The goal of this thesis is to determine the relationship between the macroscopic stress and the macroscopic strain for a variety of complex multiphase materials exhibiting rate-independent non-linear response at the micro-scale, based on experimental data obtained both at the local and macroscopic scales. A micro-macro secant mean field model (SMF model) based on the result of Eshelby and the approach of Mori and Tanaka is developed to model the behaviour of three particular systems which we have worked out by ourselves: 1) a ferrite-martensite steel produced by rolling in which we quantify the plastic anisotropy due to the morphological texture in terms of the Lankford's coefficient and pseudo yield surface; 2) a composite made of two continuous and interpenetrating phases: an aluminium matrix reinforced by a preform of sintered Inconel601 fibres. We quantify the coupled effects of temperature and phases co-continuity on the phases and overall stresses; 3) a TRIP-aided multiphase steel, in which the dispersed metastable austenite phase transforms to martensite. We derive the relationship between the overall uniaxial elastoplastic response and the progress of phase transformation, itself influenced by the thermodynamical, microstructural and mechanical properties. The stress-state dependence of the martensitic transformation is enlightened and explained. We demonstrate the existence of thermomechanical treatments leading to optima of ductility and strength-ductility balance. Finally, we show that the formability of TRIP-aided multiphase steels depends on the stability criterion.

TRIP-assisted multiphase steels exhibit an excellent balance of strength and ductility, which makes them very attractive for the automotive industry. These remarkable mechanical properties can be attributed mainly to the continuous transformation of retained austenite into martensite during straining (TRansformation Induced Plasticity). The aim of this thesis was to clarify the interaction between the hot rolling conditions, the formation of microstructure, and the resulting mechanical properties. Various rolling simulation techniques were employed to determine how the composite microstructure is formed during the various steps of multi-stage thermomechanical processing. The interaction between deformation and phase transformation is highlighted, particularly from the viewpoint of the transformation texture.

TRIP-assisted multiphase steels exhibit an excellent balance of strength and ductility, which makes them very attractive for the automotive industry. These remarkable mechanical properties can be attributed mainly to the continuous transformation of retained austenite into martensite during straining (TRansformation Induced Plasticity). The aim of this thesis was to clarify the interaction between the hot rolling conditions, the formation of microstructure, and the resulting mechanical properties. Various rolling simulation techniques were employed to determine how the composite microstructure is formed during the various steps of multi-stage thermomechanical processing. The interaction between deformation and phase transformation is highlighted, particularly from the viewpoint of the transformation texture.

Transformation-induced plasticity (TRIP) steels have excellent strength, ductility and work hardening behaviour, which can be attributed to a phenomenon known as the TRIP effect. The TRIP effect involves a metastable phase, retained austenite (RA), transforming into martensite as a result of applied stress or strain. This transformation absorbs energy and improves the work hardening rate of the steel, delaying the onset of necking. This work describes two distinct TRIP steel microstructures and focuses on how microstructure affects the RA-to-martensite transformation and the uniaxial tensile behaviour. A two-step heat treatment was applied to an aluminum-alloyed TRIP steel to obtain a microstructure consisting of equiaxed grains of ferrite surrounded by bainite, martensite and RA -- the equiaxed microstructure. The second microstructure was produced by first austenitizing and quenching the steel to produce martensite, followed by the two-step heat treatment. The resulting microstructure (labelled the lamellar microstructure) consisted of elongated grains of ferrite with bainite, martensite and RA grains. Both microstructural variants had similar initial volume fractions of RA. A series of interrupted tensile tests and ex-situ magnetic measurements were conducted to examine the RA transformation during uniform elongation. Similar tests were also conducted on an equiaxed microstructure and a lamellar microstructure with similar ultimate tensile strengths. Results show that the work hardening rate is directly related to the RA transformation rate. The slower transformation rate, or higher RA stability, that was observed in the lamellar microstructure enables sustained work hardening at high strains. In contrast, the equiaxed microstructure has a lower RA stability and thus exhibits high values of work hardening at low strains, but the effect is quickly exhausted. Several microstructural factors that affect RA stability were examined, including RA grain size, aspect ratio, carbon content and spatial distribution of the phases. Two of these factors were characteristic of only the lamellar microstructures and led to higher RA stabilities: elongated RA grains and RA grains being primarily surrounded by bainite. The results were also compared with previous work on a silicon-alloyed TRIP steel to show that the aluminum-alloyed compositions could achieve similar, if not better, combinations of strength and ductility. / Thesis (Master, Mechanical and Materials Engineering) -- Queen's University, 2012-09-24 16:52:28.032

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.

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.

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