Obtenção de nanopartículas de hexaferrita de bário pelo método pechini

In this study barium hexaferrite was (general formulae BaFe12O19) was synthesized by the Pechini method under different conditions of heat treatment. Precursors like barium carbonate and iron nitrate were used. These magnetic ceramic, with magnetoplumbite type structure, are widely used as permanent magnet because of its excellent magnetic properties, such as: high Curie temperature, good magnetic anisotropy, high coercivity and corrosion resistance. The samples were characterized by thermal analysis (DTA and TG), X- ray Diffraction (XRD), Fourier transform infrared spectroscopy (FTIR), Scanning Electron Microscopy (SEM) end Vibrating sample Magnetometer (VSM). The results confirm the expected phase, which was reinforced according to our analysis. A single phase powder at relatively high temperatures with particle sizes around 100 nm was obtained. The characteristic magnetic behavior one of the phases has been noted (probably superparamagnetic material), while another phase was identified as a ferrimagnetic material. The ferrimagnetic phase showed vortex configuration with two central and slightly inclined plateaus. In general, increase of heat treatment temperature and time, directly influenced the technological properties of the samples

Síntese e caracterização de espinélios a base de Cu, Fe e Cr para pigmentos cerâmicos

Inorganic pigment comprises a host lattice, which is part of the chromophore component (usually a transition metal cation) and possible components modifiers, which stabilize, add or restate the properties pigments. Among the materials with spinel, ferrites, and the chromite stand out, because they have broad technological importance in the area of materials, applicability, pigments, catalytic hydrogenation, thin film, ceramic tiles, among others. The present work, pigments containing CuFe2O4, CuCr2O4,e CuFeCrO4, were synthesized by a method that makes use of gelatin as organic precursor using their application to ceramic pigments. The pigments were characterized by X-ray diffraction (XRD), Infrared spectroscopy, scanning electron microscopy (SEM) spectroscopy in the UV-visible and Colorimetry. The results confirmed the feasibility of the synthetic route used, with respect to powders synthesized, there is the formation of spinel phase from 500°C, with an increase in crystallinity and the formation of other phases. The pigments were shown to be crystalline and the desired phases were obtained. The copper chromite have hues ranging from green to black according to the calcination temperature, while the copper chromite doped with iron had brownish. The ferrites showed copper color and darker brown to black, which may indicate an interesting factor because of the importance of black pigment

Construção, caracterização e aplicação de eletrodos para descarga por arco de cátodo oco

The system built to characterize electrodes and, consequently, deposited fine films are constituted by a hollow cathode that works to discharges and low pressures (approximately 10-3 to 5 mbar), a source DC (0 to 1200 V), a cylindrical camera of closed borossilicato for flanges of stainless steel with an association of vacuum bombs mechanical and spread. In the upper flange it is connected the system of hollow cathode, which possesses an entrance of gas and two entrances for its refrigeration, the same is electrically isolated of the rest of the equipment and it is polarized negatively. In front of the system of hollow cathode there is a movable sample in stainless steel with possibility of moving in the horizontal and vertical. In the vertical, the sample can vary its distance between 0 and 70 mm and, in the horizontal, can leave completely from the front of the hollow cathode. The sample and also the cathode hollow are equipped with cromel-alumel termopares with simultaneous reading of the temperatures during the time of treatment. In this work copper electrodes, bronze, titanium, iron, stainless steel, powder of titanium, powder of titanium and silício, glass and ceramic were used. The electrodes were investigated relating their geometry change and behavior of the plasma of the cavity of hollow cathode and channel of the gas. As the cavity of hollow cathode, the analyzed aspects were the diameter and depth. With the channel of the gas, we verified the diameter. In the two situations, we investigated parameters as flow of the gas, pressure, current and applied tension in the electrode, temperature, loss of mass of the electrode with relationship at the time of use. The flow of gas investigated in the electrodes it was fastened in a work strip from 15 to 6 sccm, the constant pressure of work was among 2.7 to 8 x 10-2 mbar. The applied current was among a strip of work from 0,8 to 0,4 A, and their respective tensions were in a strip from 400 to 220 V. Fixing the value of the current, it was possible to lift the curve of the behavior of the tension with the time of use. That curves esteem in that time of use of the electrode to its efficiency is maximum. The temperatures of the electrodes were in the dependence of that curves showing a maximum temperature when the tension was maximum, yet the measured temperatures in the samples showed to be sensitive the variation of the temperature in the electrodes. An accompaniment of the loss of mass of the electrode relating to its time of use showed that the electrodes that appeared the spherical cavities lost more mass in comparison with the electrodes in that didn't appear. That phenomenon is only seen for pressures of 10-2 mbar, in these conditions a plasma column is formed inside of the channel of the gas and in certain points it is concentrated in form of spheres. Those spherical cavities develop inside of the channel of the gas spreading during the whole extension of the channel of the gas. The used electrodes were cut after they could not be more used, however among those electrodes, films that were deposited in alternate times and the electrodes that were used to deposit films in same times, those films were deposited in the glass substrata, alumina, stainless steel 420, stainless steel 316, silício and steel M2. As the eletros used to deposit films in alternate time as the ones that they were used to deposit in same times, the behavior of the thickness of the film obeyed the curve of the tension with relationship the time of use of the electrode, that is, when the tension was maximum, the thickness of the film was also maximum and when the tension was minimum, the thickness was minimum and in the case where the value of the tension was constant, the thickness of the film tends to be constant. The fine films that were produced they had applications with nano stick, bio-compatibility, cellular growth, inhibition of bacterias, cut tool, metallic leagues, brasagem, pineapple fiber and ornamental. In those films it was investigated the thickness, the adherence and the uniformity characterized by sweeping electronic microscopy. Another technique developed to assist the production and characterization of the films produced in that work was the caloteste. It uses a sphere and abrasive to mark the sample with a cap impression, with that cap form it is possible to calculate the thickness of the film. Through the time of life of the cathode, it was possible to evaluate the rate of waste of its material for the different work conditions. Values of waste rate up to 3,2 x 10-6 g/s were verified. For a distance of the substratum of 11 mm, the deposited film was limited to a circular area of 22 mm diameter mm for high pressures and a circular area of 75 mm for pressure strip. The obtained films presented thickness around 2,1 µm, showing that the discharge of arch of hollow cathode in argon obeys a curve characteristic of the tension with the time of life of the eletrodo. The deposition rate obtained in this system it is of approximately 0,18 µm/min

Adição de nanopartículas de Ti em matriz de Fe através da deposição por magnetron sputtering

Microalloyed steels constitute a specific class of steel with low amount of carbon and microalloying elements such as Vanadium (V), Niobium (Nb) and Titanium (Ti). The development and application of microalloyed steels and steels in general are limited to the handling of powders with particles of submicron or nanometer dimensions. Therefore, this work presents an alternative in order to construction of microalloyed steels utilizing the deposition by magnetron sputtering technique as a microalloying element addiction in which Ti nanoparticles are dispersed in an iron matrix. The advantage of that technique in relation to the conventional metallurgical processes is the possibility of uniformly disperse the microalloying elements in the iron matrix. It was carried out deposition of Ti onto Fe powder in high CH4, H2, Ar plasma atmosphere, with two deposition times. After the deposition, the iron powder with nanoparticles of Ti dispersed distributed, were compacted and sintered at 1120 ° C in resistive furnace. Characterization techniques utilized in the samples of powder before and after deposition of Ti were Granulometry, Scanning Electron Microscopy (SEM), energy-dispersive X-ray spectroscopy (EDX) and X-ray diffraction (DRX). In the case of sintered samples, it was carried out characterization by SEM and Vickers Microhardness assays. The results show which the deposition technique by magnetron sputtering is practicable in the dispersion of particles in iron matrix. The EDX microanalysis detected higher percentages of Ti when the deposition were carried out with the inert gas and when the deposition process was carried out with reactive gas. The presence of titanium in iron matrix was also evidenced by the results of X-ray diffraction peaks that showed shifts in the network matrix. Given these results it can be said that the technique of magnetron sputtering deposition is feasible in the dispersion of nanoparticles of iron matrix in Ti.

Síntese e impregnação de peneiras moleculares Fe MCM-41 derivada de sílica da casca do arroz

The mesoporous molecular sieves of the MCM-41 and FeMCM-41 type are considered promissory as support for metals used as catalysts in oil-based materials refine processes and as adsorbents for environmental protection proposes. In this work MCM-41 and FeMCM41 were synthesized using rice husk ash - RHA as alternative to the conventional silica source. Hydrothermal synthesis was the method chosen to prepare the materials. Pre-defined synthesis parameters were 100°C for 168 hours, later the precursor was calcinated at 550°C for 2 hours under nitrogen and air flow. The sieves containing different proportions of iron were produced by two routes: introduction of iron salt direct synthesis; and a modification post synthesis consisting in iron salt 1 % and 5% impregnation in the material followed by thermal decomposition. The molecular sieves were characterized by X ray diffraction XRD, Fourier transform infrared spectroscopy FT-IR, X ray fluorescence spectroscopy XFR, scanning electronic microscopy SEM, specific surface area using the BET method, Termogravimetry TG. The kinetic model of Flynn Wall was used with the aim of determining the apparent activation energy of the surfactant remove (CTMABr) in the MCM- 41 porous. The analysis made possible the morphology characterization, identifying the presence of hexagonal structure typical for mesoporous materials, as well as observation of the MCM41 and iron of characteristic bands.

Síntese de pigmentos cerâmicos inorgânicos nanométricos e encapsulados com estrutura core-shell pela rota dos precursores poliméricos

The present work has as objective the development of ceramic pigments based in iron oxides and cobalt through the polymeric precursor method, as well as study their characteristics and properties using methods of physical, chemical, morphological and optical characterizations.In this work was used iron nitrate, and cobalt citrate as precursor and nanometer silica as a matrix. The synthesis was based on dissolving the citric acid as complexing agent, addition of metal oxides, such as chromophores ions and polymerization with ethylene glycol. The powder obtained has undergone pre-ignition, breakdown and thermal treatments at different calcination temperatures (700 °C, 800 °C, 900 °C, 1000 °C and 1100 °C). Thermogravimetric analyzes were performed (BT) and Differential Thermal Analysis (DTA), in order to evaluate the term decomposition of samples, beyond characterization by techniques such as BET, which classified as microporous materials samples calcined at 700 ° C, 800 º C and 900 º C and non-porous when annealed at 1000 ° C and 1100 º C, X-ray diffraction (XRD), which identified the formation of two crystalline phases, the Cobalt Ferrite (CoFe2O4) and Cristobalite (SiO2), Scanning Electron Microscopy (SEM) revealed the formation of agglomerates of particles slightly rounded;and Analysis of Colorimetry, temperature of 700 °C, 800 °C and 900 °C showed a brown color and 1000 °C and 1100 °C violet

Estudo da sinterabilidade de ligas de níquel obtidas por meio dos portadores de liga sic, si3n4 ou si metálico com grafita

Nickel alloys are frequently used in applications that require resistance at high temperatures associated with resistance to corrosion. Alloys of Ni-Si-C can be obtained by means of powder metallurgy in which powder mixtures are made of metallic nickel powders with additions of various alloying carriers for such were used in this study SiC, Si3N4 or Si metal with graphite. Carbonyl Ni powder with mean particle size of 11 mM were mixed with 3 wt% of SiC powders with an average particle size of 15, 30 and 50 μm and further samples were obtained containing 4 to 5% by mass of SiC with average particle size of 15 μm. Samples were also obtained by varying the carrier alloy, these being Si3N4 powder with graphite, with average particle size of 1.5 and 5 μm, respectively. As a metallic Si graphite with average particle size of 12.5 and 5 μm, respectively. The reference material used was nickel carbonyl sintered without adding carriers. Microstructural characterization of the alloys was made by optical microscopy and scanning electron microscopy with semi-quantitative chemical analysis. We determined the densities of the samples and measurement of microhardness. We studied the dissociation of carriers alloy after sintering at 1200 ° C for 60 minutes. Was evaluated also in the same sintering conditions, the influence of the variation of average particle size of the SiC carrier to the proportion of 3% by mass. Finally, we studied the influence of variation of the temperatures of sintering at 950, 1080 and 1200 ° C without landing and also with heights of 30, 60, 120 and 240 minutes for sintering where the temperature was 950 °C. Dilatometry curves showed that the SiC sintered Ni favors more effectively than other carriers alloy analyzed. SiC with average particle size of 15 μm active sintering the alloy more effectively than other SiC used. However, with the chemical and morphological analyzes for all leagues, it was observed that there was dissociation of SiC and Si3N4, as well as diffusion of Si in Ni matrix and carbon cluster and dispersed in the matrix, which also occurred for the alloys with Si carriers and metallic graphite. So the league that was presented better results containing Si Ni with graphite metallic alloy as carriers, since this had dispersed graphite best in the league, reaching the microstructural model proposed, which is necessary for material characteristic of solid lubricant, so how we got the best results when the density and hardness of the alloy

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

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

Síntese de nanopartículas de magnetita via decomposição térmica em meio não-aquoso

This work aims at obtaining nanoparticles of iron oxide, the magnetite one (Fe3O4), via synthesis by thermal decomposition through polyol. Thus, two routes were evaluated: a simple decomposition route assisted by reflux and a hydrothermal route both without synthetic air atmosphere using a synthesis temperature of 260ºC. In this work observed the influence of the observe of surfactants which are generally applied in the synthesis of iron oxide nanoparticles decreasing cluster areas. Further, was observed pure magnetite phase without secondary phases generally found in the iron oxide synthesis, a better control of crystallite size, morphology, crystal structure and magnetic behavior. Finally, the introduction of hydroxyl groups on the nanoparticles surface was analyzed besides its employment in the polymer production with OH radicals. The obtained materials were characterized by XRD, DLS, VSM, TEM, TG and DSC analyses. The results for the magnetite obtainment with a particle size greater than 5 nm and smaller than 11 nm, well defined morphology and good magnetic properties with superparamagnetic behavior. The reflux synthesis was more efficient in the deposition of the hydroxyl groups on the nanoparticles surface

Desenvolvimento de membranas porosas de alumina para fins de tratamento de efluente industrial têxtil

Textile production has been considered as an activity of high environmental impact due to the generation of large volumes of waste water with high load of organic compounds and strongly colored effluents, toxic and difficult biodegradability. This thesis deals with obtaining porous alumina ceramic membranes for filtration of textile effluent in the removal of contaminants, mainly color and turbidity. Two types of alumina with different particle sizes as a basis for the preparation of formulation for mass production of ceramic samples and membranes. The technological properties of the samples were evaluated after using sintering conditions: 1,350ºC-2H, 1,450ºC-30M, 1,450ºC-2H, 1,475ºC-30M and 1,475ºC-2H. The sintered samples were characterized by XRD, XRF, AG, TG, DSC, DL, AA, MEA, RL, MRF-3P, SEM and Intrusion Porosimetry by Mercury. After the characterization, a standard membrane was selected with their respective sintering condition for the filterability tests. The effluent was provided by a local Textile Industry and characterized at the entry and exit of the treatment plant. A statistical analysis was used to study the effluent using the following parameters: pH, temperature, EC, SS, SD, oil and grease, turbidity, COD, DO, total phosphorus, chlorides, phenols, metals and fecal coliform. The filtered effluent was evaluated by using the same parameters. These results demonstrate that the feasibility of the use of porous alumina ceramic membranes for removing contaminants from textile effluent with improved average pore size of 0.4 micrometre (distribution range varying from 0,025 to 2.0 micrometre), with total porosity of 29.66%, and average percentages of color removal efficiency of 89.02%, 92.49% of SS, turbidity of 94.55%, metals 2.70% (manganese) to 71.52% (iron) according to each metal and COD removal of 72.80%

Compósitos de matriz metálica à base níquel com adição de TaC e NbC produzidos via metalurgia do pó

Carbide reinforced metallic alloys potentially improve some important mechanical properties required for the overall use of important engineering materials such as steel and nickel. Nevertheless, improved performance is achieved not only by composition enhancement but also by adequate processing techniques, such as novel sintering methods in the case of powder metallurgy. The method minimizes energy losses in addition to providing uniform heating during sintering. Thus, the general objective of this study was to evaluate the density, hardness, flexural strength, dilatometric behavior and to analyze the microstructure of metal matrix composites based nickel with addition of carbides of tantalum and / or niobium when sintered in a conventional furnace and Plasma assisted debinding and sintering (PADS). Initially, were defineds best parameters of granulation, screening and mixing procedure. After, mixtures of carbonyl Ni and 5%, 10% and 15 wt.% NbC and TaC were prepared in a Y-type mixer under wet conditions during 60 minutes. The mixtures were then dried and granulated using 1.5 wt. % paraffin diluted in hexane. Granulates were cold pressed under 600 MPa. Paraffin was then removed from the pressed pellets during a pre-sintering process carried out in a tubular furnace at 500 °C during 30 min. The heating rate was 3 ºC/min. The pellets were then sintered using either a plasma assisted reactor or a conventional resistive tubular furnace. For both methods, the heating rate was set to 8 ºC/min up to 1150 °C. The holding time was 60 minutes. The microstructure of the sintered samples was evaluated by SEM. Brinell hardness tests were also carried out. The results revealed that higher density and higher hardness values were observed in the plasma-assisted sintered samples. Hardness increased with the concentration of carbides in the Ni-matrix. The flexural strength also increased by adding the carbides. The decline was larger for the sample with addition of 5% 5% TaC and NbC. In general, compositions containing added carbide 10% showed less porous and more uniform distribution of carbides in the nickel matrix microstructural appearance. Thus, both added carbide and plasma sintering improved density, hardness, flexural strength and microstructural appearance of the composites

Avaliação do efeito de particulados sólidos na eficiência de um inibidor de corrosão recomendado para meios salinos com CO2

The main problem on the exploration activity on petroleum industry is the formation water resulted on the fields producing. The aggravating of this problem is correlated with the advancing technologies used on the petroleum extractions and on its secondary approach objecting the reobtainment of this oil. Among the main contaminants of the water formation are corrosives gases such as: O2, CO2 and H2S, some solids in suspension and dissolved salts. Concerning to those gases the CO2 is the one that produce significant damage for carbon steel on corrosion process of the petroleum and gas industries. Corrosion inhibitors for carbon steel in formation water is one of the most used agents in control of those damages. In this context, the poor investigations of carbon steel corrosion proceeding from solids in suspension is an opened field for studies. On this work the inhibitor effect of the commercial CORRTREAT 703 was evaluated on some specific solids in suspension at saline medium containing 10.000 ppm of de-aerated chloride using CO2 until non oxygen atmosphere been present. For that, quartz, calcium carbonate, magnetite and iron sulphide were subjected to this investigation as the selected solids. The effect of this inhibitor on corrosion process correlated with those specific solids, was measured using electrochemical (resistance of linear polarization and galvanic pair) and gravimetrical techniques. During all the experimental work important parameters were monitored such as: pH, dissolved oxygen, temperature, instantaneous corrosion rate and galvanic current. According to the obtained results it was proved that the suspension solids calcium carbonate and iron sulphide decrease the corrosion process in higher pH medium. Meanwhile the quartz and magnetite been hardness increase corrosion by broking of the passive layer for erosion. In the other hand, the tested inhibitor in concentration of 50 ppm, showed to be effective (91%) in this corrosion process

Diagnóstico da possível influência da atividade petrolífera em sedimentos de fundo da Bacia Piranhas-Açu, região Baixo Açu/RN

It is located in an area of increasing oil exploration, the region of the Lower Açu is at the mercy of a possible pollution generated by this economic activity, which includes various chemical substances harmful to health, such as metals. This thesis aims to, diagnose the areas of River Piranhas-Açu, a region of the Lower Açu, which are polluted by traces factors and more. In this study, it was determined the concentration of the chemica elements Al, CD, Cr, Cu, Fe, Mn, Ni, P, Pb, V and Zn, through the technique of ICP-OES analysis and the size of sediments and their contents organic matter. Were mapped by GPS, 12 points from collections. The interpretations of the results, together associating that allowed pollution to a possible contamination by oil activity. The results showed tha some regions have low concentrations of cadmium, lead, copper, manganese and zinc unable to promote damage to human health. However, there are places where the concentrations of certain metals chromium, iron and zinc are moderately polluted compared to the results with the reference values of literature and others that are highly polluted by iron. However, due to a greater number of wells in production in those locations, those higher concentrations, it can be suggested a possible influence of oi production in some areas with concentrations of chromium and lead are higher than the rest of the points of monitoring. Moreover, it is observed that the highest levels of metals found in sediment of finer texture and more organic matter content

Estudo de reatores eletroquímicos para remoção de Cu2+ , Zn2+, Fenol e BTEX em água produzida

The production of water has become one of the most important wastes in the petroleum industry, specifically in the up stream segment. The treatment of this kind of effluents is complex and normally requires high costs. In this context, the electrochemical treatment emerges as an alternative methodology for treating the wastewaters. It employs electrochemical reactions to increase the capability and efficiency of the traditional chemical treatments for associated produced water. The use of electrochemical reactors can be effective with small changes in traditional treatments, generally not representing a significant additional surface area for new equipments (due to the high cost of square meter on offshore platforms) and also it can use almost the same equipments, in continuous or batch flow, without others high costs investments. Electrochemical treatment causes low environmental impact, because the process uses electrons as reagent and generates small amount of wastes. In this work, it was studied two types of electrochemical reactors: eletroflocculation and eletroflotation, with the aim of removing of Cu2+, Zn2+, phenol and BTEX mixture of produced water. In eletroflocculation, an electrical potential was applied to an aqueous solution containing NaCl. For this, it was used iron electrodes, which promote the dissolution of metal ions, generating Fe2+ and gases which, in appropriate pH, promote also clotting-flocculation reactions, removing Cu2+ and Zn2+. In eletroflotation, a carbon steel cathode and a DSA type anode (Ti/TiO2-RuO2-SnO2) were used in a NaCl solution. It was applied an electrical current, producing strong oxidant agents as Cl2 and HOCl, increasing the degradation rate of BTEX and phenol. Under different flow rates, the Zn2+ was removed by electrodeposition or by ZnOH formation, due the increasing of pH during the reaction. To better understand the electrochemical process, a statistical protocol factor (22) with central point was conducted to analyze the sensitivity of operating parameters on removing Zn2+ by eletroflotation, confirming that the current density affected the process negatively and the flow rate positively. For economical viability of these two electrochemical treatments, the energy consumption was calculated, taking in account the kWh given by ANEEL. The treatment cost obtained were quite attractive in comparison with the current treatments used in Rio Grande do Norte state. In addition, it could still be reduced for the case of using other alternative energy source such as solar, wind or gas generated directly from the Petrochemical Plant or offshore platforms