Orientador: Rubens Caram Júnior / Dissertação (mestrado) - Universidade Estadual de Campinas, Faculdade de Engenharia Mecânica / Made available in DSpace on 2018-08-23T05:01:49Z (GMT). No. of bitstreams: 1 Verissimo_NathaliaCarolina_M.pdf: 4539752 bytes, checksum: 5f6eb6507fb9a034b3aca9ed35fdea93 (MD5) Previous issue date: 2013 / Resumo: Ligas de Ti do tipo 'beta' contendo elementos biocompatíveis são potencialmente interessantes em aplicações ortopédicas e odontológicas. Enquanto as propriedades mecânicas dessas ligas podem ser controladas por meio de tratamentos térmicos, suas propriedades de superfície podem ser otimizadas por meio da formação de camada de nanotubos de TiO2 usando processos de anodização. Neste trabalho, amostras de Ti CP e das ligas Ti-35Nb e Ti-35Nb-4Sn, obtidas por fusão a arco voltaico em atmosfera inerte, foram anodizadas sob potencial constante de 20V durante 1 hora, usando uma solução aquosa de HF, a fim de obter uma camada de nanotubos de TiO2 amorfa. Tais camadas amorfas foram tratadas termicamente visando promover transformações de fase amorfo-anatase e anatase-rutilo. As amostras foram caracterizadas por meio de microscopia eletrônica de varredura. Os resultados obtidos indicam que camadas amorfas de nanotubos de TiO2 com espessura superior a 800 nm foram produzidas. Tratamentos térmicos combinados com ensaios de difração de raios-X permitiram identificar a formação de anatase em 225ºC em Ti CP, em 295ºC na liga Ti-35Nb e em 392ºC na liga Ti-35Nb-4Sn. A estrutura cristalina do rutilo foi observada no Ti CP em 398ºC e em 557ºC na liga Ti-35Nb. A formação de cristais de rutilo sobre a liga Ti-35Nb-4Sn ocorreu em 605ºC. Observou-se que o Nb combinado com Sn tem forte efeito estabilizador da fase anatase. Medidas de molhabilidade indicam que a fase anatase apresenta valores elevados de ângulo de contato, enquanto que a fase rutilo exibe valores menores e com características hidrofílicas. Os resultados obtidos sugerem que a combinação anatase-rutilo é a mais adequada para aplicações biomédicas e crescimento celular por não ser altamente hidrofílica / Abstract: 'beta' type Ti alloys containing biocompatible elements are potentially interesting for orthopedic and dental applications. While the mechanical properties of these alloys can be controlled by means of heat treatments, its surface properties can be optimized by formation of TiO2 nanotube layer using anodizing processes. In this work, samples of CP Ti and Ti-35Nb and Ti-35Nb-4Sn alloys obtained by arc melting under inert atmosphere were anodized using HF-based electrolyte for 1 hour, obtaining amorphous layers of TiO2 nanotubes. These layers were heat treated aiming to promote the amorphous structure and phases like anatase, mixture anatase-rutile and rutile. Samples were characterized by scanning electron microscopy. The results indicate that amorphous layers of TiO2 nanotubes with a thickness exceeding 800 nm were produced. Heat treatments combined with X-ray diffraction experiments allowed identifying the formation of anatase at 225ºC in CP Ti, at 295ºC in the Ti-35Nb alloy and at 392ºC in the Ti-35Nb-4Sn alloy. The crystal structure of rutile was observed in CP Ti at 398ºC and at 557ºC in the alloy Ti-35Nb. The formation of rutile crystals on the alloy Ti-35Nb-4Sn occurred at 605°C. It was observed that Nb combined with Sn shows a strong stabilizing effect of anatase. Wettability measurements indicate that the anatase phase shows high values of contact angle, while the rutile phase exhibits lower values and hydrophilic characteristics. The results suggest that the combination anatase-rutile is the most suitable for biomedical applications and cell growth because they are not highly hydrophilic / Mestrado / Materiais e Processos de Fabricação / Mestra em Engenharia Mecânica

Orientador: Rubens Caram Junior / Tese (doutorado) - Universidade Estadual de Campinas, Faculdade de Engenharia Mecânica / Made available in DSpace on 2018-08-21T09:06:40Z (GMT). No. of bitstreams: 1 Cremasco_Alessandra_D.pdf: 50106196 bytes, checksum: 2a7da86acd168979590189fcdb26056f (MD5) Previous issue date: 2012 / Resumo: Ligas de titânio com altos teores de elementos _ estabilizadores, solubilizadas em altas temperaturas e resfriadas rapidamente exibem limitada resistência mecânica e boa ductilidade, o que e resultado da formação de martensita ortorrômbica ou da manutenção da fase _ metaestável. Tal resistência pode ser significativamente aumentada por meio da aplicação de tratamentos térmicos de envelhecimento, que promovem a precipitação de novas fases, combinados com encruamento produzido por deformação plástica a frio. Este trabalho teve como objetivo o desenvolvimento de ligas do sistema Ti-Nb-Sn com propriedades mecânicas otimizadas visando sua utilização como biomaterial. Inicialmente, ligas de titânio com diferentes elementos de liga foram submetidas a ensaios de citocompatibilidade in vitro. Os resultados obtidos sugerem que ligas Ti-Nb-Sn sao biocompativeis. Na sequencia, amostras de ligas Ti-Nb-Sn preparadas em forno de fusao a arco foram tratadas termicamente objetivando homogeneizacao quimica e microestrutural, solubilizadas em alta temperatura, resfriadas rapidamente e deformadas plasticamente a frio. Tais amostras foram tratadas termicamente para promover a recuperacao, a recristalizacao e o envelhecimento da microestrutura. Os resultados obtidos indicam que a aplicacao de deformacao plastica e recozimento produz o refinamento da microestrutura. A aplicacao de tratamentos termicos de envelhecimento a 350 °C resultou na decomposicao da fase martensita ortorrombica e na formacao das fases _, w e a. Constatou-se que o comportamento mecanico das amostras envelhecidas reflete a combinacao das fases e suas respectivas fracoes volumetricas. O refino microestrutural e a precipitação da fase a resultaram em expressivo aumento da dureza, modulo de elasticidade e resistencia mecanica, bem como na queda da ductilidade. Finalmente, a aplicacao de condicoes de processamento otimizadas resultou em amostras com elevada resistencia mecanica e razoavel ductilidade. A liga Ti-35Nb-4Sn apresentou reduzido modulo de elasticidade e alta resistencia a tracao, condicao ideal para aplicacao biomedica / Abstract: Titanium alloys with high _ stabilizing elements content, solution heat treated at high temperatures and rapidly cooled to room temperature, exhibit limited mechanical strength and good ductility as a result of orthorhombic martensite formation or maintenance of the _ metastable phase. However, mechanical strength may be significantly improved by applying aging heat treatment, which leads to precipitation of new phases, combined with hardening provided by cold plastic deformation. The aim of this work is the development of alloys in the Ti-Nb-Sn system with optimized mechanical properties to be applied as biomaterial. Initially, titanium alloys with different alloying elements were tested in terms of cytocompatibility. The results suggest that Ti-Nb-Sn alloys are biocompatible. Following, Ti-Nb-Sn samples were prepared in arc furnace, heat treated aiming chemical and microstructural homogeneity, solution heat treated at high temperature, rapidly cooled to room temperature and cold plastically deformed. These samples were heat treated to promote recovery, recrystallization and aging of the microstructure. The results indicate that application of plastic deformation and annealing produces very refined microstructure. Application of aging heat treatments at 350 ° C resulted in decomposition of orthorhombic martensite phase and formation of _, w and a phases. It was found that mechanical properties of aged samples reflect the combination of such phases and their volume fractions. Microstructural refinement and a phase precipitation resulted in significant increase in hardness, elastic modulus and mechanical strength, as well as a decrease in ductility. Finally, application of optimal processing conditions resulted in samples with high mechanical strength and reasonable ductility. The Ti-35Nb-4Sn alloy showed lower elastic modulus and superior tensile strength. These results consist in ideal conditions for biomedical applications / Doutorado / Materiais e Processos de Fabricação / Doutora em Engenharia Mecânica

Deux problèmes surviennent lorsque nous étudions les effets du grenaillage de précontrainte sur le processus de la fatigue. Le premier est la caractérisation des contraintes résiduelles (CR) et de l’écrouissage. Le second est l’évolution de CR et de l’écrouissage pendant le cyclage.Pour résoudre le premier problème, cette thèse propose une méthode pour mesurer les contraintes et l’écrouissage par nanoindentation. Ici, l’écrouissage est représenté par la déformation plastique cumulée (PP). A l’aide d’une série de simulations par éléments finis (MEF) en supposant le comportement du matériau connu, les réponses obtenues par indentation permettent d’obtenir simultanément contrainte et déformation plastique. Bien que satisfaisante d’un point vue numérique, les performances expérimentales obtenues sur un alliage de titane temps T40 restent insuffisantes. Cependant, si le profil de contrainte est connu, on peut toutefois obtenir le profil de déformation plastique. Les biais induits par la préparation de la surface ont été analysés en détail. Pour le second problème, une série d'essais de fatigue ont été effectués sur un alliage Ti-18. Quatre traitements ont été testés sur 100 cycles sous 3 amplitudes différentes de déformation. Des mesures par diffraction des rayons X ont montré que la relaxation des contraintes et l’adoucissement cyclique augmentent avec l'amplitude de déformation. Les essais d’indentation ont montré un adoucissement de la couche grenaillée / There are two problems when investigating the effects of shot-peening on fatigue process. The first one is characterizing residual stresses (RS) and strain hardening (WH) on the sample surface. The second one is the evolution of RS and WH during fatigue. In order to solve the first problem, this thesis proposes a “simultaneous function method” to measure RS and WH with nanoindentation. Accumulated plastic strain (PP) is used to represent WH. Then, by establishing functions of normalized indentation responses through a series of finite element method (FEM) simulations, normalized indentation responses obtained from nanoindentation experiments can be used to extract RS and PP values, assuming that the constitutive behavior is known. Although the simultaneous function method shows fairly high accuracy from a pure numerical view point, experiments performed on T40 commercial pure titanium are not completely satisfying. However, if the residual stress profile is known, the method can be used to derive the work hardening profile.In order to study the second problem, a series of strain-controlled fatigue tests are performed on Ti-18 alloy. Fatigue specimens of 4 material states, including raw, shot-peened, prestrained and prestrained + shot-peened, were tested under 3 different strain amplitudes over 100 cycles. X-ray diffraction tests on the sample surfaces showed that the RS relaxation and the cyclic softening increase together with the strain amplitude. IIT tests showed that shot-peening may induce a softening of the surface of Ti-18 alloy samples

Les matériaux super-élastiques sous forme de couche minces présentent un domaine d’applications assez large. Grâce à leur aptitude à accommoder de grandes déformations de manière réversible, les films super-élastiques peuvent être utilisés comme sous couches entre le substrat et les revêtements dures. Cela permet d’améliorer significativement de nombreuses propriétés telles que : l’adhésion, le taux d’usure et le coefficient de frottement. Elles peuvent également être utilisées dans la fabrication des dispositifs médicaux tels que les stents. Bien que les alliages β-métastable à base de titane présentent des propriétés remarquables, une grande partie de la littérature publiée sur les films super-élastiques est consacrée aux alliages Ni-Ti. Ainsi, le but de ce travail est de développer de nouvelles couches super-élastiques de type β-métastable, obtenues par pulvérisation cathodique magnétron. Dans ce sens, deux types d’alliages ont été étudiés, les alliages binaires Ti-Nb et l’alliage quaternaire Ti-Nb-Ta-Zr. Après une description du dispositif expérimental utilisé pour la synthèse des couches, nous étudions plus particulièrement l’influence des paramètres de dépôt sur les propriétés des revêtements. La morphologie des revêtements a été caractérisée par microscope électronique à balayage. La diffraction de rayons X a été employée pour l’étude de la microstructure et la texture des films déposés. Enfin, l’effet super-élastique a été caractérisé par deux méthodes, l’indentation sphérique et la compression de micro-piliers usinés par faisceau d’ions focalisés / Superelastic thin films have a fairly wide field of applications. Thanks to their ability to accommodate a large deformation reversibly, superelastic films may be used as intermediate layers between the substrate and the hard layers. This significantly improves many properties such as adhesion, wear and coefficient of friction. They can also be used in the manufacture of medical devices such as stents. Although β-metastable titanium-based alloys have excellent properties, much of the published literature on the superelastic films is devoted to Ni-Ti. Thus, the purpose of this work is to develop new superelastic β-metastable titanium-based films, obtained by magnetron sputtering. After describing the experimental device used for the synthesis of thin films, we study more specifically the influence of deposition parameters on the properties of coatings. The morphology was characterized by the observation of fractured cross-sectional by scanning electron microscope. The X-ray diffraction was used to study the microstructure and texture of the deposited films. Finally, the superelastic effect was characterized by two methods, the spherical indentation and micro-pillars compression machined by focused ion beam

Le but de ce travail de thèse est de mieux comprendre les mécanismes de déformation à température ambiante dans les alliages de titane bêta-métastable Ti17 et Ti5553. Les microstructures étudiées sont composées de grains bêta transformé, dans lesquels la phase alpha peut précipiter, selon les relations de Burgers, sous la forme de douze variants différents. Une approche multi-échelles est donc préconisée avec trois niveaux représentatifs: macroscopique, mésoscopique (ex-grains bêta), et microscopique (variants alpha et matrice bêta de chaque grain). Différents modèles à champs moyens sont adaptés pour reproduire le comportement mécanique du Ti17 et du Ti5553. Ces modèles impliquent deux transitions d'échelle, et sont basés sur l'homogénéisation des comportements locaux, avec plusieurs manières de représenter les interactions intergranulaires. Les relations entre microstructures et propriétés mécaniques sont également considérées. Les modèles les plus complexes développés dans cette étude vont permettre de simuler l'anisotropie élastique et l'écoulement visqueux de chaque variant alpha (hcp) et de chaque matrice bêta (bcc), en employant la plasticité cristalline avec des écrouissages de type cinématique et isotrope. L'identification des paramètres matériaux est faite à partir d'une vaste base de données expérimentale provenant du projet PROMITI. Pour comprendre le rôle de chaque phase dans le processus de déformation, un calcul EF a également été fait afin de reproduire l'essai de traction sur une très fine éprouvette plate. Dans cette étude, le niveau mésoscopique est explicitement représenté en reprenant fidèlement la géométrie et l'orientation cristallographique de chaque grain bêta transformé. Des comparaisons entre expérience et simulation sont faites à l'échelle macroscopique pour les courbes contrainte - déformation, ainsi qu'au niveau mésoscopique, en considérant les champs de déplacement hors-plan et les champs de déformation. / The purpose of this PhD work is to investigate deformation mechanisms at room temperature in beta-metastable titanium alloys Ti17 and Ti5553. Studied microstructures are composed of beta-grains, in which alpha phase can precipitate under twelve different variants according to Burgers relationship. A multiscale approach is then proposed with three levels to consider: macroscopic, mesoscopic (prior beta grains) and microscopic (alpha variants and beta matrix of each grain). Different mean field models are adapted to depict Ti17 and Ti5553 mechanical behaviors. These models are based on the two scale-transition homogenization of local behaviors, with various ways of representing intergranular interactions. Relationships between microstructures and mechanical properties are also considered. The most advanced micromechanical models developed in this work depict elastic anisotropy and viscoplastic flow of each hcp alpha variant and each bcc beta matrix, using crystal plasticity with kinematic and isotropic hardening. Identification of material parameters is done using a large experimental database from PROMITI project. To understand the role of each phase in the deformation process, a FE computation was also made to reproduce the uniaxial tensile test of a very thick micro-specimen. In this study, the mesoscopic scale is explicitly represented: each beta grain has a real geometry and crystallographic orientation, according to a measured EBSD map in SEM. Comparisons between experiment and the numerical simulation are made on macroscopic stress - strain curves as well as on the mesoscopic scale, by considering out-of-plane displacement and strain fields.

No description available.

The alloys of Ti are extensively used in a number of industries with the α+β alloy Ti-6Al-4V (referred to as Ti64 hereafter) being the most popular. Recently, it was demonstrated that the addition of a small amount of B – as small as 0.04 wt.% – results in an order-of-magnitude reduction in the as-cast grain size. Consequently, there is considerable current interest in understanding the mechanical behaviour of B-modified alloys, with particular emphasis on correlating the microstructural changes with the property variations and the deleterious effects – if any – of TiB particles especially in the context of fatigue. Prior studies have indicated that the addition of 0.1 wt.% B to Ti64 yields the most optimum combination of room temperature properties. The research reported in the current thesis builds further on it, with the objective of exploring the utility of Ti64-B alloys in the engineering applications context. Towards this end, mechanical behaviour of cast and wrought Ti64-B alloys at cryogenic and high temperatures, the possible effect of hydrogenation on the tensile properties, and strain-controlled low cycle fatigue was experimentally evaluated as detailed below. While extensive work is reported on as-cast alloys, the mechanical properties of wrought alloys have not been examined hitherto. Keeping this in view, room temperature tensile and fatigue properties of wrought Ti64-B alloys were investigated. Microstructures of wrought alloys show kinking of the  lamellae and alignment of TiB particles along the flow direction. Marginal enhancement in tensile and fatigue properties upon forging is noted. Decrease in fatigue strength of wrought Ti64-0.04B is observed due to increase in volume fraction of the grain boundary α phase with B addition, which acts as a crack nucleation site. No significant effect of TiB particles on tensile and fatigue properties is observed. Next, strain-controlled fatigue behaviour was investigated. Results show significant softening when the strain amplitudes, ΔεT/2, are ≥0.75%. B addition was found to improve the fatigue life for ΔεT/2 ≤ 0.75% as it corresponds to the elastic regime and hence strength dominated. At ΔεT/2 = 1%, in contrast, the base alloy exhibits higher life as TiB particle cracking due to strain incompatibility renders easy crack nucleation in the B-modified alloys. To examined whether the addition of B to Ti64 is beneficial in enhancing its high temperature mechanical behavior, tensile and creep tests are carried out in the temperature range of 475-550 °C. Experimental results show that the B addition enhances both elevated temperature strength and creep properties of Ti64, especially at the lower end of the temperatures investigated. The steady state creep rate in the B-modified alloys were lower than that in the base alloy, and both the strain at failure as well as the time for rupture increases with the B content. These marked improvements in the creep resistance due to B addition to Ti64 were attributed primarily to the increased number of inter-phase interfaces – a direct consequence of the microstructural refinement that occurs with the B addition – that provide resistance to dislocation motion. Titanium alloys are widely used in various ambient and high temperature applications. However, in some instances these alloys are exposed to hydrogen and low operating temperature environments. Ti64 alloy shows poor ductility in hydrogen and cryogenic environments. Whether the microstructural refinement that occurs with the B addition also improves its relative mechanical performance in such environments is examined. For this purpose, alloys were H charged at 500 and 700 °C for up to 4 h. Microstructures and room temperature tensile properties of the resulting alloys have been evaluated. Experimental results show that charging at 700 °C for 2 h leads to the formation of titanium hydride in the microstructure, which in turn causes severe embrittlement. For shorter durations of charging, a marginal increase in strength was noted, which is attributed to the solid solution strengthening by hydrogen. The mechanical performance of the B modified alloys was found to be relatively better, implying that B addition is beneficial in applications that involve H environment. Finally, the utility of B-modified Ti64 for cryogenic applications is examined through notched and unnotched tensile tests at 77 and 20 K. While the addition of B up to 0.3 wt.% increases the strength at both 77 and 20 K. However, the ductility of the alloys decreases drastically with decrease in temperature. The tensile stress-strain responses of Ti64-B alloys exhibit serrations beyond yielding at 20 K. The extent of serrations were found to be maximum in coarse grained B-free Ti64 alloy, while only one serration could be identified in B-containing alloys. Activation of deformation twinning at 20 K results in the formation of serrations. Three twinning modes were identified in coarse grained B-free Ti64 alloy- {10 ̅2}, {11 ̅1} and {5 ̅1 ̅} while only{10 ̅2}twinning mode was activated in B-containing alloys. Extensive deformation through twinning results in higher ductility of B-free Ti64 alloy at 20 K in comparison to B containing alloys.

Les alliages à mémoire de forme (AMF) font partie des matériaux qui ont besoin d'une caractérisation de leur comportement sous sollicitations dynamiques afin de pouvoir être intégrés dans des solutions de conception de structures prévues pour l'absorption d'énergie ou pour subir de grandes déformations à des régimes de vitesses équivalents à des impacts. Même si les phénomènes mis en jeu dans ce type de matériau commencent à être maîtrisés, la caractérisation de leur comportement en dynamique est un point qui nécessite encore beaucoup d'études d'approfondissement. Leurs propriétés singulières et leur bonne capacité d'absorption d'énergie font d'eux de bons candidats à l'application dans des technologies innovantes et motivent la poursuite de leur étude. Ces travaux de thèse présentés dans ce manuscrit portent sur un AMF à base de Nickel-Titane (NiTi).Les deux propriétés singulières principales des AMF sont la superélasticité (ou pseudo-élasticité) et l'effet mémoire. La propriété sur laquelle cette étude se concentre est la superélasticité : celle-ci correspond à une transformation martensitique activée par une sollicitation mécanique.Afin de pouvoir caractériser le NiTi pour des applications soumises à des impacts ou à des sollicitations dynamiques, il est nécessaire de pouvoir, dans un premier temps, observer la transformation martensitique pour ces régimes et de tenir compte de ces résultats pour l'élaboration de lois de comportement.Ces travaux de thèse, essentiellement expérimentaux, s'inscrivent dans la mise en place d'un projet visant à pouvoir prédire le comportement des alliages à mémoire de forme soumis à des sollicitations dynamiques multiaxiales et sont centrés sur trois thèmes : les AMF, les essais de traction dynamique, la corrélation d'image pour les essais aux barres de Hopkinson et pour la mesure de la transformation martensitique des AMF. / The specific properties of the shape memory alloys are mainly due to the martensitic transformation occuring in the material turning the austenitic phase into a stress-induced martensitic phase when mechanical or thermal loadings are applied. This study focus on pseudoelasticity which allows SMAs to recover their initial state after undergoing large deformation. when a mechanical load is experienced.This study is focused on the behavior of SMAs under dynamic loading. Several experimental methods were developped : a Split Hopkinson Tensile Bar (SHTB) was set up and digital image correlation (DIC) was adapted to this case and allows us to measure heterogeneous strain fields on the surface specimen due to martensitic transformation.This work present a lot of experimental results and aim at helping researchers to develop behaviour models of SMAs for dynamic loading. The DIC was also adapted to fast imaging measure and Hopkinson bar tests, providing complementary results to the forces and velocities obtained with the bars.

Titanium and aluminium alloys are among the most used construct materials due to their physical and mechanical properties except steels. The joining of these alloys can improve properties of whole construction but it is still difficult task. Especially welding of titanium and aluminium alloys is difficult cause formation of undesirable intermetalic phases in the weld. This thesis focuses on influences of electron beam welding parameters especially focusing and deflection of beam and preheating of base material to quality of heterogeneous join of titanium alloy Ti6Al4V and aluminium alloy EN AW-6061 – T651. There is described preparation of welded joins and brazed joins in the thesis, which are evaluated by light microscopy, scanning electron microscopy and EDS analysis of chemical composition. There was evaluated presence and chemical composition of formated intermetalic phases in the welded joins and quality and defects in the brazed joins.

The problematics of weldability of heterogeneous welds of aluminium and titanium alloys produced by electron beam welding is discussed in this work. Homogenous welds of selected alloys were analyzed in the first stage. Welding of these materials relates to formation of intermetallic phases at the interface of base materials due to differences in physical, chemical and metallurgical properties of base materials. One of the prerequisites for producing high quality weld joints is to find optimal process parameters. The influence of selected process parameters to integrity, structure and mechanical properties of heterogeneous Al/Ti joints is evaluated.