No preparo dos canais radiculares, eminentemente os curvos, a abordagem cérvico-apical amplamente difundida promovendo a dilatação da região cervical do canal radicular previamente à atuação de instrumentos em sua região apical constitui técnica e inegavelmente uma forma adequada, tanto do ponto de vista mecânico como microbiológico, de interagir com o espaço endodôntico em busca de uma experiência bem sucedida e previsível. De outra forma, os mais recentes instrumentos endodônticos, muito mais flexíveis em decorrência das novas ligas de baixo módulo de elasticidade empregadas em sua fabricação e dotados de novos índices de conicidade, surgem melhorando tais perspectivas. Desde o surgimento da liga de Níquel-Titânio na Endodontia, na década de oitenta, uma gama imensa de instrumentos desta derivados e para serem empregados com dispositivos mecânicos, eletromecânicos ou pneumocânicos, têm reavivado a esperança de se obter um dispositivo ideal que simulando a cinemática manual supere as limitações operacionais decorrentes, principalmente, da configuração anatômica do canal radicular. Assim, neste experimento verificou-se o desempenho de quatro diferentes recursos técnicos no desgaste da região cervical do canal radicular. Constituíram-se quatro amostras, cada qual composta de 10 espécimes (raízes mésio-vestibulares de primeiros molares superiores), para serem preparadas com (i) Brocas Gates-Glidden, (ii) Brocas Largo-Peeso, (iii) ProFile® .04/.06 & Orifice Shapers e (iv) Pow-R Coronal Shapers. Imagens digitais obtidas antes e após o preparo do canal radicular foram analisadas também digitalmente estudo morfométrico computadorizado avaliando-se a variação das áreas das mesmas em função do desgaste promovido pelos referidos instrumentos. Todos os instrumentos produziram desgaste de ambas as paredes, mesial e distal, do canal radicular na região analisada. A análise estatística das variações de área para o fator parede mesial não mostrou diferenças estatisticamente significantes entre os grupos experimentais para =5%. No entanto quando da comparação dos grupos experimentais para o fator parede distal verificou-se diferenças estatisticamente significantes entre os grupos #1 e #3 para =5%. Ainda, para o fator área total (paredes mesial e distal) verificou-se diferenças estatisticamente signifcantes entre os grupos #3 e #4 para =5%. Concluiu-se que todos os instrumentos testados produzem desgaste tanto da parede mesial como da parede distal do canal radicular e, conseqüentemente, da estrutura dentinária global da região cervical do canal radicular. Por outro lado verificou-se uma tendência da Broca Gates-Glidden em promover maior desgaste da parede distal que o Sistema ProFile® .04/.06 & Orifice Shapers e do Sistema Pow-R Coronal Shapers em promover maior desgaste da estrutura toal que o Sistema ProFile® .04/.06 & Orifice Shapers. / Nowadays is common sense among endodontists that in root canal preparation, mainly the curved ones, the crown-down approach enlarging the cervical third prior instrumentation of the apical third regions provides better interaction between the instrument and the canal walls than the conventional methods. Technically it provides an adequate form to achieve the best and predictable results in cleaning and shaping the root canal system. Additionally the most recent nickel-titanium made endodontic instruments more flexible than the stainless steel instruments and the new taper design have been appeared to improve the endodontic panorama. Since the introduction of the nickel-titanium alloy in Endodontics by Walia et al. in 1988 a number of instruments produced by such alloy in conjunction with the engines new generation have brought new perspectives to deal tridimensionally with the still challenger endodontic space. In this study the performance of four different instruments in the root canal cervical third enlargement was evaluated. Four experimental groups comprised by ten upper molars mesiobuccal roots each were prepared by either (i) Gates bur, (ii) Largo bur, (iii) Profile® .04/.06 & Orifice Shapers or (iv) Pow-R Coronal Shapers. Before and after preparation digitally acquired images were evaluated for area changes within both mesial and distal root canal walls. All instruments produced some amount of wear in both walls and the distals have changed more than the mesials in most times probably due an excentric performance of all evaluated instruments. Comparison of root canal walls wearing among the four experimental groups showed no statistically significant differences (=5%) for mesial wall. However, statistically analyze (=5%) showed significant differences between Experimental Group #1 (Gates-Glidden burs) and Experimental Group #3 (Profile® .04/.06 & Orifice Shapers) for distal walls with the first showing greater wearing than the latter. Also, the results showed statistically significant differences between Experimental Group #4 (Pow-R & Coronal Shapers) and Experimental Group #3 (Profile® & Orifice Shapers) for the entire structure i.e. mesial and distal walls with the first showing the greater than the latter wearing . It was concluded that all tested instruments wear so the mesial as the distal root canal walls. Experimental results have showed that in first upper molaras mesiobuccal roots Gates-Glidden bur for distals and Pow-R nickel-titanium instruments for both walls, i.e. the cervical dentin entire structure, are supposed to wear more root canal cervical third dentin than the others instruments which they were compared.

O objetivo do presente estudo foi avaliar a resistência à fadiga cíclica flexural de instrumentos rotatórios de níquel-titânio de número 25, conicidade 0,04 e 25 mm de comprimento (K3, SybronEndo), submetidos a variados torques de acionamento e repetidos ciclos de usos em canais simulados, valendo-se de dispositivo apropriado para ensaios dinâmicos. Procurou-se determinar se, além do fator de variação número de uso, há influência relacionada com o torque e, ainda, a possibilidade de interação entre número de uso e torque. Valendo-se motor elétrico acionado à velocidade de 300 rpm foram instrumentados 320 canais simulados, utilizado-se 80 instrumentos divididos em 4 grupos com 20 espécimes cada, de acordo com os torques (0,5 Ncm, 1,0 Ncm, 2,0 Ncm e 6,0 Ncm) a que seriam submetidos. Cada grupo foi subdividido em 4 subgrupos com 5 espécimes, de acordo com o número de usos (1, 3, 5 e 7 ciclos de usos). Todos os instrumentos foram submetidos a ensaio de fadiga cíclica flexural que foi realizado num dispositivo que permitia ao instrumento girar livremente, reproduzindo a instrumentação rotatória num canal curvo (40º e raio de curvatura de 5 mm), simulando o movimento de pecking, onde o instrumento deslizava pelo sulco criado no anel de aço temperado. Foi utilizada peça de mão com contra-ângulo redutor de 16:1, acionado por motor elétrico na velocidade de 300 rpm e torque idêntico ao empregado durante a fase de preparo dos canais simulados. A fratura do instrumento era facilmente detectada pelo sensor, e neste momento o contador e o temporizador paravam imediatamente. Os dados registrados no contador e no temporizador foram tranformados em segundos. Para a avaliação estatística empregou-se ANOVA e o teste t de Student (p<0,01). No que diz respeito ao fator de variação número de uso, não houve diferença estatística significante, enquanto as comparações feitas com o torque de 6,0 Ncm apresentaram valores de t calculado altamente significativo, com p < 0,01. Também não ocorreu interação significante entre os fatores de variação número de usos e torque. Baseado nos resultados deste estudo pode-se concluir que o torque afetou a resistência à fadiga cíclica flexural dos instrumentos rotatórios de NiTi, sendo menor naqueles submetidos à torque elevado, enquanto o número de usos em até 7 vezes não afetou . / The aim of the present study was to evaluate the flexural cyclic fatigue resistance of nickel-titanium rotary instruments, number 25, taper 0,04, and length of 25mm (K3, SybronEndo), when submitted to several torque values and number of uses in simulated canal blocks, by using devices appropriated for dynamic tests. It was tried to detect whether, in addition to the factor number of uses, there would be an influence related to torque, or even the possibility of an interaction between number of uses and torque. The data was collected from 320 simulated canals that were prepared, driven by an electrical motor at 300 rpm, using 80 instruments divided in 4 groups of 20 sample each, based on torque values (0,5 Ncm, 1,0 Ncm, 2,0 Ncm e 6,0 Ncm). Each group was randomly divided in 4 subgroups of 5 samples each, according to the number of uses (1, 3, 5 and 7 cycles). All files were submitted to flexural cyclic fatigue test realized in a device that allows the instrument to freely rotate, reproducing the movement of an instrument rotating in a curved canal (40º angle and 5 mm of radius), simulating the pecking movement, where the instrument slide over the groove created in the hardened steel. An electric motor hand-piece was used with a contra-angle 16:1 reduction set at 300 rpm and torque value identical to that used during preparation of simulated canals. The fracture of the instrument was easily detected at moment which the counter and the timer were immediately stopped. Data collected by the counter and the timer were converted in seconds and analysed by ANOVA and t Student test (p<0.01). In regards to the number of uses factor, there was not a statistically significant difference, while comparisons made with torque value set at 6,0 Ncm showed t values significantly high, with p<0.01. It was not seen any interaction between both variables, number of uses and torque. Based on the results of this investigation, it can be concluded that torque affected the resistance to flexural cyclic fatigue of nickel-titanium rotary instruments, being low on those tested at high torque value; while the factor number of uses up to 7 times did not affect the results.

O presente estudo teve por objetivo avaliar ex vivo a eficiência de sistemas para retratamento (ProTaper Universal Retratamento, Mtwo Retratamento e D-Race), na desobturação de canais mésio vestibulares curvos de molares superiores, por meio de tomografia computadorizada por feixe cônico. Foram utilizados canais mésio vestibulares com curvatura entre 20° e 40°, de 36 molares superiores, preparados com Protaper Universal (até instrumento F2), obturados com cone ProTaper F2 e cimento AH Plus, pela técnica de condensação lateral. Para a desobturação, os dentes foram divididos em grupos (I: ProTaper Universal Retratamento, II: Mtwo Retratamento e III: D-Race). A captura das imagens foi realizada após a obturação e após a desobturação dos canais radiculares, por meio de tomografia computadorizada por feixe cônico de pequeno volume (Prexion 3D XTrillion Inc). As imagens foram segmentadas utilizando o programa InVesalius, para verificar o material obturador remanescente. O tempo para desobturação também foi analisado. De posse dos valores, iniciais e finais, de volume de material obturador e de estrutura dentinária, a proporção dos volumes foi calculada. Para a análise estatística, os resultados foram avaliados pelos testes de ANOVA e de Múltiplas Comparações de Bonferroni. Os grupos ProTaper Universal Retratamento (13,97%) e D-Race (9,87%), apresentaram os menores volumes percentuais médios de material obturador remanescente, não havendo diferença estatística significante entre eles; porém, apresentaram diferença estatística significante (p 0,05) do grupo Mtwo Retratamento (33,88%). Os três sistemas provocaram desgaste semelhante de dentina após a desobturação. O grupo D-Race apresentou menor tempo para desobturação, estatisticamente diferente em relação aos demais sistemas. As características dos sistemas de retratamento podem interferir na eficiência de desobturação quanto ao tempo e volume de material remanescente. / The present study aimed to evaluate, ex vivo, the efficiency of systems for retreatment (ProTaper Universal Retreatment, Mtwo Retreatment and D-Race), in removal filling material of curved mesiobuccal canals of maxillary molars, using cone beam computed tomography. Were used mesiobuccal canals with curvature between 20 ° and 40 °, of 36 molars prepared with ProTaper Universal (until instrument F2), filled with cone F2 ProTaper and AH Plus sealer by lateral condensation. For the removal procedure of filling material, the teeth were divided into groups (I: Protaper Universal Retreatment, II: Mtwo Retreatment and III: D-Race). The capture of images was performed after filling and after the removal procedure of root canal through cone beam computed tomography of small volume (Prexion 3D - XTrillion Inc). The images were segmented using the software InVesalius to check the remaining filling material. The time for removal procedure was also analyzed. Possession of values, initial and final, of volume filling material and dentin structure, the ratio of the volumes was calculated. For statistical analysis, the results were evaluated by ANOVA and Bonferroni\'s Multiple Comparisons. ProTaper Universal Retreatment (13.97 %) and D-Race (9.87 %) groups had the lowest average percent volume remaining filling material, with no statistically significant difference between them, but showed a statistically significant difference (p 0.05) group Mtwo Retreatment (33.88 %). The three systems caused similar wear dentin after removal procedure. The group D-Race had less time for removal procedure, statistically different compared to the other systems. The characteristics of retreatment systems may interfere with the efficiency of removal procedure on the time and volume remaining material.

O preparo químico-cirúrgico é uma das etapas mais importantes do tratamento endodôntico, pois promove a desinfecção do sistema de canais radiculares através da limpeza e da modelagem. Realizar o preparo de canais curvos é um grande desafio, devido à ocorrência freqüente de acidentes operatórios como o transporte do canal. A introdução de instrumentos fabricados em ligas de níquel-titânio (NiTi) contribuiu consideravelmente para a melhora na qualidade da instrumentação dos canais. Os diferentes sistemas rotatórios que são apresentados continuamente ao profissional devem ser estudados com detalhes, pois o seu comportamento pode variar de acordo com o desenho de cada instrumento e as suas características de produção. O objetivo deste estudo foi avaliar, ex vivo, a qualidade do preparo de canais curvos realizado pelos sistemas rotatórios Twisted File (TF; Sybron Endo), torcidos, e EndoSequence (ES; Brasseler), usinados, quanto à habilidade em manter o canal centralizado, analisando a extensão e a direção dos eventuais transportes e o índice de centralização do instrumento (IC), por meio de cortes transversais e da microtomografia computadorizada (CT). Trinta molares inferiores foram divididos em dois grupos, e preparados conforme o delineamento de cada método: G1 - Bramante Modificado e G2 - CT. No G1, os dentes foram incluídos em blocos de resina, e seccionados a 2,0, 3,5 e 5,0 mm do ápice radicular. As secções foram fotografadas, e os blocos, remontados, foram submetidos à instrumentação rotatória. No G2, os dentes foram incluídos em material de moldagem e escaneados com um microtomógrafo, antes e após o preparo. As imagens das seções transversais foram reconstruídas e os cortes axiais correspondentes às distâncias de 2,0, 3,5 e 5,0 mm do ápice radicular foram selecionados. Os resultados foram submetidos ao teste estatístico não-paramétrico Mann-Whitney, para comparações duas a duas. Em ambos os grupos, o transporte do canal e o IC para os sistemas TF e ES foram semelhantes, havendo diferença estatística significante apenas no G2, na secção 3,5 mm, quando o sistema TF causou menos transporte do que o sistema ES, obtendo também um melhor IC (p < 0,05). Quando realizada a comparação entre os métodos, independentemente do instrumento utilizado, o transporte do canal foi significantemente menor (0,17 mm) no grupo 2, do que no grupo 1 (0,27 mm) (p < 0,05). A 3,5 e 5,0 mm, o sistema TF promoveu menos transporte no grupo 2 do que no grupo 1 (p < 0,05). Para o sistema ES, diferença estatística foi encontrada a 2,0 mm, aonde o transporte também foi menor no grupo 2 (p < 0,05). Concluiu-se que os sistemas TF e ES se comportaram de modo semelhante quanto ao transporte do canal e ao IC, permitindo o preparo de canais curvos com pouco desvio. Os dois instrumentos apresentaram desvios tanto para o sentido mesial, quanto para o sentido distal. E quando comparados apenas os métodos de avaliação, no método da CT o transporte do canal foi menor do que no método de Bramante Modificado. / The chemomechanical preparation is one of the most important phases of endodontic treatment, because it promotes disinfection of the root canal system by cleaning and shaping. The preparation of curved canals is a major challenge due to the frequent occurrence of operative accidents as the canal transportation. The introduction of instruments of nickel-titanium (NiTi) alloy has contributed considerably to the improvement of canal instrumentation quality. The different rotary systems that are continuously presented to dental professionals should be studied in detail, because their mechanical properties can vary according to the design of each instrument and the manufacture characteristics. The aim of this study was to evaluate, ex vivo, the quality of preparation of curved canals and centering ability of the rotary systems Twisted File (TF) (Sybron Endo), twisted, and EndoSequence (ES) (Brasseler), ground, analyzing the extent and direction of any transportation and the centering ratio of instrument, by cross sections and microcomputed tomography (CT). Thirty lower molars were divided into two groups, and prepared according to the design of each method: G1 Bramante Modified and G2 - CT. In G1, the teeth were embedded in resin blocks and sectioned at 2,0, 3,5 and 5,0 mm from the apex. The sections were photographed and the blocks were reassembled and subjected to rotary instrumentation. In G2, the teeth were embedded in an impression material and scanned with a microtomograph, before and after preparation. The images were reconstructed from the cross sections and the axial sections corresponding to distances of 2,0, 3,5 and 5,0 mm from the apex were selected. The results were submitted to statistical nonparametric test Mann-Whitney. In both groups, the canal transportation and IC for TF and ES systems were similar, with statistical difference only for the 3.5 mm section, while TF system caused less canal transportation than ES system, obtaining also better IC (p <0.05). When compared only the methods, regardless of instrument used, the canal transportation was significantly smaller (0.17 mm) in group 2 than in group 1 (0.27 mm) (p <0.05). At 3.5 and 5.0 mm, TF system promoted less transportation in group 2 than in group 1 (p <0.05). For ES system, statistical difference was found at 2.0 mm, where transportation was also lower in group 2 (p <0.05). It was concluded that the systems TF and ES behaved similarly about the canal transportation and the centering ability, allowing the preparation of curved canals with little deviation. The two instruments showed deviations for both the mesial and distal direction. When comparing only the methods of assessment, at CT the canal transportation was lower than in Bramante Modified method.

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

NiTi-based shape memory alloys (SMAs) offer a good combination of high-strength, ductility, corrosion resistance, and biocompatibility that has served them well and attracted the attention of many researchers and industries. The alloys unique thermo-mechanical ability to recover their initial shape after relatively large deformations by heating or upon unloading due to a characteristic reversible phase transformation makes them useful as damping devices, solid state actuators, couplings, etc. However, there is a need to increase the temperature of the characteristic phase transformation above 150 °C, especially in the aerospace industry where high temperatures are often seen. Prior researchers have shown that adding ternary elements (Pt, Pd, Au, Hf and Zr) to NiTi can increase transformation temperatures but most of these additions are extremely expensive, creating a need to produce cost-effective high temperature shape memory alloys (HTSMAs). Thus, the main objective of this research is to examine the relatively unstudied NiTiZr system for the ability to produce a cost effective and formable HTSMA. Transformation temperatures, precipitation paths, processability, and high-temperature oxidation are examined, specifically using high energy X-ray Diffraction (XRD) measurements, in NiTi-20 at.% Zr. This is followed by an in situ XRD study of the phase growth kinetics of the favorable H-phase nano precipitates, formed in NiTiHf and NiTiZr HTSMAs, based on prior thermo-mechanical processing in a commercial NiTi-15 at.% Hf HTSMA to examine the final processing methods and aging characteristics. Through this research, knowledge of the precipitation paths in NiTiZr and NiTiHf HTSMAs is extended and methods for characterization of phases and strains using high energy XRD are elucidated for future work in the field.

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.

Shape memory alloys (SMAs) are a new generation material which exhibits unique nonlinear deformations due to a phase transformation which allows it to return to its original shape after removal of stress or a change in temperature. It shows a shape memory effect (martensitic condition) and pseudoelasticity (austenitic condition) properties depends on various heat treatment conditions. The reason for these properties depends on phase transformation through temperature changes or applied stress. Many technological applications of austenite SMAs involve cyclical mechanical loading and unloading in order to take advantage of pseudoelasticity, but are limited due to poor fatigue life. In this thesis, I investigated two important mechanical feature to fatigue behavior in pseudoelastic NiTi SMA wires using high energy synchrotron radiation X-ray diffraction (SR-XRD). The first of these involved simple bending and the second of these involved relaxation during compression loading. Differential scanning calorimetry (DSC) was performed to identify the phase transformation temperatures. Scanning electron microscopy (SEM) images were collected for the initial condition of the NiTi SMA wires and during simple bending, SEM revealed that micro-cracks in compression regions of the wire propagate with increasing bend angle, while tensile regions tend to not exhibit crack propagation. SR-XRD patterns were analyzed to study the phase transformation and investigate micromechanical properties. By observing the various diffraction peaks such as the austenite (200) and the martensite (100), (110), and (101) planes, intensities and residual strain values exhibit strong anisotropy depending upon whether the sample is in compression or tension during simple bending. This research provides insight into two specific mechanical features in pseudoelastic NiTi SMA wires.

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