Aufgabenstellung: Aus einem Rohrstück des Materials P91 soll nach der Erarbeitung eines Probenplans zunächst das Gefüge in allen 3 Orientierungen metallographisch charakterisiert werden. Anschließend wird das Material mechanisch - technologisch sowie bruchmechanisch und fraktographisch untersucht. Die daraus erhaltenen Werkstoffkennwerte sollen mit dem Gefüge und dem fraktographischen Befund in Beziehung gesetzt werden.

Aufgabenstellung: Aus einem Rohrstück des Materials P91 soll nach der Erarbeitung eines Probenplans zunächst das Gefüge in allen 3 Orientierungen metallographisch charakterisiert werden. Anschließend wird das Material mechanisch - technologisch sowie bruchmechanisch und fraktographisch untersucht. Die daraus erhaltenen Werkstoffkennwerte sollen mit dem Gefüge und dem fraktographischen Befund in Beziehung gesetzt werden.

A utilização do aço ASTM A 335 P91 tem sofrido um aumento considerável, especialmente em função da necessidade de materiais com maior resistência à fluência para aplicações em unidades de utilidades (geração de vapor) e de processo. Por ser um material de difícil soldabilidade, diversos problemas são enfrentados durante a construção das unidades e, posteriormente, durante manutenção, geralmente em função de problemas de soldagem oriundos da fase de fabricação e construção. As normas de projeto e construção utilizadas internacionalmente vêm sofrendo adaptações a fim de melhorar a utilização deste material, mas seus requisitos ainda apresentam importantes lacunas em relação às principais práticas recomendadas pela literatura técnica mais atual. Visando uma melhor utilização deste material, obtendo juntas soldadas com propriedades mecânicas e metalúrgicas mais consistentes, o presente trabalho foi desenvolvido avaliando-se a influência de parâmetros de soldagem energia de soldagem e temperatura de tratamento térmico pós-soldagem (TTPS) sobre as propriedades mecânicas e metalúrgicas, incluindo resistência à fluência, de juntas soldadas de aço ASTM A 335 P91. Foram testadas nove juntas soldadas, combinando três níveis de energia de soldagem com três temperaturas de TTPS. Os resultados obtidos indicam que é possível ter melhor controle sobre as propriedades deste material, desde que se opere com níveis mais restritos de energia de soldagem e maiores temperatura de TTPS, observando-se as limitações pertinentes, especialmente no que tange à temperatura crítica de transformação Ac1. / The use of ASTM A 335 P91 has been increased considerably specially because of the need for materials with higher creep resistance for power generation (nuclear and thermoelectric) and oil and gas processing applications. As this is a material with poor weldability, several issues are faced during construction of these unities, and later during maintenance usually associated with welding problems originated in the fabrication and construction phase. The design and construction codes most used worldwide are receiving important revisions targeting to enhance the use condition of this material but its requirements still show important lacks when compared to the main practices recommended by the more recent technical literature. Aiming a better usage of this material obtaining sound welded joints with more consistent metallurgical and mechanical properties, this work was developed assessing the influence of some welding parameters welding heat input and temperature of post-­weld heat treatment (PWHT) on the metallurgical and mechanical properties, including creep strength, of welded joints of ASTM A 335 P91 steel. Nine welded joints were submitted to testing, combining three different levels of welding heat input with three different PWHT temperatures. The results show that it is possible to have a better control over the properties of this material since it is used lower welding heat inputs combined to higher PWHT temperatures, taking care about the limitations regarding the critical transformation temperature Ac1.

A utilização do aço ASTM A 335 P91 tem sofrido um aumento considerável, especialmente em função da necessidade de materiais com maior resistência à fluência para aplicações em unidades de utilidades (geração de vapor) e de processo. Por ser um material de difícil soldabilidade, diversos problemas são enfrentados durante a construção das unidades e, posteriormente, durante manutenção, geralmente em função de problemas de soldagem oriundos da fase de fabricação e construção. As normas de projeto e construção utilizadas internacionalmente vêm sofrendo adaptações a fim de melhorar a utilização deste material, mas seus requisitos ainda apresentam importantes lacunas em relação às principais práticas recomendadas pela literatura técnica mais atual. Visando uma melhor utilização deste material, obtendo juntas soldadas com propriedades mecânicas e metalúrgicas mais consistentes, o presente trabalho foi desenvolvido avaliando-se a influência de parâmetros de soldagem energia de soldagem e temperatura de tratamento térmico pós-soldagem (TTPS) sobre as propriedades mecânicas e metalúrgicas, incluindo resistência à fluência, de juntas soldadas de aço ASTM A 335 P91. Foram testadas nove juntas soldadas, combinando três níveis de energia de soldagem com três temperaturas de TTPS. Os resultados obtidos indicam que é possível ter melhor controle sobre as propriedades deste material, desde que se opere com níveis mais restritos de energia de soldagem e maiores temperatura de TTPS, observando-se as limitações pertinentes, especialmente no que tange à temperatura crítica de transformação Ac1. / The use of ASTM A 335 P91 has been increased considerably specially because of the need for materials with higher creep resistance for power generation (nuclear and thermoelectric) and oil and gas processing applications. As this is a material with poor weldability, several issues are faced during construction of these unities, and later during maintenance usually associated with welding problems originated in the fabrication and construction phase. The design and construction codes most used worldwide are receiving important revisions targeting to enhance the use condition of this material but its requirements still show important lacks when compared to the main practices recommended by the more recent technical literature. Aiming a better usage of this material obtaining sound welded joints with more consistent metallurgical and mechanical properties, this work was developed assessing the influence of some welding parameters welding heat input and temperature of post-­weld heat treatment (PWHT) on the metallurgical and mechanical properties, including creep strength, of welded joints of ASTM A 335 P91 steel. Nine welded joints were submitted to testing, combining three different levels of welding heat input with three different PWHT temperatures. The results show that it is possible to have a better control over the properties of this material since it is used lower welding heat inputs combined to higher PWHT temperatures, taking care about the limitations regarding the critical transformation temperature Ac1.

Il s'agit dans ce travail de développer une démarche multiéchelles, afin d'identifier puis de modéliser le comportement mécanique d'un matériau à gradient de propriétés (un cordon de soudure) en relation avec les hétérogénéités microstructurales responsables de la déformation et de l'endommagement par fluage des aciers P91, matériaux retenus pour des applications de tenue mécanique à chaud des centrales thermiques à flamme. Cette étude porte sur l'utilisation des techniques de mesure de champs cinématiques par corrélation d'images couplées aux simulations numériques par éléments finis. Les différentes zones d'intérêt sont : le métal de base, l'ICHAZ (intercritical heat affected zone), la FGHAZ (fine grain heat affected zone), la CGHAZ (coarse grain heat affected zone) et le métal fondu. L'identification a porté dans un premier temps sur le comportement en traction et traction–relaxation à l'ambiante et à 625°C. Cette phase a permis d'établir une loi de comportement pour chacune des zones du joint soudé et de prédire la zone de localisation de déformation pour une gamme assez large de vitesse de sollicitation.Une attention particulière a ensuite été portée aux essais de fluage, pour lequel le glissement intergranulaire joue un rôle essentiel dans le comportement du cordon de soudure et notamment dans l'ICHAZ. Afin de mettre en évidence le glissement intergranulaire, une technique de microlithographie a été adoptée. L'effet de ce mécanisme sur le comportement macroscopique et à l'échelle locale a été étudié au moyen de simulations numériques par éléments finis avec introduction de zones cohésives. Pour cela une loi cohésive a été élaborée et validée sur une configuration simplifiée à quatre grains. Ce modèle permet également de rendre compte de la transition fluage dislocation – fluage diffusion en retardant le déclenchement du glissement aux joints de grains quand la vitesse de sollicitation augmente.Cette étude est financée par la Chaire EDF-GDF-SUEZ-GRT gaz - ENSMP –ENPC sur la «durabilité des matériaux et des structures pour l'énergie ». / The goal of this study is to develop a micromechanical approach, to identify and model the elementary mechanisms in connection with the microstructural heterogeneities accountable for the deformation and for the creep damage of P91 steels, material used for applications at high temperature in thermal power plants. This study deals with the use of kinematic full-fields measurements by digital image correlation coupled with finite element numerical simulations for the identification of constitutive equation parameters of materials presenting a strongly heterogeneous microstructure, leading to gradients of mechanical properties. The welded joint in P91 presents various microstructures along the joint: base metal, ICHAZ (intercritical heat affected zone), FGHAZ (fine grain heat affected zone), CGHAZ (coarse grain heat affected zone) and weld metal, which will be characterized by uniaxial tensile tests and tensile-relaxation tests performed at room temperature and at 625°C. These experimental tests enable to establish a constitutive law for each part of the welded joint and for a wide range of strain rate.A particular attention has then been focused on the behaviour at high temperature (creep) for which the intergranular glide plays an essential role, in particular within the ICHAZ. To characterize the grain boundary gliding mechanisms, a technique of microlithography is used. This mechanism is modelled with cohesive zones. A cohesive constitutive equation has been proposed and validated with a simplified four grain configuration. This model is able to take into account the dislocation creep – diffusion creep transition by delaying the beginning of the grain boundaries sliding when the strain rate increases.This study is granted by the EDF-GDF-SUEZ-GRT gas – Mines ParisTech – Ecole des Ponts ParisTech chair on the "durability of materials and structures for the energy ".

Coordenação de Aperfeiçoamento de Pessoal de Nível Superior / Pouco se sabe a respeito das consequências da operação de reparo nas propriedades mecânicas e metalúrgicas das juntas do aço ASTM A335 grau P91 soldadas por Arame Tubular. Neste trabalho foi realizado um estudo para analisar e caracterizar juntas de um tubo do aço P91 soldadas pelo processo Arame Tubular com proteção gasosa, antes e após situação de duplo reparo. Foram utilizadas técnicas de microscopia eletrônica de varredura (MEV), análise química semiquantitativa por EDS (Energy Dispersive Spectroscopy), microscopia óptica (MO), além da obtenção de medidas de microdureza Vickers e realização de ensaios de impacto e tração à temperatura ambiente. A macrografia revelou a existência de uma nova zona termicamente afetada formada no centro da junta reparada e a análise micrográfica mostrou que esta zona apresentou uma pequena tendência a formação de grãos menores do que na zona de fusão que sofreu reparo, além disso, a região tinha grãos colunares que não são característicos de uma zona termicamente afetada e quantidade de carbonetos menor comparativamente. Não houve variações significativas nos valores de tração e microdureza. Os ensaios de impacto revelaram baixos valores de energia absorvida na zona de fusão do 2 reparo, no entanto, todas as outras zonas avaliadas das juntas com e sem reparo apresentaram valores dentro das especificações. / Little is known about the consequences of the repair operation on the mechanical and metallurgical properties of ASTM A335 grade P91 steel joints welded by Flux-Cored Arc Welding (FCAW). In this work, a study was made to analyze and characterize joints of P91 steel tube, welded by FCAW with shielding gas, before and after double repair situation. Techniques of scanning electron microscopy (SEM), chemical analysis by semi-quantitative EDS (Energy Dispersive Spectroscopy) and optical microscopy (OM) were used, in addition, Vickers microhardness measurements, impact and tensile tests at room temperature, were carried out. The macrography revealed the existence of a new heat affected zone formed in the center of the repaired joint and the micrographic analysis showed that this zone has a tendency to formation of smaller grains compared to the repaired fusion zone, furthermore, the region has columnar grains which are not characteristics of a heat affected zone and comparatively lesser amounts of carbides. There were no significant variations in the tensile and hardness values. Impact tests showed low values of absorbed energy in the fusion zone of the second repair; however, all other evaluated zones, with and without repair, had values within specifications.

Coordenação de Aperfeiçoamento de Pessoal de Nível Superior / Pouco se sabe a respeito das consequências da operação de reparo nas propriedades mecânicas e metalúrgicas das juntas do aço ASTM A335 grau P91 soldadas por Arame Tubular. Neste trabalho foi realizado um estudo para analisar e caracterizar juntas de um tubo do aço P91 soldadas pelo processo Arame Tubular com proteção gasosa, antes e após situação de duplo reparo. Foram utilizadas técnicas de microscopia eletrônica de varredura (MEV), análise química semiquantitativa por EDS (Energy Dispersive Spectroscopy), microscopia óptica (MO), além da obtenção de medidas de microdureza Vickers e realização de ensaios de impacto e tração à temperatura ambiente. A macrografia revelou a existência de uma nova zona termicamente afetada formada no centro da junta reparada e a análise micrográfica mostrou que esta zona apresentou uma pequena tendência a formação de grãos menores do que na zona de fusão que sofreu reparo, além disso, a região tinha grãos colunares que não são característicos de uma zona termicamente afetada e quantidade de carbonetos menor comparativamente. Não houve variações significativas nos valores de tração e microdureza. Os ensaios de impacto revelaram baixos valores de energia absorvida na zona de fusão do 2 reparo, no entanto, todas as outras zonas avaliadas das juntas com e sem reparo apresentaram valores dentro das especificações. / Little is known about the consequences of the repair operation on the mechanical and metallurgical properties of ASTM A335 grade P91 steel joints welded by Flux-Cored Arc Welding (FCAW). In this work, a study was made to analyze and characterize joints of P91 steel tube, welded by FCAW with shielding gas, before and after double repair situation. Techniques of scanning electron microscopy (SEM), chemical analysis by semi-quantitative EDS (Energy Dispersive Spectroscopy) and optical microscopy (OM) were used, in addition, Vickers microhardness measurements, impact and tensile tests at room temperature, were carried out. The macrography revealed the existence of a new heat affected zone formed in the center of the repaired joint and the micrographic analysis showed that this zone has a tendency to formation of smaller grains compared to the repaired fusion zone, furthermore, the region has columnar grains which are not characteristics of a heat affected zone and comparatively lesser amounts of carbides. There were no significant variations in the tensile and hardness values. Impact tests showed low values of absorbed energy in the fusion zone of the second repair; however, all other evaluated zones, with and without repair, had values within specifications.

Les aciers ferritiques à faible teneur en chrome tel que le T/P91 sont largement utilisés dans les centrales de productions d’électricité pour leurs bonnes propriétés mécaniques et leur faible coefficient d’expansion thermique. Cependant, la demande croissante en énergie alliée à la nécessité de réduire les émissions de gaz à effet de serre, conduisent à envisager l’augmentation des conditions d’utilisation (température et pression) de ces matériaux. Des études ont montré qu’en modifiant la température de fonctionnement et la pression de vapeur d’eau de 538°C/18.5 MPa à 650°C/30 MPa, le rendement des centrales thermiques progressait d’environ 8%. Se pose alors la question de la tenue à la corrosion à haute température des aciers à 9% de chrome. Au cours de ces travaux, le comportement d’un acier ferritique/ martensitique à 9% de chrome a été étudié à 650°C sous air sec et sous vapeur d’eau de matière isotherme et en conditions de cyclage thermique. La prise de masse des échantillons renseigne sur la cinétique de la réaction d’oxydation et l’adhérence des couches d’oxydes formées. Les produits de corrosion ont été caractérisés par plusieurs techniques d’analyses dans l’optique de clairement identifiés les oxydes en présences et leurs mécanismes de formation. Des oxydes mixtes de fer et de chrome (Cr,Fe)2O3 sont dans un premier temps formés et assurent s’avèrent être temporairement protecteur. Pour des longs temps d’oxydation ou des températures supérieures à 650°C, la magnétite Fe3O4 et l’hématite Fe2O3 sont les principaux oxydes formés, montrant ainsi l’inadéquation des nuances à faible teneur en chrome pour une utilisation dans des conditions aussi drastiques. Dans l’optique d’augmenter la résistance à la corrosion à haute température de cet alliage, diverses solutions ont été envisagées tel que l’aluminisation par cémentation en caisse, les revêtements d’oxydes de terre rare par MOCVD, ou encore l’ajout d’éléments d’addition. Ces solutions ont été également testées à 650°C sous air sec et sous vapeur d’eau. / The improvement of high temperature oxidation resistance of low chromium content steels, such as T/P91, is of great interest in regards with their application in thermal power generating plants. Indeed, they possess good creep properties, and low thermal expansion coefficient. Important needs in energy together with environmental issues place power generation plants under constraints which lead to develop high efficiency systems. A usual way to increase the efficiency consists in increasing temperature and pressure parameters of the power generating plant. Studies has shown that the total efficiency of a plant increases by nearly 8 % when changing the steam parameters from 538°C/18.5 MPa to 650°C/30 MPa. Then, the problem of corrosion resistance of 9% chromium steel in those conditions is asked. In this work, the behavior of a ferritic / martensitic 9% chromium steel has been studied at 650°C in dry air and in water vapor containing environment in both isothermal and thermal cyclic conditions. The weight gain of samples provides information on the kinetics of the oxidation reaction and the adhesion of formed oxide scale. Corrosion products were characterized by several analytical techniques in order to identify oxides with accuracy and to understand their formation mechanisms. Mixed iron and chromium oxides (Cr, Fe) 2O3 are initially formed and provide temporary protection to the substrate. For long time exposure or temperatures above 650°C, magnetite, Fe3O4 and hematite Fe2O3 are the main oxides formed, highlighting the fact that low chromium steel are inappropriate for applications in such drastic conditions. In order to increase the high temperature corrosion resistance of this alloy, various solutions have been proposed as aluminizing by pack cementation, reactive element oxides coatings of by MOCVD, or addition of alloying elements in the steel composition. These solutions were then tested at 650 ° C in dry air and in water vapor environments.

This thesis deals with a high temperature testing of fracture toughness and studies the size effect on measured values using miniature size CT specimen. Two types of specimen geometry were manufactured from P91 steel, the standard size and the quarter size specimen. J-R curves were obtained in the temperature range from 23°C to 600°C. No specimen size effect was observed at room temperature tests. The realized experiments together with fractography analysis demonstrated the drop of toughness at 400°C caused by the effect of dynamic strain aging.

The thesis deals with the determination of fracture toughness using compact tension (CT) test specimens at elevated and high temperatures. The experimental material steel P91 designated for application at temperatures 550650°C was used. The fracture toughness in the ductile fracture region of the steel was characterized by the R curve, which characterises the resistance against crack propagation depending on the crack length. The effect of temperature on the R curve at range 23600°C was evaluated. Next the specimen size effect using three sizes of CT specimens at 23°C and the effect of loading rate (2, 0,2 a 0,02 mm/min) at 600°C was examined. The results showed that the temperature has distinct effect on the R-curve, which yields minimal values at 400°C. Only the smallest test specimen size with thickness 6.25mm showed the specimen size effect giving about 10% lower values of toughness comparing to larger specimens. The effect of loading rate was clearly distinguishable. The values of toughness varied about 20% of the toughness value comparing individual loading rate.