Title: Investigation of titanium alloys using neutron diffraction Author: Gergely Németh Department / Institute: Department of Physics of Materials Supervisor of the master thesis: prof. RNDr. Kristián Mathis, Ph.D., DrSc., Department of Physics of Materials Abstract: Titanium grade 2 was treated by multiple passes of the continuous equal- channel angular pressing technique (CONFORM ECAP) and, after each pass, additionally by rotary swaging. The residual strain field in samples processed by only CONFORM ECAP was studied by neutron diffraction strain scanning. In order to elucidate the microscopic background and calculate the related residual stress field, the local microstructure was thoroughly investigated by various experimental techniques. The microstructure and the deformation behavior of the rotary swaged samples was studied by transmission electron microscopy and by in-situ neutron diffraction during compression. The results of the analyses indicated that microstructural gradients were present in the material as the result of the inhomogeneous deformation during the CONFORM ECAP treatment. These gradients were identified as the main reason of the presence of residual stress fields. The distributions of stress fields calculated based on microstructural parameters were in correlation with simulation...

Объектом исследования являются медь и малолегированные бронзы, подвергнутые интенсивной пластической деформации. Целью работы было определение текущего состояния научных исследований по использованию меди и малолегированных бронз. А также предложить состав и исследовать структуру и свойства бронзы выбранного состава после интенсивной пластической деформации методом динамического канально-углового прессования. В процессе работы проводился анализ литературных источников. В результате исследования было установлено текущее состояние по проблематике работы и определен вектор исследований. Методами оптической металлографии, дюрометрического анализа, просвечивающей электронной микроскопии и сканирующей электронной микроскопии с применением дисперсионно-энергетического анализа и анализа на основе обратного рассеяния электронов было проведено исследование сплава Cu-0,8 вес.% Hf. При различных обработках методом динамического канально-углового прессования. Эксперимент включал различное состояние бронзы перед деформированием. Также было проведено исследование термической стабильности полученных методом динамического канально-углового прессования образцов. Было установлено, что гафниевая бронза после прессования обладает высокими механическими характеристиками и ультрамелкодисперсной структурой. При этом полученная структура стабильна при комнатной температуре и при последующем отжиге вплоть до 400 °С. Что позволяет рекомендовать данный материал как основу для широкого спектра электротехнических изделий. / The object of research is copper and low-alloy bronzes after severe plastic deformation. The purpose of this work was to review scientific research on the use of copper and low-alloy bronzes. As well as the development of the composition and study of the structure and properties of bronze after severe plastic deformation by the method of dynamic channel-angular pressing had been carried out. Literature analysis was carried out. Methods of optical metallography, durometric analysis, transmission electron microscopy and scanning electron microscopy using energy dispersion analysis and analysis based on electron backscattering had been used to study the Cu-0.8 wt.% Hf alloy. Various processings had been carried out by the method of dynamic canal-angular pressing. The state of the bronze before deformation was variouse. We also studied the thermal stability of samples obtained by the method of dynamic channel-angular pressing. It was found that hafnium bronze after pressing has high mechanical characteristics and an ultrafine structure. In this case, the resulting structure is stable at room temperature and upon subsequent annealing up to 400 °C. That allows us to recommend this material as a basis for a wide range of electrical products.

Объект исследования – деформированные в результате интенсивной пластической деформации кручением под высоким давлением образцы на основе платины и алюминия. Цель работы – разработка технологии получения интерметаллида PtAl2 с последующим изучением микроструктуры и механических свойств полученных образцов. Методы исследования – проведение механосинтеза, изучение микроструктуры, измерение микротвердости. Результаты работы – методом кручения под высоким давлением из исходных металлических порошков получены образцы в виде пластин, содержащие интерметаллическую фазу. Образцы были исследованы в сканирующем электронном микроскопе и в рентгеновском дифрактометре. Произведены испытания микротвердости образцов. Рентгенофазовый анализ, показал наличие интерметаллида в продеформированных образцах. Новизна исследования состоит в способе получения интерметаллида PtAl2 путем механосинтеза при комнатной температуре (методом кручения под высоким давлением). Область применения – полученные результаты могут быть использованы при создании покрытий на основе интерметаллидов PtAl2 для авиастроения и машиностроения. / Subject of the research are samples based on platinum and aluminum and deformed by using high pressure torsion. The purpose of the work is to develop a technique to produce PtAl2 intermetallic compounds with subsequent study of the microstructure and mechanical properties of the obtained samples. Research methods: carrying out mechanical alloying, studying the microstructure, conducting mechanical hardness tests of samples. As a result of the research samples in the form of plates containing an intermetallic phase were obtained by high pressure torsion the starting metal powders. Samples were examined using a scanning electron microscope and an X-ray diffractometer. The microhardness of the samples was tested. X-ray phase analysis showed the presence of intermetallic in deformed samples. The novelty of the study is to obtain intermetallic using high pressure torsion. Application field: the obtained results can be used to create PtAl22 intermetallic compounds for aircraft and machine building.

Industrial products of high-strength Al-alloys are currently manufactured by thermo-mechanical processes, which are only applicable in the integrated plants requiring high investment cost. Moreover, reduction of the average grain size not less than 10 &mu / m and re-adjustment of process parameters for each alloy type is evaluated as disadvantage. Therefore, recently there have been many research studies for development of alternative manufacturing techniques for aluminum alloys. Research activities have shown that it is possible to improve the strength of Al-alloys remarkably by severe plastic deformation which results in ultra-fine grain size. This study aims to design and manufacture the laboratory scale set-ups for severe plastic deformation of aluminum alloys, and to characterize the severely deformed samples. The stages of the study are summarized below: First, for optimization of die design and investigation of parameters affecting the deformation finite element modeling simulations were performed. The effects of process parameters (die geometry, friction coefficient) and material properties (strain hardening, strain-rate sensitivity) were investigated. Next, Equal Channel Angular Pressing (ECAP) system that can severely deform the rod shaped samples were designed and manufactured. The variations in the microstructure and mechanical properties of 2024 Al-alloy rods deformed by ECAP were investigated. Finally, based on the experience gained, a Dissimilar Channel Angular Pressing (DCAP) system for severe plastic deformation of flat products was designed and manufactured / then, 6061 Al-alloy strips were deformed. By performing hardness and tension tests on the strips that were deformed by various passes, the capability of the DCAP set-up for production of ultra-fine grain sized high-strength aluminum flat samples were investigated.

Title: Physical properties of ultrafine-grained magnesium based alloys prepared by various severe plastic deformation techniques Author: Jitka Stráská Department / Institute: Department of Physics of Materials Supervisor of the doctoral thesis: Doc. RNDr. Miloš Janeček, CSc. Abstract: The objective of the doctoral thesis is the complex investigation of ultrafine-grained magnesium alloy AZ31 prepared by two different severe plastic deformation techniques, in particular the hot extrusion followed by equal-channel angular pressing (EX-ECAP) and high pressure torsion (HPT). These severe plastic deformation methods, and as well as many others, are described in detail in the introductory theoretical section. Experimental results are summarized in the following experimental part of the thesis. Mechanical properties, lattice defect structure and especially microstructure were investigated using various experimental techniques. Thermal stability of ultrafine-grained microstructure of AZ31 after EX-ECAP was investigated and the activation energies for grain growth in different temperature ranges were calculated using kinetic equation for grain growth and Arrhenius equation. Results from the dislocation density measurements proved temperature ranges of the recovery and the following grain growth. Results from the...

La surface des pièces mécaniques est une zone sensible soumise à des conditions de sollicitations particulières, tant mécaniquement (frottement, contrainte maximale) que chimiquement (atmosphère ambiante, corrosion). Ainsi, la ruine des pièces de service est généralement initiée en surface ; les grands secteurs industriels sont donc à la recherche de solutions technologiques permettant une amélioration des propriétés mécaniques globales par une modification des propriétés de surface. De nombreuses techniques ont été développées dans ce but, notamment les traitements de surface mécaniques. Parmi ceux-ci, le grenaillage ultrasonique permet de déformer sévèrement et superficiellement les pièces par de nombreux impacts de billes ayant des trajectoires aléatoires au sein de la chambre de traitement. Le propos de cette étude repose sur l'analyse et la compréhension des microstructures de déformation induites par un traitement de grenaillage ultrasonique, particulièrement sous conditions cryogéniques ; sujet très peu exploré à ce jour voir nouveau concernant i) des métaux susceptibles de subir une transformation martensitique et ii) l'influence d'un tel traitement sur la tenue en fatigue cyclique. Pour ce faire, plusieurs nuances d'aciers inoxydables austénitiques présentant des stabilités différentes vis-à-vis de la transformation de phase ont été traitées à très basses températures et les propriétés obtenues ont été comparées à celles mesurées sur les échantillons traités à température ambiante. Les premières observations ont montré que, suite à un traitement sous condition cryogénique (-130 °C), une baisse de dureté intervient en sous-couche de l'alliage 310S stable, associée à une hausse des propriétés mécaniques sous basse température rendant le matériau plus difficile à écrouir. Ce phénomène est complètement supprimé au sein de l'alliage métastable 304L par une transformation martensitique facilitée, intervenant plus profondément qu'à température ambiante et entrainant une augmentation de la dureté de sous-couche. Deux alliages métastables (304L et 316L) ont donc été sélectionnés afin de détailler l'influence des paramètres de traitement sur le durcissement de sous-couche par une étude paramétrique comprenant l'amplitude de vibration (40 et 60 µm), la durée (3 et 20 min) ainsi que la température de traitement (ambiante, -80 et -130 °C). Il en ressort qu'augmenter l'énergie de traitent par une hausse de l'amplitude et/ou de la durée de grenaillage entraine une augmentation des duretés de surface et de sous-couche, accompagnée par la production de couches durcies plus épaisses. L'utilisation de températures cryogéniques permet une augmentation du potentiel de durcissement, et ce principalement en sous-couche. En associant les gradients de dureté aux distributions de martensite le long des épaisseurs affectées, il a été montré que la fraction de martensite était directement liée au potentielle de durcissement en profondeur. La fraction de martensite produite étant dépendante de la température de déformation et, afin de prendre en compte la stabilité initiale de l'alliage comme paramètre additionnel, des mesures complémentaires ont été faites sur l'alliage 316L plus stable. Les résultats ont alors montré qu'il est primordial d'adapter la température de traitement à la stabilité de l'échantillon afin d'optimiser l'efficacité du durcissement de sous-couche et éviter ainsi une baisse de la dureté en profondeur. Finalement, les structures de déformation obtenues sous condition cryogénique ont été reliées à la tenue mécanique sous sollicitations cycliques en flexion rotative. Comparé à un traitement réalisé à température ambiante, un grenaillage cryogénique permet une baisse la rugosité de surface et la production de contraintes résiduelles de compression plus élevées par la présence de martensite. Cependant, une plus grande relaxation de ces dernières associée à une réduction de l'épaisseur [...] / The surface of mechanical components is a sensitive zone subjected to particular mechanical (friction, maximum stress) and chemical (ambient atmosphere, corrosion) interactions. Hence, the rupture is generally initiated on the surface. In order to increase the global integrity of the working parts, the industrial groups are still seeking technological solutions allowing the modifications of the surface properties. Nodaway, plenty of surface modification techniques have been developed like the mechanical surface treatments. Among them, the ultrasonic shot peening (or surface mechanical attrition treatment) focus on superficially deform the mechanical parts through numerous collisions of peening medias having random trajectories inside a confined chamber. The purpose of this study is based on the analysis and the comprehension of the deformed microstructures induced by the ultrasonic shot peening treatment, especially under cryogenic temperatures. To do so, several austenitic stainless steel grades having different stabilities regarding the martensitic transformation have been treated under cryogenic conditions and compared to the properties obtained under room temperature. The first observations have shown that, after a cryogenic peening, a decrease of the subsurface hardness takes place in the stable 310S alloy which was attributed to an increase of the mechanical properties under cryogenic temperature. This phenomenon is suppressed in the metastable 304L by triggering a martensitic phase transformation promoted under low temperature and happening deeper compared to room temperature, increasing substantially the subsurface hardness. Two metastable alloys (304L and 316L) were then selected to conduct an ultrasonic shot peening parametric study including the vibration amplitude (40 and 60 µm), the treatment duration (3 and 20 min) and temperature (room temperature, -80 and -130 °C). It has been shown that increasing the treatment energy by raising the vibration amplitude and/or the duration leads to an increase of the surface and subsurface hardnesses as well as the affected layer thickness. The use of cryogenic temperatures allows an additional increase of the hardness, especially in subsurface. By comparing the different hardness gradients with the martensite distributions along the hardened layers, a direct correlation with the hardening rate and the martensite fraction was observed. The initial stability of the treated material was also taken in account by carried out additional observations on the 316L having a higher stability. The results have indicated that the deformation temperature needs to be wisely chosen regarding the stability of the processed material in order to avoid a decrease of the subsurface hardness. Finally, the deformed microstructures generated under cryogenic ultrasonic shot peening were associated to the mechanical behaviors of cylindrical specimens using rotating bending fatigue tests. Compared to a room temperature treatment, a cryogenic peening allows a decrease of the surface roughness and the generation of higher surface compressive residual stresses by the formation of martensite. However, compared to a room temperature treatment, the fatigue behavior was not increased after a cryogenic peening because of a more pronounced surface residual stress relaxation and a reduction of the affected layer. However, the potential increase of the fatigue life after a cryogenic surface deformation was depicted by the study of the rupture surfaces. It was observed that, if the involvement of the surface defects introduced by the high surface roughness can be lowered, a single subsurface crack initiation can be produced increasing considerably the fatigue behavior of the processed material

L'hyperdéformation est une technique efficace pour transformer la microstructure des métaux en une structure de grain de taille inférieure au micron ou même en nanostructure (<100 nm). Cette très petite taille de grain confère d'excellentes propriétés mécaniques au matériau. Dans ce travail de thèse, deux techniques d'hyperdéformation récemment développées, appelées High Pressure Tube Twisting (HPTT) and Cyclic Expansion and Extrusion (CEE) ont été appliquées à température ambiante sur différents matériaux métalliques. La fragmentation de la microstructure ainsi que le développement de la texture cristallographique ont été analysés en détails par la diffraction d'électrons rétrodiffusés (EBSD), par microscopie électronique en transmission (TEM), par transmission Kikuchi diffraction (TKD) ainsi que par diffraction des rayons X (XRD). Le gradient de déformation de cisaillement dans l'épaisseur des tubes d'aluminium déformés par HPTT a été déterminé par une méthode de mesure locale du cisaillement. Ce gradient de cisaillement induit une hétérogénéité aussi bien de microstructure que de texture dans les échantillons d'aluminium et de magnésium purs ainsi que dans l'alliage Al-4%Mg en solution solide. La micro-dureté et la taille de grain dans différentes zones ont été mesurées et analysées en fonction du taux cisaillement local. Les tailles de grain limites atteintes de façon stationnaire pour ces différents matériaux produit par HPTT sont respectivement de 700 nm, 900 nm et 100 nm. L'évolution de texture du magnésium pur après HPTT jusqu'à un cisaillement de 16 a été simulée par cisaillement simple par le model auto-cohérent (VPSC), le résultat de simulation a montré de bons accords avec les mesures de texture obtenues par XRD. Sur la base des mesures de distribution de désorientation dans l'aluminium déformé par HPTT, une nouvelle technique de détermination du taux de cisaillement local dans les procédés d'hyper déformation a été proposée. Cette nouvelle technique a été appliquée sur deux échantillons d'aluminium produit par twist extrusion (TE) et par torsion à extrémités libres. Les échantillons d'aluminium et de cuivre ont été déformés intensément par CEE. Les évolutions de texture et de microstructures ont été mesurées par EBSD, montrant un gradient du centre à la périphérie des échantillons cylindriques. L'évolution de texture dans le cuivre déformé par CEE a été simulée par le modèle VPSC en utilisant un modèle de ligne de courant pour décrire la déformation dans le procédé. Les résultats de simulation confirment les caractéristiques de la texture expérimentale observées après CEE. Le comportement en traction du cuivre pré-déformé par grande déformation en torsion a ensuite été testé. En dépit du gradient de cisaillement existant dans la barre, une technique a été proposée pour obtenir la courbe contrainte-déformation pour ce type de matériau. / Severe plastic deformation (SPD) is an efficient technique to transform the microstructure of bulk metals into ultra fine grained structure with grain sizes less than 1 µm or even into nanostructure with nano-grains of less than 100 nm in diameter. The very small grain size attributes excellent mechanical properties to the material. In present thesis work, two recently developed SPD techniques, namely, High Pressure Tube Twisting (HPTT) and Cyclic Expansion and Extrusion (CEE) were performed on different metallic materials at room temperature. Details of fragmentation of microstructure and metallographic texture evolution were investigated by electron backscattered diffraction (EBSD), transmission electron microscopy (TEM), transmission kikuchi diffraction (TKD) and X-ray diffraction (XRD). Shear strain gradient across the thickness of the HPTT deformed Al tube sample was found by a local shear measurement method. This shear strain gradient induced the inhomogeneity of microstructure and texture in HPTT deformed pure Al, solid solution alloy Al-4%Mg and pure Mg. The microhardness and average grain size in different zones as a function of shear strain were measured. The limiting steady grain sizes in the steady state for these different materials produced by HPTT were 700 nm, 100 nm and 900 nm, respectively. The texture evolution of pure Mg in HPTT up to a shear strain of 16 was simulated in simple shear using the self-consistent (VPSC) polycrystal model and showed good agreements with the experimental results measured by XRD. Based on the measured disorientation distribution function in HPTT deformed Al, a new technique for the magnitude of local shear strain in SPD was proposed. This new technique was applied to a protrusion produced in twist extrusion (TE) and to an Al sample deformed in free-end torsion. Cu and pure Al samples were intensively deformed by the CEE SPD technique. The microstructure and texture evolutions were measured by EBSD, showing a gradient from the center-zone to the edge part of the rod sample. The texture evolution of CEE deformed Cu was simulated by the VPSC polycrystal model using a flow line function. The simulation results confirmed the experimental texture features observed in the CEE process. The tensile testing behavior of large strain torsion pre-processed Cu was examined. In spite of the shear strain gradient existing in the bar, a technique was proposed to obtain the tensile stress-strain curve of such gradient material.

No description available.

<p>Structural metallic materials exposed to energetic particle bombardments often experience various types of irradiation-induced microstructural damage, thus degrading the mechanical properties of the materials in form of irradiation hardening and embrittlement. Nanostructured materials have shown better radiation resistance than their coarse-grained (CG) counterparts due to the existence of abundant defect sinks, such as grain boundaries, twin boundaries, and phase boundaries. However, recently developed nanocrystalline (NC) steels show limited room-temperature tensile ductility (< 1%), which may become a concern for their future application for nuclear reactors. The focus of this thesis is to explore the strength-ductility dilemma in modified 9Cr1Mo (T91) ferritic/martensitic (F/M) steel processed by thermomechanical treatment (TMT) and surface severe plastic deformation (SSPD) with an attempt to fabricate strong, ductile and radiation resistant F/M steels. </p> <p><b>Carbon partitioning</b> between the quenched martensite and the other phases (bainitic ferrite or retained austenite) is critical for enhancing the strength and ductility of T91 steel. The tensile properties of partially tempered (PT) T91 steel can be tailored through introducing bainitic ferrite with high-density nanoscale transition carbides and refined lath martensite. In addition, retained austenite was introduced by increasing the carbon concentration of T91 steel to 0.6 wt.%. The carbon-modified steel processed by quenching partitioning (Q-P) treatment exhibits an ultrahigh strength, ~ 2 GPa, with a uniform strain of ~ 5% due to the existence of coherent carbides, ultrafine martensite and retained austenite. </p> <p>Meanwhile, surface mechanical grinding treatment (SMGT) on T91 steel reveals that introducing <b>gradient structures</b> on the sample surface contributes to a higher strength and an improved plasticity than its homogeneously structured counterpart. The deformation mechanism of the gradient structures was investigated with the assistance of quasi <i>in situ</i> crystal orientation analyses. Furthermore, <i>ex situ</i> He ion irradiation on the gradient T91 steel indicates that radiation-induced damage, such as bubble-induced swelling and irradiation hardening, were gradually mitigated by grain refinement from the sample surface to the center, resulting in superior radiation resistance. The results obtained from this thesis may facilitate the design and fabrication of strong, ductile and radiation-tolerant F/M steels.</p>

Les effets du pressage à canaux égaux (ECAP), un procédé de déformation plastique sévère, ont été examinés dans un alliage Al-2.5Cu-1.5Mg (pourcentage en masse) prône à être durci par traitement thermique et précipitant dans la région α + S. Une multitude de techniques microscopiques, calorimétriques et analytiques ont été utilisés pour caractériser et quantifier les microstructures, incluant la diffraction Kikuchi, la microscopie électronique en transmission, la calorimétrie différentielle à balayage et la sonde atomique tomographique. Quatre différents traitements thermiques initiaux ont été réalisés pour créer quatre microstructures différentes, contenant soit aucun précipités, des clusters Cu-Mg ou/et des composés intermétalliques Al2CuMg. Chaque spécimen a été soumis au procédé ECAP à température ambiante et les effets correspondants sur la microstructure et les propriétés mécaniques ont été analysés. Des expériences en compression pour de petite déformation (inférieures à 7%) ont aussi été entreprises sur les échantillons trempés pour étudier les effets de la compression sur la formation des clusters. Après la trempe et la compression, des clusters Cu-Mg ont été trouvés dans la matrice et il a été élucidé que la formation des clusters était déclenchée par la compression. La fraction volumique des clusters est corrélée directement par la déformation appliquée : plus la déformation est importante, plus la fraction volumique des clusters est importante. Après ECAP, la microstructure est constituée de longues bandes nanocristallines séparée par de gros grains non-déformés pour les échantillons contenant seulement des clusters avant la déformation, tandis que la présence de phase S, avant ECAP, conduit à des microstructures constituées de zones à gros grains et de zones à grains raffinés, distribués d’une façon homogène à travers les échantillons. Bien que les spécimens présentaient clairement des microstructures différentes après ECAP, impliquant que différents mécanismes de renforcement entre en jeux, la limite élastique se situait au-delà de 500 MPa. La limite élastique des échantillons fabriqués par ECAP a été modélisée en superposant les différents mécanismes de renforcement et en saisissant les paramètres microstructurels venant de la caractérisation dans le modèle. Il a été démontré qu’une très bonne corrélation existait entre les limites élastiques provenant du modèle et celles expérimentales. / The effects of equal channel angular pressing (ECAP), a severe plastic deformation (SPD) technique, were investigated in an age hardenable Al-2.5Cu-1.5Mg (weight percent (wt.%)) alloy precipitating in the α + S phase field. A variety of microscopy, calorimetry and analytical techniques were employed to characterize and quantify the microstructure, including transmission kikuchi diffraction (TKD), transmission electron microscopy (TEM), differential scanning calorimetry (DSC) and atom probe tomography (APT). Four different initial heat-treatments were conducted to achieve four different microstructures, containing either no precipitates, Cu-Mg clusters or/and Al2CuMg intermetallics. Each specimen was subjected to ECAP at room temperature and the related effects on the microstructure and mechanical properties were analysed. Compression experiments for small strains (less than 7%) were also undertaken on the as-quenched samples to investigate the effects of compression on the formation of clusters.After quenching and compression, Cu-Mg clusters were found in the matrix and it was elucidated that the formation of clusters was triggered by pressing. The volume fraction of clusters was found to be correlated to the strain applied: the higher the strain, the higher the volume fraction.After ECAP, the microstructure was constituted of long nanocrystalline bands separated by large undeformed grains for the samples containing only clusters before deformation, while the presence of S phase, prior to ECAP, lead to microstructures constituted of both coarse and refined zones distributed homogeneously throughout the sample. Although the samples presented clearly different microstructures after ECAP, implying that different strengthening mechanisms were active, the yield strength was found to lie above 500 MPa. The yield strength of the ECAP processed samples was modelled by superposing the different strengthening mechanisms altogether and by inputting the microstructural parameters coming from characterisation in the model. It was demonstrated that a very good correlation existed between the modelled and experimental yield strength values.