Gelöster Wasserstoff in Metallen führt in vielen Fällen zu einer Reduzierung der Güte von mechanischen Eigenschaften. Dies äußert sich auf vielfältige Weise und wird unter dem Begriff Wasserstoffversprödung zusammengefasst. Für ein grundlegendes Verständnis dieses Phänomens müssen die Vorgänge im Metall auf mikroskopischer Skala ergründet werden. Im Rahmen dieser Arbeit wurde daher ein Aspekt der Wasserstoffversprödung, die Interaktion von Wasserstoff mit Versetzungen, näher untersucht. Zur Untersuchung des Einflusses von Wasserstoff auf die Versetzungsbildung wurden verschiedene Verformungsexperimente an Palladium und Vanadium durchgeführt. Prinzipielle Vorgänge der Defektbildung wurden durch Versuche an einzelnen Versetzungen unter Verwendung von Nanoindentation und Zugexperimenten im ETEM durchgeführt, um einen breiten Überblick zu erlangen. Zusätzlich wurden zum besseren Verständnis der Vorgänge Molekulardynamiksimulationen von derartigen Versuchen ausgeführt. Zur Untersuchung der Interaktion von Versetzungen miteinander wurden Säulen im Mikrometerbereich verformt und Blech durch Kaltwalzen verformt. Des Weiteren wurde durch Hochdruck-Torsion maximale Verformungen realisiert. Die verwendeten Modellmaterialien erlauben es verschiedene prinzipielle Vorgänge der Defektbildung zu untersuchen und so einen breiten Überblick über prinzipielle Vorgänge im kfz Gitter (Palladium) bzw. krz Gitter (Vanadium) zu erhalten.

Crystallographic texture and its evolution are known to be major sources of anisotropy in polycrystalline metals. Highly simplified phenomenological models cannot usually provide reliable predictions of the materials anisotropy under complex deformation paths, and lack the fidelity needed to optimize the microstructure and mechanical properties during the production process. On the other hand, physics-based models such as crystal plasticity theories have demonstrated remarkable success in predicting the anisotropic mechanical response in polycrystalline metals and the evolution of underlying texture in finite plastic deformation. However, the integration of crystal plasticity models with finite element (FE) simulations tools (called CPFEM) is extremely computationally expensive, and has not been adopted broadly by the advanced materials development community. The current dissertation has mainly focused on addressing the challenges associated with integrating the recently developed spectral database approach with a commercial FE tool to permit computationally efficient simulations of heterogeneous deformations using crystal plasticity theories. More specifically, the spectral database approach to crystal plasticity solutions was successfully integrated with the implicit version of the FE package ABAQUS through a user materials subroutine, UMAT, to conduct more efficient CPFEM simulations on both fcc and bcc polycrystalline materials. It is observed that implementing the crystal plasticity spectral database in a FE code produced excellent predictions similar to the classical CPFEM, but at a significantly faster computational speed. Furthermore, an important application of the CPFEM for the extraction of crystal level plasticity parameters in multiphase materials has been demonstrated in this dissertation. More specifically, CPFEM along with a recently developed data analysis approach for spherical nanoindentation and Orientation Imaging Microscopy (OIM) have been used to extract the critical resolved shear stress of the ferrite phase in dual phase steels. This new methodology offers a novel efficient tool for the extraction of crystal level hardening parameters in any single or multiphase materials.

<p>Predstavljena je nova metoda intenzivne plastične deformacije &ndash; višefazno sabijanje V-alatom. Koristeći ovu metodu, sabijanjem u osamnaest faza, unapređene su mehaničke osobine niskougljeničnog čelika Č.1221 &ndash; tvrdoća, čvrstoća i deformabilnost. Za ispitivanje mikrostrukture korišćeni su svetlosni, skening i transmisioni mikroskop. Prosečna veličina kristalnog zrna početnog materijala od 19 mikrometara je smanjena na 250 nanometara nakon dvanaest faza sabijanja. Nakon osamnaest faza sabijanja na čelu uzorka ostvarena je ukupna deformacija u iznosu od 3,38.</p> / <p>A new severe plastic deformation method has been presented - multistage upsetting by V-shape dies. By using this method, in eighteen upsetting stages, mechanical propreties (hardness, strenght and formability) of C15E low carbon steel has been improved. For microstructure analysis light, scanning and transmission microscopes have been employed. Initial average grain size of 19 &mu;m has been reduced to 250 nm after twelve upsetting stages. After eighteen upsetting stages, total effective deformation at the sample forehead of 3,38 has been obtained.</p>

Este trabalho estuda a aplicação de um Ensaio Não-Destrutivo de Inspeção (ENDI), baseado na técnica Ruído Magnético de Barkhausen (RMB), na detecção de regiões não homogêneas em chapas de aços carbono. Apresentando os avanços no desenvolvimento de uma nova variante de ensaio não-destrutivo magnético, denominada Escaneamento Contínuo de Ruído Magnético de Barkhausen (ECRMB). O RMB é gerado por abruptas mudanças na magnetização de materiais magnéticos quando são submetidos a campos magnéticos variáveis. Essas mudanças são afetadas pela micro-estrutura e a presença e distribuição de tensões elásticas (compressão e tração), deformação plástica e alteração da micro-estrutura. Neste trabalho analisou-se a sensibilidade dos sinais de RMB na detecção de deformações plásticas em parâmetros tais como, frequência de campo magnético de excitação e a velocidade de movimentação da sonda. O comportamento do parâmetro RMSRMB dos sinais de RMB se correlacionou com a posição das regiões não homogêneas detectadas nas amostras. Sendo, contudo ainda feita uma avaliação da técnica aplicada para a medição, fazendo uma comparação dos resultados obtidos com a técnica de Ruído Magnético de Barkhausen Estático (RMBE) que é uma técnica já estabelecida na literatura. Os resultados mostraram, que para cada um dos casos estudados, é possível detectar a posição do dano produzido. Essa nova técnica aumenta o espectro de soluções de ENDI para problemas não contemplados pelas técnicas existentes. / This work the application of a technique of Non-Destructive Inspection Test (NDIT) based on the technical Magnetic Barkhausen Noise (MBN), the detection of non-homogeneous regions in sheets of carbon steels. It presents advances in the development of a new technique of magnetic non-destructive testing. Particularly a variant nominated Scanning Continuous Magnetic Barkhausen Noise (SCRMB). The MBN are generated by abrupt changes in the magnetization of materials when subjected to varying magnetic fields. These changes are affected by the microstructure and the presence and distribution of elastic stresses (compression and tension). We analyzed the sensitivity of the signal MBN detection plastic deformation on parameters such as magnetic field excitation frequency and the probe movement speed. The RMSMBN parameter behavior of MBN signals correlated with the position of non-homogeneous regions detected in the samples. An evaluation of the technique applied to the measurement was performed by making a comparison of the results obtained with MBNE technique, is a technique already established in the literature. The results showed that for each of the studied cases, it is possible to detect the position of the damage produced. This new technique increases the spectrum of NDIT solutions for problems not covered by existing techniques.

Nesta Dissertação são apresentados os resultados do estudo da evolução microestrutural de um aço inoxidável dúplex UNS S32205 durante o processo de laminação a frio e posterior recozimento em 1080ºC. Amostras do aço na condição como-recebida, laminadas a frio e recozidas isotermicamente foram caracterizadas utilizando as técnicas de microscopia ótica e eletrônica de varredura, dilatometria, espectroscopia de energia dispersiva (EDS), microdureza Vickers, difração de raios X, magnetização de amostra vibrante, macrotextura e difração de elétrons retroespalhados (EBSD). No material na condição como-recebido foi possível observar uma microestrutura com a austenita parcialmente recristalizada (53%) apresentando maclas de recozimento e a ferrita recuperada. Uma fração volumétrica de cerca de 50% de cada fase foi encontrada. Cálculos termodinâmicos e análises químicas via EDS mostram boa concordância quanto à partição de soluto existente entre a ferrita e a austenita. Análises de magnetização mostraram que não houve variação considerável na fração de fase magnética nas amostras laminadas a frio até 79% de redução em espessura, ou seja, não foi possível observar a formação de martensita induzida por deformação nas condições de laminação utilizadas. Medidas do campo coercivo (Hc) e magnetização remanente (MR) mostram, porém, um comportamento quase linear em relação ao grau de deformação. Por meio de medidas de difração de raios X, utilizando uma análise qualitativa do alargamento de picos difratados, observou-se maior encruamento da austenita durante a laminação a frio. O mesmo comportamento foi encontrado em medidas de dureza individual de fases, assim como em análises de desorientação média de kernel (KAM) obtidos via EBSD. Análises de macrotextura e microtextura mostraram que o material na condição como-recebido possui uma textura forte, principalmente a ferrita, apesar de ser proveniente de um processo de laminação a quente. Durante a laminação a frio não foram observadas grandes mudanças nas componentes de textura em ambas as fases, porém, observou-se a intensificação da componente Goss-Latão na austenita, devido à deformação plástica e à formação de bandas de cisalhamento. Na ferrita observou-se uma típica intensificação da fibra ??com o aumento da deformação plástica. As amostras deformadas 43% e 64% recozidas em 1080 ºC apresentaram uma microestrutura totalmente recristalizada após 3 min de tratamento, caracterizada pela formação de uma estrutura tipo \"bambu\". Com 1 min de tratamento, através de análises de espalhamento da orientação de grão (GOS), observou-se a ocorrência de recristalização primária na ferrita (42% de grãos recristalizados) na amostra laminada 43%. Por outro lado, a austenita manteve uma microestrutura levemente recuperada. Com uma deformação de 64%, a fração recristalizada da ferrita não foi alterada significativamente enquanto que a austenita apresentou uma fração recristalizada de 43%. Análises de KAM mostraram uma maior diferença de energia armazenada na austenita do que na ferrita entre as amostras laminadas até 43% e 64%. Após o recozimento não foram observadas mudanças significativas na microtextura de ambas as fases. Porém, na ferrita observou-se um aumento considerável da fração dos contornos especiais (CSL) ?3, ?13b e ?29a (entre 11% e 12% no total) enquanto que na austenita somente um aumento na fração dos contornos tipo ?3 (cerca de 15%) associados aos contornos de macla foi identificado. / In this Dissertation, results of the study of the microstructural evolution of a duplex stainless steel UNS S32205 during the cold rolling process and further isothermal annealing at 1080ºC are reported. Samples of the steel in the as-received, cold-rolled and annealed conditions were characterized using light and scanning electron microscopy, dilatometry, energy dispersive spectroscopy (EDS), Vickers hardness, X-ray diffraction (XRD), vibrating sample magnetization, macrotexture (XRD) and electron backscatter diffraction (EBSD). In the as-received material it was possible to observe a microstructure with partially recrystallized austenite (53%) with the presence of annealing twins and recovered ferrite. A volume fraction of approximately 50% of each phase was found. Thermodynamic calculations and chemical analysis via EDS showed good agreement on solute partitioning between ferrite and austenite. Magnetization analysis showed that there was no considerable changes in the magnetic phase fraction in the samples cold rolled up to 79% in thickness reduction. Hence, it was not possible to observe the formation of deformation induced martensite with the rolling conditions used in this work. Measurements of the coercive field (Hc) and remnant magnetization (MR) show, however, an almost linear behavior in relation to the degree of deformation. Through X-ray diffraction measurements, using a qualitative analysis of the diffracted peaks broadening, a higher work hardening of austenite was observed during cold rolling. The same behavior was found in hardness measurements of individual phases, and in the average kernel misorientation analysis (KAM) obtained by EBSD. Analysis of macrotexture and microtexture showed a strong texture in the as-received material, especially in ferrite, although this material was obtained by a hot-rolling process. During cold-rolling, no significant changes were observed in the texture components of both phases. However, an increase of the Goss-to-Brass component in austenite was noticed, and it may be related to the work hardening and to the formation of shear bands. In ferrite, the strengthening of the ?-fiber was noticed with increasing strain. The samples deformed 43% and 64% and annealed at 1080ºC showed a fully recrystallized microstructure after 3 min of annealing, forming a \"bamboo\" like structure. After 1-min annealing, by using grain orientation spread (GOS) analyzes, it was possible to observe the occurrence of primary recrystallization in ferrite (42% of recrystallized grains) in the 43% cold-rolled sample. On the other hand, austenite kept a slightly recovered microstructure. With a strain of 64%, the recrystallized fraction of ferrite did not change significantly, whereas austenite presented a recrystallized fraction of 45%. KAM analyzes showed a higher stored energy difference in austenite than in ferrite between the 43% and 64% rolled samples. Nevertheless, after annealing, a considerable increase in the fraction of special boundaries (CSL) ?3, ?13b and ?29a (between 11% and 12% in total) was observed in ferrite, while in austenite only an increase in the ?3 boundaries (about 15%), associated with the twin coherent boundaries, was identified.

L’objectif de cette étude est de quantifier la contribution intra et intergranulaire lors d’une sollicitation à haute température d’un alliage de magnésium (AZ31). Afin de répondre à cette problématique scientifique, un essai de traction in situ à haute température dans un MEB a été mis en place. Un important travail de développement a été réalisé autour de cet essai afin de lever un nombre de verrous technique conséquent. Ces verrous expliquent en partie pourquoi il existe aujourd’hui peu d’étude in situ à haute température sur des alliages de magnésium. Un marqueur local ayant la forme d’une microgrille a été déposé sur notre échantillon étant donné que celui-ci n’offre aucun contraste local pour la corrélation d’image numérique (CIN). Afin le dépôt du marqueur local, une cartographie EBSD a été réalisée. À l’aide des joints de grains issus de la carte EBSD, on peut venir superposer les joints de grains aux champs de déformation issue de la CIN.À l’aide des essais de traction in situ à haute température, on a pu mettre en avant l’effet de la température sur les différents mécanismes de déformation actif. Tout ce travail de développement nous permet ainsi de pouvoir localiser les hétérogénéités de déformation plastique à la fois en fonction de l’évolution de la déformation et pour plusieurs températures. D’après les essais menés, on a pu mettre en évidence le fait que plus la température est élevée, que plus les hétérogénéités de déformation plastique se localisent au voisinage des joints de grains. Basé sur une hypothèse cœur/manteau, on a pu venir quantifier la contribution intergranulaire, et mettre en avant que celle-ci devenait plus importante avec la température. / The aim of this study is to quantify the intra and intergranular contribution of the deformation during a high temperature micromechanical test on a magnesium alloy (AZ31). In order to answer this scientific issue, we have developed an in situ tensile test at high temperature within a SEM. It has required a significant preparation work in order to push the current technical limits of this type of test on magnesium alloy. These technical limits can partly explain why there are currently few in situ studies at high temperature on magnesium alloys. A local marker in the form of a microgrid was placed on our sample as it does not provide any local contrast for digital image correlation (DIC). Before the deposition of the microgrid, EBSD mapping was made. Using the grain boundaries from the EBSD, we can superimpose the deformed grain boundaries on the strain map from the DIC.Using high temperature in-situ tensile tests, we were able to highlight the effect of the temperature on the different active deformation mechanisms. This whole development work enables us to locate the plastic deformation heterogeneities both according to the evolution of the deformation and for several temperatures. From the tests conducted, it has been shown that the higher the temperature, the more heterogeneous the plastic deformation heterogeneities are located in the vicinity of the grain boundaries. Based on a heart/coat hypothesis, we were able to quantify the intra and intergranular contribution, and show that it became more important with temperature.

Gamma-TiAl is an ordered intermetallic compound characterized by high strength to density ratio, good oxidation resistance, and good creep properties at elevated temperatures. However, it is intrinsically brittle at room temperature. This thesis investigates the potential for the use of grinding to process TiAl into useful shapes. Grinding is far from completely understood, and many aspects of the individual mechanical interactions of the abrasive grit with the material and their effect on surface integrity are unknown. The development of new synthetic diamond superabrasives in which shape and size can be controlled raises the question of the influence of those variables on the surface integrity. The goal of this work is to better understand the fundamentals of the abrasive grit/material interaction in grinding operations. Experimental, analytical, and numerical work was done to characterize and predict the resultant deformation and surface integrity on ground lamellar gamma-TiAl. Grinding tests were carried out, by analyzing the effects of grit size and shape, workpiece speed, wheel depth of cut, and wear on the subsurface plastic deformation depth (PDD). A practical method to assess the PDD is introduced based on the measurement of the lateral material flow by 3D non-contact surface profilometry. This method combines the quantitative capabilities of the microhardness measurement with the sensitivity of Nomarski microscopy. The scope and limitations of this technique are analyzed. Mechanical properties were obtained by quasi-static and split Hopkinson bar compression tests. Residual stress plots were obtained by x-ray, and surface roughness and cracking were evaluated. The abrasive grit/material interaction was accounted by modeling the force per abrasive grit for different grinding conditions, and studying its correlation to the PDD. Numerical models of this interaction were used to analyze boundary conditions, and abrasive size effects on the PDD. An explicit 2D triple planar slip crystal plasticity model of single point scratching was used to analyze the effects of lamellae orientation, material anisotropy, and grain boundaries on the deformation.

The aim of this thesis work is to design and manufacture a Dissimilar Channel Angular Pressing (DCAP) system for severe plastic deformation of aluminum alloy sheets in order to obtain ultra-fine grained structure. First, a DCAP system was designed by Finite Element Analysis and constructed after various optimization trials. Next, 6061-T0 aluminum alloy plates were severely deformed by various DCAP passes through the system. The samples were characterized by metallography, X-ray diffraction, tension and hardness tests. It has been observed that the yield strength was improved about 100 % after 2 DCAP passes, and 45 nm sub-grain size was obtained.

A study was carried out on the selection of processing condition that would yield Mg-Ti with most favourable hydrogenation properties. Processing routes under consideration were / mechanical milling under inert atmosphere, reactive milling i.e. milling under hydrogen atmosphere, ECAP (equal channel angular pressing) and thermal plasma synthesis. Structure resulting from each of these processing routes was characterized with respect to size reduction, coherently diffracting volume and the distribution of Ti catalyst. Mechanical milling yielded a particulate structure made up of large Mg agglomerates with embedded Ti fragments with a uniform distribution. Mg agglomerates have sizes larger than 100 &micro / m which arises as a result of a balance between cold welding process and ductile fracture. Repeated folding of Mg particles entraps Ti fragments inside the Mg agglomerates resulting in a very uniform distribution. Coherently diffracting volumes measured by X-ray Rietveld analysis have small sizes ca. 26 nm which implies that the agglomerates typically comprise 1011 crystallites. Mechanical milling under hydrogen, i.e. reactive milling, led to drastic reduction in particle size. Mg and Ti convert to MgH2 and TiH2 which are milled efficiently due to their brittleness resulting in particle sizes of sub-micron range. Hydrogenation experiments carried out on Mg-10 vol % Ti milled under argon yields enthalpy and entropy values of -76.74 kJ/mol-H2 and -138.64 J/K.mol-H2 for absorption and 66.54 kJ/mol H2 and 120.12 J/K.mol H2 for desorption, respectively. For 1 bar of hydrogen pressure, this corresponds to a hydrogen release temperature of 280 &deg / C. This value is not far off the lowest desorption temperature reported for powder processed Mg based alloys. ECAP processing is a bulk process where the powders, consolidated in the first pass, have limited contact with atmosphere. This process which can be repeated many times lead to structural evolution similar to that of milling, but for efficient mixing of phases it was necessary to employ multi-pass deformation. An advantage of ECAP deformation is strain hardening of the consolidated powders which has improved milling ability. Based on this, a new route was proposed for the processing of ductile hydrogen storage alloys. This involves several passes of ECAP deformation carried out in open atmosphere and a final milling operation of short duration under inert atmosphere. The plasma processing yields Mg particles of extremely small size. Evaporation of Mg-Ti powder mixture and the subsequent condensation process yield Mg particles which are less than 100 nm. Ti particles, under the current experimental condition used, have irregular size distribution but some could be quite small, i.e. in the order of a few tens of nanometers. Of the four processing routes, it was concluded that both reactive milling and thermal plasma processing are well suited for the production of hydrogen storage alloys. Reactive milling yield particles in submicron range and plasma processing seems to be capable of yielding nanosize Mg particles which, potentially, could be decorated with even smaller Ti particles.

Rapid development and stiff competition in material related industries such as the automotive, demand very high precision in end products in very quick time. The transformation of raw material into an intricate-shaped final product involves various intermediate steps like design, material selection, manufacturing processes, etc. In all these steps, an in-depth understanding of material behavior plays an important role. The available traditional methods such as trial-and-error, especially in the case of die design, become highly inefficient in terms of time and money. This, there is a growing interest in simulation of the final product in order to predict different parameters which are important in design and manufacturing. Currently available simulation techniques are based on existing theories of plasticity or large deformation. These theories have been developed over several decades and many theoretical and practical issues have been debated over the years. Though the theories have great utility in understanding and solving some practical problems, there are ranges of applications for which no acceptable models are available. Most of these theories are either materials or process-specific with oversimplified real physical situations using assumptions and empirical relations. Development of field equations from first principles to stimulate elasto-plastic deformation is one such, still a subject of on-going discussion. Materials and composites exhibit hysteresis even at very low stresses, i.e., inelasticity is always present under all types of loading. This observation shows that the representing constitutive relation cannot treat the elastic and plastic deformations separately. The deformation is due to changes in size and shape, and studies with varying strain rates show considerable material sensitivity to the rate of deformation. Therefore, a generalized field equation is developed from first principles in the Eulerian coordinate system using material resistance to changes in size and shape, and their rates. The formulation uses a unified approach representing continuous effect of elastic and plastic strains and strain rates. The field equation involves eight material parameters, viz. bulk modulus, shear modulus, material shear velocity, material bulk viscosity, and four more constants associated with activation points related to deviatoric and volumetric strains and plastic strain rates. The elastic moduli, bulk and shear, are constants, and so also the material viscosities, while plastic stain rates are functions of elastic strain rates. The field equation redces to Cauchy’s equation in the solid limit and Navier-Stokes equation in the fluid limit. Simple experimental measurements are suggested to obtain the numerical values of the material parameters. Uniaxial tension tests are carried out on commercially available mild steel and aluminium alloy at different strain rates to quantify any variations in the values of material parameters during large deformation. Experimental results and the classical understanding of material deformation reveal the constant nature of elastic moduli during large deformation and, from fluids, the viscosities seem to remain constant. Around the yield region, materials experience a sharp increase in absorbed energy which is modeled to represent the plastic strain rates. The variations and contributions from elastic and plastic strains, both volumetric and deviatoric, and the corresponding stresses are observed. The effects of strain rate on plastic stress and energy absorbed are investigated. The model is checked for different materials and loading conditions to ascertain the proposed changes to earlier theories. Available experimental data in the literature are used for this purpose. The analysis shows that, though the overall stress-strain relations of different materials look similar, their internal responses differ. The internal response of a material depends on various microstructural factors, like alloying elements, impurities, etc. The present model is able to capture those internal differences between various materials. Numerical solution of different plasticity problems have to be undertaken to ascertain the applicability, generality, realism, accuracy and feasibility of the model.