Co-20Cr-15W-10Ni alloy (L-605) is a cobalt-based superalloy combining high strength with keeping high ductility, biocompatible and corrosion resistant. It has been used successfully for heart valves for its chemical inertia, and this alloy is a good candidate for stent elaboration. Control of grain size distribution can lead to significant improvement of mechanical properties: in one hand grain refinement enhance the material strength, and on the other hand large grains provide the ductility necessary to avoid the rupture in use. Therefore, tailoring the grain size distribution is a promising way to adapt the mechanical properties to the targeted applications. The grain size can be properly controlled by dynamic recrystallization during the forging process. Therefore, the comprehension of the recrystallization mechanism and its dependence on forging parameters is a key point of microstructure design approach. The optimal conditions for the occurrence of dynamic recrystallization are determined, and correlation between microstructure evolution and mechanical behavior is investigated. Compression tests are carried out at high-temperature on Thermec-master Z and Gleeble forging devices, followed by gas or water quench. Mechanical behavior of the material at high temperature is analyzed in detail, and innovative methods are proposed to determine the metallurgical mechanisms at stake during the deformation process. Mechanical properties of the material after hot-working and annealing treatments are investigated. The grain growth kinetics of L-605 alloy is determined, and experimental results are compared with the static recrystallization process. Microstructures after hot deformation are evaluated using SEM-EBSD and TEM. Significant grain refinement occurs by dynamic recrystallization for high temperature and low strain rate (T≥1100 ◦ C, strain rate < 0.1s−1), and at high strain rate (strain rate > 10s−1). Dynamic recrystallization is discontinuous and takes place from the grain boundaries, leading to a necklace structure. The nucleation mechanism is most likely to be bulging from grain boundaries and twin boundaries. A new insight of the modeling of dynamic recrystallization taking as a starting point the experimental data is proposed. By combining the results from the mechanical behavior study and microstructure observation, the recrystallization at steady-state is thoroughly analyzed and provides the mobility of grain boundaries. The nucleation criterion for the bulging from grain boundaries is reformulated to a more general expression suitable for any initial grain size. Nucleation frequency can be deduced from experimental data at steady-state through modeling, and is extrapolated to any deformation condition. From this point, a complete analytical model of the dynamic recrystallization is established, and provides a fair prediction on the mechanical behavior and the microstructure evolution during the hot-working process.

Low temperature cleavage fracture behaviour was investigated using four experimental microalloyed bainitic plate steels. The four plate samples were produced by different thermomechanical processing (TMP) schedules and had yield strengths in the range 540 - 670 MPa. Microstructures were characterized by optical microscopy (OM), scanning electron microscopy (SEM) and electron back scattered diffraction (EBSD). Quantitative data was obtained for prior austenite grain (PAG) size, volume fractions of two bainite types (conventional bainite and acicular ferrite) and EBSD 15° domain size. Charpy impact tests (using two notch orientations) were carried out over a range of temperatures. Cleavage facet sizes were measured on -196°C Charpy samples. The range of TMP schedules produced variations in PAG width, type of bainite and 15° domain size. The effects of these three microstructural features on cleavage crack propagation are discussed. Results indicate that the microstructures are controlled by i) deformation below TNR and ii) accelerated cooling rate. Domain structure reflects TMP. There is no clear correlation between domain size and cleavage facet size. / Thesis (Master, Mechanical and Materials Engineering) -- Queen's University, 2009-07-30 19:17:01.25

The design techniques of the components on the macro level are established in the scientific community, however are far behind from the real material performance limits. To obtain those limits, the deeper understanding of the material structure is required. The methods of a new comonents production through standard alloying are the basis of the modern material science manufacturing. The design of the materials with expected required performance limits is the next conceptual step for the materials scientist. As results, to make this step, the problem of a precise material structure analyses on the microstructural level is one os the major importance for the next generation materials design. The complexity of the material structure across the scales(macro-micro) requires a new non deterministic methods for better understanding of the connectivity betwen a materials performance and material microstructure features. This work presents a various new research methodologies and techniques of the material microstructure characterization and numerical design with future applications to the anlyses of the material behavior. The focus of the particular research was to analyse a new cross correlation function of the material structure on the micro length scale and develop a novel framework which allows a better understanding of various important material phenomenas such as failure initiation and recrystallization.

A Faixa Araçuaí foi formada no Neoproterozóico a partir da colisão E-W entre os continentes Sul-Americano e Africano. Sua porção leste compreende uma extensa área migmatítica (~300 km de comprimento por 50-100 km de largura) onde afloram anatexitos e leucogranitos (unidade Carlos Chagas), kinzigitos e granulitos migmatizados, que provavelmente são o registro de uma ampla fusão parcial da crosta intermediária a inferior. Observações de campo associadas com evidências micro-estruturais indicam que a deformação ocorreu quando as rochas estavam incompletamente solidificadas. Estimativas de temperaturas sincinemáticas realizadas a partir do geotermômetro TitaniQ (titânio-em-quartzo) indicam que a temperatura mínima para a cristalização de cristais de quartzo é ~750°C. Tais temperaturas combinadas com composição química de leucossomas dos anatexitos sugerem que a viscosidade das rochas crustais foi reduzida para pelo menos 108 Pa s. Baixo valor de viscosidade associado às evidências de campo e de micro-estruturas são consistentes com a geração de no mínimo 30% de volume de magma durante a orogênese. Grandes quantidades de magma promovem um drástico enfraquecimento da resistência mecânica das rochas à deformação, e atestam que a crosta anatética do extremo leste da Faixa Araçuaí representa um análogo de litosferas quentes (hot orogen), tal como a Himalaiana. Investigação mineralógica detalhada permitiu caracterizar um comportamento dominantemente paramagnético para os anatexitos e ferromagnético para os granulitos. Medidas de orientação preferencial cristalográfica (OPC) a partir da técnica de EBSD (electron backscatter diffraction) revelam que a foliação magnética surge, sobretudo, a partir da orientação preferencial dos eixos [001] da biotita orientados perpendicularmente ao plano de fluxo. Contudo, dada a fraca anisotropia linear desse mineral, apenas uma secundária contribuição de sua subtrama foi observada para a origem da lineação magnética (k1). A correspondência entre os eixos [001] de feldspatos e k1 ocorre devido a OPC de pequenas inclusões de ilmenita que imitam a OPC de seus minerais hospedeiros. Correlação entre k1 da Anisotropia de Remanência Anistéretica (ARA) e k1 da Anisotropia de Suscetibilidade Magnética (ASM) demonstra que, na escala do espécime, a lineação magnética tem uma contribuição da anisotropia dos minerais ferromagnéticos. Assim sendo, a lineação magnética nos anatexitos é o resultado da combinação da trama cristalográfica de feldspatos e de biotita com o alinhamento preferencial de grãos ferromagnéticos. Medidas de ASM realizadas para recuperar a trama mineral e investigar o fluxo nos migmatitos revela um padrão de deformação complexo, no qual, em função das direções de lineação, especialmente, é possível caracterizar três setores estruturais. A porção norte (região estrutural 1) com foliações dominantemente sub-horizontais e lineação fortemente orientada na direção NW-SE representa uma região de escape tectônico que ocorre através de um fluxo horizontal de canal (channel flow). Fluxos de canais possivelmente resultam da atuação de forças gravitacionais (gravity-driven flow). O setor sul (regiões estruturais 2 e 3) com variadas direções de foliação (NE-SW, E-W e NW-SE) e lineações com caimentos para Norte e Oeste, provavelmente refletem um regime de fluxo influenciado, sobretudo, pela tectônica de convergência E-W (collision-driven flow). Ambos os setores sugerem que na escala regional o fluxo crustal registrado pelos migmatitos resulta de um regime de deformação que envolve forças gravitacionais, devido a carga topográfica da crosta superior sobreposta à crosta intermediária parcialmente fundida, com viscosidade baixa, e forças tectônicas, associadas à colisão entre os continentes Sul-Americano e Africano. / The Araçuaí belt was formed by the collision between South American and African protocontinents during the Neoproterozoic. Its eastern part consists of an extensive migmatitic area (~300 km long x 50-100 km wide) where crop out anatexites and leucogranites (Carlos Chagas unit), migmatitic kinzigites and granulites that probably are the record of a widespread partial melting of the middle to lower crust. Field observations associated with microstructural evidences indicate that the deformation occurred when the rocks were incompletely solidified. Synkinematic temperature estimates realized using the TitaniQ (titaniun-in-quartz) geotermomether suggest that the minimum temperature for the quartz crystallization is ~750°C. Such temperatures combined with bulk rock composition of leucosome in the anatexites suggest that the viscosity of crustal rocks was dropped to at least 108 Pa s. Low viscosity values associated with field and microstructural evidences are consistent with the generation of at least 30% volume of melt during the orogeny. The presence of large volumes of melt promotes a drastic weakening of the mechanical strength of rocks and suggests that the anatectic crust of the eastern Araçuaí belt represents an analogue of present day hot orogen such the Himalayas. Detailed mineralogy investigation permitted to characterize the paramagnetic behaviour of the anatexites and the ferromagnetic behaviour of the granulites. Crystallographic preferred orientation (CPO) measurements using the EBSD (Electron Backscatter Diffraction) technique reveal that the magnetic foliation results from the preferred orientation of the biotite [001] oriented normal to the flow plane. However, given the feeble linear anisotropy of this mineral, only a subsidiary contribution of its subfabric to the origin of the magnetic lineation (k1) was observed. Correspondence between [001] of feldspars and k1 is due to the CPO of small inclusions of ilmenite that mimic the CPO of their host minerals. Correlation between k1 of the Anisotropy of Anhysteretic Remanent Magnetization (AARM) and k1 of the Anisotropy of Magnetic Susceptibility (AMS) demonstrate that, at the specimen scale, the magnetic lineation has a contribution of the anisotropy of the ferromagnetic minerals. AMS measurements realized to recover the mineral fabric and investigate the migmatitic flow field revealed a complex strain pattern in which, considering the lineation trends, especially, it is possible to characterize three structural sectors. The north region (structural sector 1) with foliations dominantly sub-horizontal and lineation trending NW-SE is interpreted as a region of tectonic escape that may represent a horizontal channel flow. This oblique tectonic escape probably results from gravity forces (gravity-driven flow). The Southern region (structural sectors 2 and 3) with variable trending foliations (NE-SW, E-W and NW-SE) and lineation plunging to North and West, probably reflect a flow regime dominantly influenced by the E-W convergence of the African and South-American continents (collision-driven flow). Altogether, the characteristics of the various domains suggest that the deformation of the partially molten middle crust of the Araçuaí belt was the result of the combination of gravity forces due to the topographic load and tectonic forces due to the convergence between the African and South-American continents.

The subject of this master’s thesis was to find the causes of impact toughness scattering of forgings of the test disk with dimension range of 540 – 170 mm. The experimental samples were developed from steel A694 F60. To reach the main aim light microscopy, electron microscopy, EBSD technique, fractographic analysis and hardness measurement HV10 were utilized.

Electron Backscatter Diffraction (EBSD) is a well-developed technique used to perform quantitative microstructure analysis in the Scanning Electron Microscope (SEM); however, it has not been widely applied towards studying nanostructures. This work focuses on the use and limitations of EBSD in the characterization of Au nanoparticles on an MgAl2O4 substrate. Samples under investigation are prepared by depositing a thin film of Au on an MgAl2O4 substrate, and then finally heated in a furnace to induce dewetting and cluster formation. The challenges of obtaining crystallographic information from nanoparticles using EBSD are qualitatively and quantitatively described through an evaluation of the quality of the diffraction pattern at various locations of the primary electron beam on the nanoparticle. It is determined that for a high quality Electron Backscatter Diffraction Pattern (EBSP), the production of diffracted backscattered electrons travelling towards the detector must be high and the depth of the source point must be low. The top of the nanoparticle, where the local geometry of the system is similar to the geometry of a macroscopically flat sample, is found to produce diffraction patterns of the highest quality. On the other hand, reversed-contrast EBSPs are observed when the beam is positioned near the bottom of the nanoparticle. In addition, crystallographic information for each individual nanoparticle is gathered using EBSD. Each individual AuNP is observed to be single crystalline. Finally, the complete ensemble of crystalline orientations for individual nanoparticles is then compared to the global averaged crystallinity of the sample, as measured by X-ray diffraction. These results show that EBSD promises to be a powerful and robust technique in the characterization of nanoparticles. / Thesis / Master of Applied Science (MASc)

No description available.

The Cold-Gas Dynamic-Spray process also known as Cold Spray (CS) has been researched for three decades. The CS process is a solid-state deposition technique via supersonic velocity of powder particles at a temperature significantly below the melting point of the spray material. This thesis presents background on the overall CS process parameters, and additional information on the microstructural and mechanical properties of typical Cold Sprayed materials.This Thesis primarily presents a study on the microstructural annealing response of CS Al 6061. It should be noted that for this study, the term “annealing” is used in the sense of the classical metallurgical definition of annealing, and not a specific temper designation for the 6061 alloy. Cross sections of CS Al 6061 were imaged with a scanning electron microscope (SEM) in secondary electron (SE), backscatter electron (BSE), and electron backscatter diffraction (EBSD) imaging mode for quantitative and qualitative information on the grain size and orientation of the CS microstructure. The detailed SE, BSE and EBSD mode images present the grain size and grain orientation of the original powder, as received (AR) state and after heat treating at 200°C for 1 hour, 10 hours, and 100 hours. Three different regions, characterized with distinctly differing microstructures, are labeled as low, medium, and high deformation regions, and their microstructures, and evolving features are discussed. Vickers microhardness testing are performed to examine the differences in hardness values between different heat treatments, and for correlation with the level of deformation and grain refinement in the microstructure. SEM imaging was used in BSE mode to correlate microhardness variation to the different regions within the CS microstructure.

Cette thèse s’inscrit dans une démarche d’investigation des mécanismes d’endommagement de réfractaires électrofondus à très haute teneur en zircone. L’accent est en particulier mis sur la compréhension du phénomène de microfissuration, mécanisme de dégradation le plus dommageable pour ces matériaux. S’opérant au refroidissement, il conduit à la fracture des blocs électrofondus. Réalisés dans le cadre du programme NOREV (NOouveau REfractaires Verriers) soutenu par l’ANR, les travaux présentés sont le fruit d’une collaboration avec Saint Gobain CREE, le Centre des Matériaux P.M. FOURT de l’Ecole des Mines de Paris, le laboratoire GEMH de l’ENSCI de Limoges, ICAR et Euro Physical Acoustics. Ils font suite aux travaux réalisés lors du programme PROMETHEREF (2002-2005). Des expériences préliminaires ont permis de définir et d’affiner les orientations de l’étude. Prenant en considération l’anisotropie de dilatation de la zircone monoclinique et quadratique décrite dans la littérature, l’imagerie des électrons rétrodiffusés a notamment permis de révéler un lien entre l’arrangement de domaines cristallographiques et la fissuration observée. D’autres expérimentations conduites dans le domaine de l’émission acoustique ont mis en lumière son applicabilité et ses apports pour notre problématique ainsi que la nécessité de développer un algorithme de traitement adapté. Ainsi, trois axes de recherche ont été développés. Ils visent, par leur complémentarité, à permettre une analyse à plusieurs échelles de l’endommagement des matériaux de l’étude tout en s’appuyant sur leur comparaison. Ils permettent respectivement d’évaluer l’endommagement de manière indirecte, d’en examiner les origines à l’échelle microscopique et d’en déterminer l’occurrence en température à l’échelle globale de l’échantillon. Le premier volet consiste en une évaluation des propriétés mécaniques en températures soulignant les incidences de la fissuration. La mise en évidence de la fissuration sous-critique, l’évolution des propriétés élastiques ainsi que la détermination des propriétés à la rupture apportent autant d’éléments qui permettent ensuite d’enrichir l’étude fractographique. Le deuxième volet s’attache, après une interrogation quant à la présence simultanée de zircone monoclinique et quadratique, à déterminer les paramètres de maille et les coefficients de dilatation de ces deux structures pour les différents matériaux. La modélisation des mailles correspondantes se révèle alors d’un grand intérêt pour l’analyse de cartographies EBSD. Enfin, la validation et l’application d’un process de traitement novateur des données d’émission acoustique, intégrant un algorithme génétique, permet de quantifier l’endommagement et d’apporter des précisions quant à son action en température. Ces constatations sont confortées par des suivis par acousto-ultrasons. / This thesis falls under an approach of investigation on the damage mechanisms of high zirconia fused-cast refractories. The focus is particularly set on the comprehension of the phenomenon of microcracking responsible for the degradation of these materials. Taking place at cooling time, it leads to the fracture of the fused-cast blocks. Realized within the framework of the French research programme NOREV (NOouveau REfractaires Verriers) supported by the ANR, the work presented in this manuscript is the fruit of a collaboration with Saint Gobain CREE, the Centre des Materiaux P.M. FOURT of the Ecole des Mines de Paris, the laboratory GEMH of the ENSCI of Limoges, ICAR and Euro Physical Acoustics. It follows the works completed at the time of the previous programme (PROMETHEREF, 2002-2005). Preliminary experiments have enabled to define and specify the directions of this study. Taking into account the thermal expansion anisotropy of both monoclinic and tetragonal zirconia as described in the literature, the imagery of the backscatter electrons has in particular revealed a link between the presence of crystallographic domains and the observed cracking. Other experiments conducted in the field of acoustic emission have clarified its applicability and its contributions to our problems as well as the need for developing an adapted algorithm to process data. Thus, three research orientations have been developed. They aim, by their complementarity, to allow an analysis of the different scales of the damage on the study materials and is based on their comparison. They respectively allow to assess the damage in an indirect way, to examine its origins at a microscopic level and to determine its occurrence in temperature at the global scale of the sample. The first axis consists in the evaluation of the mechanical properties in temperatures emphasizing the incidences of cracking. The description of subcritical cracking, the evolution of the elastic properties as well as the determination of the fracture properties bring elements which enable to enrich the fractographic study. The second axis aims, after an interrogation as for the simultaneous presence of monoclinic and tetragonal zirconia, to determine the cell parameters and the thermal expansion coefficients of both structures for the different materials. The modeling of the corresponding cells then appears of great interest for the analysis of EBSD maps. Lastly, the validation and the application of an innovative process for the treatment of the acoustic emission data integrating a genetic algorithm enable to quantify the damage and to bring precise details as for its action in temperature. These observations are consolidated by acousto-ultrasounds follow-ups.

Gegenstand der vorliegenden Arbeit ist die templatgestützte Erzeugung metallischer Stäbchen und Ringstrukturen im Mikrometer- und Nanometerbereich. Derartige Strukturen besitzen vor allem aufgrund ihres außergewöhnlichen Verhaltes gegenüber elektromagnetischen Wellen ein hohes Potential für optische, elektronische, magnetische oder sensorische Anwendungen. Zunächst wird das Vorgehen zur Herstellung mesoskopischer Ringe durch die Infiltration von Kolloidkristallen aus Siliziumdioxid mittels geeigneter Präkursorlösungen detailliert betrachtet. Daraufhin werden Ansätze zur Optimierung einzelner Teilschritte vorgestellt. Im Anschluss erfolgt die Übertragung des Verfahrens auf die Herstellung von Goldringen. Neben der elektronenmikroskopischen Charakterisierung der Proben wird unter anderem durch energiedispersive Röntgenspektroskopie (EDXS), Elektronenrückstreubeugung (EBSD) und Röntgenphotoelektronenspektroskopie (XPS) bestätigt, dass die entstandenen Strukturen aus metallischem Gold bestehen. Ein weiterer Inhalt dieser Arbeit ist die Konzeption und Umsetzung einer Apparatur zur elektrochemischen Erzeugung von mesoskopischen Metallstäbchen im Inneren von porösen Aluminiumoxidmembranen. Im Anschluss wird die Herstellung von Silber- und Goldstäbchen beschrieben. Außerdem wird aufgeführt, wie die sequenzielle Abscheidung der beiden Metalle unter anschließender Auflösung des metallischen Silbers zur Erhöhung der Ausbeute an isolierten Goldstäbchen führt.