Aplicação de tensoativos não iônicos na recuperação de fluidos de perfuração poliméricos

The drilling fluid used to assist in the drilling operation of oil wells, accumulates solids inherent in the formation as it is circulated in the well, interfering in the fluid performance during operation. It is discarded after use. The disposal of these fluids causes one of the most difficult environmental problems in the world. This study aims to promote liquid phase separation of drilling fluids, which have circulated in oil wells, and enable this recovered liquid to formulate a new fluid. For this, non-ionic surfactants were used in order to select the best outcome in phase separation. Five real water-based drilling fluids were utilized, which were collected directly from the fields of drilling oil wells, classified as polymeric fluids. The methodology used consisted in combining the fluid with surfactant and then subjecting it to a process of centrifugation or decantation. The decantating tests were scheduled through experimental planning 23 and 32, using as variables the percentage (%) of surfactant utilized and the stirring time in minutes. The surfactants used were ethoxylated nonylphenol and lauryl alcohol ethoxylated with different degrees of ethoxylation. Phase separation was monitored first by tests of stability, and subsequently by the height of the interface in beakers of 100 mL. The results showed that from the surfactants studied, the lauryl alcohol ethoxylated with 3 ethoxylation units has been the most effective in the phase separation process of the drilling fluids tested. The statistical tool used was of great industrial value regarding the programming phase separation in drilling fluids. In conclusion, the liquid phase separated using surfactant can be reused for a new formulation of drilling fluid with similar properties of a new fluid, assuring its efficiency. And in the resulting analysis it is also suggested that the adsorption is the mechanism that leads the phase separation, with surfactant adsorbing in the active solids

Aspectos dinâmicos da água versus álcool e acetona por técnicas de congelamento

Water still represents, on its critical properties and phase transitions, a problem of current scientific interest, as a consequence of the countless open questions and of the inadequacy of the existent theoretical models, mainly related to the different solid and liquid phases that this substance possesses. For example, there are 13 known crystalline forms of water, and also amorphous phases. One of them, the amorphous ice of very high density (VHDA), was just recently observed. Other example is the anomalous behavior in the macroscopic density, which presents a maximum at the temperature of 277 K. In order to experimentally investigate the behavior of one of the liquid-solid phase transitions, the anomaly in its density and also the metastability, we used three different cooling techniques and, as comparison systems, we made use of the solvents: acetone and ethyl alcohol. The first studied cooling system employ a Peltier plate, a device recently developed, which makes use of small cubes made up of semiconductors to change heat among two surfaces; the second system is a commercial refrigerator, similar to the residential ones. Finally, the liquid nitrogen technique, which is used to refrigerate the samples in a container, in two ways: a very fast and other one, almost static. In those three systems, three Beckers of aluminum were used (with a volume of 80 ml, each), containing water, alcohol and acetone. They were closed and maintained at atmospheric pressure. Inside of each Becker were installed three thermocouples, disposed along the vertical axis of the Beckers, one close to the inferior surface, other to the medium level and the last one close the superior surface. A system of data acquisition was built via virtual instrumentation using as a central equipment a Data-Acquisition board. The temperature data were collected by the three thermocouples in the three Beckers, simultaneously, in function of freezing time. We will present the behavior of temperature versus freezing time for the three substances. The results show the characterization of the transitions of the liquid

Remoção, por flotação, de óleo em águas produzidas na indústria de petróleo: eficiência e modelagem do processo

The separation oil-water by the use of flotation process is characterized by the involvement between the liquid and gas phases. For the comprehension of this process, it s necessary to analyze the physical and chemical properties command float flotation, defining the nature and forces over the particles. The interface chemistry has an important role on the flotation technology once, by dispersion of a gas phase into a liquid mixture the particles desired get stuck into air bubbles, being conduced to a superficial layer where can be physically separated. Through the study of interface interaction involved in the system used for this work, was possible to apply the results in an mathematical model able to determine the probability of flotation using a different view related to petroleum emulsions such as oil-water. The terms of probability of flotation correlate the collision and addition between particles of oil and air bubbles, that as more collisions, better is the probability of flotation. The additional probability was analyzed by the isotherm of absorption from Freundlich, represents itself the add probability between air bubbles and oil particles. The mathematical scheme for float flotation involved the injected air flow, the size of bubbles and quantity for second, the volume of float cell, viscosity of environment and concentration of demulsifier. The results shown that the float agent developed by castor oil, pos pH variation, salt quantity, temperature, concentration and water-oil quantity, presented efficient extraction of oil from water, up to 95%, using concentrations around 11 ppm of demulsifier. The best results were compared to other commercial products, codified by ―W‖ and ―Z‖, being observed an equivalent demulsifier power between Agflot and commercial product ―W‖ and superior to commercial product ―Z‖

Utilização de uma coluna de flotação para remoção de compostos orgânicos da água de produção

Innovative technologies using surfactant materials have applicability in several industrial fields, including petroleum and gas areas. This study seeks to investigate the use of a surfactant derived from coconut oil (SCO saponified coconut oil) in the recovery process of organic compounds that are present in oily effluents from petroleum industry. For this end, experiments were accomplished in a column of small dimension objectifying to verify the influence of the surfactant SCO in the efficiency of oil removal. This way, they were prepared emulsions with amount it fastens of oil (50, 100, 200 and 400 ppm), being determined the great concentrations of surfactant for each one of them. Some rehearsals were still accomplished with produced water of the industry of the petroleum to compare the result with the one of the emulsions. According to the experiments, it was verified that an increase of the surfactant concentration does not implicate in a greater oil removal. The separation process use gaseous bubbles formed when a gas stream pass a liquid column, when low surfactant concentrations are used, it occurs the coalescence of the dispersed oil droplets and their transport to the top of the column, forming a new continuous phase. Such surfactants lead to a gas-liquid interface saturation, depending on the used surfactant concentration, affecting the flotation process and influencing in the removal capacity of the oily dispersed phase. A porous plate filter, with pore size varying from 40 to 250 mm, was placed at the base of the column to allow a hydrodynamic stable operation. During the experimental procedures, the operating volume of phase liquid was held constant and the rate of air flow varied in each experiment. The resulting experimental of the study hydrodynamic demonstrated what the capturing of the oil was influenced by diameter of the bubbles and air flow. With the increase flow of 300 about to 900 cm3.min-1, occurred an increase in the removal of oil phase of 44% about to 66% and the removal kinetic of oil was defined as a reaction of 1° order.

Estudo de duas pseudoligas de Nb-Cu obtidas pela rota da metalurgia do pó

The Nb-Cu pseudoalloys present themselves as potential substitutes for the alloys from a well known system and already commercially applied, as the W-Cu alloys, used in applications such as heat sinks, electrical contacts and coils for the generation of high magnetic fields. Because it is an immiscible system, where there is mutual insolubility and low wettability of the liquid Cu on the Nb surface, the processing route used in this work was the Powder Metallurgy. Two Nb alloys were used, with additions of 10% and 20% in weight of Cu, and times of 20, 30 and 40 hours for the high energy milling of the starting powders. The milling evolution of the powders is presented through the characterization techniques, such as the LASER diffraction for particle size, XRD, SEM, EDS, DSC, dilatometry, TEM and chemical analysis. After the milling, portions of the loads were submitted to the annealing heat treatment. The process used for the samples consolidation was the hot pressing, which has been applied both on some milled powders samples, as on the annealed powders. Subsequent heat treatments were performed in the samples at temperatures of 1000ºC (solid phase) and 1100ºC (in the Cu liquid phase). All sets of consolidated samples, and also the two sets of the heat treated, were analyzed by XRD, SEM, EDS, density and Vickers microhardness. Moreover, other Nb powder samples with 10% and 20% in weight of Cu obtained by simple mechanical mixing, were consolidated, thermally treated and characterized with the same techniques applied to the others, and the results were compared among themselves. Despite the difficulty of consolidation and densification of the two pseudoalloys of the Nb-Cu system of this study, on the route that passes through the HEM, samples were obtained with densities around 90% of the theoretical density. And, on the processing route of which were only mixed, the values reached up to 97%. Therefore, in this work are also emphasized the processes that made possible these results.

Produção de filtrantes ativados a partir de aproveitamento de resíduos: uma proposta para a proteção respiratória ocupacional

A Proteção Respiratória Ocupacional é atualmente uma exigência legal do Ministério do Trabalho e Emprego para garantia da saúde e segurança de milhares de trabalhadores que labutam com exposição habitual a substâncias nocivas que possam ocasionar doenças ocupacionais por inalação de ar contaminado no local de trabalho, cuja principal via de penetração no organismo humano é o Sistema Respiratório. Carvões ativados são materiais obtidos a partir de fontes carbonáceas e utilizados como elemento tecnológico filtrante nos equipamentos destinados a proteção respiratória individual. Fomentada por esse contexto, e visando potencializar conceitos de eco-eficiência e sustentabilidade em produção de materiais, este trabalho destina-se a produção de carvão ativado com potencial filtrante a partir de um rejeito agrícola abundante na região Nordeste do Brasil através de uma rota que favorece carbonização e ativação simultâneas, seguido de neutralização térmica. A biomassa precursora foi caracterizada por Ensaios padrões para determinação do teor de umidade e cinzas, Análise Química Elementar, Análises Térmicas (TG e DSC) e Distribuição Granulométrica por difração a laser. As amostras de carvões ativos sintetizadas foram caracterizadas por Difração de Raios X (DRX), Medidas de área específica por BET, Microscopia Eletrônica de Varredura (MEV), Análise assistida com ultravioleta visível e Redução à Temperatura Programada (TPR) por Amônia. A rota empregada favorece uma tecnologia alternativa para o aproveitamento de resíduos e aplicável para a Proteção Respiratória Ocupacional. A atmosfera de queima influencia diretamente na produção. A temperatura de carbonização variou conforme a estabilidade térmica da amostra. A cristalinidade, morfologia, teor mineralógico, área superficial específica e a adsorção em fase líquida e gasosa variaram em função da interação do resíduo precursor com o tipo e concentração de ácido utilizado. Os ensaios de adsorção demonstraram a efetividade da ativação segundo a rota experimental proposta. O potencial catalítico dos materiais produzidos para uso em máscaras respiratórias foi evidenciado pelo ensaio de TPR. O processo de produção estudado se mostrou eficaz para obtenção dos carvões promovendo processamentos e aplicações mais nobres para materiais cujo uso tem sido restrito a meras aplicações primárias ou descarte, mas cujo potencial tecnológico é amplo, empreendedor, sustentável, viável em escala industrial e de baixo custo.

Avaliação do desempenho da paligorsquita modificada e do carvão da pirólise do lodo de esgoto no processo de degradação fotocatalítica do fenol

The uncontrolled disposal of wastewaters containing phenolic compounds by the industry has caused irreversible damage to the environment. Because of this, it is now mandatory to develop new methods to treat these effluents before they are disposed of. One of the most promising and low cost approaches is the degradation of phenolic compounds via photocatalysis. This work, in particular, has as the main goal, the customization of a bench scale photoreactor and the preparation of catalysts via utilization of char originated from the fast pyrolysis of sewage sludge. The experiments were carried out at constant temperature (50°C) under oxygen (410, 515, 650 and 750 ml min-1). The reaction took place in the liquid phase (3.4 liters), where the catalyst concentration was 1g L-1 and the initial concentration of phenol was 500 mg L-1 and the reaction time was set to 3 hours. A 400 W lamp was adapted to the reactor. The flow of oxygen was optimized to 650 ml min-1. The pH of the liquid and the nature of the catalyst (acidified and calcined palygorskite, palygorskite impregnated with 3.8% Fe and the pyrolysis char) were investigated. The catalytic materials were characterized by XRD, XRF, and BET. In the process of photocatalytic degradation of phenol, the results showed that the pH has a significant influence on the phenol conversion, with best results for pH equal to 5.5. The phenol conversion ranged from 51.78% for the char sewage sludge to 58.02% (for palygorskite acidified calcined). Liquid samples analyzed by liquid chromatography and the following compounds were identified: hydroquinone, catechol and maleic acid. A mechanism of the reaction was proposed, whereas the phenol is transformed into the homogeneous phase and the others react on the catalyst surface. For the latter, the Langmuir-Hinshelwood model was applied, whose mass balances led to a system of differential equations and these were solved using numerical methods in order to get estimates for the kinetic and adsorption parameters. The model was adjusted satisfactorily to the experimental results. From the proposed mechanism and the operating conditions used in this study, the most favored step, regardless of the catalyst, was the acid group (originated from quinone compounds), being transformed into CO2 and water, whose rate constant k4 presented value of 0.578 mol L-1 min-1 for acidified calcined palygorskite, 0.472 mol L-1 min-1 for Fe2O3/palygorskite and 1.276 mol L-1 min-1 for the sludge to char, the latter being the best catalyst for mineralization of acid to CO2 and water. The quinones were adsorbed to the acidic sites of the calcined palygorskite and Fe2O3/palygorskite whose adsorption constants were similar (~ 4.45 L mol-1) and higher than that of the sewage sludge char (3.77 L mol-1).

Avaliação do desempenho da paligorsquita modificada e do carvão da pirólise do lodo de esgoto no processo de degradação fotocatalítica do fenol

The uncontrolled disposal of wastewaters containing phenolic compounds by the industry has caused irreversible damage to the environment. Because of this, it is now mandatory to develop new methods to treat these effluents before they are disposed of. One of the most promising and low cost approaches is the degradation of phenolic compounds via photocatalysis. This work, in particular, has as the main goal, the customization of a bench scale photoreactor and the preparation of catalysts via utilization of char originated from the fast pyrolysis of sewage sludge. The experiments were carried out at constant temperature (50°C) under oxygen (410, 515, 650 and 750 ml min-1). The reaction took place in the liquid phase (3.4 liters), where the catalyst concentration was 1g L-1 and the initial concentration of phenol was 500 mg L-1 and the reaction time was set to 3 hours. A 400 W lamp was adapted to the reactor. The flow of oxygen was optimized to 650 ml min-1. The pH of the liquid and the nature of the catalyst (acidified and calcined palygorskite, palygorskite impregnated with 3.8% Fe and the pyrolysis char) were investigated. The catalytic materials were characterized by XRD, XRF, and BET. In the process of photocatalytic degradation of phenol, the results showed that the pH has a significant influence on the phenol conversion, with best results for pH equal to 5.5. The phenol conversion ranged from 51.78% for the char sewage sludge to 58.02% (for palygorskite acidified calcined). Liquid samples analyzed by liquid chromatography and the following compounds were identified: hydroquinone, catechol and maleic acid. A mechanism of the reaction was proposed, whereas the phenol is transformed into the homogeneous phase and the others react on the catalyst surface. For the latter, the Langmuir-Hinshelwood model was applied, whose mass balances led to a system of differential equations and these were solved using numerical methods in order to get estimates for the kinetic and adsorption parameters. The model was adjusted satisfactorily to the experimental results. From the proposed mechanism and the operating conditions used in this study, the most favored step, regardless of the catalyst, was the acid group (originated from quinone compounds), being transformed into CO2 and water, whose rate constant k4 presented value of 0.578 mol L-1 min-1 for acidified calcined palygorskite, 0.472 mol L-1 min-1 for Fe2O3/palygorskite and 1.276 mol L-1 min-1 for the sludge to char, the latter being the best catalyst for mineralization of acid to CO2 and water. The quinones were adsorbed to the acidic sites of the calcined palygorskite and Fe2O3/palygorskite whose adsorption constants were similar (~ 4.45 L mol-1) and higher than that of the sewage sludge char (3.77 L mol-1).

Estudo da molhabilidade de ligas de adição à base de prata sobre insertos cerâmicos para aplicação em brocas perfuração de poços de petróleo

Metal-ceramic interfaces are present in tricone drill bits with hard ceramic inserts for oil well drilling operations. The combination of actions of cutting, crushing and breaking up of rocks results in the degradation of tricone drill bits by wear, total or partial rupture of the drill bit body or the ceramic inserts, thermal shock and corrosion. Also the improper pressfitting of the ceramic inserts on the bit body may cause its total detachment, and promote serious damages to the drill bit. The improvement on the production process of metal-ceramic interfaces can eliminate or minimize some of above-mentioned failures presented in tricone drill bits, optimizing their lifetime and so reducing drilling metric cost. Brazing is a widely established technique to join metal-ceramic materials, and may be an excellent alternative to the common mechanical press fitting process of hard ceramic inserts on the steel bit body for tricone drill bit. Wetting phenomena plays an essential role in the production of metal/ceramic interfaces when a liquid phase is present in the process. In this work, 72Silver-28Copper eutectic based brazing alloys were melted onto zirconia, silicon nitride and tungsten carbide/Co substrates under high vacuum. Contact angle evolution was measured and graphically plotted, and the interfaces produced were analysed by SEM-EDX. The AgCu eutectic alloy did not wet any ceramic substrates, showing high contact angles, and so without chemical interaction between the materials. Better results were found for the systemns containing 3%wt of titanium in the AgCu alloy. The presence os titanium as a solute in the alloy produces wettable cand termodinamically stable compounds, increasing the ceramics wetting beahviour

Adição de subprodutos da cinza da casca de café (coffea canephora) em massa cerâmica para porcelanato

To produce porcelain tiles fluxing agents are used in order to obtain a liquid phase during firing. This liquid phase fills the pores decreasing porosity, water absorption and contributes to material densification. In the porcelain tiles industry, feldspar is the main flux material used, with quantities ranging between 35 and 50%. Studies focus on the discovery of materials with flux characteristics that can reduce the consumption of feldspar by porcelain tiles industry. In this context, the coffee husk ashes, a residue obtained when coffee husks are burned to produce heat for the dryers during the processing of the green fruit, have as main chemical constituents potassium, calcium and magnesium, giving them characteristics of fluxing material. Brazil is the largest coffee producer in the world and is responsible for over 30% of the world s production. In this work a physical treatment of coffee husk ash was carried out in order to eliminate the organic matter and, after this, two by-products were obtained: residual wastes R1 and R2. Both residues were added separately as single fluxes and also in association with feldspar in mixtures with raw materials collected in a porcelain industry located in Dias d Ávila-Ba. The addition of these residues aimed to contribute to the reduction of the consumption of feldspar in the production of porcelain tiles. Specimens were produced with dimensions of 60 mm x 20 mm x 6 mm in an uniaxial die with compacting pressure of 45 MPa. The samples were heated to a temperature of 1200 °C, for 8 minutes. Tests were performed to characterize the raw materials by XRF, XRD, particle size analysis, DTA and TGA and, additionally, the results of the physical properties of water absorption, apparent porosity, linear shrinkage, density, dilatometry, flexural strength and SEM of sintered body were analyzed. Additions of less than 8% of the residue R1 contributed to the decrease of porosity, but the mechanical strength of the samples was not satisfactory. Additions of 5% the R2 residue contributed significantly to decrease the water absorption and apparent porosity, and also to increase the mechanical strength. Samples with addition of feldspar associated with the R2 residue, in proportions of 6.7% of R2 and 6.7% of feldspar, led to results of water absorption of 0.12% and mechanical strength of 46 MPa, having parameters normalized to the manufacture of porcelain stoneware tiles

Estudo da moagem de alta energia e sinterização de pós compósitos W-Cu

The Tungsten/copper composites are commonly used for electrical and thermal objectives like heat sinks and lectrical conductors, propitiating an excellent thermal and electrical conductivity. These properties are dependents of the composition, crystallite size and production process. The high energy milling of the powder of W-Cu produces an dispersion high and homogenization levels with crystallite size of W very small in the ductile Cu phase. This work discusses the effect of the HEM in preparation of the W-25Cu composite powders. Three techniques of powder preparation were utilized: milling the dry with powder of thick Cu, milling the dry with powder of fine Cu and milling the wet with powder of thick Cu. The form, size and composition of the particles of the powders milled were observed by scanning electron microscopy (SEM). The X-ray diffraction (XRD) was used to analyse the phases, lattice parameters, size and microstrain of the crystallite. The analyse of the crystalline structure of the W-25Cu powders milled made by Rietveld Method suggests the partial solid solubility of the constituent elements of the Cu in lattice of the W. This analyse shows too that the HEM produces the reduction high on the crystallite size and the increase in the lattice strain of both phases, this is more intense in the phase W

Estudo da sinterização de cavacos de aço ferritico

This research studies the sintering of ferritic steel chips from the machining process. Were sintered metal powder obtained from machining process chips for face milling of a ferritic steel. The chip was produced by machining and characterized by SEM and EDS, and underwent a process of high energy mill powder characterized also by SEM and EDS. Were constructed three types of matrixes for uniaxial compression (relation l / d greater than 2.5). The differences in the design of the matrixes were essentially in the direction of load application, which for cylindrical case axial direction, while for the rectangular arrays, the longer side. Two samples were compressed with different geometries, a cylindrical and rectangular with the same compaction pressure of 700 MPa. The samples were sintered in a vacuum resistive furnace, heating rate 20 °C / min., isotherm 1300 °C for 60 minutes, and cooling rate of 25 °C / min to room temperature. The starting material of the rectangular sample was further annealed up to temperature of 800 ° C for 30 min. Sintered samples were characterized by scanning electron microscopy, optical microscopy and EDS. The sample compressed in the cylindrical matrix did not show a regular density reflecting in the sintered microstructure revealed by the irregular geometry of the pores, characterizing that the sintering was not complete, reaching only the second phase. As for the specimen compacted in the rectangular array, the analysis performed by scanning electron microscopy, optical microscopy and EDS indicate a good densification, and homogeneous microstructure in their full extent. Additionally, the EDS analyzes indicate no significant changes in chemical composition in the process steps. Therefore, it is concluded that recycling of chips, from the processed ferritic steel is feasible by the powder metallurgy. It makes possible rationalize raw material and energy by manufacture of known properties components from chips generated by the machining process, being benefits to the environment

Desenvolvimento e validação de método analítico para determinação de teor de ácido gálico e catequina no fitoterápico sanativo® por cromatografia líquida de alta eficiência

The herbal medicine Sanativo® is produced by the Pernambucano Laboratory since 1888 with indications of healing and hemostasis. It is composed of a fluid extract about Piptadenia colubrina, Schinus terebinthifolius, Cereus peruvianus and Physalis angulata. Among the plants in their composition, S. terebinthifolius and P. colubrina have in common phenolic compounds which are assigned most of its pharmacological effects. The tannins, gallic acid and catechin were selected as markers for quality control. The aim of this study was the development and validation of analytical method by HPLC/UV/DAD for the separation and simultaneous quantification of gallic acid (GAC) and catechin (CTQ) in Sanativo®. The chromatographic system was to stationary phase, C-18 RP column, 4,6 x 150 mm (5 mm) under a temperature of 35 ° C, detection at 270 and 210 nm. The mobile phase consisted of 0.05% trifluoroacetic acid and methanol in the proportions 88:12 (v/v), a flow rate of 1 ml/min. The analytical method presented a retention factor of 0.30 and 1.36, tail factor of 1.8 and 1.63 for gallic acid and catechin, respectively, resolution of 18.2, and theoretical plates above 2000. The method validation parameters met the requirements of Resolution n º 899 of May 29, 2003, ANVISA. The correlation coefficient of linear regression analysis for GAC and CTQ from the standard solution was 0.9958 and 0.9973 and when performed from the Sanativo® 0.9973 and 0.9936, the matrix does not interfere in the range 70 to 110 %. The limits of detection and quantification for GAC and CQT were 3.25 and 0.863, and 9.57 and 2.55 mg/mL, respectively. The markers, GAC and CQT, showed repetibility (coefficient of variation of 0.94 % and 2.36 %) and satisfactory recovery (100.02 ± 1.11 % and 101.32 ± 1.36 %). The method has been characterized selective and robust quantification of GAC and CTQ in the Sanativo® and was considered validated

Influência do teor e granulometria da calcita e da temperatura de sinterização no desenvolvimento de massas cerâmicas para revestimento poroso(BIII)

This work aims at studying the influence of the concentration of calcite, its grain size and sintering temperature to obtain porous coating formulations that meet the design specifications. The experiments involved the physical-chemical and mineralogical caracterization of the raw materials, and mechanical tests on specimens dried and sintered, performing a planning mixture and factorial experiment, using the response surface methodology. The ceramic bodies studied were prepared by dry process, characterized, placed in conformity by uniaxial pressing and sintered at temperatures of 940 º C, 1000ºC, 1060ºC, 1120°C and 1180°C using a fast-firing cycle. The crystalline phases formed during sintering at temperatures under study, revealed the presence of anorthite and wolastonite, and quartz-phase remaining. These phases were mainly responsible for the physical and mechanical properties of the sintered especimens. The results shown that as increases the participation of carbonate in the composition of ceramic bodies there is an increase of water absorption and a slight reduction in linear shrinkage for all sintering temperatures. As for the mechanical strength it was observed that it tended to decrease for sintering at temperatures between 940 ° C and 1060 ° C and to increase for sintering at temperatures above 1060 ° C occurring with greater intensity for compositions with higher content of calcite. The resistence decreased with increasing participation of quartz in all sintering temperatures. The decrease in grain size of calcite caused a slight increase in water absorption for formulation with the same concentration of carbonate, remaining virtually unchanged the results of linear shrinkage and mechanical strength. In conclusion, porous ceramic coating (BIII) can be obtained using high concentrations of calcite and keeping the properties required in technical standards and that the particle size of calcite can be used as tuning parameter for the properties of ceramic products.

Síntese, sinterização e caracterização de ferritas à base de Ni-Zn

Were synthesized different ferrites NixZn1-xFe2O4 (0,4 ≤ x ≤ 0,6) compositions by using citrate precursor method. Initially, the precursors citrates of iron, nickel and zinc were mixed and homogenized. The stoichiometric compositions were calcined at 350°C without atmosphere control and the calcined powders were pressed in pellets and toroids. The pressed material was sintered from 1100º up to 1200ºC in argon atmosphere. The calcined powders were characterized by XRD, TGA/DTG, FTIR, SEM and vibrating sample magnetometer (VSM). All sintered samples were characterized using XRD, SEM, VSM and measurements of magnetic permeability and loss factor were obtained. It was formed pure ferromagnetic phase at all used temperatures. The Rietveld analyses allowed to calculate the cations level occupation and the crystallite size. The analyses obtained nanometric crystals (12-20 nm) to the calcined powder. By SEM, the sintered samples shows grains sizes from 1 to 10 μm. Sintered densities (ρ) were measured by the Archimedes method and with increasing Zn content, the bulk density decrease. The better magnetization results (105-110 emu/g) were obtained for x=0,6 at all sintering temperatures. The hysteresis shows characteristics of soft magnetic material. Two magnetization processes were considered, superparamagnetism at low temperature and the magnetic domains formation at high temperatures. The sintered toroids presents relative magnetic permeability (μr) from 7 to 32 and loss factor (tanδ) of about 1. The frequency response of toroids range from 0,3 kHz to 0,2 GHz. The composition x=0,5 presents both greater μr and tanδ values and x=0,6 the most broad range of frequency response. Various microstructural factors show influence on the behavior of μr and tanδ, such as: grain size, porosity across grain boundary and inside the grain, grain boundary content and domain walls movement during the process of magnetization at high frequency studies (0,3kKz 0,2 GHz)