Influência da adição de cálcio nas propriedades de pastas geopoliméricas destinadas a cimentação de poços de petróleo

Nowadays, the search for new technologies that are able to follow the upcoming challenges in oil industry is a constant. Always trying properties improvements of the used materials, looking for the best performance and greater life time. Besides the search for technologies that show an improvement of performance, the search for materials environmentally correct along the whole production process. In Oil well cementing, this search for new technologies passes through the development of slurry systems that support these requests and that are also environmentally friendly. In this context, the use of geopolymer slurries is a great alternative route to cementing oil wells. Besides having good properties, comparable to Portland cement slurries, this alternative material releases much less CO2 gas in the production of their root materials when compared the production of Portland cement, which releases tons of CO2. In order to improve the properties of geopolymer slurries has been added Calcium Oxide, as observed in other studies that slurries where the Calcium is present the values of compressive strength is greater. The addition has been realized based in the CaO/SiO2 molar ratio of 0.05, 0.10 and 0.15. Have been performed compressive strength tests, thickening time, rheology and fliud loss control test of the slurries, following NBR 9831, as well as the physical chemical characterization of XRD, SEM and TG. Has been observed in most of the tests the slurries follow a tendency until the ratio of 0.10, which inverses in the ratio 0.15. This behavior can be explained by two phenomena that occur simultaneously, the first one is the break of the polymer chains and a consequent increase in molucules mobility, which prevails until the ratio of 0.1, and the second is possible approach of the chains due to the capacity of the calcium ions stabilize the charges of two different aluminum. There is only one linearity in the mechanical behavior that can be attributed to the appereance of the C-S-H phase. Based on this, it is concluded that the phenomenon of breaking the polymer chains predominates until the ratio of 0.1, causing an increase of the filtrate volume, lower rheological parameters and increasing thickening time. From the ratio of 0.15 the approach of the chains predominates, and the behavior is reversed

Utilização de nanosílica como aditivo estendedor para pastas cimentantes de baixa densidade destinadas à cimentação de poços petrolíferos

Cementing operations are conducted at different times of the well s life and they have high importance, because the functions are fundamental to keep good properties during a long life of the well, such as, maintain the mechanical stability of the well, to promote the isolation hydraulic and support the tubing. In some situations, the rocky zones have low fractures pressures and require the use of lightweight slurries to prevent the hydrostatic pressure in the formation is greater than the pressure of fracture. There are three ways to reduce the density of cement slurries: exterders water additives, microspheres and foamed slurries. The most used extender water additive is sodium bentonite, which is a clay with a good capacity of water absorption and expansion of its volume, the main disadvantage of this additive is the reduction of the strength. Currently, the use of nanoscale particles has received special attention, mainly because they get new functionalities. Following this trend, this paper aims to use a colloidal solution of nano-silica as an exterders water additives for use in oil wells. Slurries were designed with fixed 13lb/gal density and concentration of nano silica 0.1 gpc; 0.4 gpc; 0.7 and 1gpc, the influence of nano-silica was studied at these levels in isolation and combined varying concentrations of CaCl2,. Tests including rheology, stability, strength, thickening time, porosity and permeability. Besides the API tests, microstructural characterizations were performed after 28 days of the slurries, X-ray diffraction (XRD) and scanning electron microscopy (SEM)

Otimização do processo de síntese do aluminato de cobalto via método de polimerização de complexos (MPC) através do planejamento fatorial fracionado

In the ceramics industry are becoming more predominantly inorganic nature pigments. Studies in this area allow you to develop pigments with more advanced properties and qualities to be used in the industrial context. Studies on synthesis and characterization of cobalt aluminate has been widely researched, cobalt aluminate behavior at different temperatures of calcinations, highlighting especially the temperatures of 700, 800 and 900° C that served as a basis in the development of this study, using the method of polymerization of complex (CPM), economic, and this method applied in ceramic pigment synthesis. The procedure was developed from a fractional factorial design 2 (5-2) in order to optimize the process of realization of the cobalt aluminate (CoAl2O4), having as response surfaces the batch analysis data of Uv-vis spectroscopy conducted from the statistic software 7.0, for this were chosen five factors as input variables: citric acid (stoichiometric manner), puff or pyrolysis time (h), temperature (° C), and calcinations (° C/min), at levels determined for this study. By applying statistics in the process of obtaining the CoAl2O4 is possible the study of these factors and which may have greater influence in getting the synthesis. The pigments characterized TG/DSC analyses, and x-ray diffraction (XRD) and scanning electron microscope (SEM/EDS) in order to establish the structural and morphological aspects of pigment CoAl2O4, among the factors studied it were found to statically with increasing calcinations temperature 700°< 800 <900 °C, the bands of Uv-vis decrease with increasing intensity of absorbance and that with increasing time of puff or pyrolysis (h) there is an increase in bands of Uv-vis proportionally, the generated model set for the conditions proposed in this study because the coefficient of determination can explain about 99.9% of the variance (R²), response surfaces generated were satisfactory, so it s possible applicability in the ceramics industry of pigments

Síntese de catalisadores do tipo LaNixFe1-xO3 como precursores catalíticos para reação oxidação parcial do metano

Nickel-bases catalysts have been used in several reform reactions, such as in the partial oxidation of methane to obtain H2 or syngas (H2 + CO). High levels of conversion are usually obtained using this family of catalysts, however, their deactivation resulting from carbon deposition still remains a challenge. Different approaches have been tested aiming at minimizing this difficulty, including the production of perovskites and related structures using modern synthesis methods capable of producing low cost materials with controlled microstructural characteristics at industrial scale. To establish grounds for comparison, in the present study LaNixFe1-xO3 (x=0, 0.3 or 0.7) perovskites were prepared following the Pechini method and by microwave assisted self-combustion. All samples were sub sequently calcined at 900 °C to obtain the target phase. The resulting ceramic powders were characterized by thermogravimetric analysis, infrared spectroscopy, X ray diffraction, specific area and temperature programmed reduction tests. Calcined samples were also used in the partial oxidation reaction of methane to evaluate the level of conversion, selectivity and carbon deposition. The results showed that the calcined samples were crystalline and the target phase was formed regardless of the synthesis method. According to results obtained by Rietveld refinement, we observed the formation of 70.0% of LaNi0.3Fe0.7O3 and 30.0% of La2O3 for samples LN3F7-900- P, LN3F7-900-M and 41,6% of LaNi0.7Fe0.3O3, 30.7% of La2NiO4 and 27.7% of La2O3 for samples LN7F3-900-P and LN7F3-900-M.Temperature-programmed profiles of the LaNiO3 sample revealed the presence of a peak around 510 °C, whereas the LaFeO3 sample depicted a peak above 1000°C. The highest l evel of methane conversion was obtained for LaNiO3 synthesized by the Pechini method. Overall, catalysts prepared by the Pechini method depicted better conversion levels compared to those produced by microwave assisted self-combustion

Estudo da incorporação da cal em composições binárias de solo-cimento para produção de tijolos maciços

The use of binders in the soil for the production of solid bricks is an old construction technique that has been used by several civilizations over time. At the same time, the need for environmental preservation and the tendency of scarcity of natural resources make the construction invest in researching new concepts, methods and materials for building systems for the sustainability of their economic activities. Thus arises the need to obtain building materials with low power consumption, capable of reducing the growing housing shortage of rural and urban population. Currently, research has been conducted on this topic to better understand the cementitious and pozzolanic reactions that occur in the formation of the microstructure of the soil-cement when added to other materials such as, for example, lime, and the relationship between microstructure and formed interfaces with the physical, mechanical and chemical analysis in compounds made from these ternary compositions. In this context, this study aimed to analyze the results of the influence of the incorporation of lime to the soil-cement to form a ternary mixture to produce soil-cement bricks and mortar without structural purposes. From the inclusion of contents of 6 %, 8 %, 10% and 12% lime to the soil, and soil-cement mixes in amounts of 2 %, 3 %, 4 % and 5 % were shaped-bodies of -cylindrical specimens to determine the optimum moisture content and maximum dry apparent specific weight. Then they were cured, and subjected to the tests of compressive strength, absorption and durability modified. Compositions obtained the best results in the tests performed on the bodies-of-proof cylindrical served as a parameter for molding of solid bricks, which underwent the same experimental methodology previously cited. The raw materials used, as well as compositions in which the bricks were molded solid, were characterized by physical and chemical tests, X-ray diffraction and scanning electron microscopy. The results obtained in the study indicate that the compositions studied, that showed the best results in terms of compressive strength, water absorption and durability ternary composition was soil, 10 % cement and 2 % lime

Estudo do efeito da adição da escória de aciaria no processamento e propriedades finais de telhas cerâmicas

This research presents an overview of the addition steelwork dust of ceramic shingles in order to contribute to the utilization use of such residue. The ceramic industry perspective in the Brazilian State of Piauí is quite promising. Unlike other productive sectors, the ceramic industry uses basically natural raw materials. Its final products are, in short, the result of transforming clay compounds. These raw materials are composed primarily of aluminum oxide, silicon, iron, sodium, magnesium, end calcium, among others. It was verified that steelwork dust is composed primarily of these same oxides, so that its incorporation in to structural ceramics is a very reasonable idea. Both clay and steelwork powder were characterized by AG, XRF, XRD, TGA and DTA. In addition, steelwork dust samples containing (0%, 5%, 10%, 15%, 20% and 25%) were extruded and burned at 800°C, 850°C, 900°C and 950°C. Then t echnological tests of linear shrinkage, water uptake, apparent porosity, apparent density and flexural strengthwere carried at. The results showed the possibility of using steelwork powder in ceramic shingles until 15% significant improvement in physical and mechanical properties. This behavior shows the possibility of burning at temperatures lower than 850ºC, thus promoting a product final cost reduction

Estudo da viabilidade técnica para obtenção de superfície duplex em aço inoxidável martensítico AISI 410 através do processo de deposição a plasma por gaiola catódica

The technique of plasma nitriding by the cathode cage mainly stands out for its ability to produce uniform layers, even on parts with complex geometries. In this study, it was investigated the efficiency of this technique for obtaining duplex surface, when used, simultaneously, to nitriding treatment and thin film deposition at temperatures below 500°C. For this, were used samples of AISI 41 0 Martensitic Stainless Steel and performed plasma treatment, combining nitriding and deposition of thin films of Ti and/or TiN in a plasma atmosphere containing N2-H2. It was used a cathodic cage of titanium pure grade II, cylindrical with 70 mm diameter and 34 mm height. Samples were treated at temperature 420ºC for 2 and 12 hours in different working pressures. Optical Microscopy (OM), Scanning Electron Microscopy (SEM) with micro-analysis by Energy Dispersive Spectroscopy (EDS), X-Ray Diffraction (XRD), Atomic Force Microscopy (AFM) and analysis of Vickers Microhardness were used to investigate coating properties such as homogeneity and surface topography, chemical composition, layer thickness, crystalline phase, roughness and surface microhardness. The results showed there is a direct proportionality between the presence of H2 in plasma atmosphere and the quantity of titanium in surface chemical composition. It was also observed that the plasma treatment at lowpressure is more effective in formation of TiN thin film

Diagnóstico das espécies ativas do plasma usado em tratamentos termoquímicos do titânio

Plasma diagnostics by Optical Emission Spectroscopy were performed for electrical discharge in three gas mixture respecting the combinations z N2 y Ar x H2, z N2 y Ar x O2 e z N2 y Ar x CH4, in which the indexes z and y systematically vary from 1 to 4 and x varies from 0 to 4, every one has dimension SCCM, resulting in 80 combinations. From the all obtained spectrums, the species CH (387,1 nm), N2+ (391,4 nm), Hβ (486,1 nm), Hα (656,3 nm), Ar (750,4 nm), O (777,4 nm) e O (842,6 nm) were analyzed because of their abundance and importance on the kinetic of reaction from the plasma to surface, besides their high dependences on the gases flows. Particularly interesting z, y and x combinations were chosen in order to study the influence of active species on the surface modification during the thermochemical treatment. From the mixtures N2 Ar O2 e N2 Ar CH4 were chosen three peculiar proportions which presented luminous intensity profile with unexpected maximum or minimum values, denominated as plasma anomaly. Those plasma concentrations were utilized as atmosphere of titanium treatment maintaining constant the control parameters pressure and temperature. It has been verified a relation among luminous intensity associated to N2+ and roughness, nanohardness and O atoms diffusion into the crystalline lattice of treated titanium and it has been seen which those properties becomes more intense precisely in the higher points found in the optical profile associated to the N2+ specie. Those parameters were verified for the mixture which involved O2 gas. For the mixture which involves CH4 gas, the relation was determinate by roughness, number of nitrogen and carbon atoms diffused into the titanium structure which presented direct proportionality with the luminous intensity referent to the N2+ and CH. It has been yet studied the formation of TiCN phases on the surface which presented to be essentially directly proportional to the increasing of the CH specie and inversely proportional to the increasing of the specie N2+

Estudo sobre a redução aluminotérmica de Ta2O5 e TiO2 usando descarga de cátodo oco

In this study it was used two metallic oxides, Ta2O5 and TiO2, in order to obtain metallic powders of Ta and Ti through aluminothermic reduction ignited by plasma. Ta2O5 and TiO2 powders were mixed with Al in a planetary mill, using different milling times. A thermal analysis study (DTA and TG) was carried out, in order to know the temperature to react both the mixtures. Then, these mixtures were submitted to a hollow cathode discharge, where they were reacted using aluminothermic reduction ignited by plasma. The product obtained was characterized by XRD and SEM, where it was proven the possibility of producing these metallic particles, different from the conventional process, where metallic ingots are obtained. It was verified that the aluminothermic reduction ignited by plasma is able to produce metallic powders of Ta and Ti, and a higher efficiency was observed to the process with Ta2O5-Al mixtures. Among different microstructural aspects observed, it can be noted the presence of metallic nanoparticles trapped into an Al2O3 matrix, besides acicular structures (titanium) and dendritic structures (tantalum), which are a product characteristic from a fast cooling

Síntese, aplicação e avaliação do efeito do teor de fósforo da celulose fosfatada em argamassa de alvenaria com aditivo comercial a base de hidroxi-etil-metil celulose (HEMC)

Generally, cellulose ethers improves mortar properties such as water retention, workability and setting time, along with adherence to the substrate. However, a major disadvantage of the addition of cellulose ethers in mortars is the delay in hydration of the cement. In this paper a cellulose phosphate (Cp) was synthesized water soluble and has been evaluated the effect of their incorporation into mortar based on Portland cement. Cellulose phosphate obtained was characterized by spectrophotometry Fourier transform infrared (FTIR), X-ray diffraction (XRD), elemental analysis and scanning electron microscopy (SEM). Mortar compositions were formulated with varying phosphorus content in cellulose and cellulose phosphate concentrations, when used in partial or total replacement of the commercial additive based hydroxyethyl methyl cellulose (HEMC). The mortars formulated with additives were prepared and characterized by: testing in the fresh state (consistency index, water retention, bulk density and air content incorporated) and in the hardened state (absorption by capillarity, density, flexural and compression strength). In mixtures the proportion of sand:cement of 1:5 (v / v) and factor a / c = 1.31 and water were held constant. Overall, the results showed that the celluloses phosphates employed in mortars added acted significantly when partially substituting the commercial additive. With regard to consistency index, water retention and bulk density in the fresh state and absorption by capillarity and bulk density apparent in the hardened state, showed no appreciable differences as compared to the commercial additive. The incorporated air content in the fresh state reduced markedly, but did not affect other properties. The mortars with cellulose phosphate, partially replacing the commercial additive showed an improvement of the properties of flexural strength and compressive strength

Efeito da adição de feldspato e/ou resíduo de caulin em formulações à base de argila ilítica

The red pottery industry in Piauí state is well developed and stands out at the national context for the technical quality of its products. The floor and wall tile industry, however, is little developed since the state has only one company that produces red clay-based ceramic tiles. This thesis aims at using the predominantly illitic basic mass of the above mentioned industry, with the addition of feldspar and/or kaolin residue in order to obtain products of higher technical quality. Kaolin residue consists basically of kaolinite, muscovite mica and quartz; the feldspar used was potassic. In this experiment, basic mass (MB) was used for experimental control and fifteen formulations codified as follows: F2, F4, F8, F16, F32, FR2, FR4, FR8, FR16, FR32, R2, R4, R8, R16 and R32. All raw materials were dry-milled, classified, formulated and then humidified to 10% water. Thereafter, test samples were produced by unixial pressing process in a rectangular steel matrix (60.0 x 20.0 x 5.0) mm3 at (25 MPa). They were fired at four temperatures: 1080°C, 1120°C, 1160°C, with a heating rate of 10°C/min during up to 10 min in an electric oven, and the last one in an industrial oven with a peak of 1140°C, aim ing to confirm the results found in laboratory and, finally, technological tests were performed: MEA, RL, AA, PA, TRF and PF. The results revealed that the residue under study can be considered a raw material with large potential in the industry of red clay-based ceramic tiles, since the results found both in laboratory and in the industry have shown that the test samples produced from the formulations with up to 4% feldspar and those produced with up to 8% feldspar and residue permitted a reduction in the water absorption rate and an increase in the mechanical resistance while those samples produced with up to 4% residue had an increase in the mechanical resistance when compared to those produced from the basic mass and that the formulation with 2% feldspar and residue presented the best technological properties, lowering the sintering temperature down to 1120°C

Simulador radiográfico antropomórfico de mama humana

Mammography is a diagnostic imaging method in which interpretation depends on knowledge of radiological aspects as well as the clinical exam and pathophysiology of breast diseases. In this work a mammography phantom was developed to be used for training in the operation of mammographic x-ray equipment, image quality evaluation, self-examination and clinical examination of palpation. Polyurethane was used for the production of the phantoms for its physical and chemical properties and because it is one of the components normally used in prostheses. According to the range of flexibility of the polyurethane, it was possible to simulate breasts with higher or lower amount of adipose tissue. Pathologies such as areolar necrosis and tissue rejection due to surgery reconstruction after partial mastectomy were also simulated. Calcifications and nodules were simulated using the following materials: polyethylene, poly (methyl methacrylate), polyamide, polyurethane and poly (dimethyl silicone). Among these, polyethylene was able to simulate characteristics of calcification as well as breast nodules. The results from mammographic techniques used in this paper for the evaluation of the phantoms are in agreement with data found in the literature. The image analyses of four phantoms indicated significant similarities with the human skin texture and the female breast parenchyma. It was possible to detect in the radiographic images produced regions of high and low radiographic optical density, which are characteristic of breasts with regions of different amount of adipose tissue. The stiffnesses of breast phantoms were adjusted according to the formulation of the polyurethane which enabled the production of phantoms with distinct radiographic features and texture similar to human female breast parenchyma. Clinical palpation exam of the phantoms developed in this work indicated characteristics similar to human breast in skin texture, areolar region and parenchyma

Tratamentos de fibras de carnaúba [copernicia prunífera (miller) h. e. moore] para o desenvolvimento de compósito biodegradável com matriz de polihidroxibutirato

The use of raw materials from renewable sources for production of materials has been the subject of several studies and researches, because of its potential to substitute petrochemical-based materials. The addition of natural fibers to polymers represents an alternative in the partial or total replacement of glass fibers in composites. In this work, carnauba leaf fibers were used in the production of biodegradable composites with polyhydroxybutyrate (PHB) matrix. To improve the interfacial properties fiber / matrix were studied four chemical treatments to the fibers..The effect of the different chemical treatments on the morphological, physical, chemical and mechanical properties of the fibers and composites were investigated by scanning electron microscopy (SEM), infrared spectroscopy, X-ray diffraction, tensile and flexural tests, dynamic mechanical analysis (DMA), thermogravimetry (TGA) and diferential scanning calorimetry (DSC). The results of tensile tests indicated an increase in tensile strength of the composites after the chemical treatment of the fibers, with best results for the hydrogen peroxide treated fibers, even though the tensile strength of fibers was slightly reduced. This suggests a better interaction fiber/matrix which was also observed by SEM fractographs. The glass transition temperature (Tg) was reduced for all composites compared to the pure polymer which can be attributed to the absorption of solvents, moisture and other low molecular weight molecules by the fibers

Uso de resíduo e de minerais de pegmatito da região do seridó RN e de argilas portuguesas em formulações de grês porcelanato

In the State Rio Grande do Norte, Brazil, the most significant deposits of minerals in the production of granite and pegmatite are Seridó region. Municipalities of Parelhas and Equador are the main responsible for the production of feldspar, quartz, kaolin and granite. The ceramic industries are always in search of competitiveness by investing in new products or improving existing techniques. The stoneware is a type of pottery that stands in the market because it presents technical and aesthetic characteristics superior to other existing products. Characteristics of the raw materials initially obtained with chemical analysis and mineralogical analysis are crucial in getting a product that satisfies the conditions in a manufacturing process and is, in principle, directly related to the firing cycle. This research aimed at developing new formulations for the mass production of ceramic stoneware. The raw materials initially characterized were feldspar, quartz, kaolin and granite. As part of the research was developed at the University of Aveiro, in Portugal, we used two clays used in the production of Portuguese ceramics. The raw material Brazilian and Portuguese and the final product, both in Portugal and Brazil, were analyzed for X-ray fluorescence, X-ray diffraction, granulometric analysis, dilatometric analysis, thermal analysis and analysis of scanning electron microscopy (MEV). The specimens prepared at the University of Aveiro (DECV) were sintered at 10000C and 12000C and the specimens prepared in UFRN were sintered at 10000C, 10500C, 11000C, 11500C, 12000C, 12500C and 13000C, but the best results and demonstrating the presence of the mineral mullite were at temperatures of 12000C, 12500C and 13000C. The results showed that the granite waste used may be considered raw material of excellent quality for use in the ceramic industry and coating floors and more accurately by the industry of stoneware. Physical and mechanical tests conducted on samples of the formulations F01 and F02 developed in UFRN showed a water absorption and mechanical strength suitable for the stoneware

Efeito da incorporação de diatomita na estabilidade e permeabilidade de compósitos cimentíceos espumados aplicados a poços de petróleo

Lightweight oilwell cement slurries have been recently studied as a mean to improve zonal isolation and sheath-porous formation adherence. Foamed slurries consisting of Portland cement and air-entraining admixtures have become an interesting option for this application. The loss in hydrostatic pressure as a consequence of cement hydration results in the expansion of the air bubbles entrapped in the cement matrix, thus improving the sheath-porous formation contact. Consequently, slurries are able to better retain their water to complete the hydration process. The main objective of the present study was to evaluate the effect of the addition of an air-entraining admixture on the density, stability and permeability of composite slurries containing Portland cement and diatomite as light mineral load. Successful formulations are potential cementing materials for low fracture gradient oilwells. The experimental procedures used for slurry preparation and characterization were based on the American Petroleum Institute and ABNT guidelines Slurries containing a pre-established concentration of the air-entraining admixture and different contents of diatomite were prepared aiming at final densities of 13 to 15 lb/gal. The results revealed that the reduction of 15 to 25% of the density of the slurries did not significantly affect their strength. The addition of both diatomite and the air-entraining admixture increased the viscosity of the slurry providing better air-bubble retention in the volume of the slurry. Stable slurries depicted bottom to top density variation of less than 1.0 lb/gal and length reduction of the stability sample of 5.86 mm. Finally, permeability coefficient values between 0.617 and 0.406 mD were obtained. Therefore, lightweight oilwell cement slurries depicting a satisfactory set of physicochemical and mechanical properties can be formulated using a combination of diatomite and air-entraining admixtures for low fracture gradient oilwells