Many industries including the medical, aerospace, and automobile industries have increasingly adopted the use of shape memory alloys (SMAs) for a plethora of applications due to their unique thermomechanical properties. From the commercially available SMAs in the market, binary NiTi SMAs have shown the most desirable properties. However, SMA properties can be significantly affected by the fabrication process. One of the most familiar applications of NiTi SMAs is in the design of actuating devices where the shape memory effect properties are highly advantageous. Spring NiTi SMA actuators are among the most commonly used and are generally made by torsion loading a straight wire. Consequently, stress concentrations are formed causing a reduction in recovery force. Other methods for producing springs and other NiTi SMA components is the fast emerging manufacturing method of additive manufacturing (AM). AM often uses metal powders to produce the near-net shape components. A major challenge for SMAs, in particular, is their well-known composition sensitivity. Therefore, it is critical to control composition in NiTi SMAs. In this thesis, a novel method for processing NiTi SMAs for pre-alloyed NiTi SMA powders and springs is presented. A low pressure and low temperature hydriding-pulverization-dehydriding method is used for preparing the pre-alloyed NiTi SMA powders with well-controlled compositions, size, and size distributions from wires. By hydrogen charging as-drawn martensitic NiTi SMA wires in a heated H3PO4 solution, pulverizing, and dehydriding, pre-alloyed NiTi powders of various well-controlled sizes are produced. In addition, a low pressure and low temperature hydriding-dehydriding method is used for producing NiTi SMA helixes from wires. The helix pattern in the pre-alloyed NiTi SMA wires was obtained by hydrogen charging NiTi SMA 500 μm diameter wires at different time intervals, followed by dehydriding to remove the hydrogen. The wires, powders, and resulting helixes were characterized using scanning electron microscopy (SEM), differential scanning calorimetry (DSC), and x-ray diffraction (XRD). The relationship between the wire diameter, powder particle size, and helix geometry as a function of hydrogen charging time is investigated. Lastly, the recovery behavior due to the shape memory effect is also investigated after dehydriding.

Thesis (M. Tech. (Engineering: Mechanical)) -- Central University of Technology, Free State, / The Centre for Rapid Prototyping and Manufacturing (CRPM) at the Central University of Technology, Free State (CUT) manufactures implants using Electro Optical Systems (EOS) titanium Ti-6Al-4V alloy powder (further referred to as EOS Ti64 powder) by means of Direct Metal Laser Sintering (DMLS) process on the EOSINT M 270 machine. For this reason, there is a need to characterise and acquire knowledge of the basic properties of direct metal laser sintered EOS titanium Ti-6Al-4V alloy samples (further referred to as DMLS Ti64 samples) under static tensile loading in order to provide the CRPM with engineering design data. The first objective of this Master’s study is to acquire the characteristics of EOS Ti64 powder in order to ascertain its suitability in the DMLS process. Secondly, the study aims to assess tensile properties and elastic constants of DMLS Ti64 samples produced from the set process parameters of EOSINT M 270 machine. Thirdly, it is to investigate microstructures of DMLS Ti64 samples subjected to different heat treatment techniques which will eventually assist in the determination of a suitable heat treatment technique that will yield higher ductility. Finally, the study aims to validate the static behaviour of DMLS Ti64 samples subjected to the static tensile loading up to a yield point in order to determine failure due to yielding. The samples were manufactured at CRPM Bloemfontein. The metallographic examinations, heat treatment and the determination of mechanical properties were done at the CSIR in Pretoria. Optical Microscope (OM) and Scanning Electron Microscope (SEM) were used to determine microstructures of DMLS Ti64 samples while Energy Dispersive X-Ray (EDX) analyses were performed using SEM. The samples were heat treated at temperatures of 700, 1000 and 1100°C respectively, and subsequently either cooled with the furnace, air or were water quenched. The mechanical property tests included tensile, hardness and determination of elastic constants. The static behaviour of DMLS Ti64 samples under static tensile load up to a yield point was predicted and verified using ABAQUSTM Finite Element Analysis (FEA). The stress-strain curves from ABAQUSTM were interpreted using MDSolid program. The point of interest was Von Mises yield stress at 0.2% offset, in order to determine failure due to yielding. EOS Ti64 powder particles were spherical in shape and the alpha and alpha+beta phases were identified. As-laser sintered samples possess a very fine and uniform alpha case with islands of martensitic plates; samples were brittle and showed low levels of ductility with an average elongation of 2.6% and an area reduction of 3.51%. Ultrasonic test results showed that DMLS Ti64 samples have Young’s modulus of 115 GPa, Shear modulus of 43 GP, a bulk modulus of 109 GPa and Poisson’s ratio of 0,323 while the density was 4.4 g/cm3. Slow cooling of DMLS Ti64 samples from 1000 and 1100oC resulted in a microstructure constituted more by the alpha phase of lower hardness than those from 700oC and as-laser sintered samples. High hardness was obtained by water quenching. The water quenched samples showed martensitic transformation and high hardness when compared to furnace cooled samples. Beta annealing tailored a microstructure of as-laser sintered samples into a lamellar structure with different lath sizes as per cooling rate. Beta annealing improved ductility levels up to 12.67% elongation for samples furnace cooled for 4 hours and even higher to 18.11% for samples furnace cooled for 34 hours, while area reduction increased to 25.94% and 33.39%, respectively. Beta annealing conversely reduced yield strength by 19.89% and ultimate tensile strength was reduced by 23.66%. The calculated maximum Von Mises stresses found were similar to the FEA interpreted results. The average percentage error, without the stress concentration factor, was approximately 8.29%; with the stress concentration factor included, it was 0.07%. The small reaction forces induced in both x-axis and z-axis contributed to this error of 0.07% between the calculations and ABAQUSTM FEA results. Samples that were not heat treated fell outside the Von Mises criterion and failed due to yielding. This justified the brittleness found in the tensile test results where elongation and area reduction were 2.6% and 3.51% respectively. However, all samples that were heat treated fell within the Von Mises criterion. The objectives of this study were achieved; the mechanical properties were similar to those of standard specification for wrought annealed Ti-6Al-4V alloy for surgical implant applications and EOS GmbH manufacturer’s material data sheet. DMLS Ti64 samples must be beta annealed in order to attain higher levels of ductility. A recommendation was made to further investigate the effect of heat treatment on the other mechanical properties. Furthermore, detailed results of basic properties of DMLS Ti64 samples are provided in the appendices in chart format and were written on a CD disc.

Les alliages de titane α/β ont beaucoup d’applications dans des domaines industriels divers comme l’aéronautique. Le phénomène de globularisation qui se produit lors de traitements thermomécaniques est un phénomène important dans la mesure où une microstructure globulaire présente une tenue mécanique et une ductilité accrues.Les microstructures lamellaires sont constituées de colonies de lamelles de phase α parallèles qui se développent dans les grains β au cours de leur refroidissement. La globularisation se fait en deux étapes : les lamelles se subdivisent d’abord en segments plus courts, puis ces segments globularisent, au cours de la déformation à chaud et des traitements thermiques. La subdivision des lamelles se fait au niveau des sous-joints formés au cours de la déformation à chaud. Lors de traitements thermiques prolongés, les plus gros globules de phase α grossissent au détriment des plus petits. La formation des sous-joints et le grossissement des globules n’ont pas été étudiés en détail dans ce travail. L’accent a été mis sur les mécanismes de migration des interfaces α/β et α/α qui conduisent à la subdivision des lamelles et à leur globularisation.Des essais de compression à chaud et des traitements thermiques appliqués à des échantillons de Ti-6Al-4V ont permis de confirmer que l’épaisseur des lamelles et de leur orientation sont des facteurs importants pour la globularisation. Les lamelles plus fines et celles orientées parallèlement à l’axe de compression globularisent plus facilement. Ce travail expérimental a permis de mieux appréhender la complexité du phénomène de globularisation et d’introduire un cadre numérique adapté pour sa simulation. Une méthode à champ complet, basée sur la méthode Level-Set dans un cadre Eléments Finis, a ainsi été testée pour simuler les mécanismes physiques de migration interfaciale menant à la subdivision des lamelles et à l'évolution vers une forme globulaire. Les premiers résultats sont très prometteurs et illustrent le potentiel du cadre numérique proposé. / Α/β titanium alloys have many industrial applications in various fields such as aeronautics. Spheroidization is a phenomenon that occurs in initially lamellar α/β titanium alloys during thermomechanical processing and receives considerable attention as spheroidized microstructures exhibit enhanced strength and ductility.Lamellar microstructures are made of colonies of parallel α lamellae developed inside β grains while they are cooled down. Spheroidization actually proceeds in two successive steps: the lamellae first split into smaller α laths, which subsequently undergo spheroidization. This occurs during hot-deformation and subsequent annealing. Lamella splitting occurs where subboundaries were formed inside lamellae during hot-deformation. Over long term annealing the spheroidized α phase particles undergo coarsening. The formation of subboundaries and coarsening were not addressed in this work. The focus has been placed on the interfacial kinetics mechanisms leading α lamellae splitting during the first stages of spheroidization.Hot compression tests and subsequent annealings carried out on Ti-6Al-4V samples confirmed that the thickness and the orientation of the lamellae are important factors with regards to spheroidization. Thinner lamellae and lamellae oriented parallel to the compression axis spheroidize faster. Those experiments contributed to a better understanding of the phenomenon and allowed to introduce a suitable numerical framework to simulate the early stages of spheroidization. A full field method in a Finite Element/ Level Set framework has thus been tested for simulating the involved physical mechanisms of interface migration that lead to lamellae splitting and the subsequent shape evolution of the α laths towards a spheroidal shape. First results are promising and illustrate the potential of this numerical framework

Orientador: Carlos Roberto Grandini / Banca: Marize Varella de Oliveira / Banca: Nilson Tadeu Camarinho de Oliveira / O Programa de Pós-Graduação em Ciência e Tecnologia de Materiais, PosMat, tem caráter institucional e integra as atividades de pesquisa em materiais de diversos campi da Unesp / Resumo: Desde 1970, o titânio e algumas de suas ligas são vastamente usados na fabrição de próteses e dispositivos especiais nas áreas médica e odontológica devido às suas propriedades como baixos valores de módulo de elasticidade (Módulo de Young), resistência à corrosão e características de biocompatibilidade. A presença de elementos intersticiais (oxigênio, carbono, nitrogênio e hidrogênio) altera de maneira significativa as propriedades mecânicas da liga, principalmente suas propriedades elásticas, causando endurecimento ou fragilização da liga. As medidas de espectroscopia mecânica constituem uma ferramenta poderosa para o estudo da interação destes elementos substitucionais e intersticiais com a matriz metálica. O objetivo do trabalho foi prepararA LIGA Ti-15Mo por fusão a arco, e estudar a influência de tratamentos térmicos e do oxigênio presente em solução sólida, na estrutura, propriedades mecânicas, químicas, anelásticas e biocompatibilidade da liga. Os resultados de difração de raios X analisados pelo método de Rietveld permitiram quantificar as fases presentes na microestrutura, estando de acordo com as micrografias obtidas. Os resultados de dureza e módulo de elasticidade mostraram ser sensíveis à concentração de oxigênio e à microestrutura da liga. Nos ensaios de corrosão houve uma melhora significativa do potencial de corrosão após as dopagens com oxigênio. As medidas de espectroscopia mecânica apresentaram estruturas de relaxação e foram identificados os processos constituintes. Os ensaios de biocompatibilidade mostraram que a liga em questão pode ser considerada biocompatível / Abstract: Since 1970, titanium and some of its alloys have been widely used in the manufacture of special devices and prostheses in medical and dental areas due to properties which include low elasticity modulus values, corrosion resistance and characteristics of biocumpatibility. The presence of interstial elements (carbon, nitrogen, oxygen and hydrogen) significantly alters the alloy's mechanical properties, mainly its elastic properties, causing either a hardening or softening of the alloy. Mechanical spectroscopy measurements are a powerful tool to study the interaction of these substitutional and interstitial elements with a metallic matrix. The aim of this work was to prepare the Ti-15Mo alloy by arc-melting and study the influence of heat treatments and oxygen present in the solid solution of the structure, as well as the mechanical, chemical and anelastic properties, and biocompatibility of the alloys. The results of x-ray diffraction were analyzed by the Rietveld Method to allow the phases present in the microestructure to be quantified according to the obtained micrographies. The hardness and elasticity modulus results were sensitive to the oxygen concentration and the alloy microstructure. In corrosion tests there was a significant improvement of the corrosion potential after the oxygen dopyng. The mechanical spectroscopy measurements showed relaxation structures, and constituent relaxation processes were identified. The biocompatibility tests showed that the alloy in question can be considered biocompatible / Mestre

The area of research dealing with joining of dissimilar metals has been active in recent time. Although fusion and non-fusion techniques of joining have been effectively used for manufacturing components, a comprehensive scientific understanding of the process is lacking. This void exists both in fusion and non-fusion welding methods. The present investigation addresses some of these aspects. The investigation consists of two sections - Part A and Part B. Part A is on Friction welding and Part B deals with Fusion welding using laser. Each section has two chapters each. Following an introductory chapter, basic aspects of friction welding is presented in chapter 2. Chapter 3 deals with the work on friction welding of Fe-Cu couple. Fe-Cu couple is a system with positive heat of mixing. After a brief introduction on various non-equilibrium processes that can occur in this system, experimental details and results are presented. Using the results an attempt is made to understand the flash formation, formation of pores at the interface and the formation of chemically altered zone. It is observed that a chemically altered layer forms predominantly on the Cu side of the interface. It consists of Fe entrapped as fragments/fine crystals and as solid solution in Cu matrix. This zone has higher thickness at the edges than at the center. The mechanism of formation of this interfacial layer which is central to the joining process is related to the fracture and transport of fragments during plastic deformation. Fe forms solid solution in copper under non-equilibrium conditions promoted by shear energy. Using the concept of ballistic mixing, the formation of solid solution is explored. Using nano-indentation experiments mechanical properties of the weldment is estimated and an attempt is made to correlate mechanical properties with the amount of second element present in that location. The chapter 4 in part A deals with the friction welding of Ni-Ti couple. Ni-Ti system has negative heat of mixing and it forms a number of intermetallics. After a brief introduction to the chapter, various experimental techniques and strategies followed to carry out the experiments are explained. Following these, the results are presented. It is observed that TiNi3 formed at initial stage. Theories based on effective heat of formation and surface energy also predict the nucleation of TiNi3. With the continuation of frictional processes, the formation of TiNi and Ti2Ni phases were also observed. Formation of Ti2Ni was shown to greatly accelerate due to shear process. In this system two complementary processes like ballistic mixing and thermal assisted diffusion accelerate Ti2Ni formation. From mechanical tests it is found that Ti2Ni layer in the weldment is weak and hence formation of Ti2Ni in the weldment is detrimental. In chapter 5 an introduction to fusion welding of dissimilar metals is presented as background materials for the subsequent chapters. Chapter 6 deals with nature of segregation of Ag during laser welding of Fe-Ni couple. Ag is used as a tracer to probe fluid flow in the Fe-Ni couple during laser welding. Ag is immiscible both in Fe and Ni whereas Fe and Ni form a complete solution at an elevated temperature and in liquid state. Besides the experimental work, numerical simulation of the weld pool were carried out using homogeneous mixture model using SIMPLER algorithm. Experiments and simulations indicate that fluid flow is asymmetrical and in the deep penetration welding strong convection in the pool drives the tracer to the top of the pool. Overall distribution of the tracer is due to the combined effect of convection and diffusion. In shallow welding there exists a boundary region where tracer does not penetrate. In chapter 7 the results of instrumented indentation experiments on laser welded Fe-Cu weldment has been presented. It was earlier reported that during laser welding of Fe-Cu couple, a variety of microstructures evolves at various locations in the weldment and hardness of the weldment were found to be very high. Here an attempt has been made to explore in details the origin of such a high hardness. The chapter starts with a description of various microstructures that are observed in this weldment followed by the various procedures used for extracting data from instrumented indentation tests. It is followed by the presentation of the experimental results. It is found that rule of mixture along with Hall-Petch strengthening explains the observed increase in hardness of the weldment. The fine scale microstructure consisting of alternate Fe rich and Cu rich layers increases the hardness of the weldment. On copper side of the weldment, composition and scale of microstructure fluctuates and so also the hardness. Finally in chapter 8 overall conclusions of the various chapters in the thesis have been summarised.

L'optimisation des états de surface constitue un enjeu majeur pour les biomatériaux utilisés dans le domaine biomédical. Le titane (Ti) et ses alliages à base de nickel (NiTi) restent à ce jour les biomatériaux métalliques de prédilection dans nos applications cliniques en Odontologie (implants dentaires, instruments endodontiques, et arcs orthodontiques). Le but de nos recherche est d'optimiser les surfaces du Ti et NiTi en les fonctionnalisant par des films multicouches de polyélectrolytes (FMP). Notre travail propose d'étudier différents paramètres devant être impérativement validés avant d'envisager une quelconque application biomédicale in vivo avec ce type de revêtement. Une recherche bibliographique exhastive appuie notre recherche expérimentale. Le premier axe du travail propose de déterminer si des FMP peuvent effectivement s'adsorber chimiquement sur le Ti et le NiTi. qui plus est, une étude biologique est réalisée avec des cellules humaines pour tester la biocompatibilité des ces surfaces fonctionnalisées. La deuxième partie se concentre sur la biocompatibilité de la couche précurseur des FMP à base de polyéthyléneimine (PEI). Les résultats mettent en lumière une certaine cytotoxicité de la PEI envers des ostéoblastes et des fibroblastes gingivaux humain. Pour clore ce travail, nous réalisons des essais de stérilisation afin d'évaluer l'influence d'un tel procédé sur les FMP en terme de caractérisations physico-chimique et biologique des surfaces. La perspective d'une application biomédicale avec les FMP semble prometteuse, notamment en y introduisant des molécules bioactives. Cependant, bien d'autres paramètres sont encore à étudier avant d'envisager une application expérimentale et/ou clinique in vivo. Nous pouvons citer par exemple, le vieillissement des FMP, leur comportement en milieu salivaire ou fluoré, ou encore leur résistance à l'usure. Ces différents éléments rentrent dans les perspectives d'un projet post-doctoral. / Optimization of surface properties is a fundamental priority for biomaterials uses in biomedical applications. Titanium (Ti) and nickel-titanium alloys (NiTi) are the references in terms of metallic biomaterials for clinical applications in Odontology (Dental implants, endodontic instrumentations, and orthodontic arches). The aim of our work is to study the Ti and NiTi surfaces coated with polyelectrolytes multilayers films (PEM). Our work study various parameters needed to be validated before using this functionalized surface treatment for biomedical and clinical applictions in vivo. The first part of this work aims at defining the possibility to chemically adsorb PEM coating on Ti and on NiTi surfaces. Moreover, we have realized a biological study with human cells to test the biocompatibility of functionalized surfaces. In the second part of this thesis, we tested the biocompatibility of the multilayered structure in regards to the precursor base layer of PEM, the polyethyleneimine (PEI). Our reuslts show that the PEI is not cytotoxic towards osteoblasts and human gingival fibroblasts. Finally, we relaized tests of sterilization to evaluate PEM stability in terms of physico-chemical and biological surface characterizations. The development of specific biomedical applications for PEM is an exciting perspective, especially when these firms are functionalized with bioactive molecules. However, many other parameters murst be studied before imagining an experimental or clinical application in vivo. As an example, PEM degradation as well as behaviour in salivary or fluoride solution, still needs to be tested.

Coordenação de Aperfeiçoamento de Pessoal de Nível Superior / No presente trabalho, foram realizados ensaios de tribocorrosão no aço inoxidável AISI 304L, no titânio comercialmente puro (CPTi) e na liga de titânio Ti6Al4V em solução aquosa de 0,90% m/v NaCl. Amostras de ligas de titânio com tratamento térmico superficial de refusão a laser também foram utilizadas. Um tribômetro do tipo pino-no-disco com contracorpo de alumina foi usado. Técnicas eletroquímicas in situ de monitoramento em circuito aberto, espectroscopia de impedância eletroquímica, curvas de polarização e amperimetria de resistência nula foram empregadas. Os resultados obtidos indicam que o desgaste tribocorrosivo das ligas de titânio é mais intenso do que o observado no aço inoxidável, apresentando perfis de superfície mais irregulares. A análise da impedância eletroquímica mostrou que todos os materiais utilizados apresentam uma rápida recuperação da camada passiva, exibindo módulos e fases um pouco menores do que os medidos antes do desgaste. Sob atrito, os diagramas de impedância apresentam uma forte redução do módulo. Sob desgaste, o expoente α do elemento de fase constante (CPE) atinge seu valor mais baixo, enquanto o parâmetro γ é máximo. As curvas de polarização exibem potenciais menores e densidades de corrente de corrosão maiores durante o desgaste. O tratamento de refusão a laser, embora mude a microestrutura e a dureza superficial das amostras, não indica uma mudança aparente nos parâmetros eletroquímicos sob tribocorrosão, bem como do coeficiente de atrito. Nos ensaios de amperimetria de resistência nula, foi possível estimar a corrente mensurada no ARN por meio do emprego de um circuito elétrico equivalente. A densidade espectral de potência dos sinais de potencial e de corrente exibe a frequência de rotação (1,25 Hz) e seus harmônicos. Para baixas frequências (abaixo de 10 mHz), o decaimento obedece à relação 1 ⁄ e 1⁄ para os sinais de potencial e corrente, respectivamente. / In this study, tribocorrosion tests were performed in stainless steel AISI 304L, commercially pure titanium (CPTI) and Ti6Al4V titanium alloy in 0.9% m/v NaCl aqueous solution of. Titanium alloy sample with laser remelting treatments were also tested. A pin-on-disc tribometer with alumina counterbody was used. In situ electrochemical techniques of open circuit monitoring, electrochemical impedance spectroscopy, polarization curves and zero resistance ammeter were employed. Results indicate tribocorrosion wear of titanium alloys is more intense than that observed in stainless steel, presenting more irregular surface profiles. Analysis of electrochemical impedance spectroscopy showed all materials used have a fast recovery of the passive layer, showing modulus and phase slightly smaller than those measured prior to wear. Under friction, impedance diagrams show a strong reduction of the modulus. Under rubbing, exponent α of the constant phase element (CPE) reaches its lowest value, while γ parameter is maximum. Polarization curves show lower corrosion potential and higher corrosion current density during rubbing. Laser remelting treatments, although changes microstructure and surface hardness of the samples, does not indicate an apparent change in electrochemical parameters under tribocorrosion, as well as in coefficient of friction. In zero resistance ammeter tests, it was possible to estimate the current measured in ZRA using an electrical equivalent circuit. Power spectral density of the potential and current signals exhibits the rotation frequency (1.25 Hz) and its harmonics. For lower frequencies (below 10 mHz), the decay follows 1⁄ and 1⁄ roll-off for signals of potential and current, respectively.

O câncer de cabeça e pescoço tem maior prevalência em homens, predominantemente de meia ou terceira idade, caracterizando um grupo de indivíduos com grande probabilidade em ter realizado implantes dentários ósseointegrados. A maior parte desses implantes é feito de titânio e a interação dos fótons de raios X com esse material de alto número atômico e elevada densidade eletrônica gera grande espalhamento de radiação e perturbação de dose nas suas interfaces, gerando incertezas dosimétricas nos tratamentos de radioterapia de cabeça e pescoço. O objetivo desse estudo é avaliar a influência dosimétrica dos implantes dentários de titânio em VMAT de cabeça e pescoço. Para isso, foi realizada irradiação de um fantoma de água sólida com a presença de um implante dentário de titânio por campo direto e com a aplicação adaptada para VMAT dos testes CShape Easy e Head and Neck, propostos pelo TG 119. O planejamento desses casos foi realizado conforme critérios determinados pela AAPM, com o software Monaco 5.0, e a execução do tratamento em Acelerador Linear Synergy, da Elekta. As medidas foram realizadas com câmara de ionização Semiflex e eletrômetro UNIDOS PTW, filme radiocrômico GafChromic EBT3 com varredura no scanner Epson Expression XL e análise com o software VeriSoft 6.0. Os resultados da distribuição e perfis de dose encontrados na irradiação de campo direto comprovam que a presença de implante dentário de titânio causa perturbações de dose significativas. Em decorrência da presença do material, também foi aumentada a diferença entre dose calculada e medida, quando comparada à irradiação de fantoma homogêneo. Porém na dosimetria dos casos do TG 119 essa diferença foi irrelevante. A dose calculada pelo software e a medida com a câmara de ionização tiveram diferenças insignificantes, assim como a concordância do critério gamma para os casos com e sem a presença do implante dentário de titânio. Os resultados encontrados são satisfatórios e compatíveis com testes de outros autores em irradiações de fantomas homogêneos. O impacto da presença do implante dentário de titânio pode ser minimizado através do delineamento manual do objeto metálico e do artefato gerado por ele e através da atribuição de valores de densidade eletrônica corrigidos a eles, além de incluí-los como órgãos com restrição de dose na otimização do planejamento. A partir da aplicação dos testes CShape Easy e Head and Neck do TG 119 da AAPM, foi comprovado que seguindo as recomendações descritas, o sistema de planejamento Monaco 5.0 com é capaz de realizar cálculos de dose com elevado grau de exatidão para VMAT de cabeça e pescoço em pacientes com implante dentário de titânio. / The head and neck cancer is more prevalent in men, predominantly middle or elderly age, featuring a group of individuals with high probability of having done osseointegrated dental implants. Most of these implants are made of titanium and the interaction of X-ray photons with this high atomic number material and high electron density generates scattering and disturbance on radiation dose in their interfaces, generating dosimetric uncertainties in the head and neck radiotherapy treatments. The aim of this study is to assess the dosimetric impact of dental implants of titanium in head and neck VMAT. For this, irradiation of phantom was performed in the presence of a titanium dental implant for direct field and with application of CShape Easy and Head and Neck tests proposed by the TG 119, adapted to VMAT. The planning of these cases was conducted according to criteria determined by the AAPM, with Monaco 5.0 software, and the treatment is in Linear Accelerator Synergy Elekta. The measurements were performed with Semiflex ionization chamber and electrometer US PTW, radiochromic film GafChromic EBT3 scanned with the Epson Expression XL scanner and analysis with the software VeriSoft 6.0. The results of the distribution and dose profiles found in direct irradiation field show that the presence of titanium dental implant causes significant dose disturbance. Due to the presence of the material was also increased the difference between the calculated and the measured dose when compared to irradiation of the homogeneous phantom. But in the dosimetry of TG 119 cases this difference was irrelevant. The dose calculated by the software and the measure with the ionization chamber had negligible differences, as well as the consent of the gamma criterion for cases with and without the presence of dental titanium implant. The results are satisfactory and consistent with other author’s tests in homogeneous phantoms. The impact of dental titanium implant presence can be minimized through the manual delimitation of the metal object and artifact generated and by assigning the electron density values corrected them, and include them as organs with dose constraints on optimization planning. From the testing CShape Easy and Head and Neck TG 119 of the AAPM, we have verified that following the recommendations described, the planning system Monaco 5.0 is capable of performing dose calculations with high degree of accuracy for head and neck VMAT in patients with titanium dental implant.

Coordenação de Aperfeiçoamento de Pessoal de Nível Superior / No presente trabalho, foram realizados ensaios de tribocorrosão no aço inoxidável AISI 304L, no titânio comercialmente puro (CPTi) e na liga de titânio Ti6Al4V em solução aquosa de 0,90% m/v NaCl. Amostras de ligas de titânio com tratamento térmico superficial de refusão a laser também foram utilizadas. Um tribômetro do tipo pino-no-disco com contracorpo de alumina foi usado. Técnicas eletroquímicas in situ de monitoramento em circuito aberto, espectroscopia de impedância eletroquímica, curvas de polarização e amperimetria de resistência nula foram empregadas. Os resultados obtidos indicam que o desgaste tribocorrosivo das ligas de titânio é mais intenso do que o observado no aço inoxidável, apresentando perfis de superfície mais irregulares. A análise da impedância eletroquímica mostrou que todos os materiais utilizados apresentam uma rápida recuperação da camada passiva, exibindo módulos e fases um pouco menores do que os medidos antes do desgaste. Sob atrito, os diagramas de impedância apresentam uma forte redução do módulo. Sob desgaste, o expoente α do elemento de fase constante (CPE) atinge seu valor mais baixo, enquanto o parâmetro γ é máximo. As curvas de polarização exibem potenciais menores e densidades de corrente de corrosão maiores durante o desgaste. O tratamento de refusão a laser, embora mude a microestrutura e a dureza superficial das amostras, não indica uma mudança aparente nos parâmetros eletroquímicos sob tribocorrosão, bem como do coeficiente de atrito. Nos ensaios de amperimetria de resistência nula, foi possível estimar a corrente mensurada no ARN por meio do emprego de um circuito elétrico equivalente. A densidade espectral de potência dos sinais de potencial e de corrente exibe a frequência de rotação (1,25 Hz) e seus harmônicos. Para baixas frequências (abaixo de 10 mHz), o decaimento obedece à relação 1 ⁄ e 1⁄ para os sinais de potencial e corrente, respectivamente. / In this study, tribocorrosion tests were performed in stainless steel AISI 304L, commercially pure titanium (CPTI) and Ti6Al4V titanium alloy in 0.9% m/v NaCl aqueous solution of. Titanium alloy sample with laser remelting treatments were also tested. A pin-on-disc tribometer with alumina counterbody was used. In situ electrochemical techniques of open circuit monitoring, electrochemical impedance spectroscopy, polarization curves and zero resistance ammeter were employed. Results indicate tribocorrosion wear of titanium alloys is more intense than that observed in stainless steel, presenting more irregular surface profiles. Analysis of electrochemical impedance spectroscopy showed all materials used have a fast recovery of the passive layer, showing modulus and phase slightly smaller than those measured prior to wear. Under friction, impedance diagrams show a strong reduction of the modulus. Under rubbing, exponent α of the constant phase element (CPE) reaches its lowest value, while γ parameter is maximum. Polarization curves show lower corrosion potential and higher corrosion current density during rubbing. Laser remelting treatments, although changes microstructure and surface hardness of the samples, does not indicate an apparent change in electrochemical parameters under tribocorrosion, as well as in coefficient of friction. In zero resistance ammeter tests, it was possible to estimate the current measured in ZRA using an electrical equivalent circuit. Power spectral density of the potential and current signals exhibits the rotation frequency (1.25 Hz) and its harmonics. For lower frequencies (below 10 mHz), the decay follows 1⁄ and 1⁄ roll-off for signals of potential and current, respectively.

L’apparition d’inclusions exogènes demeure un problème majeur pour les élaborateurs de titane. Afin d’améliorer la propreté inclusionnaire des lingots élaborés par le procédé de refusion à l’arc sous vide (Vacuum Arc Remelting), une étude numérique et expérimentale a été réalisée. La partie numérique de la thèse consiste à modéliser le comportement d’un défaut hard-α provenant de l’électrode consommable et tombant dans le puits liquide du lingot. Un modèle décrivant le processus de dissolution prédit l’évolution de la taille d’une inclusion durant son séjour dans le puits liquide. La trajectoire est déterminée à l’aide d’un modèle lagrangien tenant compte de la turbulence de l’écoulement en modifiant le coefficient de trainée. Les deux modèles ont été couplés et implémentés dans le logiciel SOLAR, qui simule la croissance d’un lingot VAR.Les résultats mettent en évidence la difficulté d’éliminer une inclusion hard-α avec une seule refusion, principalement à cause de la croissance d’une couche de phase β pendant les premiers moments de l’immersion. Le comportement global du défaut dépend fortement de l’hydrodynamique du puits et des caractéristiques de l’inclusion.Pour étudier la dissolution expérimentalement, des défautssynthétiques (hard-α et HDI) ont été immergés dans un bain de titane liquide chauffé dans un four à bombardement électronique. Les vitesses de dissolution ont été déterminées en mesurant les dimensions des défauts avant et après les expériences et ont été ensuite utilisées pour valider les modèles numériques. Par ailleurs, nous avons mis en évidence la grande influence de la température et de la vitesse de l’écoulement sur les cinétiques de dissolution / The presence of exogeneous inclusions has always been a major concern for the titanium industry. To help improve the inclusional cleanliness of VAR (Vacuum Arc Remelting) titanium ingots, a numerical and experimental study was undertaken.The numerical model is capable of predicting the motion and dissolution of a hard-α defect falling from the electrode tip into the ingot melt pool during vacuum arc remelting. It is implemented in SOLAR, a CFD code that simulates the ingot growth and solidification. The dissolution of the inclusion is governed by nitrogen diffusion from the defect towards the surrounding molten metal. A model describing this phenomenon predicts the particle size evolution and the nitrogen profile at each moment. The motion of the spherical particle is tracked using a Lagrangian model and the influence of turbulence is accounted for by a modification of the drag coefficient.Results show that inclusion removal is difficult with a single melt since the growth of a β-phase layer leads to an initial increase in the defect size. The inclusion behaviour is highly dependent on the pool hydrodynamics and on inclusion characteristics.In order to clarify dissolution aspects of these defects and to measure their dissolution kinetics, synthetically processed defects were introduced into molten titanium heated in an electron beam melting furnace. Dissolution rates were calculated by measuring the size of the defects before and after the experiments and the results were used to validate the numerical models. Furthermore, the experiments show that dissolution kinetics highly depend on fluid motion and temperature