Les aciers inoxydables ferritiques stabilisés, aussi performants dans de nombreux domaines et moins chers que les aciers inoxydables austénitiques, souffrent cependant d’une formabilité inférieure (mise en forme + défaut de chiffonnage / roping). Il convient donc d’optimiser les microstructures et textures finales de ces produits, ce qui passe entre autres par une meilleure connaissance de l’évolution du matériau durant le laminage à chaud (LAC).Des essais de bipoinçonnement effectués sur une machine Gleeble®, simulant la compression plane à cœur du matériau durant le LAC, ont permis de simuler des schémas de laminage mono et multipasses. Les effets de la déformation, de la température, de la vitesse de déformation, de la taille de grains initiale et de la composition chimique sur les évolutions dynamiques (durant une passe de laminage) et post-dynamiques (durant un temps interpasse) ont été investigués.Une passe de LAC fragmente la microstructure en cristallites par recristallisation dynamique continue (RDC). Une partie de ces cristallites deviendront les germes de la recristallisation post-dynamique (RPD) au cours du temps interpasse. Celui-ci se caractérise par la simultanéité d’activation de nouveaux germes, de la croissance de grains recristallisés au sein de zones écrouies mais également au détriment d’autres grains recristallisés.Le couplage d’un modèle de RDC existant avec un modèle de RPD créé à partir des observations expérimentales, permet de simuler des schémas de LAC multipasses et de retranscrire les effets de la majorité des paramètres opératoires. / Stabilized ferritic stainless steels are as efficient as austenitic stainless steels in many areas and less expensive. However, they suffer from a lower formability (forming + roping defect). It is therefore necessary to optimize the final microstructures and textures of these products, which requires in particular a better understanding of the evolution of the material during hot rolling.Plane strain compression tests carried out on a Gleeble® machine, reproducing the deformation during hot rolling in the center of the material, permitted to perform single- and multi-pass rolling schedules. The effects of deformation, temperature, strain rate, initial grain size and chemical composition on dynamic (during a rolling pass) and post- dynamic (during an inter-pass time) evolutions were investigated.A hot rolling pass fragments the microstructure and creates crystallites by continuous dynamic recrystallization (CDRX). A part of these crystallites becomes nuclei for the post-dynamic recrystallization (PDRX) during inter-pass time. The latter is characterized by the simultaneous activation of new nuclei and growth of recrystallized grains, not only within strain-hardened zones but also at the expense of other grains already recrystallized.The coupling of an existing CDRX model with a PDRX model based on experimental results allows to simulate multi-pass hot rolling schedules and to reproduce the effects of most of the operating parameters.

Hydrogen is the smallest element in the periodical table. It has been shown in several studies that hydrogen has a large influence on the corrosion and cracking behaviour of stainless steels. Hydrogen is involved in several of the most common cathode reactions during corrosion and can also cause embrittlement in many stainless steels. Some aspects of the effect of hydrogen on corrosion and hydrogen-induced stress cracking, HISC, of stainless steels were studied in this work. These aspects relate to activation of test specimens for uniform corrosion testing, modification of a test cell for dewpoint corrosion testing and the mechanism of hydrogen-induced stress cracking. The results from uniform corrosion testing of superduplex stainless steels indicated that there is a large difference between passive and activated surfaces in hydrochloric acid and in lower concentrations of sulphuric acid. Hence, initial activation of the test specimen until hydrogen evolution can have a large influence on the results. This may provide another explanation for the differences in iso-corrosion curves for superduplex stainless steels that have previously been attributed to alloying with copper and/or tungsten. In concentrated sulphuric acid, potential oscillations were observed; these oscillations activated the specimen spontaneously. Due to these potential oscillations the influence of activation was negligible in this acid. An experimental set-up was developed for testing dewpoint corrosion of stainless steels in a condensate containing 1 % hydrochloric acid. There was an existing experimental set-up that had to be modified in order to avoid azeotroping of the water and hydrogen chloride system. A separate flask with hydro chloric acid was included in the experimental set-up. The final set-up provided reasonably good agreement with field exposures in contrary to much higher corrosion rates in the original set-up. Relaxation and low temperature creep experiments have been performed with several stainless steels in this work. The aim was to understand how creep and relaxation relates to material properties and the relative ranking between the tested materials. For low temperature creep with a load generating stresses below the yield strength, as well relaxation at stress levels above and below the yield strength, the same ranking with respect to changes in mechanical properties of the steel grades was found. For low temperature creep with a load level above the yield strength, the same ranking was not obtained. This effect can most probably be explained by annihilation and generation of dislocations. During low temperature creep above the yield strength, dislocations were generated. In addition, low temperature creep experiments were performed forone superduplex stainless steel in two different product forms with differentaustenite spacing in the microstructure. The superduplex material experienced low temperature creep at a lower load level for the material with large austenite spacing compared to the one with smaller austenite spacing. Also this differenceis influenced by dislocations. In a material with small austenite spacing the dislocations have more obstacles that they can be locked up against. Studies of the fracture surfaces of hydrogen induced stress cracking, HISC, tested duplex stainless steels showed that HISC is a hydrogen-enhanced localised plasticity, HELP, mechanism. Here a mechanism that takes into account the inhomogeneous deformation of duplex stainless steels was proposed. This mechanism involves an interaction between hydrogen diffusion and plastic straining. Due to the different mechanical properties of the phases in a superduplex stainless steel, plastic straining due to low temperature creep can occur in the softer ferrite phase. A comparison between low temperature creep data showed that for the coarser grained material, HISC occurs at the load levelwhen creep starts. However, in the sample with small austenite spacing, HISC did not occur at this load level. Microhardness measurements indicated that the hydrogen level in the ferrite was not high enough to initiate cracking in the coarser material. The proposed mechanism shows that occurrence of HISC is an interaction between local plasticity and hydrogen diffusion. / QC20100618

In the present work the effect of isothermal ageing treatment on the microstructure and on the localized corrosion resistance of a duplex stainless steel (DSS) was investigated. Specimens taken from a hot rolled cylindrical duplex stainless bar with 22% Cr grade were solution annealed at 1050&deg / C and then sensitization heat treatments were conducted at 650, 725 and 800&deg / C with duration ranging from 100 to 31622 min. The microstructural changes were examined by the light optical microscopy (LOM) and scanning electron microscopy (SEM). XRD technique and EDS analysis were used for microstructural evolution. Double Loop Electrochemical Potentiodynamic Reactivation (DLEPR) and standard weight loss immersion acid tests were performed in order to determine the degree of sensitization (DOS) to intergranular corrosion. The surfaces remained after the DLEPR test and the weight loss immersion test were also examined to observe the attack locations and their relationship with the chromium depleted zones. The degree of sensitization is measured by determining the ratio of the maximum current generated by the reactivation (reverse) scan to that of the anodic (forward) scan, (Ir/Ia) x 100. Ir is very small (less than 10-5 A/cm2) for solution annealed samples at 1050&deg / C for 1 hr and those aged at 650&deg / C for 100 and 316 min after the solution heat treatment, with the Ir/Ia ratios of 0.027634%, 0.033428% and 0.058928% respectively. Hence these samples were considered as unsensitized and their microstructure was composed of primary ferrite and austenite. However, Ir increased to values as high as 10-2 A/cm2 and even approached Ia for all samples aged for other temperatures and times, associated with high Ir/Ia ratios. The increased degree of sensitization can be attributed to stronger effect of chromium and molybdenum depleted areas. The microstructure was composed of primary ferrite and austenite including also sigma phase and the secondary austenite that would be responsible for the localized chromium impoverishment. The time required for sensitization was shorter in samples aged at higher temperatures. Accordingly ageing times of 1000 min at 725&deg / C and of 316 min at 800&deg / C were sufficient, whereas times longer than 10000 min was needed to achieve a sensitized structure at 650&deg / C.

Thesis (Ph.D.); Submitted to Iowa State Univ., Ames, IA (US); 19 Dec 2004. / Published through the Information Bridge: DOE Scientific and Technical Information. "IS-T 2322" Yoon-Jun Kim. US Department of Energy 12/19/2004. Report is also available in paper and microfiche from NTIS.

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Aços inoxidáveis duplex (AID) são materiais amplamente utilizados para uma grande variedade de aplicações desde a indústria química, de alimentos, petroquímica, naval, farmacêutica, energia nuclear e em muitos outros campos devido à combinação de suas excelentes propriedades mecânicas e de resistência à corrosão. Particularmente na indústria petroquímica, os aços AID’s são muito utilizados como materiais estruturais para a construção de gasodutos que transportam altos volumes de CO2 e na confecção das camadas internas dos tubos flexíveis (oleodutos offshore), utilizadas na produção de óleo. A soldagem a arco dos AID’s pode acarretar, dependendo das taxas de resfriamento envolvidas, a formação de precipitados de segunda fase que degradam suas propriedades mecânicas. Um processo alternativo para evitar o problema de precipitação de fases indesejáveis é a utilização do processo de soldagem/reparo por fricção com pino consumível (SFPC). O objetivo do presente trabalho é a caracterização metalúrgica e mecânica de juntas de solda de aço inoxidável duplex UNS S31803 obtidas através dos processos SFPC e de soldagem de costura por fricção (SCF). Na soldagem SCF, o objetivo do estudo foi a verificação da influência do passo de soldagem na formação e alteração das estruturas e nas propriedades mecânicas. Os resultados dos ensaios foram comparados com as propriedades obtidas do material base (MB) “como recebido”. A partir das juntas soldadas obtidas por fricção, foram extraídos corpos de prova para ensaios de microtração e Charpy para avaliação da resistência mecânica e da resistência ao impacto. Análises da microestrutura em microscopia ótica (MO) e perfis de microdurezas ao longo da região de solda também foram realizadas. Verificou-se que os processos de soldagem SFPC e SCF provocam um intenso refinamento de grão na zona de mistura (região da interface entre material do pino e da base), modificando a estrutura lamelar de grãos alongados da matriz ferrítica/austenítica, ocasionado por uma ação conjunta de aquecimento e deformação plástica oriunda do processo de solda por fricção. Os resultados dos ensaios de microtração indicam que as juntas soldadas aumentaram sua resistência mecânica com relação ao material base, fato que se deve ao aumento da quantidade da ferrita na zona termomecanicamente afetada (ZTMA), à formação de nitretos de cromo no centro dos grãos ferríticos e ao refino de grão. O aumento da quantidade de ferrita na ZTMA ocorre devido às altas taxas de resfriamento envolvidas no processo de soldagem e verificados por análise térmica. As elevadas taxas de resfriamento dificultam a difusão do nitrogênio que tem um importante papel no equilíbrio de fases da estrutura duplex (ferrita-austenita), na soldagem. O nitrogênio aprisionado no interior do grão ferrítico produz nitretos de cromo deixando de agir como elemento gamagênico aumentando a quantidade da fase ferrita. As juntas soldadas verificadas apresentaram tenacidade aceitável de acordo com o exigido pela norma ASTM A923. / Duplex stainless steels (DSS) are materials widely used for a variety of applications from the chemical, food, petrochemical, marine, pharmaceutical, nuclear industry and other fields due to the combination of their excellent mechanical properties and corrosion resistance. Particularly in the petrochemical industry, the DSS’s steels are extensively used as structural materials for the construction of gas pipelines that carry high volumes of CO2 and making the inner layers of flexible pipes (pipelines offshore) used in offshore oil production. The arc welding of DSS's can lead, depending on cooling rates involved, the formation of second phase precipitates which degrade their mechanical properties. An alternative method to avoid the problem of precipitation of unwanted phase is to use the welding process Friction Hydro Pillar Processing (FHPP). The aim of this work is the metallurgical and mechanical characterization of joints welds of UNS S31803 duplex stainless steel obtained through FHPP processes and Friction Taper Stitch Welding (FTSW). In FTSW welding, the objective of the study was to verify the influence of the welding step on the formation and alteration of structures and mechanical properties. The test results were compared with the properties of the obtained base material "as received". From the welds joints obtained by friction welding, specimens for microtensile testing and charpy were extracted to evaluate the mechanical strength and toughness. Microstructural analysis in optical microscopy (OM) and scanning electron microscopy (SEM) and microhardness profiles along the weld region were also performed. It was found that the welding process FHPP and FTSW causes an intense grain refinement in bonding zone, modifying the lamellar structure of elongate grains of matrix ferritic/austenitic, caused by action of heating and plastic deformation arising from the welding process by friction. The results of the microtensile tests indicate that the welded joints increased their mechanical resistance with respect to the base material, due to the increase in the amount of the ferrite in the thermomechanically affected zone (ZTMA), the formation of chromium nitrides in the center of ferritic grains and grain refining. The increase in the amount of ferrite in the ZTMA occurs due to the high cooling rates involved in the welding process and verified by thermal analysis. The high cooling rates difficult the nitrogen diffusion, which plays an important role in the phase equilibrium of the duplex structure (ferrite-austenite) in welding. The nitrogen trapped inside the ferritic grain produces chromium nitrides ceasing to act as gamogenic element by increasing the amount of the ferrite phase. The welds joints verified also had acceptable ductility and toughness according required by standard ASTM A923.

[pt] Os aços inoxidáveis duplex (AID) são uma classe de aços que combinam a alta resistência mecânica da ferrita e a ductilidade da austenita possuindo alto limite de escoamento e resistência à corrosão, sendo empregados em meios corrosivos com solicitações mecânicas elevadas. As boas propriedades mecânicas e de resistência à corrosão se devem a microestrutura duplex (ferrita e austenita), com proporções volumétricas similares, e cujo balanço é controlado por meio da composição química e tratamentos térmicos durante a fabricação. No entanto, durante processos de fabricação e manutenção, como a soldagem por fusão, em função do processo utilizado e dos ciclos térmicos impostos, assim como pela presença de gases de proteção que induzem determinada atmosfera, as propriedades do metal de solda e da zona termicamente afetada (ZTA), podem ser alteradas. Deste modo, a composição química, a distribuição dos elementos de liga e balanço das fases destas regiões serão suscetíveis a transformações de fases como ferritização, precipitação de fases indesejáveis e perda de elementos de liga, como níquel e nitrogênio, resultando em redução da resistência à corrosão. A presença de nitrogênio nos aços duplex, tanto em conjunto ou como substituto para o níquel, influencia na formação da austenita e também no controle da cinética de transformação de fases durante o resfriamento. O presente trabalho teve como objetivo estudar os efeitos do nitrogênio e do níquel na transformação de fases de dois aços inoxidáveis duplex (SAF 2304 e 2507) durante dois processos de soldagem: autógena e com metal de adição contendo Ni. Ambas as soldagens foram realizadas com aporte térmico fixo e com um e dois passes, utilizando a técnica de cordão sobre chapa para a soldagem com metal de adição. Foram utilizados dois gases de proteção, Ar e Ar + N2. Foram avaliadas a dureza e a resistência à corrosão por cloreto. A microestrutura da ZTA e composição química final do metal de solda alteraram significativamente, comparados ao metal de base. A fração volumétrica da fase austenítica na ZTA reduziu em todas as situações avaliadas. A presença de nitrogênio no gás de proteção manteve o teor deste elemento constante ou mais elevado no metal de solda. Cada conjunto de condições de soldagem aplicada apresentou diferentes características de dureza e resistência à corrosão por pites, sendo que na soldagem autógena do SAF 2507 foram encontradas durezas mais altas e menores perdas de massa após ensaio de corrosão. Com a adição de N2 no gás de proteção o teor de nitrogênio final aumentou em relação ao teor de nitrogênio no metal base, porém a fração volumétrica de austenita não se elevou da mesma forma. / [en] Duplex stainless steels (DSS) combines high yield stress from ferrite and ductility from austenite, good mechanical and corrosion resistance. It has been used in corrosive environments associated with severe mechanical stress. The good mechanical strength and corrosive resistance properties are due to the duplex microstructure (ferrite and austenite), with the same volumetric fraction, whose balance is controlled by chemical composition and heat treatment during steel manufacturing. However, when welded by process such as fusion welding the high thermal cycles and the presence of shielding gases inducing a certain atmosphere, the properties of the weld metal (WM) and the heat affected zone (HAZ) can be significantly changed. Therefore, the chemical composition, element partioning and the phase balance in these regions (WM and HAZ) will be susceptible to phase transformations such as ferritization, precipitation of secondary phases and alloy element losses, such as nitrogen and nickel, resulting in the decrease of the corrosion resistance. The presence of nitrogen in the duplex steels, either together or as a substitute for nickel, influences the austenite formation and controls phase transformation kinetics during cooling as well. The objective of this work was to study the effect of nitrogen and nickel on the phase transformation of two duplex stainless steels (SAF 2304 and 2507) during two welding processes: autogenous and with Ni-containing filler metal, considering a fixed thermal input and welds with one and two passes, using the technique of bead on plate for the weld with filler metal. Two shielding gases were used, Ar and Ar + N2. Hardness and corrosion resistance in chloride environment were evaluated for each studied condition. Both HAZ microstructure and final chemical composition of the weld metal modified significantly, when compared to the base metal. The HAZ volume fraction of austenite was reduced, and the presence of nitrogen in the shielding gas helped to keep the nitrogen content the same or increased in the weld metal. Each set of weld parameters applied presented different characteristics of hardness and pitting resistance corrosion. The autogenous welding of the SAF 2507 presented higher hardness and low weight losses. In a general way, the addition of N2 in the shielding gas increased the nitrogen content of the weld metal for all conditions of lean duplex material, compared to the base metal, but the austenite volumetric phase did not increased in the HAZ.

Submitted by Maike Costa (maiksebas@gmail.com) on 2017-05-23T14:29:46Z No. of bitstreams: 1 arquivo total.pdf: 4795148 bytes, checksum: c54fd3a89b2f0d0910af969c83f2d9b6 (MD5) / Made available in DSpace on 2017-05-23T14:29:47Z (GMT). No. of bitstreams: 1 arquivo total.pdf: 4795148 bytes, checksum: c54fd3a89b2f0d0910af969c83f2d9b6 (MD5) Previous issue date: 2015-06-18 / Duplex stainless steels (AID) are characterized for having good mechanical strength and corrosion. However, when subjected to manufacturing processes requiring the material thermal cycles with temperatures above 600 ° C, occurs emergence of fragile phases that compromise his toughness and corrosion resistance. Among these phases there is the presence of σ phase, rich in chromium and high hardness. In this paper we sought to develop a monitoring technique of the formation of σ phase. This technique is based on the study of the interaction between microstructure of the duplex stainless steel and the magnetic field applied to the material. Specimen with different amounts of σ phase were obtained by aging at temperatures of 800 °C and 900 °C. Aged AID was characterized by optical microscopy and scanning electron, hardness tests, impact tests and X-ray diffraction. The volumetric percentage of this phase was estimated by X-ray diffraction and processing of optical microscopy images. The magnetic field measurements were performed with a Hall effect sensor. The results show that the rise of the phase reduced the σ value of the magnetic permeability of the material, indicating that the magnetic properties and permeability measurements, as well as the resultant magnetic field, can be used for monitoring formation of this phase. The study proves to be developed effective technique for monitoring the duplex stainless steel embrittlement. / Os aços inoxidáveis duplex (AID) se caracterizam por apresentarem boa resistência mecânica e à corrosão. Contudo, quando submetidos a processos de fabricação que impõe ao material ciclos térmicos com temperaturas acima de 600 oC, ocorre surgimento de fases fragilizantes que comprometem a sua tenacidade e resistência à corrosão. Entre essas fases destaca-se a presença da fase σ, rica em cromo e de elevada dureza. Neste trabalho buscou-se desenvolver uma técnica de acompanhamento da formação da fase σ. Essa técnica se baseou no estudo da interação entre microestrutura do aço inoxidável duplex e ao campo magnético aplicado ao material. Amostras com diferentes quantidades de fase σ foram obtidas pelo envelhecimento nas temperaturas de 800ºC e 900ºC. O AID envelhecido foi caracterizado por microscopia ótica e eletrônica de varredura, ensaios de dureza, testes de impacto e difração de raios X. O percentual volumétrico dessa fase foi estimado por difração de raios X e processamento de imagens de microscopia óptica. As medidas de campo magnético foram realizadas com um sensor de efeito Hall. Os resultados mostram que o surgimento da fase σ reduziu o valor da permeabilidade magnética do material, indicando que as propriedades magnéticas e que medidas de permeabilidade, bem como do campo magnético resultante, podem ser utilizadas para acompanhamento de formação dessa fase. O estudo comprova ser a técnica desenvolvida eficaz para monitoramento da fragilização de aço inox duplex.

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Made available in DSpace on 2014-10-09T12:34:50Z (GMT). No. of bitstreams: 0 / Made available in DSpace on 2014-10-09T14:03:21Z (GMT). No. of bitstreams: 0 / Dissertação (Mestrado) / IPEN/D / Instituto de Pesquisas Energeticas e Nucleares - IPEN-CNEN/SP