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

Impregnação de metais em xisto retortado para uso como adsorventes

Concern with the environment has lead to an increase in the research for new adsorption techniques, low cost adsorvent materials and with high availability. Many works search the development of higher selectivity modified adsorvents. The Brazil has the second world reserve of oiled shale, because of it, the use of that reject is of great interest. This study has the goal of characterize and analyze the retorted shale, reject of the pirobetuminous shale pyrolysis, and the retorted shale modified through the humid impregnation method, wich the precursors were the metals nitrates ( Cobalt, Nickel and Copper), to the usage has adsorvent materials. The samples were characterized chemically, textually and structurally by the X ray fluorescence (XRF), BET, X ray diffraction (XRD) and scanning electronic microscopy (SEM) techniques. The impregnated samples showed a reduction in the superficial area and in the pore volume when compared with the retorted shale. Besides that, diffractions referred to the impregnated metals where observed in the XRD analysis, wich were the same metals detected in the XRF and SEM analysis. The materials showed homogeneity in it s composition. The results shows that the materials presents adequate adsorption characteristics

Efeito da tecnologia de microondas nas propriedades tecnológicas dos componentes de cerâmica estrutural

O processamento térmico de materiais cerâmicos via energia de microondas, no estágio atual, vem ganhando cada dia mais importância, tendo em vista suas inúmeras aplicações, como por exemplo: aplicação de microondas na área de processamento mineral (aquecimento de minérios antes da moagem, secagem, redução carbotérmica de óxidos minerais, lixiviação, fusão, pré-tratamento de minérios e concentrados de ouro refratário, regeneração de carvão, etc. de acordo com Kigman & Rowson, 1998). Em virtude de uma série de vantagens em potencial, frente aos métodos convencionais de aquecimento, como redução no tempo de processamento; economia de energia; diminuição do diâmetro médio das partículas e melhoramento nas propriedades tecnológicas em geral, esta tecnologia vem se destacando. Neste contexto, o objetivo geral deste trabalho, é desenvolver uma pesquisa visando identificar e caracterizar novas opções de matérias-primas cerâmicas como argilas, feldspatos e caulins que sejam eficazes para definir a formulação de uma ou mais massas para produção de componentes de cerâmica estrutural com propriedades físicas, mecânicas e estéticas adequadas após passarem por sinterização convencional e por energia de microondas destacando as vantagens desta última. Além dos requisitos técnicos e de processo, as formulações apresentadas deverão atender às expectativas de preço e de logística de fornecimento. No estudo foram conformados corpos-de-prova por extrusão e prensagem, sinterizados em fornos microondas e convencional, sob ciclos de queima mais rápidos que os atualmente praticados. As matérias-primas foram caracterizadas e analisadas, utilizando as técnicas de fluorescência por raios X (FRX), difração por raios X (DRX), análise térmica diferencial (DTA), análise térmica gravimétrica (DTG), análise granulométrica (AG), microscopia eletrônica de varredura (MEV), absorção d agua (AA), massa especifica aparente (MEA), porosidade aparente (PA), retração linear (RL) e tensão de ruptura e flexão (TRF). Os resultados obtidos indicaram que as propriedades tecnológicas de Absorção de água (AA) e Tensão de Ruptura e flexão (TRF), proposto no trabalho foram adquiridos com sucesso e estão bem além do limite exigido pelas especificações das normas da ABNT NBR 15.270/05 e 15.310/09

Estudo da adição de resíduo de scheelita em matriz cerâmica: formulação, propriedades físicas e microestrutura

Extractivism mineral is considered an activity highly degrading, due to the large volume of material that he moves in the form of ore and residues. The vast majority of mining companies do not show any technology or economically viable application that will allow the recycling of mineral residue, these being launched in areas receiving located the "open skies" degrade the environment. In Rio Grande do Norte to the production of ceramic red restricts their activities to the production of products such as: solid bricks, ceramic blocks, tiles, among others. Seeking to unite experiences and technical information that favor sustainable development, with important benefits to the construction sector and civil society in general, the present work studies the incorporation of the residue of scheelite in ceramic matrix kaolinitic, coming from the municipality of Boa Saúde - RN, in percentage of 5 %, 10 %, 20 %, 30% 40% and 50 %, by evaluating its microstructure, physical properties and formulation. The raw materials were characterized through the trials of X ray fluorescence, Diffraction of X rays, Differential Thermal Analysis and Termogravimetric Analysis. The samples were formed and fired at temperatures of 850o, 900o, 1000o, 1050o, 1100o, 1150o and 1200 oC, with isotherm of 1 hour and heating rate of 10 oC/min. Assays were performed technological of loss to fire, Water Absorption, Apparent Porosity, Apparent Density, Mass Loss in Fire and Bending Resistance; in addition to the Scanning Electron Microscopy, analyzing their physical and mechanical properties. The use of residue of scheelite in ceramic mass kaolinitic provided a final product with technological properties that meet the technical standards for the production of bricks and roofing tiles, with the percentage of 20% of waste that showed the best results

Estudo da potencialidade da incorporação de resíduo de granito e da queima da casca do café em cerâmica vermelha

The industrial production of ornamental rocks and the burning of coffee husk generate waste that is discarded into the environment. However, with the study of the incorporation of these residues in ceramic products, may be found an alternative to reducing environmental impacts and detrimental effects on human health caused by its indiscriminate disposal of waste in nature. Thus, this work aimed to study the addition of ashes of the coffee husk and granite residue in matrix of red ceramic. The raw materials were dry milled and sieved to mesh 100. To characterize the raw materials were carried out analyzes of X-ray diffraction (XRD), X-ray fluorescence (XRF), particle size analysis (PSA), differential thermal analysis (DTA) and thermogravimetric analysis (TG). Six formulations were prepared where the clay content was kept constant (70%wt) and ashes contents and granite residue varied from 10, 15, 20 and 30%. Dilatometrics analyzes were performed at four selected formulations, containing them: 100% clay (A100); 70% clay and 30% ashes (A70C30); 70% clay and 30% granite residue (A70G30); and 70% clay, 15% granite residue and 15% ashes (A70G15C15). The samples were prepared by uniaxial compaction with pressure of 25 MPa, and fired at temperatures of 800°C, 850ºC, 900ºC, 950ºC, 1000ºC and 1100°C. Assays were performed to determine the linear shrinkage of burning (LSB), water absorption (WA), apparent porosity (AP), density (D) and tensile bending. Also were performed analyzes of X-ray diffraction (XRD) and scanning electron microscopy (SEM) of the samples fired. The formulations incorporating granite residue and/or ashes reached the required limits of water absorption according to NBR 15270-1 and NBR 15310 and tensile bending according to classical literature (SANTOS, 1989) necessary for the production of tiles and ceramic block for masonry sealing

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

Formulação de massas cerâmicas para porcelanas elétricas utilizando resíduos oriundos de corpos de fusíveis

The power industry generates as waste ceramic bodies of electrical fuses that are discarded after use. The formulation of ceramic bodies for porcelain electrical insulators using waste from the bodies fuse allocation promotes environmentally appropriate, through the reuse of the material. This work evaluated the technical feasibility of using waste for use in electrical porcelains with formulations containing the residue, feldspar and kaolinite. The raw materials were processed through grinding and sieving to 200 mesh. The ceramic material obtained from the proposed formulations with 25%, 30%, 34% and 40% of the residue went through a vibratory mill for grinding and homogenization, and then were sieved at 325 mesh. The samples were shaped in a uniaxial press, with the application of 25 MPa and sintered at 1100° C, 1150°C, 1200°C, 1225°C and 1250°C, at levels of 20 and 45 minutes. Were also developed bodies of evidence with reference formulations obtained without residue, to establish a comparison on physical, mechanical and electrical. The tests were conducted and technology: linear shrinkage, porosity, water absorption, resistance to bending to three points, measuring insulation resistance electrical resistivity of the material, X-ray diffraction and X-ray fluorescence Waste characterizations pointed to the existence of two phases: mullite and quartz phases are of great importance in the microstructure of the ceramic and this fact reveals a possibility for reuse in electrical porcelains. The mullite is an important constituent because it is a phase that makes it possible to increase the mechanical strength in addition to the body allows the use at high temperatures. The use of ceramic bodies residue fuses, proved feasible for application in electrical porcelain and the most significant results were obtained by the formulations with 25% waste and sintering at 1200°C

Análise comparativa entre as propriedades do gesso obtido de rejeito da produção de sal e gesso comerciais

The environmental impacts, caused by the solid residues generation, are an often quoted concern nowadays. Some of these residues, which are originated from different human activities, can be fully reused, reducing the effects of the poor waste management on the environment. During the salt production process, the first formed crystals are discarded as industrial waste. This is mainly made of gypsum that is a calcium sulfate dihydrate (CaSO4.2H2O). The gypsum in question may go through a calcination process due to the plaster (CaSO4.0,5H2O) production and then the application on the cement industry. Considering the necessity of development and application for these industrial wastes, this paper aims to analyze the plaster, called Salgesso, from the gypsum that was generated during the salt production, and its use viability on the civil construction industry in order to create environmental and economical benefits. For characterization, the following experiments were performed: X-ray Fluorescence (XRF), X-ray Diffraction (XRD), thermal analysis (TG/DTG) and Scanning Electron Microscopy (SEM) with EDS. The following tests were also performed to obtain the mechanical characteristics: Thinness Modulus, Unit Mass, Setting Time and Compressive Resistance. Three commercial plasters used on civil construction were taken as references. All of these tests were performed according to the current standards. It was noticed that although there were some conflicting findings between the salt and commercial plasters in all of the studied properties, the Salgesso has its values within the standard limits. However, there is the possibility to improve them by doing a more effective calcination process. Three commercial plasters, used in construction, were used as reference material. All tests were performed according to standards in force. It was observed that although some tests present conflicting findings between the salt and gypsum plasters commercial properties in all of the studied Salgesso have values within the limits imposed by the standard, but can be improved simply by calcination process more effective

Formulação de bloco intertravado cerâmico com adição de resíduos urbanos e industriais

The production of waste from urban and industrial activities is one of the factors of environmental contamination and has aroused attention of the scientific community, in the sense of its reuse. On the other hand, the city of Salvador/Ba, with approximately 262 channels, responsible for storm water runoff, produces every year, by the intervention of cleaning and clearing channels, a significant volume of sediments (dredged mud), and thus an appropriate methodology for their final destination. This study aims to assess the influence of incorporation of these tailings in arrays of clay for production of interlocked block ceramic, also known as ceramic paver. All the raw materials from the metropolitan region of Salvador (RMS) were characterized by x-ray fluorescence, x-ray diffraction, thermal analysis (TG and TDA), particle size analysis and dilatometry. With the use of statistical experimental planning technique, ternary diagram was defined in the study region and the analyzed formulations. The specimens were prepared with dimensions of 60x20x5mm³, by uniaxial pressing of 30 MPa and after sintering at temperatures of 900°, 1000º and 1100ºC the technological properties were evaluated: linear shrinkage, water absorption, apparent porosity, apparent specifies mass, flexural rupture and module. For the uniaxial compression strength used cylindrical probe body with Ø 50 mm. The standard mass (MP) was prepared with 90% by weight of clay and 10% by weight of Channel sediment (SCP), not being verified significant variations in the properties of the final product. With the incorporation of 10% by weight of manganese residue (PFM) and 10% by weight of the Ceramic waste (RCB) in the mass default, in addition to adjusting the plasticity due to less waste clay content, provided increased linear firing shrinkage, due the significant concentration of K2O, forming liquid phase at low temperature, contributing to decreased porosity and mechanical resistance, being 92,5 MPa maximum compressive strength verified. After extract test leachate and soluble, the piece containing 10% of the PFM, was classified as non-hazardous and inert material according to NBR10004/04 ABNT. The results showed the feasibility on using waste, SCP, RCB and PFM clay mass, at temperatures above 900ºC, paver ceramic production, according to the specifications of the technical standards, so that to exceed the 10% of the PFM, it becomes imperative to conduct studies of environmental impacts

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

Aplicação de termogravimetria acoplada à espectrometria de massas para caracterização de petróleo e determinação da curva de evolução de gás sulfídrico

With the new discoveries of oil and gas, the exploration of fields in various geological basins, imports of other oils and the development of alternative fuels, more and more research labs have evaluated and characterized new types of petroleum and derivatives. Therefore the investment in new techniques and equipment in the samples analysis to determine their physical and chemical properties, their composition, possible contaminants, especification of products, among others, have multiplied in last years, so development of techniques for rapid and efficient characterization is extremely important for a better economic recovery of oil. Based on this context, this work has two main objectives. The first one is to characterize the oil by thermogravimetry coupled with mass spectrometry (TG-MS), and correlate these results with from other types of characterizations data previously informed. The second is to use the technique to develop a methodology to obtain the curve of evaluation of hydrogen sulfide gas in oil. Thus, four samples were analyzed by TG-MS, and X-ray fluorescence spectrometry (XRF). TG results can be used to indicate the nature of oil, its tendency in coke formation, temperatures of distillation and cracking, and other features. It was observed in MS evaluations the behavior of oil main compounds with temperature, the points where the volatilized certain fractions and the evaluation gas analysis of sulfide hydrogen that is compared with the evaluation curve obtained by Petrobras with another methodology

Quantificação de Fases Cristalinas de Incrustações em Colunas de Produção de Petróleo pelo Método Rietveld

The scale is defined as chemical compounds from inorganic nature, initially soluble in salt solutions, which may precipitate accumulate in columns of production and surface equipment. This work aimd to quantify the crystalline phases of scale through the Rietveld method. The study was conducted in scale derived from columns production wells in development and recipients of pigs. After collecting samples of scale were performed the procedure for separations of inorganic and organic phase and preparation to be analyzed at the X-ray Laboratory. The XRD and XRF techniques were used to monitor whether identifying and quantifying crystalline phases present in the deposits. The SEM technique was used to visualize the morphology of the scales and assess their homogeneity after the milling process. XRD measurements were performed with and without milling and with or without the accessory spinner. For quantify crystalline phases the program DBWStools was used. The procedure for conducting the first refinement was instrumental in setting parameters, then the structural parameters of the phases in the sample and finally the parameters of the function profile used. In the diffraction patterns of samples of scale observed that the best measures were those that passed through the mill and used the accessory spinner. Through the results, it was noted that the quantitative analysis for samples of scale is feasible when need to monitor a particular crystalline phase in a well, pipeline or oil field. Routinely, the quantification of phases by the Rietveld method is hardwork because in many scale was very difficult to identify the crystalline phases present

Avaliação da corrosão em dutos por técnica gravimétrica e de resistência elétrica

With the increasing of demand for natural gas and the consequent growth of the pipeline networks, besides the importance of transport and transfer of oil products by pipeline, and when it comes to product quality and integrity of the pipeline there is an important role regarding to the monitoring internal corrosion of the pipe. This study aims to assess corrosion in three pipeline that operate with different products, using gravimetric techniques and electrical resistance. Chemical analysis of residues originated in the pipeline helps to identify the mechanism corrosive process. The internal monitoring of the corrosion in the pipelines was carried out between 2009 and 2010 using coupon weight loss and electrical resistance probe. Physico-chemical techniques of diffraction and fluorescence X-rays were used to characterize the products of corrosion of the pipelines. The corrosion rate by weight loss was analyzed for every pipeline, only those ones that has revealed corrosive attack were analyzed located corrosion rate. The corrosion potential was classified as low to pipeline gas and ranged from low to severe for oil pipelines and the pipeline derivatives. Corrosion products were identified as iron carbonate, iron oxide and iron sulfide

Efeito da adição de microfibras de lã de vidro na tenacidade à ruptura de pastas de cimento para poços de petróleo

Although there are a wide variety of additives that act in fresh state, to adjust the properties of cement, there is also a search by additions that improve the tenacity of the cement in the hardened state. This, in turn, can often be increased by inserting fibers, which act on the deflection of microcracks. This study aimed to use a microfiber glass wool (silica-based) as an additive reinforcing the cement matrix, improving the rupture tenacity, in order to prevent the propagation of microcracks in the cement sheath commonly found in oil wells submitted to high temperatures. The fibers were added at different concentrations, 2 to 5% (BWOC) and varied average sizes, grinding for 90 s, 180 s, 300 s, 600 s. The cement slurries were made with a density of 1,90 g/ cm3 (15,6 lb/gal), using Portland cement CPP- Special Class as the hydraulic binder and 40% silica flour. The characterization of the fiber was made by scanning electron microscopy (SEM), particle size by sieving, X-ray fluorescence (XRF), X-ray diffraction (XRD) and thermogravimetry (TG / DTG). Were performed technological tests set by the API (American Petroleum Institute) by rheology, stability, free water, compressive strength, as well as testing rupture energy, elastic modulus and permeability. The characterization results showed good thermal stability of the microfiber glass wool for application in oil wells submitted to steam injection and, also, that from the particle size data, it was possible to suggest that microfibers milled up to 300 s, are ideal to act as reinforcement to the cement slurries. The rheological parameters, there was committal of plastic viscosity when larger lengths were inserted of microfiber (F90). The values obtained by free water and stability were presented according to API. The mechanical properties, the incorporation of microfiber to the cement slurries gave better rupture tenacity, as compared to reference cement slurries. The values of compressive strength, elastic modulus and permeability have been maintained with respect to the reference cement slurries. Thus, cement slurries reinforced with microfiber glass wool can ensure good application for cementing oil wells submitted to steam injection, which requires control of microcracks, due to the thermal gradients

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