Dissertationen zum Thema „Metallurgical powder“

The MAX phases constitute a group of ternary ceramics which has received intense attention over the last decade due to their unique combination of properties. The Ti3SiC2 is the most well studied MAX phase to date and it has turned out to be a promising candidate for high temperature applications. It is oxidation resistant, refractory and not susceptible to thermal shock, while at the same time it can be machined with conventional tools which is of great technological importance. Most attempts to synthesize bulk Ti3SiC2 have involved pure titanium in the starting powder mixtures, but Ti powder is oxidising and requires an inert atmosphere throughout the synthesis process which makes the procedures unsuitable for large scale production. The aim of the first part of this study was to delineate the influence of sintering time and temperature on the formation of Ti3SiC2 from a starting powder which does not contain pure titanium. Titanium silicon carbide MAX phase was synthesised from ball milled TiC/Si powders, sintered under vacuum for different times and temperatures. After heat treatment the samples were evaluated using scanning electron microscopy (SEM) and x-ray diffraction (XRD). This study showed that TiC was always present in the final products whereas TiSi2 was an intermediate phase to the Ti3SiC2 formation. The highest amount of Ti3SiC2 was achieved for short holding times of 2-4 hours, at high temperatures, 1350-1400¢ªC. More elevated temperatures or extended times resulted in silicon loss and decomposition of Ti3SiC2. In the second part of this study the sintering reactions and the mechanisms of formation of Ti3SiC2 were investigated by x-ray diffractometry, thermodilatometry, thermogravimetry, differential scanning calorimetry and mass spectrometry. TiC/Si powders of the different ratios; 3:2 and 3:2.2, were heated to different temperatures under flowing argon gas in a dilatometer and examined by XRD. The TiC/Si powder samples of the ratio 3:2 were further investigated by the other thermal analysis methods. The results confirmed the presence of the intermediate phase TiSi2. From 1500¢ªC silicon evaporation and MAX phase decomposition were observed, and the results show that the MAX phase formation may be concurrent with the melting of silicon. TiC was always present in the final products, either as a reactant or as a decomposition product. The extra silicon of the 3:2.2 TiC/Si powder significantly increased the Ti3SiC2 conversion and no intermediate phases were observed for this powder mixture. The Si of these samples did not melt or evaporate, and only minor decomposition was observed even at 1700¢ªC. These results indicate that the silicon content of the initial powder mixture is decisive to the reaction mechanisms of the sintering process.

Godkänd; 2007; 20070523 (ysko)

Dissertação (mestrado) - Universidade Federal de Santa Catarina, Centro Tecnológico, Programa de Pós-Graduação em Ciência e Engenharia de Materiais, Florianópolis, 2015.
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Abstract : Biodegradable metal alloys are a new class of implant materials suitable for implants such as stents, bone plates and screws. The corrosion of magnesium alloys might provide a new mechanism where they could be used as degradable metal implants to be applied in musculo-skeletal surgery. In this case, a secondary surgery for implant retrieval is not needed. For that, magnesium alloys with controlled in vivo corrosion rates need to be developed. There is a high demand to design magnesium alloys with adjustable corrosion rates and suitable mechanical properties. An approach to this challenge is a magnesium metal matrix composite (Mg-MMC) composed of the magnesium alloy ZK60 and hydroxyapatite (HA) particles for tailoring its properties such as mechanical properties and corrosion resistance. The composite was produced by mechanical alloying followed by hot extrusion. HA in contact with molten magnesium releases toxic gases like phosphine (PH3), so solid-state processing such as mechanical milling and extrusion is feasible. This work presents the influence of different amounts of HA on the degradation behavior and mechanical properties, which shows that the HA addition has a substantial increase in the compression strength (up to 14% for 20 wt.% HA addition) and no negative effect on the controlled degradation behavior of this biomaterial.

Ligas metálicas biodegradáveis são uma nova classe de materiais de implante adequados para a cirurgia óssea. A corrosão de ligas de magnésio pode proporcionar um novo mecanismo onde tais ligas podem ser utilizadas como implantes metálicos degradáveis a serem aplicados em cirurgia músculo-esquelética. Nestes casos, a segunda cirurgia para retirada do implante não seria necessária. Para isso, ligas de magnésio com taxas de corrosão in vivo controladas precisam ser desenvolvidas. Há uma grande procura para projetar ligas de magnésio com taxas de corrosão ajustáveis e propriedades mecânicas aplicáveis. Uma abordagem a este desafio é um compósito de matriz metálica (CMM) composto pela liga de magnésio ZK60 e hidroxiapatita (HA) para aperfeiçoar suas propriedades como resistência mecânica e resistência à corrosão. O compósito é produzido via moagem de alta energia seguida de extrusão à quente. Uma vez que HA em contato com magnésio líquido libera gases tóxicos como fosfina (PH3), esta é a melhor forma de sua produção. Este trabalho mostra a influência de diferentes quantidades de hidroxiapatita na taxa de degradação e propriedades mecânicas do compósito, as quais evidenciam um aumento substancial na resistência à compressão com a adição de HA (até 14% para o compósito com 20% de HA), sem detrimento às propriedades de degradação controlada do biomaterial.

Ternary transition metal cubic carbides have high hardness and are potential carbides in cemented carbide and cermet tools, as well as hard coatings used to improve metal cutting performance. In the present work, (Ti,Zr)C, (V,Nb)C, and (V,Ta)C ternary cubic carbides were synthesized using traditional powder-metallurgical methods. The effect of synthesis temperature and starting materials on synthesis is investigated, and the microstructure evolution during aging is studied. (Ti,Zr)C was found to decompose into lamellae upon aging at the temperature range from 1150 to 1800 °C. A similar microstructure was observed in (V,Ta)C and (V,Nb)C- 0.5 wt% Fe. All of these structures were found to form through discontinuous precipitation.The grain misorientation distribution of (Ti,Zr)C aged at 1400 °C is investigated. It was found that decomposition tends to occur at high-angle grain boundaries above 25°. The hardness of as-synthesized (Ti,Zr)C powder was found to be 41±6 GPa. Fully decomposed (Ti,Zr)C particles were found to be slightly harder than the undecomposed counterpart. On the other hand, in (V,Nb)C-0.5 wt% Fe, the decomposed structure formed upon aging at 1200 °C was found to have a hardness of 26±2 GPa, which is basically the same as the unaged alloy.Furthermore, the sintering behavior of (Ti,Zr)C with WC-Co is investigated. There are two γ-phases in the final microstructure, one TiC-rich and one ZrC-rich. (Ti,Zr)C was found to decompose at an early stage of sintering, and the final grain size of WC and the two γ-phases was found to be 10% smaller than that in a reference WC-TiC-ZrC-Co composite.

QC 20170529

In this study, prealloyed austenitic stainless steel and premixed soft magnetic Ni-Fe permalloy compacts were consolidated through microwave and conventional sintering routes at combinations of various sintering temperatures and compaction pressures. Sintered alloys were characterized in terms of their densification, microstructural evolution as well as mechanical and magnetic properties. The effect of sintering method in terms of the applied sintering parameters on the final properties of the compacts were investigated in a comparative manner. It was determined that microwave sintered permalloys are superior compared to their conventionally sintered counterparts in densification response, microstructural characteristics such as pore shape and distribution as well as mechanical properties for both austenitic stainless steel and permalloy compacts. However, permeability of the microwave sintered permalloys was inferior to their conventionally sintered counterparts in some cases due to microstructural refinement associated with microwave sintering route.

The physical properties of the protective passive films formed on the surface of stainless steels under electrochemical polarization in different electrolytes were studied. The structure of these films was analyzed as a function of depth using photoelectron spectroscopy (PES). Depth profiling (using PES) of the surface layer was achieved by either changing the angle of incidence to achieve different analysis depths (ARXPS), by argon ion etching, or by varying the energy of the incoming x-rays by the use of synchrotron radiation. The use of hard x-rays with high resolution (HAXPES) provided novel quantified information about the nickel content underneath the passive films. A complex environment was found in these surface layers composed of an outermost monolayer of iron on top of a layer of chromium hydroxides covering an underlayer of chromium oxides. Molybdenum was enriched in the interface between the metal and oxide. Nickel is enriched underneath the passive film and therefore nickeloxides are only present in the surface layer in low concentrations. A comparison was performed on austenitic and duplex stainless prepared by hot isostatically pressed (HIP) or cast and forged processes. HIP stainless steel was produced using the burgeoning technique of pressing gas atomized powders together. The structure of these steels is far more homogenous with a lower porosity than that of the conventionally prepared equivalents. It was shown that hot HIP austenitic steel had better pitting corrosion resistance than its conventional counterpart. Finally, the duplex steel was cycled in a Li-ion battery to explore its potential application as a current collector. It was shown that the passive film formed in the organic solvents is similar in composition and thickness to the films formed in aqueous solutions. However, it is doubtful if steel could be used as current collector in batteries due to its high reactivity with lithium.

La poudre de silicium métallurgique (MG-Si, pureté 99 %) ont été étudiées, en se focalisant particulièrement sur les particules fines (taille comprise entre 1 et 10 μm) Ce matériau est utilisé dans l’industrie siliconière pour la synthèse directe du diméthyldichlorosilane et est obtenu par broyage de blocs de silicium. Les propriétés de cette poudre sont cruciales pour le procédé industriel, à la fois en termes de surface spécifique, composition chimique et coulabilité. Comprendre l’influence des particules fines, qui dégradent la coulabilité, et leur origine au cours du broyage est donc d’une importance cruciale. Une nouvelle caractérisation, chimique et cristallographique, des poudres de MG-Si montre que les particules fines sont en moyennes moins chargées en éléments d’alliage que les particules plus grosses. La structure cristalline du silicium est inchangée au cours du broyage, sauf pour les particules superfines (taille inférieure à 1 μm). Celles-ci présentent des zones amorphes : cela montre qu’elles sont soumises à des contraintes plus importantes au cours du broyage, comme cette transformation étant obtenue au-delà d’un seuil de pression. Le comportement du MG-Si en broyage a été étudié pour la première fois. A l’échelle de la particule unique, il est confirmé que les fissures suivent une propagation transgranulaire. De plus, des particules fines peuvent être produites au cours d’un unique événement de broyage, en raison de l’activation simultanée de multiples systèmes de fissures qui peuvent brancher entre elles. La taille critique en-deçà de laquelle la déformation plastique est énergétiquement plus favorable que la propagation de fissure a été estimée à environ 1 μm par une méthode basée sur l’indentation. Ces deux résultats sont cohérents avec la répartition des éléments d’alliages en fonction de la taille de particule. A l’échelle multiparticulaire, une étude pilote en broyeur à tambour tournant a été menée. Les résultats de cette étude ne sont pas disponibles dans cette version publique du manuscrit. Veuillez vous reporter au manuscrit complet. Les conséquences sur la coulabilité de la présence de particules fines dans la poudre de MG-Si produite par broyage ont été caractérisées par mesures d’angle de repos, de dynamique de compaction et en fluidisation. En particulier, un nouveau comportement d’élutriation a été identifié et décrit : l’élutriation séquentielle se produit lorsque des particules fines sont initialement présentes dans le lit fluidisé et se caractérise par l’envolement d’abord des inférieures à environ 30 μm puis seulement des particules de taille supérieure. Ce comportement n’est pas observé en l’absence de fines dans le lit initial. L’explication de ce phénomène pourrait se trouver dans la formation de clusters polydisperses, formés seulement en présence de particules fines. En parallèle de l’élutriation séquentielle, des mesures électrostatiques avec un électromètre externe à la colonne ont montré la présence de potentiels très importants (10 kV), dont le signe correspond à la gamme de taille de particules envolées. Ceci suggère que l’adhésion au sein des clusters pourrait être électrostatique
Metallurgical-grade silicon (MG-Si, 99 %) powders were extensively investigated, particularly focusing on the fine particles (whose size is between 1 and 10 μm) comprised in these powders. This material is a reactant widely used in the silicones industry for the Direct Synthesis and is obtained by size reduction of millimetric silicon lumps. Powder properties are major stakes of the industrial process. Smaller sizes favor high specific surfaces and high rates of production, but can decrease the lowability, thus inducing poor heat evacuation resulting in hot spots and a decrease in selectivity. Such lowability issues are particularly associated with fine particles, hence understand the generation of these particles during grinding is of critical importance. New chemical and crystallographic characterization of MG-Si is presented, showing that fine particles contain on average less alloying elements than larger particles, yet their crystallographic structure is preserved through grinding. On the contrary, superfine particles (smaller than 1 μm) exhibit amorphous zones: this transformation is pressure induced, showing that these particles experience larger stresses during the grinding step. The behavior of MG-Si in grinding mills has been studied for the first time. At the single particle level, it has been confirmed that transgranular fracture is preferred in MG-Si. Moreover, fine particles can be produced from a single fracture event, due to multiple crack propagation and branching. The critical size under which plastic deformation preferentially occurs over fracture has been evaluated to be approximately 1 μm. These two facts are consistent with a lower level of impurities in fines, yet remaining crystalline, and with superfines exhibiting amorphous areas. At the multiple particle level, pilot scale batch milling experiments have been performed. The results are not included in this public version of the manuscript, please refer to the full manuscript. The consequences of the presence of fine particles in ground MG-Si powder on lowability has been assessed by means of angle of repose, compaction tests and fluidization experiments. A new elutriation behavior has been observed and characterized: for naturally ground MS-Si powders (including fine particles), particles smaller than 30 μm are entrained first, then only larger particles. This was not the case in absence of fine particles. The explanation may probably lie within the presence of polydisperse clusters, formed only in presence of fine particles. Parallel to this elutriation behavior, electrostatic measurements with an external electrometer showed that high potential with sign correlated with the type of particle elutriated are attained during elutriation. This may suggest that electrostatics is responsible for cluster formation

The diploma thesis deals with the study of the influence of process parameters of AlSi7Mg0.6 aluminum alloy processing using the additive technology Selective Laser Melting. The main objective is to clarify the influence of the individual process parameters on the resulting porosity of the material and its mechanical properties. The thesis deals with the current state of aluminum alloy processing in this way. The actual material research of the work is carried out in successive experiments from the welding test to the volume test with subsequent verification of the mechanical properties of the material. Material evaluation in the whole work is material porosity, stability of individual welds, hardness of the material and its mechanical properties. The results are compared with the literature.

The present study was carried out to investigate the formation and evolution of non-metallic inclusions during ingot casting. Emphasize have been on understanding the types of inclusions formed and developed through the casting process and on the development of already existing inclusions carried over from the ladle during casting. Industrial experiments carried on at Uddeholm Tooling together with laboratory work and Computational Fluid Dynamics (CFD) simulations. Ingots of 5.8 tons have been sampled and the types of inclusions together with their distribution within the ingot have been characterized. Two new types of inclusions have been found. Type C1 is found originated from casting powder and in the size from a few μm to 30 μm. Type C2 is of macro inclusion type sizing up to 70 μm. The presence of C2 inclusions are few but very detrimental for the quality of the steel. Both types, C1 and C2 consist of alumina, indicating that reoxidation is the main reason for their existence. The protecting argon shroud has been studied by the use of a 1:1 scaled 2D model. Both flow pattern and oxygen measurement have been carried out. CFD has also been used as an auxiliary tool. It has been found that the oxygen pickup through argon gas shroud depends mostly on the distance between the ladle and the collar placed on top of runner. Further increase of gas flow rate above 2.5 m3.h-1 had very little effect on the oxygen distribution since both the flushing effect and the entraining effect with respect to oxygen are enhanced by further increase of inert gas flow rate. In the case of dual gas inlet, the flow in the shroud was found much less diffused compared with either vertical or horizontal injection system. The oxygen content in this arrangement was also greatly reduced. Studies of the runner after casting revealed a sparse non-metallic network structure around the periphery of the steel rod remained in the runner. The surface of the refractory had been severely attacked by the mechanical force from the streaming steel. The erosions of the centre stone and the end stone were on the other hand negligible. CFD calculations showed that the flow at those locations is almost stagnant. The surface of the refractory in contact with the steel was found to have an increased content of alumina. The source for the alumina could come from either exchange reaction of dissolved aluminium replaces the silica or reoxidation products origin from oxygen pick up during the transfer from the ladle to the vertical runner. Inclusions were also found entrapped in the steel refractory interface. It was also found that a formation of a liquid slag film as early as possible during casting would increase the possibility to remove inclusions and especially inclusions generated by the casting powder.
QC 20100617

O aquecimento indutivo e uma técnica utilizada na indústria para obter resultados de fundição, brasagem, forjaria e também tratamento térmico, aplicação foco deste trabalho. O aquecimento indutivo dá-se através de campos eletromagnéticos induzidos a uma peca metálica, a qual se deseja aquecer. Isso faz com que haja um aumento de temperatura sobre a peca devido ao efeito joule, corrente de foucault e histerese, entre outros efeitos. Para gerar os efeitos acima relatados, são necessários conversores de alta potência e frequência. Tais conversores são compostos em muitos casos de: um retificador, um capacitor filtro de barramento, um inversor e um circuito ressonante. Neste trabalho e proposto a topologia de um circuito ressonante LLC sendo chaveado por um inversor ponte completa. Como todo circuito ressonante, em operação a frequências próximas da ressonância, as correntes são elevadas e consegue-se operar com chaveamento em comutação suave. Entre algumas vantagens da topologia LLC frente a topologias como a série-ressonante, por exemplo, podem-se citar: proteção contra curto-circuito e fácil casamento de impedância entre o circuito ressonante e o inversor. No entanto, conversores com retificadores comuns possuem baixo fator de potência, FP=0,5. Para resolver este problema, propõe-se a utilização de um retificador de alto fator de potência integrado ao conversor através do inversor, formando um sistema de aquecimento indutivo integrado a um retificador com alto fator de potência. Através de um dos braços de comutação do inversor, dá-se o controle do retificador e do conversor ao mesmo tempo. A técnica apresentada resulta em um projeto de custo reduzido e baixo nível de complexidade de implantação. Para controlar a potência do sistema e utilizada uma modulação PWM assimétrica com razão cíclica variável que controla os dois conversores simultaneamente.
Induction heating is a technique used in industry to get results like casting, brazing, forging and heat treatment also, application focus of this work. Induction heating occurs through electromagnetic fields induced in a metal part, which it wants to warm up. This means that there is an increase in temperature on the piece it wants to heat up due to the Joule effect, eddy current and hysteresis, among other effects. To generate the effects reported above, high power converters and frequency are required. These converters are composed in many cases by: a rectifier, filter capacitor DC Link, an inverter and a resonant circuit. This paper proposes the topology of LLC resonant circuit being switched by a full bridge inverter. Like any resonant circuit operating at near of the resonance frequencies, the currents are high and it is possible to operate with soft switching. Among some advantages of the LLC topology against other topologies such as series resonant, for example, can be mention: protection against short-circuit and easy impedance matching between the resonant circuit and the inverter. However, converters with common rectifiers have low power factor. To solve this problem, the use of a rectifier high power factor built into the converter is proposed. This rectifier is integrated into the converter through the inverter, forming a single stage high power factor induction heating system. Through an arm of the inverter is given the control of the rectifier and the converter at the same time. The technique presented results in low cost and low complexity implementation. An asymmetric PWM modulation is used with variable duty cycle to control the power system, which controls both converters at the same time.

Lo scopo della presente ricerca è valutare l’idoneità dell’acciaio da utensili innovativo K890, prodotto da Böhler con metallurgia delle polveri, ad essere impiegato per la realizzazione di componenti motore di moto da corsa, quali alberi a camme e a gomiti, in sostituzione dell’acciaio da nitrurazione GKHW, prodotto da Aubert&Duval con processo ESR (Electro Slag Remelting). Lo studio è stato condotto a valle di una precedente sperimentazione condotta su provini non intagliati ed ha previsto l'esecuzione di prove di trazione e prove di fatica a flessione rotante con intaglio oltre a prove di durezza ed analisi microstrutturali e frattografiche. Sono stati testati due lotti di acciaio K890, aventi durezza di 752 e 821 HV rispettivamente. Durante i test di fatica il lotto in K890 a durezza maggiore ha mostrato un limite di fatica con intaglio superiore al GKHW nitrurato. I risultati ottenuti sui due lotti di K890 sono stati impiegati per valutare l’applicabilità di relazioni empiriche per la stima del coefficiente di concentrazione a fatica delle tensioni ad acciai ultra-alto resistenziali. E’ emerso che le relazioni più tradizionali sovrastimano l’effetto dell’intaglio per questa tipologia di acciaio. A conclusione dello studio, considerando l'esito delle stesse prove condotte sull'acciaio GKHW nitrurato attualmente in uso, si può affermare che l'acciaio K890 è un possibile candidato per la produzione di alberi in ambito racing. La disamina dei risultati sperimentali è preceduta da tre capitoli incentrati su un inquadramento teorico, derivanti da ricerche bibliografiche: il primo riporta un’introduzione al funzionamento ed alle caratteristiche degli alberi a camme e a gomiti; il secondo è relativo alle proprietà degli acciai da utensili tradizionali ed innovativi; infine il terzo riguarda una trattazione sul danneggiamento da fatica, con particolare riguardo all’effetto dell’intaglio ed alle caratteristiche del fenomeno negli acciai ultra-alto resistenziali.

Titanium is well known for its excellent properties, such as high strength-to-weight ratio and outstanding corrosion resistance. However the high cost of this metal has confined its applications to those mostly within the aerospace and military industries. The high purchase price of titanium is primarily driven by the need for intricate metal extraction processes, as well as the sensitivity towards conventional metal working operations. Among the potential solutions, powder metallurgy (P/M) technology provides an economical approach to bring down the price of finished titanium products. However, there are still many problems, such as the residual porosity in the sintered body, that need to be overcome. In this thesis, a fundamental study was carried out focusing on the P/M press-and-sinter technique, using commercially pure titanium (CP Ti) as well as two binary titanium alloys, namely Ti-Ni and Ti-Sn. The influence of several processing parameters including compaction pressure, lubricant type/concentration, sintering time/temperature were performed on both the CP and binary systems. The principal tools utilized for mechanical characterization were hardness and tensile testing, whereas optical microscopy, x-ray diffraction (XRD), and scanning electron microscopy were employed to identify the microstructural features present. Press-and-sinter P/M strategies were successfully developed for all of the blends studied. For CP-Ti, a maximum tensile strength >750MPa and near full theoretical density (~99%) were achieved. Transitions in the size and the size distribution of pores and ?-Ti grains were also observed and quantified. It was found these transitions, as well as the powder impurities present (i.e. oxygen and carbon), greatly influenced the final mechanical properties. In the case of the binary alloys, it was shown that liquid phase sintering (LPS) significantly improved the sintered density for the Ti-10%Ni composition, when sintered at l100°C. A eutectic microstructure (CP-Ti + Ti2Ni), coupled with grains of CP-Ti, were identified as the principal phases present. On the other hand, the Ti-Sn alloys only showed a modest increase in sintered density compared to the CP-Ti, owing to the high solubility of Sn in Ti. In terms of crystal structure, XRD highlighted that the Sn containing samples were fully CP-Ti.

碩士
國立高雄科技大學
機械工程系
107
The objective of this research is to study aluminum added with carbon fiber for powder metallurgy. At first, the aluminum powder added with 1w%, 1.5w%, 2w% carbon fiber in the ball mill for 24 hours, and samples were pressed over a wide range of pressures from 2 tons to 6 tons. The second part is the sintering experiment, the samples were placed in a stainless steel tray and sintered in a flowing argon atmosphere with a reported purity of 99.99%.Sintering was done in the range of 400–630 °C and the post sinter cooling was performed by a furnace cooling to the room temperature. The sintering response and mechanical properties of the alloy were investigated in laboratory settings. It was determined that compaction at 6 tons and sintering at 630 °C for 20 min produced the best properties in the sintered product. Carbon fiber itself has a low density, so adding too much carbon fiber will reduce the overall density. High proportion of carbon fiber promotes expansion at high temperatures, resulting in a gradual decrease in density. However, there is no direct impact at low temperatures. Therefore, the discrimination of low proportion carbon fibers is advantageous for sintering at high temperatures.

Ni-based superalloys remain state-of-the-art materials for use in the high-temperature, corrosive environments experienced by turbine blades in gas turbine engines used for propulsion and energy generation. Increasing the operating temperatures of turbine engines can yield increased engine efficiencies. However, appreciably higher operational temperatures can exceed the capabilities of Ni-based superalloys. Consequently, interest exists to develop high-melting refractory complex concentrated alloys (RCCAs) with the potential to surpass the hightemperature property limitations of Ni-based alloys. RCCAs are multi-principal element alloys, often comprising 5 or more elements in equal or near equal amounts. Conventional solidificationbased processing methods (e.g., arc melting) of RCCAs tend to yield coarse-grained samples with a large degree of microsegregation, often requiring long subsequent homogenization annealing times. Additionally, the large differences in melting temperatures of component elements can further complicate solidification-based fabrication of RCCAs.

碩士
大同大學
材料工程學系(所)
102
Ti-153 sheet specimens were adopted in this study to be treated by thermohydrogen processing to obtain the original alloy powder. The alloy powder was further employed in producing porous cathodes with various porosities to see their hydrogen uptake ability after a designed cyclic hydrogenation treatment and hydrogen evolution ability after vacuum degassing at 300oC - 3.0×10-2 torr. The microstructural changes were investigated by using X-ray diffractometry (XRD). Particle size, surface morphology variations and pore distribution were observed by employing scanning electron microscopy (SEM). Elemental analyzer (EA) was applied to obtain hydrogen contents of processed specimens. The optimal cathode was acquired after Ti-153 sheet specimens processed according to the HPb parameters: (1) powder processing – 300oC-H2(g) 5MPa-15hrs and (2) hot press sintering (25MPa) – 700oC-1.0×10-2 torr.-2hrs. The apparent density of the optimal cathode is 3.857 g/cm3 and the porosity was evaluated as 20.60%. The hydrogen content of the HPb specimen after the designed cyclic hydrogenation treatment was 2.854wt% which is close to the saturated concentration of hydrogen in titanium alloys. After the HPb specimen had been degassed at 300oC- 3.0×10-2 torr for two hours (designated as bVH4D), of which the hydrogen content was lowered to 1.224wt%. The calculated hydrogen uptake and hydrogen evolution payloads for the porous specimen (HPb) in contrast to the bulk one (B0) are 1.82 and 2.21 respectively.

Dissertação de Mestrado Integrado em Engenharia de Mecânica
No âmbito do projeto desenvolvido na empresa Ferespe – Fundição de Ferro e Aço, Lda. surge esta Dissertação de Mestrado, cujo tema passa pelo desenvolvimento e conceção de um equipamento que permita a injeção de gases e pós no banho de metal líquido. Sendo o principal objetivo a promoção da sua limpeza e homogeneização da composição do metal fundido. Com o intuito de obter conhecimento relativamente às práticas, equipamentos e recursos utilizados nesta fase do processamento do metal fundido, recorreu-se a pesquisas bibliográficas bem como foi realizada uma visita à Siderurgia Nacional, S.A. e paralelamente efetuou-se um acompanhamento in loco do processo na empresa. O estudo dos diversos dispositivos utilizados na injeção de gás e pós, as variáveis operacionais com influência na hidrodinâmica do banho, os processos de transporte e a gama de elementos normalmente utilizados nas práticas de refinação no forno, serviram de suporte ao desenvolvimento do projeto apresentado nesta dissertação. A definição do modo operativo do equipamento, bem como os diferentes passos para a sua construção, foram os alicerces essenciais para o desenvolvimento do trabalho. Com base nas práticas aplicáveis na empresa em conjunto com a informação recolhida, definiram-se diversos fatores do processo, como a determinação do árgon e da cal, elementos a insuflar. No seguimento destas opções foram definidos os principais subsistemas do equipamento de injeção, como o invólucro refratário, a tipologia de alimentação e o circuito de insuflação. Um primeiro esboço da lança, em particular a extremidade de injeção, possibilitou o início dos passos de experimentação para o dimensionamento dos subsistemas da lança. Foram realizados diversos testes, complementados por métodos numéricos, que permitiram estudar o sistema de insuflação. Numa primeira fase contemplando apenas a aspiração dos pós para posteriormente ser coadjuvado pela pressurização do depósito. Após os ensaios de todos os subconjuntos efetuou-se a sua assemblagem, originando a estrutura do protótipo final para o trabalho experimental no forno. O processo evolutivo de todos os componentes, ao longo do projeto, foi conseguido graças aos inúmeros testes realizados na fundição do metal líquido, onde foram adaptadas e otimizadas as técnicas de construção do refratário. Devido aos obstáculos presentes, como a frequente obstrução da lança, houve a necessidade de redefinir os valores teóricos da pressão a injetar, para posteriormente conjugá-los com a velocidade do fluxo, de modo a conferir estabilidade no comportamento de homogeneização do banho. Na sequência dos testes realizados para a otimização do protótipo, concluiu-se que os efeitos das suas ações sobre o banho são inofensivos. A consequente análise química e física às amostras recolhidas evidenciou os progressos na limpeza do banho fundido, em resultado das reações ao nível da composição das inclusões de óxidos e sulfuretos. Por fim foi realizada a automatização e dimensionamento do equipamento otimizado.
Under the project developed in FERESPE company - Iron and Steel Foundry Ltd. has appeared this Master's Thesis, which the main subject involves the development and design of an equipment that allows the injection of gases and powders in the liquid metal bath. The main goal is the promotion of its cleanliness and the homogenization of the molten metal composition. In order to obtain knowledge regarding to this application, equipments and resources were used at this phase of the molten metal processing, literature research and a visit to the National Steel Mill, SA were made and in the meantime makes a in loco process monitoring in the company. They were made studies to support the development of the presented project, such as, several devices were used during the gas injection and after that, operating variables which influence in the hydrodynamic bath, the transport processes and the range of elements normally utilized in oven refining practices. The setting of the operating equipment mode and the different steps for its construction, were crucial for the development work. Based on the company practices and information gathered, the process factors were defined, such as, argon flow and lime like the elements to insufflate. After get the major subsystems of the injection equipment they were defined the refractory casing, the feed type and the blowing circuit. A first draft of the spear, in particular the extremity of the injection, it made possible starting the experimental steps for the spear subsystems designing. Several tests were made, complemented by numerical methods, allowed studying the insufflation system. Initially looking only on the aspiration of the powders and later to be assisted by pressurizing the deposit. After testing all the system subsets its assembly has been made, creating the structure of the final prototype for the realization of the experimental work in the oven. Evolutionary process of all components throughout the project, was achieved due to the numerous tests performed on the fusion of the liquid metal, which have been adapted and optimized the refractory construction techniques. Due to present obstacles, like the frequent obstruction of the spear, there was the necessity to redefine the theoretical values of the pressure to inject for later conjugate them with the speed of the flow, in order to establish stability in the homogenization of the bath behavior. Following the tests carried out to achieve the main objective, it was concluded the optimization of the prototype, that the effects of their actions on the bath are inoffensive. The chemical and physical analysis results to the collected samples shows progress in the cleaning of the molten bath, as a result of the reactions in terms of the composition of inclusions of oxides and sulphides. Finally, the automation and the design of the optimized equipment was performed.