Nucleation of dislocation loop at the crack tip in a material subjected to uniaxial loading is investigated. Analytical expression for the total energy of rectangular dislocation loop at the crack tip is found. Depencence of the nucleation energy barrier on dislocation loop shape and stress intensity factor at the crack tip is determined. It is established that the energetic barrier for nucleation of dislocation loop strongly depends on the stress intensity factor. Nucleation of dislocation loop is very sensitive to stress field modifiers (forest dislocations, precipitates, clusters of point defects, etc.) in the crack tip vicinity.

Nucleation of dislocation loop at the crack tip in a material subjected to uniaxial loading is investigated. Analytical expression for the total energy of rectangular dislocation loop at the crack tip is found. Depencence of the nucleation energy barrier on dislocation loop shape and stress intensity factor at the crack tip is determined. It is established that the energetic barrier for nucleation of dislocation loop strongly depends on the stress intensity factor. Nucleation of dislocation loop is very sensitive to stress field modifiers (forest dislocations, precipitates, clusters of point defects, etc.) in the crack tip vicinity.

Nous avons étudié la sensibilité du T91 à la fragilisation par le sodium liquide. Une procédure expérimentale a été mise en place afin de procéder à des essais mécaniques en sodium sous atmosphère inerte. Grâce à l’introduction d’une étape préliminaire d’exposition au sodium, la mouillabilité du T91 par le sodium liquide et la structure de l’interface sodium/acier ont pu être étudiés en fonction des différents paramètres d’exposition. Une réduction significative des propriétés mécaniques est observée quand le mouillage de l’acier par le sodium est bon. L’utilisation de différentes teneurs en oxygène et en hydrogène suggère que l’oxygène joue un rôle primordial dans l’amélioration de la mouillabilité du T91. La sensibilité du phénomène de fragilisation à la vitesse de sollicitation et à la température a été caractérisée. A partir de ces résultats, l’existence d’une transition fragile/ductile, fonction de ces deux paramètres a été mis en évidence. L’étude de cette transition suggère qu’une étape de diffusion du sodium dans les joints de grains du T91 est limitante pour la fragilisation. Des analyses en microscopie électronique en transmission et par cartographies d’orientation de fissures arrêtées ont également permis de constater que le mode de rupture est interlatte ou intergranulaire, fournissant ainsi une image cohérente du processus de fragilisation. La même méthodologie a été appliquée à l’acier non allié XC10. Les résultats montrent un comportement en tous points similaire à celui de l’acier T91 et suggèrent donc un mécanisme commun pour les aciers cubiques centrés. De plus, ils confirment que la transition fragile ductile observée semble la conséquence d’une vitesse de propagation de fissure fragile relativement limitée. Cette propagation est activée thermiquement avec une énergie d’activation d’environ 50 kJ/mol. Enfin, il a été montré que l’acier austénitique 304L est également sensible à la fragilisation par le sodium liquide. Certaines surfaces de rupture témoignent clairement d’une rupture intergranulaire, cependant des interrogations persistent à propos du chemin de fissuration. / We studied the sensitivity of T91 steel to embrittlement by liquid sodium. An experimental procedure was set up to proceed to mechanical testing in sodium under an inert atmosphere. The introduction of a liquid sodium pre-exposure step prior to mechanical testing enabled the study of both the wettability of T91 by sodium and the structure of the sodium steel/interface as a function of the exposure parameters. The mechanical properties of T91 steel are significantly reduced in liquid sodium provided the wetting conditions are good. The use of varying oxygen and hydrogen concentrations suggests that oxygen plays a major role in enhancing the wettability of T91. The sensitivity of the embrittlement to strain rate and temperature was characterized. These results showed the existence of a ductile to brittle transition depending on both parameters. Its characterization suggests that a diffusion step is the limiting rate phenomenon of this embrittlement case. TEM and EBSD analysis of arrested cracks enabled us to establish that the fracture mode is interlath or intergranular. This characteristic is coherent with the crack path commonly reported in liquid metal embrittlement. A similar procedure was applied to the unalloyed XC10 steel. The results show a behavior which is similar to the one of T91 steel and suggest a common mechanism for liquid sodium embrittlement of body centered cubic steels. Moreover, they confirm that the ductile to brittle transition seems associated with a limited crack propagation rate. The propagation is thermally activated with activation energy of about 50 kJ/mol. Finally, it was shown that 304L austenitic steel is sensitive to liquid sodium embrittlement as well. Some fracture surfaces testify of an intergranular fracture mode, but some questions still remain about the crack path.

<p>U disertaciji je izvršena karakterizacija mikrostrukture i mehaničkih osobina<br />nelegiranog austemperovanogi nodularnog liva (ADI materijala), kao i uticaja<br />mikrostrukture na prelaznu temperaturu u intervalu od -196 do +100&deg;C.<br />Utvrđeno je da mehaničke osobine ADI-ja zavise od morfologije ausferitne<br />mikrostrukture i količine zadržanog austenita, tj. parametara austemperovanja.<br />Na osnovu mehaničkih osobina utvrđen je i opseg procesiranja u skladu sa<br />standardima ASTM, ISO i EN. Zaključeno je da prelazna temperatura ADI<br />materijala zavisi od količine i stabilnosti zadržanog austenita. U višem<br />temperaturnom opsegu (iznad cca. -25&deg;C) dominantna je količina zadržanog<br />austenita, dok na nižim temperaturama, stabilnost. Visoka obogaćenost<br />ugljenikom, stabilnog zadržanog austenita sprečava stvaranje martenzita na<br />niskim temperaturama, a time i pojavu krtosti kod ADI-ja.</p> / <p>The object of this thesis was to characterize microstructure and mechanical properties<br />of the unalloyed ADI material (Austempered Ductile Iron). In addition, the influence of<br />microstructure on the ductile to brittle transition temperature (DBTT) by Charpy impact<br />test in temperature interval from 196 to +100&deg;C has been studied. The all properties<br />obtained depend on the morphology of microstructure and the amount of retained<br />austenite, i.e. on the austempering parameters. According to the mechanical properties<br />and standard requirements (ASTM, ISO and EN) the processing window has been<br />proposed, also. It was found that DBTT is influenced by amount and stability of retained<br />austenite. In upper temperature range (above cca. 25&deg;C) the most influence factor on<br />DBTT is amount of retained austenite, while at the lower temperatures the stability is<br />more prominent. Stability of high carbon retained austenite at lower temperatures<br />prevents transformation to martensite and thus the embrittlement of ADI.</p>

Em projetos de oleodutos e gasodutos utilizam-se aços de alta resistência e baixa liga (ARBL), como o aço API 5L X80. Na soldagem multipasse destas tubulações, a zona afetada pelo calor (ZAC) do passe de raiz é submetida a um novo ciclo térmico pelos passes de soldagem subsequentes. Isto resulta em alterações nos valores das propriedades físicas. Nos aços ARBL, a ZAC de grãos grosseiros reaquecida intercriticamente (IC-ZACGG) pode se tornar uma zona frágil localizada, isto é, uma zona com maior dureza. Consequentemente, falhas estruturais podem ocorrer, ocasionando paradas não desejadas no transporte de fluidos. O objetivo deste trabalho é desenvolver uma metodologia baseada no modelo de fontes de calor distribuídas de Mhyr e Gröng, para avaliar o fluxo de calor na soldagem considerando as propriedades físicas dependentes da temperatura. Estender a aplicação desta ferramenta em soldagens multipasses para identificar sub-regiões da ZAC de um passe anterior sendo afetada pela ZAC de passes subsequentes. As isotermas simuladas foram validadas através de medições realizadas em macrografias de juntas soldadas. Os ciclos térmicos simulados foram validados através das temperaturas máximas atingidas e pelos tempos de resfriamento de 800 a 500 ºC (?t8-5) dos ciclos térmicos experimentais. Ao aplicar a metodologia proposta, foi possível delimitar com acurácia as regiões reaquecidas da ZAC e analisar os efeitos dos passes subsequentes em cada uma das sub-regiões da ZAC do passe de raiz. A IC-ZACGG na região do passe de raiz foi localizada, mas não se comportou como zona frágil devido à boa soldabilidade do aço API 5L X80 comprovada pelos ensaios de dureza e de tenacidade ao impacto Charpy-V. / In pipelines projects, the high strength low alloy (HSLA) steels are used, such as the API 5L X80 steel. During the multipass welding of these pipes, the heat affected zone (HAZ) of the root pass is subjected to a new thermal cycle by the subsequent welding passes. This results in changes in the values of the physical properties. In the HSLA steels, the intercritical reheated coarse-grained heat-affected zone (IR-CGHAZ) can become a local brittle zone, that is, a region with greater hardness. Consequently, structural failures could happen, causing undesired shutdowns in fluid transportation. The objective of this work is to develop a methodology based on the distributed heat sources model of Mhyr and Gröng, to evaluate the heat flux in the welding considering the temperature-dependent physical properties. Extend the application of this tool in multipass welds to identify HAZ subregions of a previous pass being affected by the HAZ of subsequent passes. The simulated isotherms were validated through measurements made on macrographs of welded joints. The simulated thermal cycles were validated through the maximum temperatures reached and the cooling times from 800 °C to 500 ºC (?t8-5) of the experimental thermal cycles. By applying the proposed methodology, it was possible to accurately delimit reheated HAZ regions and analyze the effects of subsequent passes in each of the root pass HAZ subregions. The IRCGHAZ in the root pass region was localized, but it did not behave as a brittle zone due to the good weldability of the API 5L X80 steel as proven by the hardness and Charpy-V impact tests.

En esta tesis se ha caracterizado el acero, virgen e irradiado, de la vasija de una central nuclear española actualmente en servicio, en la región de temperaturas conocida como Zona de Transición Dúctil-Frágil. Para ello, se han ensayado probetas propias de la Mecánica de Fractura, reconstruidas a partir de mitades de probetas de impacto previamente ensayadas. Para describir la tenacidad a fractura en la Zona de Transición se ha empleado el modelo de la Curva Patrón.Finalmente, se ha analizado el impacto del procedimiento de caracterización y del modelo de la Curva Patrón sobre la Integridad Estructural de la vasija, comparando sus predicciones con las que se obtienen de aplicar los procedimientos convencionales que contempla la normativa vigente, representada por el Código ASME. En esta comparación se ha hecho uso del procedimiento FITNET de Integridad Estructural. / In this thesis, the steel, virgin and irradiated, from the vessel of a Spanish Nuclear Plant currently operating, has been characterized in the range of temperatures known as Ductile to Brittle Transition Region. For this purpose, Fracture Mechanics specimens, reconstituted from halves of impact specimens previously broken, have been tested. To describe fracture toughness in the Transition Region, the Master Curve method has been used.Eventually, the influence of the characterization procedure together with the Master Curve method on the Structural Integrity of the vessel has been analyzed, comparing their predictions with those coming from applying conventional procedures proposed by the current regulations, represented by the ASME Code. In this comparison, the FITNET Structural Integrity procedure has been used.

Em projetos de oleodutos e gasodutos utilizam-se aços de alta resistência e baixa liga (ARBL), como o aço API 5L X80. Na soldagem multipasse destas tubulações, a zona afetada pelo calor (ZAC) do passe de raiz é submetida a um novo ciclo térmico pelos passes de soldagem subsequentes. Isto resulta em alterações nos valores das propriedades físicas. Nos aços ARBL, a ZAC de grãos grosseiros reaquecida intercriticamente (IC-ZACGG) pode se tornar uma zona frágil localizada, isto é, uma zona com maior dureza. Consequentemente, falhas estruturais podem ocorrer, ocasionando paradas não desejadas no transporte de fluidos. O objetivo deste trabalho é desenvolver uma metodologia baseada no modelo de fontes de calor distribuídas de Mhyr e Gröng, para avaliar o fluxo de calor na soldagem considerando as propriedades físicas dependentes da temperatura. Estender a aplicação desta ferramenta em soldagens multipasses para identificar sub-regiões da ZAC de um passe anterior sendo afetada pela ZAC de passes subsequentes. As isotermas simuladas foram validadas através de medições realizadas em macrografias de juntas soldadas. Os ciclos térmicos simulados foram validados através das temperaturas máximas atingidas e pelos tempos de resfriamento de 800 a 500 ºC (?t8-5) dos ciclos térmicos experimentais. Ao aplicar a metodologia proposta, foi possível delimitar com acurácia as regiões reaquecidas da ZAC e analisar os efeitos dos passes subsequentes em cada uma das sub-regiões da ZAC do passe de raiz. A IC-ZACGG na região do passe de raiz foi localizada, mas não se comportou como zona frágil devido à boa soldabilidade do aço API 5L X80 comprovada pelos ensaios de dureza e de tenacidade ao impacto Charpy-V. / In pipelines projects, the high strength low alloy (HSLA) steels are used, such as the API 5L X80 steel. During the multipass welding of these pipes, the heat affected zone (HAZ) of the root pass is subjected to a new thermal cycle by the subsequent welding passes. This results in changes in the values of the physical properties. In the HSLA steels, the intercritical reheated coarse-grained heat-affected zone (IR-CGHAZ) can become a local brittle zone, that is, a region with greater hardness. Consequently, structural failures could happen, causing undesired shutdowns in fluid transportation. The objective of this work is to develop a methodology based on the distributed heat sources model of Mhyr and Gröng, to evaluate the heat flux in the welding considering the temperature-dependent physical properties. Extend the application of this tool in multipass welds to identify HAZ subregions of a previous pass being affected by the HAZ of subsequent passes. The simulated isotherms were validated through measurements made on macrographs of welded joints. The simulated thermal cycles were validated through the maximum temperatures reached and the cooling times from 800 °C to 500 ºC (?t8-5) of the experimental thermal cycles. By applying the proposed methodology, it was possible to accurately delimit reheated HAZ regions and analyze the effects of subsequent passes in each of the root pass HAZ subregions. The IRCGHAZ in the root pass region was localized, but it did not behave as a brittle zone due to the good weldability of the API 5L X80 steel as proven by the hardness and Charpy-V impact tests.

La bonne ténacité des aciers pour gazoducs aux basses températures est nécessaire pour éviter la propagation de fissures de manière catastrophique. Cette étude vise à améliorer la compréhension physique et l'évaluation quantitative du comportement à rupture des aciers pour gazoducs laminés à chaud, en nous intéressant plus particulièrement aux températures au pied de la transition ductile-fragile .La résilience de ces aciers est généralement validée à l'aide d'essais dits drop weight tear tests (DWTT), après lesquels le faciès de rupture doit contenir moins de 15% de zone fragile. Pour les aciers mis en forme par laminage thermomécanique (TMCP), des ruptures fragiles hors plan, comme le délaminage (qui se propage dans le plan de laminage de la tôle), et la rupture fragile en biseau le long des plans dits thêta (inclinés de 40° autour de la direction de laminage par rapport au plan de laminage) apparaissent dans la transition ductile-fragile. Ces modes de rupture, observés lors des essais de résilience (DWTT, Charpy) et de ténacité (CT), affectent la résistance à la rupture de ces aciers.L'anisotropie de l'écoulement plastique, puis celle de la sensibilité à la rupture par clivage ont été caractérisées en fonction de la température, à l'aide d'essais de traction sur des éprouvettes lisses et entaillées conçues pour cette étude. L'analyse mécanique de ces essais à l'aide de calculs par éléments finis a permis de déterminer des contraintes critiques de clivage dans les directions perpendiculaires au plan de laminage et aux plans thêta. Les valeurs obtenues dans ces directions sont de 25% inférieures à celles correspondant aux directions de laminage et travers long.L'anisotropie de la contrainte critique de clivage a été quantitativement corrélée à l'anisotropie de microtexture du matériau. Des entités appelées « facettes de clivage potentielles » ont été définies et mesurées dans cette étude, comme des régions contenant un plan {100} défavorablement orienté et dans lesquelles les fissures de clivage se propagent sans être arrêtées. Par exemple, un plan contenant 20% de facettes de clivage potentielles aurait une contrainte critique de clivage de 20% moins élevée qu'un plan présentant seulement 10% de facettes de clivage potentielles.La taille et la forme de ces facettes de clivage potentielles évoluent avec la déformation plastique. Par conséquent, la contrainte critique de clivage est affectée par l'historique de déformation. Dans le cas du délaminage, les facettes de clivage potentielles s'allongent au cours d'un chargement dans la direction travers long, conduisant à une augmentation de leur taille effective et par conséquent à une diminution (qui peut atteindre 30%) de la contrainte critique de clivage dans le plan de la tôle. Cette diminution facilite in fine l'apparition du délaminage. De plus, la présence de micro-fissures ductiles facilite la rupture par délaminage en modifiant l'état de contrainte local. Un critère a ainsi été proposé pour prédire numériquement l'amorçage du délaminage dans des éprouvettes de traction et/ou de résilience Charpy.L'application de cette approche à des échantillons traités thermiquement et à des échantillons pré-déformés a montré que la sensibilité au délaminage pouvait être contrôlée en modifiant la texture locale initiale du matériau. / High toughness of pipeline steels at low temperature is required to avoid catastrophic propagation of brittle crack. The aim of the study is to improve physical understanding and quantitative assessment of the toughness behavior of hot-rolled pipeline steels, focusing on the lower part of the ductile to brittle transition temperature range.The impact toughness of these steels is commonly validated using drop weight tear tests (DWTT), on the basis of fracture surfaces that must exhibit less than 15% of brittle fracture appearance. In thermomechanical control processed steels, brittle out-of-plane cracks such as delamination (which propagates along the rolling plane), and brittle tilted fracture (BTF) along theta-planes (tilted around RD by 40° with respect to rolling plane), have been characterized in the ductile to brittle transition temperature range, for both industrial (DWTT) and laboratory Charpy impact tests. In both cases, as well as in fracture toughness tests, such brittle out-of-plane cracking has been shown to impair the impact toughness.The anisotropy in plastic flow and sensitivity to cleavage fracture has been characterized as a function of temperature, by using tensile tests on specifically designed smooth and notched specimens. From finite element mechanical analysis of these tests, critical cleavage stresses normal to the rolling plane and the theta-plane are considerably lower (around 25%) than for planes normal to the rolling and transverse directions.The anisotropy in critical cleavage stress has been quantitatively correlated to microtexture anisotropy. So-called “potential cleavage facets” have been defined and measured in this study, as regions with unfavorably oriented {100} planes, which are taken as unit crack paths for cleavage propagation. A sample containing 20% of potential cleavage facets had a critical cleavage stress 20% lower than a sample with only 10% of potential cleavage facets.The size and shape of these potential cleavage facets evolve during plastic deformation. Therefore, the critical cleavage stress was found to be affected by plastic strain history. In the case of delamination, potential cleavage facets along the rolling plane were elongated during loading, their area was increased and the corresponding critical cleavage stress decreased by around 30% with respect to the undeformed case. This made delamination cracking easier. Moreover, the presence of a ductile crack at the initiation site of delamination locally modified the stress state and also facilitated delamination occurrence. A criterion has been developed to numerically predict the onset of delamination in tensile and Charpy specimens.Application of this approach to heat-treated and to prestrained specimens eventually showed that it was possible to modify the sensitivity to delamination by strongly modifying the initial microtexture anisotropy.

No description available.

The effect of Laves phase (Fe2Nb) formation on the Charpy impact toughness of the ferritic stainless steel type AISI 441 was investigated. The steel exhibits good toughness after solution treatment at 850°C, but above and below this treatment temperature the impact toughness decreases sharply. With heat treatment below 850°C the presence of the Laves phase on grain boundaries and dislocations plays a significant role in embrittlement of the steel whereas above that temperature, an increase in the grain size from grain growth plays a major role in the impact embrittlement of this alloy. The toughness results agree with the phase equilibrium calculations made using Thermo–Calc® whereby it was observed that a decrease in the Laves phase volume fraction with increasing temperature corresponds to an increase in the impact toughness of the steel. Annealing above 900°C where no Laves phase exists, grain growth is found which similarly has a very negative influence on the steel’s impact properties. Where both a large grain size as well as Laves phase is present, it appears that the grain size may be the dominant embrittlement mechanism. Both the Laves phase and grain growth, therefore, have a significant influence on the impact properties of the steel, while the Laves phase’s precipitation behaviour has also been investigated with reference to the plant’s manufacturing process, particularly the cooling rate after a solution treatment. The microstructural analysis of the grain size shows that there is a steady increase in grain size up to about 950°C, but between 950°C and 1000°C there is a sudden and rapid 60 % increase in the grain size. The TEM analysis of the sample that was annealed at 900°C shows that the Laves phase had already completely dissolved and cannot, therefore, be responsible for “unpinning of grain boundaries” at temperatures of 900°C and higher where this “sudden” increase in grain size was found. The most plausible explanation appears to be one of Nb solute drag that loses its effectiveness within this temperature range, but this probably requires some further study to fully prove this effect. During isothermal annealing within the temperature range of 600 to 850°C, the time – temperature – precipitation (TTP) diagram for the Laves phase as determined from the transformation kinetic curves, shows two classical C noses on the transformation curves. The first one occurring at the higher temperatures of about 750 to 825°C and the second one at much lower temperatures, estimated to possibly be in the range of about 650 to 675°C. The transmission electron microscopy (TEM) analyses show that there are two independent nucleation mechanisms that are occurring within these two temperature ranges. At lower temperatures of about 600°C, the pertaining nucleation mechanism is on dislocations and as the temperature is increased to above 750°C, grain boundary nucleation becomes more dominant. Also, the morphology of the particles and the mis-orientation with the matrix changes with temperature. At lower temperatures the particles are more needle-like in shape, but as the temperature is increased the shape becomes more spheroidal. The effect of the steel’s composition on the Laves phase transformation kinetics shows that by lowering the Nb content in these type 441 stainless steels, had no significance effect on the kinetics on precipitation of the Laves phase. However, a Mo addition and a larger grain size of the steel, retard the formation of the Laves phase, although the optimum values of both parameters still need further quantification. The calculation made for the transformation kinetics of the Laves phase, using the number density of nucleation sites No and the interfacial energy, as the fitting parameters in this work, demonstrated a reasonable agreement with experimental results. / Thesis (PhD)--University of Pretoria, 2010. / Materials Science and Metallurgical Engineering / unrestricted