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

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 influência da adição de níquel em alumina pela rota da metalurgia do pó

Ceramic materials alumina basis have been widely used in structural components, mainly because owning properties such as high hardness, chemical inertness and good wear resistance, however, the low toughness is a factor that compromises its use in many other applications, featuring the addition of nickel as a possible solution to this problem, in this context, this work aims to study the addition of nickel alumina using the route of powder metallurgy processing of the material. The percentage of nickel were added 2, 4 and 6 wt%; and each composition to high energy milling in a planetary mill was performed for 2, 4, 9 and 16h. Subsequently, the samples were compacted at 300 MPa and sintered in a vacuum oven at 1400⁰C for 2h. The samples were characterized as the physical and mechanical properties, observing, in general, an improvement in sinterability of the material with increasing grinding time and nickel content, and mixing with a decrease of porosity and increase of hardness, density values above 80% of theoretical were obtained. The milling time of 4 hours and addition of 2% nickel, particularly if achieved higher hardness (HV 1068.7 +/- 32.6) and density of about 99% theoretical density.

Estudo da influência da adição de níquel em alumina pela rota da metalurgia do pó

Ceramic materials alumina basis have been widely used in structural components, mainly because owning properties such as high hardness, chemical inertness and good wear resistance, however, the low toughness is a factor that compromises its use in many other applications, featuring the addition of nickel as a possible solution to this problem, in this context, this work aims to study the addition of nickel alumina using the route of powder metallurgy processing of the material. The percentage of nickel were added 2, 4 and 6 wt%; and each composition to high energy milling in a planetary mill was performed for 2, 4, 9 and 16h. Subsequently, the samples were compacted at 300 MPa and sintered in a vacuum oven at 1400⁰C for 2h. The samples were characterized as the physical and mechanical properties, observing, in general, an improvement in sinterability of the material with increasing grinding time and nickel content, and mixing with a decrease of porosity and increase of hardness, density values above 80% of theoretical were obtained. The milling time of 4 hours and addition of 2% nickel, particularly if achieved higher hardness (HV 1068.7 +/- 32.6) and density of about 99% theoretical density.

Estudo do efeito do tempo e do meio de moagem de alta energia para obtenção de pós nanométricos de hidretos de titânio e nióbio

Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)

Estudo de duas pseudoligas de Nb-Cu obtidas pela rota da metalurgia do pó

The Nb-Cu pseudoalloys present themselves as potential substitutes for the alloys from a well known system and already commercially applied, as the W-Cu alloys, used in applications such as heat sinks, electrical contacts and coils for the generation of high magnetic fields. Because it is an immiscible system, where there is mutual insolubility and low wettability of the liquid Cu on the Nb surface, the processing route used in this work was the Powder Metallurgy. Two Nb alloys were used, with additions of 10% and 20% in weight of Cu, and times of 20, 30 and 40 hours for the high energy milling of the starting powders. The milling evolution of the powders is presented through the characterization techniques, such as the LASER diffraction for particle size, XRD, SEM, EDS, DSC, dilatometry, TEM and chemical analysis. After the milling, portions of the loads were submitted to the annealing heat treatment. The process used for the samples consolidation was the hot pressing, which has been applied both on some milled powders samples, as on the annealed powders. Subsequent heat treatments were performed in the samples at temperatures of 1000ºC (solid phase) and 1100ºC (in the Cu liquid phase). All sets of consolidated samples, and also the two sets of the heat treated, were analyzed by XRD, SEM, EDS, density and Vickers microhardness. Moreover, other Nb powder samples with 10% and 20% in weight of Cu obtained by simple mechanical mixing, were consolidated, thermally treated and characterized with the same techniques applied to the others, and the results were compared among themselves. Despite the difficulty of consolidation and densification of the two pseudoalloys of the Nb-Cu system of this study, on the route that passes through the HEM, samples were obtained with densities around 90% of the theoretical density. And, on the processing route of which were only mixed, the values reached up to 97%. Therefore, in this work are also emphasized the processes that made possible these results.

Sinterização de aço inoxidável reforçado com partículas nanométricas dispersas de carbeto de nióbio - NbC

Metal powder sintering appears to be promising option to achieve new physical and mechanical properties combining raw material with new processing improvements. It interest over many years and continue to gain wide industrial application. Stainless steel is a widely accepted material because high corrosion resistance. However stainless steels have poor sinterability and poor wear resistance due to their low hardness. Metal matrix composite (MMC) combining soft metallic matrix reinforced with carbides or oxides has attracted considerable attention for researchers to improve density and hardness in the bulk material. This thesis focuses on processing 316L stainless steel by addition of 3% wt niobium carbide to control grain growth and improve densification and hardness. The starting powder were water atomized stainless steel manufactured for Höganäs (D 50 = 95.0 μm) and NbC produced in the UFRN and supplied by Aesar Alpha Johnson Matthey Company with medium crystallite size 16.39 nm and 80.35 nm respectively. Samples with addition up to 3% of each NbC were mixed and mechanically milled by 3 routes. The route1 (R1) milled in planetary by 2 hours. The routes 2 (R2) and 3 (R3) milled in a conventional mill by 24 and 48 hours. Each milled samples and pure sample were cold compacted uniaxially in a cylindrical steel die (Ø 5 .0 mm) at 700 MPa, carried out in a vacuum furnace, heated at 1290°C, heating rate 20°C stand by 30 and 60 minutes. The samples containing NbC present higher densities and hardness than those without reinforcement. The results show that nanosized NbC particles precipitate on grain boundary. Thus, promote densification eliminating pores, control grain growth and increase the hardness values

Sinterização de aço inoxidável reforçado com partículas nanométricas dispersas de carbeto de nióbio - NbC

Metal powder sintering appears to be promising option to achieve new physical and mechanical properties combining raw material with new processing improvements. It interest over many years and continue to gain wide industrial application. Stainless steel is a widely accepted material because high corrosion resistance. However stainless steels have poor sinterability and poor wear resistance due to their low hardness. Metal matrix composite (MMC) combining soft metallic matrix reinforced with carbides or oxides has attracted considerable attention for researchers to improve density and hardness in the bulk material. This thesis focuses on processing 316L stainless steel by addition of 3% wt niobium carbide to control grain growth and improve densification and hardness. The starting powder were water atomized stainless steel manufactured for Höganäs (D 50 = 95.0 μm) and NbC produced in the UFRN and supplied by Aesar Alpha Johnson Matthey Company with medium crystallite size 16.39 nm and 80.35 nm respectively. Samples with addition up to 3% of each NbC were mixed and mechanically milled by 3 routes. The route1 (R1) milled in planetary by 2 hours. The routes 2 (R2) and 3 (R3) milled in a conventional mill by 24 and 48 hours. Each milled samples and pure sample were cold compacted uniaxially in a cylindrical steel die (Ø 5 .0 mm) at 700 MPa, carried out in a vacuum furnace, heated at 1290°C, heating rate 20°C stand by 30 and 60 minutes. The samples containing NbC present higher densities and hardness than those without reinforcement. The results show that nanosized NbC particles precipitate on grain boundary. Thus, promote densification eliminating pores, control grain growth and increase the hardness values

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

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 da liga Ti-35Nb por metalurgia do pó para utilização em próteses ortopédicas

Pós-graduação em Engenharia Mecânica - FEG

Comparação dos efeitos de compressão isostática e compressão uniaxial na obtenção da liga NiTi por metalurgia do pó

Several alloys present the shape memory effect and among them, the equiatomic NiTi alloy, nitinol, is the most important one. It is usually used in several engineering applications and also in biomedical devices, in the fabrication of orthodontic wire, stents and Judet staples. Although a considerable amount of these biomedical devices is utilized in Brazil and a fraction of it is already made here, all nitinol used is bought abroad. Thus, it is important to develop the necessary know-how to fabricate NiTi wire and sheet. It would mean less importation with job creation and wealth generation for the country. In this work nitinol was obtained powder metallurgy from elemental powders of Ti and Ni using uniaxial compression and uniaxial compression followed by isostatic compression. The final densities achieved were determined by the Archimedes method. The precipitation of intermetallic secondary phases was studied and the samples were characterized by metallographic analysis, optical microscopy and X-ray diffraction. Results indicated that 50 hours sintering route showed a low amount of intermetallics, and no trace of unreacted powder. XRD and metallography at room temperature indicated B19’ as the predominant phase, which corresponds to martensite. Although density results showed little dispersion, the most dense sample was compacted under uniaxial compression and presented 4.8 g/cm3, corresponding to 20.84% porosity. Density variation was considered normal to the measurement process and independent of the compaction mode

Estudo de tempos e temperaturas de sinterização na obtenção da liga NiTi por metalurgia do pó

The nickel-titanium alloys are very attractive and so it is widely used in industry, engineering applications in general and also in biomedical and dental applications. Besides showing the shape of memory effect, biocompatibility and superelastic, the alloy commercially known as Nitinol, has excellent mechanical properties. Most devices used in Brazil have been produced nationally, but using imported material is also necessary, which shows the need of produce the alloy nationally. In this study we have investigated the influence of sintering temperatures and times to obtain nickel-titanium alloys by powder metallurgy alloys and the characterization of the precipitated intermetallic phases by using the post-mix of elemental nickel and titanium in proportion of 49.5% Ti - 50.5% Ni. The samples were sintered at 930ºC for periods of 30, 40 and 50 hours and were characterized by optical microscopy using metallography and x-ray diffraction. The results of the study show that the 50 hours sintering time was the most suitable time for obtaining the alloy, observing a low volume of precipitated intermetallic phases and absence of Ni and Ti residuals

Redução in situ de NIO durante a sinterização de misturas NI/NIO produzidas por metalurgia do pó

The nickel alloys are widely used in the production of various materials, especially those that require mechanical strength characteristics associated with resistance to corrosion, for example, the stainless steel. Another use is the production of nickel alloy sintered from powder of metallic nickel. A promising alternative for the production of sintered components of nickel with an important reduction in costs of starting material is the use of mixtures of powders of Ni-NiO. This work aimed to study in situ reduction of NiO during sintering mixtures of Ni / NiO produced by powder metallurgy. The nickel mixtures have been processed by the technique of powder metallurgy and were pre-sintered in an oven under plasma reducing atmosphere of hydrogen. Mixtures Ni +15%NiO, Ni +25%NiO and Ni +35%NiO were studied and compared with samples consisting only of metallic Ni. Dilatometric tests were performed to study the sintering conditions of the mixtures. The consolidated material was analyzed for their microstructure and microhardness. Dilatometry graphs showed that the addition of nickel oxide in all compositions the active sintering the mixtures studied. In tests of microhardness indentations were made at different points of the sample surface. All compositions showed microhardness values close to the consolidated material from metallic nickel. However, sample containing Ni+35% NiO, showed a large dispersion of the values of microhardness tests performed at different points of the sample surface. Microstructural analysis of the material showed a higher concentration of voids and the presence of oxides in the waste composition of the mixtures Ni 35% NiO. The samples containing Ni+15%NiO showed microstructural characteristics and mechanical properties similar to metallic nickel consolidated under the same conditions of the compositions studied in this work and therefore had great potential for production of sintered nickel alloys

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