La présente thèse doctorale vise à analyser le comportement tribologique, en corrosion et en tribocorrosion des nouveaux aciers inoxydables martensitiques et leurs mécanismes de dégradation pour applications aéronautiques. Pour ce faire, techniques électrochimiques, tribo-électrochimiques et d’analyse de surface ex-situ ont été utilisés. L'usure est affectée par la dureté du matériau et le durcissement lors du glissement de contact. Les aciers inoxydables martensitiques ont montré une augmentation de résistance à la rayure, mais une plus grande perte de matière lors des essais tribologiques à sec par rapport à l'acier inoxydable austénitique. La résistance à la corrosion des aciers inoxydables martensitiques est favorisée par leur passivité, dont la cinétique du film passif peut être décrite par un modèle de type high-field. La vitesse de dissolution passive dépend de la composition chimique de la surface du matériau, ce qui diminue la teneur en Cr dans la couche passive. Les mécanismes de dégradation en tribocorrosion des aciers inoxydables martensitiques comprennent déformation plastique, shakedown et fatigue de de type oligo-cyclique. Les conséquences de ces mécanismes impliqués dépendent des conditions électrochimiques qui prévalent. / The present Doctoral Thesis aimed to analyze the tribological, corrosion and tribocorrosion behavior of new martensitic stainless steels and their degradation mechanisms for aeronautical applications. For this, electrochemical, tribo-electrochemical and ex-situ surface analysis techniques were used. Wear damage was found to be critically affected by the hardness of the material and its hardening during sliding. Martensitic stainless steels showed higher scratch wear resistance but higher wear material loss when compared to the austenitic stainless steel. Corrosion resistance of martensitic stainless steels is driven by their passivity, whose kinetics can be described through a high field conduction model. Passive dissolution rate depends on the surface chemistry of the material, thus decreasing with the Cr content in the passive film. Degradation mechanisms involved in tribocorrosion of martensitic stainless steels included plastic deformation, shakedown and low-cycle fatigue. The consequences of those involved mechanisms depended on the prevailing electrochemical conditions. / La presente Tesis Doctoral tiene como objetivo analizar el comportamiento tribológico, frente a la corrosión y a la tribocorrosión de nuevos aceros inoxidables martensíticos y sus mecanismos de degradación en aplicaciones aeronáuticas. Para ello, se han utilizado técnicas electroquímicas, tribo-electroquímicas y de análisis de superficie ex-situ. El desgaste depende de la dureza del material y de su endurecimiento durante el deslizamiento. Los aceros inoxidables martensíticos mostraron una mayor resistencia al rallado pero una mayor pérdida de material en el ensayo tribológico de desgaste si se compara con el acero inoxidable austenítico. La resistencia a la corrosión de los aceros inoxidables martensíticos es promovida por su pasividad, cuya cinética puede ser descrita a través de un modelo de tipo high field. La velocidad de disolución pasiva depende de la química de la superficie del material, disminuyendo por lo tanto con el contenido de Cr en la película pasiva. Los mecanismos de degradación en tribocorrosión de los aceros inoxidables martensíticos incluyen deformación plástica, shakedown y fatiga de bajo ciclo. Las consecuencias de esos mecanismos dependen de las condiciones electroquímicas del sistema. / La present Tesi Doctoral té com a objectiu analitzar el comportament tribològic, front a la corrosió i a la tribocorrosió de nous acers inoxidables martensítics i els seus mecanismes de degradació en aplicacions aeronàutiques. Per tot això, s'han utilitzat tècniques electroquímiques, tribo-electroquímiques i d'anàlisi de superfície ex-situ. El desgast depen de la duresa del material i del seu enduriment durant el lliscament. Els acers inoxidables martensítics van mostrar una major resistència al ratllat però una major pèrdua de material en l'assaig tribològic de desgast si es compara amb l'acer inoxidable austenític. La resistència a la corrosió dels acers inoxidables martensítics és promoguda per la seva passivitat, i la seua la cinètica pot ser descrita a través d'un model de tipus high field. La velocitat de dissolució passiva depen de la química de la superfície del material, disminuint per tant amb el contingut de Cr en la pel·lícula passiva. Els mecanismes de degradació en tribocorrosió dels acers inoxidables martensítics inclouen deformació plàstica, shakedown i fatiga de baix cicle. Les conseqüències d'aquests mecanismes depenen de les condicions electroquímiques del sistema.

L’acier inoxydable martensitique durci par précipitation 15-5PH est utilisé dans le domaine del’aéronautique comme matériau constitutif des pièces liant les réacteurs aux ailes, il est ainsi soumisen utilisation à des températures de l’ordre de 300°C, ce qui entraine sa fragilisation. Cettefragilisation des aciers inoxydables dans ce domaine de températures est causée par la démixtion dufer et du chrome, principaux constituants de la matrice, par décomposition spinodale. De plus, lamicrostructure complexe du 15-5PH contient également des précipités de cuivre assurant ledurcissement initial de l’alliage, de l’austénite de réversion, connue dans ce type d’aciers pourapporter un regain de ductilité, apparaissant lors du traitement de précipitation du cuivre et de laphase G apparaissant au cours du vieillissement. L’évolution de ces phases pourrait égalemententrainer une modification des propriétés mécaniques de l’alliage. Pour observer les différentesévolutions de la microstructure nous avons utilisé une combinaison de techniques apportant desinformations complémentaires afin d’en obtenir une caractérisation la plus complète possible. Nousavons ainsi pu montrer que les modifications de propriétés sont causées par la décompositionspinodale de la matrice. L’évolution de ses caractéristiques microstructurales a pu être décrite pardes lois phénoménologiques, fonctions de la durée et de la température de vieillissement. Nousavons également pu fournir une méthode permettant la mesure indirecte de l’avancée duvieillissement du 15-5PH, validée par les observations microstructurales, ainsi qu’un modèlephénoménologique permettant de prévoir la dureté de l’alliage.Mots clés : acier martensitique, décomposition spinodale, vieillissement, diffusion aux petits angles,sonde atomique tomographique, calorimétrie différentielle à balayage. / The precipitation hardened martensitic stainless steel grade 15-5PH is used in the airplane industryas constitutive material of parts joining reactors to wings. Due to its application it is subjected totemperatures around 300°C leading to its embrittlement. Stainless steels embrittlement in thistemperature range is due to iron-chromium unmixing by spinodal decomposition. In addition, the 15-5PH grade has a complex microstructure comprising copper precipitates responsible for the initialhardening of the alloy, reversed austenite, known in this kind of steels to improve the toughness,which appears during the precipitation thermal treatment and G phase that precipitates duringaging. The evolutions of these microstructure components could also lead to some modifications ofthe material mechanical properties. In order to study the microstructure evolutions we use acombination of characterization techniques aiming at their most complete description. We show thatthe mechanical properties evolution is controlled by the spinodal decomposition of the matrix whoseevolution we are able to depict by simple phenomenological laws. We propose an indirect methodfor the measurement of aging kinetics of the 15-5PH steel, which we have correlated to directmeasurements, and a phenomenological law allowing the prediction of the alloy hardness based onits thermal history.

O presente trabalho avaliou o efeito de tratamentos térmicos ou diferentes graus de deformação plástica na transformação da austenita do microconstituinte AM de uma chapa de aço alta resistência baixa liga (ARBL) classe API 5L X80 usada para gasodutos. A chapa tem espessura de 19 mm e passaria pelo processo de conformação UOE, mas a deformação foi realizada por laminação a frio, a temperatura ambiente, com reduções de 5 a 20%. O propósito foi compreender melhor o microconstituinte AM, explorar a transformação martensítica induzida por deformação (SIMT) e a decomposição austenítica por tratamento térmico, com ênfase em seu comportamento magnético. A transformação da austenita foi acompanhada através de medidas de polarização magnética, comparada com a densidade de massa e difração de raios X. A deformação plástica e os tratamentos térmicos alteraram a polarização magnética de saturação e a densidade de massa da amostra de aço de forma compatível com a eliminação da austenita retida metaestável. O método de densidade hidrostática foi considerado sensível para mensurar transformações de fase. Os dados obtidos revelam expansão volumétrica de aproximadamente 0,13%, correspondendo a 3,2% a quantidade de austenita retida original do material, enquanto os valores obtidos por polarização magnética de saturação são 2,8% pelo histeresígrafo e 2,1% por MAV. A difração de raios X nas amostras sob deformação ou tratamentos térmicos resultaram em queda nos primeiros picos da austenita quando comparadas com a amostra como recebida. / This study evaluated the effect of different degrees of plastic deformation or heat treatment on the transformation of austenite into martensite of an HSLA steel plate API 5L X80 for pipelines. A 19 mm thickness plate would be submitted to UOE forming process, but the cold work instead occurred by cold rolling at room temperature, with reductions of 5 up to 20%. The purpose was to better understand the MA constituent, explore the strain-induced martensitic transformation (SIMT) and austenitic decomposition by heat treatment with emphasis on its magnetic behavior. The transformation was accompanied by saturation magnetization measurements, compared with the mass density and X-ray diffraction. The plastic deformation or the heat treatment altered the saturation magnetization and the mass density in a manner consistent with the elimination of metastable retained austenite. The density method is sensible to measure phase transformations induced by strain. The data obtained shows a volumetric expansion of about 0.13%, corresponding to an amount of retained austenite of the original material of 3.2%, while the values obtained by magnetization saturation are 2.8% by hysteresigraph and 2.1% by VSM. By X-ray diffraction there is a clear drop in first peaks of austenite of the samples under deformation or heat treatment compared with the sample as-received.

Cette thèse porte sur l’influence des transformations de phases solide-solide sur la propagation de fissure. On souhaite ainsi mieux comprendre les variations de ténacité en cours de soudage par exemple, ou bien pendant la réparation d’une fissure. Dans ce travail, la ténacité est obtenue à partir de l’intégrale J. Il existe de nombreuses méthodes expérimentales permettant d’obtenir la ténacité critique JIC mais qui sont difficilement applicables pour des essais se déroulant pendant une transformation de phase. C’est pourquoi nous avons proposé une méthode couplant essai mécanique et mesure par corrélation d’images avec de la simulation par éléments finis. Les essais sont réalisés sur de simples éprouvettes plates pré fissurées, faciles à usiner et simple à chauffer par induction. Les essais sont conduits pour différentes températures et jusqu’à rupture. En sus des mesures d’efforts et déplacements de traverse, la corrélation d’images nous fourni également les champs de déplacement sur chaque face de l’éprouvette. Chaque essai est ensuite simulé par éléments finis où la ténacité critique est calculée par la méthode G-Theta au maximum de la charge supportée par l’éprouvette. Les simulations précédentes intègrent les conditions aux limites obtenues par corrélation et le comportement mécanique considéré est celui que nous avons identifié sur des essais de caractérisation. Deux nuances de matériau ont été étudiées avec cette méthode ; l’acier inoxydale 15-5PH ainsi que l’acier ferritique 16MND5. Pour ces deux matériaux, différentes températures d’essai ont été choisies avant, pendant et après la transformation pour effectuer les essais de rupture ainsi que de caractérisation du comportement mécanique. Les résultats de cette étude montrent que la transformation de phase peut avoir un impact non négligeable sur la ténacité. Ainsi, pour le 15-5PH, le taux d’austénite résiduel est un facteur important et les essais pendant la transformation martensitiques montrent que la ténacité critique peut être inférieure pendant celle ci à celle du matériau purement austénitique. Dans le cas du 16MND5, la ténacité est beaucoup plus faible à 600°C (et bainitique) qu’à température ambiante ce qui est assez logique. Par contre, lors du refroidissement, depuis 600° (austénitique) jusqu’à la température ambiante (bainitique), nous avons obtenu une ténacité critique relativement constante. En conclusion, cette étude apporte une solution quant à la mesure de la ténacité critique de matériau pendant des transformations de phases, ce que ne permettent pas forcément les essais normalisés. Pour le 15-5PH, la ténacité critique semble évoluer pendant la transformation martensitique et est assez dépendante du taux d’austénite résiduelle. Il semble par contre que pour le 16MND5, la ténacité critique soit assez peu dépendante de la fraction volumique d’austénite et la valeur obtenue varie peu au cours du refroidissement du matériau depuis 600°C. / Ou study focuses on the effects of phase transformations on crack propagation. We want to understand the changes of fracture toughness during welding. In this work, fracture toughness is expressed by J-integral. There are many experimental methods to obtain the critical toughness JIC but they are impractical for our investigation during phase transformation. That is the reason why we have proposed a method coupling mechanical tests, digital image correlation and finite element simulation. The fracture tests are implemented on pre-cracked single edge notched plate sample which is easy for machining and heat conduct during phase transformation. The tests are conducted at different temperatures until rupture. Digital image correlation gives us the displacement information on every sample. Each test is then simulated by finite element where the fracture toughness is evaluated by the method G-Theta at the crack propagation starting moment found by potential drop method and digital image correlation technical. Two materials have been studied, 15Cr-5Ni martensitic precipitation hardening stainless steel and 16MND5 ferritic low carbon steel. For these two materials, different test temperatures were chosen before, during and after phase transformation for testing and failure characterization of the mechanical behavior. Investigation result shows that metallurgical phase transformation has an influence on fracture toughness and further crack propagation. For 15-5PH, the result of J1C shows that the as received 15-5PH has higher fracture toughness than the one at 200°C. The toughness is also higher than the original material after one cycle heat treatment probably due to some residual austenite. Meanwhile, pure austenite 15-5PH at 200°C has higher fracture toughness than pure martensitic 15-5PH at 200°C. For 16MND5, the result also proves that the phase transformation affects fracture toughness. The as received material has bigger J1C than the situation where it was heated to 600°C. On the other hand, the material at 600°C just before isothermal bainite transformation after the austenitization during cooling process also has higher fracture toughness than the one at 600°C before austenitization. These two conclusions are consistent well with the result of 15-5PH. But the final situation of 16MND5 after one cycle heat treatment has a slightly smaller J1C than the receiving situation. It means that one cycle heat treatment hasn't an significant influence on 16MND5fracture toughness. Conclusions show that one should pay attention to the heating period before austenitization of the substrate material when people do the welding as the higher temperature will bring the lower fracture toughness during this process. While during cooling period, the fracture toughness doesn't change a lot during, before or after the cooling induced phase transformation. Even for 15-5PH, it has a better fracture toughness after the martensite transformation than before.

Lors de l’usinage, les conditions de pression et de température à la surface usinée sont trèsélevées. La microstructure et l’état mécanique du matériau sont impactés, ce qui a desconséquences sur la réactivité chimique de la surface usinée. Dans cette thèse, ons’intéresse au tournage de superfinition de l’acier inoxydable martensitique X4CrNiMo16-5-1traité thermiquement (dénommé APX4 optimisé). Il présente la particularité d’êtremultiphasé à la température ambiante (martensite, ferrite et austénite). L’objectif est dequantifier les relations entre les conditions de coupe, les propriétés d’usage et ladégradation par corrosion des surfaces usinées. Des essais d’usinage en coupe orthogonale(type QST) ont été réalisés afin de comparer directement les résultats expérimentaux auxprédictions numériques 2D des surfaces usinées.Les changements de phase du matériau ont été étudiés par des essais de calorimétriejusqu’à 1200°C. Les cycles thermiques réalisés ont mis en évidence différentestransformations métallurgiques. L’étude bibliographique complémentaire permet deconclure quant aux possibilités de transformation de phase en usinage, qui sont quasiinexistantes du fait des cinétiques de chauffage extrêmement élevées en tournage.Les échantillons usinés ont été caractérisés avec une étude microstructurale parmicrographie optique et par MEB-EBSD. Ces deux techniques mettent en évidence lesdéformations importantes en extrême surface indiquées par l’étirement des îlots de ferriteparallèlement à la surface usinée. Ces résultats microstructuraux ont été mis en relationavec les résultats de microdureté Vickers. Une relation de la dureté superficielle a étéexprimée en fonction des conditions de coupe. La technique EBSD a permis de montrer pourles échantillons usinés dans les conditions les plus sévères la déformation de la ferrite avecapparition de sous-joints de grain, un affinement microstructural de la martensite et uneaccentuation de l’affinement de la matrice martensitique à proximité de la ferrite déformée.Une simulation numérique de prédiction des déformations à l’échelle macroscopiquea été réalisée. Ces résultats numériques ont été comparés aux résultats de déformation etde microdureté issus d’une campagne d’essais. Des essais numériques complémentairesappliqués à l’échelle de la microstructure (matériau considéré biphasé) permettent ded’appréhender la déformation de la phase ferritique et son influence locale sur ladéformation de la matrice martensitique. Ces résultats sont cohérents avec les résultatsexpérimentaux.Les phénomènes de corrosion par piqûres ont été étudiés par le biais d’essais depolarisation à l’aide de la microcellule électrochimique et d’essais spécifiques pulsés. Cesderniers essais ont permis l’analyse des piqûres générées (en diamètre et en densité). Larésistance à la corrosion localisée des surfaces d’acier inoxydable martensitique reste bonneaprès usinage, même améliorée (densité de piqûres plusieurs fois plus faible que l’état deréférence). Ce comportement est corroboré à l’état de compression de la surface.La microdureté de surface, qui est contrôlée majoritairement par l’avance, conditionne lepotentiel de piqûre. L’augmentation du diamètre de piqûre a été reliée à l’affinementmicrostructural (observé à partir d’un certain seuil de microdureté superficielle). / During machining, pressure and temperature conditions at the machined surface are veryintensive. Machined material microstructure and mechanical state are changed, whichimpacts the chemical reactivity of the machined surface. In this PhD study, we focus onsuperfinish turning of heat treated martensitic stainless steel X4CrNiMo16-5-1 (namedoptimized APX4). It has to be mentioned that this material has a multiphased microstructureat ambient temperature (martensite, ferrite and austenite). The aim is then to quantifyrelationships between cutting conditions, properties and the deterioration (corrosion) ofmachined surfaces. Machining trials in orthogonal cutting configuration (QST) have beenrealized in order to compare experimental results directly to 2D numerical forecast ofmachined surfaces.Material phase transformations have been studied by calorimetry tests until 1200°C. Testshave evidenced different metallurgical transformations. The complementary bibliographystudy allows to conclude that phase transformation possibilities during machining are veryquasi nonexistent due to extremely high heating kinetics in turning.Machined samples have been characterized by a microstructural study by opticalmicrography and SEM-EBSD. Both techniques highlight high strains in extreme machinedsurface as indicated by the stretching of ferrite islands in parallel to the machined surface.Microstructural results have been linked to the Vickers microhardness results. Surfacehardness has been expressed as a function of the cutting conditions.EBSD measurements have shown for machined samples in the most severe conditionsstraining of the ferrite with low angle grain boundaries, microstructural refining ofmartensite and heightening of martensitic matrix close to the strained ferrite.A numerical simulation predicting strains at the macroscopic scale has been carried out.These numerical results have been compared to strain and microhardness results arise fromone trials campaign. Further numerical simulations applied at the microstructure level(considered as biphased material) allow understanding of ferritic phase strain and its localinfluence on martensitic matrix strain. These results are consistent with experimentalresults.Pitting corrosion phenomenon has been studied by polarization testing using theelectrochemical microcell and specific pulsed testing. Last used method has been conductedto analyze the generated pits (diameter and density). Localized corrosion resistance ofmachined martensitic stainless steel surfaces remains good, even improved (few times lowerpitting density than the reference state). This behaviour is corroborated to the compressivestate of the surface.Surface microhardness, which is mainly controlled by the feed rate, conditions the criticalpitting potential. Increased pitting diameter has been linked to microstructural refining(observed above a surface microhardness level).

Cíle této práce jsou: (i) vyhodnocení vlivu Y2O3 kelímku na kontaminaci indukčně tavené NiTi slitiny obohacené niklem, (ii) optimalizace podmínek, při kterých jsou tavby uskutečněny a (iii) získání nových DSC a 3D AP dat o vlivu vodíkové atmosféry na martenzitickou transformaci a na strukturu NiTi slitin obohacené niklem s tvarovou pamětí. Byly provedeny následující experimenty: – Pět taveb bylo navrženo a provedeno tak, aby byla snížena maximální tavící teplota. – Pět přetaveb bylo uskutečněno při teplotě 1500 C s dobou výdrže 2, 10 a 20 minut a při teplotách 1450 C a 1550 C s 20 minutovou dobou výdrže. Experiment byl navržen tak, aby byl vyšetřen vliv tavící teploty a doby výdrže na obsah kyslíku pocházejícího z kelímku Y2O3 v tavenině. – Tepelné zpracování NiTi slitiny obohacené niklem v režimu I (žíhání) a v režimu II (kombinace žíhání se stárnutím) pod atmosférou vodíku, směsi vodíku s héliem a pod referenční atmosférou čistého hélia. Získané výsledky jsou: – Navržené tavící postupy vedou ke snížení maximální tavící teploty a to z 1800 C na 1400 C. Přesto toto velké snížení maximální tavící teploty nevedlo k významnému poklesu obsahu kyslíku. – Během přetavby uskutečněné při teplotě 1500 C s dobou výdrže 2 minuty se obsah kyslíku navýšil o trojnásobek jeho počáteční hodnoty a příliš se nelišil od obsahu kyslíku naměřeného ve slitině, která byla přetavena při stejné teplotě s dobou výdrže 10 minut. K nárustu o čtyřnásobek počáteční hodnoty obsahu kyslíku došlo u přetavby vedené na teplotě 1450 C po dobu 20 minut a hodnota obsahu kyslíku se příliš nelišila od hodnoty naměřené ve slitině přetavené při teplotě 1550 C se stejnou dobou výdrže. – S rostoucím parciálním tlakem vodíku dochází k potlačení jednokrokové martenzitické transformace. Významný pokles výšky DSC píku nastává při parciálním tlaku 100 mbar. 3D AP analýza odhalila, že nedochází k žádné lokální změně koncentrace a nebo pozic niklových a titanových atomů ve vzorku, který byl žíhán v režimu I ve vodíku. Bylo objeveno, že vodík tvoří stabilní intersticiální tuhý roztok v NiTi B2 mřížce, kde vytváří systém nanodomén s obsahem vodíku vyšší než 10 at%.

<p align='justify'>This thesis is devoted to the micromechanical study of the size-dependent strengthening in Transformation Induced Plasticity (TRIP) steels. Such grades of advanced high-strength steels are compelling for the automotive industry, due to their improved mechanical properties. Among others, they combine a good strength versus ductility balance. In this context, many research works have been carried out to study these grades of steels. In particular, from a numerical point of view, earlier studies within the framework of classical plasticity do not properly reproduce the strengthening levels characterizing TRIP steels and obtained experimentally.</p> <p><p align='justify'>In this study, the strain gradient plasticity theory presented by Fleck and Hutchinson (2001) is chosen to account for the strengthening effect resulting from the phase transformation. A two-dimensional embedded cell model of a simplified microstructure composed of small cylindrical metastable austenitic inclusions, partially undergoing the phase transformation, within a ferritic matrix is used.</p><p><p align='justify'>First, the single-parameter version of the strain gradient plasticity theory under small strain assumption is used for the simulations. The impact of the higher order boundary conditions is assessed. It is shown that, when the plastic flow is unconstrained at the elasto-plastic boundaries, the transformation strain has no significant impact on the overall strengthening. The strengthening is essentially coming from the composite effect with a marked inclusion size effect resulting from the appearance during deformation of new boundaries (at the interface between parent and product phases) constraining the plastic flow.</p><p><p align='justify'>Second, the multi-parameter version of the strain gradient plasticity theory, incorporating separately the rotational and extensional gradients in the formulation, is employed under small strain assumption. The effect of the plastic strain gradients resulting from the transformation strain is better captured. In particular, the results show a significant influence of the shear component of the transformation strain. An implicit confinement effect is revealed at the elasto-plastic boundaries which is partly responsible for the transformation strain effect. Size effects on the overall strengthening are also revealed, due to a combined size dependent effect of the transformation strain and of the evolving composite structure.</p><p align='justify'>Third, the extension of the strain gradient plasticity theory to a finite strain description is applied. A significant effect of the transformation strain is obtained with the multi-parameter version of the theory as well as an optimal austenite grain size improving the damage resistance of the martensite, in agreement with the typical grain size of the current TRIP-assisted steels (Jacques et al. 2007).</p> / Doctorat en Sciences de l'ingénieur / info:eu-repo/semantics/nonPublished

Introduction: One of the key prerequisites of high-quality endodontic treatment is the use of endodontic NiTi instruments for the preparation of root canals. The purpose of this dissertation is to evaluate the effect of individual factors which influence the life of endodontic instruments during the clinical treatment of root canals. The dissertation will evaluate the effect the curvature of the canals, the shape of the tip of the instrument, the speed and type of rotation, and the influence of sterilization. The effect of low-temperature plasma nitriding on the fatigue life of the instruments will also be investigated. Materials and methods: Several endodontic systems used for the machine preparation of root canals were studied. The study focused predominantly on the cyclic fatigue of rotary endodontic instruments, wherein the files were rotated in artificial curved root canals. Additionally, the influence of sterilization on the life of the instruments was also examined. Finally, the instruments were treated using thermal plasma nitridation for the purpose of improving their properties. The instruments were then analyzed using a scanning electron microscope and a microhardness meter. Results: Testing cyclic fatigue in artificial root canals with radii R3 and R5 revealed that instruments with a...

Deformation phenomena in shape memory alloys involve stress-, temperature-induced phase transformations and crystallographic variant conversion or reorientation, equivalent to a twinning operation. In near equiatomic NiTi, Ti rich compositions can exist near room temperature as a monoclinic B19' martensitic phase, which when deformed undergoes twinning resulting in strains as large as 8%. Upon heating, the martensite transforms to a cubic B2 austenitic phase, thereby recovering the strain and exhibiting the shape memory effect. Ni rich compositions on the other hand can exist near room temperature in the austenitic phase and undergo a reversible martensitic transformation on application of stress. Associated with this reversible martensitic transformation are macroscopic strains, again as large as 8%, which are also recovered and resulting in superelasticity. This work primarily focuses on neutron diffraction measurements during loading at the Los Alamos Neutron Science Center at Los Alamos National Laboratory. Three phenomena were investigated: First, the phenomena of hysteresis reduction and increase in linearity with increasing plastic deformation in superelastic NiTi. There is usually a hysteresis associated with the forward and reverse transformations in superelastic NiTi which translates to a hysteresis in the stress-strain curve during loading and unloading. This hysteresis is reduced in cold-worked NiTi and the macroscopic stress-strain response is more linear. This work reports on measurements during loading and unloading in plastically deformed (up to 11%) and cycled NiTi. Second, the tension-compression stress-strain asymmetry in martensitic NiTi. This work reports on measurements during tensile and compressive loading of polycrystalline shape-memory martensitic NiTi with no starting texture. Third, a heterogeneous stress-induced phase transformation in superelastic NiTi. Measurements were performed on a NiTi disc specimen loaded laterally in compression and associated with a macroscopically heterogeneous stress state. For the case of superelastic NiTi, the experiments related the macroscopic stress-strain behavior (from an extensometer or an analytical approach) with the texture, phase volume fraction and strain evolution (from neutron diffraction spectra). For the case of shape memory NiTi, the macroscopic connection was made with the texture and strain evolution due to twinning and elastic deformation in martensitic NiTi. In all cases, this work provided for the first time insight into atomic-scale phenomena such as mismatch accommodation and martensite variant selection. The aforementioned technique of neutron diffraction for mechanical characterization was also extended to engineering components and focused mainly on the determination of residual strains. Two samples were investigated and presented in this work; first, a welded INCONEL 718 NASA space shuttle flow liner was studied at 135 K and second, Ti-6Al-4V turbine blade components were investigated for Siemens Westinghouse Power Corporation. Lastly, also reported in this dissertation is a refinement of the methodology established in the author's masters thesis at UCF that used synchrotron x-ray diffraction during loading to study superelastic NiTi. The Los Alamos Neutron Science Center is a national user facility funded by the United States Department of Energy, Office of Basic Energy Sciences, under Contract No. W-7405-ENG-36. The work reported here was made possible by grants to UCF from NASA (NAG3-2751), NSF CAREER (DMR-0239512), Siemens Westinghouse Power Corporation and the Space Research Initiative.

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