Conclusion: None of the proposed treatments increased the adhesion of blood components in a significant way when compared to the control group. Although the Er:YAG laser did not interfere in the adhesion of blood components, it caused more changes on the root surface, whereas the Diode laser inhibited the adhesion.

Comparative scanning electron microscopic study of the effect of different dental conditioners on dentin micromorphology

This study evaluated comparatively by scanning electron microscopy (SEM) the effect of different dental conditioners on dentin micromorphology, when used according to the same protocol. Forty dentin sticks were obtained from 20 caries-free third human molars and were assigned to 4 groups corresponding to 3 conditioners (phosphoric acid 37%, Clearfil SE Bond and iBond) and an untreated control group. After application of the conditioners, the specimens were immersed in 50% ethanol solution during 10 s, chemically fixed and dehydrated to prepare them to SEM analysis. In the control group, dentin surface was completely covered by smear layer and all dentinal tubules were occluded. In the phosphoric acid-etched group, dentin surface was completely clean and presented exposed dentinal tubule openings; this was the only group in which the tubules exhibited the funnel-shaped aspect. In the groups conditioned with Clearfil SE Bond primer and iBond, which are less acidic than phosphoric acid, tubule openings were occluded or partially occluded, though smear layer removal was observed. SE Bond was more efficient in removing the smear layer than iBond. In the Clearfil SE Bond group, the cuff-like aspect of peritubular dentin was more evident. It may be concluded all tested conditioners were able to change dentin morphology. However, it cannot be stated that the agent aggressiveness was the only cause of the micromorphological alterations because a single morphological pattern was not established for each group, but rather an association of different aspects, according to the aggressiveness of the tested conditioner.

Proliferation of the vascular endothelium of the iris following total debridement of the corneal epithelium and limbal excision of rabbits

Background Damage to the corneal epithelium causes not only a reaction for its repair but also affects other parts of the cornea as well as different components of the anterior segment of the eye. The purpose of this investigation was to analyze the consequences, following epithelial and limbal damage, to the iris of rabbits (Oryctolagus cuniculus).Methods The corneal epithelium was thoroughly scraped followed by surgical excision of the limbus. Next, (3)H-thymidine ((3)H-TdR) was injected intravitreally both into the right (experimental) and left (control) eyes which had their anterior segments processed for autoradiography at intervals of 2, 7 and 21 days after surgery (three rabbits per interval). The irises were also examined with scanning-electron and confocal microscopy after Evans blue injection.Results There was a high frequency of labeling in the cells of the iris blood vessels in the experimental eye, particularly the endothelial ones. The ratio of labeled cells between experimental and control irises was 40:1, with a population of nuclei increasing by 25% and remaining labeled up to 21 days. There was also an increase in the volume of the iris vasculature as shown by confocal microscopy. The high labeling frequencies of the vascular cells were observed throughout the iris from the ciliary to the pupillary regions.Conclusions The lesions on the corneal epithelium elicit proliferation of the iris vascular cells, mainly its endothelium, as well as an early breakdown of the blood-aqueous barrier. The daughter cells resulting from the damage to the eye surface were detected up to 21 days after a single injection of (3)H-TdR, most likely due to their slow turnover. As a consequence of this proliferation, the vasculature of the iris increased in volume.