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Etude et formalisation du comportement tribologique d'un contact polytetrafluoroéthylène/Alliage de titane soumis à des sollicitations de fretting-reciprocatingToumi Krir, Sana 09 June 2017 (has links)
Les polymères sont de plus en plus répandus dans différents secteurs industriels comme une alternative aux métaux. En effet, les composants en polymère permettent une réduction accrue du poids et une meilleure inertie chimique dans les structures où ils sont utilisés. Ils permettent également une réduction du frottement sans recourir à des systèmes de lubrification externe. Parmi ces polymères, le PTFE - connu sous le nom du Teflon et découvert en 1938 - se caractérise par une morphologie semi-cristalline particulière où les molécules de PTFE forment des superstructures dites « à bandes ». Il possède d’excellentes propriétés thermiques, un très faible coefficient de frottement et une très bonne inertie chimique justifiant sa vaste utilisation dans différentes applications : comme renfort de type lubrifiant solide, revêtement antiadhésif, isolant électrique des câbles dans le domaine de l’aéronautique, récipients pour des produits chimiques réactifs. Ce travail de thèse s’inscrit dans ce contexte et adopte une démarche tribologique globale. Il étudie les réponses tribologiques d’un contact PTFE/Ti-6Al-4V sollicité en fretting-usure alternatif - notamment en mode glissement total et reciprocating - dans une configuration cylindre/plan. Les paramètres étudiés sont : nombre de cycles, vitesse de glissement, force normale et propriétés thermomécaniques et surfaciques des matériaux. Cette étude propose de nouvelles formalisations analytiques basées sur l’approche d’Archard et établit des lois de frottement et d’usure qui intègrent les effets de ces paramètres. Le rôle joué par le film de transfert dans la détermination des réponses tribologiques est également mis en évidence. / The tribology of thermoplastic polymers is nowadays one of the major issues in several engineering fields. These non-metallic materials increasingly provide a useful alternative to metals that are in contact with a harder counterface. Areas of application are various and include offshore oil-drilling, aeronautics and the automotive industry and biomedical applications such as prosthesis designs. The aim of polymer-metal, and especially PTFE/Ti-6Al-4V, designs is to reduce wear and friction. Polytetrafluoroethylene (PTFE) is one such interesting thermoplastic polymer that has been closely studied since it was discovered in 1938. It is a high-performance engineering polymer characterized especially by a high melting point, chemical inertness and low coefficient of friction due to its banded structure. PTFE is a tribologically attractive material, widely used especially as a solid lubricant in a variety of dry sliding tribosystems. The purpose of this study is to evaluate friction and wear rate evolution for gross slip fretting-reciprocating sliding conditions of PTFE/Ti-6Al-4V interface in a cylinder/plane configuration. Various investigations have been made to study the influence of wear test conditions: number of cycles, sliding speed, normal force, materials thermomechanical and surface properties. Analysis aimed to determine tribological processes as well as formulation of experimental evolution of friction and wear rates regarding selected parameters. Finally, characterization of the transfer film formed on the counterpart under repeated cyclic sliding is undertaken to determine its role and its interference with wear and friction response.
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Využití kmenových buněk v inženýrství kostní tkáně / Application of the stem cells in bone tissue engineeringKročilová, Nikola January 2016 (has links)
Problems with musculoskeletal system, such as of developmental disorders, fractures or damage of the bone by age, inflammatory or tumor diseases, are still increasing in orthopaedics. Sometimes the bone tissue is not capable to completely regenerate to exert its physiological function in the organism. For this reason, using the bone replacements is necessary and common nowadays. Despite of an intensive research and testing of a wide range of the potential biomaterials and their combinations, the usage of metal materials for construction of the bone implants, still remains to be the gold standard. Ti-6Al-4V alloy is one of the commercialy used metal materials, which is known for the high mechanical and chemical resistance and a good biocompatibility. For a good biological response of the patient's organism for the bone implant, is an ability of osteointegration into the surrounding bone tissue, the key. This ability can be influenced in the case of the metals, by their surface structure. As it is known from earlier studies, the surface topography of the material is very important for the adhesion and proliferation of the bone cells, which are able to discriminate, very sensitively, between various stages of the material surface roughness. For this reason we have focused on studying of an influence...
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Role Of Boron On The Evolution Of Microstructure And Texture In Ti-6AL-4V-0.1B AlloyRoy, Shibayan 07 1900 (has links) (PDF)
Titanium and its alloys constitute an important class of materials for aerospace, biomedical, and chemical industries, primarily due to their high specific strength and fracture toughness with good corrosion resistance. Owing to their hexagonal crystal structure at room temperature, both microstructure and texture play a crucial role in the processing and hence the properties of titanium alloys. The basis for tailoring the microstructure and texture in titanium alloys centers around the transformation of high temperature β (body-centered cubic) to the low temperature α (hexagonal close packed) phase. One of the most widely used titanium alloy is Ti-6Al-4V, which exists as two phase (α+β) alloy at room temperature. The cast structure of the alloy Ti-6Al-4V is generally coarse and has strong solidification texture that leads to inferior properties.
Recently, trace boron addition has been reported to produce substantial refinement in cast microstructure for Ti-6Al-4V. Significant improvements in some of the mechanical properties have been reported for the Ti-6Al-4V-0.1B alloy in the as-cast condition. The reasons for microstructural refinement in the boron modified alloy and associated improvements in properties, however, needs to be investigated since the property attributes strongly depend on finer microstructural details including crystallographic texture. In addition, the titanium alloys are processed through thermo-mechanical treatments that involve deformation and annealing response of the alloy. The effect of boron modification on the processing response during thermo-mechanical treatments (TMP) has also not been studied. All these aspects shape the framework of the thesis, wherein microstructure and texture evolution is probed from starting cast condition through different stages of TMP. Micro-mechanisms are identified at every stage from the interrelation of these two intrinsic factors.
In the first part of the study, the spatial variation of microstructure and texture in the cast ingot has been studied using SEM-EBSD technique. It has been found that trace boron addition (0.1 wt%) to Ti-6Al-4V alloy ensures excellent microstructural homogeneity throughout the cast ingot. A subdued thermal gradient due to constitutional undercooling persists during solidification and maintains equivalent β grain growth kinetics at different locations in the ingot. For Ti-6Al-4V-0.1B alloy, both high temperature β and room temperature α phase textures weaken. The microstructural attributes of boron addition manifests as the absence of grain boundary α-phase and the presence of TiB particles. Both these features strongly affect the mechanism of β→α phase transformation and consequently weaken the α phase texture.
The evolution of microstructure and texture during β-processing of Ti-6Al-4V-0.1B alloy is examined in the second part of the work. Boron modified alloy shows the typical features of β worked microstructure with fine prior β grains, however without the formation of shear bands, which is generally observed in the microstructure of β worked Ti-6Al-4V alloy. The transformed α texture is almost same for the two alloys indicating similarity in the transformation behaviour of boron modified and boron free Ti-6Al-4V alloy due to complete dynamic recrystallization during β processing. The microstructural features as well as the crystallographic texture indicates dominant grain boundary sliding for the boron added alloy which leads to homogeneous deformation response without instability (shear band) formation.
In the third part of the study, the deformation response in the (α+β) regime has been studied by carrying out hot compression tests at different temperature under constant true strain rate to simulate experimental processing conditions for the cast Ti-6Al-4V-0.1B alloy. The critical combinations of temperature and strain rate suitable for processing are identified based on flow curves and kinetic analyses. Microstructural features display dynamic recovery of the α-phase at low temperatures and softening due to globularization and/or dynamic recrystallization at high temperatures irrespective of boron addition. The transition temperature for the two mechanisms is comparatively lower for boron added alloy. Unlike Ti-6Al-4V, no sign of instability formation has been observed in Ti-6Al-4V-0.1B. The absence of macroscopic instabilities and early initiation of softening mechanisms has been attributed to microstructural features and texture of boron modified alloy in the initial as-cast condition.
In the fourth part, the large strain deformation response has been studied for the Ti-6Al-4V-0.1B alloy by rolling in the (α+β) regime. Microstructure in near α rolling regime is characterized by a few kinked and bent α colonies while others are elongated along the rolling direction. Dynamic softening at higher temperatures is more dominant for the boron added alloy. Microstructural features are strongly orientation sensitive while relative differences are inherited from the starting cast alloys. Texture evolution, however, does not markedly vary for the two alloys and indicates little difference in the slip based deformation processes under plane strain condition. The influence of transformation texture appears early for the boron added alloy and affects the final texture in much stronger way at higher temperature. Subsequent to the (α+β) rolling, static annealing of warm rolled alloys has been carried out. A faster annealing kinetics for boron added alloy has been observed, which is related to deformation prior to annealing leading to additional diffusion pathways due to microstructural factors. Texture of the annealed material is similar to the deformed state for shorter annealing times but substantially modifies by epitaxial growth of primary α phase during long time annealing.
The final part of the work deals with the deformation response of boron added alloy under superplastic conditions. Out of the two alloys with similar microstructure and texture, higher elongation for boron modified alloy is justified by the absence of slip based deformation and improved grain boundary sliding. Increase in α/β interfaces due to globularization during warm rolling and static annealing contribute to the grain boundary sliding.
The outcomes of the thesis have been presented as a summary at the end and suggestions have been made indicating the scope for future investigations pertaining to this area.
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Produktivní obrábění titanových slitin / Productive Machining of Titanium AlloysSlabý, Ondřej January 2012 (has links)
This diploma thesis is focused on a productive machining of titanium alloys. At the beginning it deals about titanium and its alloys. It describes chip generation mechanism, tool blunting and surface quality. Further it contains modern strategies of efficient titanium alloys machining. Then it analyzes contemporary manufacturing technology of hinge made of titanium alloy Ti-6Al-4V in Frentech Aerospace s.r.o. company, and at the end finds possibility of savings by inovation of roughing process.
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Improving Fatigue Life of LENS Deposited Ti-6Al-4V through Microstructure and Process ControlPrabhu, Avinash W. 02 June 2014 (has links)
No description available.
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Etude de la contribution de la technique spark plasma sintering à l'optimisation des propriétés mécaniques de l'alliage de titane TA6V / Investigation of the contribution of the Dpark Plasma Sintering technique to the mechanical properties optimisation of the TA6VKus, Ugras 25 January 2017 (has links)
Les coûts de revient des alliages de titane limitent leurs applications à des domaines de forte valeur ajoutée. La diminution des coûts de mise en forme des pièces tout en maitrisant les microstructures et les propriétés mécaniques est donc un enjeu important. Les procédés de mise en forme issus de la métallurgie des poudres comme le Spark Plasma Sintering (SPS) peuvent permettre d'atteindre ces objectifs. Les premiers instants du frittage ont été étudiés selon la compacité initiale du corps granulaire. Lorsque cette dernière est faible, les surfaces des cous entre les granules, mises en évidences par microtomographie, sont plus importantes. Ces observations peuvent être expliquées par le fait que les densités de courant au niveau des points de contacts sont plus importantes quand les surfaces de contacts sont plus faibles. De plus, les densités finales très proches malgré les compacités initiales différentes laissent penser que les mécanismes de frittage en action sont différents. Une modélisation Electro-Thermique et Mécanique par éléments finis a permis de décrire de façon très réaliste la densification du TA6V. La loi de densification du matériau a été paramétrée par le biais de campagnes d'essais en fluage menés dans le SPS ainsi que d'essais de compaction du corps granulaire. Des voies d'amélioration du modèle ont également été proposées. Dans la dernière partie de l'ouvrage, un panel des microstructures obtenues par frittage SPS du TA6V ainsi qu'un transfert d'échelle des échantillons modèles cylindriques de petites tailles vers des formes plus complexes et massives ont été étudiés. De plus, les propriétés mécaniques en traction sur pièces près des cotes ont été caractérisées. Les domaines (température et pressions) d'obtention de microstructures denses, homogènes et répétables ont été identifiés. Le transfert d'échelle révèle que la répétabilité du SPS est validée tant en termes de microstructures que de propriétés mécaniques des pièces densifiées. De plus, les propriétés en traction sont au niveau des matériaux forgés, notamment avec des allongements à rupture de près de 13%. / The cost prices of the titanium alloys limit their applications to strong added value fields. The decrease of the pieces shaping costs while mastering microstructures and mechanical properties is an important issue. Shaping processes from powder metallurgy as Spark Plasma Sintering (SPS) can allow to reach these goals. The first moments of the sintering were studied according to the initial compactness of the granular body. When the latter is low, the area of necks between granules, highlighted by microtomography, are bigger. These observations can be explained by the fact that current densities at contact points are higher when the contact areas are lower. Furthermore, the very close final densities in spite of the different initial compactness let think that the mechanisms in action during sintering are different. An electro-thermal and mechanical modelling by finished element allowed to describe in a very realistic way the densification of the TA6V. The densification law of the material was configured by means of creep tests programmes performed dine the SPS chamber as well as of compaction tests of the granular body. Ways of improvement of the model were also proposed. In the last part of the word, a panel of microstructures obtained by SPS of TA6V as well as a scale transfer from the small cylindrical samples towards more massive and complex shapes was studied. Furthermore, the tensile properties of near-net-shape specimens were characterised. Domains (temperature and pressure) of dense, homogeneous and repeatable microstructures obtaining were identified. The scale transfer reveals that the SPS repeatability is both validated in terms of microstructures and mechanical properties of the densified specimens. Furthermore, tensile properties are at the same level as the forged materials, in particular an elongation at break of about 13%.
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Comportement thermomécanique et évolution microstructurale d'un alliage Ti-6Al-4V forgé α+β, durant la trempe : expérimentations, analyses et modélisation / Thermomechanical behaviour and microstructural evolution of a forged α+β – Ti-6Al-4V alloy during quenching : experiments, analysis and modellingJulien, Renaud 20 February 2017 (has links)
Cette étude s'inscrit dans le cadre du projet FUI TiMaS (Titanium Machining and Simulation) dont l'objectif est de développer un outil d'analyse et d'optimisation continu du procédé de production et visant à maîtriser et à prédire la création des contraintes résiduelles pour les pièces de structure en alliage de titane. Les contraintes résiduelles peuvent être générées notamment durant la trempe qui suit les traitements thermomécaniques. L'objectif de cette étude est d’étudier le comportement mécanique ainsi que l'évolution microstructurale de l’alliage Ti-6Al-4V, induits par le refroidissement depuis le domaine α+β, et d’intégrer cela dans une démarche de modélisation. Pour cela, un moyen expérimental, composé d’une machine d'essais hydraulique et d'un chauffage par induction, a été développé afin d’analyser la réponse mécanique de l'alliage Ti-6Al-4V sous différentes conditions mécaniques et thermiques. Ce moyen a permis la réalisation d’essais de traction/relaxation/traction à différentes températures. Parallèlement, une étude par analyse de micrographies a permis de quantifier les fractions de phases α et β ainsi que les épaisseurs de lamelles αII lors du refroidissement. Les observations ont pu être confrontées aux résultats des essais mécaniques afin d’expliquer l’influence du traitement thermique sur la résistance du matériau. Deux modèles de comportement ont été proposés pour prédire la réponse thermomécanique de l’alliage Ti-6Al-4V à l'issue de cette analyse. Le premier est un modèle élasto-visco-plastique incluant un l'écrouissage isotrope prenant en compte l'adoucissement par restauration statique du matériau. Il est valable pour différentes vitesses de refroidissement. Le second est un modèle non-unifié basé sur une loi des mélanges de phases. Il reproduit plus fidèlement le comportement mécanique et permet notamment de modéliser le phénomène de yield point par l'intermédiaire du mouvement des dislocations mobiles. / This research is part of the TiMaS project (Titanium Machining and Simulation). The main goal of this project is to develop an analysis and optimization tool of the global production process to control and assess the generation of residual stresses for titanium alloys structures parts. Residual stresses can be generated during thermal and mechanical treatment quenching steps. The main goal of this work is to study the mechanical behaviour and the microstructural evolution of Ti-6Al-4V alloy, induce by quenching from the α+β phase field, and incorporate these results in a modelling approach. For this purpose, a new experimental facility, using conventional hydraulic testing machine and induction heating, was developed to investigate the mechanical behaviour of Ti-6Al-4V alloy under different thermal and mechanical loads. This experiment has permitted to realise tensile/relaxation/tensile tests. Furthermore, an image analysis protocol was developed to study fraction of α and β phases and αII lamellae thickness. Microstructural observations can explain some aspects of the material hardening during quenching. Two mechanical behaviour models were proposed to assess the mechanical behaviour of the Ti-6Al-4V alloy. The first one is an elasto-visco-plastic model with isotropic hardening that taking account of the static recovery. It can predict the mechanical behaviour under different quenching rates. The second one is a non-unified model based on a phases mixing law. It permits a better assessment of the mechanical behaviour and allows the modelling of the yield point phenomenon by using mobile dislocations motion.
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Fusion Laser Selective de poudres de TA6V : microstructure et mécanismes de formation des porosités en lien avec les paramètres du procédé SLM et les propriétés structurales / Selective laser melting of TA6V powders : microstructure and mechanisms of formation of voids in relationship with process parameters and structural propertiesStef, Jonathan 17 December 2018 (has links)
Le procédé de fusion laser sélective (SLM) est un procédé de fabrication additive des matériaux métalliques de type « Lit de poudre ». Il s’inscrit dans le concept de l’usine 4.0 et s’oppose aux procédés d’élaboration conventionnels où la matière est soustraite, déformée ou moulée. A partir d’un modèle numérique, les pièces sont élaborées couche par couche par ajout de matière. Le procédé SLM possède d’indéniables avantages car il permet de réaliser des économies de matière, de réduire les coûts de transport et d’élaborer des produits de petites tailles et/ou de formes complexes. Il s’inscrit également dans le concept de personnalisation de masse et de relocalisation des usines à proximité des lieux de consommation. Il souffre cependant d’un manque de répétabilité et de contrôle des propriétés des matériaux élaborés, ce qui entrave son développement à une plus grande échelle. Cela vient principalement du fait que les propriétés résultantes dépendent d’interactions complexes et encore mal cernées entre les caractéristiques des poudres entrantes, les paramètres du procédé et les paramètres microstructuraux. Dans le cadre de ces travaux de thèse, nous proposons de mieux comprendre les liens qui existent entre les paramètres d’élaboration de pièces en titane Ti-6Al-4V, la formation de porosités, leur microstructure et leurs propriétés structurales. Pour ce faire, une étude paramétrique a été conduite afin d’évaluer l’influence des paramètres puissance du laser, vitesse de balayage et espacement de lasage. Trois densités d’énergie ont été considérées (50, 75 et 100 J/mm3) et une stratégie de lasage rotative a été imposée. A partir d’une approche originale combinant des analyses 2D de faciès de rupture et des analyses 3D par tomographie X des pièces, deux mécanismes de formation des porosités ont été identifiés et caractérisés pour une densité d’énergie de 50J/mm3 : le manque de fusion et la dénudation. Dans ce cas, il est montré que la distribution spatiale des porosités est liée à la stratégie de lasage et que la fraction et la densité volumiques des porosités dépendent du couple « puissance du laser » et « vitesse de balayage ». Pour des densités d’énergie plus élevées (75 et 100 J/mm3), deux nouveaux mécanismes de formation des porosités ont été identifiés : celui par surfusion de la matière et celui par piégeage de gaz. Au niveau microstructural, l’ensemble des échantillons analysés présentent une structure martensitique α’ peu texturée. Pour une même densité d’énergie, la morphologie des grains de la phase mère β et la taille des aiguilles martensitiques α’ dépendent des paramètres du procédé. Une étude fine menée en Microscopie Electronique en Transmission a permis d’identifier avec certitude des macles non répertoriées dans la littérature. Il s’agit premièrement de macles de type {01-11} <-211-1>a' ou {0-111} <2-1-11>a’ avec une rotation de 57° autour de l’axe de zone [2-1-10]a’, un cisaillement dû au maclage de 0,542, et deuxièmement, de macles de type {01-11}<-12-15>a’ ou {-1011}<7-814>a’ avec une rotation de 63° autour de l’axe de zone [1-2-21]a’ et un cisaillement dû au maclage de 0,963. Ces macles témoignent d’un phénomène de relaxation des contraintes qui seraient induites par les vitesses de refroidissement importantes et la transformation martensitique. Au niveau des propriétés mécaniques, la présence de porosités diminue la ductilité du matériau, même pour des fractions de porosités relativement faibles (<1%). La reconstructions 3D d’un échantillon rompu par traction montre qu’il existe un lien biunivoque entre la répartition des porosités et le chemin des fissures. Enfin, les porosités formées par manque de fusion et par dénudation sont plus préjudiciables aux propriétés mécaniques que celles formées par surfusion. Ceci est à mettre en parallèle avec les fractions volumiques et les morphologies des porosités pour chaque mécanisme de formation. / Selective Laser Melting (SLM) is an additive manufacturing process of metallic parts based on powder bed fusion (PBF). SLM is part of the industry 4.0 concept and is opposed to conventional manufacturing processes where the material is either subtracted, deformed or molded. From a numerical model, parts are built by material addition layer by layer. The SLM process has incontestable advantages as it offers the possibility of making small parts with complex shapes and reducing transportation costs. It also promotes mass customization and relocation of factories close to customers. However, the SLM process suffers of a lack of repeatability and control of manufactured parts which hinders its development on a larger scale. Among the possible reasons, the control of part properties is made difficult since it depends on many complex interactions between the input powders, the process parameters and microstructural features.In this work, we propose to investigate the relationships between manufacturing process parameters of Ti-6Al-4V titanium alloy parts, the mechanisms of formation of their voids, their microstructure and their structural properties. In this purpose, a parametric study was conducted to evaluate the influence of laser power, scanning speed and hatch-spacing parameters. Three energy densities were considered (50, 75 and 100J/mm3), and a rotative scanning strategy was chosen.From an original approach based on 2D fracture surface and 3D-Xray tomography analysis of parts, two mechanisms of pore formation were identified and investigated. For 50J/mm3, the spatial distribution of voids is shown to be dependent to the scanning strategy. The volume fraction and density of pores depend on the laser power and the scanning speed. For higher energy densities (75 and 100 J/mm3), two new mechanisms of pore formation were identified corresponding to over-melting and gas trapping.Concerning the microstructure, the whole characterized specimens have shown a weakly textured α’ martensitic structure. For a same energy density, prior-β grain morphology and α’ needle size were revealed to be dependent to the process parameters. Fine investigations carried out by Transmission Electron Microscopy underscored the presence of un-identified twins in literature. They are first, twins of type {01̅11} <2̅111̅>a’ or {01̅11} <21̅1̅1>’ with a rotation of 57° around the [21̅1̅0]a’ zone axis and a twinning shear of 0,542, and secondly, twins of type {011̅1}<7̅ 21 14 11>a’ or {1̅011}<11 14 1̅ 0>a’ with a rotation of 63° around the [12̅2̅1]a’ zone axis and a twinning shear of 0,963. These twins would indicate that a stress relaxation phenomenon takes place, induced by the high cooling rates and the martensitic transformation.Concerning mechanical properties, porosity affects the material ductility. Its behavior is more brittle even when the volume fraction of voids is small (<1%). 3D reconstruction of a tensile broken specimen attests a one to one relationship between the spatial distribution of pores and the crack path. Finally, pores formed by a lack of fusion and denudation are more detrimental for mechanical properties than over melting ones. This analyze is also performed by comparison with the volume fraction and the morphology of voids corresponding to each mechanism of formation.
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Estudo dos fenômenos da fluência, corrosão e oxidação isotérmica na liga Ti-6Al-4V submetida aos revestimentos de TiN e TiAlN depositados pela técnica de PVD assistida por plasma / Study of the creep, corrosion and isothermal oxidation phenomenon in the Ti-6Al-4V alloy subjected to plasma-assisted PVD TiN and TiAlN coatingsOliveira, Verônica Mara Cortez Alves de 11 July 2014 (has links)
O presente trabalho teve como objetivo principal avaliar o efeito dos recobrimentos TiN e TiAlN depositados por PVD a plasma na liga Ti-6Al-4V sob condições de fluência a 600 °C e corrosão em meios contendo cloreto a 25, 60 e 80 °C. O trabalho foi complementado com análises microestruturais e dos revestimentos superficiais utilizando-se as técnicas de difração de raios X, microscopias óptica, eletrônica de varredura e de transmissão, medidas de microdureza e oxidação isotérmica. Os resultados permitiram concluir que a liga Ti-6Al-4V constituída pela configuração de Widmanstätten apresentou dureza média de 343 HV para a condição como recebida. Após os tratamentos por PVD a plasma observou-se um recobrimento à base de TiN de espessura de 2,2 ?m e composição igual a Ti0,7N. O recobrimento a base de TiAlN/TiAlCrN apresentou espessura em torno de 6 ?m e composição igual a (Ti0,38Al0,62)N/(Ti0,31Al0,50Cr0,19)N. As medidas do potencial em circuito aberto e polarização mostraram que a liga Ti-6Al-4V apresentou comportamento ativo com transição ativo-passiva em solução HCl e comportamento passivo em solução NaCl a 25, 60 e 80 °C. As amostras recobertas por TiN e TiAlN/TiAlCrN apresentaram comportamento passivo nas duas soluções corrosivas e em todas as temperaturas estudadas. A amostra revestida por TiN depositado por PVD apresentou os menores valores de taxa secundária em fluência para tensões maiores que 222 MPa, contudo a amostra nitretada a plasma apresentou maiores valores de vida útil e níveis de ductilidade. A análise conjunta dos expoentes de tensão, energia de ativação e estrutura de discordâncias indicaram que o principal mecanismo de deformação por fluência foi controlado por escalagem de discordâncias. O cálculo do parâmetro de tolerância ao dano (W) contribuiu para indicar que os revestimentos TiN e TiAlN/TiAlCrN, apesar de protegerem a superfície da oxidação, diminuíram a capacidade de deformação plástica ao longo do estágio terciário e vida útil da liga Ti-6Al-4V, reduzindo a ductilidade. Finalmente, os tratamentos superficiais utilizados neste trabalho foram eficientes por seu efeito de proteção através da deposição de um elemento cerâmico mais estável na superfície e não por transformações causadas na microestrutura. / This study aimed to evaluate the effect of the plasma-assisted PVD TiN and TiAlN/TiAlCrN coatings in the Ti-6Al-4V alloy under creep conditions at 600 °C and under corrosion conditions in environments containing chloride at 25, 60 and 80 °C. The study was complemented by microstructural and surface coatings analysis using XRD, optical, scanning and transmission electron microscopy, microhardness and isothermal oxidation. The results showed that the Ti-6Al- 4V alloy with Widmanstätten morphology presented an average hardness of 343 HV for as received condition. After treatment by plasma PVD, it was observed a TiN based coating, with 2,2 ?m and composition of Ti0,7N. The TiAlN/TiAlCrN based coating presented 6 ?m of thickness and composition of (Ti0,38Al0,62)N/(Ti0,31Al0,50Cr0,19)N. Anodic polarization and open circuit potential showed that Ti-6Al-4V alloy had active behavior with active - passive transition in HCl solution and passive behavior in NaCl solution at 25, 60 and 80 °C. The TiN and TiAlN/TiAlCrN coated samples showed passive behavior in both corrosive solutions and at all studied temperatures. The TiN coated sample showed the lowest values of secondary creep rate for stresses greater than 222 MPa, however, the plasma nitrided sample showed higher levels of service life and ductility. The analysis of stress exponents, activation energy and dislocations structures indicated that the main mechanism of creep was controlled by climbing dislocations. The damage tolerance parameter (W) calculation contributed to indicate that TiN and TiAlN/TiAlCrN coatings, although protect the surface from oxidation, decreased plastic deformation ability throughout tertiary stage and service life of the Ti-6Al-4V alloy, decreasing ductility. Finally, the surface treatments, used in this study, were efficient for their protective effect by depositing a more stable ceramic compound on surface and not by transformations caused on microstructure.
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Aderência bacteriana: estudo in vitro de superfície de aço inoxidável e liga de titânio-alumínio-vanádio de uso ortopédico / Bacterial adherence: an in vitro study of stainless steel and titanium-aluminium-vanadium alloy surfaces of orthopedic useBasso, Ana Cristina 24 June 2009 (has links)
O uso de metais na fabricação de implantes ortopédicos iniciou-se nas primeiras décadas do século XX. O aumento do uso de biomateriais implantáveis aumentam também os casos de infecção. A colonização da superfície do biomaterial pode ter início no momento da inserção do corpo estranho no organismo e geralmente é causada por microrganismos da microbiota da pele ou região adjacente ao implante. Este estudo teve por objetivo avaliar por métodos microbiológicos e microscópio eletrônico de varredura (MEV), a aderência bacteriana à superfície de aço inoxidável e liga de titânio de uso médico, bem como a molhabilidade da superfície destes metais. As bactérias usadas foram Staphylococcus epidermidis ATCC 12228 e Staphylococcus aureus ATCC 25923. Os discos de aço inoxidável (15,0 mm de diâmetro x 2,0 mm de espessura) e de liga de titânio (12,0 mm de diâmetro x 2,0 mm de espessura) foram inseridos, asséptica e separadamente, em tubos contendo 15,0 mL de caldo Mueller Hinton e 200,0 \'mü\'L de suspensão bacteriana da ordem de \'10 POT.8\' UFC/mL. Cada bactéria foi estudada individualmente. Os tubos foram incubados por 1, 6, 24, 48 e 72 horas sob agitação a 37 graus Celsius. Após os períodos de incubação, os discos foram retirados do caldo de cultura e submetidos ao banho de ultrassom em 5,0 mL de solução fisiológica 0,85% esterilizada. Deste líquido, foram realizadas diluições da ordem de \'10 POT.-1\' a \'10 POT.-4\' para a quantificação de células viáveis. Os valores foram expressos em UFC/mL. Para S. epidermidis sobre a liga de titânio, o número de células viáveis foi em 1 hora: 7,20 x \'10 POT.4\'; 6 horas: 3,90 x \'10 POT.6\'; 24 horas: 3,80 x \'10 POT.6\'; 48 horas: 9,70 x \'10 POT.6\' e 72 horas: 1,00 x \'10 POT.7\'. Sobre o aço inoxidável, o número de células viáveis foi em 1 hora: 3,00 x \'10 POT.3\'; 6 horas: 2,90 x \'10 POT.6\'; 24 horas: 3,20 x \'10 POT.6\'; 48 horas: 1,41 x \'10 POT.7\' e 72 horas: 1,88 x \'10 POT.7\'. Para S. aureus ) sobre a liga de titânio, o número de células viáveis foi em 1 hora: 2,00 x \'10 POT.3\'; 6 horas: 1,00 x \'10 POT.4\'; 24 horas: 3,10 x \'10 POT.4\'; 48 horas: 4,30 x \'10 POT.4\' e 72 horas: 5,80 x \'10 POT.3\'. Sobre o aço inoxidável, o número de células viáveis foi em 1 hora: 6,00 x \'10 POT.3\'; 6 horas: 2,00 x \'10 POT.3\'; 24 horas: 1,50 x \'10 POT.4\'; 48 horas: 3,20 x \'10 POT.5\' e 72 horas: 6,00 x \'10 POT.3\'. Ambas as superfícies metálicas foram caracterizadas como de média molhabilidade, onde a liga de titânio teve média \'+ OU -\' desvio padrão de 39,016 \'+ OU -\' 11,267 e o aço inoxidável 58,083 \'+ OU -\' 7,165. Tanto o S. aureus quanto o S. epidermidis aderiram às superfícies dos biomateriais estudados, como foi observado por meio de MEV. Com base nos resultados é possível concluir que os dois microrganismos são capazes de aderir a superfícies metálicas. Isto aumenta a preocupação quanto à patogênese das infecções relacionadas a implantes ortopédicos, uma vez que esses microrganismos estão presentes na pele humana e oferecem o risco de reações inflamatórias e infecção, promovendo a perda do implante para efetivar a cura. / The utilization of metals in the manufacture of orthopedic implants started in first decades of twentieth century. The increased use of implantable biomaterials increased also infection cases. Biomaterial surface colonization can start at the moment of foreign body insertion in the organism and is usually caused by microorganisms of skin microbiota or adjacent region to the implant. This study aimed to evaluate microbiological methods and scanning electron microscopy (SEM), the bacterial adhesion to surface of stainless steel and titanium alloy of medical use, as well as the surface wetability of these metals. The used bacteria were Staphylococcus epidermidis ATCC 12228 and Staphylococcus aureus ATCC 25923. The stainless steel (15,0 mm diameter x 2,0 mm thick) and titanium alloy (12,0 mm diameter x 2,0 mm thick) discs were inserted, aseptic and individually, into tubes containing 15,0 mL Mueller Hinton broth and 200,0 \'mü\'L of bacterial suspension with \'10 POT.8\' CFU/mL concentration. Each bacterium was individually studied. The tubes were incubated for 1, 6, 24, 48 and 72 hours under agitation at 37 Celsius degrees. After incubation periods, the discs were removed from culture broth and submitted to the ultrasound bath in 5,0 mL of sterile saline. From this liquid were realized dilutions of \'10 POT.-1\' to \'10 POT.-4\' to quantify the viable cells. Values were expressed in CFU/mL. S. epidermidis over titanium alloy viable cells number was in 1 hour: 7,20 x \'10POT.4\'; 6 hours: 3,90 x \'10 POT.6\'; 24 hours: 3,80 x \'10 POT.6\'; 48 hours: 9,70 x \'10 POT.6\' and 72 hours: 1,00 x \'10 POT.7\'. Over stainless steel viable cells number was in 1 hour: 3,00 x \'10 POT.3\'; 6 hours: 2,90 x \'10 POT.6\'; 24 hours: 3,20 x \'10 POT.6\'; 48 hours: 1,41 x \'10 POT.7\' and 72 hours: 1,88 x \'10 POT.7\'. To S. aureus over titanium alloy viable cells number was in 1 hour: 2,00 x \'10 POT.3\'; 6 hours: 1,00 x \'10 POT.4\'; 24 hours: 3,10 x \'10 POT.4\'; 48 hours: 4,30 x \'10 POT.4\' and 72 hours: 5,80 x \'10 POT.3\' and over stainless steel viable cells number was in 1 hour: 6,00 x \'10 POT.3\'; 6 hours: 2,00 x \'10 POT.3\'; 24 hours: 1,50 x \'10 POT.4\'; 48 hours: 3,20 x \'10 POT.5\' and 72 hours: 6,00 x \'10 POT.3\'. Both metal surfaces were characterized as medium wetability, where the contact angle of titanium alloy was mean \'+ OU -\' standard deviation 39,016 \'+ OU -\' 11,267 and stainless steel 58,083 \'+ OU -\' 7,165. Both S. aureus as S. epidermidis adhered to surfaces of biomaterials studied, as observed by SEM. Based on the results we concluded that two microorganisms are able to adhere to metal surfaces. This increases the concern about the pathogenesis of infections related to orthopedic implants, since these microorganisms are present in human skin and provide the risk of infection and inflammatory reactions, furthering implant loss to effective cure.
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