Orientador: Yukio Kobayashi / Banca: Carlos Alberto Soufen / Banca: Antônio de Padua Lima Filho / Resumo: A identificação e a qualificação dos constituintes microestruturais de uma junta soldada são de grande importância pela relação que existe entre a microestrutura do cordão e as propriedades mecânicas, particularmente a tenacidade. Trabalhando com variações nos parâmetros de pulso, corrente de pico e tempo de pico, e também na temperatura de pré-aquecimento, foram quantificados os constituintes ferrita acicular e microfases presentes no metal de solda; sendo ambos considerados controladores da tenacidade. Os resultados deste trabalho demonstraram que aumentou a quantidade de ferrita acicular para os menores níveis dos parâmetros de pulso e da temperatura de pré-aquecimento. Quanto às microfases, ocorreu uma redução na quantidade à medida que se elevaram os níveis dos parâmetros de pulso e da temperatura de pré-aquecimento. Observou-se, também, qual foi a influência da velocidade de resfriamento na microestrutura final do metal de solda. Foi utilizado o processo de soldagem a arco elétrico com proteção gasosa, no modo pulsado e arame tubular. A soldagem foi realizada em chapa de aço estrutural de alta resistência e baixa liga (COS-AR 50), com chanfro em "X" e ângulo de 30º. Como metal de adição foi utilizado o arame tubular de fluxo metálico E70C-6M, com diâmetro de 1,2 mm. / Abstract: The identification and qualification of the microstructural constituents present in the welded joint are very important for the relationship between the microstructure of the weld beads with the mechanical properties, particularly toughness. Working with variations of pulse parameters, peak current and peak time, and also preheating temperature, had been quantified the constituents acicular ferrite and microphases present in weld metal; being both considered controllers of toughness. The results of this work demostrated that greater amounts of acicular ferrite had been occurred in the lowest levels of pulse parameters and preheating temperature. As for microphases, it has a reduction of the amount with the increase of pulse parameters and preheating temperature. It was observed, also, the influence of the cooling speed in the final microstructure of the weld metal. The samples were welded by the metal gas arc welding, using pulsed arc and tubular wire. As metal base was used HSLA structural steel plate (COS-AR 50), with "X"-groove and bevel angle 30º. The addition metal was the tubular metal-cored wire "E70C-6M" with diameter of 1.2 mm. / Mestre

Thinner walled (about 6 mm thickness) line pipe steels for smaller diameter pipelines tend to have a relatively high ratio of yield strength to ultimate tensile strength (YS/UTS) of 0.93 or higher. This study focused on the effect of the microstructures, prior deformation in the austenite, cooling rate, coiling simulation and the additions of some micro-alloying elements on the YS/UTS ratio of a currently produced Nb-Ti and some experimental Nb-Ti-Mo line pipe steels. The experimental research included the design of the chemical compositions for five experimental alloys, simulation of the controlled hot rolling process, the determination of the strain-free as well as the strain affected continuous cooling transformation (CCT) diagrams, phase identification and quantitative assessment of the microstructures by optical microscopy, scanning electron microscopy (SEM) and transmission electron microscopy (TEM), the latter especially on shadowed carbon extraction replicas and, tensile tests etc. This study indicated that the transformed microstructures of the alloys were a mixture of acicular ferrite plus polygonal ferrite and the volume fraction of acicular ferrite varied from 46.3 to 55.4%. Molybdenum additions did not markedly affect the formation of acicular ferrite after hot rolling and rapid cooling. The microstructural details of the acicular ferrite were successfully revealed by TEM on shadowed extraction replicas. This technique was useful to distinguish the acicular ferrite from the polygonal ferrite through a more smooth surface relief after etching in 2% Nital of the little etched polygonal ferrite whereas the deeper etched acicular ferrite showed parallel sets of internal striations. This made it possible to measure the volume fraction of acicular ferrite in the mixed microstructures of acicular ferrite and polygonal ferrite. The continuous cooling transformation behaviors of two alloys with no molybdenum and with 0.22% Mo were constructed with no prior deformation as well as with prior deformation of the austenite. Molybdenum additions shifted the strain-free CCT diagram towards longer times and expanded the region in which acicular ferrite formed from a cooling rate range of 0.3 to 5 ºCs-1 (Mo-free) to 0.1 to 15 ºCs-1 (with 0.22% Mo). However, its effect was significantly overshadowed by prior deformation in the austenite. The strain affected CCT diagrams for both alloys appear to be similar. The prior deformation had a stronger effect on the CCT diagram than molybdenum additions and promoted acicular ferrite formation, whereas it suppressed the formation of bainite. The prior deformation had two effects in acicular ferrite formation: it promoted nucleation and suppressed its growth and, therefore, resulted in a finer overall grain size. The effect on the YS/UTS ratio at various cooling rates ranging from 1 to 34, 51, 54 or 60 ºCs-1 was investigated in three cases: (i) without prior deformation and coiling simulation, (ii) with no prior deformation but with coiling simulation at 575 and 600 ºC and, (iii) with prior deformation of 33% reduction in the austenite below the Tnr followed by coiling simulation at 575 ºC for 1 hour. It was determined that the YS/UTS ratio was a function of the microstructure and cooling rate in the case treatment (i)) without any coiling simulation and prior deformation. The coarse bainite or acicular ferrite, which was formed at high cooling rates, raised the YS/UTS ratio under conditions of no deformation prior to the transformation. The yield strength and ultimate tensile strength also increased with an increase in cooling rate. With coiling conditions (treatment (ii)), the ratio was not sensitive to the cooling rate or the microstructure for the reference Mo-free alloy #6 because the coiling allows recovery of dislocations, thereby decreasing the difference in dislocation density that had arisen between a low and a high cooling rate. The YS/UTS ratio ranged from 0.75 to 0.8 after a simulated coiling at 575 ºC and from 0.76 to 0.78 after a coiling simulation at 600 ºC. Prior deformation (treatment (iii)) in the austenite raised the ratio from 0.81 to 0.86. However, the YS/UTS ratio was not sensitive to cooling rate after coiling at 575 ºC for 1 hour in the cases with and without prior deformation in the austenite. Deformation with a 33% reduction below the Tnr prior to the transformation increased the yield strength more than the ultimate tensile strength, leading to a high YS/UTS ratio that ranged from 0.81 to 0.86. The prior deformation, therefore, had a stronger effect on the YS/UTS ratio than the microstructure. Towards cache optimization in finite automata / Thesis (PhD (Metallurgical Engineering))--University of Pretoria, 2007. / Materials Science and Metallurgical Engineering / PhD / unrestricted

Made available in DSpace on 2014-06-11T19:24:47Z (GMT). No. of bitstreams: 0 Previous issue date: 2008-11-24Bitstream added on 2014-06-13T18:52:41Z : No. of bitstreams: 1 godoy_wl_me_bauru.pdf: 10498563 bytes, checksum: a471999a6640d177cb8963731e9bafe8 (MD5) / Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES) / A identificação e a qualificação dos constituintes microestruturais de uma junta soldada são de grande importância pela relação que existe entre a microestrutura do cordão e as propriedades mecânicas, particularmente a tenacidade. Trabalhando com variações nos parâmetros de pulso, corrente de pico e tempo de pico, e também na temperatura de pré-aquecimento, foram quantificados os constituintes ferrita acicular e microfases presentes no metal de solda; sendo ambos considerados controladores da tenacidade. Os resultados deste trabalho demonstraram que aumentou a quantidade de ferrita acicular para os menores níveis dos parâmetros de pulso e da temperatura de pré-aquecimento. Quanto às microfases, ocorreu uma redução na quantidade à medida que se elevaram os níveis dos parâmetros de pulso e da temperatura de pré-aquecimento. Observou-se, também, qual foi a influência da velocidade de resfriamento na microestrutura final do metal de solda. Foi utilizado o processo de soldagem a arco elétrico com proteção gasosa, no modo pulsado e arame tubular. A soldagem foi realizada em chapa de aço estrutural de alta resistência e baixa liga (COS-AR 50), com chanfro em X e ângulo de 30º. Como metal de adição foi utilizado o arame tubular de fluxo metálico E70C-6M, com diâmetro de 1,2 mm. / The identification and qualification of the microstructural constituents present in the welded joint are very important for the relationship between the microstructure of the weld beads with the mechanical properties, particularly toughness. Working with variations of pulse parameters, peak current and peak time, and also preheating temperature, had been quantified the constituents acicular ferrite and microphases present in weld metal; being both considered controllers of toughness. The results of this work demostrated that greater amounts of acicular ferrite had been occurred in the lowest levels of pulse parameters and preheating temperature. As for microphases, it has a reduction of the amount with the increase of pulse parameters and preheating temperature. It was observed, also, the influence of the cooling speed in the final microstructure of the weld metal. The samples were welded by the metal gas arc welding, using pulsed arc and tubular wire. As metal base was used HSLA structural steel plate (COS-AR 50), with X-groove and bevel angle 30º. The addition metal was the tubular metal-cored wire E70C-6M with diameter of 1.2 mm.

A utilização do eletrodo tubular no processo de soldagem a arco submerso leva a um aumento na produtividade com um custo relativamente baixo, pois não requer investimentos complementares em equipamentos. A mudança do eletrodo sólido para o tubular acarreta variações microestruturais no metal de solda que influenciam as propriedades mecânicas, tais como dureza, tração e tenacidade ao impacto. Este trabalho tem como objetivo principal estudar a tenacidade à fratura dinâmica do metal de solda, mostrando que o uso do eletrodo tubular diminui a propagação de trincas ao impacto, além de melhorar as propriedades de dureza e tração. Para a confecção da junta soldada foi utilizado o aço ASTM-A516 com espessura de 37,5 mm; para o metal de solda, o eletrodo sólido AWS EM12K, com diâmetro de 4,0 mm, e fluxo AWS F6A4 e o eletrodo tubular AWS E71T-5, com diâmetro de 4,0 mm, fabricado em caráter experimental, untamente com os fluxos AWS F6A4 e AWS F7A8 (Fluxo Neutro). Os ensaios de impacto, dureza e tração foram realizados em corpos de prova com e sem alívio de tensão, e o ensaio Charpy instrumentado em corpos de prova entalhados e em corpos de prova entalhados e com trinca por fadiga, nas temperaturas de 25, 200, 400 e 600OC. O metal de solda utilizando eletrodo sólido foi o que mostrou menor percentual de ferrita acicular (54%), enquanto que o utilizando eletrodo tubular e fluxo AWS F6A4 foi o que mostrou maior percentual de ferrita acicular (89%). Os ensaios de dureza mostraram uma influência do microconstituinte ferrita acicular: maior dureza para o maior percentual de ferrita acicular. Os limites de resistência e de escoamento também sofreram o efeito deste microconstituinte, apresentando maiores valores quando os percentuais de ferrita acicular foram maiores. Para a análise da tenacidade para o início de propagação da trinca foram utilizados os métodos da variação da taxa da flexibilidade elástica, o método da energia da carga máxima revisada e o método da energia da carga máxima. Foram calculados os valores de JId e de KJd (K derivado de J). Os únicos valores validados, de acordo com a norma, foram os de JId calculados pelo método da variação da taxa da flexibilidade elástica. Os resultados encontrados, utilizando este método, mostraram, à 600OC, a influência da ferrita acicular, sendo que o metal de solda com maior percentual deste microconstituinte forneceu maior valor de tenacidade. Os valores de JId utilizando o método da variação da taxa da flexibilidade elástica para os corpos de prova com trinca por fadiga ficaram próximos aos resultados encontrados quando o ensaio foi realizado em corpos de prova somente entalhados. Os resultados mostraram que a substituição do eletrodo sólido pelo tubular levou à maior tenacidade e a propriedades mecânicas superiores. / The cored wire application in the submerged arc welding process leads to a increase productivity with relative low cost, because it doesn’t require complementary investments in equipments. Changing from solid to cored wire promotes microstructural modification in the weld metal that enhances mechanical properties, such as hardness, stretching and impact toughness. The principal aim of this work is to study the dynamic fracture toughness of the weld metal. The use of cored wire reduces the impact crack propagation, as well as hardness and strength properties. The welded plate was composed of ASTM-A516 steel with 37.5 mm thickness and for making the weld metal was utilized AWS EM12K wire, with 4.0 mm diameter, and AWS F6A4 flux, and AWS E71T-5 cored wire, with 4.0 mm diameter, making in experimental mode, with AWS F6A4 and AWS F7A8 (Neutral Flux) fluxes. Impact, hardness and tensile tests were carried out in specimens with and without stress relief. The instrumented Charpy tests were carried out at notch and notch plus fatigue crack specimens, at 25, 200, 400 and 600OC temperatures. The solid wire weld metal produced 53.9% of acicular ferrite, while the cored wire weld metal and AWS F6A4 flux produced 88.8% of acicular ferrite. The hardness values were influenced by acicular ferrite and showed higher hardness for acicular ferrite higher values. Tensile strength and yield stress data suffered the same effect of this micro constituent also, they had bigger amount when the acicular ferrite percentiles were bigger. For toughness analysis to crack propagation start were utilized the compliance changing rate method, the energy revised method, and the maximum load energy method. JId and KJd (K derived of J) values were calculated according to the standards. The results met for this method had acicular ferrite influence at 600OC, where the weld metal with the biggest micro constituent had bigger toughness value. The JId values utilized the compliance changing rate method for the precracked specimen got values near to the notched specimen. The change solid wire by the cored wire had better toughness, and it gets better the other mechanical properties.

Low temperature cleavage fracture behaviour was investigated using four experimental microalloyed bainitic plate steels. The four plate samples were produced by different thermomechanical processing (TMP) schedules and had yield strengths in the range 540 - 670 MPa. Microstructures were characterized by optical microscopy (OM), scanning electron microscopy (SEM) and electron back scattered diffraction (EBSD). Quantitative data was obtained for prior austenite grain (PAG) size, volume fractions of two bainite types (conventional bainite and acicular ferrite) and EBSD 15° domain size. Charpy impact tests (using two notch orientations) were carried out over a range of temperatures. Cleavage facet sizes were measured on -196°C Charpy samples. The range of TMP schedules produced variations in PAG width, type of bainite and 15° domain size. The effects of these three microstructural features on cleavage crack propagation are discussed. Results indicate that the microstructures are controlled by i) deformation below TNR and ii) accelerated cooling rate. Domain structure reflects TMP. There is no clear correlation between domain size and cleavage facet size. / Thesis (Master, Mechanical and Materials Engineering) -- Queen's University, 2009-07-30 19:17:01.25

Abstract This research work focuses on how to improve the toughness of heat affected zones (HAZs) of low heat input welds in the case of high strength thermomechanically processed (TMCP) and recrystallization controlled rolled and accelerated cooled (RCR) plates with yield strengths of 355–500 MPa. Experimental work was aimed at the investigation of the intragranular nucleation of acicular ferrite or bainite in hot-rolled plates and the evaluation of the Charpy V and CTOD toughness of the most critical sub-zones of the weld HAZ using simulated specimens with a cooling time t8/5 = 5 s. The zones studied were the coarse grained HAZ (CGHAZ), the intercritically reheated coarse-grained HAZ (ICCGHAZ) and the intercritical HAZ (ICHAZ), the metallographical analyses consisted of microstructural investigations complemented with hardness measurements. Optical, scanning and transmission electron microscopy techniques were employed together with image and electron backscatter diffraction (EBSD) analysis. The test results showed that the toughness of the various sub-zones of the HAZ is improved by promoting intragranularly nucleated ferritic-bainitic (acicular) microstructure in both the CGHAZ and in the base plate. In this way, the sub-zones subjected to intercritical thermal cycles (the ICCGHAZ and the ICHAZ) develop evenly distributed M-A constituents between ferrite and bainite laths. These favourable microstructures can be achieved by using titanium killing or by avoiding niobium microalloying by using copper plus nickel alloying instead. In the laboratory experiments titanium killed steel, containing titanium-manganese oxide/manganese sulphide inclusions with a number density of 300–750 particles/mm2, develops a largely acicular ferritic microstructure in the base plate provided the austenite grain size is greater than about 120 μm and the cooling rate is in the range 6–11 °C/s down to 500 °C. Under plate mill conditions, no significant amount of acicular ferrite could be obtained, because it was not possible to achieve austenite grain sizes larger than about 70 μm after rolling. However, a significant fraction of acicular ferritic-bainitic microstructure was achieved in the CGHAZ, when the austenite grain size exceeded 90 μm. When achieved, a uniform distribution of M-A particles in an acicular ferritic-bainitic microstructure improves toughness. Cracks nucleate at numerous sites on M-A/ferrite boundaries or bainite packet interfaces, but they are initially arrested in the acicular matrix. Crack growth finally occurs by linking of the numerous arrested microcracks.

A utilização do eletrodo tubular no processo de soldagem a arco submerso leva a um aumento na produtividade com um custo relativamente baixo, pois não requer investimentos complementares em equipamentos. A mudança do eletrodo sólido para o tubular acarreta variações microestruturais no metal de solda que influenciam as propriedades mecânicas, tais como dureza, tração e tenacidade ao impacto. Este trabalho tem como objetivo principal estudar a tenacidade à fratura dinâmica do metal de solda, mostrando que o uso do eletrodo tubular diminui a propagação de trincas ao impacto, além de melhorar as propriedades de dureza e tração. Para a confecção da junta soldada foi utilizado o aço ASTM-A516 com espessura de 37,5 mm; para o metal de solda, o eletrodo sólido AWS EM12K, com diâmetro de 4,0 mm, e fluxo AWS F6A4 e o eletrodo tubular AWS E71T-5, com diâmetro de 4,0 mm, fabricado em caráter experimental, untamente com os fluxos AWS F6A4 e AWS F7A8 (Fluxo Neutro). Os ensaios de impacto, dureza e tração foram realizados em corpos de prova com e sem alívio de tensão, e o ensaio Charpy instrumentado em corpos de prova entalhados e em corpos de prova entalhados e com trinca por fadiga, nas temperaturas de 25, 200, 400 e 600OC. O metal de solda utilizando eletrodo sólido foi o que mostrou menor percentual de ferrita acicular (54%), enquanto que o utilizando eletrodo tubular e fluxo AWS F6A4 foi o que mostrou maior percentual de ferrita acicular (89%). Os ensaios de dureza mostraram uma influência do microconstituinte ferrita acicular: maior dureza para o maior percentual de ferrita acicular. Os limites de resistência e de escoamento também sofreram o efeito deste microconstituinte, apresentando maiores valores quando os percentuais de ferrita acicular foram maiores. Para a análise da tenacidade para o início de propagação da trinca foram utilizados os métodos da variação da taxa da flexibilidade elástica, o método da energia da carga máxima revisada e o método da energia da carga máxima. Foram calculados os valores de JId e de KJd (K derivado de J). Os únicos valores validados, de acordo com a norma, foram os de JId calculados pelo método da variação da taxa da flexibilidade elástica. Os resultados encontrados, utilizando este método, mostraram, à 600OC, a influência da ferrita acicular, sendo que o metal de solda com maior percentual deste microconstituinte forneceu maior valor de tenacidade. Os valores de JId utilizando o método da variação da taxa da flexibilidade elástica para os corpos de prova com trinca por fadiga ficaram próximos aos resultados encontrados quando o ensaio foi realizado em corpos de prova somente entalhados. Os resultados mostraram que a substituição do eletrodo sólido pelo tubular levou à maior tenacidade e a propriedades mecânicas superiores. / The cored wire application in the submerged arc welding process leads to a increase productivity with relative low cost, because it doesn’t require complementary investments in equipments. Changing from solid to cored wire promotes microstructural modification in the weld metal that enhances mechanical properties, such as hardness, stretching and impact toughness. The principal aim of this work is to study the dynamic fracture toughness of the weld metal. The use of cored wire reduces the impact crack propagation, as well as hardness and strength properties. The welded plate was composed of ASTM-A516 steel with 37.5 mm thickness and for making the weld metal was utilized AWS EM12K wire, with 4.0 mm diameter, and AWS F6A4 flux, and AWS E71T-5 cored wire, with 4.0 mm diameter, making in experimental mode, with AWS F6A4 and AWS F7A8 (Neutral Flux) fluxes. Impact, hardness and tensile tests were carried out in specimens with and without stress relief. The instrumented Charpy tests were carried out at notch and notch plus fatigue crack specimens, at 25, 200, 400 and 600OC temperatures. The solid wire weld metal produced 53.9% of acicular ferrite, while the cored wire weld metal and AWS F6A4 flux produced 88.8% of acicular ferrite. The hardness values were influenced by acicular ferrite and showed higher hardness for acicular ferrite higher values. Tensile strength and yield stress data suffered the same effect of this micro constituent also, they had bigger amount when the acicular ferrite percentiles were bigger. For toughness analysis to crack propagation start were utilized the compliance changing rate method, the energy revised method, and the maximum load energy method. JId and KJd (K derived of J) values were calculated according to the standards. The results met for this method had acicular ferrite influence at 600OC, where the weld metal with the biggest micro constituent had bigger toughness value. The JId values utilized the compliance changing rate method for the precracked specimen got values near to the notched specimen. The change solid wire by the cored wire had better toughness, and it gets better the other mechanical properties.

L’industrie automobile cherche constamment à augmenter la part des pièces fabriquées à partir de tôles minces en aciers plus résistants et à plus bas coût. Le parallèle entre les diagrammes de phases Fe-N et Fe-C montre qu’il est possible de développer des aciers similaires dans le système Fe-N. Les objectifs de cette étude étaient l’élaboration des aciers binaires Fe-N et le développement des structures équivalentes à celles dans les aciers au carbone. Les approches envisagées s’articulent autour de : Elaboration : la nitruration gazeuse en phase austénitique suivie de traitements d’homogénéisation ont permis de charger des tôles minces de fer pur en concentrations importantes d’azote. Une simulation de la diffusion de l’azote a été proposée. Genèse des microstructures : Le refroidissement lent de l’austénite Fe-N conduit à des structures perlitiques lamellaires et globulaires, constituées de ferrite et du nitrure non-stoechiométrique Fe4N. Une structure aciculaire particulière a été identifiée. Il s’agit de la ferrite se développant dans le nitrure Fe4N. Le refroidissement lent de la ferrite Fe-N sursaturée conduit à la précipitation des nitrures stables Fe4N et métastable Fe16N2. Des microstructures multiphasées [alpha+alpha'+gamma] ont été obtenues par des maintiens dans le domaine intercritique suivis de trempe. Le domaine intercritique a été réexaminé en utilisant le modèle des sous-réseaux. Des essais in-situ en MET ont relevé l’évolution des précipités de Fe16N2 dans la ferrite au cours du vieillissement à 85 °C. Des proportions importantes de l’austénite résiduelle ont été relevées, ce qui serait à la base du développement des aciers TRIP à l’azote / Car designers are seeking ways to increase the proportion of parts made of sheet steels of higher strength and lower cost. The parallel between the Fe-N and Fe-C phase diagrams shows that it is possible to develop similar steels in the Fe-N system. The objective of this study was to prepare binary Fe-N steels and to develop structures equivalent to those in carbon steels. Approaches to meet the objectives are considered: Preparations of Fe-N steels: gas nitriding in austenite domain followed by homogenization treatments allowed to introduce high amount of nitrogen in pure iron sheet. A simulation of the nitrogen diffusion was proposed to describe the weight increase during nitriding. Genesis of microstructures: The slow cooling of the Fe-N austenite led to lamellar and globular pearlitic structures composed of ferrite and nitrideFe4N. An acicular microstructure, which is the consequence of the precipitation of the ferrite in the nitride Fe4N, was also identified. The slow cooling of the supersaturated Fe-N ferrite led to the precipitation of the stable nitride Fe4N and the metastable nitride Fe16N2, which witnessed a rapid diffusion of nitrogen in ferrite at low temperature, comparable to that of carbon. The multiphase microstructures [alpha+alpha'+gamma] were obtained by intercritical treatments followed by quenching. The intercritical domain was reviewed using the sub-lattice model. In-situ TEM investigations have identified the precipitation of Fe16N2 nitride in the ferrite during the aging at 85 °C. High amount of the residual austenite have been identified, which would be the basis for development of TRIP nitrogen steels

Des nuances d’aciers à moyen carbone, microalliés au vanadium, ont été élaborées avec l’objectif d’obtenir de nouvelles microstructures, majoritairement constituées de ferrite aciculaire (FA). Le contrôle de la composition chimique (0.1-0.3 % V) et la vitesse de refroidissement (2.0 °Cs-1) conduit à des fractions de FA atteignant 80 %. Un paramètre empirique, le pouvoir ferritisant, P, a été introduit pour évaluer l’effet combiné de la composition chimique et de la vitesse de refroidissement sur la fraction de FA. Les caractérisations par MEB et MET montrent que la FA se développe à partir de la ferrite proeutectoïde recouvrant les inclusions de MnS. Une précipitation interphase de carbonitrures de vanadium, V(C,N), serait à l’origine d’un appauvrissement local en carbone de la matrice austénitique autour des aiguilles de FA, favorisant une germination autocatalytique. Le caractère fractal de la FA a été mis en évidence par des caractérisations morphologiques. Les dimensions fractales, D, et les longueurs de coupure ont été déterminées par la méthode de comptage de boîtes à partir d’images MEB. Des essais mécaniques isothermes-quasistatiques révèlent des propriétés mécaniques équivalentes à celles des microstructures bainitiques. Les courbes contrainte-déformation montrent un comportement mécanique de type Hollomon. Les structures de ces aciers présentent des taux de consolidation qui augmentent avec l’accroissement de la fraction de FA. Une corrélation entre les propriétés mécaniques et la dimension fractale a été établie. Ce lien s’exprime par des relations de type exponentiel : [delta]M = c exp [[alpha](D -2)] où M représente? les propriétés mécaniques (Re, Rm, etc.) et c? et ?[alpha] des constantes / Medium carbon vanadium microalloyed steels have been developed to obtain new microstructures, mainly formed of acicular ferrite (AF). Controlling the chemical composition and (0.1-0.3 % V) and the cooling rates (2.0 °Cs-1) lead to AF fractions up to 80 %. An empirical parameter, the ferritisant power, P, has been introduced to evaluate the combined effect of chemical composition and cooling conditions. Scanning (SEM) and transmission (TEM) electron microscopy investigations indicate that AF develops from proeutectoid ferrite enveloping MnS inclusions. An interphase precipitation of vanadium carbo-nitrides, V(C,N) has been identified. It is suggested that this precipitation is at the origin of carbon depletion in the austenitic matrix surrounding the AF plates. The formation of the AF is then enhanced by an autocatalytic effect. The fractal nature of AF has been determined by SEM and TEM characterisations. Fractal dimensions, D, and cut off lengths have been derived by the counting box method applied to SEM images. Mechanical tests conducted in isothermal and quasistatic conditions reveal that mechanical properties of AF are of the same grade of that of bainitic microstructures. Experimental strain-stress curves are described by the Hollomon law. The work hardening of the studied microstructures increases with the AF fraction. The mechanical properties have been linked to the fractal dimension by the following exponential relation : [delta]M = c exp [[alpha] (D -2)], where M represents the mechanical property (Re, Rm, etc.) and c and [alpha] are constants parameters

En perspective de la prolongation de la durée de vie en service des REPs, il est de plus en plus important d’obtenir une évaluation fiable de l’évolution de la microstructure des aciers constituant la cuve des REPs et de leurs propriétés correspondantes. Un mécanisme de fragilisation non-durcissante, dû à la ségrégation intergranulaire du P qui affaiblirait la cohésion des joints de grains, pourrait contribuer à la fragilisation et doit donc être étudié. Les présents travaux ont pour objectifs d’étudier la ségrégation intergranulaire du P dans un acier de cuve de réacteur afin (i) de connaître l’influence du type de joint de grain sur la ségrégation du P, (ii) de clarifier l’influence des conditions de vieillissement (vieillissement thermique et irradiation ionique) sur la ségrégation du P et (iii) de faire une comparaison avec les modèles disponibles et proposés ici.Pour cela, une méthodologie corrélative -Diffraction des Électrons Rétrodiffusés (EBSD), Diffraction de Kikuchi en Transmission (TKD) et Sonde Atomique Tomographique (APT) -a été adoptée pour étudier la ségrégation intergranulaire. Les informations cristallographiques (5 paramètres) et la composition chimique ont été collectées et systématiquement corrélées. Les aciers ont une microstructure complexe de ferrite aciculaire et de carbures intergranulaires. La ségrégation des solutés aux joints des grains (joints des grains faiblement désorientés (LAGB), joints des grains fortement désorientés généraux (HAGB) et Σ3HAGBs) et aux interfaces (interfaces carbure-ferrite M2.0-3.2C et interfaces cémentite-ferrite) a été quantifiée. Il existe une ségrégation évidente d'un élément ou de plusieurs espèces chimiques (C, P, Mn, Mo, Cr, Si et Ni) pour tous ces types de défauts plans. Tenant compte de la nature des éléments ségrégants et de la cristallographie du joint de grain, les ségrégations interstitielles et substitutionnelles ont été quantifiées et discutées. Sur la base d’un grand nombre de données, il apparaît que les niveaux moyens des segrégations en P sont plus élevés dans les HAGBs généraux ou les LAGBs que les autres types d'interfaces quel que soit le vieillissement envisagé. Par ailleurs, les résultats expérimentaux ont été comparés avec les résultats prévus par des modèles analytiques pour des systèmes binaires, ternaires et multi-composants. Bien qu'ayant un niveau de ségrégation du P prédit plus élevé, le modèle ternaire Fe-P-C se rapproche le plus des résultats expérimentaux. / With expectations for extending the service lifespans of PWRs, it is of great importance to get a reliable evaluation of the microstructural evolution and the corresponding property changes of RPV steels. A non-hardening mechanism, due to intergranular P segregation that impairs the grain boundary (GB) cohesion, may contribute to the embrittlement and thus needs to be studied. The present work aims to investigate the intergranular P segregation behavior in a RPV steel in order to (i) determine the influence of GB type on P segregation behavior, (ii) clarify the influence of ageing conditions (thermal ageing and ion irradiation) on P segregation behavior and (iii) make a comparison with the existing analytical models. To reach these objectives, a correlative - Electron Backscatter Diffraction (EBSD), Transmission Kikuchi Diffraction (TKD) and Atom Probe Tomography (APT) - methodology was adopted to study the GB segregation behavior. The crystallographic information (5 parameters) and chemical composition were collected simultaneously. The steels have a complex microstructure of acicular ferrite and intergranular carbides. The solute segregation at GBs (Low Angle Grain Boundaries (LAGBs), general High Angle Grain Boundaries (HAGBs) and Σ3 HAGBs) and interfaces (M2.0-3.2C carbide-ferrite interfaces and cementite-ferrite interfaces) were quantified. There is an obvious segregation of one element or several chemical species (C, P, Mn, Mo, Cr, Si and Ni) at all boundary types. Taking into account the nature of segregants and the five-parameter GB crystallography, both interstitial and substitutional segregation behaviors were discussed. Based on a large dataset, it appears that the average P segregation levels are higher in general HAGBs or LAGBs than in other boundary types. Besides, the experimental results were compared to the predicted ones from analytical models for binary, ternary and multicomponent systems. Though with a higher predicted P segregation level, the Fe-P-C ternary model seems to better fit the experimental results in all ageing conditions.