Estudo de um compósito Nb-15%pCu obtidos por moagem de alta energia e sinterizados por fase líquida

There is great difficulty in forming a composite refractory metal niobium with copper. This is due to the fact that Nb-Cu system is almost mutually immiscible and may be neglected solubility between them. These properties hinder or prevent obtaining homogeneous and high-density structures, conventionally prepared. This study aims to analyze the use of high-energy milling process (MAE) to implement these natural difficulties, with regard to the densification of the sintered bodies. The MAE and the press were used in the preparation of powders, to obtain a fine and homogeneous distribution of the grain size. Four loads Nb and Cu powders containing 15% by weight of Cu were then milled for MAE in a planetary type ball mill under various milling times and speeds. The results obtained by MAE were analyzed by scanning electron microscopy (SEM), according to the parameters of time and grinding speed. The samples were compacted under pressure of 200 MPa, were then sintered in liquid phase in a vacuum furnace at temperatures of 1100 ° C / 60 min and 1200 ° C / 60 min. Then it was used to characterize diffraction of X-rays to identify the phases. The microstructures of the sintered samples were observed and evaluated using scanning electron microscopy (SEM). Vickers Microhardness tests were performed, obtaining higher values for the sintered bodies in the largest of the post milling times and the larger grinding speeds. It was found that the liquid phase sintering of the samples that were processed by MAE produced at the end of a homogeneous and densified structure in 77,4% relative to the value of the theoretical density of the composite

Sinterização de aço inoxidável reforçado com partículas nanométricas dispersas de carbeto de nióbio - NbC

Metal powder sintering appears to be promising option to achieve new physical and mechanical properties combining raw material with new processing improvements. It interest over many years and continue to gain wide industrial application. Stainless steel is a widely accepted material because high corrosion resistance. However stainless steels have poor sinterability and poor wear resistance due to their low hardness. Metal matrix composite (MMC) combining soft metallic matrix reinforced with carbides or oxides has attracted considerable attention for researchers to improve density and hardness in the bulk material. This thesis focuses on processing 316L stainless steel by addition of 3% wt niobium carbide to control grain growth and improve densification and hardness. The starting powder were water atomized stainless steel manufactured for Höganäs (D 50 = 95.0 μm) and NbC produced in the UFRN and supplied by Aesar Alpha Johnson Matthey Company with medium crystallite size 16.39 nm and 80.35 nm respectively. Samples with addition up to 3% of each NbC were mixed and mechanically milled by 3 routes. The route1 (R1) milled in planetary by 2 hours. The routes 2 (R2) and 3 (R3) milled in a conventional mill by 24 and 48 hours. Each milled samples and pure sample were cold compacted uniaxially in a cylindrical steel die (Ø 5 .0 mm) at 700 MPa, carried out in a vacuum furnace, heated at 1290°C, heating rate 20°C stand by 30 and 60 minutes. The samples containing NbC present higher densities and hardness than those without reinforcement. The results show that nanosized NbC particles precipitate on grain boundary. Thus, promote densification eliminating pores, control grain growth and increase the hardness values

Estudo e desenvolvimento de um capacitor eletrolítico de nióbio

It seeks to find an alternative to the current tantalum electrolytic capacitors in the market due to its high cost. Niobium is a potential substitute, since both belong to the same group of the periodic table and because of this have many similar physical and chemical properties. Niobium has several technologically important applications, and Brazil has the largest reserves, around 96%. There are including niobium in reserves of tantalite and columbite in Rio Grande do Norte. These electrolytic capacitors have high capacitance specifies, ie they can store high energy in small volumes compared to other types of capacitors. This is the main attraction of this type of capacitor because is growing demand in the production of capacitors with capacitance specifies increasingly high, this because of the miniaturization of various devices such as GPS devices, televisions, computers, phones and many others. The production route of the capacitor was made by powder metallurgy. The initial niobium powder supplied by EEL-USP was first characterized by XRD, SEM, XRF and laser particle size, to then be sieved into three particle size, 200, 400 e 635mesh. The powders were then compacted and sintered at 1350, 1450 and 1550°C using two sintering time 30 and 60min. Sintering is one of the most important parts of the process as it affects properties as porosity and surface cleaning of the samples, which greatly affected the quality of the capacitor. The sintered samples then underwent a process of anodic oxidation, which created a thin film of niobium pentóxido over the whole porous surface of the sample, this film is the dielectric capacitor. The oxidation process variables influence the performance of the film and therefore the capacitor. The samples were characterized by electrical measurements of capacitance, loss factor, ESR, relative density, porosity and surface area. After the characterizations was made an annealing in air ate 260ºC for 60min. After this treatment were made again the electrical measurements. The particle size of powders and sintering affected the porosity and in turn the specific area of the samples. The larger de area of the capacitor, greater is the capacitance. The powder showed the highest capacitance was with the smallest particle size. Higher temperatures and times of sintering caused samples with smaller surface area, but on the other hand the cleaning surface impurities was higher for this cases. So a balance must be made between the gain that is achieved with the cleaning of impurities and the loss with the decreased in specific area. The best results were obtained for the temperature of 1450ºC/60min. The influence of annealing on the loss factor and ESR did not follow a well-defined pattern, because their values increased in some cases and decreased in others. The most interesting results due to heat treatment were with respect to capacitance, which showed an increase for all samples after treatment

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

Síntese e caracterização de TaC e óxido misto de tântalo e cobre nanoestruturados a partir do precursor oxálico de tântalo através de reações gás-sólido e sólido-sólido a baixa temperatura

The research and development of nanostructured materials have been growing significantly in the last years. These materials have properties that were significantly modified as compared to conventional materials due to the extremely small dimensions of the crystallites. The tantalum carbide (TaC) is an extremely hard material that has high hardness, high melting point, high chemical stability, good resistance to chemical attack and thermal shock and excellent resistance to oxidation and corrosion. The Compounds of Tantalum impregnated with copper also have excellent dielectric and magnetic properties. Therefore, this study aimed to obtain TaC and mixed tantalum oxide and nanostructured copper from the precursor of tris (oxalate) hydrate ammonium oxitantalato, through gas-solid reaction and solid-solid respectively at low temperature (1000 ° C) and short reaction time. The materials obtained were characterized by X-ray diffraction (XRD), Rietveld refinement, Scanning Electron Microscopy (SEM), Spectroscopy X-Ray Fluorescence (XRF), infrared spectroscopy (IR), thermogravimetric (TG), thermal analysis (DTA) and BET. Through the XRD analyses and the Reitiveld refinement of the TaC with S = 1.1584, we observed the formation of pure tantalum carbide and cubic structure with average crystallite size on the order of 12.5 nanometers. From the synthesis made of mixed oxide of tantalum and copper were formed two distinct phases: CuTa10O26 and Ta2O5, although the latter has been formed in lesser amounts

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

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

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

Adsorção de cobre e cromo utilizando fibra de sisal visando o tratamento da água produzida pela indústria petrolífera

Currently, the oil industry is the biggest cause of environmental pollution. The objective was to reduce the concentration of copper and chromium in the water produced by the oil industry. It was used as adsorbent natural sisal fiber Agave sp treated with nitric acid and sodium hydroxide. All vegetable fibers have physical and morphological properties that enablies the adsorption of pollutants. The basic composition of sisal is cellulose, hemicellulose and lignin. The features are typically found in the characterization of vegetable fibers, except the surface area that was practically zero. In the first stage of adsorption, it was evaluated the effect of temperature and time skeeking to optimize the execution of the factorial design. The results showed that the most feasible fiber was the one treated with acid in five hours (30°C). The second phase was a factorial design, using acid and five hours, this time was it determined in the first phase. The tests were conducted following the experimental design and the results were analyzed by statistical methods in order to optimize the main parameters that influence the process: pH, concentration (mol / L) and fiber mass/ metal solution volume. The volume / mass ratio factor showed significant interference in the adsorption process of chromium and copper. The results obtained after optimization showed that the highest percentages of extraction (98%) were obtained on the following operating conditions: pH: 5-6, Concentration: 100 ppm and mass/ volume: 1 gram of fiber/50mL solution. The results showed that the adsorption process was efficient to remove chromium and copper using sisal fibers, however, requiring further studies to optimize the process.

Valores de referência para cobre e zinco no plasma e no eritrócito em adultos universitários na cidade de Natal-RN

This study aimed builds reference values for copper and zinc, of healthy adults in Natal-RN, and to identify the influence of the gender, age, body mass index (BMI) and diet, on those values. They were assessed 123 healthy students of the Universidade Federal do Rio Grande do Norte (UFRN), both genders, with age between 19 and 41 years. The project was approved by the Ethics Committee in Research of UFRN. BMI was determined and the food consume was accomplished through a 24h recordatory. Dietary was evaluated as the energy, macronutrients, copper and zinc, according to the recommendations of National Academy of Sciences (2001; 2002). Analyses of the copper and zinc concentrations in the plasma and erythrocytes were accomplished by flame atomic absorption spectrometry. The casuistic came quite homogeneous as for the distribution for gender and age, being the largest number of individuals between the 19 and 24 years old. Most of the volunteers presented anthropometric nutritional state inside of the normality patterns. Chronic diseases family antecedents and sedentarysm were observed. Diet was characterized with low consumption of zinc, appropriate of copper and of lipids. Average concentrations of plasma copper (p=0,002), erythrocyte copper (μg/dL, p=0,036; μg/gHb, p=0,038), and plasma zinc (p=0,022) were different among the genders, what was demonstrated by the largest values of copper in the female gender and larger of zinc in the masculine. Plasma copper values still suffered interference of the variables: energy, carbohydrate and copper consumption, all classified in agreement with the median, besides the protein classified according to the percentage contribution for the dietary total energy. The study allowed to establish reference values for erythrocyte zinc (1.261,6-1.344,0 μg/dL e 51,0-54,3 μg/gHb) and to suggest "indicative" of reference values for plasma (108,4 130,2 μg/dL) and erythrocyte (female = 85,0 91,4 μg/dL; masculine = 80,2 86,5 μg/dL) copper and plasma zinc (female = 98,8 105,8 μg/dL; masculine = 104,6 111,6 μg/dL)

Estudo tribológico de biolubrificantes com adição de nanopartículas de óxidos (zinco e cobre)

Currently, vegetable oils have been studied for bio-lubricants base that fits the new environmental standards. Since, in a world full of finite natural resources, mineral oils bring consequences to the environment due to its low biodegradability and toxicity, also it is important to consider that synthetic oils have a high cost The aim of this work is to obtain a biolubricant additived with oxide nanoparticles (ZnO and CuO) for better resistance to friction and wear, which is not toxic to the environment and have better adherence under boundary lubrication. The methodology consisted in the synthesis of bio-lubricants (soybean and sunflower base) by epoxidation reaction. Then, some physical-chemical analysis in bio-lubricants are made to characterize theses lubricants, such as, density, acidity, iodine value, viscosity, viscosity index. Later, the lubricants were additive with nanoparticles. The tribological performance was evaluated by the equipment HFRR (High Frequency Reciprocating Rig) consisting of a wear test ball-plan type. The characterization of wear analysis was performed by SEM / EDS. The results show that bio-lubricants may be synthesized by reaction of epoxidation with good conversion. Tribological point of view, the epoxidized oils are more effective than lubricant additived with the oxide nanoparticles, they had lower coefficients of friction and better rate of film formation in the study. However, because they are environmentally friendly, bio-lubricants gain the relevant importance in tribological field

Remoção do cobre de efluente galvânico aplicando tensoativos derivado de óleos vegetais

Copper is one of the most used metals in platingprocesses of galvanic industries. The presence of copper, a heavy metal, in galvanic effluents is harmful to the environment.The main objective of this researchwas the removal ofcopperfromgalvanic effluents, using for this purpose anionic surfactants. The removal process is based on the interaction between the polar head group of the anionic surfactant and the divalent copper in solution. The surfactants used in this study were derived from soybean oil (OSS), coconut oil (OCS), and sunflower oil (OGS). It was used a copper synthetic solution (280 ppm Cu+2) simulating the rinse water from a copper acid bath of a galvanic industry. It were developed 23and 32 factorial designs to evaluate the parameters that have influence in theremoval process. For each surfactant (OSS, OCS, and OGS), the independent variables evaluated were: surfactant concentration (1.25 to 3.75 g/L), pH (5 to 9) and the presence of an anionic polymer (0 to 0.0125 g/L).From the results obtained in the 23 factorial design and in the calculus for estimatingthe stoichiometric relationship between surfactants and copper in solution, it were developed new experimental tests, varying surfactant concentration in the range of 1.25 to 6.8 g/L (32 factorial design).The results obtained in the experimental designs were subjected to statistical evaluations to obtain Pareto charts and mathematical modelsfor Copper removal efficiency (%). The statistical evaluation of the 23 and 32factorial designs, using saponifiedcoconut oil (OCS), presented the mathematical model that best described the copper removal process.It can be concluded that OCS was the most efficient anionic surfactant, removing 100% of the copper present in the synthetic galvanic solution

Utilização De Polímeros à Base De Acrilamida Na Remoção De Cobre De Meio Aquoso

Environmental Laws and Regulations to dump wastewater are increasingly relevant and, together with pressure from environmentalists, provide awareness of academics in search of solutions. In Brazil, federal law, through Resolution No. 357 of 17/03/05 of the National Environmental Council - CONAMA, in Article 24 deals with the disposal of these effluents. Water pollution with heavy metals is concern because of the difficulty of the treatment and removal from the environment. Copper, for example, is a metallic element and in the form of salt is very soluble in water which dificults its removal. In this context, this study aims to evaluate the extraction of copper with acrylamide polymers through the process of assisted flocculation followed by filtration. Therefore, we used acrylamide polymers, produced by SNF Floerger, with varying degrees of ionicity which is the parameter examined on the extraction of copper. We used the FA polymers FA 920 SH, AH 912 SH, AN 905 SH, AN 910 SH, AN 923 SH, AN 945 SH, AN 956 SH and AN 977 SH, which have anionicities different from each other and growing in that order. The parameters temperature, pH, concentration of the copper solution and stirring speed are fixed. The polymer solution was added to a solution of 200 ppm copper, varying the concentration of polymer. After stirring, an assisted flocculation occurred followed by filtration of the effluent. The filtrate was analyzed by atomic absorption spectrophotometer and the percentage removal of copper ranged from 63 % to 97 %, noting that polymers with higher ionic charge were responsible for the highest percentage of copper extraction. The results of this study showed that these polymers can be applied in the treatment of wastewaters containing metals such as copper

Avaliação cinética e potencial do Nb2O5 obtido a partir de um complexo de nióbio para formação do oleato de metila através da reação de esterificação do ácido oleico

Among the heterogeneous catalysts materials made from niobium show up as an alternative to meet the demand of catalysts for biodiesel production. This study aims to evaluate the potential of a heterogeneous catalyst derived from a complex of niobium in the reaction of methyl esterification of oleic acid. The catalyst was synthesized after calcination at different temperatures of a niobium complex ((NH4)3[NbO(C2O4)3].H2O) generating a niobium oxide nanostructure with a different commercial niobium oxide used to synthesize the complex. The commercial niobium oxide, the complex niobium and niobium catalyst were characterized by thermogravimetry (TG and DTA), surface area analysis (BET), scanning electron microscopy (SEM) and X-ray diffraction (XRD), showing the catalyst has researched morphological and crystallographic indicating a catalytic potential higher than that of commercial niobium oxide characteristics. Factorial with central composite design point, with three factors (calcination temperature, molar ratio of alcohol/oleic acid and mass percentage of catalyst) was performed. Noting that the optimal experimental point was given by the complex calcination temperature of 600°C, a molar ratio alcohol/oleic acid of 3.007/1 and the catalyst mass percentage of 7.998%, with a conversion of 22.44% oleic acid in methyl oleate to 60 min of reaction. We performed a composite linear and quadratic regression to determine an optimal statistical point of the reaction, the temperature of calcination of the complex at 450°C, the molar ratio of alcohol/oleic acid 3.3408/1 and mass percentage of catalyst of 7.6833% . Kinetic modeling to estimate parameters for heterogeneous catalysis it set well the experimental results with a final conversion of 85.01% with 42.38% of catalyst and without catalyst at 240 min reaction was performed. Allowing to evaluate the catalyst catalytic studied has the potential to be used in biodiesel production

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

Complexos metálicos de cobalto, níquel e cobre com a Pirazina-2-carboxamida e 4- hidrazida ácida piridincarboxílica: síntese e caracterização

This work involved the synthesis, characterization and proposing the molecular structure of coordination compounds involving ligands pyrazine-2-carboxamide (PZA) and 4- hydrazide acidic pyridine carboxylic (INH) and metals of the first transition series (M = Co2+, Ni2+ and Cu2+). For the characterization of the compounds used were analytical techniques such as infrared absorption spectroscopy average (FT-IR) molar conductivity measurements, CHN elemental analysis, EDTA Complexometric, measurement of melting point, X-ray diffraction by powder method, Thermogravimetry (TG) and Differential Thermal Analysis (DTA) and Simultaneous Differential Scanning Calorimetry (DSC). The absorption spectra in the infrared region suggested that the ligand coordination to the metal center occurs through the carbonyl oxygen atom and nitrogen alpha pyrazine ring to those complexes formed with PZA. For INH complexes with metal-ligand coordination is through the carbonyl oxygen and nitrogen of the terminal hydrazide grouping. The conductivity measurements of the complexes in aqueous solution they suggest to all behavior of the type 1:2 electrolytes, and conduct of non-electrolytes in acetonitrile. The results obtained by CHN elemental analysis and EDTA Complexometric allowed to infer the stoichiometry of the compounds synthesized. For all of the complexes obtained was possible to record the melting points, neither of which melted near the melting temperature of the free ligands. The X-ray diffraction showed that the complexes of pyrazinamide exhibited diffraction lines, suggesting that these compounds are crystalline, while compounds of isoniazid, with the exception of cobalt, exhibited diffraction lines, indicating that they are crystalline. The results from the TG-DTA and DSC allowed information regarding the dehydration and thermal decomposition of these complexes