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Medium Mn TRIP steels are amongst the most widely researched third generation advanced high strength steels (3G-AHSSs) as they are ideal candidates for automotive light-weighting applications owing to their superior strength and ductility balance. However, the thermal processing cycles of these steels need to be compatible with the industrial continuous galvanizing line (CGL) in order to successfully employ them in the automotive manufacturing industry. The main objective of the present research was to develop a CGL compatible thermal processing cycle for a prototype medium Mn steel that would produce significant volume fractions of chemically stable retained austenite and exhibit mechanical properties consistent with established 3G-AHSS targets. In that regard, the effects of intercritical annealing (IA) time and temperature and starting microstructure were determined in the first part of this research. The as-received tempered martensite (S-TM) and heat treated martensite (S-M) were the two different starting microstructures studied in this research. In this case, the overaging temperature (OT) treatment (460°C for 20s) was kept constant. It was found that high volume fractions (≥ 0.30) of retained austenite were achieved for S-M samples intercritically annealed at 675°C for shorter times (i.e. 60 to 120s) compared to S-TM samples. TEM analysis of the S-M samples showed that most of the retained austenite was present in a film type morphology, which is known to be more stable chemically and mechanically compared to the block type morphology. The tensile test results showed that although both the S-TM and S-M samples exhibited a high strength/ductility balance, the S-M samples, particularly the S-M 675°C + 120s samples, showed more potential in terms of CGL compatibility and achieving 3G-AHSS target mechanical properties. The effect of OT holding time was determined in the second part of this research. In that regard, the OT holding time was varied form 20s to 120s for selected S-TM and S-M samples. The S-TM 710°C samples with increased OT holding times (60s and 120s) had a significant increase in retained austenite volume fraction compared to the baseline 20s OT samples. However, the retained austenite volume fractions did not change for S-M samples regardless of OT holding time. It was also found that the mechanical properties of the annealed S-TM and S-M steels depended on the OT holding time. For the S-TM samples with > 120s IA holding times, longer OT holding times (60s and 120s) produced chemically unstable retained austenite which transformed rapidly at low strain resulting in low UTS × TE products. However, although longer OT holding times significantly increased the yield strength of the annealed S-M samples, the UTS × TE product decreased significantly owing to decreased retained austenite stability. Finally, based on the results of this research, it was concluded that the prototype medium Mn TRIP steel can achieve 3G-AHSS target mechanical properties using CGL-compatible thermal processing cycles. Moreover, depending on successful reactive wetting, it may be possible to perform both thermal processing and galvanizing of this steel in the industrial CGL. / Thesis / Master of Applied Science (MASc)

L’allégement des véhicules est l’un des objectifs prioritaires des constructeurs automobile pour répondre aux directives environnementales d’émission de CO2. Le développement des aciers multiphasés à très haute résistance mécanique est l’une des solutions communément adoptées pour réduire l’épaisseur des tôles dans les véhicules tout en conservant leur capacité à assurer la sécurité des passagers. La présente étude porte sur l’optimisation des paramètres du procédé de production industrielle de l’une des ces familles d’aciers : les aciers Dual Phase microalliés au titane et au niobium de haut grade ; c'est-à-dire possédant une résistance à la rupture supérieure à 800MPa.A partir d’une microstructure initiale bainite + martensite laminée à froid, les différents phénomènes se produisant au cours du recuit, de la chauffe jusqu’à la fin du maintien intercritique, sont caractérisés. L’influence des paramètres du recuit comme la vitesse de chauffe, la température et le temps de maintien est étudiée. Le système d’interactions triple entre la précipitation des éléments de microalliage, la recristallisation et la formation de l’austénite est au cœur du problème. Un scénario des évolutions microstructurales a été établi à partir de la caractérisation des divers phénomènes. La finesse de la microstructure étudiée (sub-micrométrique) a nécessité l’emploi combiné de techniques de caractérisation multi-échelles : MEB, MET, sonde atomique tomographique, nano-SIMS. / Lightening the weight of vehicles is one of the main challenging objectives of the automotive industry to reach the environmental regulation in term of CO2 emissions. The development of multiphase high strength steels is a common solution to reduce the thickness of sheet steel used in vehicles while keeping the same level of passenger’s safety requirements. The present study deals with the optimization of industrial process parameters applied to obtain one of these steels: the high strength microalloyed Dual Phase steels; i.e. with ultimate tensile strength superior to 800MPa.From an initial cold rolled microstructure made of bainite + martensite, the phenomena occurring during the annealing are characterized since the heating up to the end of the intercritical holding. The influence of process parameters as the heating rate, the holding temperature and the holding time are studied. The triple interactions system between the precipitation of microalloying elements, the recrystallization and the austenite formation is the core of the problem. A scenario of microstructural evolutions has been established based on the characterized phenomena. The studied fine microstructure (sub-microns) requires the combination of multiscale characterization techniques: SEM, TEM, atom probe tomography, nano-SIMS.

Face à l'augmentation générale de la consommation d'énergie, l'exploitation du Gaz Naturel Liquéfié (GNL) connaît un intérêt croissant, d'où un marché en forte expansion avec de nombreux projets d'installation de terminaux méthaniers. Les installations de gaz naturel liquéfié ont la particularité de fonctionner à très basses températures (~ -160°C), ce qui exige l'utilisation de matériaux particuliers présentant des caractéristiques adaptées aux températures extrêmes. Cette étude nous a permis d'évaluer le comportement structural de l'acier 9% Ni métal de base, consistant en une phase ferrique d'un grain martensitique en présence d'austénite, utilisé dans la construction du réservoir interne de stockage du GNL.Ce métal présente des domaines inhomogènes au niveau mésoscopique principalement formés par la phase austénitique riche en Ni mis en évidence par la diffusion des neutrons aux petits angles. Suite à une déformation mécanique, une augmentation du pourcentage de la phase austénitique est observée au niveau de la zone de déformation plastique. Ce phénomène est probablement dû à la diffusion préférentielle du Ni le long des dislocations au cours du traitement mécanique et son accumulation au niveau de cette zone. Au cours du processus de soudage, une diffusion intergranulaire du Ni au sein de la zone affectée thermiquement (ZAT) est observée. Ce phénomène permet de stabiliser la phase austénitique au niveau de la ZAT et d'améliorer les propriétés mécaniques au sein de cette zone. La déformation mécanique appliquée à basse température sur l'acier 9% Ni, ne détériore pas les propriétés structurales de ce matériau. / Due to the overall increase in energy consumption, the use of the Liquefied Natural Gas (LNG) is experiencing an increasing interest, resulting in a rapidly growing market with many LNG terminals installation projects. LNG installations have the particularity of operating at extremely low temperatures (~ -160°C), which requires materials with specific characteristics suitable to extreme temperatures. This study allowed us to evaluate the structural behavior of the base metal 9% Ni steel, consisting of a ferritic phase with a martensitic grain in the presence of residual austenite, used in the construction of the inner wall of LNG storage tank. This metal presents, at the mesoscopic level, non-homogeneous domains formed primarily by the Ni rich austenitic phase revealed by small angle neutron scattering. Due to a mechanical deformation, an increase in the percentage of the austenitic phase is observed at the plastic deformation zone. This phenomenon is probably due to the preferential diffusion of Ni along dislocations during the mechanical treatment and its accumulation at this area. During the welding process, a grain boundary diffusion of Ni in the Heat Affected Zone (HAZ) is observed. This phenomenon allows the stabilization of the austenitic phase at the HAZ and the improvement of the mechanical properties within this area. Mechanical deformation applied at low temperatures on the 9% Ni steel, does not deteriorate the structural properties of the material.

[pt] O processo de Têmpera e Partição (T&P) possibilita a produção de aços com frações controladas de austenita retida, a partir do enriquecimento da austenita pela partição de carbono da martensita sem a precipitação de carbonetos. A austenita retida proporciona o efeito TRIP (plasticidade induzida por transformação), que confere ao material uma deformação uniforme e uma melhor absorção de energia durante o impacto. Os aços produzidos por este processo atendem principalmente às necessidades da indústria automobilística, que busca aços com melhores propriedades para a diminuição de peso e aumento da segurança dos automóveis. Nesta dissertação, ligas de aço com diferentes composições e tamanhos de grão foram produzidos pelo processo de Têmpera e Partição e a fração de austenita retida foi medida por difração de raios-X. As ligas também foram caracterizadas por nanoindentação, microscopia ótica e microscopia eletrônica de varredura. As amostras estudadas foram produzidas com uma austenitização completa a 930°C, realizada para promover um aumento no tamanho de grão, e os resultados foram comparados com amostras estudadas anteriormente com temperatura de austenitização de 890°C. Os resultados obtidos indicaram um aumento da fração de austenita retida com o aumento do grão austenítico original. Estes resultados foram interpretados com base no modelo teórico desenvolvido para o processo T&P. / [en] The Quenching and Partitioning (Q&P) process allows the production of steels with controlled fractions of retained austenite from the enrichment of the austenite by carbon partitioning from the martensite without carbide precipitation. The retained austenite is responsible for the TRIP effect (transformation induced plasticity), which enhances the material behavior providing a uniform strain and a better energy absorption during impact. Steels produced by this process match the requirements of the automotive industry, which looks for weight reduction and safety improvements in cars. In the present dissertation, steels with different compositions and grain sizes were produced by the Quenching and Partition process and their retained austenite fraction was measured by x-ray diffraction. The steels were also characterized by nanoindentation, optical microscopy and scanning electron microscopy. The specimens studied were produced by a complete austenitization at 930°C, to promote an increase in the austenitic grain size, and the results were compared with previously studied specimens produced by a complete austenitization at 890°C. The experimental results indicate an increase of austenite fraction with an increase in grain size of the original austenite. These results were analyzed based on the theoretical model develop for the Q&P process.

Les aciers multiphasés à très haute résistance mécanique destinés à l’industrie automobile font l’objet d’importantes activités de recherche et développement dans le contexte de l’allègement des structures. L’obtention de meilleurs compromis entre résistance et ductilité nécessite de comprendre l’influence du couple composition chimique nominale – paramètres du procédé d’élaboration sur la formation des microstructures.La présente étude s’inscrit dans cette démarche de compréhension et porte en particulier sur les mécanismes se produisant lors du recuit des nuances d’aciers Dual Phase de haut grade microalliés au Ti et au Nb, dont la microstructure initiale laminée à froid est composée de bainite et de martensite. Ces mécanismes (précipitation des éléments de microalliage Ti, Nb et Mo, recristallisation de la ferrite et formation de l’austénite) présentent des interactions complexes. Le scénario des évolutions microstructurales lors du recuit est caractérisé à l’aide d’une étude expérimentale s’appuyant sur des techniques d’analyses complémentaires à différentes échelles (DRX in situ, MEB, MET, SAT). L’influence respective des éléments de microalliage Ti, Nb et Mo et des paramètres du recuit sur ce scénario est clarifiée à l’aide d’une caractérisation systématique des évolutions microstructurales couplée à la mise en œuvre d’une démarche de modélisation des mécanismes et de leurs interactions. / To meet the need for weight reductions in the automotive industry, new advanced high-strength steels are being developed. The achievement of a better balance between high strength and high formability requires a deep understanding of both the effect of chemical composition and processing parameters on the formation of microstructures. The present work contributes to such an objective and deals with the mechanisms occurring during annealing of Dual Phase steels microalloyed with Ti and Nb. Microstructural changes during this stage include precipitation of microalloying elements, ferrite recrystallization and austenite formation. These mechanisms are investigated using complementary experimental techniques at different scales such as in situ XRD, SEM, TEM and APT in various Dual Phase steel grades having the same bainite-martensite initial cold-rolled microstructure. Using combined experimental and modeling approaches, the present work clarifies the separate influence of microalloying elements Ti, Nb and Mo and heating rate on the mechanisms occurring during annealing and their interactions.

L’acier Ferrium® M54® présente une composition chimique optimisée, basée sur 40 ans d’évolution et de développement des aciers à durcissement secondaire à précipitation de carbures M2C. Le compromis de propriétés Rm/KIC/KISCC obtenu par la nuance M54® permet d’envisager son utilisation dans les trains d’atterrissage d’avions gros porteurs. Cependant, les premiers essais mécaniques, réalisés par l’utilisateur pour la montée en maturité de la nuance, ont montré une variabilité des propriétés mécaniques suivant le traitement thermique appliqué. Ce travail de thèse s’applique donc à décrire les évolutions microstructurales au cours du traitement thermique de la nuance M54® et les impacts sur les propriétés mécaniques en se concentrant notamment sur le traitement par le froid. Les différentes conditions de mise en solution et de revenu testées ont montré une certaine stabilité de la précipitation au revenu et des propriétés mécaniques qui en découlent. La précipitation a été caractérisée à différentes échelles afin de la comparer avec celle issue des nuances de la même famille. En revanche, selon les conditions de traitement par le froid réalisées, la limite d’élasticité varie de manière significative sans qu’aucun des paramètres liés à la précipitation ne soient modifiés. Le taux d’austénite est en revanche un paramètre déterminant pour la limite d’élasticité et est très sensible aux conditions de traitement par le froid : temps et température entre la trempe à l’huile et le traitement cryogénique et température de traitement cryogénique. Un traitement thermique amélioré a ainsi été proposé pour obtenir un taux d’austénite réduit et constant et limiter ainsi les variations de limite d’élasticité. / Ferrium® M54® steel presents an optimized composition, based on 40 years of research and development on secondary hardening steels. This alloy exhibits an excellent Rm/KIC/KISCC balance that allows considering its use in landing gears applications of wide-body aircrafts in the future. However, initial mechanical tests performed by the end-user have shown variability in mechanical properties depending on the applied heat treatment. The main goal of this work is to describe the microstructural evolutions of the alloy M54® during heat treatment and their impact on the resulting mechanical properties with a specific focus on the effect of the cryogenic treatment.The different austenitizing and tempering conditions investigated have shown a stability of the tempering precipitation and mechanical properties. This precipitation has been characterized at different scales and compared with other grades of the same family. On the other hand, depending on cryogenic treatment conditions, a significant variation of the mechanical properties and in particular of the yield strength is observed without any modification in the precipitation distribution and volume fraction or size. Austenite content is critical for the yield strength and is very sensitive to the cryogenic treatment conditions: time and temperature before cryogenic treatment and temperature of cryogenic treatment. An improved heat treatment to obtain reduced and constant austenite content is proposed.

Investigou-se o efeito do tamanho de grão austenítico na cinética e na morfologia do produto da reação bainítica de um ferro fundido nodular austemperado (FFNA). Foram estudados 3 tamanhos de grão austeníticos, a saber: GG (grão grosseiro), GM (grao mediano); e GR (grao refinado). A condição GR foi obtida pela austenitização rápida de microestruturas martensíticas. A condição GG foi obtida por tratamento de austenitização em duas etapas, de modo a, respectivamente, provocar o crescimento de grão e manter o teor de carbono igual aos das demais condições. Na segunda etapa do tratamento da condição GG ocorreu precipitação de grafita secundária, que acelerou significativamente a taxa de reação bainítica, possibilitando estudar o efeito da.variação na quantidade de interfaces austenita/grafita e austenita/ austenita sobre a cinética e a morfologia da reação bainítica. O refino do grão austenítico acelerou a cinética de reação, aumentou a proporção de ferrita alotriomorfa de contorno de grão, refinou a microestrutura bainítica (ferrita + austenita retida) e melhorou em 14% o limite de escoamento dos FFNA. Finalmente, a predominância de ferrira alotriomorfa na condição mais fina indica que a formação de interfaces incoerentes (mecanismo difusional ao inves de reação displaciva) durante a austenitização rápida da martensita (aquecimento de 100°C/ s). / The effect of austenite grain size on the kinetics and the morphology of the bainitic reaction in an austempered ductile iron (ADI) has been investigated, Three austenite grain sizes were produced: GG (coarse grain), GH (medium grain) and GR (fine grain), The GR condition was obtained by the rapid austenitization of martensitic microstructures The secondary graphite precipitation observed in GG condition strongly accelerated the rate of bainite formation and made possible the study of the effect of austenite/graphite interface on the kinetics of this reaction, The austenite grain refinement also accelerated the bainite precipitation, increased the proportion of grain boundary alotriomorphs ferrite, refined the bainitic microstructure and improved by 14% the yield stress of ADI, The predominance of grain boundary alotriomorphs in GR was associated to the structure of austenite/austenite interface formed during the rapid austenitization of the studied ductile iron at heating rates of 100oC/s. It is suggested that the dominant mechanism of austenitization in this condition is a thermally activated one (not a displacive transformation). The different morphologies of the austenite decomposition used the Duhê\'s morphological system.

A presente tese de doutorado avalia a Emissão Magnética Espontânea (SME), fenômeno descrito recentemente no grupo de pesquisa do professor Hélio Goldenstein e que já demonstrou ser uma ferramenta promissora para monitorar a transformação martensítica nos aços. O SME é utilizado para monitorar a velocidade de propagação de plaquetas de martensita; identificar a temperatura em que ocorre o inicio da primeira transformação (Ms); observar martensita induzida por deformação ou tensões durante a deformação de aços contendo austenita metaestável e também estudar a transformação isotérmica da austenita em martensita. A duração dos picos individuais magnéticos emitidos no início (Ms) e no final (Mf) da transformação martensítica durante o resfriamento contínuo foram medidos e comparados com os tamanhos médios das placas de martensita, obtidos através da metalografia quantitativa. O SME, um fenômeno mais sensível do que outras medidas globais como a resistividade, dilatometria, Ruído Magnético de Barkhausen (MBN), etc., não exige um volume crítico de transformação para ser detectado, e é capaz de detectar sinais de placas individuais crescentes. / This PhD thesis evaluates the Spontaneous Magnetic Emission (SME), a phenomenon recently described in the research group of Professor Hélio Goldenstein that has proved to be a promising tool to monitor the Martensitic Transformation in steels. The SME is used to monitor the speed of propagation of martensite plates; to identify the temperature at which the first transformation occurs (Ms); to observe martensite straininduced or stresses during deformation of steels containing metastable austenite and also study the isothermal transformation of austenite in martensite. The duration of individual magnetic peaks issued at the start (Ms) and in the end (Mf) of the martensitic transformation during the continous cooling were measured and compared with the average size of the martensite plates obtained by quantitative metalography. The SME, a phenomenon more sensitive than other global measures such as resistivity, dilatometry, Magnetic Barkhausen Noise (MBN), etc., does not require a critical volume of transformation to be detected, and is able to detect signs of growing individual plates.

Made available in DSpace on 2017-07-21T20:43:47Z (GMT). No. of bitstreams: 1 Ludiere Lucas Toldo Boneti.pdf: 5901766 bytes, checksum: 4f1a93e8f2d24f82e2576b7891703690 (MD5) Previous issue date: 2014-08-29 / The present study aimed to evaluate the influence of the austempering heat treatment parameters on microstructure and mechanical properties of a ductile cast iron produced in industrial conditions, containing 3.59% carbon, 2.68% silicon, 0.46% copper (in wt%) and a carbon equivalent of 4.50%. The material was produced in a foundry located in the southwest region of Parana state, Brazil. The specimens were obtained by casting the alloy into Y-block molds. The austempering heat treatments consisted of pre-heating at 500°C, followed by austenitizing step at 870°C, 900°C and 930°C during 60 minutes. Austempering was carried out in molten metal baths at temperatures of 300°C and 370°C for 30 minutes. Microstructural characterization was carried out by light optical microscopy (LOM) with image analysis, scanning electron microscopy (SEM-FEG) and X-ray diffraction with Rietveld refinement. The mechanical properties were evaluated by tensile and Vickers hardness tests. The as-cast microstructure displayed a very heterogeneous microstructure, characterized by the presence of regions with graphite flotation and carbide containing intercellular regions. The graphite nodules showed low nodularity, of 85%, which was attributed to the fading effect of magnesium alloy. Austempered samples were characterized by the presence of bainitic ferrite, interspersed with retained austenite in films and blocks. The austempering at 300°C resulted in a finer microstructure containing smaller volume fractions of retained austenite. All heat treated samples displayed transformation gradients between graphite flotation and intercellular regions. These gradients affected the mechanical properties, as well as the fracture characteristics. The best results of mechanical properties were obtained in the specimen austenitized at 900°C followed by austempering at 300°C, allowing the ADI produced to fit into a high strength class, according to ASTM A897. The study of fracture surfaces showed a sharp transition between graphite flotation and intercellular regions. The fracture at the vicinity of graphite nodules have occurred by a ductile mechanism, characterized by dimples. It was observed a rapid transition to the cleavage mode at intercellular regions, containing solidification carbides. / O presente trabalho teve como objetivo avaliar a influência dos parâmetros de tratamento térmico de austêmpera na microestrutura e nas propriedades mecânicas de tração e dureza, em uma liga de ferro fundido nodular produzida em condições industriais. A liga em estudo possui de teor de carbono de 3,59%, silício de 2,68% e adições de 0,46% de cobre, possuindo ainda um carbono equivalente de 4,50%. O material foi produzido em condições industriais, em uma fundição localizada no sudoeste do estado do Paraná. Os corpos de prova para retirada de amostras foram obtidos pelo vazamento da liga em moldes de blocos Y. Os tratamentos térmicos de austêmpera consistiram de pré-aquecimento a 500°C, seguido da etapa de austenitização a 870°C, 900°C e 930°C, por um tempo fixo de 60 minutos. A etapa de austêmpera foi realizada em banhos de metais fundidos, em temperaturas de 300°C e 370°C, durante 30 minutos. A caracterização microestrutural de amostras foi realizada pelas técnicas de microscopia ótica, com análise de imagens, microscopia eletrônica de varredura e difração de raios X, com refinamento pelo método de Rietveld. As propriedades mecânicas foram avaliadas por meio de ensaios de tração e dureza Vickers. A liga no estado bruto de fundição apresentou microestrutura bastante heterogênea, caracterizada pela presença de regiões com flotação de grafita e regiões intercelulares contendo carbetos de solidificação. Os nódulos de grafita apresentaram baixo grau de nodularização, de 85%, resultado que foi atribuído ao efeito de fadiga térmica da liga nodularizante. A microestrutura de amostras austemperadas foi caracterizada pela presença de agrupamentos de feixes de ripas de ferrita bainítica, entremeadas por austenita retida, na forma de filmes e blocos. A austêmpera a 300°C produziu microestruturas mais refinadas e com menores frações volumétricas de austenita retida. Em todas as amostras tratadas termicamente, foi observado um gradiente de transformação entre as regiões de flotação de grafita e regiões intercelulares. Estes gradientes afetaram tanto os resultados de propriedades mecânicas, como as características de fratura dos corpos de prova. Os melhores resultados de propriedades mecânicas foram obtidos para a condição de austenitização a 900°C seguida de austêmpera, permitindo enquadrar o ADI em uma classe de alta resistência, segundo a norma ASTM A897. As análises das superfícies de fratura dos corpos de prova de tração mostraram uma mudança nas características de fratura entre as regiões de flotação de grafita e as regiões intercelulares. Nas proximidades dos nódulos de grafita houve predominância do mecanismo de fratura dúctil, caracterizada pela presença de cavidades alveolares (“dimples”), com rápida transição para o modo de fratura por clivagem nas regiões com baixos números de nódulos de grafita, contendo carbetos de solidificação.