Les aciers multiphasés à effet TRIP sont étudiés depuis plusieurs années maintenant et suscitent un intérêt industriel grandissant, non seulement de la part des sidérurgistes mais également de la part des "clients" de ces derniers, à savoir les constructeurs automobiles. Il semble en effet tout à fait clair que la combinaison au sein de la même microstructure de différentes phases de l'acier (ferrite, bainite, martensite) et l'existence de l'effet TRIP (c'est-à-dire une transformation martensitique induite mécaniquement) améliore de façon importante les propriétés de résistance et de ductilité d'aciers faiblement alliés. Dans ce contexte, notre projet a eu pour objectif de trouver des alternatives aux éléments d'alliage actuellement utilisés (silicium et aluminium) pour la genèse de microstructures conférant aux aciers TRIP les propriétés de résistance et de ductilité désirées. En particulier, nous avons étudié l'un des plus utilisés en sidérurgie, à savoir le niobium. Notre travail s'est donc attaché à étudier l'effet d'additions importantes de niobium (jusque 0.12% en poids) sur les transformations de phase ayant lieu durant le traitement thermique imposé aux aciers multiphasés à effet TRIP ainsi que sur la microstructure et les propriétés mécaniques résultantes. Le niobium influence considérablement les différentes transformations de phase et en particulier la recristallisation de la matrice ferritique se produisant lors du réchauffage et du maintien intercritique. / TRIP-assisted multiphase steels have been studied for several years and arouse a growing industrial interest, not only on behalf of the steelmakers but also on behalf of the “customers” of these, namely the car manufacturers. It seems completely clear that the combination within the same microstructure of various steel phases (ferrite, bainite, martensite…) and the existence of the TRIP effect (i.e. a mechanically induced martensitic transformation) improves in a large way the properties of resistance and ductility of low-alloy steels. In this context, this project aimed to find alternatives to alloy elements currently used (silicon and aluminium) for the generation of microstructures conferring to the TRIP steels the desired properties of resistance and ductility. In particular, we studied the niobium that is one of the most used in iron and steel industry. Our work thus attempted to study the effect of important additions of niobium (until 0.12% in weight) on phase transformations taking place during the heat-treatment imposed to TRIP-aided multiphase steels and on the resulting microstructure and mechanical properties. Niobium influences considerably the various phase transformations and in particular the recrystallization of the ferrite matrix occurring during reheating and intercritical annealing.

Estudou-se a cinética das transformações de fase em resfriamento contínuo e em tratamentos isotérmicos de cinco ligas de aços TRIP microligados com Nb, contendo teores variáveis de Mn e Si, através de ensaios dilatométricos, de caracterização morfológica dos produtos de transformação e de cálculos termodinâmicos e simulações numéricas usando os programas Thermocalc ® e Dictra®. Foram determinados os diagramas RC para a transformação da austenita, e foi estudada a influência da precipitação de ferrita pró-eutetóide e de bainita na fração volumétrica de austenita retida. Através dos diagramas de resfriamento contínuo foi possível delimitar a extensão do campo intercrítico dos cinco aços analisados, com determinação da janela de resfriamento e seus intervalos de temperaturas. Isso permitiu projetar os ciclos de resfriamento controlado a serem aplicados durante o processamento termomecânico dos Aços TRIP-D, TRIP-E e TRIP-H. Os cálculos pelo modelo numérico de redistribuição de carbono e de elementos substitucionais na interface ferrita/austenita, bem como as medidas de microanálise química por WDS e EDS permitiram verificar que a taxa de crescimento da ferrita pró-eutetóide é controlada pela difusão do carbono na austenita. Para tempos curtos de tratamento, o modelo de crescimento que melhor se ajusta é o do equilíbrio local com partição negligível de soluto. Verificou-se através de tratamentos isotérmicos no campo bainítico, que o silício atrasa a precipitação de carbonetos durante a reação bainítica, o que justifica o aumento da estabilidade da austenita retida no aço de maior Si (TRIP-H), quando comparado com o aço de menor Si (TRIP-E). Baseado nos resultados dos estudos das transformações de fase por resfriamento contínuo foram selecionadas as ligas TRIP-D, TRIP-E e TRIP-H, para simular dois esquemas de laminação controlada por meio de ensaios de torção a quente. Nesses ensaios foram variados o grau de deformação e a temperatura de acabamento, de modo a estudar os efeitos dos parâmetros de deformação mecânica na fração transformada dos diferentes constituintes microestruturais, e em particular na fração volumétrica de austenita retida. O primeiro ensaio refere-se à laminação controlada por recristalização estática (LCRE) e o segundo à laminação convencional (LCC), com temperatura de acabamento de 1030°C e 850°C, respectivamente. O resfriamento consistiu em dois tratamentos isotérmicos consecutivos: o primeiro no campo intercrítico (austenita + ferrita), e o segundo no campo bainítico. O aumento do grau de deformação na simulação por torção a quente da laminação controlada por recristalização estática, levou a um aumento da porcentagem de austenita retida obtida durante o resfriamento controlado (de 9 a 14,0 %). O acúmulo de energia de deformação abaixo da TNR na simulação do processo de laminação controlada convencional provocou uma diminuição da fração volumétrica de austenita retida bem como da concentração de carbono contido nela. Os perfis de Mn e C obtidos a partir de análises químicas com EDS e WDS em amostras do aço TRIP-E, deformadas com deformação total de 2,1 e deformação total de 2,8, mostram a contribuição do refinamento de grão para a difusão destes elementos na frente da interface ferrita/austenita, durante a precipitação de ferrita pró-eutetóide. / The phase transformation kinetics of five Nb microalloyed Si-Mn TRIP steels was studied under continuous cooling and isothermal treatments, using dilatometric techniques, morphologic characterization, Thermocalc computational thermodynamics and Dictra numerical simulation. WDS and EDS X-ray microanalysis and Dictra numerical modeling of C, Mn and Si distribution during transformation showed that the reaction is carbon diffusion controlled and growth occurs under local equilibrium with negligible partition. CCT diagrams for austenite transformation were determined and the effect of the amount of proeutectoid ferrite and bainite precipitation on the volume fraction of retained austenite was also estimated. The CCT diagrams allowed determining the boundaries of the critical zone and the processing window to obtain bainite plus austenite microstructures. Based on this information cooling cycles were selected to perform thermomechanical treatments. Three TRIP steels were selected to simulate, in a hot torsion testing machine, two different controlled rolling sequences: Recrystallization Controlled Rolling and Conventional Controlled Rolling. The influence of the degree of deformation and the finishing temperature on the amount of retained austenite was studied. After rolling the cooling cycle comprised two isothermal treatments, one in the austenite + ferrite field and the other in the bainitic field. Increasing the strain during simulation of Recrystallization Controlled Rolling led to an increase in the volume fraction of retained austenite to the range 9 to 14 %. The energy stored during simulation bellow TNR of the Conventional Controlled Rolling led to a decrease in the volume fraction and in the carbon content of retained austenite. The Mn and C contents measured by EDS and WDS analysis of TRIP-E steel, showed that grain refinement due to recrystallization contributes to diffusion of these elements in front of the ferrite/austenite interface during precipitation.

Seit vielen Jahren wächst die Nachfrage bezüglich sparsamer Fahrzeuge; die Autohersteller konkurrieren miteinander und werben mit neuen Fahrzeugkonzepten, in denen hochmoderne Werkstoffe ihre Anwendung finden. In dieser Arbeit werden Legierungskonzepte und entsprechende Warmwalztechnologien einer ultrahochfesten bainitischen Stahlsorte mit Restaustenit vorgestellt, die der genannten Anwendung angepasst werden können. Der gewählte Werkstoff gehört zu den Stählen mit mittleren Kohlenstoffgehalten, die sich nach der - im Rahmen dieser Arbeit entwickelten - Behandlung durch hohe Zugfestigkeit bei vergleichsweise hoher Bruchdehnung auszeichnen. Es werden erweiterte Modelle zur Beschreibung der Phasenumwandlung von Stählen im Bainitgebiet vorgestellt. Die Ergebnisse aus den Experimenten wurden genutzt, um die Modelle zu ergänzen und zu evaluieren. Dabei wird nicht nur der Warmwalzprozess, sondern auch die chemische Zusammensetzung der Stähle selbst optimiert. Die hier präsentierte Arbeit erstreckt sich über die gesamte Produktionskette und zeigt geeignete Herstellungsbedingungen, die in Betriebsanlagen leicht realisierbar sind und umgesetzt wurden.:1 Einführung 10 2 Literaturauswertung 12 3 Aufgabestellung 52 4 Eigene Arbeiten 53 5 Versuchsdurchführung 55 6 Ergebnisse 67 7 Zusammenfassung und Ausblick 129 8 Literaturverzeichnis 131 9 Abbildungsverzeichnis 141 10 Tabellenverzeichnis 144 11 Angewendete Simulationsanlagen 146 12 Anhang 151

In the pipe manufacturing and pipe processing industry, the demand for cost-effective pipes with high strength and good ductility is increasing. In the present study, the inductive longitudinal welding process was combined with a Quenching and Partitioning (Q&P) treatment to manufacture pipes with enhanced mechanical properties. The aim of the Q&P process is to establish a martensitic structure with increased retained austenite content. This allows for the beneficial use of both phases: the strength of martensite as well as the ductility of retained austenite. A 42SiCr steel, developed for Q&P processes, was joined at the longitudinal seam by a high-frequency induction (HFI) welding process and was subsequently heat-treated. The applied heat treatments included normalizing, austenitizing, quenching, and two Q&P strategies (Q&P-A/Q&P-B) with distinct quenching (Tq = 200/150 °C) and partitioning temperatures (Tp = 300/250 °C). Investigations of the microstructures revealed that Q&P tubes exhibit increased amounts of retained austenite in the martensitic matrix. Differences between the weld junction and the base material occurred, especially regarding the morphology of the martensite; the martensite found in the weld junction is finer and corresponds more to the lath-type morphology, compared to the base material in the circumference. In all zones of the welded tube circumference, retained austenite has been found in similar distributions. The mechanical testing of the individual tubes demonstrated that the Q&P treatments offer increased strength compared to all other states and significantly improved ductility compared to the quenched condition. Therefore, the approach of Q&P treatment of HFI-welded tubes represents a route for the mass production of high-strength tubular products with improved ductility.

京都大学 / 新制・課程博士 / 博士(工学) / 甲第23507号 / 工博第4919号 / 新制||工||1768(附属図書館) / 京都大学大学院工学研究科材料工学専攻 / (主査)教授 辻 伸泰, 教授 安田 秀幸, 教授 奥田 浩司 / 学位規則第4条第1項該当 / Doctor of Philosophy (Engineering) / Kyoto University / DFAM

The third-generation advanced high strength steels, AHSS, represent an opportunity for today’s steel development, where lighter materials with maintained strength and toughness are in demand. The unique properties of these materials often stem from a tailored microstructure. In the continued development of these steels, without relying on expensive alloying methods, process design in the form of precise heat treatments plays an increasingly important role. This work focuses on Medium Mn AHSS with the aim of investigating one of these heat treatments, intercritical annealing, which is essential for achieving the desired material properties. Experimental testing of annealing effects is acknowledged to be a challenging process, and this study aims to present a novel approach for these types of tests. During experimental testing of intercritical annealing, the thermomechanical testing system Gleeble 3800 is a recognized tool. The mounting technique employed in the Gleeble results in an inhomogeneous heat distribution in the samples, generating a thermal gradient. This report aims to utilize this gradient as an opportunity to test the effect of several intercritical annealing temperatures on one sample, thereby increasing the efficiency of experimental work. The method is based on data retrieved from thermocouples attached to the specimen during Gleeble trials with the intent to identify the thermal gradient. This data is combined with x-ray diffraction measurements where the retained austenite fraction is measured. Thermodynamic calculations of expected retained austenite fraction following intercritical annealing are performed parallel to experimental work. The results of this work show that it is possible to utilize the thermal gradient to retrieve extensive data regarding the effect of intercritical annealing using only one sample. The results show a distinct thermal gradient and a corresponding gradient of retained austenite fraction along the specimen. The results for retained austenite fraction at room temperature can be rationalized on the basis of computational predictions. These variations potentially arise due to the material not reaching equilibrium within the annealing timeframe. This conclusion is supported by other computational results concerning austenite composition. In summary, the present work illustrates a new approach streamlining experimental work that, with some refinements, has the potential to benefit the broader scienitific community, in addition to providing a powerful new tool for rapid technological advancement in the steel industry / Tredje generationens avancerade höghållfasta stål representerar en möjlighet för dagens stålutveckling där lättare material med bibehållen styrka och seghet efterfrågas. De unika egenskaperna hos dessa material härrör ofta frän en skräddarsydd mikrostruktur. Vid fortsatt utveckling av dessa stål är det önskvärt att minimera användningen av legeringsämnen, vilket betyder att processdesign i form av korrekta värmebehandlingar blir  av  stor  betydelse.  Detta  arbete  fokuserar  på  Medium  Mn  avancerade höghållfasta stål med syftet att undersöka en av dessa värmebehandlingar, interkritisk glödgning,  vilken  har  en  avgörande  betydelse  för  att  uppnå önskad  prestanda. Experimentell  testning  av  glödgningseffekter  anses  vara  en  utmanande  process och avsikten med denna studie är att presentera ett nytt tillvägagångssätt för denna typ av test. Under experimentell utvärdering av glödgningseffekter används ofta det termomekaniska testsystemet  Gleeble  3800.  Provmonteringen  i  Gleeblen  resulterar i en  inhomogen värmefördelning i proverna vilket medför en temperaturgradient. Denna rapport syftar till att använda gradienten som en möjlighet att testa effekten av flera  glödgningstemperaturer  på  ett  enda  prov  och  därigenom  öka  effektiviteten i det  experimentella  arbetet.  Metoden  grundas  på  data  från  termoelement  fästa  på provet under Gleebleförsök, med avsikt att identifiera den termiska gradienten. Denna data kombineras sedan med XRD-mätningar där austenitfraktion efter värmebehandling utvärderas.  Termodynamiska  beräkningar  av  förväntad  austenitfraktion  efter interkritisk glödgning genomförs parallellt med experimentellt arbete. Resultaten  från  detta  arbete  påvisar  att  den  presenterade  metoden  är  genomförbar då omfattande data gällande interkritisk glödgningseffekt grundat på endast ett prov erhålls. Resultaten visar en tydlig termisk gradient och en motsvarande gradient av austenitfraktion längs provet, vilka är i överensstämmelse med tidigare experimentella resultat för samma material. Resultaten för austenitfraktion vid rumstemperatur uppvisar  betydande  likheter  med  de  termodymiska  beräkningarna, med  några  undantag. Orsaken till dessa variationer ¨ar troligen en otillräcklig glödgningstid, vilket gör att  materialet  inte  når  jämvikt.  Denna  hypotes  stöds  av andra  beräkningsresultat gällande austenitens sammansättning. Sammanfattningsvis presenterar denna rapport ett nytt tillvägagångssätt för att effektivisera experimentellt arbete, som med vissa förbättringar har potential att gynna det bredare forskarsamhället.

O presente trabalho avaliou o efeito de tratamentos térmicos ou diferentes graus de deformação plástica na transformação da austenita do microconstituinte AM de uma chapa de aço alta resistência baixa liga (ARBL) classe API 5L X80 usada para gasodutos. A chapa tem espessura de 19 mm e passaria pelo processo de conformação UOE, mas a deformação foi realizada por laminação a frio, a temperatura ambiente, com reduções de 5 a 20%. O propósito foi compreender melhor o microconstituinte AM, explorar a transformação martensítica induzida por deformação (SIMT) e a decomposição austenítica por tratamento térmico, com ênfase em seu comportamento magnético. A transformação da austenita foi acompanhada através de medidas de polarização magnética, comparada com a densidade de massa e difração de raios X. A deformação plástica e os tratamentos térmicos alteraram a polarização magnética de saturação e a densidade de massa da amostra de aço de forma compatível com a eliminação da austenita retida metaestável. O método de densidade hidrostática foi considerado sensível para mensurar transformações de fase. Os dados obtidos revelam expansão volumétrica de aproximadamente 0,13%, correspondendo a 3,2% a quantidade de austenita retida original do material, enquanto os valores obtidos por polarização magnética de saturação são 2,8% pelo histeresígrafo e 2,1% por MAV. A difração de raios X nas amostras sob deformação ou tratamentos térmicos resultaram em queda nos primeiros picos da austenita quando comparadas com a amostra como recebida. / This study evaluated the effect of different degrees of plastic deformation or heat treatment on the transformation of austenite into martensite of an HSLA steel plate API 5L X80 for pipelines. A 19 mm thickness plate would be submitted to UOE forming process, but the cold work instead occurred by cold rolling at room temperature, with reductions of 5 up to 20%. The purpose was to better understand the MA constituent, explore the strain-induced martensitic transformation (SIMT) and austenitic decomposition by heat treatment with emphasis on its magnetic behavior. The transformation was accompanied by saturation magnetization measurements, compared with the mass density and X-ray diffraction. The plastic deformation or the heat treatment altered the saturation magnetization and the mass density in a manner consistent with the elimination of metastable retained austenite. The density method is sensible to measure phase transformations induced by strain. The data obtained shows a volumetric expansion of about 0.13%, corresponding to an amount of retained austenite of the original material of 3.2%, while the values obtained by magnetization saturation are 2.8% by hysteresigraph and 2.1% by VSM. By X-ray diffraction there is a clear drop in first peaks of austenite of the samples under deformation or heat treatment compared with the sample as-received.

O presente trabalho avaliou o efeito de tratamentos térmicos ou diferentes graus de deformação plástica na transformação da austenita do microconstituinte AM de uma chapa de aço alta resistência baixa liga (ARBL) classe API 5L X80 usada para gasodutos. A chapa tem espessura de 19 mm e passaria pelo processo de conformação UOE, mas a deformação foi realizada por laminação a frio, a temperatura ambiente, com reduções de 5 a 20%. O propósito foi compreender melhor o microconstituinte AM, explorar a transformação martensítica induzida por deformação (SIMT) e a decomposição austenítica por tratamento térmico, com ênfase em seu comportamento magnético. A transformação da austenita foi acompanhada através de medidas de polarização magnética, comparada com a densidade de massa e difração de raios X. A deformação plástica e os tratamentos térmicos alteraram a polarização magnética de saturação e a densidade de massa da amostra de aço de forma compatível com a eliminação da austenita retida metaestável. O método de densidade hidrostática foi considerado sensível para mensurar transformações de fase. Os dados obtidos revelam expansão volumétrica de aproximadamente 0,13%, correspondendo a 3,2% a quantidade de austenita retida original do material, enquanto os valores obtidos por polarização magnética de saturação são 2,8% pelo histeresígrafo e 2,1% por MAV. A difração de raios X nas amostras sob deformação ou tratamentos térmicos resultaram em queda nos primeiros picos da austenita quando comparadas com a amostra como recebida. / This study evaluated the effect of different degrees of plastic deformation or heat treatment on the transformation of austenite into martensite of an HSLA steel plate API 5L X80 for pipelines. A 19 mm thickness plate would be submitted to UOE forming process, but the cold work instead occurred by cold rolling at room temperature, with reductions of 5 up to 20%. The purpose was to better understand the MA constituent, explore the strain-induced martensitic transformation (SIMT) and austenitic decomposition by heat treatment with emphasis on its magnetic behavior. The transformation was accompanied by saturation magnetization measurements, compared with the mass density and X-ray diffraction. The plastic deformation or the heat treatment altered the saturation magnetization and the mass density in a manner consistent with the elimination of metastable retained austenite. The density method is sensible to measure phase transformations induced by strain. The data obtained shows a volumetric expansion of about 0.13%, corresponding to an amount of retained austenite of the original material of 3.2%, while the values obtained by magnetization saturation are 2.8% by hysteresigraph and 2.1% by VSM. By X-ray diffraction there is a clear drop in first peaks of austenite of the samples under deformation or heat treatment compared with the sample as-received.

Lors d’un recuit inter-critique d’un acier dit « Medium Manganèse », dont la teneur en Mn est située entre 4 et 12 %, avec une microstructure initiale complètement martensitique, la formation de l’austénite obéit à un mécanisme spécifique qui porte le nom d'ART - « Austenite Reverted Transformation » (transformation inverse de l’austénite). L’objectif de ce travail de thèse était d’étudier et de modéliser les évolutions microstructurales en lien avec les propriétés mécaniques lors d’un recuit ART. Il a été déterminé que la microstructure finale se compose de phases de nature (ferrite, austénite résiduelle et martensite de trempe) et morphologie (en forme d’aiguille et polygonale) différentes. Une attention particulière a été accordée aux cinétiques de dissolution des carbures et de formation de l’austénite. Une vision complète de ces processus a été construite. En outre, le mécanisme de stabilisation de l’austénite résiduelle à la température ambiante a été étudié et discuté. Enfin, des essais de traction ont été réalisés afin d’évaluer le comportement mécanique de l’acier après différents recuits ART et établir le lien avec la microstructure. Une analyse plus détaillée du comportement de chaque constituant de la microstructure a été effectuée. A l'issue de cette thèse, un modèle complet est disponible pour calculer les courbes de contrainte vraie - déformation vraie d’un acier Medium Mn / During the intercritical annealing of fully martensitic Medium Mn steel, containing from 4 to 12 wt.% Mn, the formation of austenite happens through the so-called “Austenite Reverted Transformation” (ART) mechanism. In this PhD work, the evolution of both microstructure and tensile properties was studied as a function of holding time in the intercritical domain. The microstructure evolution was studied using a double experimental and modeling approach. The final microstructure contained phases of different natures (ferrite (annealed martensite), retained austenite and fresh martensite) and of different morphologies (lath-like and polygonal). A particular attention was paid to the kinetics of austenite formation in connection with cementite dissolution and to the morphology of the phases. A mechanism was proposed to describe the formation of such microstructure. The critical factors controlling thermal austenite stability, including both chemical and size effects, were determined and discussed, based on the analysis of the retained austenite time-evolution. At last, tensile properties of the steel were measured as a function of holding time and the relation between microstructure and mechanical behavior was analyzed. Advanced analysis of the individual behavior of the three major constituents was performed. As a final output of this work, a complete model for predicting the true-stress versus true-strain curves of medium Mn steels was proposed

The use of pre-hardened mold steels has increased appreciably over the years; more than 80% of the plastic mold steels are used in pre-hardened condition. These steels are delivered to the customer in finished state i.e. there is no need of any post treatment. With hardness around ~40HRC, they have properties such as good polishability, good weldability, corrosion resistance and thermal conductivity. Machinability is a very important parameter in pre-hardened mold steels as it has a direct impact on the cost of the mold. In normal machining operations involving intricate or near net shapes, machining constitutes around 60% of the total mold cost. Efforts are underway to explore every possible way to reduce costs associated with machining and to make production more economical. All the possible parameters which are considered to affect the machinability are being investigated by the researchers. This thesis work focuses on the effect of prior austenite grain size on the machinability of pre-hardened mold steel (Uddeholm Nimax).  Austenitizing temperatures and holding times were varied to obtain varying grain sized microstructures in different samples of the same material. As it was difficult to delineate prior-austenite grain boundaries, experimental and empirical methods were employed to obtain reference values. These different grain sized samples were thereafter subjected to machining tests, using two sets of cutting parameters. Maximum flank wear depth=0.2mm was defined for one series of test which were more akin to rough machining, and machining length of 43200mm or maximum wear depth=0.2mm were defined for second series of tests which were similar to finishing machining. The results were obtained after careful quantative and qualitative analysis of cutting tools. The results obtained for Uddeholm Nimax seemed to indicate that larger grain sized material was easier to machine. However, factors such as retained austenite content and work hardening on machined surface, which lead to degradation of machining operations were also taken into consideration. Uddeholm Nimax showed better machinability in large grained samples as retained austenite(less than 2%) content was minimal in the large grained sample. Small grained sample in Uddeholm Nimax had a higher retained austenite (7+2%) which resulted in degradation of machining operation and a lesser cutting tool life.