Desenvolvimento de cerâmica vermelha utilizando rejeitos da construção civil

The Industry of the Civil Construction has been one of the sectors that most contribute to the pollution of the environment, due to the great amount of residues generated by the construction, demolition and the extraction of raw material. As a way of minimizing the environmental impacts generated by this industry, some governmental organizations have elaborated laws and measures about the disposal of residues from the building construction (CONAMA - resolution 307). This work has as objective the reutilization of residues compound of sand, concrete, cement, red bricks and blocks of cement and mortar for the production of red ceramic, with the objective of minimizing costs and environmental impacts. The investigated samples contained 0% to 50% of residues in weight, and they were sintered at temperatures of 950°C, 1000°C, 1050°C, 1100°C and 1150°C. After the sinterization, the samples were submitted to tests of absorption of water, linear retraction, resistance to bending, apparent porosity, specific density, XRD and SEM. Satisfactory results were obtained in all studied compositions, with the possible incorporation of up to 50% of residues in ceramic mass without great losses in the mechanical strength, giving better results to the incorporation of 30% of residues in the fabrication of ceramic parts, such as roofing tiles, bricks masonry and pierced bricks

Estudo da viabilidade do sistema LZAS para uso como selante de PaCOS

Cells the solid oxide fuel are systems capable to directly convert energy of a chemical reaction into electric energy in clean, quiet way and if its components in the solid state differentiate of excessively the techniques for having all. Its more common geometric configurations are: the tubular one and to glide. Geometry to glide beyond the usual components (anode, cathode and electrolyte) needs interconnect and sealant. E the search for materials adjusted for these components is currently the biggest challenge found for the production of the cells. The sealants need to present chemical stability in high temperatures, to provoke electric isolation, to have coefficient of compatible thermal expansion with the excessively component ones. For presenting these characteristics the glass-ceramics materials are recommended for the application. In this work the study of the partial substitution of the ZrO2 for the Al2O3 in system LZS became it aiming at the formation of system LZAS, this with the addition of natural spodumene with 10, 20 and 30% in mass. The compositions had been casting to a temperature of 1500°C and later quickly cooled with the objective to continue amorphous. Each composition was worn out for attainment of a dust with average diameter of approximately 3μm and characterized by the techniques of DRX, FRX, MEV, dilatometric analysis and particle size analysis. Later the samples had been conformed and treated thermally with temperatures in the interval between 700-1000 °C, with platform of 10 minutes and 1 hour. The analyses for the treated samples had been: dilatometric analysis, DRX, FRX, electrical conductivity and tack. The results point with respect to the viability of the use of system LZAS for use as sealant a time that had presented good results as isolating electric, they had adhered to a material with similar α of the components of a SOFC and had presented steady crystalline phases

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 hidrotérmica assistida por micro-ondas de tiO2, e aplicação em nanocompósito

In recent decades have seen a sharp growth in the study area of nanoscience and nanotechnology and is included in this area, the study of nanocomposites with self-cleaning properties. Since titanium dioxide (TiO2) has high photocatalytic activity and also antimicrobial, self-cleaning surfaces in your application has been explored. In this study a comparison was made between two synthesis routes to obtain TiO2 nanoparticles by hydrothermal method assisted by microwave. And after analysis of XRD and SEM was considered the best material for use in nanocomposites. It was deposited nanocomposite film of poly (dimethyl siloxane) (PDMS) with 0.5, 1, 1.5 and 2% by weight of nanoparticles of titanium dioxide (TiO2) by the spraying method. The nanocomposite was diluted with hexane and the suspension was deposited onto glass substrate, followed by curing in an oven with forced air circulation. The photocatalytic activity of the nanocomposite impregnated with methylene blue was evaluated by UV- vis spectroscopy from the intensity variation of absorption main peak at 660nm with time of exposure to the UV chamber. Changes in the contact angle and microhardness were analyzed before and after UV aging test. The effect of ultraviolet radiation on the chemical structure of the PDMS matrix was evaluated by spectrophotometry Fourier transform infrared (FTIR).The results indicated that the addition of TiO2 nanoparticles in the coating PDMS gave high photocatalytic activity in the decomposition of methylene blue, an important characteristic for the development of self-cleaning coatings

Efeito da Gália como aditivo de sinterização em eletrólitos cerâmicos à base de céria sintetizados pelo método de complexação de cátions

Fuel cells are considered one of the most promising ways of converting electrical energy due to its high yield and by using hydrogen (as fuel) which is considered one of the most important source of clean energy for the future. Rare earths doped ceria has been widely investigated as an alternative material for the electrolyte of solid oxide fuel cells (SOFCs) due to its high ionic conductivity at low operating temperatures compared with the traditional electrolytes based on stabilized zirconia. This work investigates the effect of gallium oxide (Gallia) as a sintering aid in Eu doped ceria ceramic electrolytes since this effect has already been investigated for Gd, Sm and Y doped ceria electrolytes. The desired goal with the use of a sintering aid is to reduce the sintering temperature aiming to produce dense ceramics. In this study we investigated the effects on densification, microstructure and ionic conduction caused by different molar fraction of the dopants europium (10, 15 and 20%) and gallium oxide (0.3, 0.6 and 0.9%) in samples sintered at 1300, 1350 and 1450 0 C. Samaria (10 and 20%) doped ceria samples sintered between 1350 and 1450 °C were used as reference. Samples were synthesized using the cation complexation method. The ceramics powders were characterized by XRF, XRD and SEM, while the sintered samples were investigated by its relative density, SEM and impedance spectroscopy. It was showed that gallia contents up to 0.6% act as excellent sintering aids in Eu doped ceria. Above this aid content, gallia addition does not promote significant increase in density of the ceramics. In Ga free samples the larger densification were accomplished with Eu 15% molar, effect expressed in the microstructure with higher grain growth although reduced and surrounded by many open pores. Relative densities greater than 95 % were obtained by sintering between 1300 and 1350 °C against the usual range 1500 - 1600 0 C. Samples containing 10% of Sm and 0.9% of Ga reached 96% of theoretical density by sintering at 1350 0 C for 3h, a gain compared to 97% achieved with 20% of Sm and 1% of Ga co-doped cerias sintered at 1450 0 C for 24 h as described in the literature. It is found that the addition of gallia in the Eu doped ceria has a positive effect on the grain conductivity and a negative one in the grain boundary conductivity resulting in a small decrease in the total conductivity which will not compromise its application as sintering aids in ceria based electrolytes. Typical total conductivity values at 600 and 700 °C, around 10 and 30 mS.cm -1 respectively were reached in this study. Samples with 15% of Eu and 0.9 % of Ga sintered at 1300 and 1350 °C showed relative densities greater than 96% and total conductivity (measured at 700 °C) between 20 and 33 mS.cm -1 . The simultaneous sintering of the electrolyte with the anode is one of the goals of research in materials for SOFCs. The results obtained in this study suggest that dense Eu and Ga co-doped ceria electrolytes with good ionic conductivity can be sintered simultaneously with the anode at temperatures below 1350 °C, the usual temperature for firing porous anode materials

Rejeito de xisto como adsorvente para remoção de fenol em águas produzidas na indústria de petróleo

Produced water is the main effluent linked to the activity of extraction of oil and their caring management is necessary due to the large volume involved, to ensure to minimize the negative impacts of discharges of these waters in the environment. This study aimed to analyze the use of retorted shale, which is a reject from the pyrolysis of pirobituminous shale, as adsorbent for the removal of phenols in produced water. The material was characterized by different techniques (grain sized analysis, thermal analysis, BET, FRX, FT-IR, XRD and SEM), showing the heterogeneity in their composition, showing its potential for the removal of varied compounds, as well as the phenols and their derivatives. For the analysis of the efficiency of the oil shale for the adsorption process, assays of adsorption balance were carried through, and also kinetic studies and dynamics adsorption, in the ETE of the UTPF of Petrobras, in Guamaré-RN. The balance assays shown a bigger conformity with the model of Langmuir and the kinetic model more adjusted to describe the adsorption of phenols in retorted shale was of pseudo-second order. The retorted shale presented a low capacity of adsorption of phenols (1,3mg/g), when related to others conventional adsorbents, however it is enough to the removal of these composites in concentrations presented in the produced water of the UTPF of Guamaré. The assays of dynamics adsorption in field had shown that the concentration of phenol in the effluent was null until reaching its rupture (58 hours). The results showed the possibility of use of the reject for removal of phenols in the final operations of the treatment process, removing as well, satisfactorily, the color and turbidity of the produced water, with more than 90% of removal

Desenvolvimento de pastas cimentantes utilizando cimentos portland compostos para cimentação de poços petrolíferos

The Compound Portland cements are commonly used in construction, among them stand out the CPII-Z, CPII-F and CPIV. These types of cement have limited application on oil well cementing, having its compositional characteristics focused specifically to construction, as cement for use in oil wells has greater complexity and properties covering the specific needs for each well to be coated. For operations of oil wells cementing are used Portland cements designed specifically for this purpose. The American Petroleum Institute (API) classifies cements into classes designated by letters A to J. In the petroleum industry, often it is used Class G cement, which is cement that meets all requirements needed for cement from classes A to E. According to the scenario described above, this paper aims to present a credible alternative to apply the compound cements in the oil industry due to the large availability of this cement in relation to oil well cements. The cements were micro structurally characterized by XRF, XRD and SEM tests, both in its anhydrous and hydrated state. Later technological tests were conducted to determine the limits set by the NBR 9831. Among the compound cements studied, the CPII-Z showed satisfactory properties for use in primary and secondary operations of oil wells up to 1200 meters cementing

Desenvolvimento de nanocompósito (hidroxiapatita/ poliuretano) pela gelação (gelling) de poli ( álcool vinílico) (PVA) para remoção de metais pesados

Removing microcontaminants from effluents is a challenge today, because of its high cost and low efficiency, especially in the treatment of effluents containing heavy metals. An alternative that has emerged is the use of biodegradable nanocomposites, which exhibit good removal and recovery performances, in addition to its low cost. With this in mind, the present study aimed to develop and characterize a nanocomposite based on hydroxyapatite (HAP), polyurethane (PU) and polyvinyl alcohol (PVA) for removing heavy metals. Thus, the research was conducted in several steps: i)- Physico-chemical and microbiological hospital effluent characterization; ii)- Production of hydroxyapatite by aqueous precipitation technique, and their characterization; iii)- Production of the nanocomposite in which the hydroxyapatite was added to the polyurethane prepolymers and then the polyvinyl alcohol/hydroxyapatite film was produced; iv)- Polyvinyl composite without film PU/HAp was also produced in the proportions of 20 and 40% HAp; v)- The composites was characterized by the techniques of XRD, FTIR, SEM / EDS, BET, Zeta Potential and TGA; vi)- The sisal and coconut fibres were washed and dried for comparative tests of adsorption; vii)- Adsorption tests for evaluating the removal of heavy metals (nickel and cadmium). Initial screening adsorption capacity (HAp; PU/HAp - 20 and 40%; PU / HAp / PVA), kinetic studies of adsorption of Cd (II) by HAp; multifactorial design analysis (factorial design) for identifying the most important variables in the adsorption of Cd (II) by composite PU/HAp. Also comparative analysis of adsorption of Cd and Ni by composite PU/HAp were conducted, as well as comparative tests of adsorption of Cd (coconut fibre) and Ni (sisal fibre). It was possible to verify that the composite PU/HAp 40% showed better effectiveness for the removal of Cd (II) and Ni (II), above 80%, equivalent to the lignocellulosic fibre used and HAp produced. As main conclusion, it can be referred that the composite PU/HAp 40% is an effective adsorvent to wastewater treatment for heavy metal removal, with low cost and high efficiency

Redução carbotérmica de TiO2 por descarga em cátodo oco

In this study we used the plasma as a source of energy in the process of carbothermic reduction of rutile ore (TiO2). The rutile and graphite powders were milled for 15 h and placed in a hollow cathode discharge produced by in order to obtain titanium carbonitride directly from the reaction, was verified the influence of processing parameters of plasma temperature and time in the synthesis of TiCN. The reaction was carried out at 600, 700 and 800˚C for 3 to 4 hours in an atmosphere of nitrogen and argon. During all reactions was monitored by plasma technique of optical emission spectroscopy (EEO) to check the active species present in the process of carbothermal reduction of TiO2. The powder obtained after the reactions were characterized by the techniques of X-ray diffraction (XRD) and scanning electron microscopy (SEM). The technique of EEO were detected in all reactions the spectra CO and NO, and these gas-phase resulting from the reduction of TiO2. The results of X-ray diffraction confirmed the reduction, where for all conditions studied there was evidence of early reduction of TiO2 through the emergence of intermediate oxides. In the samples reduced at 600 and 700˚C, there was only the phase Ti6O11, those reduced to 800˚C appeared Ti5O9 phases, and Ti6O11 Ti7O13, confirming that the carbothermal reduction in plasma, a reduction of the ore rutile (TiO2) in a series of intermediate titanium oxide (TinO2n-1) where n varies between 5 and 10

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

Desenvolvimento de processos de síntese de sodalita a partir de rejeitos de caulins da região Amazônica

No estudo da síntese de Sodalita foram utilizados dois rejeitos de caulins provenientes de duas empresas de beneficiamento de caulim para cobertura de papel, localizadas na região Amazônica, que operam na região do Rio Capim (CRC) e do Rio Jari (CRJ). Além desses rejeitos, também foi utilizado como fonte de alumina e sílica o metacaulim, obtida através da calcinação dos caulins (MRC e MRJ, respectivamente). Dessa forma, para obter informações das suas características foram realizadas análises químicas e mineralógicas destes caulins. A síntese da Sodalita foi realizada variando alguns parâmetros, como material de partida: partindo-se diretamente de caulim nas temperaturas de 80, 100, 120 e 150 °C; e, partindo-se de metacaulim na temperatura de 95 °C. Posteriormente, as sínteses foram realizadas variando-se as soluções básicas a fim de verificar a influencia da presença dos íons OH^-, Cl^- e CO₃^2-, bem como a influencia da relação Na₂O/Al₂O₃ na síntese, com a temperatura fixa em 95 ºC para o material de partida MRC. Verificou-se ainda, a influência da temperatura de síntese variando as em 85, 90 e 95 °C, fixando-se a relação Na₂O/Al₂O₃ na mistura reacional para determinar as condições ótimas de síntese de Sodalita. Os materiais de partida e os produtos de síntese foram identificados e caracterizados através de DRX, FRX, MEV, ATD/TG e EIV. O método de síntese que apresentou melhor resultado foi utilizou o metacaulim como material de partida, com solução NaOH + Na₂CO₃ apresentando relação Na₂O/Al₂O₃de 3,89 conduzida sob agitação, a 95°C, pressão atmosférica e tempo de 4 horas, para os dois tipos de caulins (CRC e CRJ). A utilização do metacaulim MRC, a partir do caulim do Rio Capim, nas condições mencionadas acima obteve-se a conversão de 86,5% em massa de Sodalita, e o metacaulim MRJ, caulim do Rio Jari, a conversão foi de 73,6% em sodalita. No que se refere ao tamanho de poros, os produtos partindo de metacaulim tanto do Rio Capim quanto do Rio Jari foram caracterizados como materiais mesoporosos, porém o produto partindo de metacaulim do Rio Jari apresentou maior área especifica.

Reaproveitamento de lama vermelha na obtenção de compostos do tipo hidrotalcita do sistema (Zn-Ni-Cu/Fe-Al)-SO4

Compostos do tipo hidrotalcita, também conhecidos como hidróxidos duplos lamelares (HDLs), do sistema (Zn-Ni-Cu/Fe-Al)-SO₄ foram obtidos por meio de co-precipitação a pH variável (crescente) utilizando lama vermelha (LV) como material de partida devido a sua elevada porcentagem de Fe³⁺ e Al³⁺. Para tal estudo, a LV, previamente caracterizada por FRX e DRX, foi submetida à abertura ácida com HCl_conc. e H₂SO₄ 2N. Para os HDLs obtidos, foram avaliados a influência do tipo de cátion bivalente, da variação do pH de síntese (pH 5, 7, 8, 9, 10 e 12) e da variação de razão molar teórica r = M^II/M^III (2, 3 e 4) na sua estrutura cristalina mediante as seguintes técnicas de caracterização: DRX, FT-IR, MEV/EDS, TG/ATD. Os resultados FRX revelaram que a LV é composta principalmente por Fe₂O₃ (32,80%), Al₂O₃ (19,83%), SiO₂ (18,14%) e Na₂O (11,55%). DRX corrobora os resultados da análise química, visto que foram identificados os minerais: hematita, goethita, gibbsita, sodalita, calcita, anatásio e quartzo. Zn-HDLs mostraram que a o aumento de pH de síntese colabora para um melhor ordenamento cristalino do material, uma vez que os picos se tornam melhor definidos, culminando com a melhor condição experimental em pH 9 e r = 3, cujo HDL foi identificado como o mineral natroglaucocerinita (d~11 Ǻ). Nesses valores de pH, a incorporação de SO₄^2- no espaçamento interlamelar foi favorecida apesar da competição com o CO₂ presente no ar atmosférico no momento da síntese. FT-IR também indica a presença do sulfato. As análises por MEV revelam a presença de cristais muito finos e pequenos, > 2μm, de forma hexagonal que pela análise via EDS indicaram, em sua composição, os elementos Na, Zn, Fe, Al, S, C e O. TG/ATD evidenciaram quatro etapas de perda de massa: desidratação, desidroxilação, desoxidenação e dessulfatação, para os HDLs com melhor ordenamento cristalino. Para os materiais menos cristalinos, as duas primeiras etapas ocorrem simultaneamente. Ni-HDLs apresentaram três picos com posições próximas às do mineral carrboydita a partir de pH igual a 7. No entanto, a partir de pH 9, surge hematita como uma fase acessória. Também há disputa entre os ânions SO₄^2- e CO₃^2- no espaço interlamelar, visto que os valores de espaçamento basal d diminuem (de aproximadamente 9,5 até 7,8 Ǻ). Tal fato também foi observado pelo FT-IR. As análises por MEV mostraram aglomerados de minerais anédricos menores que 2μm que, via EDS indicaram composição Ni, Fe, Al, S, C e O. As análises de TG/ATD apresentaram o mesmo comportamento do sistema anterior, evidenciaram as etapas de desidratação, desidroxilação, desoxigenação e dessulfatação e, para os materiais menos cristalinos, as duas primeiras etapas também ocorrem simultaneamente. Cu-HDLs, em valores de pH entre 7 e 10, não cristalizaram a fase HDL tal qual verificada para os sistemas contendo zinco ou níquel. O cobre distorce a estrutura do octaedro causando o chamado Efeito Jahn-Teller: distorção tetraédrica no ambiente octaédrico. As análises por FT-IR apresentaram o mesmo comportamento dos sistemas anteriores, apesar de o material se apresentar amorfo via DRX. O MEV também revela aglomerados amorfos que, de acordo com o EDS, indicaram em sua composição os elementos Cu, Fe, Al, S, C e O. As análises de TG/ATD apresentaram o mesmo comportamento que os materiais menos cristalinos dos dois sistemas anteriores, para os quais as etapas de desidratação e desidroxilação ocorreram simultaneamente. Mt-HDLs (mistura de Zn²⁺, Ni²⁺, Cu²⁺), apresentaram comportamento semelhante aos HDLs de níquel, com quatro picos em posições próximas aos da carrboydita a partir de pH igual a 7. A disputa entre sulfato e carbonato também se repete, visto que os valores de espaçamento basal d diminuem (de aproximadamente 9,5 até 7,9 Ǻ), o que também pode ser notado nos espectros de FT-IR. O MEV dessas amostras também apresentaram aglomerados com tamanhos menores que 2μm e, via EDS, indicaram em sua composição os elementos Zn, Cu, Ni, Fe, Al, S, C e O. Aqui também o comportamento das curvas TG/ATD foi semelhante aos materiais pouco cristalinos obtidos anteriormente.

Síntese e caracterização do compósito SnO2/TiO2 nanoestruturado

Pós-graduação em Ciência e Tecnologia de Materiais - FC

Síntese e caracterização dielétrica de filmes finos de Bi3NbO7 obtidos pelo método dos precursores poliméricos

Bi3NbO7 thin films were prepared by the polymeric precursor method. The precursor solutions were prepared with excess of bismuth ranging from 0% to 10% and the pH was controlled to be maintained between 8 and 9. This control was done by adding to the solution niobium and ethylene glycol. The final solution was clear and free of precipitation. After obtaining the precursor solution, has begun the process of characterization of powders with thermogravimetry (TG), differential thermal analysis and X-ray analysis (XRD). The films were obtained by the polymeric precursors, the method is advantageous because it is simple, and low cost involves steps and controlled stoichiometry. The films were annealed and characterized by XRD and SEM and also characterized according to their dialectics properties. We observed that the best results were obtained when the film is thermally at 800 ° C for two hours and 860 ° C for two hour. Under these conditions we obtain Bi3NbO7 thin films with good homogeneity, uniform distribution of the grains, but with the formation of secondary phase, which does not occur in treatments with lower temperature. The dielectric characterization showed that the produced film showed good characteristics with high dielectric constant and low loss

Um estudo teórico e experimental de nanoestruturas de 'ZnS': propriedades físicas e químicas

Pós-graduação em Química - IQ