Title: Phase transformations in ultra-fine grained titanium alloys Author: Kristína Bartha Department: Department of Physics of Materials Supervisor of the doctoral thesis: PhDr. RNDr. Josef Stráský, Ph.D., Department of Physics of Materials Abstract: Ti15Mo alloy in a metastable β solution treated condition was processed by high pressure torsion (HPT) and equal channel angular pressing (ECAP). The microstructure after HPT is severely deformed and ultra-fine grained, while ECAP deformation results in rather coarse-grained structure with shear bands containing high density of lattice defects. Two types of thermal treatments - isothermal annealing and linear heating - were carried out for the solution treated condition and both deformed materials. Wide spectrum of experimental techniques was employed to elucidate the differences in phase transformations, especially in α phase precipitation, occurring in deformed and non-deformed material upon thermal treatment. It was shown that the α phase precipitation is accelerated in the deformed materials due to a high density of lattice defects, which provide a dense net of preferred sites for nucleation and also fast diffusion paths necessary for accelerated growth. The enhanced precipitation of the α phase in deformed materials also affects the stability of the ω...

To test nanosize surface patterning for application as implant material, a suitable titanium composition has to be found first. Therefore we investigated the effect of surface chemistry on attachment and differentiation of osteoblast-like cells on pure titanium prepared by pulsed laser deposition (TiPLD) and different Ti alloys (Ti6Al4V, TiNb30 and TiNb13Zr13). Early attachment (30 min) and alkaline phosphatase (ALP) activity (day 5) was found to be fastest and highest, respectively, in cells grown on TiPLD and Ti6Al4V. Osteoblasts seeded on TiPLD produced most osteopontin (day 10), whereas expression of this extracellular matrix protein was an order of magnitude lower on the TiNb30 surface. In contrast, expression of the corresponding receptor, CD44, was not influenced by surface chemistry. Thus, TiPLD was used for further experiments to explore the influence of surface nanostructures on osteoblast adhesion, differentiation and orientation. By laser-induced oxidation, we produced patterns of parallel Ti oxide lines with different widths (0.2–10 μm) and distances (2–20 and 1,000 μm), but a common height of only 12 nm. These structures did not influence ALP activity (days 5–9), but had a positive effect on cell alignment. Two days after plating, the majority of the focal contacts were placed on the oxide lines. The portion of larger focal adhesions bridging two lines was inversely related to the line distance (2–20 μm). In contrast, the portion of aligned cells did not depend on the line distance. On average, 43% of the cells orientated parallel towards the lines, whereas 34% orientated vertically. In the control pattern (1,000 μm line distance), cell distribution was completely at random. Because a significant surplus of the cells preferred a parallel alignment, the nanosize difference in height between Ti surface and oxide lines may be sufficient to orientate the cells by contact guiding. However, gradients in electrostatic potential and surface charge density at the Ti/Ti oxide interface may additionally influence focal contact formation and cell guidance. / Dieser Beitrag ist mit Zustimmung des Rechteinhabers aufgrund einer (DFG-geförderten) Allianz- bzw. Nationallizenz frei zugänglich.

L’objet de cette étude est la tenue en fatigue de la tige coulissante d’une jambe de train d’atterrissage fabriquée par SAFRAN Landing Systems. L’alliage utilisé pour réaliser cette pièce forgée est la nuance de titane haute performance Ti-5Al-5V-5Mo-3Cr (Ti5553). Pour assurer les meilleures caractéristiques en service, ces pièces subissent différents traitements mécaniques dont un grenaillage qui améliore la tenue mécaniques du matériau en proche surface. L’homogénéité du grenaillage dépend de la géométrie de la pièce. La connaissance des contraintes résiduelles résultant de ce traitement est un paramètre important qui influence la durée de vie en fatigue. La microstructure biphasée du matériau rend les estimations de contraintes difficiles sur ce matériau. Un protocole complet d’analyse de contraintes par diffraction des rayons-X a été mis en place et validé par test in-situ. Il a ensuite permis d’obtenir des estimations quantitatives de contraintes résiduelles sur les éprouvettes testées dans ce travail. L’alliage Ti5553 a la particularité de présenter une très haute limite élastique pour une tenacité plus faible. Les pièces actuelles sont dimensionnées par leur résistance à l’amorçage sans défaut de surface. Pour exploiter au mieux les performances de cet alliage, il faut affiner la connaissance du processus d’amorçage en présence de défauts. Plusieurs types d’analyses et essais ont été réalisés (comportement élasto-plastique, étude de l’amorçage et de la propagation de fissure). En particulier, des essais sont effectués sur des éprouvettes présentant des faces et des coins avec des rayures usinées ou des indentations. L’influence de ces défauts sur la durée de vie en fatigue est analysée en fonction de leur type, de leur taille et du grenaillage. / The prediction of the fatigue life of sliders made by SAFRAN Landing Systems is the goal of this work. To manufacture big forged parts, high performance Ti-5Al-5V-5Mo-3Cr (Ti5553) alloy is used.To ensure the in-service life, various mechanical treatments are carried out. Shot-peening at the end of the process is of prime importance in order to improve the mechanical performance. The knowledge of residual stresses resulting from this treatment is necessary to understand fatigue results for all part location. The two-phase microstructure of the alloy makes stress analyses difficult. A complete protocol to analyse stresses by X-ray diffraction has been developed and validated through in-situ test. The Ti5553 alloy exhibits high yield stress coupled with weaker toughness. Lifing of parts made of Ti5553 is currently carried out with no specific account of surface defects. To improve the knowledge of initiation processes in this alloy in the presence of defects, various tests have been carried out (elasto-plastic behavior, crack initiation and propagation studies). Tests are carried out on coupons with faces and edges with calibrated defects (i.e., machined scratches and indents). The influence of such defects on the fatigue lifetime are studied in terms of type, size and shot-peening level.

No description available.

This is predominantly a qualitative study on the manufacturing of micronozzles with an additive manufacturing (AM) technique, namely the laser-powered powder bed fusion (PBF-LB).  Manufacturing of micronozzles with standard microelectromechanical system technology often results in 2.5-D or close to 3-D structures and does not yield a fully rotationally symmetric nozzle. For this reason, AM can be a better solution. However, the structures obtained with PBF-LB exhibit very rough surfaces which will impair the performance of the micronozzle. To improve the surface finish electropolishing was performed on the interior walls.  Given the shape and the scale of the components, uniformity of the polishing is a challenge, calling for an inventive electrode configuration and electrolyte feed solution. The approach was to integrate an electrode on the inside of the converging part of the nozzle, to serve as a cathode for the electropolishing, already in the process, and to make the nozzle itself the vital part of the fluidic system.  With this, titanium micronozzles were manufactured with throat diameters varying between 300 and 800 μm. With the resolution of the used AM technique, it was possible to integrate the internal electrode in the micronozzles with a designed throat diameter down to 600 μm. Below this, the anode, and cathode, sometimes made contact short-circuiting the cell. Profilometry showed a decrease of the average surface roughness (𝑅𝑅𝑎𝑎) with 15-60 % for the electropolished micronozzles. The Schlieren imaging showed an exhaust that followed the throat’s axial direction and also demonstrated pressure disks and, hence, a supersonic jet exhaust. This study has shown that AM is a viable choice for manufacturing of rotationally symmetric micronozzles, and that electropolishing could be used to decrease the surface roughness on their inside uniformly with the integration of a cathode.

O presente trabalho visou determinar a tenacidade à fratura dinâmica, KID, primeiramente pelos conceitos da Mecânica da Fratura Elástica Linear (MFEL) e posteriormente pela Mecânica da Fratura Elasto-Plástica (MFEP), JID, em materiais que em operação podem estar sujeitos a impactos em diferentes temperaturas. Os materiais estudados, de uso na indústria aeronáutica, foram uma liga de titânio Ti6Al4V (norma SAE AMS 4911), na condição recozida e uma liga de aço inoxidável PH 15-5 (norma SAE AMS 5659), na condição H1000. Os corpos de prova pré-trincados e entalhados foram retirados nas orientações L-T e L-S, a fim de que fossem determinadas e comparadas a relação tenacidade/densidade ou tenacidade específica dos materiais estudados. Em seguida os corpos de prova foram ensaiados sob condições de carga dinâmica em uma máquina de ensaio Charpy instrumentado, marca Instron-Wolpert PW30, conforme a norma ASTM-E23, com velocidade de carregamento de 5,52 m/s e nas temperaturas de 23 e 400ºC. Os valores das tenacidades, posteriormente comparados e correlacionados, foram obtidos de acordo com as expressões matemáticas mencionadas na literatura. A razão entre as energias estimadas de iniciação (Ei) e de propagação (Ep), (Ei/Ep), foi obtida a partir dos gráficos de carga-deslocamento x tempo. A determinação e caracterização dos aspectos macro e microscópicos da fratura foram realizadas através de microscopia ótica e de varredura. Em seguida, confrontaram-se os valores e os aspectos preponderantes dos mecanismos de fratura apresentados por cada material. / The present work aimed to evaluate the dynamic fracture toughness, KID, firstly using the Linear Elastic Fracture Mechanics parameter, (LEFM), and secondly using the Elasto-Plastic Fracture Mechanics (EPFM), JID. The materials used in this work are from aeronautic grade and are subjected to in service impact loads and temperature variation. The materials are a titanium alloy Ti6Al4V (standard SAE AMS 4911), in the annealed condition and a PH 15-5 stainless steel (standard SAE AMS 5659), H1000 condition. Both precracked and notched specimens were taken in the L-T and L-S directions, for the evaluation and comparison of the toughness/density ratio, i. e., the specific dynamic fracture toughness of the materials studied. Therefore, the specimens were tested under dynamic load using an Instron-Wolpert PW30 Instrumented Charpy Equipment, following the ASTM-E23 standard, with load speed of 5,52 m/s at 23 and 400ºC. The fracture toughness values were compared using mathematical expression from literature. The ration between the initiation (Ei) and propagation (Ep) energies, (Ei/Ep), was obtained from the load-displacement x time. The characterization of the macro and microscopic aspects of the fracture mechanisms were carried out using optical microscope and scan electronic microscope. The fracture toughness values and the fractographic observations were correlated and compared for the two materials studied.

L’usinage par électroérosion est un procédé d’enlèvement de matière par fusion, vaporisation et érosion, réservé aux matériaux conducteurs et semi-conducteurs.Il peut être utilisé pour usiner les métaux et alliages, les aciers trempés, les alliages céramiques, les carbures métalliques, certaines céramiques et même des matériaux plus durs tels que le diamant polycristallin. La pièce ainsi chauffée voit ses caractéristiques mécaniques chuter et modifier, ce qui augmente son usinabilité. Les travaux réalisés ont porté sur l'influence de l'usinage par électroérosion à fil sur; l'intégrité de surface, l'usinabilité, la productivité et la précision de procédé, de plusieurs matériaux, tels que, le titane pur, l'alliage de titane Ti-6Al-4V, le composite intermétallique à base Ti-Al, le composite Ti17 et le composite Ti6242.En usinage par électro-érosion à fil, et plus précisément en finition, le procédé est caractérisé par un débit de matière, une largeur de kerf, un durcissement superficiel, une zone affectée thermiquement et un état de surface variant en fonction de plusieurs paramètres tels que, le courant de décharge, le temps d’impulsion, la tension d’amorçage, la vitesse de coupe, la pression d'injection de lubrifiant et la tension de fil.Toutefois, il s’agit d’une étude d’optimisation et de modélisation empirique des conditions de coupe des matériaux composites à base métallique et des alliages de titane, afin de maitriser et d'améliorer l'intégrité de surface usinée, d'augmenter la productivité et de perfectionner la précision du procédé. Par la suite, atteindre les exigences de la qualité et de la sûreté de fonctionnement des pièces aéronautiques.Dans cette étude, on a utilisé des méthodes de type Plan d'expériences, méthode de Taguchi et la Méthodologie des surfaces de réponses pour le calage et le contrôle des paramètres de l’usinage par électroérosion à fil, et ses conditions opératoires. / EDM machining is a process for the removal of material by melting, spraying and erosion, which is reserved for conductive and semiconductor materials.It can be used for machining metals and alloys, hardened steels, ceramic alloys, metal carbides, some ceramics and even harder materials such as polycrystalline diamond. The heated part has its mechanical characteristics drop, which increases its machinability. The work carried out focused on the influence of WEDM machining on surface integrity, machinability, productivity and process precision, of several materials: pure titanium, Ti6Al4V alloy, composite intermetallicTi-Al based, Ti17 composite and Ti6242 composite.In ripping, and more precisely in finishing, the process is characterized by a flow of material,kerf width, surface hardening, heat affected zone and surface condition varying with discharge current, pulse time and voltage, cutting speed, lubricant injection pressure and wire tension.In fact, the machining conditions of metal-based composite materials and titanium alloys have been modeled and optimized to improve machined surface integrity, increase productivity, and improve process accuracy. Subsequently, meet the quality and safety requirements of aeronautical parts.Methods such as Experimental Design, Taguchi and Surface of Response were used for calibration and process control parameters and operating conditions.

Dans l'industrie aéronautique, les alliages de titane sont utilisés pour leur excellent comportement mécanique associé à une faible masse volumique. Ils sont largement employés sous forme de tôles dont la mise en forme peut se faire par le biais de trois procédés : à température ambiante par opération d'emboutissage, à très hautes températures (T≈900°C) par formage superplastique (SPF) et à des températures intermédiaires (T=730°C, 880°C) par formage à chaud (HF). Le projet repose sur le développement du procédé d'emboutissage à chaud d'une tôle d'alliage de titane Ti-6Al-4V en conditions isothermes à des températures inférieures à 700°C. Par conséquent, la détermination des paramètres procédés et matériaux constitue une étape importante pour la mise en œuvre de simulations numériques et contribue à la réussite des opérations d'emboutissage de pièces industrielles. Ces paramètres procédés sont liés à la vitesse du poinçon, aux efforts de serre-flan et au frottement induit entre le flan et l'outillage. Leur analyse a permis de déterminer deux niveaux de températures (400°C et 500°C) offrant une chute drastique du coût énergétique, en comparaison des procédés HF ou SPF, tout en conservant des niveaux d'allongement suffisants. Les paramètres matériaux influençant le comportement de l'alliage sont analysés et quantifiés. Ils peuvent être influencés par plusieurs mécanismes : élasticité, viscosité, anisotropie (Hill48, Barlat91) et nature de l’écrouissage (isotrope, cinématique). Dans cette étude, un modèle de comportement élasto-viscoplastique anisotrope, capable de considérer les trajets de chargement subis par la tôle lors de sa mise en forme, a été formulé pour les deux niveaux de température. L’implantation du modèle de comportement a été réalisée dans le code de calcul éléments finis Abaqus/Standard 6.14® interfacé avec le logiciel ZMAT®. Elle a permis d’une part des simulations d’emboutissage de profil Omega pour lesquelles des comparaisons avec les expériences ont été réalisées et d’autre part, des calculs sur une pièce de forme complexe. / In the aerospace industry, titanium alloys are used for their excellent mechanical behavior associated with low density. They are widely available in sheet form and the final shape can be obtained through three processes: at room temperature by stamping operation, at very high temperatures (T≈900°C) by superplastic forming (SPF) and at intermediate temperature (T=730°C, 880°C) by hot forming (HF). The project is based on the development of the hot stamping process of Ti-6Al-4V titanium alloy sheet under isothermal conditions at temperatures below than 700°C. Therefore, the determination of the process and material parameters constitutes an important stage for implementing the numerical simulation while contributing to the success of the stamping operation at the scale of an industrial part. The process parameters are related to the punch speed, the blank holder forces and the friction induced between the sheet and the tool. Their analysis allowed to determine two temperature levels (400°C et 500°C) leading a drastic drop in energy cost, compared to HF or SPF processes, while maintaining enough elongation levels. The material parameters influencing the behavior of the alloy are analyzed and quantified. They can be influenced by several mechanisms: elasticity, viscosity, anisotropy (Hill48, Barlat91) and nature of hardening (isotropic, kinematic). In this study, an anisotropic elasto-viscoplastic behavior model, able to consider the loading path undergone by sheet during forming, has been formulated for both temperature levels. The implementation of the behavior model is achieved in Abaqus/Standard 6.14® Finite Element code with the material library plugin ZMAT®. It enables, on the one hand, stamping numerical simulations of a simple shape Omega profile for which experimental comparisons were done, on the other hand, calculations on an industrial part with a complex shape.

Les alliages de titane β-métastables comme le Ti-10V-2Fe-3Al se substituent progressivement aux alliages α/β dans les applications aéronautiques du fait de leur résistance spécifique améliorée. Leurs microstructures d'emploi sont cependant complexes et multi-échelles, constituées d'une matrice β (de grains millimétriques) partiellement transformée en nodules primaires αp (micrométriques) et en lamelles secondaires αs (sub-micrométriques). Les propriétés finales peuvent être très sensibles aux variations locales de microstructures et sont souvent non maîtrisées lors du forgeage de pièces massives. De plus la matrice β qui représente ~40% du volume et qui a un comportement élastique et plastique fortement anisotrope, comme la phase α, complique la compréhension des mécanismes de déformation en jeu. Le premier objectif de cette thèse est de mettre en œuvre des techniques de caractérisation multi-échelles (la diffraction des neutrons, l'imagerie électronique couplée à l'analyse d'image et l'EBSD, la reconstruction des microtextures de haute température β/αp) pour analyser efficacement la microstructure/texture des constituants β/αp/αs et caractériser leurs hétérogénéités au sein de demi-produits et de pièces obtenues par matriçage. Les résultats permettent d'analyser la fragmentation des grains β en sous-grains, les macrozones αp, le maintien de relation d'orientation entre β/αp et l'organisation des lamelles αs en colonies ou paniers tressés, en pointant les différences de taille de domaines révélés par la cristallographie et l'imagerie standard. Le second objectif est d'appliquer cette méthodologie à l'analyse de facies de rupture d'éprouvettes présentant un comportement singulier (en traction ou en fatigue) pour caractériser les configurations microstructurales à l'origine de l'amorçage de fissures. Cette analyse a principalement été réalisée par polissage manuel du faciès couplé à des acquisitions EBSD mais également en exploitant le potentiel de l'imagerie 3D par MEB-FIB (Focus Ion Beam) et la technique TKD (Transmission Kikuchi Diffraction) sur lame mince prélevée au niveau d'un site d'amorçage par FIB. Enfin, cette étude expérimentale a été complétée par une première approche en simulation micromécanique sur une microstructure modèle 100% β. L'objectif était d'évaluer l'influence de l’anisotropie élastique de la phase β sur la genèse de contraintes d'incompatibilités dans les régimes élastique et élasto-plastique. L'ensemble des résultats contribue à une meilleure compréhension des variations de propriétés mécaniques en lien avec la microstructure locale / The β-metastable titanium alloys such as Ti-10V-2Fe-3Al are gradually replacing α/β alloys in aeronautical applications thanks to their improved specific strength. However, their microstructures are complex and multi-scale, consisting of a β matrix (of millimetric grains) partially transformed into primary αp nodules (micrometric) and secondary αs lamellae (sub-micrometric). The final mechanical properties are very sensitive to local variations of the microstructure, which are not always fully controlled during forging of massive parts. Moreover, the β matrix, which represent 40% of the volume and whose elastic and plastic behavior is strongly anisotropic (like the α phase) complicates the understanding of the mechanisms of deformation. The first objective of this thesis was to efficiently characterize the microstructure/texture of the different constituents (β/αp/αs) and their heterogeneities within half-finished products and forged parts by using techniques of multi-scale characterization (neutron diffraction, electronic imaging coupled with image analysis and EBSD, reconstruction of high temperature microtextures β/αp). As a result the fragmentation of the β grains into subgrains, the αp macrozones, the destruction of the orientation relation between β/αp and the organization of the αs lamellae in colonies or basket weave was quantified and the differences in size of domains revealed by crystallography and by standard imaging were pointed out. The second objective is to apply this methodology to the analysis of fracture surfaces of samples exhibiting singular behavior (in tension or in fatigue) in order to characterize the microstructural configurations leading to early cracking. This analysis was mainly performed by manual polishing coupled with EBSD acquisitions but also by using 3D imaging by SEM-FIB (Focus Ion Beam) and TKD (Transmission Kikuchi Diffraction) technique on a thin foil FIB-extracted from the crack initiation site. Finally, this experimental study was completed by a micromechanical simulation on a 100% β model microstructure. The objective was to evaluate the influence of the elastic anisotropy of the β phase on the genesis of incompatibility stresses in the elastic and elasto-plastic regimes. The overall results contribute to a better understanding of the variations of mechanical properties related to the local microstructure

Fretting fatigue is a damage process that may arise in engineering applications where small cyclic relative displacements develop inside contacts leading to detrimental effects on the material fatigue properties. Fretting is located in regions not easily accessible, which makes it a dangerous phenomenon. It is therefore important to be able to make reliable predictions of the fretting fatigue lives. The work presented in this thesis has its focus on different aspects related to fretting fatigue in the titanium alloy Ti-17. A fretting experiment was developed which allowed for separate control of the three main fretting loads. Initially, the evolution of the coefficient of friction inside the slip region was investigated experimentally and analytically. Subsequently, 28 fretting tests were performed in which large fatigue cracks developed. The fretting tests were firstly evaluated with respect to fatigue crack initiation through five multiaxial fatigue criteria. The criteria predicted a too high fretting fatigue limit. A possible clue to the discrepancy was found in the fretting induced surface roughness with the asperity-pit interactions. The fatigue growth of the large fretting cracks was numerically modelled through a parametric crack growth procedure. The predicted lives were compared to the experimental outcome. The numerical simulations showed that linear elastic fracture mechanics was an appropriate tool for the prediction of fretting fatigue propagation lives in the long crack regime. Fatigue cracks spend most of their propagation life in the small crack regime. The possibility of modelling the small crack behaviour is therefore very important from the engineering point of view. The fatigue growth of through thickness short cracks was studied experimentally and numerically in the four-point bend configuration. It was found that linear elastic fracture mechanics and closure-free material growth data furnished conservative estimates for cracks longer than 50 μm. One method to improve fretting fatigue life is to shot peen the contact surfaces. Experimental results on fretting life with or without shot peening were simulated. The fatigue life enhancement in shot peened specimens could be explained by slower crack growth in the surface material layer with residual compressive stresses. / QC 20100827