Dissertations / Theses on the topic 'Sinter (Metallurgy) Powder metallurgy'

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Tese (Doutoramento)
IPEN/T
Instituto de Pesquisas Energeticas e Nucleares - IPEN/CNEN-SP

The pores in pressed and sintered components constitute weak points in the material since the stress concentration is larger than the nominal stress there. Therefore, fatigue cracks initiate at the pores. Specifically, it can be assumed that the fatigue cracks initiate at the largest pore in the stressed volume. Studies have previously looked at finding ways to model the fatigue strength of the material based on the largest pore. This thesis looks at a model previously derived for hardened pressed and sintered materials that is based on linear elastic fracture mechanics and investigates if said model can be modified to include non-hardened pressed and sintered materials that do not necessarily behave linear elastically. A model describing the influence of the size of the largest pore on the fatigue limit using empirical coefficients is suggested. Furthermore, the area of the largest pore is modelled using extreme value statistics. The model proved successful in modelling the density effect of the porosity on the fatigue strength for two materials with different microstructures: one with a homogeneous microstructure and one with a heterogeneous microstructure. For the material with the homogenoeous microstructure the model also accounted well for the notch effect when tested on samples with a different geometry. However, for the heterogeneous material the model did not account for the notch effect. Deformation hardening due to local plastic deformation in the softer phases was suggested as a possible explanation and was supported by tensile tests.

O objetivo principal do projeto foi desenvolver, através da metalurgia do pó (M/P), núcleos para transformadores monofásicos de baixa potência. O processo compreende o desenvolvimento de ligas metálicas utilizando pós de ferro, níquel e resina fenólica HRJ. Essas ligas foram misturadas, compactadas e sinterizadas ou curadas, conforme o tipo de liga. Após a confecção dos protótipos, foram feitos testes relacionados às características eletromagnéticas. A partir dos resultados obtidos puderam-se fazer comparações entre um transformador convencional, construído com um núcleo de chapas laminadas de Fe-Si com os núcleos maciços confeccionados utilizando-se a metalurgia do pó. Entre os transformadores construídos a partir da metalurgia do pó, também puderam ser observados os comportamentos com núcleos formados a partir de pó de ferro, liga de ferro e níquel, que foram sinterizados e ainda uma liga de ferro com 1% de resina fenólica HRJ que foi curada para obtenção do núcleo magnético.
The main goal this design was to develop, through process of powder Metallurgy, single-phase transformer cores for low Power. The process include the development alloys using powders of iron, nickel and phenolic resin HRJ. These alloys were mixed, compacted and sintered or cured, according to the type of alloy. After the prototype creation, tests were made related to the electromagnetic characteristics. When the results were ready comparisons were made between a conventional transformer, built with a Fe-Si rolled sheet core and bulky cores made using the powder metallurgy. Between transformers built from the powder metallurgy, could also be observed behaviors with cores formed from iron powder, iron and nickel alloy that was sintered and observed too an iron alloy with 1% phenolic resin HRJ was cured to obtain the magnetic core.

Die exzellenten Eigenschaften einer Keramik beziehen sich auf den hohen Schmelzpunkt, die gute Hochtemperaturfestigkeit sowie hohe Elastizitätsmodul- und Härtewerte. Weiterhin zeichnen sich die anorganisch-nichtmetallischen Werkstoffebesonders durch ihre gute Korrosions- und Verschleißbeständigkeit aus.Bedingt durch die erschwerte Versetzungsbewegung weisen keramische Werkstoffeeine höhere Sprödigkeit auf. Metallische Werkstoffedagegen sind in der Regel duktil und zeigen meist ein duktiles Bruchverhalten. Lokale Spannungsspitzen können durch plastische Verformung abgebaut werden.Das Ziel dieser Arbeit ist es, das grundsätzlich unterschiedliche Werkstofferhalten einer Keramik und eines Metalls miteinander zu kombinieren, um die Bruchzähigkeit des Keramik-Metall-Verbundwerkstoffes zu erhöhenDie fein verteilten Metalle sollen die Rissausbreitung behindern. Es können unterschiedliche Mechanismen wirken. Im Vergleich zur unverstärkten Keramik ist eine höhere Bruchenergie aufzubringen, um den Riss voran zu treiben. Die Erhöhung der Bruchenergie spiegelt sich in einer höheren Bruchzähigkeit wieder.Um eine duktile Phase in einer spröden Zirkoniumdioxidmatrix zu erzeugen, werden für die Untersuchungen unterschiedliche Metalle eingebracht. Dadurch soll die Bruchzähigkeit als Schadenstoleranz gegenüber dem Totalversagen erhöht werden. Die resultierenden Eigenschaften der Keramik-Metall-Verbundwerkstoffewerden analysiert und charakterisiert.Die Untersuchungen umfassen das pulvermetallurgische Einbringen von metallischen Pulvern mit verschiedenen Teilchengrößen sowie die chemische Einbringung von Präkursoren, die in nanokristalline Metallpartikel umgewandelt werden. Dabei kommen verschiedene Metalle mit unterschiedlichen Wechselwirkungen und Spannungen durch thermische Fehlpassungen in der Matrix zur Anwendung. Zusätzlich wird die Auswirkung der Variation der Verstärkungsform (Partikel/Faser) und des Metallgehaltes untersucht.

Este trabalho tem por objetivo a utilização do núcleo de estator de uma máquina elétrica construído a partir do processo da Metalurgia do Pó utilizando a liga ferro com 2% fósforo (Fe2%P). O núcleo obtido substitui o núcleo comercial (laminado) do gerador síncrono de imãs permanentes com potência de 1kW. O gerador elétrico utilizado no trabalho é encontrado em geradores eólicos de pequeno porte. Esta máquina elétrica é um gerador com fluxo axial excitado através de imãs permanentes, sendo nomeada de Torus por utilizar um núcleo em formato toroidal. Foram realizados ensaios de rendimento do gerador em bancada com ambos os núcleos, comercial e o concebido a partir de metalurgia do pó. Com estes ensaios foi possível a comparação do desempenho da máquina com os dois núcleos. O núcleo do estator obtido pelo processo de metalurgia do pó obteve rendimentos elétricos equivalentes ao da máquina utilizando núcleo comercial, porém durante o teste em vazio o gerador com núcleo de Fe2%P apresentou uma potência mecânica de acionamento superior a máquina utilizando núcleo comercial. A máquina com núcleo comercial possui uma eficiência geral de no mínimo oito por cento superior a máquina que utiliza núcleo do estator com Fe2%P.
The purpose of this paper is to use the stator core of an electrical machine built from the Powder Metallurgy process using iron alloy with 2% (Fe 2% P). The core obtained replaces the commercial core (laminated) of the synchronous generator with permanent magnet power of 1kW. The electric generator used at work is found in small wind generators. This electric machine is a generator with an axial flow excited by permanent magnets that have been named Torus for using a core in the toroidal format. Bench Generator performance tests were conducted with both the commercial and the powder metallurgy designed cores. With these tests, a comparison between the machine’s performance and both cores was possible. The stator core obtained by the powder metallurgy process achieved an electrical performance equivalent to that of the machine using the commercial core, however, during the no load test, the generator with the Fe2% P core presented a higher mechanical power drive to that of the machine using the commercial core. The machine with a commercial core has an overall efficiency of at least eight per cent higher than that of the machine that uses the stator core with Fe2%P.

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Atualmente, uns dos grandes desafios para a indústria automobilística é aumentar o desempenho do conjunto mecânico responsável por selar a câmara de combustão interna de motores automotivos e também reduzir os seus custos de obtenção. O objetivo deste trabalho foi o de tratar termicamente insertos de assentos de válvulas (do inglês valve seat insert, VSI) obtidos pela rota de metalurgia do pó. Esta técnica possibilitou a substituição do cobalto e do chumbo, devido ao seu elevado custo e efeito toxicológico, respectivamente. Ao longo do trabalho foram avaliados VSI obtidos com três misturas de pós diferentes, sendo que os elementos comuns nestas três misturas foram os pós de ferro, sulfeto de manganês, carboneto de nióbio, grafite, estearato de zinco e cobre. Em cada uma destas misturas variou-se apenas os tipos de pós de aços rápidos e aço ferramenta utilizado, sendo estes o aço rápido AISI M3:2 (Mistura 1), aço rápido AISI M2 (Mistura 2) e aço ferramenta AISI D2 (Mistura 3). Os tratamentos térmicos aplicados aos VSI consistiram em têmpera ao ar e têmpera ao óleo, ambas seguidas de duplo revenimento em sete temperaturas equidistantemente diferentes, variando de 100 °C a 700 °C. Os ciclos dos tratamentos térmicos foram determinados por meio da utilização de termopares do tipo k acoplados à um sistema de aquisição de dados. As propriedades físicas e mecânicas dos VSI foram determinadas através da dureza aparente, densidade aparente e resistência à ruptura radial. A caracterização microestrutural foi realizada utilizando-se a microscopia óptica e microscopia eletrônica de varredura. A composição química foi determinada por meio da análise elementar e por espectrometria de fluorescência de energia dispersiva de raios X. Os melhores resultados em relação às propriedades mecânicas dos VSI foram obtidas para os insertos temperados ao ar e duplamente revenido a 600 °C para a Mistura 1 e Mistura 2, e a 500 °C para Mistura 3. Já para a têmpera ao óleo, as melhores respostas foram para os VSI obtidos com a Mistura 1 duplamente revenida a 400 °C e a, 300 °C para os componentes obtidos com a Mistura 2 e Mistura 3.
Dissertação (Mestrado em Tecnologia Nuclear)
IPEN/D
Instituto de Pesquisas Energéticas e Nucleares - IPEN-CNEN/SP

In the present study
the effects of the powder metallurgical parameters such as the mixing method, compaction pressure, initial tungsten (W) particle size, composition, sintering temperature and sintering time on the sintering behavior of selected high density W-Ni-Cu alloys were investigated. The alloys were produced through conventional powder metallurgy route of mixing, cold compaction and sintering. The total solute (Ni-Cu) content in the produced alloys was kept constant at 10 wt%, while the copper concentration of the solutes was varied from 2.5 wt% to 10 wt%. Mainly liquid phase sintering method was applied in the production of the alloys. The results of the study were based on the density measurements, microstructural characterizations including optical and scanning electron microscopy and mechanical characterizations including hardness measurements. The results showed that the nature of the mixing method applied in the preparation of the powder mixtures has a considerable effect on the final sintered state of W-Ni-Cu alloys. Within the experimental limits of the study, the compaction v pressure and initial W particle size did not seem to affect the densification behavior. It was found that the sintering behavior of W-Ni-Cu alloys investigated in this study was essentially dominated by the Ni content in the alloy and the sintering temperature. A high degree of densification was observed in these alloys with an increase in the Ni content and sintering temperature which was suggested to be due to an increase in the solubility and diffusivity of W in the binder matrix phase with an increase in these parameters, leading to an increase in the overall sintering kinetics. Based on the results obtained in the present study, a model explaining the kinetics of the diffusional processes governing the densification and coarsening behavior of W-Ni-Cu alloys was proposed.

Ve všeobecnosti, poznatky o design slitin, jejich výrobě a výběru legujúcich prvků sú omezené na slitiny s jedním základním prvkem. Tento fakt ale výrazně limituje možnosti a volnost výběru prvků pro dosáhnuti speciálních vlastností a mikrostruktur. V poslední dekádě se ukázalo, že materiálová věda a inženýrství nejsou ještě zdaleka prozkoumané v důsledku objevu nové třídy materiálů nazvané vysoko entropické slitiny (HEA high entropy alloys). Jejich objev upoutal pozornost vědecké komunity. Základní koncept pro jejich design je, že namísto jednoho, nebo dvou základních prvků obsahují minimálně 5 prvků v podobných atomových koncentracích. V posledních letech se objevila skupina materiálů odvozená od HEA, nazvaná slitiny so střednou entropii (MEA medium entropy alloys). Na rozdíl od HEA ale obsahují 3, nebo 4 prvky. Táto práce je věnovaná studiu přípravy a charakterizaci HEA, MEA a jejich kompozitů s pomocí metod práškové metalurgie. V této práci byli dohromady zkoumány tři kompozice: AlCoCrFeNiTi0.5, Co1.5Ni1.5CrFeTi0.5 a CoCrNi, kompozity s kovovou matricí (MMC metal matrix composites) vyztužené částicemi B4C s CoCrNi jako matricí. Hloubková mikrostrukturní a mechanická analýza těchto materiálů byla provedena pomoví metod rastrovací a transmisní elektronové mikroskopie spojené s tahovými a ohybovými zkouškami. V průběhu celé studie se objevovaly problémy s kontaminací kyslíkem, co se projevilo vznikem značného množství oxidů v připravených materiálech. U Slitiny AlCoCrFeNiTi0.5 byla naměřena tvrdost přesahující 800 HV. Její houževnatost ale byla velice omezena. V její mikrostruktuře byly identifikovány částice in-situ TiC v důsledku přítomnosti organického, anti-aglomeračního činidla (metanolu) v mlecí misce. Tato reakce může být použita v budoucnu k přípravě MMC se záměrnou disperzí TiC. Na druhé straně, slitina CoCrNi ukázala vysoké hodnoty tažnosti (26%) a meze pevnosti přes 1000 MPa. Mikrostruktura obsahovala majoritní FCC fázi s BCC precipitáty. Tahle slitina byla z důvodu vysoké tažnosti zvolena pro přípravu kompozitu s výztuží B4C. V průběhu slinování ale došlo k reakci mezi přítomným Cr a B4C, které výsledkem byl Cr5B3 borid. Tento kompozit mel pevnost v tahu 1400 MP a extrémne jemnozrnnou strukturu. Celková tažnost ale klesla na 1.9 %. Slitina AlCoCrFeNiTi0.5, která mela strukturu složenou jen z FCC tuhého roztoku dosáhla nejlepší kombinaci mechanických vlastností s pevností přesahující 1300 MPa a dostatečnou tažností 4%. Prášková metalurgie se ukázala jako vhodná metoda pro přípravu HEA a MEA slitin a jejich kompozitů, s dobrou kombinací pevnosti a tažnosti. Tato metoda dovoluje měnit mikrostrukturní parametry připravených materiálů jednoduchou úpravou parametrů procesu.

Vývoj nových materiálů pro součásti v moderních technologiích vystavené extrémním podmínkám má v současné době rostoucí význam. Děje se tak v důsledku neustále se zvyšujících požadavků průmyslových odvětví na lepší konstrukční vlastnosti nosných materiálů. Ve světle těchto faktů si tato studie klade za cíl posoudit nové složení slitin s vysokou entropií, které se vyznačují vysokým aplikačním potenciálem pro kritické aplikace. Slitiny jsou připravovány práškovou metalurgií, t.j. kombinací mechanického legování a slinování v pevné fázi. Pro účely srovnávaní vlastností jsou vybrané kompozice vyrobeny také tradičními metalurgickými metodami v roztaveném stavu, jako je vakuové indukční tavení a následné lití nebo vakuové obloukové tavení. Prášková metalurgie umožňuje postupný vývoj kompozitů s kovovou matricí (MMC) prostřednictvím přípravy oxidicky zpevněných HEA slitin. To je možné díky inherentním in-situ reakcím během procesu výroby. Když se naopak zvolí výrobní postup z taveniny, připravený kovový materiál vykazuje velké rozdíly v mikrostrukturách a souvisejících vlastnostech, v porovnání se stejným materiálem vyrobeným práškovou cestou (PM). Vyrobené práškové a tavené materiály jsou detailně charakterizovány s ohledem na komplexní vyhodnocení vlivu různých metod zpracování. Práce se zejména orientuje na mikrostrukturní charakteristiky materiálů a jejich mechanické vlastnosti, včetně vlivu tepelného zpracování na fázové transformaci a mikrostrukturní stabilitu připravených materiálů.

The mechanisms involved in the production of chromate-phosphate conversion coatings on aluminium have been investigated. A sequence of coating nucleation and growth has been outlined and the principle roles of the constituent ingredients of the chromate-phosphate solution have been shown. The effect of dissolved aluminium has been studied and its role in producing sound conversion coatings has been shown. Metallic contamination has been found to have a dramatic influence on chromate-phosphate coatings when particular levels have been exceeded. Coating formation was seen to be affected in proportion to the level of contaminaton; no evidence of sudden failure was noted. The influence of substrate and the effect of an acidic cleaner prior to conversion coating have been studied and explained. It was found that the cleaner ages rapidly and that this must .be allowed for when attempting to reproduce industrial conditions in the laboratory. A study was carried out on the flowing characteristics of polyester powders of various size distributions as they melt using the hot-stage microscopy techniques developed at Aston. It was found that the condition of the substrate (ie extent of pretreatment), had a significant effect on particle flow. This was explained by considering the topography of the substrate surface. A number of 'low-bake' polyester powders were developed and tested for mechanical, physical and chemical resistance. The best formulation had overall properties which were as good as the standard polyester in many respects. However chemical resistance was found to be slightly lower. The charging characteristics of powder paints during application by means of electrostatic spraying was studied by measuring the charge per unit mass and relating this to the surface area. A high degree of correlation was found between charge carried and surface area, and the charge retained was related to the powder's formulation.

Homogenization of alloying elements is desired during sintering of powder metallurgy components. The redistribution processes such as penetration of liquid phase into the interparticle/grain boundaries of solid particles and subsequent solid-state  diffusion of alloy element(s) in the base powder, are important for the effective homogenization of alloy element(s) during liquid phase sintering of the mixed powders. The aim of this study is to increase the understanding of alloy element redistribution processes and their effect on the dimensional properties of the compact by means of numerical and experimental techniques. The phase field model coupled with Navier-Stokes equations is used for the simulations of dynamic wetting of millimeter- and micrometer-sized metal drops and liquid phase penetration into interparticle boundaries. The simulations of solid particle rearrangement under the action of capillary forces exerted by the liquid phase are carried out by using the equilibrium equation for a linear elastic material. Thermodynamic and kinetic calculations are performed to predict the phase diagram and the diffusion distances respectively. The test materials used for the experimental studies are three different powder mixes; Fe-2%Cu, Fe-2%Cu-0.5%C, and Fe-2%(Cu-2%Ni-1.5%Si)-0.5%C. Light optical microscopy, energy dispersive X-ray spectroscopy and dilatometry are used to study the microstructure, kinetics of the liquid phase penetration, solid-state diffusion of the Cu, and the dimensional changes during sintering. The wetting simulations are verified by matching the spreading experiments of millimeter-sized metal drops and it is observed that wetting kinetics is much faster for a micrometer-sized drop compared to the millimeter-sized drop. The simulations predicted the liquid phase penetration kinetics and the motion of solid particles during the primary rearrangement stage of liquid phase sintering in agreement with the analytical model. Microscopy revealed that the C addition delayed the penetration of the Cu rich liquid phase into interparticle/grain boundaries of Fe particles, especially into the grain boundaries of large Fe particles, and consequently the Cu diffusion in Fe is also delayed. We propose that the relatively lower magnitude of the sudden volumetric expansion in the master alloy system could be due to the continuous melting of liquid forming master alloy particles.

QC 20140515

Particulate reinforced Al alloy composites (AlMCs) are recognized as important structural materials due to their lightweight, high modulus and strength and high wear resistance. In order to understand the effect of matrix, reinforcement and secondary processing techniques on the microstructure development and mechanical properties of AlMCs produced by powder metallurgy routes, Al alloy composites reinforced with three types of reinforcements by different secondary processing techniques have been produced and examined. Fabrication of Al or 6061Al alloy based composites reinforced with nano-sized SiC particles (~500nm), micro-sized (<25µm) quasicrystalline alloy particles (hereinafter referred to as “NQX”) and micro-sized Nb particles (~130µm) has been carried out by powder metallurgy routes followed by extrusion or cold rolling. After extrusion, a homogeneous distribution of secondary particles has been obtained with rare interfacial reaction products. The 6061Al/SiC composites exhibit superior mechanical properties than either monolithic alloys or composites reinforced with micro-sized particles with retained ductility while the 6061Al/NQX and 6061Al/Nb composites show limited improvement in tensile strength mainly due to their reinforcement size and poor interfacial bonding. After cold rolling, the evolution in microstructure, texture and strength has been analysed. A typical near β fibre texture with highest intensities near Copper and Brass orientations has been developed for 6061Al/NQX and 6061Al/Nb composites. For 6061Al/SiC composites, a randomized texture with very small grains has achieved due to the presence of the non-deformable SiC particles. Mechanical property tests including microhardness, three-point bending tests and tensile tests have been carried out on cold rolled samples and the results exhibit some level of improvement when compared with as-extruded samples due to work hardening. Finally, the work moves on to the general discussion based on the previous result chapters. The microstructural development related to reinforcement, matrix and interfacial areas during extrusion and cold rolling has been summarised and the correlation between microstructure and mechanical properties has been discussed. The thesis provides a thorough understanding of AlMCs produced by powder metallurgy routes in terms of matrix, reinforcement and processing techniques. It can provide reference to the future development of AlMCs for high strength applications.

The synthesis of silicon nitride (Si$ sb3$N$ sb4$) by carbothermal reduction of silica was sensitive to the processing steps used for the starting materials (SiO$ sb2$, C) and to the reaction conditions. A good degree of intimacy between the starting materials was required in order to obtain fine ceramic powders.
The formation of Si$ sb3$N$ sb4$ was known to occur over a narrow temperature range (1450-1550$ sp circ$C). The morphology of the silicon nitride powder produced was also shown to vary widely depending on the reaction temperature.
The amount and morphology of the silicon carbide formed was sensitive to impurities present in the precursors prior to the reaction. The nitrogen flow rate during reaction as well as the position of pellets in the reactor played a key role in the final SiC content of the powder.
Results showed that the strength values of two carbothermal powders were excellent (507 and 577 MPa) considering their lower sintered densities which was the result of residual carbon present in the powder. (Abstract shortened by UMI.)

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Ion nitriding is a process of thermo-physical-chemical treatment that provides a surface hardening, originated by interstitial diffusion of nitrogen on the ferrous and nonferrous alloys surfaces. Understanding and controlling the formation of the nitrided layer have considerable industrial interest due to the improvements regarding wear, corrosion and fatigue resistances on the metals and their alloys. In this work, it was performed the surface modification in sintered iron samples by ion nitriding process, with a gaseous mixture of 80% vol H2 and 20% vol N2, during times of 3 and 5 hours, using ion nitriding temperature of 500°C, 540°C and 580°C. The samples were characterized by scanning electron microscopy (SEM) and X-ray diffraction (XRD) analyses, and wear and micro-hardness tests, comparing the results with sintered and steam treatment samples. The results showed that both nitride thickness and wear resistance increased with higher nitriding time and temperature, where the temperature was the variable that most influenced the aforementioned characteristics. The XRD analysis indicated that the nitrided layer near to the surface, for all samples, consisted in a mixture of y-Fe4N and e-Fe3N phases.
A nitretação iônica é um processo de tratamento termo-físico-químico que consiste em um endurecimento superficial, provocado pela difusão intersticial de nitrogênio atômico na superfície de ligas ferrosas e não ferrosas. O entendimento e o controle da formação da camada nitretada apresentam considerável interesse industrial devido às melhorias alcançadas nas resistências ao desgaste, corrosão e à fadiga dos metais e suas ligas. Neste trabalho, promoveu-se a modificação superficial de amostras de ferro sinterizado por meio do processo de nitretação a plasma, com uma mistura gasosa de 80% vol H2 e 20% vol N2, nos tempos de 3 e 5 horas, e temperaturas de nitretação de 500°C, 540°C e 580°C. As amostras foram caracterizadas por meios de análise de microscopia eletrônica de varredura (MEV) e difração de raios X (DRX), e quantificadas quanto aos níveis de desgaste e microdureza, em comparação com amostras sinterizada e ferroxidada. Os resultados mostraram que tanto as espessuras das camadas de nitretos como as resistências ao desgaste das amostras aumentaram com o tempo e temperatura de nitretação, sendo a temperatura a variável que mais influenciou nas características mencionadas. A análise de DRX indicou que a camada nitretada próxima a superfície, para todas as amostras, consiste de uma mistura de fases de  -Fe4N e -Fe3N.

Titanium and its alloys have been widely used in oral implantology due to their mechanical properties, corrosion resistance and biocompatibility. However, under in vivo conditions the implants are subjected to the tribocorrosion phenomenon, which consists in the degradation mechanisms due to the combined effect of wear and corrosion. This process contributes to limiting the life span of the implant and may generate clinical problems in patients as metallic ions are released. Another cause of dental implant failure may be the loosening of the implant as metal does not promote osseointegration. The powder-metallurgy process is a promising alternative to the traditional casting fabrication process of titanium alloys for bone implants design, as the porous structure would allow the bone to grow into the pores. This would result in a better fixation of the metal implant without the need of sandblasting /acid etching the surface. The present Doctoral thesis aims at describing the corrosion and tribocorrosion behavior of titanium alloys and their degradation mechanisms when processed by powder metallurgy, as a possible alternative to standard casting for dental implant application. For this, model Ti6Al4V titanium alloy and possible substitute Ti6Al7Nb alloy, where Vanadium has been replaced by Niobium in order to avoid cytotoxicity of the resulting biomaterial, have been studied. Electrochemical and tribo-electrochemical characterization of the biomaterials have been carried out under different physico-chemical conditions with biological relevance (in artificial saliva (AS) with different fluoride content, pH and oxidising conditions) which noticeably influences the degradation mechanisms of the studied materials. A new tribocorrosion technique that allows measuring the galvanic potential and current between the wear track (anode) and the passive material (cathode) through Zero-Resistance Ammetry (ZRA) has been also used to elucidate tribocorrosion mechanisms of the model Ti6Al4V cast alloy in AS. The ZRA technique for tribocorrosion allowed predicting the real depassivated area and therefore, the deviation of the wear mechanisms from Archard wear law at Open Circuit Potential (OCP). All alloys show passivity in artificial saliva although active dissolution occurs in presence of high fluoride concentration (1000 ppm) and acidic conditions, pH 3. The degradation mechanism of sintered alloys is mainly governed by the mechanical wear in AS and only determined by the active dissolution when fluorides are added to acidified artificial saliva (pH 3). Wear was found to be governed by the prevailing oxidizing condition (simulated by changes in the electrode potential). Ti6Al4V alloy processed by powder metallurgy showed a similar tribocorrosion resistance when compared to commercially available cast alloy suggesting that powder metallurgy is a promising fabrication process for implant applications. The influence of the alloying elements, Al and Nb, on the corrosion and tribocorrosion behavior of different titanium alloys, Ti6Al7Nb, Ti7Nb and Ti6Al has been studied and in all cases, the corrosion resistance is improved when compared to pure titanium. Wear damage was found to be critically affected by the ductility of the material, thus by the alloying element. Ti6Al7Nb showed a better corrosion resistance and similar tribocorrosion behaviour when compared to Ti6Al4V. The results of this thesis have shown that Ti6Al7Nb obtained by Powder metallurgy is a promising biomedical alloy for oral implants. Wear damage of sintered Ti alloys depends on the electrochemical potential and their tribocorrosion behaviour is critically affected by a high content of fluoride found in common daily dental health care products.
El titanio y sus aleaciones han sido utilizados en implantología oral debido a sus propiedades mecánicas, resistencia a la corrosión y biocompatibilidad. Sin embargo, bajo condiciones in vivo los implantes están sometidos al fenómeno de tribocorrosión, que consiste en mecanismos de degradación debido al efecto combinado de desgaste y corrosión. Este proceso disminuye la vida útil del implante y genera problemas clínicos a medida que se liberan iones metálicos. La pérdida de fijación del implante es otra causa de fracaso del implante, por falta de osteointegración. El proceso de pulvimetalurgia es una alternativa prometedora al proceso tradicional de fabricación (colada, forja) de aleaciones de titanio para el diseño de implantes óseos, ya que la estructura porosa permitiría que el hueso crezca dentro de los poros, dando lugar a una mejor fijación del implante. La presente tesis doctoral pretende describir el comportamiento frente a la corrosión y tribocorrosión de las aleaciones de titanio y sus mecanismos de degradación cuando se procesan mediante pulvimetalurgia, como una posible alternativa a la colada estándar para la aplicación de implantes dentales. Se ha estudiado el modelo de aleación de titanio Ti6Al4V y posible sustitución por la aleación Ti6Al7Nb, donde el Vanadio ha sido sustituido por Niobio para evitar la citotoxicidad del biomaterial. La caracterización electroquímica y tribo-electroquímica de los biomateriales se ha llevado a cabo en diferentes condiciones físico-químicas con relevancia biológica (en saliva artificial (AS) con fluoruro, pH y condiciones oxidantes) que influye notablemente en los mecanismos de degradación de los materiales estudiados. También se ha utilizado una nueva técnica de tribocorrosión que permite medir el potencial galvánico y la corriente entre la pista de desgaste (ánodo) y el material pasivo (cátodo) a través de la ametría de resistencia cero (Zero-Resistence Ammetry, ZRA) para elucidar los mecanismos de tribocorrosión de la aleación de forja Ti6Al4V en AS. La técnica ZRA para tribocorrosión permitió predecir el área real despasivada y, por tanto, la desviación de los mecanismos de desgaste de la ley de desgaste de Archard en OCP. Las aleaciones muestran pasividad en AS, aunque la disolución activa se produce en presencia de alta concentración de fluoruro (1000 ppm) y condiciones ácidas, pH 3. El mecanismo de degradación de las aleaciones sinterizadas se rige principalmente por el desgaste mecánico en AS y sólo determinado por la disolución activa cuando se añaden fluoruros a la saliva artificial acidificada (pH3). Se encontró que el desgaste se rige por la condición oxidante predominante (simulada por cambios en el potencial de electrodo). La aleación Ti6Al4V procesada por pulvimetalurgia mostró una resistencia similar a la tribocorrosión cuando se comparó con la aleación forjada comercial disponible, lo que sugiere que la pulimetalurgia es un prometedor proceso de fabricación para aplicaciones de implantes. Se ha estudiado la influencia de los elementos aleantes Al y Nb sobre el comportamiento de corrosión y tribocorrosión de diferentes aleaciones de titanio Ti6Al7Nb, Ti7Nb y Ti6Al y en todos los casos la resistencia a la corrosión se mejora en comparación con el titanio puro. El daño de desgaste está afectado críticamente por la ductilidad del material, por lo tanto, por el elemento de aleación. La aleación Ti6Al7Nb mostró una mejor resistencia a la corrosión y un comportamiento similar de tribocorrosión en comparación con la aleación Ti6Al4V. Los resultados de esta tesis han demostrado que el Ti6Al7Nb obtenido por pulvimetalurgia es una prometedora aleación biomédica para implantes orales. El deterioro del desgaste de las aleaciones de Ti sinterizadas depende del potencial electroquímico y su comportamiento a tribocorrosión se ve afectado de manera crítica por un alto contenido de ion flúor
El titani i els seus aliatges s'han utilitzat en l'implantologia oral degut a les seves propietats mecàniques, resistència a la corrosió i biocompatibilitat. No obstant això, en condicions in vivo els implants són sotmesos al fenomen de tribocorrosió, que consisteix en els mecanismes de degradació causats per l'efecte combinat de desgast i corrosió. Aquest procés contribueix a limitar la vida útil de l'implant i pot generar problemes clínics com l'alliberament d'ions metàl¿lics. Una altra causa de fracàs de l'implant dental pot ser la pèrdua de fixació de l'implant, ja que el metall no promou l'osteointegració. El procés de pulvimetal¿lúrgia és una alternativa prometedora al procés tradicional de fabricació (colada i forja) d'aliatges de titani per al disseny d'implants ossis, ja que l'estructura porosa permetria que l'os creixca dins dels porus. Això donaria lloc a una millor fixació de l'implant metàl¿lic. La present tesi doctoral pretén descriure el comportament enfront de la corrosió i tribocorrosió dels aliatges de titani i els seus mecanismes de degradació quan es processen mitjançant pulverimetal¿lúrgia, com una possible alternativa a la fabricació estàndard per forja per a l'aplicació d'implants dentals. Per a això, s'ha estudiat el model d'aliatge de titani Ti6Al4V i possible substitució per l'aliatge Ti6Al7Nb, on el vanadi ha estat substituït per niobi per evitar la citotoxicitat del biomaterial resultant. La caracterització electroquímica i tribo-electroquímica dels biomaterials s'ha dut a terme en diferents condicions fisicoquímiques amb rellevància biològica (en saliva artificial (AS) amb fluorur, pH i condicions oxidants) que influix notablement en els mecanismes de degradació dels materials estudiats. També s'ha utilitzat una nova tècnica de tribocorrosió que permet mesurar el potencial galvànic i el corrent entre la pista de desgast (ànode) i el material passiu (càtode) a través de la ametria de resistència zero (Zero-Resistence Ammetry, ZRA) per elucidar els mecanismes de tribocorrosió de l'aliatge de forja Ti6Al4V en AS. La tècnica ZRA per tribocorrosió va permetre predir l'àrea real despassivada i, per tant, la desviació dels mecanismes de desgast de la llei de desgast de Archard en OCP. Tots els aliatges mostren passivitat en la saliva artificial, tot i que la dissolució activa es produix en presència d'alta concentració de fluorur (1000 ppm) i condicions àcides, pH 3. El mecanisme de degradació dels aliatges sinteritzats es regix principalment pel desgast mecànic en AS i només determinat per la dissolució activa quan s'afegixen fluorurs a la saliva artificial acidificada (pH 3). Es va trobar que el desgast es regix per la condició oxidant predominant (simulada per canvis en el potencial d'elèctrode). L'aliatge Ti6Al4V processada per pulverimetal¿lúrgia va mostrar una resistència similar a la tribocorrosió quan es va comparar amb l'aliatge forjada comercial disponible, el que suggerix que la pulverimetal¿lúrgia és un prometedor procés de fabricació per a aplicacions d'implants. S'ha estudiat la influència dels elements d'aliatge Al i Nb sobre el comportament de corrosió i tribocorrosió de diferents aliatges de titani Ti6Al7Nb, Ti7Nb i Ti6Al i en tots els casos la resistència a la corrosió es millora en comparació amb el titani pur. Es va trobar que el dany de desgast està afectat críticament per la ductilitat del material, per tant, per l'element d'aliatge. L'aliatge Ti6Al7Nb va mostrar una millor resistència a la corrosió i un comportament similar de tribocorrosió en comparació amb l'aliatge Ti6Al4V. Els resultats d'aquesta tesi han demostrat que el Ti6Al7Nb obtingut per pulverimetal¿lúrgia és un prometedor aliatge biomèdic per a implants orals. El deteriorament del desgast dels aliatges de Ti sinteritzats depèn del potencial electroquímic i el seu comportament a tribocorrosió es veu afectat de manera crí
Licausi, M. (2017). Analysis of tribocorrosion behavior of biomedical powder metallurgy titanium alloys [Tesis doctoral no publicada]. Universitat Politècnica de València. https://doi.org/10.4995/Thesis/10251/90448
TESIS

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Tese (Doutoramento)
IPEN/T
Instituto de Pesquisas Energeticas e Nucleares - IPEN/CNEN-SP

"We focus attention on single-punch compaction of metal powders in cylindrical dies. In one case, we consider solid cylindrical compacts, and take the die walls to be frictionless in order to isolate the effects of initial nonuniformities in powder fill on the final green density distribution of the compact. First, a model is introduced in which the die is filled with n distinct powders that occupy concentric annular regions within the die. The model requires that the balance of mass, the balance of momentum, and a realistic equation of state be satisfied in each region, and includes a plausible constitutive relation that relates the induced radial pressure in each powder region to the corresponding axial pressure and the relative movements of the interfaces that confine the region. For specified powder properties, the model predicts the movements of the interface between the powders, the final density in each region, the pressure maintained in each region, and the total compaction load required. In the special case of two powders (n=2), we predict how the radial movement of the single interface depends on the mismatch between the properties of the two powders. For large values of n, and for powder properties that change gradually from one powder to the next, the model approximates a single powder filled nonuniformly in the die. Finally, a model is developed for a single powder with continuously varying powder properties. Formally, the model may be obtained by taking the limit of the n-powder model as n becomes unbounded. Employing the continuous model, we determine how nonuniformities in initial fill density can be offset by nonuniformities in other powder properties to yield perfectly uniform green densities. In a second case, we consider axisymmetric, hollow, cylindrical compacts, and include the effects of friction at the die wall and the core rod. The ratio of the induced radial pressure to the applied axial pressure is assumed to be constant throughout the compaction, and Coulomb friction acts between the powder and the die wall as well as between the powder and the core rod. We derive a closed form solution for the axial and radial variation of the axial pressure, radial pressure, and shear stress throughout the compact. This solution is combined with a plausible equation of state to predict the final green density distribution and the variation of applied load throughout the compact."

Thesis (M.S.)--Worcester Polytechnic Institute.
Keywords: powder metallurgy; density distribution; compaction modeling; compact; powder; compaction. Includes bibliographical references (p. 141-142).

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Dissertacao (Mestrado)
IPEN/D
Instituto de Pesquisas Energeticas e Nucleares - IPEN/CNEN-SP

Due to growing demands for steel powder properties and continuous evolution of the powder metallurgy (PM) production it is necessary to apply new investigation technics and research applications for quality investigation of the PM products. In addition, it is important to be able to predict the probable maximum size of inclusions. The industrial scale sampling of steel was made in Höganäs AB. The three dimensional (3D) analysis of non-metallic inclusions obtained by electrolytic extraction (EE) method was applied for metal samples taken from liquid steel before water-atomization and after powder forging process. It was demonstrated that the application of the 3D analysis has a perspective and possibility to be used independently or like a reference during 2D analysis of inclusions in powder metallurgy products. The tundish samples have the maximum total number of inclusions but have smaller size of complex inclusion. The size range of inclusions in the ladle and tundish samples is between 1 and 46 μm. The main type of inclusions is spherical (Si-Ca-Al-Mg-O in composition). The powder forged samples have two main types of non-metallic particles: “gray” carbon saturated (10-250 μm) and “bright” clustered oxide particles (1-37 μm with Cr-Si-Mn-Mg-Al-O in composition). The probable maximum size of inclusions was estimated based on a new particle size distribution (PSD) and the standard extreme value distribution (EVD) methods. Both methods predicted that in 1 kg of metal the maximum size of spherical inclusions is < 15 μm in liquid steel samples and the maximum length of “bright” clustered oxide particles is < 63 μm in powder forged samples. However, the prediction of the maximum size by PSD method showed necessity of the further optimization.