Estudo da síntese e sinterização de pós compósitos do sistema Ta-Cu

Ta-Cu bulk composites combine high mechanical resistance of the Ta with high electrical and thermal conductivity of the Cu. These are important characteristics to electrical contacts, microwave absorber and heat skinks. However, the low wettability of Ta under Cu liquid and insolubility mutual these elements come hard sintering this composite. High-energy milling (HEM) produces composite powders with high homogeneity and refines the grain size. This work focus to study Ta-20wt%Cu composite powders prepared by mechanical mixture and HEM with two different conditions of milling in a planetary ball mill and then their sintering using hydrogen plasma furnace and a resistive vacuum furnace. After milling, the powders were pressed in a steel dye at a pressure of 200 MPa. The cylindrical samples pressed were sintered by resistive vacuum furnace at 10-4torr with a sintering temperature at 1100ºC / 60 minutes and with heat rate at 10ºC/min and were sintered by plasma furnace with sintering temperatures at 550, 660 and 800ºC without isotherm under hydrogen atmosphere with heat rate at 80ºC/min. The characterizations of the powders produced were analyzed by scanning electron microscopy (SEM), x-ray diffraction (XRD) and laser granulometry. After the sintering the samples were analyzed by SEM, XRD and density and mass loss tests. The results had shown that to high intense milling condition produced composite particles with shorter milling time and amorphization of both phases after 50 hours of milling. The composite particles can produce denser structure than mixed powders, if heated above the Cu melting point. After the Cu to arrive in the melting point, liquid copper leaves the composite particles and fills the pores

Estudo da moagem de alta energia e sinterização de pós compósitos W-Cu

The Tungsten/copper composites are commonly used for electrical and thermal objectives like heat sinks and lectrical conductors, propitiating an excellent thermal and electrical conductivity. These properties are dependents of the composition, crystallite size and production process. The high energy milling of the powder of W-Cu produces an dispersion high and homogenization levels with crystallite size of W very small in the ductile Cu phase. This work discusses the effect of the HEM in preparation of the W-25Cu composite powders. Three techniques of powder preparation were utilized: milling the dry with powder of thick Cu, milling the dry with powder of fine Cu and milling the wet with powder of thick Cu. The form, size and composition of the particles of the powders milled were observed by scanning electron microscopy (SEM). The X-ray diffraction (XRD) was used to analyse the phases, lattice parameters, size and microstrain of the crystallite. The analyse of the crystalline structure of the W-25Cu powders milled made by Rietveld Method suggests the partial solid solubility of the constituent elements of the Cu in lattice of the W. This analyse shows too that the HEM produces the reduction high on the crystallite size and the increase in the lattice strain of both phases, this is more intense in the phase W

Efeito da moagem de alta energia na microestrutura e nas propriedades magnéticas do compósito wc-10%p.Co

This work a studied the high energy milling effect in microstructure and magnetic properties of the WC-10wt.%Co composite. The composite powders were prepared by mechanical mixed and milled at 2 hours, 100 hours, 200 hours and 300 hours in planetary milling. After this process the composite were compacted in stainless steel die with cylindrical county of 10 mm of diameter, at pressure 200 Mpa and sintered in a resistive furnace in argon atmosphere at 1400 oC for 5 min. The sintered composite were cutted, inlaid, sandpapered, and polished. The microestrutural parameters of the composite was analyzed by X-ray diffraction, scanning electronic microscopy, optical microscopy, hardness, magnetic propriety and Rietveld method analyze. The results shows, with milling time increase the particle size decrease, it possibility minor temperature of sintering. The increase of milling time caused allotropic transformation in cobalt phase and cold welding between particles. The cold welding caused the formation of the particle composite. The X-ray diffraction pattern of composite powders shows the WC peaks intensity decrease with the milling time increase. The X-ray diffraction pattern of the composite sintered samples shows the other phases. The magnetic measurements detected a significant increase in the coercitive field and a decrease in the saturation magnetization with milling time increase. The increase coercitive field it was also verified with decrease grain size with milling time increase. For the composite powders the increase coercitive field it was verified with particle size reduction and saturation magnetization variation is relate with the variation of free cobalt. The Rietveld method analyze shows at milling time increase the mean crystalline size of WC, and Co-cfc phases in composite sintered sample are higher than in composite powders. The mean crystallite size of Co-hc phase in composite powders is higher than in composite sintered sample. The mean lattice strains of WC, Co-hc and Co-cfc phases in composite powders are higher than in composite sintered samples. The cells parameters of the composite powder decrease at milling time increase this effect came from the particle size reduction at milling time increase. In sintered composite the cells parameters is constant with milling time increase

Caracterização de compósitos Nb-20%cu obtidos por moagem de alta energia e sinterizados por fase líquida

In this work, was studied the formation of a composite of the refractory metal niobium with copper, through the process of high-energy milling and liquid phase sintering. The HEM can be used to synthesize composite powders with high homogeneity and fine size particle distribution. It may also produce the solid solubility in immiscible systems such as Nb-Cu, or extend the solubility of systems with limited solubility. Therefore, in the immiscible system Cu-Nb, the high-energy milling was successfully used to obtain the composite powder particles. Initially, the formation of composite particles during the HEM and the effect of preparation technique on the microstructure of the material was evaluated. Four loads of Nb and Cu powders containing 20%wt Cu were synthesized by MAE in a planetary type ball mill under different periods of grinding. The influence of grinding time on the metal particles is evaluated during the process by the withdrawal of samples at intermediate times of milling. After compaction under different forces, the samples were sintered in a vacuum furnace. The liquid phase sintering of these samples prepared by HEM produced a homogeneous and fine grained. The composite particles forming the sintered samples are the addition of a hard phase (Nb) with a high melting point, and a ductile phase (Cu) with low melting point and high thermal and electrical conductivities. Based on these properties, the Nb-Cu system is a potential material for many applications, such as electrical contacts, welding electrodes, coils for generating high magnetic fields, heat sinks and microwave absorbers, which are coupled to electronic devices. The characterization techniques used in this study, were laser granulometry, used to evaluate the homogeneity and particle size, and the X-ray diffraction, in the phase identification and to analyze the crystalline structure of the powders during milling. The morphology and dispersion of the phases in the composite powder particles, as well the microstructures of the sintered samples, were observed by scanning electron microscopy (SEM). Subsequently, the sintered samples are evaluated for density and densification. And finally, they were characterized by techniques of measuring the electrical conductivity and microhardness, whose properties are analyzed as a function of the parameters for obtaining the composite

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

Estudo da sinterização de cavacos de aço ferritico

This research studies the sintering of ferritic steel chips from the machining process. Were sintered metal powder obtained from machining process chips for face milling of a ferritic steel. The chip was produced by machining and characterized by SEM and EDS, and underwent a process of high energy mill powder characterized also by SEM and EDS. Were constructed three types of matrixes for uniaxial compression (relation l / d greater than 2.5). The differences in the design of the matrixes were essentially in the direction of load application, which for cylindrical case axial direction, while for the rectangular arrays, the longer side. Two samples were compressed with different geometries, a cylindrical and rectangular with the same compaction pressure of 700 MPa. The samples were sintered in a vacuum resistive furnace, heating rate 20 °C / min., isotherm 1300 °C for 60 minutes, and cooling rate of 25 °C / min to room temperature. The starting material of the rectangular sample was further annealed up to temperature of 800 ° C for 30 min. Sintered samples were characterized by scanning electron microscopy, optical microscopy and EDS. The sample compressed in the cylindrical matrix did not show a regular density reflecting in the sintered microstructure revealed by the irregular geometry of the pores, characterizing that the sintering was not complete, reaching only the second phase. As for the specimen compacted in the rectangular array, the analysis performed by scanning electron microscopy, optical microscopy and EDS indicate a good densification, and homogeneous microstructure in their full extent. Additionally, the EDS analyzes indicate no significant changes in chemical composition in the process steps. Therefore, it is concluded that recycling of chips, from the processed ferritic steel is feasible by the powder metallurgy. It makes possible rationalize raw material and energy by manufacture of known properties components from chips generated by the machining process, being benefits to the environment

Síntese e caracterização estrutural, magnética e térmica da hidroxiapatita dopada com ferro

In this work, composites were prepared using high energy mechanical milling from the precursors hydroxyapatite - HAp (Ca10(PO4)6(OH)2) and metallic iron ( -Fe ). The main goal here is to study composites in order to employ them in magnetic hyperthermia for cancer therapy. The produced samples were characterized by X-ray di raction (XRD), scanning electron microscopy (SEM), energy dispersive spectroscopy (EDS), magnetization curves as a function of applied eld (MxH), and nally measurements of magnetic hyperthermia. The XRD patterns of the milled samples HAp/Fe revealed only the presence of precursor materials. The SEM showed clusters with irregular shapes. The magnetization curves indicated typical cases of weak ferromagnetic behavior. For samples submitted to grinding and annealing, the identi ed phases were: HAp (Ca10(PO4)6(OH)2), hematite (Fe2O3) and Calcium Iron Phosphate (Ca9Fe(PO4)7). Analyzing the results of MxH, there was a reduction of the saturation magnetization, given that the Fe was incorporated into HAp. Hysteresis curves obtained at 300 K are characteristics of samples possessing over a phase. At 77 K, the behavior of the hysteresis curve is in uenced by the presence of hematite, which is antiferromagnetic. Already at T = 4.2 K, it is observed a weak ferromagnetic behavior. Furthermore, there is the e ect of exchange bias. Regarding the magnetic hyperthermia, the results of temperature measurements as a function of the alternating eld are promising for applications in magnetic hyperthermia and other biomedical applications.

Estudo da obtenção de cerâmica composta de alumina e beta alumina sódica utilizando-se resíduo cerâmico de velas de ignição e pó químico de extintores de incêndio

Ceramic materials the alumina base are large industrial applications. They are required for these products, specific characteristics obtained by following strict criteria during the manufacturing process. However, after life, not always these products are reused by a suitable waste management process. In ceramist context, advance research aimed at the reuse of waste aimed at obtaining ceramics and composite materials, with marked reduction of conventional raw materials. Aiming to generate scientific, technological and environmental contribution, this work studied to obtain a composite of alumina ceramic (Al2O3) and sodium beta alumina (NaAl11O17 ), and as starting materials the residue of the ceramic insulator of spark plugs, as a source alumina (Al2O3) powder and unusable sodium bicarbonate (NaHCO3) of fire extinguishers, as a source of sodium oxide (Na2O). The final ceramic product was obtained from a conventional mixture of sodium aluminum oxide in appropriate molar proportions. Sample spark plugs were obtained, discarded by lifetime, specific to a manufacturer, which, after passing through mechanical stress (grinding, magnetic purification, washing, drying and grinding the high energy), which resulted in residue powder with ceramic content of 84.34 % alumina (Al2O3), found by FRX chemical analysis, the phases present and identified by DRX. The dry chemical fire extinguisher, baking soda-based (NaHCO3) with expired, was obtained through direct collection of the waste generated during maintenance. Subjected to heat treatment at 120 °C , the NaHCO3 powder was decomposed in sodium oxide ( Na2O), which, subjected to chemical analysis (FRX) and mineralogical (DRX) revealed a content of 86.62 % sodium oxide (Na2O) . In the following steps the experimental procedure, chemical formulations were made on a molar basis of the starting material (1:9, 1:10 and 1:11 de Na2O/ Al2O3) inclusion of additives, milling parameters, sieve analysis, dilatometry, conformation of specimens, sintering in firing steps at 800 °C , 1000 °C and 1.200 °C with varying stays 30 , 60 and 120 minutes in each of the levels. The characterization of the final product was made by the following physical tests: water absorption, porosity, linear shrinkage, mineralogical analysis by DRX and microstructural analysis by MEV. A higher formation of sodium beta alumina (NaAl11O17), in sintered specimens in levels of 1.200 °C and 120 minutes, despite the prevailing coexistence of alpha phase alumina (Al2O3). From the results obtained opens up prospects for the reuse of waste studied in this work, the potter context and in other technological areas.

Estudo da obtenção de cerâmica composta de alumina e beta alumina sódica utilizando-se resíduo cerâmico de velas de ignição e pó químico de extintores de incêndio

Ceramic materials the alumina base are large industrial applications. They are required for these products, specific characteristics obtained by following strict criteria during the manufacturing process. However, after life, not always these products are reused by a suitable waste management process. In ceramist context, advance research aimed at the reuse of waste aimed at obtaining ceramics and composite materials, with marked reduction of conventional raw materials. Aiming to generate scientific, technological and environmental contribution, this work studied to obtain a composite of alumina ceramic (Al2O3) and sodium beta alumina (NaAl11O17 ), and as starting materials the residue of the ceramic insulator of spark plugs, as a source alumina (Al2O3) powder and unusable sodium bicarbonate (NaHCO3) of fire extinguishers, as a source of sodium oxide (Na2O). The final ceramic product was obtained from a conventional mixture of sodium aluminum oxide in appropriate molar proportions. Sample spark plugs were obtained, discarded by lifetime, specific to a manufacturer, which, after passing through mechanical stress (grinding, magnetic purification, washing, drying and grinding the high energy), which resulted in residue powder with ceramic content of 84.34 % alumina (Al2O3), found by FRX chemical analysis, the phases present and identified by DRX. The dry chemical fire extinguisher, baking soda-based (NaHCO3) with expired, was obtained through direct collection of the waste generated during maintenance. Subjected to heat treatment at 120 °C , the NaHCO3 powder was decomposed in sodium oxide ( Na2O), which, subjected to chemical analysis (FRX) and mineralogical (DRX) revealed a content of 86.62 % sodium oxide (Na2O) . In the following steps the experimental procedure, chemical formulations were made on a molar basis of the starting material (1:9, 1:10 and 1:11 de Na2O/ Al2O3) inclusion of additives, milling parameters, sieve analysis, dilatometry, conformation of specimens, sintering in firing steps at 800 °C , 1000 °C and 1.200 °C with varying stays 30 , 60 and 120 minutes in each of the levels. The characterization of the final product was made by the following physical tests: water absorption, porosity, linear shrinkage, mineralogical analysis by DRX and microstructural analysis by MEV. A higher formation of sodium beta alumina (NaAl11O17), in sintered specimens in levels of 1.200 °C and 120 minutes, despite the prevailing coexistence of alpha phase alumina (Al2O3). From the results obtained opens up prospects for the reuse of waste studied in this work, the potter context and in other technological areas.

Estudo da sinterização de cavacos de aço ferritico

This research studies the sintering of ferritic steel chips from the machining process. Were sintered metal powder obtained from machining process chips for face milling of a ferritic steel. The chip was produced by machining and characterized by SEM and EDS, and underwent a process of high energy mill powder characterized also by SEM and EDS. Were constructed three types of matrixes for uniaxial compression (relation l / d greater than 2.5). The differences in the design of the matrixes were essentially in the direction of load application, which for cylindrical case axial direction, while for the rectangular arrays, the longer side. Two samples were compressed with different geometries, a cylindrical and rectangular with the same compaction pressure of 700 MPa. The samples were sintered in a vacuum resistive furnace, heating rate 20 °C / min., isotherm 1300 °C for 60 minutes, and cooling rate of 25 °C / min to room temperature. The starting material of the rectangular sample was further annealed up to temperature of 800 ° C for 30 min. Sintered samples were characterized by scanning electron microscopy, optical microscopy and EDS. The sample compressed in the cylindrical matrix did not show a regular density reflecting in the sintered microstructure revealed by the irregular geometry of the pores, characterizing that the sintering was not complete, reaching only the second phase. As for the specimen compacted in the rectangular array, the analysis performed by scanning electron microscopy, optical microscopy and EDS indicate a good densification, and homogeneous microstructure in their full extent. Additionally, the EDS analyzes indicate no significant changes in chemical composition in the process steps. Therefore, it is concluded that recycling of chips, from the processed ferritic steel is feasible by the powder metallurgy. It makes possible rationalize raw material and energy by manufacture of known properties components from chips generated by the machining process, being benefits to the environment