<p> Laser powder bed fusion (LPBF) is a rapidly emerging manufacturing technology capable of producing complex part geometries through the repeated, precise laser melting of metallic powder layers. At present, the process is primarily employed in high-value-added applications which exist in the aerospace, biomedical, and dental industries. As industrial implementation of LPBF has matured, research has focused on established materials for which there are already large bodies of literature and regulatory approval, such as Inconel 718, Inconel 625, Ti-6Al-4V, and 316 stainless steel. However, the rapid solidification process inherent to LPBF leads to vastly different microstructures with improved strength compared to these traditional materials in cast or wrought forms. In general, the high solidification velocity and thermal gradients result in cellular and dendritic solidification structures with finer grain and precipitate sizes than conventionally processed alloys. These microstructure changes warrant the exploration of new alloy systems and reevaluation of historically cast compositions with optimized microstructures, especially considering the tunability of a digitally controlled fabrication process. This work examines laser powder bed fusion of Mar-M 509, a carbide-strengthened cobalt alloy that is typically investment cast directly into complex-shaped components such as nozzle guide vanes (NGVs). NGVs are stationary components in gas turbine engines for propulsion and energy production which require strength under moderate mechanical loading at high temperatures. Investment cast microstructures have porosity defects in slower-cooled regions due to lack of liquid feed to interdendritic regions. As-printed, the cellular and dendritic Mar-M 509 LPBF microstructures lead to the formation of continuous, fiber-like, eutectic carbide structures in the intercellular and interdendritic regions, which limit macroscopic ductility. Thermo-Calc is used for calculation of phase diagrams (CALPHAD) to estimate the equilibrium transformation temperatures of MC, M23C6, and M7C3-type carbides, which informs design of isothermal heat treatments to engineer microstructures with enhanced ductility over the as-printed or cast versions of Mar-M 509 while maintaining tensile strength. Scanning and transmission electron microscopy reveals the composition and distribution of carbide phases as a function of heat treatment temperature. Lastly, heat treatment recommendations for nozzle guide vanes are made.  </p>

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Demands for designing prime reliant, energy-efficient, and high performance thermal barrier coatings (TBCs) in gas turbines have led to a growing interest toward comprehensive microstructural characterization. Over the last decade, Synchrotron X-ray Diffraction (XRD) has established itself as a high-resolution strain measurement method for the thermally grown oxide (TGO) layer of thermal barrier coatings (TBCs). In this work, we present in-situ X-ray strain measurements of the TGO layer on cycled TBC specimens under thermo-mechanical loading using powerful high energy X-rays (~80.7- 86 keV) at Sector I-ID of the Advanced Photon Source at the Argonne National Laboratory. The evolution of TGO stresses was examined over one complete thermal cycle on TBC samples at various stages of the life fraction under various mechanical loads. Synchrotron X-Ray Diffraction under thermo-mechanical loading has shown the existence of strain qualitatively within the diffraction patterns. Quantitative results obtained through Pseudo-Voigt peak fitting over selected peaks show the evolution of strain over a thermal cycle. In initial experiments, it was shown that mechanical loading at 32 MPa resulted in a tensile strain (£22 = 0.00053±0.00039 for 7 minutes) along the [024] atomic plane of a-AbO3 that was brief before going into strain relief in the compressive region but higher in magnitude than the 64 MPa (£22 = 0.00039±0.00024 for 14 minutes). Follow-on experiments indicate the presence of tensile strains within the bond coat region of the TBC system. After initial assessment of the effect of mechanical loading, our findings indicate that the effect of mechanical load during the cycle, often neglected in TBC studies, is of significance to the strain evolution within each cycle. This determination of critical conditions for strain evolution ( e.g. the first cycle) will serve to improve overall accuracy in life prediction of these coatings and contribute to developing methods of improving fatigue behavior.

Résumé : Le développement des matériaux composites et leur utilisation dans le domaine du génie civil ont fait l’objet d’une recherche extensive sur le renforcement des structures en béton armé. Dans ce contexte, les études sur la compréhension du comportement structural des tubes en matériaux composites (Polymère renforcé en Fibre, PRF) sont indispensables. De fait que les matériaux composites sont innovateurs, cela nous exige de procéder à des investigations expérimentales approfondies pour vérifier les hypothèses et les théories, avant de les produire à échelle industrielle. Ce projet présente une étude expérimentale approfondie sur l’évaluation des propriétés physiques et mécaniques des nouveaux tubes en matériaux composites (PRF), et des tests sur la durabilité du matériau utilisé, et permet d’étudier l’influence de quelques facteurs environnementaux sur ces propriétés mécaniques, ces conditions sont simulées par une immersion prolongée en milieu aqueux et l'exposition à des cycles gel-dégel en milieu humide. Les tubes considérés sont produits par le procédé d’enroulement filamentaire à l’aide des fibres de verre (E) et de résine (Vinyle-Ester). Les expérimentations seront effectuées sur des échantillons normalisés prélevés à partir du tube. Les résultats de cette étude sont d’une importance cruciale pour comprendre le comportement structural (avant et après un vieillissement accéléré) des nouveaux tubes fabriqués entièrement en polymères renforcés de fibres par le procédé de l’enroulement filamentaire. // Abstract : The development of composite materials and their integration in the field of civil engineering has been the subject of extensive research on strengthening reinforced concrete structures. In the perspective of strengthening concrete structures by tubes made of composite materials. In this context, the need for knowledge of the structural behaviour of tubes made from fibre reinforced polymer (FRP) composite materials is prominent. The large using of innovativeFRP required extensive theoretical and experimental investigations. This project presents an experimental study to evaluate both the physical and mechanical properties of FRP-composites tubes, and to investigate the impact of some environmental factors on their mechanical properties. The tubes are produced by a filament winding process using fibre (E)-glass and vinyl-Ester resin. The experiments will be performed on standardized samples of the tube. The main objective of this project is to assess the physical and mechanical properties of laminated FRP composites, and then test the durability of the material used in the manufacture of the tubes. It leads to the study of the effects of some environmental factors on the mechanical properties of material. These conditions occur during an immersion in an aqueous medium and exposure to freeze-thaw cycles. The results of this study are crucial to understand the structural behavior (before and after accelerated aging) of new FRP tubes made by filament winding process.

Ziel dieser Arbeit ist es, eine Verbindung zwischen der Mikrostruktur teilkristalliner Polymere und derer mechanischen Eigenschaften auf der Mikro- und Nanometerskala aufzubauen. Dazu wurden Methoden der Rasterkraftmikroskopie verwendet um sowohl orts- als auch zeitaufgelöst Kristallisations-, Deformations- und Diffusionsprozesse in der Mikrostruktur von elastomerem Polypropylen (ePP) abzubilden. Die mechanischen Eigenschaften wurden simultan mit Mikrozugversuchen bestimmt. So konnte beispielsweise ein Zusammenhang zwischen abnehmender Kristall-Kristall-Distanz und einem Ansteigen des Elastizitätsmoduls während der Kristallisation nachgewiesen werden. Weiterhin war es möglich die Veränderung der nano-mechanischen Eigenschaften während der Kristallisation einzelner kristalliner Lamellen in deren direkter Umgebung mit MUSIC-mode Rasterkraftmikroskopie zu untersuchen. Laterale Querexpansion (auxetisches Verhalten) konnte bei uniaxialen Zugversuchen für die Kreuzschraffur-Struktur elastomeren Polypropylens auf der Größenskala einiger Mikrometer nachgewiesen werden. Zusätzlich wurde eine Orientierungsabhängigkeit dieses Effekts beobachtet. Außerdem wurde die Diffusion einzelner Kristalle in der Mikrostruktur von ePP beobachtet. Die Heterogenität dieser Diffusion lässt auf eine kristallin-amorph Grenzschicht um alle Kristalle schließen.

Dans de nombreuses applications industrielles les matériaux polycristallins sont soumis à de hautes températures, auxquelles le mécanisme de glissement aux joints de grains (GBS pour grain boundary sliding) tient un rôle essentiel. Il est fortement couplé à la plasticité intra cristalline, cependant peu de modèles tiennent compte de ce couplage. Le GBS est encore un mécanisme mal compris pour lequel nous manquons de quantifications expérimentales. Nous avons développé à cette fin un dispositif pour réaliser des expériences de compression in-situ dans un microscope électronique à balayage, équipé d’une mesure de température sans contact. Les essais ont été menés sur un aluminium à gros grains contenant 0.1% de manganèse entre 25°C et 400°C, à faible vitesse de déformation. Les champs cinématiques mesurés par corrélation d’images numérique ont permis d’analyser la mise en place des mécanismes de plasticité durant la déformation et leur évolution en fonction de la température. Nous avons mis en évidence un fort couplage entre les mécanismes plastiques intragranulaires et le GBS. A mesure que la température augmente nous avons constaté une forte évolution de la plasticité. La déformation se localise de plus en plus aux joints de grains, tandis que la plasticité dans les grains se complexifie impliquant de plus en plus de systèmes de glissement. Une méthode de corrélation d’images a été utilisée pour mesurer les discontinuités du champ cinématique aux joints de grains et quantifier la contribution du GBS à la déformation globale à 200°C. Celui-ci s’active dès le début et tout au long de la déformation. Nous avons constaté que malgré une taille de grains importante la contribution du GBS n’est pas négligeable, elle est plus importante en début de déformation puis semble atteindre un palier. Une approche locale a été développée pour quantifier l’amplitude locale du GBS. Cela a permis d’étudier et de discuter l’influence sur celui-ci de paramètres comme l’angle de désoriention du joint, un coefficient caractérisant le transfert du glissement intragranulaire à travers le joint, et l’orientation du joint par rapport à la direction de chargement. Ce dernier paramètre semble le plus influent, mais il ne suffit pas pour caractériser l’amplitude du glissement. Il apparaît que les propriétés locales de la microstructure influencent fortement celui-ci et ne peuvent être négligés. / In many industrial applications, polycrystalline materials are subjected to high temperatures at which grain boundary sliding (GBS) plays an essential part. It is however strongly coupled with intracrystalline plasticity, but very few models account for this coupling. GBS is not well understood and poorly quantified experimentally. To do so we have developed a set-up to perform in-situ compression experiments inside a scanning electron microscope, with a contactless temperature measurement. The tests have been done with large grained aluminium samples (0.1 % wt Mn) at several temperatures between 25°C and 400°C and a low strain rate. The kinematic fields measured by digital image correlation (DIC) have allowed the analysis of the start and development of plasticity mechanisms during deformation and their evolution with temperature. We have shown a strong coupling between intragranular plasticity and GBS. At higher temperature, the deformation is more concentrated at the grain boundaries while intragranular slip gets more complex, involving more glide systems. A DIC method has been used to measure the discontinuities at the grain boundaries and thus quantify the part of GBS with respect to the total plastic deformation at 200°C. Despite a large grain size, GBS contributes significantly to the deformation. GBS appears from the start of the deformation process, then reaches a limit. A local approach has been developed to quantify the local amplitude of GBS. This has allowed to weigh the influence of some geometrical parameters, such as grain misorientation, a coefficient which measures the transfer of intragranular sliding across the grain boundary and the orientation of the grain boundary with respect to the direction of solicitation. This last parameter seems to be the most relevant, but does not suffice to characterize the amplitude of the slip. The local properties of the microstructure cannot be neglected.

Le travail présenté dans ce document vise à mettre en évidence et à comprendre l'effet de la taille nanométrique des renforts sur les propriétés des nanocomposites avec une approche expérimentale. Des nanocomposites de PMMA et particules de silice (15nm, 25nm, 60nm, 150nm et 500nm) de fractions volumiques 2 0/0, 40/0 et 6 0/0 ont été fabriqués. Des analyses multi-échelles (MET et DRX-WAXS) ont montré que les paramètres caractéristiques de la microstructure des nanocomposites varient avec la taille des nanoparticules. En effet, la diminution de la taille des nanoparticules à fraction volumique constante a entrainé une diminution de la distance intermoléculaire. Cette diminution a induit une densification de la matrice et une réduction de la mobilité des chaînes de la matrice. Des essais mécaniques (traction, DMA) ont montré que les modules de Young (E) et de conservation (E') des nanocomposites augmentent avec la diminution de la taille des nanoparticules à fraction volumique constante. Et que l'augmentation de E' est conservée avec l'augmentation de la température. Une augmentation des températures de transition vitreuse (Tg) et de dégradation (Td) a également été observée avec les essais DSC, DMA et ATG. Le modèle de la borne inférieure d'Hashin-Shtrikman étendue aux nanocomposites à renforts sphériques proposé par Brisard a été utilisé. La modélisation des modules élastiques des nanocomposites a montré que pour reproduire les données expérimentales, il faut que d'une part que les modules surfaciques caractérisant l'interface soient dépendants de la taille des nanoparticules. Et d'autre part, tenir compte de l'état de dispersion des nanoparticules. / The work presented in this paper aims to highlight and to understand the size effect of nano-reinforcements on nanocomposite properties With an experimental approach. Nanocomposites of PMMA and silica particles With different sizes (15nm, 25nm, 60nm, 150nm and 500nm) and volume fractions (20/0, 4 0/0 and 60/0) were manufactured. Multiscale analysis (MET and DRX-WAXS) have shown that the characteristic parameters of the microstructure of nanocomposites vary With the size of the nanoparticles. Indeed, the decrease in the size of nanoparticles at a given volume fraction implies a decrease of the intermolecular distance. This decrease has induced a densification of the matrix and a decrease of the matrix chain mobility. Mechanical tests (tensile, DMA) have shown that the young (E) and the conservation (E') moduli of the nanocomposites increase With the decrease in the size of the nanoparticles With a constant volume fraction. And the increase of E l is kept when temperature growing. An increase in glass transition (Tg) and degradation temperature (Td) was also observed With the DSC, DMA and ATG tests. Experimental elastic properties of the nanocomposites were used to assess the relevance of size effect micromechanical models, particularly the Hashin-Shtrikman bounds With interface effects proposed by Brisard. The modeling has shown that to reproduce the experimental elastic moduli of nanocomposites, the elastic coefficients of the interface must be dependents on particle sizes. And the state of dispersion of particles must be taken into account.

Die Schriftenreihe „Werkstoffe und werkstofftechnische Anwendungen“ behandelt Themengebiete der Werkstoffwissenschaft und -technik, der Oberflächentechnik sowie deren industriellen Anwendungen. Es werden aktuelle Forschungsergebnisse aus den vier Professuren des Instituts für Werkstoffwissenschaft und Werkstofftechnik der TU Chemnitz vorgestellt: Professur Elektronenmikroskopie und Mikrostrukturanalytik, Professur Verbundwerkstoffe und Werkstoffverbunde, Professur Werkstoff- und Oberflächentechnik, Professur Werkstoffwissenschaft. Weiterhin sind in der Schriftenreihe die Tagungsbände des jährlich am Institut stattfindenden „Werkstofftechnischen Kolloquium“ enthalten. Die einzelnen Bände beschäftigen sich mit den Forschungsgebieten Galvanische Metallabscheidung, Anodisieren, Thermisches und Kaltgas-Spritzen, Löten, Verbundwerkstoffe, Werkstoffverbunde, Wärmebehandlung, CVD-Beschichtungen/PVD-Beschichtungen, Simulation in der Beschichtungstechnik, Organisches Beschichten (Pulverbeschichten, Lackieren, Sol-Gel-Verfahren), Elektrochemisches Strukturieren, Thermomechanische Behandlung und Mechanische Werkstoffeigenschaften. / The book series „Werkstoffe und werkstofftechnische Anwendungen“ outlines up-to-date topics of material science and engineering, surface engineering as well as resulting industrial applications. Mainly, recent research results of the departments Composite Materials and Surface Engineering/Functional Materials of the Institute of Material Science and Engineering of Chemnitz University of Technology are presented. In addition, the book series includes the proceedings of the annual in-house conference “Werkstofftechnisches Kolloquium”. The separate volumes concentrate on the following fields of scientific research: Galvanised Coating, Anodising, Thermal and Cold Spraying, Soldering and Brazing, Composite Materials, Composite Structures, Thermal and Thermomechanical Treatment, CVD and PVD Coating, Simulation of Coating Processes, Organic coating (Powder Coating, Varnishing, Sol-Gel Processes), Electrochemical Structuring and Mechanical Material Properties.

Size effects in out-of-plane bending stiffness of honeycomb cellular materials were studied using analytical mechanics of solids modeling, fabrication of samples and mechanical testing. Analysis predicts a positive size-effect relative to continuum model predictions in the flexure stiffness of a honeycombed beam loaded in out-of-plane bending. A method of determining the magnitude of that effect for several different methods of constructing or assembling square-celled and hexagonal-celled materials, using both single-walled and doubled-walled construction methods is presented. Hexagonal and square-celled honeycombs, with varying volume fractions were fabricated in Nylon 12 using Selective Laser Sintering. The samples were mechanically tested in three-point and four point-bending to measure flexure stiffness. The results from standard three-point flexure tests, did not agree with predictions based on a mechanics of solids model for either square or hexagonal-celled samples. Results for four-point bending agreed with the mechanics of solids model for the square-celled geometries but not for the hexagonal-celled geometries. A closed form solution of an elasticity model for the response of the four-point bending configuration was developed, which allows interpretation of recorded displacement data at two points and allows separation the elastic bending from the localized, elastic/plastic deformation that occurs between the loading rollers and the specimen’s surface. This localized deformation was significant in the materials tested. With this analysis, the four-point bending data agreed well with the mechanics of solids predictions. / text