This doctoral thesis deals with the determination of the influence of plasma electrolytic oxidation (PEO) on fatigue behaviour of extruded AZ61 magnesium alloy in air and in the 3.5% NaCl solution. The coatings were formed in the silicate-phosphate electrolyte under pulsed current conditions at a frequency of 50 Hz. The influence of current density on coating formation was examined under current densities of 70, 130 and 200 mA cm-2 for different durations up to a maximum of 1800 s. 8 g dm-3 of KF were added to the electrolyte to study the influence of fluoride ions in plasma electrolytic oxidation. It is shown that fluoride ions inhibit localised oxidation in the initial stage of the process, associated with the secondary particles based on Al–Mn. The presence of fluoride also modified the sparking characteristics, decreased the rate of coating growth and changed the morphologies of the coatings. The influence of fluoride on the coating hardness, and the corrosion resistance of the alloy during exposure to salt spray, was negligible. Based on previous optimised PEO conditions, coatings formed under a current density of 130 mA cm-2 for 300 s in the electrolyte containing KF were chosen for fatigue testing. The high-cycle fatigue tests were carried out on cylindrical samples under a force controlled sinusoidal tension-tension cycle with asymmetry parameter R=0. The experimental data were fitted with Kohout & Věchet function. The fatigue limit of uncoated alloy in air for 107 cycles was determined at 145.4 MPa and the combination of PEO coating with chloride ions caused a reduction of ~55 %. Attention was paid to the fatigue crack initiation in different conditions of cyclic loading. The fracture surfaces underwent detailed fractography analysis including secondary crack observation on the gauge length. The contribution of Al–Mn particles were confirmed on the uncoated alloy in air and the presence of chloride ions were observed as another influential contributor to local corrosion attack. The cyclic loading caused spalling of the outer layer, and the multiple initiation was observed on PEO coated alloy, caused by cracks in the coating and stress transferring to the alloy.

Ces travaux ont pour objectif l'identification et la compréhension de l'effet de la corrosion aqueuse sur la durée de vie en fatigue à grand nombre de cycles (HCF) d'un acier inoxydable martensitique utilisé dans des applications aéronautiques. Tout d'abord, l'effet géométrique des défauts de corrosion sur la limite de fatigue à 10^7 cycles à l'air a été étudié avec quatre tailles différentes de piqûres de corrosion. A partir de ces résultats, une nouvelle approche volumique non locale de modélisation numérique a été proposée pour prendre en compte une géométrie réelle d'un défaut de corrosion issu des analyses en microtomographie X. Ensuite, les phénomènes de couplage chargement cyclique/corrosion ont été identifiés par des essais de fatigue à grande durée de vie (entre 10^5 et 10^7 cycles) dans une solution aqueuse à 0,1 M NaCl (à pH = 6) pour deux rapports de charge (R = -1 et 0,1). Le comportement électrochimique du film passif a été étudié in situ au cours des essais de fatigue-corrosion par le suivi du potentiel libre de corrosion et des mesures d'impédance électrochimique. Les observations des mécanismes d'amorçage de fissures et des mesures électrochimiques in-situ ont permis d'identifier un scénario d'amorçage de fissures de fatigue. Ce scénario implique des processus de rupture locale du film passif (induite par le chargement cyclique) et de corrosion assistée par le chargement cyclique. Finalement un modèle analytiquede prévision de la durée de vie en fatigue dans un milieu aqueux corrosif a été proposé à partir des résultats expérimentaux. / This study addresses the effects of corrosion on the high cycle fatigue (HCF)strength of a martensitic stainless steel used in aeronautic applications. First, the geometry of corrosion pits on the fatigue strength in air at 10^7 cycles were studied with four different pit sizes. A new non-local fatigue criterion was proposed to simulate real shapes of pits as identified by X-ray microtomography. Corrosion fatigue synergy phenomena was studied by HCF tests (between 10^5 and 10^7 cycles) in a 0.1 M NaCl aqueous solution (pH = 6) with two load ratios (R = -1 and 0.1). Next, the electrochemical behavior of the passive film was investigated during in situ corrosion fatigue tests by free potential measurements and electrochemical impedance spectroscopy (EIS). Based on fractography analysis and electrochemical test results, corrosion fatigue crack initiation mechanisms were investigated. A scenario of fatigue crack initiation was proposed based on physical evidence. This scenario implied combined processes of local passive film rupture (induced by the cyclic loading), stress-assisted corrosion and enhanced pitting development. Local passive film ruptures were the main cause of the corrosion fatigue crack initiation. Finally, a analytical model for corrosion fatigue crack initiation was proposed based.

<p dir="ltr">In structural metallic components, a material’s lifecycle begins with the processing route, to produce a desired structure, which dictates the in-service performance. The variability of microstructural features as a consequence of the processing route has a direct influence on the properties and performance of a material. In order to correlate the influence processing conditions have on material performance, large test matrices are required which tend to be time consuming and expensive. An alternative route to avoid such large test matrices is to incorporate physics-based process modeling and lifing paradigms to better understand the performance of structural materials. By linking microstructural information to the material’s lifecycle, the processing path can be modified without the need to repeat large-scale testing requirements. Additionally, when a materials system is accurately modeled throughout its lifecycle, the performance predictions can be leveraged to improve the design of materials and components.</p><p dir="ltr">Ni-based superalloys are a material class widely used in many critical aerospace components exposed to coupling thermal and mechanical loads due to their increased resistance to creep, corrosion, oxidation, and strength characteristics at elevated temperatures. Many Ni-based superalloys undergo high-temperature forging to produce a desired microstructure, targeting specific strength and fatigue properties in order to perform under thermo-mechanical loads. When in-service, these alloys tend to fail as a consequence of thermo-mechanical fatigue (TMF) from either inclusion- or matrix- driven failure. In order to produce safer, cheaper and more efficient critical aerospace components, the micromechanical deformation and damage mechanisms throughout a Ni-based superalloy’s lifecycle must be understood. This research utilizes process modeling as a tool to understand the damage and deformation of inclusions in a Ni-200 matrix throughout radial forging as a means to optimize the processing conditions for improved fatigue performance. In addition, microstructural sensitive performance modeling for a Ni-based superalloy is leveraged to understand the influence TMF has on damage mechanisms.</p><p dir="ltr">The radial forging processing route requires both high temperatures and large plastic deformation. During this process, non-metallic inclusions (NMIs) can debond from the metallic matrix and break apart, resulting in a linear array of smaller inclusions, known as stringers. The evolution of NMIs into stringers can result in matrix load shedding, localized plasticity, and stress concentrations near the matrix-NMI interface. Due to these factors, stringers can be detrimental to the fatigue life of the final forged component. By performing a finite element model of the forging process with cohesive zones to simulate material debonding, this research contributes to the understanding of processing induced deformation and damage sequences on the onset of stringer formation for Alumina NMIs in a Ni-200 matrix. Through a parametric study, the interactions of forging temperature, strain rate, strain per pass, and interfacial decohesion on the NMI damage evolution metrics are studied, specifically NMI particle separation, rotation, and cavity formation. The parametric study provides a linkage between the various processing conditions parameters influence on detrimental NMI morphology related to material performance.</p><p dir="ltr">The microstructural characteristics of Ni-based superalloys, as a consequence of a particular processing route, creates a variability in TMF performance. The micromechanical failure mechanisms associated with TMF are dependent on various loading parameters, such as temperature, strain range, and strain-temperature phasing. Insights on the complexities of micromechanical TMF damage are studied via a temperature-dependent, dislocation density-based crystal plasticity finite element (CPFE) model with uncertainty quantification. The capabilities of the model’s temperature dependency are examined via direct instantiation and comparison to a high-energy X-ray diffraction microscopy (HEDM) experiment under coupled thermal and mechanical loads. Unique loading states throughout the experiment are investigated with both CPFE predictions and HEDM results to study early indicators of TMF damage mechanisms at the grain scale. The mesoscale validation of the CPFE model to HEDM experimental data provides capabilities for a well-informed TMF performance paradigm under various strain-temperature phase profiles. </p><p dir="ltr">A material’s TMF performance is highly dependent on the temperature-load phase profile as a consequence of path-dependent thermo-mechanical plasticity. To investigate the relationship between microstructural damage and TMF phasing effects, the aforementioned CPFE model investigates in-phase (IP) TMF, out-of-phase (OP) TMF, and iso-thermal (ISO) loading profiles. A microstructural sensitive performance modeling framework with capabilities to isolate phasing (IP, OP, and ISO) effects is presented to locate fatigue damage in a set of statistically equivalent microstructures (SEMs). Location specific plasticity, and grain interactions are studied under the various phasing profiles providing a connection between microstructural material damage and TMF performance.</p>

Pokročilá vysoce legovaná austenitická nerezová ocel Sanicro 25 s Fe-Ni-Cr matricí byla studována za podmínek nízkocyklové únavy za pokojové a vysoké teploty 700 °C. Široká škála moderních experimentálních technik byla použita ke studiu vzájemně souvisejících efektů chemického složení slitiny, mikrostrukturních změn a deformačních mechanismů, které určují odolnost materiálu vůči poškození. Hlavní úsilí bylo zaměřeno na studium iniciace únavových trhlin a růstu krátkých trhlin, tedy dvě stádia, která hrají zásadní roli ve výsledné celkové délce únavového života materiálu v provozu. • Vnitřní deformační mechanismy byly korelovány s vývojem povrchového reliéfu, který je pozorován ve formě persistentních skluzových stop na povrchu. Bylo zjištěno, že vysoce planární charakter dislokačního skluzu způsobuje vysokou lokalizaci cyklické plastické deformace do persistentních skluzových pásů, což v důsledku vede k nukleaci “Stage I” trhlin, která je spojena s přítomností persistentních skluzových stop na povrchu ve všech studovaných vzorcích. Bylo zjištěno, že praskání dvojčatových hraníc je taktéž spojeno s přítomností persistentních skluzových stop podél povrchové stopy dvojčatové roviny. • Interkrystalická iniciace únavové trhliny byla pozorována pouze zřídka, a to za podmínek zatěžování amplitudami vysoké deformace. Bylo zjištěno že interkrystalická iniciace je spojena s přítomností persistentních skluzových stop na hranicích zrn. Hranice zrn praskají za podmínek externího tahového zatížení zejména z důvodu vysokého počtu nekompatibilit na hranicích zrn, které jsou způsobené tvarem persistentních skluzových stop. • Mechanismy růstu přirozených krátkých trhlin byly studovány na vzorcích vystavených nízkocyklove únava s nízkou i vysokou deformací. Role mikrostruktury byla analyzována pomocí experimentálních technik a diskutována. • Rychlosti šíření nejdelších trhlin byly měřeny na vzorcích s mělkým vrubem. Výsledky byly analyzovány použitím přístupů lomové mechaniky založených na amplitudě KI a J-integrálu stejně jako na amplitudě plastické deformace. Všechny přístupy byly diskutovány v souvislosti s Mansonovými-Coffinovými křivkami únavové životnosti. Jednoduchý mocninový zákon růstu krátkých trhlin založený na amplitudě plastické deformace ukazuje velice dobrou korelaci se zákonem únavové životnosti. • Byla studována role oxidace v podmínkách cyklického zatěžování za vysokých teplot. Bylo zjištěno, že křehké praskání zoxidovaných hranic zrn hraje hlavní roli v počátečních stádiích nukleace trhlin. Později po iniciaci se dráha růstu trhliny mění preferenčně na transkrystalickou. Dráha šíření trhlin je velmi podobná dráze zjištěné při cyklování za pokojové teploty.

Additive manufacturing (AM) introduces high variability in the microstructure and defect distributions, compared with conventional processing techniques, which introduces greater uncertainty in the resulting fatigue performance of manufactured parts. As a result, qualification of AM parts poses as a problem in continued adoption of these materials in safety-critical components for the aerospace industry. Hence, there is a need to develop precise and accurate, physics-based predictive models to quantify the fatigue performance, as a means to accelerate the qualification of AM parts. The fatigue performance is a critical requirement in the safe-life design philosophy used in the aerospace industry. Fatigue failure is governed by the loading conditions and the attributes of the material microstructure, namely, grain size distribution, texture, and defects. In this work, the crystal plasticity finite element (CPFE) method is employed to model the microstructure-based material response of an additively manufactured Ni-based superalloy, Inconel 718 (IN718). Using CPFE and associated experiments, methodologies were developed to assess multiple aspects of the fatigue behavior of IN718 using four studies. In the first study, a CPFE framework is developed to estimate the critical characteristics of porosity, namely the pore size and proximity that would cause a significant debit in the fatigue life. The second study is performed to evaluate multiple metrics based on plastic strain and local stress in their ability to predict both the modes of failure as seen in fractography experiments and estimate the scatter in fatigue life due to microstructural variability as obtained from fatigue testing. In the third study, a systematic analysis was performed to investigate the role of the simulation volume and the microstructural constraints on the fatigue life predictions to provide informed guidelines for simulation volume selection that is both computationally tractable and results in consistent scatter predictions. In the fourth study, validation of the CPFE results with the experiments were performed to build confidence in the model predictions. To this end, 3D realistic microstructures representative of the test specimen were created based on the multi-modal experimental data obtained from high-energy diffraction experiments and electron backscatter diffraction microscopy. Following this, the location of failure is predicted using the model, which resulted in an unambiguous one to one correlation with the experiment. In summary, the development of microstructure-sensitive predictive methods for fatigue assessment presents a tangible step towards the adoption of model-based approaches that can be used to compliment and reduce the overall number of physical tests necessary to qualify a material for use in application.