Ce travail de thèse porte sur les mécanismes de plasticité et d'endommagement des aciers complexe-phase (CP). La microstructure bainitique de ces aciers, permets d’acquérir de bonnes propriétés de formabilité, qui intéressent les constructeurs automobiles. Cependant, la complexité de ces microstructures, qui se caractérisent par une grande quantité de joints de grains et une densité élevée de dislocations, influence la plasticité et les mécanismes d'endommagement. Afin d'estimer l'impact de la microstructure, une étude des caractéristiques métallurgiques des aciers à phases complexes est réalisée. Les mécanismes de plasticité sont ensuite étudiés par des tests de tension-compression afin d’étudier les mécanismes d’écrouissage du matériau. Ensuite, l’évolution de l’endommagement au sein de la microstructure est analysée à différente taux de triaxialité des contraintes afin d’obtenir la fraction de surface volumique ainsi que le nombre et le diamètre moyen des vides en fonction de la déformation plastique. Enfin, pour examiner la stabilité thermique de ces paramètres (microstructure, plasticité et endommagement), des expériences sont effectuées dans une plage de températures allant de 20 ° C à 600 ° C. / This PhD work investigates plasticity and damage mechanisms of complex phase steels. The bainitic microstructures of such steels, which feature retained austenite islands, result in these steels exhibiting good formability properties, which are of interest to automotive companies. However, the complexity of these microstructures, which are characterised by a high amount of grain boundaries and a high density of dislocations, influences plasticity and damage mechanisms. In order to estimate the impact of a steel's microstructure on these properties, the investigation of metallurgical features of complex phase steels provided by the company Faurecia is performed. Plasticity mechanisms are then investigated by tension-compression tests to determine the influence of long- and short-range interactions on the motion dislocation. Thereafter, the evolution of damage within microstructures is analysed at different stress triaxialities in order to obtain the volume area fraction and the number and average diameter of voids as functions of plastic strain. Finally, to examine the thermal stability of these parameters (microstructure, plasticity, and damage), experiments are performed at a range of temperatures between 20°C and 600°C.

Cette thèse constitue un des éléments du projet de recherche EMOCAVI (Evolution des Modèles des Composants de puissance grand gAp au cours du VIeillissement). Elle porte sur l’étude de la fiabilité des transistors de puissance en Nitrure de Gallium (GaN) récemment apparus sur le marché. Ces travaux se focalisent sur la réalisation d’une méthodologie pour paramétrer le modèle du composant GaN GIT (Gate Injection Transistor) en fonction du vieillissement auquel il a été soumis. Pour atteindre cet objectif, nous sommes passés par plusieurs étapes. La première a été consacrée à la définition, la mise en place et la validation d’un banc de vieillissement et à la caractérisation de ces composants avant et en cours de vieillissement. Un banc de test de vieillissement en court-circuit répétitif à faible puissance a été conçu et mis en oeuvre. Ce banc a permis de valider l’hypothèse du vieillissement lié à l’énergie, d’identifier son niveau déterminant d’un point de vue fiabilité du composant et enfin mettre en évidence la dégradation progressive du composant afin d’identifier les paramètres du transistor les plus sensibles au vieillissement. La deuxième étape de nos travaux a été consacrée à l’établissement d’une méthodologie de création de modèle de vieillissement du composant GaN-GIT. En reproduisant le modèle COBRA présenté dans la littérature, nous avons réussi dans nos travaux à proposer une approche novatrice permettant d’intégrer les dépendances en température et en énergie subie par le composant pendant le stress (la durée d’impulsion Tsc et le nombre de pulse subi Nsc). La dernière étape de nos travaux a été dédiée à l’analyse physique de défaillance afin de confirmer les hypothèses faites sur les mécanismes de dégradation obtenus après vieillissement du composant. Pour réaliser ces analyses, nous avons commencé par la décapsulation du composant en combinant l’ouverture laser aux attaques chimiques de la résine constituant le packaging. Une fois le défaut localisé par photoluminescence, une analyse approfondie par des vues au microscope électronique à balayage MEB puis par découpe PFIB (Plasma Fouced Ion Beam) a été réalisée afin de déterminer le mécanisme de défaillance. Il s’agissait principalement de fissures situées dans le métal d’Al au niveau du drain ainsi que la présence de cavités dans la couche métallique qui sert à réaliser le contact ohmique au niveau de la source, ce qui explique l’augmentation de la résistance RDSON. / This thesis constitute one of the elements of the EMOCAVI research project (Evolution of the Large gAp Power Component Models during the VIeillissement). It deals with the study of the reliability of Gallium Nitride (GaN) power transistors which are recently appeared on the market. This work focuses on the realization of a methodology to parameterize the model of GaN GIT component (Gate Injection Transistor) according to the aging to which it has been subjected. To achieve this goal, it will be necessary to go through several steps. The first step was dedicated to the definition, implementation and validation of an aging bench for the component and the characterization of these components before and during aging. A low power repetitive short-circuit aging test bench was designed and implemented. This bench is used to validate the energy-related aging hypothesis, to identify its determining level from a point of view of the reliability of the component and finally to highlight the progressive degradation of the component in order to identify the parameters of the transistor which are the most sensitive to aging. The second step of our work was devoted to the establishment of a methodology to create the aging model for the GaN-GIT component. By reproducing the COBRA model presented in the literature, we have succeeded in our work in proposing an innovative approach to integrate the dependencies in temperature and energy suffered by the component during stress (the Tsc pulse duration and the number of pulse suffered Nsc). The last step of our work was dedicated to the physical failure analysis in order to confirm the hypothesis made on the degradation mechanisms obtained after aging of the component. To carry out these analyzes, we started with the de-capsulation of the component by combining the laser cutting with the chemical attacks of the resin constituting the packaging. Once the defect was localized by photoluminescence, an in-depth analysis by SEM scanning and then PFIB (Plasma Focused Ion Beam) scans was performed to determine the mechanism of failure. These were mainly cracks in the Al metal at the drain and the presence of cavities in the metal layer which is used to make the Ohmic contact at the source, which explains the increase in resistance RDSON.

L’utilisation des composites à matrice céramiques (CMC), et particulièrement les matériaux SiC/SiC, à la place des alliages métalliques dans les moteurs aéronautiques peut permettre de réduire leur consommation. Ils possèdent en effet des propriétés physiques et mécaniques très intéressantes à haute température : faible densité, résistance élevée aux chocs thermiques et rupture non-fragile. Dans ces matériaux, une fine couche est insérée entre les fibres et la matrice : l’interphase. Le nitrure de bore pyrolytique est le matériau d’interphase de choix pour les applications visées. La bibliographie souligne bien la nécessité et la difficulté de « contrôler » l’intensité des liaisons interfaciales fibres/matrice (F/M) grâce à l’interphase. Mais l’influence exacte de la cristallinité et de l’épaisseur des interphases de type BN sur son contrôle, et par conséquent sur le comportement mécanique final du CMC industriel est encore mal connue.Une première problématique abordée dans cette thèse est l’échelle du CMC de laboratoire à utiliser. En effet jusqu’ici, les matériaux modèles les plus couramment employés sont les mini- et les micro- composites 1D. Ils peuvent être élaborés facilement et rapidement par dépôt chimique en phase vapeur mais ne rendent pas compte de phénomènes inévitablement présents au sein du composite industriel. C’est pourquoi l’utilisation de nouveaux matériaux modèles 2D comme les « monostrates » comprenant un pli de tissu, l’interphase BN et une matrice de SiC dont la porosité peut être comblée par du Si comme dans le cas des CMC industriels est plus pertinente et est proposée. Cependant, de par la faible épaisseur des éprouvettes, les protocoles de caractérisation et de tests mécaniques ont dû être revus. Il s’agit notamment de caractériser la liaison F/M par deux paramètres : la contrainte de cisaillement de la liaison interfaciale (τi) et le module de cisaillement du matériau (G12).Pour la partie mécanique, des essais de traction monotone et cyclée dans l’axe des fibres du renfort (exploités à l’aide de modèles micromécaniques), des essais de cisaillement Iosipescu, ainsi que des essais de push out ont été mis au point et exploités. Des analyses de micro caractérisation par microscopie électronique (MEB, FIB-MEB, MET) ont été réalisées avant et après essais mécaniques avec des interphases de différentes configurations afin de relier les différences de microstructures et d’épaisseurs aux chemins de fissuration matricielle et aux comportements mécaniques macroscopiques des composites. La liaison F/M la plus forte est notamment obtenue quand le degré de cristallisation et l’anisotropie structurale du BN sont peu élevés, pourvu que l’épaisseur de l’interphase soit suffisante. / The use of ceramic matrix composites (CMC), and particularly SiC/SiC materials, in place of metal alloys in aircraft engines has the potential to reduce their fuel consumption. They have very interesting physical and mechanical properties at high temperatures: low density, high resistance to thermal shock and non- brittle failure. In these materials, a thin layer is inserted between the fibres and the matrix: the interphase. Pyrolytic boron nitride is the interphase material of choice to achieve the desired applications. The bibliography clearly highlights the need and difficulty of "controlling" the intensity of fibre/matrix interfacial bonds (F/M) thanks to the interphase. But the exact influence of the crystallinity and thickness of BN-type interphases on its control, and consequently on the final mechanical behaviour of the industrial CMC, is still insufficiently known.A first issue addressed in this thesis is the scale of the CMC to be used in the laboratory. Indeed, so far, the most commonly used model materials are 1D mini and micro composites. They can be easily and quickly prepared by chemical vapour deposition but do not account for phenomena inevitably present in the industrial composite. Therefore, the use of new 2D model materials such as "monostrates" comprising a single-ply woven, the BN interphase and a SiC matrix in which the porosity can be filled with Si as in the case of industrial CMCs is more relevant and is proposed. However, due to the thinness of the specimens, the characterization and mechanical testing protocols had to be reviewed. This involves characterizing the F/M bond by two parameters: the shear stress of the interfacial bond (τi) and the shear modulus of the material (G12).For the mechanical part, monotonic and cycled tensile tests in the fibre axis of the reinforcement (operated using micromechanical models), Iosipescu shear tests, as well as push-out tests were developed and used. Micro characterization analyses by electron microscopy (SEM, FIB-SEM, TEM) were performed before and after mechanical tests with interphases of different configurations in order to link the differences in microstructures and thicknesses to the matrix cracking paths and macroscopic mechanical behaviours of the composites. The strongest F/M bond is obtained notably when the degree of crystallization and structural anisotropy of the BN are low, provided that the interphase is thick enough.

<p>Predmet izučavanja ove disertacije obuhvatio je ispitivanje uticaja starenja stabilizovanog/solidifikovanog&nbsp; (S/S)&nbsp; sedimenta&nbsp; zagađenog te&scaron;kim metalima i arsenom, i efikasnost primenjenih imobilizacionih agenasa (Portland cement, kreč, leteći pepeo, zeolit, montmorilonit i kaolinit) nakon dugogodi&scaron;njeg starenja S/S sme&scaron;a. Shodno tome ispitana je dugoročna stabilnost i postojanost dobijenih S/S sme&scaron;a sa aspekta izluživanja pomenutih metala, promene u minerolo&scaron;kim i strukturnim karakteristikama, kao i uticaj su&scaron;enja i zrenja materijala na pomenute parametre. Istraživanja u disertaciji obuhvatila su dve faze. Prva faza imala je za cilj procenu rizika i&nbsp; početnu karakterizaciju netretiranog sedimenta primenom analize pseudo-ukupnog sadržaja metala kojom je utvrđen sadržaj metala u početnom uzorku sedimenta. Druga faza uključivala je primenu tretmana stabilizacije i solidifikacije na kontaminirani sediment dodavanjem različitih imobilizacionih agenasa. Analize su se vr&scaron;ile nakon 7 i 28 dana od primenjenog S/S tretmana, kao i nakon 7 godina sa ciljem da se utvrdi uticaj vi&scaron;egodi&scaron;njeg starenja i zrenja monolitnih sme&scaron;a na mobilnost metala i strukturne karakteristike sme&scaron;a. U&nbsp; okviru&nbsp; druge faze istraživanja ispitana je toksičnost S/S sme&scaron;a primenom DIN i TCLP testova izluživanja, dok je test toksičnosti primenom bakterija Vibrio Fischeri&nbsp; doprineo u&nbsp; sagledavanju&nbsp; procene rizika S/S sme&scaron;a po organizme. Nakon 28 dana i 7 godina kori&scaron;ćena je sekvencijalna ekstrakcija za&nbsp; određivanje mobilnost i biodostupnost metala u monolitnim matriksima. U cilju&nbsp; utvrđivanja mikrostukturnih karakteristika sedimenta primenjena je rendgenska difrakciona analiza (XRD) za ispitivanje kristalnih struktura&nbsp; S/S sme&scaron;a i detekciju mineralnog sastava. Pomoću elektronskog mikroskopa i energodisperzivnog detektora&nbsp; sa X-zrakom (SEM/EDS) određena je kvalitativna i kvantitativna distribucija metala i&nbsp; drugih elemenata od interesa, dok se za identifikaciju formiranih funkcionalnih grupa u monolitnim sme&scaron;ama primenio spektrometar sa infracrvenom Furijeovom transformacijom (FTIR). Na osnovu dobijenih rezultata zaključeno je da se mobilnost te&scaron;kih metala i arsena značajno smanjila nakon 7 godina za sme&scaron;e tretirane cementom (C5), krečom (L10), letećim pepelom (F30) i kaolinitom&nbsp; (K20), a efekat stabilizacije je pokazan transformacijom metala iz direktne toksične frakcije u&nbsp; stabilnije oblike. Sme&scaron;e C5 i K20 ispoljavaju&nbsp; najmanje toksične efekate od svih sme&scaron;a, jer je procenat inhibicije&nbsp; na&nbsp; bioluminiscentnim&nbsp; bakterijama manji od 13%, dok je u pogledu izdržljivosti monolitna sme&scaron;a C5 pokazala najveću pritisnu čvrstoću od svih sme&scaron;a. Dobijeni podaci su neprocenjivi za dobijanje stvarnog uvida u dugoročnu efikasnost&nbsp; primenjenog&nbsp; tretmana i mogućnost bezbedne upotrebe ili odlaganja dobijenih S/S sme&scaron;a sa aspekta za&scaron;tite životne sredine, kao i ekonomski i ekolo&scaron;ki prihvatljivog upravljanja opasnim otpadom.</p> / <p>The subject of study in this dissertation included to investigate the&nbsp; effect&nbsp; of&nbsp; aging&nbsp; of&nbsp; stabilized/solidified&nbsp; (S/S)&nbsp; sediment&nbsp; contaminated with&nbsp; heavy&nbsp; metals&nbsp; and&nbsp; arsenic,&nbsp; and&nbsp; the&nbsp; efficacy&nbsp; of&nbsp; the&nbsp; applied immobilization&nbsp; agent&nbsp; (Portland&nbsp; cement,&nbsp; lime,&nbsp; fly&nbsp; ash,&nbsp; zeolite, montmorillonite and kaolinite) after long-term aging of S/S mixtures. The<br />long&nbsp; -&nbsp; term stability and stability of the obtained S/S mixtures from the aspect of leaching of the mentioned metals, changes in mineralogical and structural characteristics,&nbsp; as&nbsp; well&nbsp; as&nbsp; the&nbsp; influence&nbsp; of&nbsp; drying&nbsp; and maturation of the material on the mentioned parameters were examined. The&nbsp; research&nbsp; in&nbsp; the&nbsp; dissertation&nbsp; included&nbsp; two&nbsp; phases.&nbsp; The&nbsp; first&nbsp; phase aimed&nbsp; at&nbsp; risk&nbsp; assessment&nbsp; and&nbsp; initial characterization&nbsp; of&nbsp; untreated sediment using pseudo-total metal content analysis which determined the<br />metal content in the initial sediment sample.&nbsp; The second phase involved applying&nbsp; stabilization&nbsp; and&nbsp; solidification&nbsp; treatments&nbsp; to&nbsp; the&nbsp; contaminated sediment&nbsp; by&nbsp; adding&nbsp; various&nbsp; immobilizing&nbsp; agents.&nbsp; The&nbsp; analyzes&nbsp; were performed after 7 and 28&nbsp; days from the applied S/S treatment, as well as after 7 years in order to determine the influence of perennial aging and maturation&nbsp; of&nbsp; monolithic&nbsp; mixtures&nbsp; on&nbsp; metal&nbsp; mobility&nbsp; and&nbsp; structural characteristics&nbsp; of&nbsp; the&nbsp; mixtures.&nbsp; In&nbsp; the&nbsp; second&nbsp; phase&nbsp; of&nbsp; the&nbsp; study,&nbsp; the toxicity&nbsp; of&nbsp; S/S&nbsp; mixtures&nbsp; using&nbsp; DIN&nbsp; and&nbsp; TCLP&nbsp; leaching&nbsp; tests&nbsp; was examined, while&nbsp; the&nbsp; toxicity&nbsp; test&nbsp; using&nbsp; bacteria&nbsp; Vibrio&nbsp; Fischeri contributed&nbsp; to&nbsp; the assessment&nbsp; of&nbsp; the&nbsp; risk&nbsp; of&nbsp; S/S&nbsp; mixtures&nbsp; to&nbsp; organisms. After&nbsp; 28 days&nbsp; and&nbsp; 7 years,&nbsp; sequential extraction was&nbsp; used to&nbsp; determine the mobility and bioavailability of metals in monolithic matrices. In order to&nbsp; determine&nbsp; the&nbsp; microstructural&nbsp; characteristics&nbsp; of&nbsp; the&nbsp; sediment,&nbsp; x-ray diffraction analysis (XRD) was used to examine the crystal structures of&nbsp; S/S mixtures and&nbsp; to detect the mineral composition.&nbsp; The qualitative and quantitative&nbsp; distribution&nbsp; of&nbsp; metals&nbsp; and&nbsp; other&nbsp; elements&nbsp; of&nbsp; interest&nbsp; was determined using an electron microscope and an energy-dispersive X-ray detector&nbsp; (SEM&nbsp; /&nbsp; EDS),&nbsp; while&nbsp; an&nbsp; infrared&nbsp; Fourier&nbsp; transform spectrometer(FTIR) was used to identify the formed functional groups in monolithic mixtures. Based on the obtained results, it was concluded that the mobility of heavy metals and arsenic decreased significantly after 7 years&nbsp; for&nbsp; mixtures&nbsp; treated&nbsp; with&nbsp; cement&nbsp; (C5),&nbsp; lime&nbsp; (L10),&nbsp; fly ash&nbsp; (F30) and&nbsp; kaolinite&nbsp; (K20),&nbsp; and&nbsp; the&nbsp; stabilization&nbsp; effect&nbsp; was&nbsp; shown&nbsp; by transformation&nbsp; of&nbsp; metals&nbsp; from&nbsp; direct&nbsp; toxic&nbsp; fractions&nbsp; into&nbsp; more&nbsp; stable forms. Mixtures&nbsp; C5&nbsp; and&nbsp; K20&nbsp; exhibit&nbsp; the&nbsp; least&nbsp; toxic&nbsp; effects&nbsp; of&nbsp; all mixtures, because the percentage of inhibition on bioluminescent bacteria is less than 13%, while in terms of durability, the monolithic mixture C5 showed&nbsp; the&nbsp; highest&nbsp; compressive&nbsp; strength&nbsp; of&nbsp; all&nbsp; mixtures.&nbsp; The&nbsp; obtained data are invaluable for gaining real insight into the long-term efficiency of the applied treatment and the possibility of safe use&nbsp; or disposal of the obtained&nbsp; S/S&nbsp; mixtures&nbsp; from&nbsp; the&nbsp; aspect&nbsp; of&nbsp; environmental&nbsp; protection,&nbsp; as well&nbsp; as&nbsp; economically&nbsp; and&nbsp; ecologically&nbsp; acceptable&nbsp; hazardous&nbsp; waste management.</p>

The penchant towards development of high performance materials for light weighting engineering systems through various thermomechanical processing routes has been soaring vigorously. Friction stir processing (FSP) - a relatively new thermomechanical processing route had shown an excellent promise towards microstructural modification in many Al and Mg alloy systems. Nevertheless, the expansion of this process to high temperature materials like titanium alloys and steels is restricted by the limited availability of tool materials. Despite it challenges, the current thesis sets a tone for the usage of FSP to tailor the mechanical properties in titanium alloys and steels. FSP was carried out on three near beta titanium alloys, namely Ti6246, Ti185 and Tiβc with increasing β stability index, using various tool rotation rates and at a constant tool traverse speed. Microstructure and mechanical property relationship was studied using experimental techniques such as SEM, TEM, mini tensile testing and synchrotron x-ray diffraction. Two step aging on Ti6246 had resulted in an UTS of 2.2GPa and a specific strength around 500 MPa m3/mg, which is about 40% greater than any commercially available metallic material. Similarly, FSP on an ultra-high strength steel―Eglin steel had resulted in a strength greater than 2GPa with a ductility close to 10% at around 4mm from the top surface of stir zone (SZ). Experimental techniques such as microhardness, mini-tensile testing and SEM were used to correlate the microstructure and properties observed inside SZ and HAZ's of the processed region. A 3D temperature modeling was used to predict the peak temperature and cooling rates during FSP. The exceptional strength ductility combinations inside the SZ is believed to be because of mixed microstructure comprised of various volume fractions of phases such as martensite, bainite and retained austenite.

The demand for Advanced High Strength Steel (AHSS) in the automotive industry is increasing day by day. It is mainly motivated by the fact that AHSS can be used as thin sheets while having high strengths. It enables weight reduction of the automobiles which consequently increases the fuel efficiency and has proven to be less harmful to the environment. It is also expected that AHSS will have even higher strength in the near future. Cold work tools steels with 5 wt.% Cr are commonly used to process AHSS. Therefore, the tool steel must meet the challenges in the future, i.e. have even higher hardness, compressive strength and toughness. One way of increasing the mechanical properties of the tool steel is by improving the heat treatment parameters. However, it is not possible without a deeper understanding of the heat treatment process. Therefore, this work presents investigations related to phase transformations occurring in a 5 wt.% Cr cold work tool steel during heat treatment. Furthermore, the influence of austenitisation and tempering temperatures on the microstructure and mechanical properties were investigated. The studies revealed that a higher austenitisation temperature can be used to achieve a higher hardness, good compressive strength and adequate toughnessof the steel. However, too high austenitisation temperature may result inexcessive coarsening of prior austenite grains which reduced the impact toughness. It was also found that retained austenite can transform during tempering by two different mechanisms. Firstly, when tempering at 525°C, carbides precipitate in retained austenite lowering its stability and permitting a transformation to marten site on cooling. Secondly, when tempering at 600°Cfor extended holding time retained austenite isothermally transforms to ferrite and carbides. This occurs by precipitation of carbides in retained austenite followed by a final transformation to ferrite and carbides.These results were used to understand the standard tempering procedure of the 5 wt.% Cr cold work tool steel. Furthermore, alternative heat treatment procedures are discussed based on the important findings presented in this thesis.

In modern turbine engines for propulsion and energy generation, thermal barrier coating (TBCs) protect hot-section blades and vanes, and play a critical role in enhancing reliability, durability and operation efficiency. In this study, thermal cyclic lifetime and microstructural degradation of electron beam physical vapor deposited (EB-PVD) Yttria Stabilized Zirconia (YSZ) with (Ni,Pt)Al bond coat and Hf- and/or Y- modified CMSX-4 superalloy substrates were examined. Thermal cyclic lifetime of TBCs was measured using a furnace thermal cycle test that consisted of 10-minute heat-up, 50-minute dwell at 1135C, and 10-minute forced-air-quench. TBC lifetime was observed to improve from 600 cycles to over 3200 cycles with appropriated Hf- and/or Y alloying of CMSX-4 superalloys. This significant improvement in TBC lifetime is the highest reported lifetime in literature with similar testing parameters. Beneficial role of reactive element (RE) on the durability of TBCS were systematically investigated in this study. Photostimulated luminescence spectroscopy (PL) was employed to non-destructively measure the residual stress within the TGO scale as a function of thermal cycling. Extensive microstructural analysis with emphasis on the YSZ/TGO interface, TGO scale, TGO/bond coat interface was carried out by scanning electron microscopy (SEM), transmission electron microscopy (TEM), and scanning electron microscopy (STEM) as a funcion of thermal cycling including after the spallation failure. Focused ion beam in-situ lift-out (FIB-INLO) technique was employed to prepare site-specific TEM specimens. X-ray diffraction (XRD) and secondary ion mass spectroscopy (SIMS) were also employed for phase identification and interfacial chemical analysis. While undulation of TGO/bond coat interface (e.g., rumpling and ratcheting) was observed to be the main mechanism of degradation for the TBCs on baseline CMSX-4, the same interface remained relatively flat (e.g., suppressed rumpling and ratcheting) for durable TBCs on Hf- and/or Y-modified CMSX-4. The fracture paths changed from the YSZ/TGO interface to the TGO/bond coat interface when rumpling was suppressed. The geometrical incompatibility between the undulated TGO and EB-PVD YSZ lead to the failure at the YSZ/TGO interface for TBCs with baseline CMSX-4. The magnitude of copressive residual stress within the TGO scale measured by PL gradually decreased as a function of thermal cycling for TBCs with baseline CMSX-4 superalloy substrates. This gradual decrease corrsponds well to the undulation of the TGO scale that may lead to relaxation of the compressive residual stress within the TGO scale. For TBCs with Hf- and/or Y-modified CMSX-4 superalloy substrates, the magnitude of compressive residual stress within the TGO scale remained relatively constant throughout the thermal cycling, although PL corresponding to the stress-relief caused by localized cracks at the TGO/bond coat interface and within the TGO scale was observed frequently starting 50% of lifetime. A slightly smaller parabolic growth constant and grain size of the TGO scale was observed for TBCs with Hf- and/or Y- modified CMSX-4. Small monoclinic HfO2 precipitates were observed to decorate grain boundaries and the triple pointes within the alpha-Al2O3 scale for TBCs with Hf- and/or Y-modified CMSX-4 substrates. Segregation of Hf/Hf4+ at the TGO/bond coat interfaces was also observed for TBCs with Hf- and/or Y-modified CMSX-4 superalloys substrates. Adherent and pore-free YSZ/TGO interface was observed for TBCs with Hf- and/or Y-modified CMSX-4, while a significant amount of decohesion at the YSZ/TGO interface was observed for TBCs with baseline CMSX-4. The beta-NiAl(B2) phase in the (Ni,Pt)Al bond coat was observed to partially transform into gama prime-Ni3Al (L12) phase due to depletion of Al in the bond coat during oxidation. More importantly, the remaining beta-NiAl phase transformed into L10 martensitic phase upon cooling even though there was no significant difference in these phase transformations for all TBCs. Results from these microstructural observations are documented to elucidate mechanisms that suppress the rumpling of the TGO/bond coat interface, which is responsible for superior performance of EB-PVD TBCs with (Ni,Pt)Al bond coat and Hf- and/or Y-modified CMXS-4 superalloy.

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Yes / Owing to their small size, good wettability, uniform dispersion ability and high thermal properties, the nickel-plated carbon nanotubes (Ni-CNTs) with different aspect ratios are used to reinforce reactive powder concrete (RPC) through modifying the nano/micro- structural units of concrete. Incorporating only 0.075 vol% of Ni-CNTs (0.03 vol% of CNTs) can significantly increase mechanical properties of RPC. The enhancement effect on compressive strength caused by the incorporation of Ni-CNTs with aspect ratio of 1000 reaches 26.8%/23.0 MPa, mainly benefiting from the high polymerization C-S-H gels, low porosity, and refined pore structure. The 33.5%/1.92 MPa increases of flexural strength can be attributed to the decrease of large pore, original cracks, molar ratio of CaO to SiO2, and gel water content when Ni-CNTs with aspect ratio of 125 are added. Ni-CNTs with aspect ratio of 1500 have the largest utilization rate of being pulled-out, resulting from the improvement of dispersibility and the pining effect of nickel coating and then leading to the increased toughness. Therefore, incorporating Ni-CNTs can fundamentally modify the nano/micro- scale structural nature of RPC, providing a bottom-up approach for controlling the properties of RPC. / Funding supported from the National Science Foundation of China (51908103 and 51978127) and the China Postdoctoral Science Foundation (2019M651116).