Les alliages de titane sont actuellement très utilisés comme implants orthopédiques de part leurs bonnes propriétés mécaniques, leur bonne résistance à la corrosion ainsi que leur excellente biocompatibilité. Cependant, l’alliage Ti-6Al-4V qui est le plus utilisé présente un module d'élasticité élevé (110GPa), ce qui peut provoquer le phénomène de « stress shielding » et finalement causer l’échec de l’implantation. De plus, l’utilisation à long terme de ce type d’alliage est remise en question à cause de la présence de certains éléments (Al et V) considérés comme cytotoxiques et/ou allergènes. Les alliages -métastables à base de titane peuvent être des candidats de remplacement intéressants grâce à l’addition d'éléments biocompatibles tel que Nb, Zr et Sn.L'alliage superélastique biocompatible de composition Ti-24Nb-4Zr-8Sn (% massique) a été étudié dans le cadre de cette thèse. Cet alliage montre des propriétés intéressantes telles qu’un bas module d’élasticité, une résistance mécanique élevée et une ductilité relativement importante.Dans ce travail de thèse, différents traitements thermomécaniques ont été réalisés afin d’obtenir des textures cristallographiques différentes. Les influences de changement de texture sur les propriétés mécaniques et la superélasticité ont été ainsi préalablement étudiées. La transformation martensitique a été caractérisée par des essais in situ de diffraction des rayons X sous rayonnement synchrotron (SXRD) pendant une sollicitation mécanique et par analyse mécanique dynamique (DMA) sous différentes contraintes statiques. De plus, les microstructures de déformation ont été observées par EBSD et MET pour caractériser précisément les mécanismes de déformation plastique, en particulier le maclage. / Titanium alloys have already been extensively used as orthopedic implants due to the good mechanical properties, corrosion resistance and excellent biocompability. However, the most widely used Ti-6Al-4V alloy exhibits high elastic modulus (110GPa) which would cause the stress shield effect and eventually lead to the implantation failure. Furthermore, elements of Al and V are proved to be toxic for long-term application. Low modulus metastable  titanium alloy can be a suitable candidate through proper addition of non-toxic alloying element such as Nb, Zr and Sn.The present investigated Ti-24Nb-4Zr-8Sn alloy is a new -type metastable alloy potentially interesting for biomedical applications. This alloy displays high strength, low elastic modulus, high ductility, superelastic property and good biocompatibility according to previous investigations.In this work, the as-cold rolled Ti-24Nb-4Zr-8Sn alloy was subjected to different thermo-mechanical treatments in order to introduce different crystallographic texture. Influences of texture change on mechanical properties and superelasticity have been preliminarily studied. Martensitic transformation which is responsible for the superelasticity has been characterized by both in situ synchrotron X-ray diffraction and dynamic mechanical analysis. Moreover, deformed microstructures have been observed by EBSD and TEM to characterize precisely the plastic deformation mechanisms, and particularly the twinning.

Ti-6Al-4V is the most widely used titanium alloy and is typically used in stages of gas turbine engines, due to its high strength-to-weight ratio, corrosion resistance and high strength at moderate temperatures. However, the alloy is susceptible to the development of strong textures during thermomechanical processing that leads to a preferred crystallographic orientation. These are referred to as macrozones and are thought to develop during the β to α phase transformation, as a result of the retention of large prior β grains during processing and variant selection. Macrozones are clusters of neighbouring grains with a common crystallographic orientation that may act as one single grain during loading and have been shown to cause scatter in the fatigue life. The focus of the current work was based on the analysing the strain behaviour of soft, hard and no macrozones within the microstructure, during various loading conditions. The local strain behaviour was studied at a micro and nanoscale, using the digital image correlation (DIC) technique, which utilises microstructural images recorded during mechanical loading. On a microscale, the no-macrozone and strong-macrozone condition loaded at 0% exhibited homogeneous strain behaviour. The strong-macrozone condition loaded at 45% and 90% to the extrusion direction, respectively, developed pronounced high strain bands correlating to regions that were favourably oriented for prismatic and basal slip, respectively. Characterisation of the slip bands provided a detailed understanding of the deformation behaviour at the nanoscale and the slip system was subsequently determined for each grain using slip trace analysis. Prismatic slip was the dominant slip system in all conditions, particularly in the soft-oriented macrozone regions of the strong-macrozone condition loaded at 45 degrees. Shear strains of 10 times the appliedstrain were observed. Further investigations on the strong-macrozone condition loaded at 45 degrees to ED during standard and dwell fatigue demonstrated early failure in the dwell sample, with higher strain accumulation for dwell.

Orientador: João Batista Fogagnolo / Dissertação (mestrado) - Universidade Estadual de Campinas, Faculdade de Engenharia Mecânica / Made available in DSpace on 2018-08-27T20:13:02Z (GMT). No. of bitstreams: 1 RodriguezPerez_JessicaMarlena_M.pdf: 4283527 bytes, checksum: 428a287377aaab009ef368ca3005561b (MD5) Previous issue date: 2015 / Resumo: O interesse em ligas do sistema titânio-nióbio para aplicações ortopédicas se deve à excelente resistência mecânica e biocompatibilidade, sendo que o módulo de elasticidade pode ser controlado pelo teor de nióbio. Existem diversos processos que podem tornar estas ligas adequadas para uso como biomaterial e que resultam em diferentes fases com diferentes propriedades. O presente trabalho teve como objetivo modificar peças sinterizadas de ligas do sistema titânio-nióbio por refusão superficial por laser. Foram utilizadas ligas com diferentes composições químicas, variando-se o teor de nióbio de 5 a 45% em peso. Foram analisados os efeitos da variação dos parâmetros de processamento, potência e velocidade de deslocamento do feixe laser, sobre a morfologia de cordões isolados. Foram obtidas camadas contínuas de refusão por sobreposição de cordões de isolados. As amostras sinterizadas com teores de nióbio entre 5 e 20% apresentaram as fases ? e ?. A amostra com teor de nióbio de 25% e maiores apresentam regiões com fase ? completamente estabilizada e regiões com as fases ? e ? devido à heterogeneidade química na distribuição de nióbio. A amostra com teor de nióbio de 45% apresenta apenas a fase ?, porém também se observa nessa amostra a heterogeneidade na distribuição de nióbio. Constatou-se que a potência do feixe de laser é o parâmetro de maior influência na morfologia e dimensões da zona fundida dos cordões isolados. Dependendo do teor de nióbio, diferentes fases são formadas nas camadas continuas de refusão. Para teor de nióbio de 5%, obtém-se a fase martensítica ?', de estrutura hexagonal. Para teor de nióbio de 15%, obtém-se majoritariamente a fase ?' com presença da fase martensítica ortorrômbica ?''. Para teor de nióbio de 25%, obtém-se a fase ?'', com pequena fração de fase ?. Para teor de nióbio de 35 e 45%, obtém-se a fase ? em toda a zona fundida e a fase ?'' na zona termicamente afetada. Tanto os cordões isolados como as camadas refundidas das amostras com teores de 15, 25, 35 e 45% em peso de nióbio apresentaram heterogeneidade química devido à microssegregação de soluto durante a solidificação. Os valores de módulo de elasticidade medidos por nanoindentação foram decrescentes para aumentos da quantidade de nióbio, tanto nas zonas modificadas pelo laser quanto no substrato sinterizado. Os valores de nanodureza mantiveram-se constantes, dentro da variação estatística dos resultados / Abstract: The interest in alloys of the titanium-niobium system for orthopedic applications is due to their excellent mechanical resistance and biocompability, as the elastic modulus may be controlled by niobium content. There are several processes that can make those alloys adequate to be used as biomaterials and that result in different metallic phases with different properties. The objective of this study was to modify, by laser surface remelting, sintered parts of alloys from the titanium-niobium system. Alloys with different chemical compositions were used; the niobium content varied from 5 to 45wt%. The effects of the variation of processing parameters (laser beam power and scan speed) on the morphology of the isolated tracks were analyzed. Continuous remelting layers were obtained by overlapping isolated tracks. The sintered samples with niobium content between 5 and 20% exhibited both ? and ? phases. The sample with a niobium content of 25% or more had regions of completely stabilized ? phase and regions of ? and ? phases due to the chemical heterogeneity in the niobium distribution. The sample with a 45% niobium content showed only the ? phase, but heterogeneity in the niobium distribution is also seen. It was found that the laser beam power is the parameter that most influences the morphology and dimensions of the molten area of isolated tracks. Depending on the niobium content, different phases are formed in the continuous remelting layers. For a niobium content of 5%, the martensitic ?' phase of hexagonal structure is obtained. For a niobium content of 15%, the ?' phase is mostly obtained, with the presence of orthorhombic, martensitic ?'' phase. For a niobium content of 25%, the ?'' phase, with a small fraction of ? phase, is obtained. For niobium contents of 35 and 45%, ? phase throughout the molten area and ?'' phase in the heat affected zone are obtained. Both the isolated tracks and the continuous remelting layers on the samples with niobium weight contents of 15,25,35 and 45wt% presented chemical heterogeneity due to solute microsegregation during solidification. The values of elastic modulus measured by nanoindentation decreased as the niobium content increased, both in the laser modified zones and in the sintered substrates. The values of nanohardness remained constant within the results' statistical variation / Mestrado / Materiais e Processos de Fabricação / Mestra em Engenharia Mecânica

Orientador: Ana Paula Risifni Alves Claro / Coorientador: Ana Lúcia do Amaral Escada / Banca: Durval Rodrigues Júnior / Banca: Cristiane Aparecida Assis Claro / Banca: Ronaldo Spezia Nunes / Resumo: O objetivo deste estudo in vivo foi avaliar as propriedades de resposta óssea da liga de Ti7,5Mo usinada em minimplantes com tratamento de superfície por anodização e compara-la, com sua versão não tratada e com a liga de Ti-CP em sua apresentação comercial, tratada por jateamento e ataque ácido, em relação às suas propriedades de osteointegração. Os minimplantes do Grupo tratado de Ti7,5Mo foram anodizados em eletrólito de NH4F por 24h e em seguida calcinados a 450ºC por 1h. As amostras foram divididas em três Grupos, Ti-CP com tratamento de superfície por jateamento seguido de ataque ácido (n=5), Ti7,5Mo usinadas (n=5) e Ti7,5Mo anodizado para crescimento de nanotubos de TiO2 (n=6). Para caracterização das amostras foram realizados a espectroscopia Raman, difração de raios X, perfilometria ótica e microscopia eletrônica de varredura. As análises histomorfométricas para determinação do BIC (bone to implant contact) e do BAFO (bone area fraction occupancy) foram realizadas após implantação das amostras de cada Grupo na tíbia de ratos Wistar sacrificados após 4 semanas. A análise estatística por meio do teste de ANOVA de 1 fator demonstrou haver diferença estatística significante apenas entre os Grupos para o BIC; o teste Tukey para avaliação do BIC demonstrou haver diferença estatística significante somente entre o Grupo Ti7,5Mo anodizado em relação ao Grupo Ti-CP em apresentação comercial; não foram detectadas diferenças estatísticas significantes para o BAFO entre os Grupos... (Resumo completo, clicar acesso eletrônico abaixo) / Abstract: The objective of this in vivo study was to evaluate the bone response of the Ti7,5Mo alloy machined in minimplants with surface treatment by anodization and compare it, with its untreated version and with the Ti-CP alloy in its commercial presentation, gritblasted and acid-etched. The Ti7,5Mo minimplants of the treated group were anodised in a NH4F electrolyte for 24h and then calcinated at 450ºC for 1h. The samples were divided into three groups, Ti-CP with surface treatment by blasting followed by acid-etched (n=5), Ti7, 5Mo machined (n=5) and Ti7, 5Mo anodized for growth of TiO2 nanotubes (n=6). To characterize the samples, Raman spectroscopy, X-ray diffraction, optical perfilometry and scanning electron microscopy (SEM) were performed. The Histomorphometric analysis for determination of the BIC (bone to implant contact) and BAFO (bone area fraction occupancy) were performed after the tibia implantation of the samples of each group in Wistar rats sacrificed after 4 weeks. The statistical analysis using the 1-factor ANOVA test showed statistically significant difference only for BIC amongst groups, Turkey test showed statistically significant difference for the evaluation of BIC only between the group Ti7, 5Mo anodized in relation to the Ti-CP group in commercial presentation, Turkey test did not detect significant statistical difference for BAFO among the groups. Pearson test did not detect direct correlation between BIC and BAFO values. The Ti7,5Mo samples with anodised s... (Complete abstract click electronic access below) / Doutor

The results from this study, on a few commercial and model metastable beta titanium alloys, indicate that the growth restriction factor (GRF) model fails to interpret the grain growth behavior in the additively manufactured alloys. In lieu of this, an approach based on the classical nucleation theory of solidification incorporating the freezing range has been proposed for the first time to rationalize the experimental observations. Beta titanium alloys with a larger solidification range (liquidus minus solidus temperature) exhibited a more equiaxed grain morphology, while those with smaller solidification ranges exhibited columnar grains. Subsequently, the printability of two candidate beta titanium alloys containing eutectoid elements (Fe) that are prone to beta fleck in conventional casting, i.e., Ti-1Al-8V-5Fe (wt%) or Ti-185, and Ti-10V-2Fe-3Al (wt%) or Ti-10-2-3, is further investigated via two different AM processing routes. These alloys are used for high-strength applications in the aerospace industry, such as landing gears and fasteners. The Laser Engineered Net Shaping and Selective Laser Melting (the two AM techniques) results show that locally higher solidification rates in AM can prevent the problem of beta fleck and potentially produce β-titanium alloys with significantly enhanced mechanical properties over conventionally cast/forged counterparts. Further, the detailed investigation of microstructure-mechanical property relationships indicates that the precipitation or formation of non-equilibrium secondary phases like α or ω in these commercial systems can be advantageous to the mechanical properties. The influence of process parameters on the evolution of such secondary phases within the β matrix grains has also been rationalized using a FEM-based multi-physics thermo-kinetic model that predicts the multiple heating-cooling cycles experienced by the layers during the LENS deposition. Overall, the results indicate that Ti-1-8-5 and Ti-10-2-3 are promising β-Ti alloys for AM processing. Further, the results also demonstrate the ability to tune the microstructure (secondary phase precipitation and grain size) via changes in the process parameters to achieve desirable mechanical properties, obviating the need for any secondary post-processing. The understanding obtained through this work can be coupled with the concept of β-phase stability prediction, via parameters like bond order (Bo), the energy level of metal d-orbital (Md), Mo equivalency, etc., to design novel beta titanium alloys with the desired microstructures tailored via AM for structural applications.

The current understanding of the mechanical properties and deformation behavior of some individual phases in titanium alloys is limited due to the fine scale at which these phases precipitate within the β-phase matrix. The α and ω phases represent the most widely observed phases in titanium alloys depending on the alloy composition and also the heat treatment procedure adopted during processing. The possibility of precipitating ω-phase depends on the content of the β-stabilizers within the system. Although a significant compositional partitioning occurs within ω-phase upon aging treatment, the knowledge of ω-phase mechanical properties as a function of composition is very limited. The initial part of the current work focuses on the effect of common β-stabilizers elements on the phase stability and mechanical properties of the ω-phase using first-principles calculations. A relation between the bonding nature, the phase stability, and elastic properties was proposed. Thereafter αʺ martensitic phase was investigated in Ti-Nb and Ti-Nb-O alloys. The phase stability and martensitic start temperature of αʺ-phase was studied as a function of Nb and oxygen content. Also, the effect of the lattice shear distortion induced by oxygen atom on stabilizing β-phase was investigated. Subsequently the effect of the β-stabilizers' elements on stacking faults energy and ductility in α-Ti alloys was studied. Both prismatic and basal slip system were investigated with different concentration of β-stabilizers at the slip plane. Lastly, while the Tadmor and Bernstein model was employed to predict the partial dislocation emission and twinning propensity, the Rice criterion was used to estimate the effect of different β-stabilizers on the ductility of α-Ti alloys.

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