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

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

Sinterização de matrizes cerâmicas à base de alumina reforçadas por carbetos a partir de precursores poliméricos

Ceramic composites produced with polymerics precursors have been studied for many years, due to the facility of obtaining a complex shape, at low temperature and reduces cost. The main objective of this work is to study the process of sintering of composites of ceramic base consisting of Al2O3 and silicates, reinforced for NbC, through the technique of processing AFCOP, as well as the influence of the addition of LZSA, ICZ and Al as materials infiltration in the physical and mechanical properties of the ceramic composite. Were produced ceramic matrix composites based SiCxOy e Al2O3 reinforced with NbC, by hidrosilylation reaction between D4Vi and D1107 mixtured with Al2O3 as inert filler, Nb and Al as reactive filler. The specimens produced were pyrolised at 1200, 1250 and 1400°C and infiltred with Al, ICZ and LZSA, respectively. Density, porosity, flexural mechanical strength and fracture surface by scanning electron microscopy were evaluated. The microstructure of the composites was investigated by X-ray diffraction to identify the presence of crystalline phases. The composites presented apparent porosity varying of 31 up to 49% and mechanical flexural strength of 14 up to 34 MPa. The infiltration process improviment of the densification and reduction of the porosity, as well as increased the values of mechanical flexural strength. The obtained phases had been identified as being Al3Nb, NbSi2, Nb5S3, Nb3Si and NbC. The samples that were submitted the infiltration process presented a layer next surface with reduced pores number in relation to the total volume

Obtenção de cerâmicas à base de tricálcio fosfatos utilizando óxido de manganês como aditivo

The calcium phosphate ceramics have been very investigated as material for bone implants. The tricalcium phosphate (β-TCP) had a great potential for application in temporary implants like a resorbable bioceramic. This material presents a limitation in its sintering temperature due to occurrence of the allotropic transformation β → α at temperatures around 1200°C, not allowing the attainment of dense ceramic bodies. This transformation also causes cracks, what diminishes the mechanical strength, limiting its use to applications of low mechanical requests. This work studies the influence of the addition of manganese oxide in the sintering of β-TCP. Two processing routes were investigated. The first was the powder metallurgy conventional process. The test bodies (samples) were pressed and sintering at temperatures of 1200 and 1250°C. The second route was uniaxial hot pressing and its objective was to obtain samples with high relative density. The samples were physically characterized through density and porosity measurements. The thermal behavior was studied through dilatometric, thermal differential and thermogravimetric analysis. The mechanical properties were characterized by three point flexure test and Vickers microhardness measurements. The microstructure was analyzed by scanning electron microscopy. The addition of manganese oxide caused an improvement of the mechanical strength in relation to the material without additive and promoting the stabilization of β-TCP to greater temperatures

Estudo do efeito da substituição de caulim por resíduo de caulim na fabricação de cerâmica de revestimento

Companies involved in kaolin mining and treatment represent an important area of industrial development in Brazil, significantly contribution to the worldwide production of such mineral. As a result, large volumes of kaolin residue are constantly generated and abandoned in the environment, negatively contributing to its preservation. In this scenario, the objective of the present study was to characterize the residue generated from kaolin mining as well as to assess its potential use as raw material for the production of ceramic tiles. Ceramic mixtures were prepared from raw materials characterized by X-ray fluorescence, X-ray diffraction, particle size analysis and thermal analysis. Three compositions were prepared using kaolin residue contents of 10%, 20% and 30%. Samples were uniaxially pressed, fired at 1200ºC and characterized aiming at establishing their mineralogical composition, water absorption, apparent porosity, specific mass, linear retraction and modulus of rupture. The results showed that the residue basically consisted of kaolinite and successfully replaced raw kaolin in the preparation of ceramic title formulations without significantly affecting the properties of the fired material

Utilização de resíduos de rochas ornamentais na produção de cerâmica branca

The marble and granite waste come from the process of mining of those ornamental rocks for use in the building industry. Brazil is one of the largest producers of blocks or finished products of ornamental rocks, extracting about 5.2 tons / year. The largest national producers are the states of Espírito Santo, Minas Gerais and Bahia which account for 80% of the Brazilian production. However, the waste total amount during processing of these blocks reaches 40% of the total. The use of the waste produced by this industry in white ceramics could be a form of disposition, because these materials, are thrownasa mud directly at decantation ponds, wastelands or in rivers, without any treatment. The present work has as main purpose to study the influence that reject of the ornamental rocks on the physical and mechanical properties of white ceramics. X-Ray characterizations of raw materials by were performed X-Ray fluorescence, X-Ray diffraction, granulometric, thermogravimetric and thermodiferencial analysis, five formulations were made (0, 10, 20, 30, 40% in granite weight) wich were burned at three temperatures: 1100°C, 1150°C and 1200ºC with 60 minutes of sorling time. After sintering, the samples were submitted to different analyser absorption of water, linear retraction, apparent porosity, apparent specific mass, flexival stronght, and scanning were obtained microscopy. Compatible technological properties within the limits demanded for the production of porcelainized stoneware

Aproveitamento de resíduos de cinza da cana de açúcar em massas cerâmicas

This study aimed to investigate the use of cane sugar ashes from small-scale stills of Eunápolis region, state of Bahia, in pottery mass that can be developed as porcelain stoneware. Bahia is the second largest producer of rum distillery in Brazil. In the production of rum is produced residue called bagasse, which is used to generate electricity in Power plants and in the distillery itself, generating ashes as residue, which is played in nature, causing environmental damage. We studied 5 (five) formulations of 0% 10% 20%, 30% and 40% by weight of the ash, without ignition and 3 (three) formulations of 10%, 20% and 30% with gray ash temperature of 1250ºC. The formulation at 0% by weight of ash was used for a comparison between the traditional mass of porcelain stoneware and the masses with the addition of ash calcined, replacing feldspar. The percentage by weight of kaolin and of Clay was kept the same, 30%, and all raw materials were derived from the state of Bahia. The samples were made in uniaxial array with dimensions of (60 x 20 x 5) mm and compressed to a pressure of 45 MPa. Assays were performed to characterize the raw by X-ray fluorescence, X-ray diffraction, ATD and ATG and Dilatometric analysis. The samples were sintered at temperatures of 1100°C, 1150°C, 1200°C and 1250°C, for the specimens with the ashes without ash and 1150° C and 1200° C for specimens with the gray level of calcined 60 minutes. and then we made a cooling ramp with the same rate of warming until reach ambient temperature. The sintered bodies were characterized by water absorption, porosity, linear shrinkage, bending strength and XRD of the fracture surface and the results analyzed. It was proven, after results of tests performed, that it is possible to use the ash residue of sugar cane bagasse on ceramic coating with the addition of up to 10% wt of the residue ash

Estudo do potencial de utilização do resíduo da extração de esmeraldas na fabricação de cerâmica de revestimento

Companies involved in emerald mining and treatment represent an important area of industrial development in Brazil, with significative contribution to the worldwide production of such mineral. As a result, large volumes of emerald waste are constantly generated and abandoned in the environment, negatively contributing to its preservation. By the other side the interest of the use of mining waste as additive in ceramic products has been growing from researchers in recent years. The ceramic industry is constantly seeking to the marked amplification for the sector and perfecting the quality of the products and to increase the variety of applications. The technology of obtaining of ceramic tiles that uses mining residues assists market niches little explored. In this scenario, the objective of the present study was to characterize the residue generated from emerald mining as well as to assess its potential use as raw material for the production of ceramic tiles. Ceramic mixtures were prepared from raw materials characterized by X-ray fluorescence, X-ray diffraction, particle size analysis and thermal analysis. Five compositions were prepared using emerald residue contents of 0%, 10%, 20%, 30% and 40%. Samples were uniaxially pressed, fired at 1000, 1100 and 1200ºC and characterized aiming at establishing their mineralogical composition, water absorption, apparent porosity, specific mass, linear retraction and modulus of rupture. The results shows that the emerald residue, basically consisted of 73% of (SiO2 + Al2O3) and 17,77% of (MgO + Na2O+ K2O) (that facilitates sintering), can be added to the ceramic tile materials with no detrimental effect on the properties of the sintered products

Obtenção de compósitos cerâmicos reforçados com carbetos refratários a partir de precursores poliméricos

In this work, were produced ceramic matrix composites based in SiCxOy e Al2O3 reinforced with NbC, by hydrosilylation reaction between D4Vi and poly(methylhydrosiloxane) mixtured with Al2O3 as inert filler, Nb and Al as reactive filler. After the mixture and compactation at 80ºC (warm pressing), the samples were pyrolised at 1200 and 1400ºC and infiltred with ICZ and LZSA respectively, and thermically, physical and structurally characterized by X-ray diffraction, density and porosity, flexural mechanical strength and fracture surface by scanning electron microscopy. The yield ceramic obtained after pyrolysis for studied composition at 1200ºC was 95%. The obtained phases had been identified as being Al3Nb, NbSi2 and NbC. The composite material presented apparent porosity varying of 15 up to 32% and mechanical flexural strenght of 32 up to 37,5MPa. After the fracture surface analysis, were observed a phases homogeneous dispersion, with some domains of amorphous and crystalline aspect. The samples that were submitted the infiltration cycle presented a layer next the surface with reduced pores number in relation to the total volume

Síntese citrato-hidrotermal e caracterização eletroquímica de LSCF para aplicação como catodo em célula a combustível de temperatura intermediária

The lanthanum strontium cobalt iron oxide (La1-xSrxCo1-yFeyO3 LSCF) is the most commonly used material for application as cathode in Solid Oxide Fuel Cells (SOFCs), mainly due to their high mixed ionic electronic conductivity between 600 and 800ºC. In this study, LSCF powders with different compositions were synthesized via a combination between citrate and hydrothermal methods. As-prepared powders were calcined from 700 to 900°C and then characterized by X-ray fluorescence, X-ray diffraction, thermal analyses, particle size analyses, nitrogen adsorption (BET) and scanning electronic microscopy. Films of composition La0,6Sr0,4Co0,2Fe0,8O3 (LSCF6428), powders calcined at 900°C, were screen-printed on gadolinium doped ceria (CGO) substrates and sintered between 1150 and 1200°C. The effects of level of sintering on the microstructure and electrochemical performance of electrodes were evaluated by scanning electronic microscopy and impedance spectroscopy. Area specific resistance (ASR) exhibited strong relation with the microstructure of the electrodes. The best electrochemical performance (0.18 ohm.cm2 at 800°C) was obtained for the cathode sintered at 1200°C for 2 h. The electrochemical activity can be further improved through surface activation by impregnation with PrOx, in this case the electrode area specific resistance decreases to values as low as 0.12 ohm.cm2 (800°C), 0.17 ohm.cm2 (750°C) and 0.31 ohm.cm2 (700°C). The results indicate that the citrate-hydrothermal method is suitable for the attainment of LSCF particulates with potential application as cathode component in intermediate temperature solid oxide fuel cells (IT-SOFCs)

Estudo do aproveitamento do rejeito da mineração de esmeraldas na produção de refratários conformados isolantes

Emerald mining is an important area of the economy in Brazil, country which is in second place among the exporting nations of this gem. Due to the process of extraction, a great amount of reject is generated. Since there is no appropriate destination, the reject is abandoned around the mining industries, contributing to environment degradation. Nowadays, some of the most relevant things to an industry in general are: energy conservation, cost reduction, quality and productivity enhancement. The production of isolating, transformed refractory materials achieves the sustainability dimension when protection of the environment is incorporated to such process. This work investigates the use of emerald mining rejects in the ceramic body of refractory materials, aiming at obtaining a product whose characteristics are compatible with commercial products and, at the same time, allow the use of such rejects to solve the environmental issue caused by its disposal in nature. X-ray fluorescence analysis show that the emerald reject obtained after the flotation to extract molybdenum and mica has 70% of silica and alumina (SiO2+Al2O3) and 21% of a basic oxides and alkaline metals and earthy alkaline mixture (Na2O, K2O, CaO e MgO). Because of the significant amount of silica and alumina present in the reject, four refractory ceramic bodies were prepared. Samples with a rectangular shape and dimensions 100x50x10 mm were pressed in a steel mold at 27,5 MPa and sintered at 1200ºC for 40 min. under environment atmosphere in a resistive oven. The sintered samples were characterized in relation to the chemical composition (FRX), mineralogical composition (DRX), microstructure (MEV) and physical and mechanical properties. The results indicate that the mixture with 45% of reject, 45% of alumina and 10% of kaolin presents a refractory quality of 1420ºC, dimensional linear variation below 2.00%, apparent specific mass of 1,56 g/cm3 and porosity of 46,68%, which demonstrates the potential use of the reject as raw material for the industry of isolating transformed refractory materials

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)

Síntese análise das propriedades magnéticas da ferrita de NiMg e características de absorção de radiação

It was synthesized different Ni1-xMgxFe2O4 (0,2 ≤ x ≤ 0,7) compositions by use of citrate precursor method. Initially, the precursory citrates of iron, nickel and magnesium were mixed and homogenized. The stoichiometric compositions were calcined from 350°C to 1200°C at ambient atmosphere or in argon atmosphere. The calcined powders were characterized by XRD, TGA/DTG, FTIR, magnetic measures and reflectivity using the wave guide method. I was observed pure magnetic phase formation between 350°C and 500°C, with formation of ferrite and hematite after 600°C at ambient atmosphere. The calcined powder at argon atmosphere formed pure ferromagnetic phase at 1100°C and 1200°C. The Rietveld analyses calculated the cations level occupation and the crystallite size. The analyses obtained nanometric crystals (11-66 nm), that at 900°C/3h presents micrometric sizes (0,45 - 0,70 Om). The better magnetization results were 54 Am2/Kg for x= 0,2 composition, calcined at 350°C/3h and 30 min, and 55,6 Am2/Kg for x= 0,2 1200°C, calcined in argon. 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 materials presented absorption less or equal the 50 % in ranges specific frequency. As for the 2,0 and 3,0 thickness (in 11,0 - 11,8 GHz), the reflectivity of the x= 0,3, 0,5 and 0,4 compositions, all calcined at 900°C/3h showed agreement with MS and O. Various factors contribute for the final radiation absortion effect, such as, the particle size, the magnetization and the polymer characteristics in the MARE composition. The samples that presented better magnetization does not obtaining high radiation absorption. It is not clear the interrelaction between the magnetization and the radiation absorption in the strip of frequencies studied (8,2 - 12,4 GHz)

Síntese e caracterização da ferrita de MnZn obtida pelo método dos citratos precursores

It was synthesized MnZn ferrite with general formulae Mn1-xZnxFe2O4 (mol%), 0,3 ≤ x ≤ 0,7 by using the citrate precursor method. The precursors decomposition was studied by thermogravimetric analysis (TGA), differential thermogravimetric analysis (DTG), differential thermal analysis (DTA) and Fourier transform infrared (FTIR) of powder calcined at 350ºC/3,5h. X-ray diffraction pattern (XRD) of samples was done from 350 to 1200ºC/2h using various atmospheres. The power calcined at 350ºC/3,5h formed spinel phase. It is necessary atmosphere control to avoid secondary phase such as hematite. From 900 to 1200ºC was obtained 90,66 and 100% of MnZn spinel ferrite phase, respectively. Analysis by dispersive energy scanning (EDS) at 350ºC shows high Mn and Zn dispersion, indicating that the diffusion process was homogeneous. Semi-quantitative analysis by EDS verified that despite the atmosphere control during calcinations at high temperatures (< 800ºC) occurred ZnO evaporation causing stoichiometric deviation. Vibrating sample magnetometer (VSM) measures show soft ferrite material characteristics with Hc from 6,5 x 10-3 to 11,1 x 10-2 T. Saturation magnetization (Ms) and initial permeability (µi) of MnZn spinel phase obtained, respectively, from 14,3 to 83,8 Am2/kg and 14,1 to 62,7 (Am2/kg)T

Preparação e caracterização do complexo sólido de estanho(II)-EDTA e influência do tratamento térmico sobre a morfologia do resíduo SnO2

Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)

Microstructural characteristics and electrochemical behavior of Co3O4 sintered electrodes

Co3O4 can be used as electrocatalyst for oxygen evolution reaction. The macro and microstructure of the oxide, obtained by compacting and sintering lithium-doped Co3O4 powder in atmosphere of dry air and in conditions of controlled temperature and time was analyzed by metallographic techniques. The porous material was characterized by XRD, SEM and EDS combined techniques. For working temperatures up to 1200°C, the pellet was consituted of particles with varying sizes over a wide range of particle size and, at higher temperatures CoO is formed and polymorphic transformation was observed. The materials were also characterized electrochemically in alkaline media by open circuit potential and potentiodynamic I/E measurements. The results were compared to those previously prepared by others by thermal deposition.