Ni/TiC metal matrix composites have been processed using the laser engineered net shaping (LENS) process. As nickel does not form an equilibrium carbide phase, addition of a strong carbide former in the form of titanium reinforces the nickel matrix resulting in a promising hybrid material for both surface engineering as well as high temperature structural applications. Changing the relative amounts of titanium and carbon in the nickel matrix, relatively low volume fraction of refined homogeneously distributed carbide precipitates, formation of in-situ carbide precipitates and the microstructural changes are investigated. The composites have been characterized in detail using x-ray diffraction, scanning electron microscopy (including energy dispersive spectroscopy (XEDS) mapping and electron backscatter diffraction (EBSD)), Auger electron spectroscopy, and transmission (including high resolution) electron microscopy. Both primary and eutectic titanium carbides, observed in this composite, exhibited the fcc-TiC structure (NaCl-type). Details of the orientation relationship between Ni and TiC have been studied using SEM-EBSD and high resolution TEM. The results of micro-hardness and tribology tests indicate that these composites have a relatively high hardness and a steady-state friction coefficient of ~0.5, both of which are improvements in comparison to LENS deposited pure Ni.

published_or_final_version / Dentistry / Master / Master of Dental Surgery

Numerous nickel titanium rotary file systems have been introduced in recent years. The recommended speed at which these files are to be operated varies widely between manufacturers. The purpose of this study was to test the number of rotations to fracture of NiTi rotary files when operated at different speeds and at different angles. Sixty size 25 Profile® nickel titanium rotary files were tested, thirty 0.04 and thirty 0.06 taper. Files were operated at speeds of 350 or 600 rpm and at angles of 25°, 28°, and 33.5°. The time to fracture was recorded and the numbers of rotations to fracture were calculated. The data was analyzed using a two-way ANOVA, and post hoc Tukey-Kramer multiple-comparison test with alpha = .001. The results show a significant difference in the number of rotations fracture according to taper and angle. Files of .06 taper fractured more readily than files of .04 taper as the speed increased, and the time to fracture decreased for both tapers as the angle increased. No significant difference was produced by the speed at which the files were operated. The number of rotations until fracture of NiTi rotary files is not related to the operational speed.

The purpose of this study was to compare the number of rotations to failure of three different rotary file systems. ProFile, Sequence, and Liberator files in sizes 25 and 40 with 0.04 taper were divided into groups of five and rotated against a grooved metal block mounted to a Universal testing machine at 31 and 34 degrees. Each file was rotated at 300 rpm until fracture occurred. The number of rotations to fracture were calculated. Use of a three-way ANOVA and Tukey's HSD multiple comparison tests revealed significant differences for the angle of deflection, size, and type of file. An increased angle of deflection resulted in a decreased number of rotations to failure for all three file types. An increased size of file also resulted in a decreased number of rotations to failure in all the groups. Liberator and Sequence files required fewer rotations to failure than ProFiles in all groups tested except the size 25 files rotated at the less severe angle. ProFiles appear to be more resistant to flexural fracture than Liberator and Sequence files unless the files are of smaller size with a less severe curvature. Care should be taken to limit the number of uses when using larger size files, especially Liberator and Sequence files, around severe curvatures.

O presente estudo teve como objetivo avaliar a resistência à fadiga cíclica flexural dos instrumentos de níquel- titânio, Hyflex CM (Coltène, EUA) e TF Adaptive (SybronEndo, EUA) em diferentes situações experimentais. Todas as limas que foram selecionadas possuíam conicidade 0,04 e diâmetro de ponta 35. Utilizou-se um dispositivo desenvolvido especificamente para realizar o ensaio flexural dinâmico. Os instrumentos TF Adaptive foram divididos em 3 grupos de acordo com o ângulo de curvatura do ensaio: 45º, 60º e 90º e cada grupo subdividido em 2 subgrupos de acordo com o tipo de movimento: rotação contínua e Adaptive. Cada subgrupo era composto por 15 instrumentos TF Adaptive, totalizando 90 instrumentos. Quinze instrumentos Hyflex CM formavam o grupo 4, no ensaio com ângulo de curvatura 90 graus e rotação contínua. A simulação foi realizada em canais artificiais de aço com ângulo de 45, 60, 90 graus e raio 5m m. O número de ciclos e o tempo em segundos até a fratura foram tabulados e analisados. Entretanto, a fadiga cíclica flexural foi significante maior nos três grupos em movimento Adaptive. E as limas TF Adaptive em seu próprio movimento tiveram maior número de ciclos e tempo até a fratura quando comparadas as Hyflex CM no ensaio de 90 graus. Portanto, conclui-se que o sistema Adaptive (limas TF Adaptive + movimento Adaptive) foi mais seguro à resistência á fadiga flexural, e no ensaio de 90 graus o sistema Adaptive foi mais resistente quando comparado com as limas Hyflex CM no movimento de rotação contínua. / The aim of this work to evaluate the cyclic fatigue resistance flexural the instruments of nickel-titanium, HyFlex CM (Coltène, USA) and TF Adaptive (SybronEndo, USA) in different experimental situations. All files that were selected had 0.04 taper and tip diameter 35. We used a device developed specifically to perform the dynamic flexural test. The TF Adaptive instruments were divided into 3 groups according to the angle of curvature of the test: 45, 60 and 90 and further divided in two subgroups according to the type of movement: continuous rotation and Adaptive. Each group consisted of 15 instruments TF Adaptive totaling 90 instruments. Fifteen HyFlex CM instruments formed the group 4 in the trial of bend angle 90 degrees and continuous rotation. The simulation was performed in artificial steel angled channels 45, 60, 90 degrees and radius 5m m. The number of cycles and the time in seconds until fracture were tabulated and analyzed. However, the cyclical flexural fatigue was significantly greater in the three groups Adaptive motion. And the TF Adaptive files on your own movement had a higher number of cycles and time to fracture when the HyFlex CM compared in 90-degree test. Therefore, it is concluded that the adaptive system (TF Adaptive Motion + Adaptive files) was safer resistance to flexural fatigue, and 90 degrees test Adaptive system is more resistant when compared with the HyFlex files into continuous.

O presente estudo avaliou a influência do hipoclorito de sódio a 1% e 2,5% na qualidade do acabamento superficial e na resistência à corrosão de duas limas endodônticas: Race® e Hyflex® através de ensaio eletroquímico de polarização potenciodinâmica cíclica (EPPC) e imagens obtidas por microscopia eletrônica de varredura (MEV). Para o EPPC foram utilizados vinte limas de cada marca comercial (#25, conicidade 0.04 e 25 mm de comprimento). Dez dos vinte instrumentos foram individualmente fixados pelo cabo a uma ponta de fio de cobre 0,12 mm de 20 cm de comprimento e posicionado no interior de uma célula eletroquímica com 500 mL de solução de hipoclorito de sódio (NaClO) 1% (Fórmula&Ação) à temperatura ambiente controlada em 23 ºC (±2) até cobrir a parte ativa do instrumento. Os registros foram feitos com o potenciostato da PAR modelo 273A. O ensaio foi repetido nos mesmos padrões para as outras dez limas da mesma marca comercial com o NaClO 2,5%. Além do EPPC, as limas foram submetidas a exames e análises em MEV antes e depois do teste de corrosão para a obtenção de fotomicrografias dos 3 (três) mm finais de cada lima com o intuito de estabelecer parâmetros para a avaliação final. Das fotomicrografias obtidas, 72 foram escolhidas, inseridas no Power Point sem legenda original de identificação, numeradas aleatoriamente para avaliação e projetadas num monitor para 06 avaliadores orientados e calibrados. Os dados obtidos foram tabulados e submetidos aos testes estatísticos pertinentes (Friedman, Wilcoxon e Mann-Whitney). A lima Hyflex® apresentou uma quantidade maior de alterações superficiais (ranhuras, manchas e materiais depositados) antes e depois do ensaio sendo mais suscetível à corrosão. Race® apresentou uma superfície mais polida e regular. Em relação a concentração do NaClO, percebeu-se que os defeitos presentes se tornavam mais evidentes para a concentração maior (2,5%). Nas duas concentrações os itens que apresentaram diferença significativa foram bordas, ranhuras, microcavidades, rebarbas e material depositado. Concluiuse que o acabamento superficial e a concentração da solução de NaClO influenciam a resistência à corrosão dos instrumentos de NiTi. A lima Race® apresentou menor corrosão e melhor acabamento de superfície do que a lima Hyflex® nas condições experimentais testadas. / The present paper evaluated the influence of 1% and 2.5% sodium hypochlorite in the quality of the surface finishing and resistance to corrosion of two endodontic files: Race® and Hyflex® by electrochemical test of cyclic power dynamics polarization (EPPC) and images obtained by scanning electronic microscopy (SEM). Twenty files of each commercial brand (#25, 0.04 taper and 25 mm length) were used in EPPC. Ten from the twenty instruments were individually fixed by the handle to a copper wire tip (0.12 mm diameter and 20 cm length) and placed in the interior of an electrochemical cell with 500 mL sodium hypochlorite solution (NaCIO) 1% (Fórmula e Ação) at the environment temperature controlled in 23ºC (±2) until covering the active part of the instrument. Recordings were made with a PAR potentiostat model 273A. The test was repeated in the same pattern to the other ten files from the same commercial brand with NaClO 2.5%. Besides EPPC, the files were submitted to the scanning electronic microscopy (SEM) test before and after the corrosion test to obtain photomicrographs of the final 3 mm of each file in order to establish the parameters for final evaluation. From the obtained photomicrographs, 72 were chosen and inserted in the Power Point without the original identification legend, randomly numbered for evaluation and projected on the screen to the 06 guided and calibrated evaluators. Data obtained were tabbed and submitted to the relevant statistical tests (Friedman, Wilcoxon and Mann-Whitney). The Hyflex® file showed a higher amount of surface alterations (grooves, stains and deposited materials) before and after the test, being more susceptible to corrosion. Race® showed a more polished and regular surface. As to the NaClO concentration, it was seen that the present defects became more evident in the higher concentration (2.5%). In the two concentrations, the items that presented significant differences were edges, grooves, micro cavities, margins and deposited materials. Conclusion was that surface finishing and the concentration of the NaClO solution influenced the resistance to corrosion of NiTi instruments. The Race® file showed the least corrosion and the best surface finishing compared to the Hyflex® file under the tested experimental conditions.

O objetivo da presente pesquisa foi avaliar o comportamento da força em função da deflexão na ativação e desativação de fios ortodônticos de níquel-titânio, de secção circular (.016"). Ensaiaram-se três marcas de fio (Forestadent, GAC e Morelli). As temperaturas de ensaio foram três (32, 37 e 42ºC). As ativações máximas foram até 1, 2, 3 e 4mm. O espécime de ensaio consistiu de uma placa de resina acrílica, sobre a qual eram fixados cilindros metálicos por meio de parafusos, simulando dentes, com distribuição semelhante aos dentes naturais. Sobre os cilindros foram cimentados os bráquetes (distância de 8mm entre eles). Sobre os bráquetes era fixado, conforme clinicamente, o arco do fio em ensaio. O “dente" correspondente ao incisivo central era liberado (desparafusado) para poder se deslocar livremente no sentido vestíbulo-lingual durante os ensaios e o fio poder sofrer a deflexão. O conjunto era levado à máquina de ensaio (Instron), com câmara de temperatura controlada. Durante o ensaio a velocidade de deslocamento para a deflexão foi de 0,5mm/min. Durante a ativação e desativação as forças foram registradas de 0,10 em 0,10mm de deflexão. Por meio de software esses valores eram impressos numericamente e em gráficos da força em função da ativação/desativação. Com 4 ativações máximas, 3 marcas de fios e 3 temperaturas obtiveram-se 36 condições experimentais e com 5 repetições (n=5) foram feitos 180 ensaios. Os gráficos obtidos mostraram uma não linearidade entre força e deflexão e com ativação de 1 e 2mm não foi detectado platô de superelasticidade, mas que foi observado na desativação, das ativações máximas de 3 e 4mm. Dos gráficos e tabelas foram extraídos valores específicos para serem analisados e comparados: 1) força máxima de ativação; 2/3) diminuição da força na desativação de 0,20mm e 0,70mm (esta só na ativação de 3 e 4mm); 4/5) extensão e forças no platô (apenas nas ativações máximas de 3 e 4mm); 6/7/8) desativação até alcançar 50g de força, a partir de 0,80 e 1,80mm (ativações de 1 e 2mm), ou no final dos platôs (ativações de 3 e 4mm), a força ao iniciar-se a desativação, afastamento da origem ao registrar 50g de força; 9) deformação permanente ao atingir a força zero. As principais conclusões foram: a força de ativação máxima aumentou com o aumento desta e da temperatura, o material Morelli apresentou a menor e o GAC a maior; a diminuição da força máxima foi tanto maior quanto maior a ativação; apenas as ativações até 3 e 4mm apresentaram platôs de superelasticidade e que foram bem mais extensos na ativação de 4mm, que por sua vez apresentaram menor força; em todos os ensaios for observada deformação permanente / The purpose of this study was to evaluate the behaviour of force as function of loading and unloading orthodontic nickel-titanium wires. Three defferent brands (Forestadent, GAC and Morelli) were tested. Testing temperature were 32, 37 and 42 o C. Loading were up to 1, 2, 3 and 4mm deflection. Specimens consisted of a acrylic base where were fixed metallic cylinders simulating teeth. Over the teeth were fixed brackets to maintain arch wire in position. Tooth corresponding to central incisor was loosened and at the correspondig bráquete was applied the force in an Instron equipment, with temperature control. Head speed was 0.5mm/min. During loading and unloading forces were read every 0.10mm deflection and registered. The pair values of forces and deflections were also plotted as graphs. With 4mm maximum loading, 3 brands and 3 temperatures were obtained 36 experimental conditions and with 5 repetitions (n=5) were performed 180 tests. Graphs showed that there is no linearity between forces and deflection and with loading up to 1 and 2mm was not obtained the formation of superelasticity plateaus. But they were observed with 3 and 4mm deflections. From the graphs and registered numerical values for each specimen were selected special values to be analysed: 1) maximum loading force; 2/3) force decrease during unloading 0.20 and 0.70mm (the last only at 3 and 4mm activation); 4/5) exte nsions and forces at plateaus (only for 3 and 4mm activations); 6/7/8) extension until 50g force, since 0.80 and 1.80mm (respectively activation up to 1 and 2mm), or ends of plateau (3 and 4mm activation). In these conditions, the force at beginning unloading. Distance of origin at register 50g force; 9) permanent deformation at zero force. The main conclusions were: maximum loading forces increase with deflection and temperature increases, and brand Morelli presented the smallest force and GAC the greatest; the decrease of forces with unloading was as larger as activation force; only the activation until 3 and 4mm presented superelasticity plateaus, and was longer with 4mm activation, but it presented lower force at plateaus; in all tests was noted permanent deformation

Orientador: Weber José da Silva Ursi / Banca: Robert Chaib Stegun / Banca: Carlos Alberto Adde / Banca: João Batista Macedo Becker / Banca: Lúcia Teramoto / Resumo: Analisaram-se separada e comparativamente três marcas comerciais de elásticos ortodônticos sintéticos e de molas de NiTi (MORELLI, ORMCO e GAC), quanto à degradação da força sofrida por estes materiais em função do tempo, quando submetidos a simulação das condições bucais. Os elásticos e molas foram inicialmente termociclados (temperaturas de 15°C e 45°C), em seguida estirados em 20mm, imersos em saliva artificial a 37°C e desativados em 0,5mm semanais. As leituras da quantidade de força gerada pelas amostras foram realizadas nos momentos: inicial, 1, 24, 48 horas, 7, 14, 21 e 28 dias. Observou-se significativa redução na quantidade de força gerada pelos elásticos na primeira hora de ativação, que variou de 49,5% a 53%, enquanto que para as molas a degradação foi signicativamente menor, com valores entre 4,2% e 18,1%. Ao término de 28 dias de testes, as amostras de elásticos sofreram redução média na quantidade de força gerada entre 82,7% e 91,2% (GAC-82,7%, ORMCO-86,0% e MORELLI- 91,2%) já as amostras de molas apresentaram degradação média de força entre 17,5% e 32,2% (MORELLI-17,5%, ORMCO-27,3% e GAC-32,2%). Concluiu-se que, em geral, os elásticos promoveram maior índice inicial de força que as molas, mas após as primeiras 24 horas de ativação a quantidade de força gerada pelos elásticos era menor que a promovida pelas molas, que assim apresentaram níveis médios de força mais constantes que os elásticos ao longo dos testes. / Abstract: Three commercial marks of synthetic elastics and NiTi coil springs (MORELLI, ORMCO, GAC) were separately and comparably analyzed, according to the force degradation generated by these materials, because of the time, when maintained stretched in artificial salivary, 37°C. The synthetic elastics and NiTi coil springs were thermal- cycled (15°C-45°C) and stretched in 20mm, and this stretch was reduced in 0,5mm weekly. The readings of the amount generated for elastics and coil springs were done in the intervals 0, 1, 24, 48h, 7, 14, 21 and 28 days. Where observed significative reduction on the amount of force generated for the elastics in the first hour of the activation (49,5%- 53%), and 82,7% - 91,2% in 28 days of the tests ( MORELLI - 91,2%, ORMCO - 86,0%, GAC - 82,7%);, while the generated force for NiTi coil springs suffered a reduction of 4,2%- 18,1%, in the first hour of the experimentation and 17,5% - 32,2% in 28 days of the stretch (MORELLI - 17,5%, ORMCO - 27,3%, GAC - 32,2%). We conclude that for most elastics delivered larger initial force that NiTi coil springs, but after 24 hours of activation the NiTi coil springs delivered larger force that the elastics and generated level of the force more constant that elastics. / Doutor

Les tubes à paroi mince en alliage à mémoire de forme Nickel-Titane (AMF NiTi) sont largement utilisés dans la fabrication de stents auto-expansibles. Leur fonctionnement repose sur la superélasticité (SE), comme de nombreuses autres applications des AMF NiTi dans le domaine biomédical. Le SE est un phénomène cristallographique réversible qui donne aux AMF la capacité de récupérer de grandes déformations par simple déchargement mécanique. En raison de la nature cristallographique du SE, les propriétés mécaniques liées à cet effet devraient être affectées par l'anisotropie inhérente du tube, qui émerge de son processus de fabrication. Cependant, le NiTi est encore souvent considéré comme isotrope dans la conception et l'optimisation de tels dispositifs. L'une des difficultés empêchant l'utilisation de modèles anisotropes est l'absence de caractérisations mécanique de l'anisotropie du tube NiTi. Le présent travail vise à effectuer une telle caractérisation pour un tube superélastique NiTi à paroi mince. Dans une campagne expérimentale, le comportement en traction du tube est analysé à différentes orientations et températures. La technique de corrélation d'image numérique (digital image correlation - DIC) est utilisée pour surveiller la distribution des déformations pendant les essais de traction. Les résultats montrent que toutes les propriétés analysées liées à la SE sont anisotropes. Toutes les dépendances d'orientation sont presque symétriques à 45° de l'axe du tube. Certaines propriétés dépendent également de la température, dépendance qui est également anisotrope. Une approche thermodynamique basée sur l'énergie libre de Gibbs est utilisée pour analyser ces dépendances d'orientation et de température. Avec cette analyse, il a été possible de relier l'hystérésis mécanique de la SE et les contributions irréversibles présentes dans le système. Enfin, l'influence de l'anisotropie sur la distribution des déformations est vérifiée. L'accent est mis sur l'analyse du phénomène de localisation de la déformation tout au long du chargement et du déchargement. L'inclinaison de la bande de localisation est caractérisée et évaluée avec une approche de plasticité. L'angle de la bande avant observé avec DIC est prédit en utilisant des données de vitesse de déformation globale. / Thin walled tubes of Nickel-Titanium shape memory alloys (NiTi SMA) are widely used in the fabrication of self-expandable stents. The operation of stents relies on the superelastic effect (SE), as many other applications of NiTi SMA in the biomedical field. The SE is a reversible crystallographic phenomenon that gives SMA the ability to recover large strains through simple unload. Due to the crystallographic nature of the SE, the mechanical properties related to this effect are expected to be affected by the inherent anisotropy of the tube, which emerges from its fabrication process. However, NiTi is still often treated as isotropic in the design and optimization of such devices. One of the difficulties preventing the use of anisotropic models is a lack of mechanical characterizations about the NiTi tube's anisotropy. The present work aims to perform such characterization for a thin walled NiTi superelastic tube. In an experimental campaign, the tensile behaviour of the tube is analysed at different orientations and temperatures. Digital Image Correlation (DIC) technique is used to monitor the strain distribution during tensile tests. Results show that all the analysed properties related with SE are anisotropic. All the orientation dependencies are nearly symmetrical to 45° from the tube's axis. Some properties are also dependent on temperature, a dependence that is also anisotropic. A thermodynamic approach based on the Gibbs free energy is used to analyse these orientation and temperature dependencies. With this analysis it was possible to relate the SE stress hysteresis and thermodynamic irreversible energy contributions. Finally, the influence of anisotropy on the strain distribution of tensile samples is verified. Focus is given to the analysis of the strain localization phenomenon throughout loading and unloading. The inclination of the localization front band is characterized and evaluated with a plasticity approach. The front angle observed with DIC is predicted using global strain rate data.

Inquestionavelmente, inovações ocorridas nos últimos anos no preparo do canal radicular revolucionaram o tratamento endodôntico. Dentre elas, destaca-se o tratamento térmico recristalizador da liga de níquel-titânio na confecção de limas endodônticas, o qual aumentou de sobremaneira sua flexibilidade e as capacidades de flexibilidade, torção e resistência à fadiga cíclica flexural quando comparadas às limas de níquel-titânio convencionais fabricadas até então. O presente estudo teve como objetivo avaliar a resistência à fadiga cíclica flexural dos instrumentos de níquel-titânio tratados termicamente Reciproc Blue R25 (VDW) e WaveOne Gold Primary (Dentsply-Maillefer) em um dispositivo desenvolvido especificamente para realizar ensaios flexurais dinâmicos. As limas selecionadas possuíam conicidade 0,08 mm e 0,07 mm respectivamente, com diâmetros de ponta 0,25 mm e foram utilizadas no motor elétrico VDW Silver Reciproc (VDW) em movimento reciprocante específico de cada sistema. Os instrumentos foram divididos em 2 grupos de 15 limas e testados em canais de aço simulados com o ângulo de 60º e raio de curvatura de 5mm. O número de ciclos e o tempo em segundos até a ocorrência de fratura dos instrumentos foram registrados e estatisticamente avaliados. As limas Reciproc Blue R25 apresentaram desempenho significativamente melhor (P<0,05), por meio do maior número de ciclos e de tempo até a fratura quando comparadas com as limas WaveOne Gold. Assim, conclui-se que o sistema Reciproc Blue R25 foi mais seguro quanto à resistência à fadiga flexural no ensaio realizado quando comparado ao sistema WaveOne Gold Primary em movimento reciprocante. / Innovations that have occurred in recent years in the preparation of the root canal have revolutionized endodontic treatment. Among them, the heat treatment of the nickel-titanium alloy in the manufacture of endodontic files, which greatly increased the flexibility, torsional and flexural fatigue resistance capacities when compared to the conventional nickel-titanium files manufactured until then. The present study aimed to evaluate the resistance to flexural cyclic fatigue of thermally treated Reciproc Blue R25 (VDW) and WaveOne Gold Primary (Dentsply-Maillefer) instruments in a device specifically developed to perform dynamic flexural tests. The selected files had taper 0.08 mm and 0.07 mm respectively, with tip diameters of 0.25 mm and were used in the reciprocating movement of each system in the VDW Silver Reciproc (VDW) electric motor. The instruments were divided into 2 groups of 15 files and tested in simulated steel channels with angle of 60º and radius of curvature of 5mm. The number of cycles and the time in seconds until the occurrence of fracture of the instruments were recorded and statistically evaluated. The Reciproc Blue R25 files presented significantly better performance (p <0.05), by the higher number of cycles and time to fracture when compared to WaveOne Gold files. Thus, it was concluded that the Reciproc Blue R25 system was safer than the WaveOne Gold Primary reciprocating system in terms of resistence of flexural fatigue