Orientador: Rubens Caram Junior / Tese de Doutorado - Universidade Estadual de Campinas, Faculdade de Engenharia Mecânica / Made available in DSpace on 2018-08-22T19:13:03Z (GMT). No. of bitstreams: 1 Contieri_RodrigoJose_D.pdf: 5581364 bytes, checksum: b95f94b00d984d338e4134cd12621962 (MD5) Previous issue date: 2013 / Resumo: Ligas do sistema Ti-Cu com composições próximas à eutetóide exibem potencial para aplicações estruturais, pois apresentam interessantes propriedades mecânicas, baixa densidade e alta resistência à corrosão. O comportamento mecânico dessas ligas depende diretamente das condições de processamento e tratamentos térmicos aplicados. Em condições de equilíbrio, a microestrutura dessas ligas é formada pela fase ? e pelo composto intermetálico Ti2Cu. Dependendo das condições de processamento, estruturas metaestáveis podem ser formadas. O objetivo deste trabalho foi avaliar o efeito de diferentes tratamentos térmicos na microestrutura e nas propriedades mecânicas de ligas Ti-Cu. Inicialmente, amostras com composições hipoeutetóide, eutetóide e hipereutetóide foram resfriadas a partir de altas temperaturas em um dispositivo de ensaio Jominy modificado e por ensaios de "splat colling". Na sequência, ensaios de envelhecimento aplicados a amostras com microestruturas metaestáveis também foram realizados. A caracterização das amostras envolveu microscopia óptica, eletrônica de varredura e de transmissão, difração de raios-X, tomografia atômica tridimensional e ensaios mecânicos. Os resultados obtidos indicam que altas taxas de resfriamento resultam na formação de microestruturas formadas por martensita ? ' e pelo composto Ti2Cu com composições diferentes das de equilíbrio. O módulo de elasticidade não apresentou variação com a taxa de resfriamento. Resultados de envelhecimento sugerem que o máximo valor de dureza Vickers e de resistência mecânica correspondem à perda de coerência entre os precipitados do composto intermetálico Ti2Cu e a matriz de fase ? / Abstract: Alloys in the Ti-Cu system with compositions close to the eutectoid exhibit potential for structural applications because they present interesting mechanical properties, low density and high corrosion resistance. The mechanical behavior of these alloys depends directly on the processing conditions and heat treatments applied. Under equilibrium conditions, the microstructure of these alloys is formed by the ? phase and the Ti2Cu intermetallic compound. Depending on the processing conditions imposed, metastable structures may be formed. The aim of this study was to evaluate the effect of different heat treatments on the microstructure and mechanical properties of Ti-Cu alloys. Initially, sample of hypoeutectoid, eutectoid and hypereutetoid compositions were cooled from high temperatures by in a modified Jominy test setup and by the "splat cooling technique". Following, aging heat treatments were applied to the samples with metastable microstructures. The sample's characterization included optical microscopy, scanning and transmission electron microscopy, X-ray diffraction, 3-dimensional atomic tomography and mechanical testing. The results suggests that high cooling rates result in the formation of microstructures formed by martensite ? ' and the Ti2Cu compound with compositions different from the equilibrium composition. The elastic modulus does not vary with the cooling rate. Aging results suggest that the maximum values of Vickers hardness and mechanical strength correspond to the loss of coherence between the Ti2Cu intermetallic compound precipitates and the ? phase matrix / Doutorado / Materiais e Processos de Fabricação / Doutor em Engenharia Mecânica

Dans le cadre de ces travaux, il a clairement été établi que l’hydrogène piégé ou diffusible pouvait avoir une forte influence sur les propriétés mécaniques des matériaux. Cependant, cet effet varie de façon importante en fonction de leur microstructure, leur composition chimique et leur traitement thermique. En effet, les aciers martensitiques trempés/revenus dédiés à des tubes pour des milieux sous-service présentent, de par leur structure, différents types de pièges tels que les dislocations, les joints de grains, les précipités, les inclusions, les lacunes et d’autres interfaces qui jouent un rôle important dans les mécanismes endommageants. Ces aciers de haute résistance mécanique, lorsqu’ils sont soumis à des contraintes mécaniques et à un environnement agressif (qui dépend de la pression en H2S et du pH de la solution) peuvent rompre à cause du phénomène de Sulphide Stress Cracking (SSC). Ce dernier est une forme de fragilisation par l’hydrogène (FPH) qui inclut un amorçage de fissure suivi d’une étape de propagation conduisant à la rupture, dont la contribution de l’hydrogène reste encore mal comprise. En parallèle de l’impact de la microstructure de l’acier, les champs de contrainte et déformation subis par le matériau modifient les effets induits par l’hydrogène. C’est pourquoi un montage de perméation sous contrainte a été utilisé afin de pouvoir réaliser des essais mécaniques jusqu’à rupture sous flux d’hydrogène et les comparer au comportement du matériau lorsque celui-ci est sollicité à l’air ou dans un environnement H2S. Ainsi, l’impact sur le comportement mécanique du flux d’hydrogène mais également de son piégeage peut être étudié. Dans ce cadre, des éprouvettes plates et axisymétriques, lisses et entaillées ont été employées. Les informations expérimentales obtenues dans ce travail ont servi à alimenter un modèle numérique qui a permis de caractériser localement l’état mécanique et les concentrations d’hydrogène piégé et diffusible dans le matériau. Ceci a rendu possible la définition d’un critère local de rupture. / The findings of this work established that the diffusible and trapped hydrogen could have a strong influence on the mechanical properties of materials. However, this effect varies significantly with the materials’ microstructure, chemical composition, and heat treatment. Due to their structure, quenched and tempered martensitic steels (developed for tubes suitable for sour service environments) have different types of traps such as dislocations, grain boundaries, precipitates, inclusions, vacancies and other interfaces that play an important role in the damage mechanisms. These high strength steels may break due to Sulphide Stress Cracking (SSC) if subjected to mechanical stress and an aggressive environment (which depends on the H2S partial pressure and pH solution). This phenomenon is a form of hydrogen embrittlement (HE) that includes a crack initiation followed by a propagation step leading to failure. However the hydrogen contribution is still insufficiently understood. In addition to the impact of the microstructure on the steel, the stress and the deformation fields in the material also modify the effects induced by hydrogen. To investigate this event, electrochemical permeation tests under stress were used to perform mechanical tests under hydrogen flux until failure is reached. The results were compared to those mechanically loaded in air or in a H2S environment. This enabled the examination of the impact of the hydrogen flux and trapping on the mechanical behavior of martensitic steel. In this framework, flat and axisymmetric, smooth and notched specimens were employed. Experimental data obtained in this work were used to provide a numerical model that enables the locally characterization of the mechanical condition and the concentrations of trapped and diffusible hydrogen in the material. These outcomes enabled us to determine a local failure criterion.

This work deals with the modelling of shape-memory alloys, in particular with the steady-state model of martensitic thin films. After the introductory motivation the crystallographic structure of the materials is described followed by the introduction of the link between the lattice and continuum model. The next parts of the work focus on the possible solutions of the given 3D variational problem (quasiconvexification, Young measures) and on derivation of thin film theories with the aid of different tools (regularization,-convergence). The last part takes over an approximation of an obtained model and sketches numerical experiments on a Ni-Mn-Ga alloy.

The purpose of the work presented in this thesis was to explore and understand the mechanisms governing toughness, ductility and ballistic performance in a class of nanostructured carbide-free bainite-austenite steels, sometimes known as ‘superbainite’. The mechanical properties of these alloys have been extensively reported, but their interpretation is not clear. The thesis begins with an introduction to both the relevant nanostructures and some of the difficulties involved in explaining observed properties, alongside a summary of the role of mixed- microstructures in alloy development. An overview of the debate regarding the mechanism of bainite formation is pre- sented in Chapter 2, in the form of a literature survey encompassing the period of explicit recognition of the bainite microstructure. Of note is the role played by the displacive theory of formation in the development of the alloy structures investigated in this thesis. A characterisation of a commonly available bainitic alloy forms the basis for Chapter 4. Observations confirm the nanoscale nature of the structure, although additional phases are found to be present, namely: cementite and martensite. This is explained as resulting from relatively low alloying additions and chem- ical segregation effects, which are modelled using thermodynamic and kinetic approaches. Chapters 5 and 6 contain a comprehensive study of the response of this alloy to the stress concentration present at the notch root of a Charpy impact sample. The work provides evidence of notch root embrittlement due to stress-induced martensite transformation. Results from synchrotron and laboratory X-ray experiments in particular reveal that machining, as well as applied stress, can initiate the austenite-martensite transformation, and methods to mitigate this effect are suggested. An innovative approach is harnessed in Chapter 7, in order to identify exper- imentally the volume fraction at which three-dimensional connectivity (‘percolation’) of austenite is lost in a superbainitic steel. Hydrogen thermal desorption techniques are applied to this problem, inspired by the tendency of such alloys to undergo tensile failure with limited or zero necking. The striking result sheds light on the importance of austenite morphology in restricting the diffusion of hydrogen into a mixed structure. The final set of experimental work is directed towards understanding the damage mechanisms that occur during projectile penetration of a coarser bainitic armour- plate alloy. The formation of adiabatic shear bands is found to be a dominant factor governing the ballistic failure of the plate. The sheared material undergoes severe high-temperature deformation, but does not change phase upon cooling, leading to the proposal of certain methods that could be implemented to improve ballistic resistance of the steel. The totality of the research presented herein is summarised in Chapter 9, which draws attention to new areas of interest that have arisen from the current work, proposing several future directions of investigation. The broader issue of understanding, common to all studies performed thus far, is that of the causes, effects, and extent, of stress-induced transformation to martensite experienced by the retained austenite that is a key feature of superbainite and similar steels.

No description available.

Les Transformation Martensitiques (TM) sont des transitions du premier ordre entre des phases cristallines qui caractérisent une classe intéressante de matériaux intelligents, les Alliages à Mémoire de Forme (AMF). Ces alliages métalliques furent découverts dans les années 1930 environ. Ils sont surtout intéressants car ils combinent deux effets particuliers : l'effet de mémoire de forme et la pseudo-élasticité. L'effet mémoire de forme consiste à mémoriser une configuration particulière et la retrouver après des cycles thermiques ou mécaniques. La Pseudo-Elasticité consiste à rejoindre des niveaux de déformation très grands qui sont, en général, plus typiques du caoutchouc que des métaux. Dans cette thèse, nous avons traité la caractérisation des transformations martensitiques en analysant des points de vue différents. La compréhension du fonctionnement des AMFs est fondamentale pour plusieurs types d'applications industrielles. Elle constitue encore un domaine de recherche très ouvert. (...) / This thesis deals with the characterization of Martensitic Transformations (MT) that are first order phase transitions among different solid states with different crystalline structures. These transitions are at the basis of the behavior of a class of smart materials, called Shape Memory Alloys (SMA). This work combines an experimental study of a mechanically-induced martensitic transformation in a Cu-Al-Be single crystal and a macroscopic model for the reproduction of permanent effects in cyclic temperature-induced and stress-induced transitions. From the experimental point of view, the novelties are in the device that has been built and used for the test and in the full-field measurement technique at the basis of the data treatment. The especially designed gravity-based device allows for a uni-axial and uni-directional tensile test with slow loading rates. Simultaneously, the full-field measurement technique, known as grid method, provides high-resolution two-dimensional strain maps during all the transformation. With all the data collected during the test, we characterize for the first time the two-dimensional strain intermittency in a number of ways, showing heavy-tailed distributions for the strain avalanching over almost six decades of magnitude. In parallel, we develop a macroscopic mathematical model for the description of fatigue and permanent effects in several kinds of martensitic transformations. We show an easy way to calibrate the model parameters in the simple one-dimensional case. Moreover, we compare the numerical results with experimental data for different tests and specimens and obtain a good qualitative agreement.

The final thesis deals with martensitic stainless steel and their mechanical properties. The theoretical part consists of information about corrosion, chemical composition, heat treatment and mechanical properties of various types of steel. The practical part deals with the influence of the cooling rate during heat treatment and nickel content on the mechanical properties and microstructure of the GX4CrNi13-4 steel.

Cette thèse a été centrée sur l’étude de la formation d’une phase martensitique dans les aciersFe-Ni-C et sur la diffusion des atomes de carbone dans cette phase à basse température. Lamodélisation à l’échelle atomique a été utilisée. Pour décrire ces phénomènes, deux approchesont été développées: un modèle discret basé sur la théorie de la fonction de densité atomique(ADF) et une approche quasiparticulaire basée sur la théorie atomique de Fratons (AFT). Dansun premier temps, pour montrer l’universalité de notre approche, nous avons appliqué l'AFTpour modéliser la cinétique d'auto-assemblage des atomes initialement désordonnés à desstructures ordonnées complexes. Cette approche a ensuite été appliquée à l'étude detransformation austénite/martensite. Il a été montré que le germe de martensite se développecomme agrégat multivariant dans la matrice austénitique. En utilisant des figures de pôles etdes diagrammes de diffraction simulés, ces variants ont été identifiés et comparés aux donnéesexpérimentales. La diffusion du carbone dans la phase de martensite a été étudiée en utilisantla théorie ADF. Deux systèmes avec différentes propriétés élastiques, Fe-C et Fe-Ni-C, ont étéconsidérés. Il a été montré qu’au cours du premier stade de vieillissement, les atomes decarbone subissent une décomposition spinodale sur les interstices octaédriques du réseautétragonal centré de martensite et forment les zones riches en carbone. Ensuite, la morphologie«tweed-like» des zones riches en carbone est développée. Les résultats des simulations sontun bon accord avec les images expérimentales obtenues par sonde atomique tomographique.La relation entre une mise en ordre de Zener et la concentration des zones riches en carbone aété discutée. / This thesis examines the formation of martensite in Fe-Ni-C steels and the diffusion of carbonatoms in this phase at low temperatures. To achieve this goal the atomistic modeling have beenused. To describe these phenomena two different approaches were developed: a discretemodel based on the Atomic Density Function (ADF) theory and the quasiparticle approachesbased on the Atomic Fraton Theory (AFT). First, the AFT was tested to model a self-assemblykinetics of initially disordered systems to three different classes of ordered one: singlecomponent crystals with fcc and diamond structures, two component crystals with zinc-blendstructure, and polymers with single-strand and double-stranded helixes structures. Then thisapproach was applied to model austenite/martensite transformation. It was shown thatmartensite nucleus grows as multivariant aggregate in austenite matrix. Using pole figures andsimulated diffraction patterns these variants were identified and compared with the experimentaldata. The carbon diffusion in martensite phase was studied using ADF theory. Two systemswith the different elastic properties corresponding to the Fe-C and Fe-Ni-C systems wereconsidered. It was shown that during a first stage of aging the carbon atoms undergo a spinodaldecomposition on the octahedral interstices of bcc lattice and form the carbon-rich zones. Then"tweed-like" morphology of carbon-rich zones is developed. The simulations results are a goodagreement with experimental images obtained by atom probe tomography. The relationbetween Zener ordering and the concentration of carbon reach zones is discussed.

A newly developed martensitic stainless steel powder, called “powder A”, designed for surface coating with laser cladding and PTA cladding was characterized. The purpose with powder A is to achieve both good corrosion resistance and wear resistance in a stainless steel grade. The investigation of powder A was divided into cladding characterization, microstructural investigation and a property comparison to existing grades 316 HSi and 431 L. Powder A was successfully deposited with laser cladding, exhibiting a wide process window, and PTA cladding. In both cases no preheating was required and no cracks were formed. The microstructure examination indicates that powder A has a martensitic structure possibly containing small amounts of ferrite in the grain boundaries. Thermodynamic calculations in computer software Thermo-Calc 4.1 supported this theory. The microstructure of powder A proved to be very stable over a wide range of cladding parameters. Powder A was significantly harder than 316 HSi and 431 L and had better corrosion resistance than 431 L in a chloride environment. Powder A had similar corrosion properties as 316 HSi in the experiments made .The wear performance of the powder A coatings was similar to 431 L. This was surprising since the hardness of the powder A coatings is significantly higher compared to 431 L.

Intercritically austempered ductile iron (IADI) with a matrix microstructure of ferrite plus metastable austenite has an excellent combination of strength and toughness. The high strength and good ductility of this material is due to the transformation of metastable austenite to martensite during deformation. In the present study, the transformation of austenite to martensite for intercritically austempered ductile irons of varying alloy chemistry (varying amounts of nickel and/or manganese) were examined using in-situ neutron diffraction under strain-controlled loading at VULCAN at the Spallation Neutron Source at Oak Ridge National Laboratory (ORNL). Both diffraction and tensile data were collected and synced using the VDRIVE software (a proprietary ORNL software package). The single peak fit method was employed in the analysis of the diffraction data. In this thesis, the stress and strain for the start of the transformation of metastable austenite to martensite were determined. The development of residual stresses during deformation and the elastic diffraction constants for both the ferrite and austenite phases were also determined. The material was characterized using optical microscopy, backscattered imaging in the scanning electron microscopy, energy dispersive spectroscopy and transmission electron microscopy. / Master of Science