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

Nitretação em plasma com gaiola catódica: investigação do mecanismo e estudo comparativo com a nitretação em plasma de tensão contínua

The ionic plasma nitriding is one of the most important plasma assisted treatment technique for surface modification, but it presents some inherent problems mainly in nitriding pieces with complex geometries. In the last four years has appeared a plasma nitriding technique, named ASPN (Active Screen Plasma Nitriding) in which the samples and the workload are surrounded by a metal screen on which the cathodic potential is applied. This new technique makes possible to obtain a perfect uniform nitrided layer apart from the shape of the samples. The present work is based on the development of a new nitriding plasma technique named CCPN (Cathodic Cage Plasma Nitriding) Patent PI 0603213-3 derived from ASPN, but utilizes the hollow cathode effect to increase the nitriding process efficiency. That technique has shown great improvement on the treatment of several types of steels under different process conditions, producing thicker and harder layers when compared with both, ASPN and ionic plasma nitriding, besides eliminating problems associated with the later technique. The best obtained results are due to the hollow cathode effect on the cage holes. Moreover, characteristic problems of ionic plasma nitriding are eliminated due to the fact that the luminescent discharge acts on the cage wall instead of on the samples surface, which remains under a floating potential. In this work the enhancement of the cathodic cage nitriding layers proprieties, under several conditions for some types of steels was investigated, besides the mechanism for nitrides deposition on glass substrate, concluding that the CCPN is both a diffusion and a deposition process at the same time

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

Obtenção de polímeros de LCC para aplicação como antioxidante de biodiesel de soja

Biodiesel is a fuel obtained from vegetable oils, such as soy, castorbean, among others. The monoester of fatty acid of these oils have chains with mono, di and tri double connections. The presence of these insaturations are susceptible to oxidization. Antioxidants are substances able to prevent oxidization from oils, fats, fat foods, as well as esters of Alquila( biodiesel). The objective of this work is to summarize a new antioxidant from the Cashew Nut Shell Liquid (CNSL) using the electrolysis technique. A current of 2 amperes was used in a single cell of only one group and two eletrodos of stainless steel 304 in a solution of methanol, together with the eletrolits: acetic acid, sodium chloride and sodium hydroxide, for two hours of agitation. The electrolysis products are characterized by the techniques of cromatography in a thin layer, spectroscopy of infrared and gravimetric analysis. The material was submitted to tests of oxidative stability made by the techniques of spectropy of impendancy and Rancimat (EN 14112). The analyses of characterization suggest that the polimerization of the electrolytic material ocurred. The application results of these materials as antioxidants of soy biodiesel showed that the order of the oxidative stability was obtained by both techniques used

Estudo da viabilidade técnica para obtenção de superfície duplex em aço inoxidável martensítico AISI 410 através do processo de deposição a plasma por gaiola catódica

The technique of plasma nitriding by the cathode cage mainly stands out for its ability to produce uniform layers, even on parts with complex geometries. In this study, it was investigated the efficiency of this technique for obtaining duplex surface, when used, simultaneously, to nitriding treatment and thin film deposition at temperatures below 500°C. For this, were used samples of AISI 41 0 Martensitic Stainless Steel and performed plasma treatment, combining nitriding and deposition of thin films of Ti and/or TiN in a plasma atmosphere containing N2-H2. It was used a cathodic cage of titanium pure grade II, cylindrical with 70 mm diameter and 34 mm height. Samples were treated at temperature 420ºC for 2 and 12 hours in different working pressures. Optical Microscopy (OM), Scanning Electron Microscopy (SEM) with micro-analysis by Energy Dispersive Spectroscopy (EDS), X-Ray Diffraction (XRD), Atomic Force Microscopy (AFM) and analysis of Vickers Microhardness were used to investigate coating properties such as homogeneity and surface topography, chemical composition, layer thickness, crystalline phase, roughness and surface microhardness. The results showed there is a direct proportionality between the presence of H2 in plasma atmosphere and the quantity of titanium in surface chemical composition. It was also observed that the plasma treatment at lowpressure is more effective in formation of TiN thin film

Desenvolvimento e caracterização de um compósito matriz metálica (CMM): aço EUROFER97 reforçado com Carbeto de Tântalo - TaC

Steel is an alloy EUROFER promising for use in nuclear reactors, or in applications where the material is subjected to temperatures up to 550 ° C due to their lower creep resistance under. One way to increase this property, so that the steel work at higher temperatures it is necessary to prevent sliding of its grain boundaries. Factors that influence this slip contours are the morphology of the grains, the angle and speed of the grain boundaries. This speed can be decreased in the presence of a dispersed phase in the material, provided it is fine and homogeneously distributed. In this context, this paper presents the development of a new material metal matrix composite (MMC) which has as starting materials as stainless steel EUROFER 97, and two different kinds of tantalum carbide - TaC, one with average crystallite sizes 13.78 nm synthesized in UFRN and another with 40.66 nm supplied by Aldrich. In order to improve the mechanical properties of metal matrix was added by powder metallurgy, nano-sized particles of the two types of TaC. This paper discusses the effect of dispersion of carbides in the microstructure of sintered parts. Pure steel powders with the addition of 3% TaC UFRN and 3% TaC commercial respectively, were ground in grinding times following: a) 5 hours in the planetary mill for all post b) 8 hours of grinding in the mill Planetary only for steel TaC powders of commercial and c) 24 hours in the conventional ball mill mixing the pure steel milled for 5 hours in the planetary mill with 3% TaC commercial. Each of the resulting particulate samples were cold compacted under a uniaxial pressure of 600MPa, on a cylindrical matrix of 5 mm diameter. Subsequently, the compressed were sintered in a vacuum furnace at temperatures of 1150 to 1250 ° C with an increment of 20 ° C and 10 ° C per minute and maintained at these isotherms for 30, 60 and 120 minutes and cooled to room temperature. The distribution, size and dispersion of steel and composite particles were determined by x-ray diffraction, scanning electron microscopy followed by chemical analysis (EDS). The structures of the sintered bodies were observed by optical microscopy and scanning electron accompanied by EDS beyond the x-ray diffraction. Initial studies sintering the obtained steel EUROFER 97 a positive reply in relation to improvement of the mechanical properties independent of the processing, because it is obtained with sintered microhardness values close to and even greater than 100% of the value obtained for the HV 333.2 pure steel as received in the form of a bar

Estudo da influência da temperatura de brasagem nas uniões zircônia/aço inox 304 utilizando metalização mecânica

Metal-Ceramic (M/C) Zirconia-stainless steel interfaces have been processed through brazing techniques due to the excellent combination of properties such as high temperature stability, high corrosion resistance and good mechanical properties. However, some M/C interfaces show some defects, like porosity and cracks results in the degradation of the interfaces, leading even to its total rupture. Most of time, those defects are associated with an improper brazing parameters selection to the M/C system. In this work, ZrO2 Y-TZP and ZrO2 Mg - PSZ were joint with the stainless steel grade 304 by brazing using a eutectic silver-copper (Ag28Cu) interlayer alloy with different thermal cycles. Ceramic surfaces were previous mechanically metallized with titanium to improve adhesion of the system. The effect of temperature on the M/C interface was studied. SEM-EDS and 3 point flexural bend test were performed to evaluate morphology, chemical composition and mechanical resistance of the M/C interfaces. Lower thermal cycle temperatures produced better results of mechanical resistance, and more regular/ homogeneous reaction layers between braze alloy and metal-ceramic surfaces. Also was proved the AgCu braze alloy activation in situ by titanium

Dynamic mechanical-thermal, microstructural and mechanical analysis of ultra-light polymer-metal composites: influence of forming

A really particular and innovative metal-polymer sandwich material is Hybrix. Hybrix is a product developed and manufactured by Lamera AB, Gothenburg, Sweden. This innovative hybrid material is composed by two relatively thin metal layers if compared to the core thickness. The most used metals are aluminum and stainless steel and are separated by a core of nylon fibres oriented perpendicularly to the metal plates. The core is then completed by adhesive layers applied at the PA66-metal interface that once cured maintain the nylon fibres in position. This special material is very light and formable. Moreover Hybrix, depending on the specific metal which is used, can achieve a good corrosion resistance and it can be cut and punched easily. Hybrix architecture itself provides extremely good bending stiffness, damping properties, insulation capability, etc., which again, of course, change in magnitude depending in the metal alloy which is used, its thickness and core thickness. For these reasons nowadays it shows potential for all the applications which have the above mentioned characteristic as a requirement. Finally Hybrix can be processed with tools used in regular metal sheet industry and can be handled as solid metal sheets. In this master thesis project, pre-formed parts of Hybrix were studied and characterized. Previous work on Hybrix was focused on analyze its market potential and different adhesive to be used in the core. All the tests were carried out on flat unformed specimens. However, in order to have a complete description of this material also the effect of the forming process must be taken into account. Thus the main activities of the present master thesis are the following: Dynamic Mechanical-Thermal Analysis (DMTA) on unformed Hybrix samples of different thickness and on pre-strained Hybrix samples, pure epoxy adhesive samples analysis and finally moisture effects evaluation on Hybrix composite structure.

Sistema de instrumentação mecanizada Hyflex EDM

A Endodontia é uma área em constante evolução. Consideráveis desenvolvimentos nos materiais e técnicas têm sido essenciais para o melhoramento dos resultados nos tratamentos realizados. É exemplo disso mesmo a constituição dos instrumentos Endodônticos primordiais, construídos em cordas de piano, com evolução para aço de carbono, material este que sofria corrosão provocado pelo cloro presente no hipoclorito de sódio. O aço de carbono evoluiu para aço inoxidável e deste as limas endodônticas passaram a ser feitas em níquel-titânio, conferindo-lhes melhor flexibilidade e efeito de memória de forma. Mesmo com todas estas melhorias significativas, fraturas de instrumentos e erros durante a instrumentação continuam a acontecer e com eles veio a necessidade da pesquisa de possíveis melhorias da constituição das limas em NiTi. Como resultado surgiram ligas como o M-wire, fase-R e CM-wire, criadas a partir de tratamentos térmicos, que trouxeram às limas Endodônticas maior flexibilidade e resistência à fratura que os instrumentos feitos em NiTi convencional. A mais recente evolução das limas Ni-Ti, desenvolvida pela Coltene Whaldent (Allstätten, Suiça), são as limas Hyflex EDM, limas para canais radiculares de 5ª geração. O seu processo de fabrico por eletroerosão cria uma superfície única fazendo com que estas limas sejam mais duras e resistam mais à quebra, aliado à sua alta flexibilidade. É possível assim reduzir o número de limas para a limpeza e modelagem dos canais durante os tratamentos endodônticos sem comprometer a preservação da anatomia dos canais. As limas Hyflex EDM possuem, tal como as limas Hyflex CM, o efeito de controle de memória (CM), o que confere propriedades muito similares entre os dois sistemas.

Finite element modeling of tube deformation during cold pilgering

A three-dimensional finite element model of cold pilgering of stainless steel tubes is developed in this paper. The objective is to use the model to increase the understanding of forces and deformations in the process. The focus is on the influence of vertical displacements of the roll stand and axial displacements of the mandrel and tube. Therefore, the rigid tools and the tube are supported with elastic springs. Additionally, the influences of friction coefficients in the tube/mandrel and tube/roll interfaces are examined. A sensitivity study is performed to investigate the influences of these parameters on the strain path and the roll separation force. The results show the importance of accounting for the displacements of the tube and rigid tools on the roll separation force and the accumulative plastic strain.

Additive Manufacturing by LPBF and WAAM of metals: correlation between production process, microstructure and mechanical properties

In the most recent years, Additive Manufacturing (AM) has drawn the attention of both academic research and industry, as it might deeply change and improve several industrial sectors. From the material point of view, AM results in a peculiar microstructure that strictly depends on the conditions of the additive process and directly affects mechanical properties. The present PhD research project aimed at investigating the process-microstructure-properties relationship of additively manufactured metal components. Two technologies belonging to the AM family were considered: Laser-based Powder Bed Fusion (LPBF) and Wire-and-Arc Additive Manufacturing (WAAM). The experimental activity was carried out on different metals of industrial interest: a CoCrMo biomedical alloy and an AlSi7Mg0.6 alloy processed by LPBF, an AlMg4.5Mn alloy and an AISI 304L austenitic stainless steel processed by WAAM. In case of LPBF, great attention was paid to the influence that feedstock material and process parameters exert on hardness, morphological and microstructural features of the produced samples. The analyses, targeted at minimizing microstructural defects, lead to process optimization. For heat-treatable LPBF alloys, innovative post-process heat treatments, tailored on the peculiar hierarchical microstructure induced by LPBF, were developed and deeply investigated. Main mechanical properties of as-built and heat-treated alloys were assessed and they were well-correlated to the specific LPBF microstructure. Results showed that, if properly optimized, samples exhibit a good trade-off between strength and ductility yet in the as-built condition. However, tailored heat treatments succeeded in improving the overall performance of the LPBF alloys. Characterization of WAAM alloys, instead, evidenced the microstructural and mechanical anisotropy typical of AM metals. Experiments revealed also an outstanding anisotropy in the elastic modulus of the austenitic stainless-steel that, along with other mechanical properties, was explained on the basis of microstructural analyses.

Joints and innovative components for automotive applications

The research activities described in this thesis were focused on two main topics: the study of shaft-hub joint performance, with particular regard to interference-fitted and adhesively bonded connection, and the fatigue characterization of additively processed metal alloys. The research on interference-fitted shaft-hub joints dealt with some studies in the field of fretting fatigue. Rotating bending fatigue tests were performed on different materials by not conventional specimens to determine the fatigue properties of interference-fitted joints and to investigate the fretting fatigue phenomenon, which led to novel and original results. In adhesively bonded and interference-fitted shaft-hub connections (called hybrid joints) the synergic effect of anaerobic adhesive and interference has the capability of improving the joint strength. However, the adhesive contribution depends on several factors. Therefore, its behavior was investigated for different coupling pressure, coupling procedure, operating temperature and joint design. The study on additively manufactured metal alloy deals with rotating banding fatigue tests. AlSi10Mg and Maraging Stainless Steel CX were involved in the campaign for their wide applicability in Automotive. Build direction, heat and surface treatments were considered as input parameters. Fatigue results were interpreted by statistical method and microscopy analyses in order to determine the effectiveness and the beneficial or detrimental effects of the considered factors. Fracture mode and microstructure were investigated by fractographic and micrographic analyses

Laser cladding and its potential to reduce particulate matter emissions from the automotive and locomotive sector

Laser Cladding (LC) is an emerging technology which is used both for coating applications as well as near-net shape fabrication. Despite its significant advantages, such as low dilution and metallurgical bond with the substrate, it still faces issues such as process control and repeatability, which restricts the extension to its applications. The following thesis evaluates the LC technology and tests its potential to be applied to reduce particulate matter emissions from the automotive and locomotive sector. The evaluation of LC technology was carried out for the deposition of multi-layer and multi-track coatings. 316L stainless steel coatings were deposited to study the minimisation of geometric distortions in thin-walled samples. Laser power, as well as scan strategy, were the main variables to achieve this goal. The use of constant power, reduction at successive layers, a control loop control system, and two different scan strategies were studied. The closed-loop control system was found to be practical only when coupled with the correct scan strategy for the deposition of thin walls. Three overlapped layers of aluminium bronze were deposited onto a structural steel pipe for multitrack coatings. The effect of laser power, scan speed and hatch distance on the final geometry of coating were studied independently, and a combined parameter was established to effectively control each geometrical characteristic (clad width, clad height and percentage of dilution). LC was then applied to coat commercial GCI brake discs with tool steel. The optical micrography showed that even with preheating, the cracks that originated from the substrate towards the coating were still present. The commercial brake discs emitted airborne particles whose concentration and size depended on the test conditions used for simulation in the laboratory. The contact of LC cladded wheel with rail emitted significantly less ultra-fine particles while maintaining the acceptable values of coefficient of friction.

High-strength steels manufactured via Laser Powder Bed Fusion: effect of post-process heat treatments and surface finishing on microstructure and mechanical properties

Laser Powder Bed Fusion (LPBF) permits the manufacturing of parts with optimized geometry, enabling lightweight design of mechanical components in aerospace and automotive and the production of tools with conformal cooling channels. In order to produce parts with high strength-to-weight ratio, high-strength steels are required. To date, the most diffused high-strength steels for LPBF are hot-work tool steels, maraging and precipitation-hardening stainless steels, featuring different composition, feasibility and properties. Moreover, LPBF parts usually require a proper heat treatment and surface finishing, to develop the desired properties and reduce the high roughness resulting from LPBF. The present PhD thesis investigates the effect of different heat treatments and surface finishing on the microstructure and mechanical properties of a hot-work tool steel and a precipitation-hardening stainless steel manufactured via LPBF. The bibliographic section focuses on the main aspects of LPBF, hot-work tool steels and precipitation-hardening stainless steels. The experimental section is divided in two parts. Part A addresses the effect of different heat treatments and surface finishing on the microstructure, hardness, tensile and fatigue behaviour of a LPBF manufactured hot-work tool steel, to evaluate its feasibility for automotive and racing components. Results indicated the possibility to achieve high hardness and strength, comparable to the conventionally produced steel, but a great sensitivity of fatigue strength on defects and surface roughness resulting from LPBF. Part B investigates the effect of different heat treatments on the microstructure, hardness, tensile and notch-impact behaviour of a LPBF produced precipitation-hardening stainless steel, to assess its feasibility for tooling applications. Results indicated the possibility to achieve high hardness and strength also through a simple Direct Aging, enabling heat treatment simplification by exploiting the microstructural features resulting from LPBF.

Characterization Of Single Use Reactor Used For The Manufacturing Of Formulated Products Within The Pharmaceutical Industry

Mixing is a fundamental unit operation in the pharmaceutical industry to ensure consistent product quality across different batches. It is usually carried out in mechanically stirred tanks, with a large variety of designs according to the process requirements. A key aspect of pharmaceutical manufacturing is the extensive and meticulous cleaning of the vessels between runs to prevent the risk of contamination. Single-use reactors represent an increasing trend in the industry since they do not require cleaning and sterilization, reducing the need for utilities such as steam to sterilize equipment and the time between production batches. In contrast to traditional stainless steel vessels, single-use reactors consist of a plastic bag used as a vessel and disposed of after use. This thesis aims to characterize the fluid dynamics features and the mixing performance of a commercially available single-use reactor. The characterization employs a combination of various experimental techniques. The analysis starts with the visual observation of the liquid behavior inside the vessel, focusing on the vortex shape evolution at different impeller speeds. The power consumption is then measured using a torque meter to quantify the power number. Particle Image Velocimetry (PIV) is employed to investigate local fluid dynamics properties such as mean flow field and mean and rms velocity profiles. The same experimental setup of PIV is exploited for another optical measurement technique, the Planar Laser-Induced Fluorescence (PLIF). The PLIF measurements complete the characterization of the reactor with the qualitative visualization of the turbulent flow and the quantitative assessment of the system performance through the mixing time. The results confirm good mixing performances for the single-use reactor over the investigated impeller speeds and reveal that the filling volume plays a significant role in the fluid dynamics of the system.