Caracterização Microestrutural e Tribocorrosiva de Sistemas Metalocerâmicos Odontológicos do Tipo Ni-Cr/Porcelana E Ni-Cr/Ti/Porcelana

The partial fixed prosthodontics restoration is used to rehabilitate form and function of partial or total compromised teeth, having to remain permanently joined to remainder tooth. The most useful material on prosthodontics is the feldspar porcelain, commercialized as aluminosilicate powders. Dental porcelains are presented with limited mechanical properties to rehabilitate extensive spaces. The association with Ni-Cr metallic systems (metal-ceramic system) allows that the metallic substructure compensates the fragile porcelain nature, preserving the thermal insulation and aesthetics desirable, as well as reducing the possibility of cracking during matication efforts. Cohesive flaws by low mechanical strength connect the metallic substructure to the oral environment, characterized by a electrolytic solution (saliva), by aggressive temperature, pH cyclic changes and mechanical requests. This process results on ionic liberation that could promote allergic or inflammatory responses, and/or clinical degradation of ceramometal system. The aim of this study was to evaluate the presence of an intermediate titanium layer on the microscopic fracture behavior of porcelains on ceramometal systems. Plasma deposition of titanium films result in regular passivating oxide layers which act as barriers to protect the metallic substrate against the hazardous effects of corrosive saliva. Tribocorrosion tests were performed to simulate the oral environment and mechanical stress, making it possible the early detection of crack formation and growth on metal-ceramic systems, which estimate the adherence between the compounds of this system. Plain samples consisting of dental feldspar porcelain deposited either onto metallic substrates or titanium films were fired and characterized by scanning electron microscopy. The result showed that the titanium film improved the adherence of the system compared to conventional metal-ceramic interfaces, thus holding crack propagation

Análise mecânica e microestrutural das ligas de cobalto-cromo de uso odontológico após sucessivas refundições

The cobalt-chromium alloy is extensively used in the Odontology for the confection of metallic scaffolding in partial removable denture. During the last few years, it has been reported an increasing number of premature imperfections, with a few months of prosthesis use. The manufacture of these components is made in prosthetic laboratories and normally involves recasting, using parts of casting alloy and parts of virgin alloy. Therefore, the objective of the present study was to analyze the mechanical properties of a commercial cobalt-chromium alloy of odontological use after successive recasting, searching information to guide the dental prosthesis laboratories in the correct manipulation of the cobalt-chromium alloy in the process of casting and the possible limits of recasting in the mechanical properties of this material. Seven sample groups were confectioned, each one containing five test bodies, divided in the following way: G1: casting only with virgin alloy; G2: casting with 50% of the alloy of the G1 + 50% of virgin alloy; G3: casting with 50% of the alloy of the G2 + 50% of virgin alloy; G4: casting with 50% of the alloy of the G3 + 50% of virgin alloy; G5: 50% of alloy of the G4 + 50% of virgin alloy; G6: 50% of alloy of the G5 + 50% of virgin alloy and finally the G7, only with recasting alloy. The modifications in the mechanical behavior of the alloy were evaluated. Moreover, it was carried the micro structural characterization of the material by optic and electronic scanning microscopy, and X ray diffraction.and fluorescence looking into the correlatation of the mechanical alterations with structural modifications of the material caused by successive recasting process. Generally the results showed alterations in the fracture energy of the alloy after successive recasting, resulting mainly of the increasing presence of pores and large voids, characteristic of the casting material. Thus, the interpretation of the results showed that the material did not reveal significant differences with respect to the tensile strength or elastic limit, as a function of successive recasting. The elastic modulus increased from the third recasting cycle on, indicating that the material can be recast only twice. The fracture energy of the material decreased, as the number of recasting cycles increased. With respect to the microhardness, the statistical analyses showedno significant differences. Electronic scanning microscopy revealed the presence of imperfections and defects, resulting of the recasting process. X ray diffraction and fluorescence did not show alterations in the composition of the alloy or the formation of crystalline phases between the analyzed groups. The optical micrographs showed an increasing number of voids and porosity as the material was recast. Therefore, the general conclusion of this study is that the successive recasting of of Co-Cr alloys affects the mechanical properties of the material, consequently leading to the failure of the prosthetic work. Based on the results, the best recommendadition is that the use of the material should be limited to two recasting cycles

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

Revestimentos a base de Ta/Al2O3 produzidos por aspersão térmica sobre substrato metálico

Metal substrates were coated by thermal spraying plasma torch, they were positioned at a distance of 4 and 5 cm from the nozzle exit of the plasma jet. The starting materials were used for deposition of tantalum oxide powder and aluminium. These two materials were mixed and ground into high-energy mill, then immersed in the torch for the production of alumina coating infused with particles of tantalum with nano and micrometric size. The spraying equipment used is a plasma torch arc not transferred, which operating in the range of 250 A and 80 V, was able to produce enough heat to ignite aluminothermic between Ta2O5 and aluminum. Upon reaching the plasma jet, the mixing powders react with the heat of the blaze, which provides sufficient energy for melting aluminum particles. This energy is transferred through mechanisms of self-propagating to the oxide, beginning a reduction reaction, which then hits on the surface of the substrate and forms a coating on which a composite is formed by a junction metal - ceramic (Ta +Al2O3). The phases and quantification of each were obtained respectively by X-ray diffraction and the Rietveld method. Morphology by scanning electron microscopy and chemical analysis by energy dispersive spectroscopy EDS. It was also performed measurements of the substrate roughness, Vickers microhardness measurements in sprays and determination of the electron temperature of the plasma jet by optical emission spectroscopy EEO. The results confirmed the expectation generated around the end product of spraying the mixture Ta2O5 + Al, both in the formation of nano-sized particles and in their final form. The electron excitation temperature was consistent with the purpose of work, in addition, the thermodynamic temperature was efficient for the reduction process of Ta2O5. The electron excitation temperature showed values of 3000, 4500 and 8000 K for flows10, 20 and 30 l / min respectively, these values were taken at the nozzle exit of the plasma jet. The thermodynamic temperature around 1200 ° C, was effective in the reduction process of Ta2O5

Preparação de óxidos mistos de níquel e zinco nanoparticulados a partir de combustíveis alternativos

The field of "Materials Chemistry" has been developing in recent years and there has been a great increase of interest in the synthesis and chemical and physical properties of new inorganic solids. New routes of synthesis and synthesis modified has been developed with the aim not only to optimize the processes in laboratory scale, but also on an industrial scale, and make them acceptable by current environmental legislation. The phenomenology of current solid state chemistry properties coupled with the high temperature superconductivity, ferromagnetism, porosity molecular and colors are evidence affected by the synthesis method, which in turn can influence the technological application of these materials. From this understanding, mixed oxides of nickel and zinc nanoparticulate were synthesized by microwave-assisted combustion route using three specific types of organic fuels employing the weight ratios 1:1/2 and 1:1 of cation metallic/fuel, in order to investigate the influence of such proportions to obtain the solids. The new fuels were chosen to replace, for example, urea or glycine that are the fuels most commonly preferred in this kind of synthesis. The powders without heat treatment were studied by Thermogravimetric analysis (TGA), X-Ray Diffraction (XRD) and then calcined at 900°C. After heat treatment, the samples were characterized by analysis of X Ray Diffraction (XRD) and Scanning Electron Microscopy (SEM). The modified synthesis route porposed was effective for obtaining powders. Both the alternative fuels chosen as the different weight ratios employed, influenced in the morphology and obtaining oxides

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

Efeito das variáveis laboratoriais protéticas na adesão da porcelana com ligas de níquel-cromo

The metalceramic crowns are usually used in dentistry because they provide a resistant structure due to its metallic base and its aesthetics from the porcelain that recovers this structure. To manufacture these crowns, a series of stages should be accomplished in the prosthetic laboratories, and many variables can influence its success. Changes in these variables cause alterations in the metallic alloy and in the porcelain, so, as consequence, in the adhesion between them. The composition of the metal alloy can be modified by recasting alloys, a common practice in some prosthetic laboratories. The aim of this paper is to make a systematic study investigating metalceramic crowns as well as analyzing the effect of recasting Ni-Cr alloys. Another variable which can influence the mechanism of metalceramic union is the temperature used in firing porcelain procedure. Each porcelain has to be fired in a fixed temperature which is determined by the manufacturer and its change can cause serious damages. This research simulate situations that may occur on laboratory procedures and observe their consequences in the quality of the metalceramic union. A scanning eletron microscopy and an optic microscopy were accomplish to analyse the metal-ceramic interface. No differences have been found when remelting alloys were used. The microhardness were similar in Ni-Cr alloys casted once, twice and three times. A wettability test was accomplished using a software developed at the Laboratório de Processamento de Materiais por Plasma, on the Universidade Federal do Rio Grande do Norte. No differences were found in the contact angle between the solid surface (metallic substratum) and the tangencial plane to the liquid surface (opaque). To analyse if the temperature of porcelain firing procedure could influence the contact area between metal and porcelain, a variation in its final temperature was achieve from 980° to 955°C. Once more, no differences have been found

Comportamento da adição do carbeto de nióbio (nBC) na matriz metálica do aço ferrítico 15kH2mfa

The 15Kh2MFA steel is a kind of Cr-Mo-V family steels and can be used in turbines for energy generation, pressure vessels, nuclear reactors or applications where the range of temperature that the material works is between 250 to 450°C. To improve the properties of these steels increasing the service temperature and the thermal stability is add a second particle phase. These particles can be oxides, carbides, nitrites or even solid solution of some chemical elements. On this way, this work aim to study the effect of addition of 3wt% of niobium carbide in the metallic matrix of 15Kh2MFA steel. Powder metallurgy was the route employed to produce this metallic matrix composite. Two different milling conditions were performed. Condition 1: milling of pure 15Kh2MFA steel and condition 2: milling of 15Kh2MFA steel with addition of niobium carbide. A high energy milling was carried out during 5 hours. Then, these two powders were sintered in a vacuum furnace (10-4torr) at 1150 and 1250°C during 60 minutes. After sintering the samples were normalized at 950°C per 3 minutes followed by air cooling to obtain a desired microstructure. Results show that the addition of niobium carbide helps to mill faster the particles during the milling when compared with that steel without carbide. At the sintering, the niobium carbide helps to sinter increasing the density of the samples reaching a maximum density of 7.86g/cm³, better than the melted steel as received that was 7,81g/cm³. In spite this good densification, after normalizing, the niobium carbide don t contributed to increase the microhardness. The best microhardness obtained to the steel with niobium carbide was 156HV and to pure 15Kh2MFA steel was 212HV. It happened due when the niobium carbide is added to the steel a pearlitic structure was formed, and the steel without niobium carbide submitted to the same conditions reached a bainitic structure

Síntese e caracterização de CuNb2O6 e CuNbC através de reação sólido- sólido e gás- sólido a baixa temperatura

The refractory metal carbides have proven important in the development of engineering materials due to their properties such as high hardness, high melting point, high thermal conductivity and high chemical stability. The niobium carbide presents these characteristics. The compounds of niobium impregnated with copper also have excellent dielectric and magnetic properties, and furthermore, the Cu doping increases the catalytic activity in the oxidation processes of hydrogen. This study aimed to the synthesis of nanostructured materials CuNbC and niobium and copper oxide from precursor tris(oxalate) oxiniobate ammonium hydrate through gas-solid and solid-solid reaction, respectively. Both reactions were carried out at low temperature (1000°C) and short reaction time (2 hours). The niobium carbide was produced with 5 % and 11% of copper, and the niobium oxide with 5% of copper. The materials were characterized by X-Ray Diffraction (XRD), Rietveld refinement, Scanning Electron Microscopy (SEM), X-Ray Fluorescence Spectroscopy (XRF), infrared spectroscopy (IR), thermogravimetric (TG) and differential thermal analysis (DTA , BET and particle size Laser. From the XRD analysis and Rietveld refinement of CuNbC with S = 1.23, we observed the formation of niobium carbide and metallic copper with cubic structure. For the synthesis of mixed oxide made of niobium and copper, the formation of two distinct phases was observed: CuNb2O6 and Nb2O5, although the latter was present in small amounts

Desenvolvimento de filtros cerâmicos impregnados com nanopartículas de prata para desinfecção de água potável

Brazil has vast amounts of hydric resources, whose quality has been deteriorating due to pollutant dumping. Household waste disposal is one of the main sources of water pollution, stimulating bacteria proliferation and introducing microorganisms, including those from fecal matter. Conventional water disinfection methods are a solution, but on the downside, they lead to the formation byproducts hazardous to human health. In this study, aiming to develop bactericidal filters for the disinfection of drinking water; silver nanoparticles were deposited on alumina foams through three routes: sputtering DC, dip coating and in situ chemical reduction of silver nitrate. The depositions were characterized through X-ray diffraction, scanning electron microscopy and EDS element mapping. The influence of the depositions on permeability and mechanical properties of the ceramic foams was assessed and, in sequence, a preliminary antibacterial efficiency analysis was carried out. Characterization results indicate that the chemical reduction routes were efficient in depositing homogeneously distributed silver particles and that the concentration of the metallic precursor salt affects size and morphology of the particles. The antibacterial efficiency analysis indicates that the chemical reduction filters have potential for water disinfection

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

Obtenção de pós de tântalo metálico a partir da redução aluminotérmica com ignição a plasma

Metallic tantalum has a high commercial value due to intrinsic properties like excellent ductility, corrosion resistance, high melt and boiling points and good electrical and thermal conductivities. Nowadays, it is mostly used in the manufacture of capacitors, due to excellent dielectric properties of its oxides. In the nature, tantalum occurs in the form of oxide and it is extracted mainly from tantalite-columbite ores. The tantalum is usually produced by the reduction of its oxide, using reductants like carbon, silicon, calcium, magnesium and aluminum. Among these techniques, the aluminothermic reduction has been used as the industrial method to produce niobium, tantalum and their alloys, due to the easy removal of the Al and Al2O3 of the system, easing further refining. In conventional aluminothermic reduction an electrical resistance is used to trigger the reaction. This reaction self-propagates for all the volume of material. In this work, we have developed a novel technique of aluminothermic reduction that uses the hydrogen plasma to trigger the reaction. The results obtained by XRD, SEM and EDS show that is possible to obtain a compound rich in tantalum through this technique of aluminothermic reduction in the plasma reactor

Estudo termo-mecânico de interconector metálico recoberto com filme de La0,8Ca0,2CrO3 e de interconector cerâmico de La0,8Sr0,2Cr0,92Co0,08O3 para PaCOS

Doped lanthanum chromite ( LaCrO3 ) has been the most common material used as interconnect in solid oxide fuel cells for high temperature ( SOFC-HT ) that enabling the stack of SOFCs. The reduction of the operating temperature, to around 800 º C, of solid oxide fuel cells enabled the use of metallic interconnects as an alternative to ceramic LaCrO3, From the practical point of view, to be a strong candidate for interconnect the material must have good physical and mechanical properties such as resistance to oxidizing and reducing environments, easy manufacture and appropriate thermo-mechanical properties. Thus, a study on the physic-mechanical interconnects La0,8Sr0,2Cr0,92Co0,08O3 ceramics for SOFC -AT obtained by the method of combustion , as well as thermo-mechanical properties of metallic interconnects (AISI 444) covered with La0,8Ca0,2CrO3 by deposition technique by spray-pyrolysis fuel cells for intermediate temperature (IT-SOFCs). The La0,8Sr0,2Cr0,92Co0,08O3 was characterized by X -ray diffraction(XRD) , density and porosity , Vickers hardness (HV) , the flexural strength at room temperature and 900 °C and scanning electron microscopy (SEM). The X -ray diffraction confirmed the phase formation and LaCrO3 and CoCr2O4, in order 6 GPa hardness and mechanical strength at room temperature was 62 MPa ceramic Interconnector. The coated metal interconnects La0,8Ca0,2CrO3 passed the identification by XRD after deposition of the film after the oxidation test. The oxidative behavior showed increased resistance to oxidation of the metal substrate covered by La0,8Ca0,2CrO3 In flexural strength of the coated metal substrate, it was noticed only in the increased room temperature. The a SEM analysis proved the formation of Cr2O3 and (Cr,Mn)3O4 layers on metal substrate and confirmed the stability of the ceramic La0,8 Ca0,2CrO3 film after oxidative test

Redução aluminotérmica do óxido de tântalo usando uma tocha de plasma como ignitor

In this work was used a plasma torch of non transferred arc with argon as work gas, using a power supply with maximum DC current of 250 A and voltage of 30 V to activate the plasma and keep it switched on. The flame temperature was characterized by optical emission spectroscopy, through Boltzmann-plot-method. The torch has been used like igniter in the aluminothermic reduction of the mixture tantalum oxide and aluminum, seeking to obtain metallic tantalum. In heating of the reagents only one particle will be considered to study interactions between plasma-particle, seeking to determinate its fusion and residence time. The early powders were characterized by laser granulometry, scanning electron microscopy (SEM) and X-ray diffraction analysis. The final product of this reaction was characterized by SEM and X-ray diffraction. Crystallite size was calculated by the Scherrer equation and microdeformation was determined using Willamsom-Hall graph. With Rietveld method was possible to quantify the percentile in weight of the products obtained in the aluminothermic reaction. Semi-quantitative chemical analysis (EDS) confirmed the presence of metallic tantalum and Al2O3 as products of the reduction. As was waited the particle size of the metallic tantalum produced, presents values in nanometric scale due the short cooling time of those particles during the process

Reforma a seco de metano com catalisadores Ni/MCM-41 sintetizados a partir de fontes alternativas de sílica

The production of synthesis gas has received renewed attention due to demand for renewable energies to reduce the emissions of gases responsible for enhanced greenhouse effect. This work was carried out in order to synthesize, characterize and evaluate the implementation of nickel catalysts on MCM-41 in dry reforming reactions of methane. The mesoporous molecular sieves were synthesized using as silica sources the tetraethyl orthosilicate (TEOS) and residual glass powder (PV). The sieves were impregnated with 10% nickel to obtain the metallic catalysts (Ni/MCM-41). These materials were calcined and characterized by Thermogravimetric Analysis (TG), Infrared spectroscopy (FTIR), X-ray Diffraction (XRD), Temperature-Programmed Reduction (TPR) and N2 Adsorption/Desorption isotherms (BET/BJH). The catalytic properties of the samples were evaluated in methane dry reforming with CO2 in order to produce synthesis gas to be used in the petrochemical industry. The materials characterized showed hexagonal structure characteristic of mesoporous material MCM-41 type, being maintained after impregnation with nickel. The samples presented variations in the specific surface area, average volume and diameter of pores based on the type of interaction between the nickel and the mesoporous support. The result of the the catalytic tests showed conversions about 91% CO2, 86% CH4, yelds about 85% CO and 81% H2 to Ni/MCM-41_TEOS_C, and conversions about 87% CO2, 82% CH4, yelds about 70% CO and 59% H2 to Ni/MCM-41_PV_C. The similar performance confirms that the TEOS can be replaced by a less noble materials