Obtenção de óxidos a base de níquel e cobalto para reação de oxidação parcial do metano

Nickel-based catalysts supported on alumina have been widely used in various reactions to obtain synthesis gas or hydrogen. Usually, higher conversion levels are obtained by these catalysts, however, the deactivation by coke formation and sintering of metal particles are still problems to be solved. Several approaches have been employed in order to minimize these problems, among which stands out in recent years the use of additives such as oxides of alkali metals and rare earths. Similarly, the use of methodologies for the synthesis faster, easier, applicable on an industrial scale and to allow control of the microstructural characteristics of these catalysts, can together provide the solution to this problem. In this work, oxides with spinel type structure AB2O4, where A represents divalent cation and B represents trivalent cations are an important class of ceramic materials investigated worldwide in different fields of applications. The nickel cobaltite (NiCo2O4) was oxides of spinel type which has attracted considerable interest due to its applicability in several areas, such as chemical sensors, flat panel displays, optical limiters, electrode materials, pigments, electrocatalysis, electronic ceramics, among others. The catalyst precursor NiCo2O4 was prepared by a new chemical synthesis route using gelatine as directing agent. The polymer resin obtained was calcined at 350°C. The samples were calcined at different temperatures (550, 750 and 950°C) and characterized by X ray diffraction, measurements of specific surface area, temperature programmed reduction and scanning electron microscopy. The materials heat treated at 550 and 750°C were tested in the partial oxidation of methane. The set of techniques revealed, for solid preparations, the presence of the phase of spinel-type structure with the NiCo2O4 NixCo1-xO solid solution. This solid solution was identified by Rietveld refinement at all temperatures of heat treatment. The catalyst precursors calcined at 550 and 750°C showed conversion levels around 25 and 75%, respectively. The reason H2/CO was around 2 to the precursor treated at 750°C, proposed reason for the reaction of partial oxidation of methane, one can conclude that this material can be shown to produce synthesis gas suitable for use in the synthesis Fischer-Tropsch process

Síntese e caracterização de ferrita ni-zn pelo método dos precursores poliméricos calcinada por energia de microondas

Magnetic ceramics have been widely investigated, especially with respect to intrinsic and extrinsic characteristics of these materials. Among the magnetic ceramic materials of technological interest, there are the ferrites. On the other hand, the thermal treatment of ceramic materials by microwave energy has offered various advantages such as: optimization of production processes, high heat control, low consumption of time and energy among others. In this work were synthesized powders of Ni-Zn ferrite with compositions Ni1- xZnxFe2O4 (0.25 ≤ x ≤ 0.75 mols) by the polymeric precursor route in two heat treatment conditions, conventional oven and microwave energy at 500, 650, 800 and 950°C and its structural, and morphological imaging. The materials were characterized by thermal analysis (TG/ DSC), X-ray diffraction (XRD), absorption spectroscopy in the infrared (FTIR), scanning electron microscopy (SEM), X-ray spectroscopy and energy dispersive (EDS) and vibrating sample magnetometry (VSM). The results of X-ray diffraction confirmed the formation of ferrite with spinel-type cubic structure. The extrinsic characteristics of the powders obtained by microwave calcination and influence significantly the magnetic behavior of ferrites, showing particles ferrimagnéticas characterized as soft magnetic materials (soft), is of great technological interest. The results obtained led the potential application of microwave energy for calcining powders of Ni-Zn ferrite

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

Efeito da velocidade de aquecimento nas propriedades de produtos da cerâmica estrutural

Heating rate is one of the main variables that determine a fire cycle. In industrial processes that use high temperatures, greater fire great can reduce the cost of production and increase productivity. The use of faster and more efficient fire cycles has been little investigated by the structural ceramic industry in Brazil. However, one of the possibilities that aims at modernizing the sector is the use of roller kilns and the inclusion of natural gas as fuel. Thus, the purpose of this study is to investigate the effect of heating rate on the technological properties of structural ceramic products. Clay raw materials from the main ceramic industries in the state of Rio Grande do Norte were characterized. Some of the raw materials characterized were formulated to obtain the best physical and mechanical properties. Next, raw materials and formulations were selected to study the influence of heating rate on the final properties of the ceramic materials. The samples were shaped by pressing and extrusion and submitted to rates of 1 °C/min, 10 °C/min and 20 °C/min, with final temperatures of 850 °C, 950 °C and 1050 °C. Discontinuous cycles with rates of 10 °C/min or 15 °C/min up to 600 °C and a rate of 20 °C/min up to final temperature were also investigated. Technological properties were determined for all the samples and microstructural analysis was carried out under a number of fire conditions. Results indicate that faster and more efficient fire cycles than those currently in practice could be used, limiting only some clay doughs to certain fire conditions. The best results were obtained for the samples submitted to slow cycles up to 600 °C and fast fire sinterization up to 950 °C. This paper presents for the first time the use of a fast fire rate for raw materials and clay formulations and seeks to determine ideal dough and processing conditions for using shorter fire times, thus enabling the use of roller kilns and natural gas in structural ceramic industries

Influência da adição de rejeitos cerâmicos nas propriedades de cerâmica vermelha da região do Recôncavo Baiano

The study of the physical and mechanic properties is an analysis of unquestioned importance on the production of the ceramic materials. In the region of the Recôncavo Baiano, there are ceramic and small brick factories, that still use rudimentary techniques, where the necessity of characterization of raw materials is denounced by the quality of the final product. The present work has for objective to study the behavior of the clay proceeding from the region of the Recôncavo, between the cities of Candeias and Camaçari/Ba, with addition of 5, 10 and 15% by weight of brick scraps, trying to optimize the physic and mechanical properties of the final product, aiming a better possibility of being manufactured, mechanic resistance, low linear retraction and water absorption. The brick scraps and the clay were characterized by FRX, DRX, TG, ATD and the granulometric analysis. Samples for testing where prepared by uniaxial pressing at 25Mpa, in 60x20x5mm size. The evaluated technological properties were: linear retraction, water absorption, apparent porosity and flexural strength. The samples were burned in electric oven in the temperatures of 850º, 950º and 1050ºC and compared its mechanical properties and the gresification. With addition of 15% by weight of brick scraps and burning at 900º-1000ºC the samples showed properties superior to that clay

Efeito da introdução de resíduo de cinza de forno cerâmico em massa para cerâmica estrutural

The red ceramics and structural ceramics, as they are known, include ceramic materials made by blocks of seals and structures, bricks, tiles, smail flagstones manacles, rustic floors and ornamental materials. Their fabrication uses raw material such as clay and clay sites, with some content of impurity. It has good durability and mechanical strength to compression, low cost, making it one of the mainly used materials in civil engineering. The incorporation of many industrial activities residue to ceramic products is a technological alternative for reducing the environmental impact caused by its carefree disposal. This incorporation can promote chemical change and inertness of metals from residue, by fixation in the glassy phase of ceramic during the burning stage. The main aim of this project is to study the technical feasibility of the addition of ceramic oven ash into formulations of mass for structural ceramics. In this project two kinds of clay (plastic and non-plastic) were used, as well as the ash from firewood used in the process of burning of structural ceramics. A group of experiments was outlined, which permitted the evaluation of the influence of the burning cycle in different temperatures of the ash content in formulations for ceramic blocks through technological properties, mechanical behavior and microstructure. Five samples were processed of each one of the masses of plastic and non-plastic clay without addition of ash and with addition of ash on the percentages of 10 % and 20 %, for temperatures of 850 °C, 950 °C, 1050 °C and 1150 °C, obtained through sinterization process. Among the studied compositions, the one which presented best performance was the mass of clay with 10 % of ash, at temperature of 1150 °C, with the smallest absorption of water, the smallest apparent porosity, specific apparent mass a bit over the others and greatest mechanical resistance to flexion. The composition made confirmed the technical feasibility of the use of ash in the mass for structural ceramics with maintenance of its necessary characteristics for its purposes

Obtenção de compósitos cerâmicos baseados em Al2O3/TiC através dos precursores poliméricos

The obtaining of ceramic materials from polymeric precursors is subject of numerous studies due to lower energy costs compared to conventional processing. The aim of this study is to investigate and improve the mechanism for obtaining ceramic matrix composite (CMC) based on SiOC/Al2O3/TiC by pyrolysis of polysiloxane in the presence of an active filler and inert filler in the pyrolysis temperature lower than the usually adopted for this technique, with greater strength. It also investigates the influence of pyrolysis temperature, the content of Alas active filler, the presence of infiltrating agents (Al, glass and polymer) after pyrolysis, temperature and infiltration time on some physical and mechanical properties. Alumina is used as inert filler and Al and Ti as active filler in the pyrolysis. Aluminum, glass and polysiloxane are used as agents infiltrating the post-pyrolysis. The results are analyzed with respect to porosity and bulk density by the Archimedes method, the presence of crystalline phases by X-ray diffraction (XRD) and microstructure by scanning electron microscopy (SEM). The ceramic pyrolyzed between 850 °C 1400 °C contain porosity 15% to 33%, density 2.34 g/cm3 and flexural strength at 4 points from 30 to 42 MPa. The microstructure features are porous, with an array of Al2O3 reinforced by TiC particles and AlTi3. The infiltration post-pyrolysis reveals decrease in porosity and increase density and strength. The composites have potential applications where thermal stability is the main requirement

Formulação e caracterização de massas de grês porcelanato preparadas a partir de matérias-primas naturais do Rio Grande do norte e com adição de chamote de telhas

Traditional ceramics have an important role in the economy of Rio Grande do Norte. The local industries manufacture over 50 million shingles a month, corresponding to 60% of their overall production. As a result of processing flaws, roughly 20% of the production must be discarded, since little or no use has been envisaged for such fired components. Therefore, the use of this kind of residue, especially in the composition of other ceramic materials, comes as an interesting option from the economical and environmental point of view. In this scenario, the objective of the present study was to assess the effect of the addition of fired shingle waste in the composition of porcelainized stoneware tiles. To that end, two porcelainized stoneware tiles compositions were initially prepared. Subsequently, contents from 10 to 30% of roofing tiles chamote were added to each one of them. All raw materials and grog were characterized by FRX, XRD, and thermal analysis. The ceramics were fired using natural gas for 30 min at different temperatures, i.e. 1150, 1200 and 1250ºC, and fully characterized. The addition of roofing tiles chamote resulted in composition with superior properties compared to additive-free compositions. Porcelainized stoneware tiles products that fulfill required standards for practical applications were achieved

Síntese de pigmentos cerâmicos inorgânicos nanométricos pela rota dos precursores poliméricos

Considering the constant evolution of technology in growth and the need for production techniques in the ceramics area to move forward together, we sought in this study, the research and development of polymeric precursor method to obtain inorganic ceramic pigments. Method that provides quality to obtain the precursor powders of oxides and pigments at the same time, offers time and cost advantages, such as reproducibility, purity and low temperature heat treatment, control of stoichiometry. This work used chromium nitrate and iron nitrate as precursors. The synthesis is based on the dissolution of citric acid as a complexing agent, addition of metal oxides, such as ion chromophores; polymerization with ethylene glycol and doping with titanium oxide. Passing through precalcination, breakdown, thermal treatments at different temperatures of calcination (700 to 1100 oC), resulting in pigments: green for chromium oxide deposited on TiO2 (CrTiO3) and orange for iron oxide deposited on TiO2 ( FeTiO3). Noticing an increase of opacity with increasing temperature. Were performed thermal analysis (TG and ATD) in order to evaluate its thermodecomposition. The powders were also characterized by techniques such as XRD, revealing the formation of crystalline phases such as iron titanate (FeTiO3) and chrome titanate (CrTiO3), SEM, demonstrating formation of rounded particles for both oxides and Spectroscopy in the UV-Visible Region, verifying the potential variation and chromaticity os pigments. Thus, the synthesized oxides were within the requirements to be applied as pigments and shown to be possible to propose its use in ceramic materials

Propriedades cerâmicas e imobilização do manganês em cerâmica estrutural

In this work is the addition of a metallic ion, of the metal Manganese, in a clay of Rio Grande do Norte state for structural ceramics use, the objective this study was to assess the evolution of ceramic properties. The clay was characterized by Chemical and Thermal analysis and Xray difraction. The metallic ion was added in the clay as aqueous solutions at concentrations of 100, 150 and 200 mg / L. The molded by extrusion and the burned were temperatures at 850, 950, 1050 and 1150 º C. Was made Chemical Analysis and investigated the following parameters environmental and ceramic: Solubility, Colour, Linear Retraction (%), Water Absorption (%), Gresification Curves, Apparent Porosity (%), Apparent Specific Mass (g/cm3) and Flexion Rupture Module (kgf/cm2). The results showed that increasing the concentration of metallic ion, properties such as Apparent Porosity (%), Water Absorption (%) decreases and the Flexion Rupture Module (kgf/cm2) increases with increasing temperature independent of the concentration of the ion. The gresification curves showed that the optimum firing temperatures were in the range between 950 and 1050 ° C. The evaluation of the properties showed that the ceramic material can be studied its use in solid brick and ceramic materials with structural function of filling. The results of solubility showed that the addition of ion offers no risk to the environment

Síntese e caracterização de tungstatos de cério e estrôncio para fins catalíticos

The main goal of this work was to produce nanosized ceramic materials of the family of the tungstates (tungstates of cerium and strontium), and test them for their catalytic activity in processes involving the transformation of methane (CH4). The methodology used for the synthesis of the ceramic powders involved the complexation combining EDTA-citrate. The materials characterization was performed using simple and differential thermogravimetry, x-ray diffraction, transmission electron microscopy, and energy dispersive spectroscopy (EDS). The microstructure analysis was performed using the refinement by the Rietveld method, and the crystallite size and distribution of the materials was elucidate by the Scherrer and Williamson-Hall methods. The conditions of the synthesis process for the three envisaged materials (SrWO4, SrWO4 using tungsten oxide concentrate as raw material, and Ce2(WO4)3) were adjusted to obtain a single phase crystalline material. The catalytic tests were carried out in the presence of methane and synthetic air, which is composed of 21% O2 and 79% N2. The analysis of the conversion of the reaction was done with the aid of an fourier transform infrared device (FTIR). The analysis showed that, structurally, the SrWO4 produced using raw materials of high and poor purity (99% and 92%, respectively) are similar. The ideal parameters of calcination, in the tested range, are temperature of 1000 °C and time of calcination 5 hours. For the Ce2(WO4)3, the ideal calcination time and are temperature 15 hours and 1000°C, respectively. The Williamson-Hall method provided two different distributions for the crystallite size of each material, whose values ranged between the nanometer and micrometer scales. According to method of Scherrer, all materials produced were composed of nanometric crystallites. The analyses of transmission electron microscopy confirmed the results obtained from the Williamson- Hall method for the crystallite size. The EDS showed an atomic composition for the metals in the SrWO4 that was different of the theoretical composition. With respect to the catalytic tests, all materials were found to be catalytically active, but the reaction process should be further studied and optimized.

Estudos de sinterização da mistura de pós cerâmicos diatomita-titânia

This work is part of an effort of consolidation of a daily search for powder technology at the Department of Physics of the Universidade Federal do Rio Grande do Norte. This work objective the study and development of new ceramic materials from raw materials abundant at the region. For this, were studied ceramic mixtures of powders from diatomite-titania to aiming at a new ceramic material from powder technology. The experimental work involved a characterization of ceramic powders from a diatomite-titania mixture. The powders obtained were pressed and then parameters like variation of mass, linear shrinkage, activation energy and the mechanism of sintering are studied in function of the time and temperature of sintering, beyond microstructural analysis. The obtained results allow us estimate the optimizing of sintering conditions of this material

Influência de defeitos e diferentes processos de fabricação nas propriedades mecânicas finais de cerâmicas

Os materiais cerâmicos são atualmente cada vez utilizados como opção na engenharia mundial. Por se tratar de materiais com alta resistência mecânica, possuem muitas aplicações em diversas áreas, como por exemplo a de mancais, a automotiva (sensores, isoladores, catalisadores, pistões, válvulas, revestimentos), a de implantes biocompatíveis (dentário, substituição óssea, válvulas cardíacas), a de produtos sujeitos ao desgaste (guias), a de refratários (revestimento de equipamento bélico, componentes de fornos), a eletrônica, e outras. Nos processos de fabricação da cerâmica há uma gama de fatores que contribuem para as características do produto final. Devido a isso, muitos pesquisadores têm trabalhado no estudo da influência de determinados defeitos e técnicas de produção de cerâmicas nas características do produto final. Este trabalho tem como objetivo fazer uma revisão bibliográfica de recentes artigos que analisam a influência de fatores como velocidade de queima, surgimento de trincas, porosidade, fases cristalinas, e tamanho de partículas, nas propriedades mecânicas finais das cerâmicas. Pode-se concluir que é possível aperfeiçoar o processo de fabricação da cerâmica a fim de promover as melhores propriedades mecânicas possíveis, conhecendo-se fatores prejudiciais e métodos adequados para se obter o melhor produto final.

Cerâmicas avançadas no processo de retificação cilíndrica externa de mergulho com rebolos diamantados com a técnica da mímima quantidade de lubrificação e refrigeração otimizada

Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)

Nanohardness and contact angle of Si wafers implanted with N and C and Al alloy with N by plasma ion implantation

Surfaces of silicon wafers implanted with N and C, respectively, and aluminum 5052 implanted with N alone by plasma immersion ion implantation WHO were probed by a nanoindentor and analyzed by the contact-angle method to provide information on surface nanohardness and wettability. Silicon nitride and silicon carbide are important ceramic materials for microelectronics, especially for high-temperature applications. These compounds can be synthesized by high-dose ion implantation. The nanohardness of a silicon sample implanted with 12-keV nitrogen PIII (with 3 X 10(17) cm(-2) dose) increased by 10% compared to the unimplanted sample, in layers deeper than the regions where the formation of the Si,N, compound occurred. A factor of 2.5 increase in hardness was obtained for C-implanted Si wafer at 35 keV (with 6 X 10(17) cm(-2) dose), again deeper than the SiC-rich layer, Both compounds are in the amorphous state and their hardness is much lower than that of the crystalline compounds, which require an annealing process after ion implantation. In the same targets, the contact angle increased by 65% and 35% for N- and C-implanted samples, respectively. Compared to the Si target, the nitrogen PIII-irradiated Al 5052 (wish 15 keV) showed negligible change in its hydrophobic character after ion implantation. Its near-surface nanohardness measurement showed a slight increase for doses of 1 X 10(17) cm(-2). We have been searching for an AlN layer of the order of 1000 A thick, using such a low-energy PIII process, but oxide formation during processing has precluded its synthesis. (C) 2002 Elsevier B.V. B.V. All rights reserved.