Made available in DSpace on 2016-03-15T19:36:50Z (GMT). No. of bitstreams: 1 Leilah Delaretti Luongo.pdf: 2162579 bytes, checksum: 76c30f5d2ee2f42b33cf84bd04999ac2 (MD5) Previous issue date: 2015-05-22 / In this work, samples of copper-silver and silver-copper-nickel alloys were synthesized by powder metallurgy. The alloys have received sintering and all of them were characterized metallographically. Different and significant effects were observed in the microstructure and conductivity of the samples studied. The influence of silver on the conductivity of the samples with nickel resulted to be lower than the alloy with chromium and nickel, studied in previous work of the research group, where the same procedures were applied to the same precursors. An interesting result is that the larger crystallite size favored the high electrical conductivity, which is presented in the samples without nickel. The presence of nickel helped to inhibit oxidation and the difference in the amount of nickel influenced the alloys behavior, however, it did not guarantee high conductivity observed in the aforementioned alloys copper-nickel-chromium. The structure of the samples was studied by the Rietveld Method, using data from x-ray diffraction. The differences in microstructure were investigated by comparing the parameters of the pure copper used as a precursor profile. / Neste trabalho foram sintetizadas amostras de ligas metálicas de cobre-prata e cobre-níquel-prata obtidas por metalurgia do pó. As ligas receberam tratamentos térmicos de sinterização e foram caracterizadas metalograficamente. Foram observados efeitos diferentes e significativos na microestrutura e na condutividade das amostras estudadas. A influência da prata na condutividade das amostras com níquel resultou ser inferior à de ligas com cromo e níquel, estudadas em trabalhos precedentes do grupo de pesquisa, onde se aplicaram os mesmos procedimentos aos mesmos precursores. Um resultado interessante é que o maior tamanho de cristalito favoreceu a condutividade elétrica, o qual se apresentou nas amostras sem níquel. A presença do níquel ajudou a inibir a oxidação e a diferença na quantidade de níquel se mostrou importante no comportamento das ligas, porém, não garantiu a alta condutividade verificada nas mencionadas ligas de cobre- níquel-cromo. A estrutura das amostras foi estudada pelo Método de Rietveld, usando dados de difração de raios x. As diferenças na microestrutura foram estudadas através da comparação com os parâmetros de perfil do cobre puro usado como precursor.

Le procédé de fusion sélective par laser est un des nombreux procédés de fabrication additive qui permet la production rapide de pièces à partir d'un fichier CAO (conception assistée par ordinateur) et de lits de poudre. Après une description du fonctionnement du procédé par l'intermédiaire de ses paramètres opératoires, le manuscrit décrit les travaux entrepris pour l'élaboration de pièces en Inconel 625. Ce superalliage à base nickel a fait l'objet d'une étude paramétrique pour déterminer un jeu de paramètre optimal permettant de produire des pièces saines. Cette étude est basée sur des considérations énergétiques qui visent à maximiser le rendement de conversion de l'énergie électromagnétique en énergie thermique tout en assurant la cohésion entre couches. Des essais de traction valident la stratégie employée au niveau de l'étude paramétrique. Un second alliage est étudié, l'Inconel 738 qui est un superalliage renforcé par la précipitation d'une phase γ'-Ni3(Al,Ti). Les travaux entrepris ne concernent pas l'élaboration mais la caractérisation de l'alliage. Il est mis en évidence que celui-ci est dans un état hors de l'équilibre thermodynamique lorsque produit par fusion laser sélective. La précipitation de la phase durcissante n'est pas complète. Ce constat peut permettre d'éviter la fissuration de l'alliage pendant la fabrication en adaptant les paramètres opératoires, notamment au niveau du préchauffage. Une étude sur les traitements thermiques montre que la gamme appliquée traditionnellement à l'alliage coulé ne convient pas pour l'alliage élaboré par fusion sélective ; cette étude ouvre sur des alternatives. Enfin, ces travaux apportent quelques éléments de réponse quant à la pertinence énergétique du procédé. / The selective laser melting (SLM) process is one of the many additive manufacturing processes that allow to rapidly build a part from a computer-aided design (CAD) file and from a powder bed. The work described here deals with the different parameters related to the process, namely the building platform stepping and the laser radiation and its interaction with the metallic matter. The first Ni-based superalloy studied here is Inconel 625 which has been subjected to a parametric study with an energetic approach. It was all about finding the maximum in the conversion of electromagnetic energy into thermal energy. Tensile tests validate the use of the energetic strategy for this alloy. The second studied alloy is Inconel 738 which is hardened by fine γ'-Ni3(Al,Ti) precipitates. Microstructure observations and differential thermal analysis reveal that the γ' precipitation is not complete when the alloy is processed by SLM. This leads to give clues for crack-free processing by adjusting the parameters and especially the preheating feature. Different heat treatments on SLMed materials have been investigated. It appears that the standard procedure applied on cast alloy to reach proper microstructure for good mechanical properties is not adapted to the SLMed alloy. New standards must be defined to comply with the initial out of equilibrium state. Last but not least, the manuscript gives information regarding the energetic use of the process which should be compared with the will of environmental impact reduction policy called by the process.

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.

Les procédés additifs, auxquels appartient la fusion laser de poudres métalliques, ont la capacité de créer des structures à géométries complexes, avec la possibilité d'intégrer des formes creuses, par exemple des canaux de refroidissement assurant un contrôle thermique optimum. Ce procédé permet de fabriquer des pièces réelles à partir de poudres métalliques, par fusion du matériau, couche par couche, en accord avec le modèle CAO. Au cours du procédé, de nombreux cycles thermiques et d'importants gradients thermiques se produisent dans la pièce au cours de sa fabrication. Ces gradients de température induisent des déformations plastiques hétérogènes et de ce fait des contraintes résiduelles. Ces contraintes peuvent nuire à la qualité de la pièce obtenue, par exemple sa résistance mécanique. Ces travaux ont pour objectifs de proposer un modèle numérique, s’appuyant sur la méthode des éléments finis afin d'étudier l'apparition des contraintes résiduelles lors du procédé de fusion laser de poudres métalliques. Le logiciel multiphysique ABAQUS® a été utilisé pour effectuer les analyses thermiques et mécaniques. La technique « d'ajout et de suppression des éléments » a été utilisée afin de simuler la fusion et la solidification de la matière au cours du procédé. Les propriétés mécaniques dépendantes de la température de l'acier maraging, utilisé dans notre cas, ont été obtenues à l’aide d’essais expérimentaux de caractérisations et intégrées dans le modèle. Les calculs sont réalisés de manière découplée, dans un premier temps le calcul thermique est effectué, puis les résultats sont utilisés pour réaliser le calcul mécanique et finalement prédire les champs de contraintes. Dans le cadre de ce travail, une méthode originale s'appuyant sur la technique de mesure des contraintes résiduelles par enlèvement de couches successives a été mise au point pour mesurer ces contraintes en direct au cours du procédé. Les résultats renseignent sur le niveau et la distribution des contraintes dans la pièce créée et le support. Deux paramètres ont été testés afin d'étudier leur influence sur le niveau des contraintes résiduelles : le temps d’étalement de la poudre entre deux couches successives et la hauteur des couches. Le modèle numérique paramétrable permet d'analyser les effets de paramètres liés au procédé sur la répartition des contraintes résiduelles dans les pièces fabriquées. Les résultats montrent que la variation de l'épaisseur du support n'affecte pas la répartition des contraintes dans la pièce créée. Le préchauffage du support à une température de 800°C réduit les contraintes résiduelles L'étude de quelques trajectoires laser montre leurs influences sur la répartition des déformations plastiques cumulées ainsi que la hauteur des couches de poudres ou de la forme du support (embase, colonnes). / The Selective Laser Melting process, belonging to Additive processes , have the ability to create structures with complex geometries , with the possibility of including cavities, such as cooling channels providing optimum temperature control. This process enables the manufacture of three-dimensional parts from metal powders by melting the material , layer by layer, in agreement with the CAD model. In the process , high temperatures and thermal gradients cycles occur in the part during the process. These temperature gradients induce heterogeneous plastic strain and residual stresses. These residual stresses may affect the quality of the part obtained, for example the fatigue life. This work aims to propose a numerical model , based on the finite element method to study the appearance of residual stresses during laser melting process of metallic powders . The ABAQUS® Multiphysics software was used to perform the thermal and mechanical analyzes. The movement of the laser beam and the resolution of the thermal problem can predict the evolution of the temperature in the part and support. The "birth and death elements" technique was used to simulate the melting and solidification of the material during the process. Dependent mechanical properties of the temperature of the maraging steel used in this case were obtained using experimental testing and characterization and were established in the model. The calculations are decoupled : initially thermal calculation is performed and the results are used to perform mechanical calculations and finally predict the residual stress fields. In this work, a novel method based on the technique of measuring residual stresses by removing layers was developed to measure these stresses directly in the process. The results provide information on the level and distribution of stresses in the created part and support. Two parameters were tested to study their influence on the level of residual stress : time to spread the powder between two successive layers and layer height. The model is used to analyze the effects of process parameters related to the distribution of residual stresses in the manufactured parts. The results show that the variation of the thickness of the support does not affect the distribution of stresses in the part created. Preheating the substrate to a temperature of 800 °C reduces the residual stresses. The study of some laser strategies shows their influence on the distribution of plastic strain thus the height of the layers of powder or in the form of support (base, columns).

Aços inoxidáveis austeníticos são materiais amplamente utilizados em sistemas que exigem elevadas resistências à oxidação e à corrosão. No entanto, quando em contato com outras superfícies, esses materiais possuem elevado coeficiente de atrito e baixa resistências ao desgaste. Uma alternativa para melhorar suas propriedades tribológicas é a utilização de lubrificantes sólidos adicionados em suas composições pela técnica de metalurgia do pó (M/P). Materiais como itria e boro têm se mostrado eficazes em melhorar as propriedades mecânicas e tribológicas de ligas Fe-Cr-Ni-Mo. Nesse contexto, o objetivo desse estudo foi avaliar o efeito da adição de boro e de itria na microestrutura e nas propriedades tribológicas de aços inoxidáveis austeníticos Fe-Cr-Ni-Mo obtidas por M/P. Foram preparadas amostras de 316L por M/P em quatro condições diferentes. Duas amostras, uma sem aditivo e outra com 0,6% p de boro adicionado à composição do 316L, foram processadas a pressão de compactação de 800 MPa e temperatura de sinterização de 1240°C. Além dessas, duas amostras, uma sem aditivo e outra com 1,0% p de itria adicionada à composição do 316L, foram processadas a pressão de compactação de 400 MPa e temperatura de sinterização de 1280°C. Determinou-se a composição química por espectrometria de emissão óptica, a microdureza Vickers, a microestrutura por MEV e EDS, o comportamento tribológico por ensaio de deslizamento alternado (coeficiente de atrito e coeficiente de desgaste específico) e por MEV e EDS (mecanismos de desgaste). Os resultados mostraram que a adição de boro aumenta significativamente a resistência ao desgaste dos materiais, devido à melhor densificação e à formação de fases duras (como boretos ricos em cromo e molibdênio) na sinterização. A adição de itria, mesmo com o aumento da dureza, diminui a resistência ao desgaste, pois dificultou a densificação devido a sua baixa interação com a matriz austenítica do material. O coeficiente de atrito se manteve em 0,8 para todos os materiais, o que indica que os aditivos não o influenciam e não atuam como lubrificantes sólidos. Os mecanismos de desgaste observados nas superfícies dos materiais desgastado foram os mecanismos por adesão e por reação triboquímica. / Austenitic stainless steel materials are widely used in systems that require high oxidation resistance and corrosion resistance. However, in contact with other surfaces, these materials show a high coefficient of friction and a low wear resistance. An alternative to improve their tribological properties is the use of solid lubricants added in their composition by the powder metallurgy technique (P/M). Materials such as yttria and boron have shown an effective role in improving the mechanical and tribological properties of Fe-Cr-Ni-Mo alloys. In this context, this study aims evaluating the effect of boron and yttria additions on the microstructure and tribological properties of austenitic stainless steels Fe-Cr-Ni-Mo obtained by P/M. Samples were prepared with 0.6 wt% boron and 1wt% yttria, using compaction pressures of 400 MPa and 800 MPa, sintering temperature 1240°C and 1280°C, in argon atmosphere. The materials were characterized by chemical analysis (optical emission spectrometry), Vickers hardness and microstructural analysis (SEM and EDS). The coefficient of friction and the wear rate of the materials were obtained by means of reciprocating sliding tests. The wear mechanisms were evaluated by SEM and EDS. The results showed that the boron addition significantly increases the wear resistance of the material, due to the improved densification and the formation of hard phases (such as chromium-rich borides and molybdenum-rich borides) during sintering. However, even though with the increased hardness, the yttria addition decreases the wear resistance, due to the not favouring of the densification and the low interaction of yttria particles with the austenitic matrix. The coefficient of friction for all materials was about 0.8, i.e., and it was not influenced by the presence of additives in the composition. The predominant mechanisms on the worn surfaces of the materials were the adhesive wear and the tribochemical reaction wear (wear by particles oxidation).

The aim of this thesis is preparation and characterization of bulk Mg–Ti based materials. In the first theoretical part properties of base materials and the complexity of preparation alloy from these metals is discussed. Second part is focused on powder metallurgy and its applicability on Mg–Ti system. In another part particle composites are described. In chapter current research another possible methods of alloy preparation from magnesium and titanium are mentioned. The experimental part of this thesis was the preparation of bulk Mg–Ti materials from metal powders. For sample preparation conventional methods of powder metallurgy and spark plasma sintering was employed. Furthermore a characterisation of these materials was done. Microstructure was observed. Present phases were found using X-ray diffraction analysis. Amounts of these phases were determined using a scanning electron microscope with energy–dispersive spectrometry and using X-ray fluorescence. Furthermore hardness was measured and bending test with evaluation was done. Significant difference in results of sample preparation using conventional methods of powder metallurgy and spark plasma sintering was observed.

Dissertation thesis deals with basic research in the field of materials from pure Zn powders and Mg, Zn, and Ca binary mixtures prepared by powder metallurgy. General powder metallurgy principles and methods, a brief description of Mg, Zn, and Ca structure and properties, and the latest research in the field of bulk materials preparation from these elements via powder metallurgy are summarized in the theoretical part of the thesis. The experimental part focuses on the preparation of materials from finer and coarser Zn powder particles by hot pressing at 300 and 400 °C using the pressure of 100, 200, 300, 400, and 500 MPa. Binary mixtures based on Mg with the addition of Zn or Ca were prepared by hot pressing in the solid-state (300 °C) and hot pressing in the semi-solid state (400 °C, 450 °C in the case of Mg-Ca system) using the pressure of 500 MPa. Binary mixtures based on Zn with the addition of Mg or Ca were prepared by hot pressing in the semi-solid state (400 °C) using the pressure of 500 MPa. The prepared materials were evaluated in terms of microstructure, elemental and phase composition, microhardness, flexural strength, and fractography. The results showed that in the case of processed from pure Zn powders, a better combination of the flexural strength and displacement was achieved in the case of the finer Zn powder, namely in the material prepared at a temperature of 400 °C and a pressure of 500 MPa. In the case of mixtures, the best connection between the powder particles was achieved in the case of a material based on finer Zn powder with 0.5 wt.% of Mg, which had a significant effect on the achieved values of flexural strength and displacement. The amount of minor powder in the mixture had a significant effect on the prepared material structure and phase composition, while the processing conditions influenced the reached strength characteristics and fracture mechanism.

Diploma thesis focuses on preparation and characterization of bulk material prepared from pure magnesium powder. The topic includes all the parts of process of bulk material preparation, sintering at hot pressing, diffusion processes and structurally-mechanical properties with respect to final material porosity of the produced material. Thesis solving focuses on study and control of processes during bulk material preparation and description of the processes from physically-chemical point of view of the structure creation and final material properties.

Mechanical properties of aluminium alloys highly depend on their phase composition and microstructure. High strength can be achieved among others by introduction of a high volume fraction of fine, homogeneously distributed second phase particles and by a refinement of the grain size. Powder metallurgy allows to prepare fine grained materials with increased solid solubility which are favourable precursors for further precipitation strengthening. Gas atomization was used for the preparation of powders of the commercial Al7075 alloy and its modification containing 1 wt% Zr. A part of gas atomized powders was mechanically milled at different conditions. Mechanical milling reduced the grain size down to the nano-size range and the corresponding microhardness exceeded the value of 300 HV. Powders were consolidated by the spark plasma sintering method to nearly fully dense compacts. Due to a short time and relatively low temperature of sintering the favourable microstructure can be preserved in the bulk material. The grain size of compacts prepared from milled powder was retained in the submicrocrystalline range and the microhardness close to 200 HV exceeded that of the specially heat treated ingot metallurgical counterparts. The prepared compacts retained their fine grained structure and high...

This diploma thesis focused on manufacturing and characterization of Ti-15Mo metastable beta-Ti alloy prepared by cryogenic milling and spark plasma sintering. Initial powder was prepared by gas atomization and consequently deformed by cryogenic milling (milled powder). Both initial and milled powders were compacted by spark plasma sintering (SPS) at temperatures from 750 řC to 850 řC. Dependence of microstructure and mechanical properties on the parameters of preparation was studied. During cryo-milling, powder particles significantly changed shape from ball-shaped to disc-shaped. Particles were not refined by milling, but severely plastically deformed. SEM observations showed that all prepared samples contain duplex alpha + beta structure. Volume fraction of alpha phase is significantly higher in the sintered milled powder due to increased beta- transus temperature caused by contamination by oxygen and also due to easier alpha phase precipitation caused by refined microstructure. Maximum microhardness of 350 HV was achieved for both types of sintered powders. High microhardness of sintered initial powder can be attributed to formation of omega phase during cooling, while sintered milled powder is strengthened by refined microstructure and small alpha phase precipitates. Cryogenic milling prior to...