Caracterização do comportamento à fadiga de instrumentos de Ni-Ti para aplicações de endodontia

Dissertação para obtenção do Grau de Mestre em Engenharia Mecânica

Tratamentos termomecânicos de ligas do sistema Ni-Ti

As ligas de Níquel‑Titânio (Ni‑Ti) são as mais atractivas entre as ligas com memória de forma devido às suas boas propriedades funcionais juntamente com a elevada resistência e melhor ductilidade. As transformações de fases associadas ao efeito de memória de forma (EMF) podem ser em uma etapa, B19’ (martensite) ↔ B2 (austenite), em duas ou em múltiplas etapas, incluindo a fase‑R intermédia dependendo da história térmica e termomecânica da liga. As temperaturas de transformação são geralmente observadas acima da temperatura ambiente para as ligas ricas em Ti, enquanto nas ricas em Ni se situam abaixo da temperatura ambiente. O objectivo da presente dissertação foi o de investigar as modificações nas propriedades funcionais e estruturais em uma liga de Ni‑Ti rica em Ti (49,0%at.Ni‑51,0%at.Ti) sujeita a diferentes tratamentos térmicos e termomecânicos de marforming e ausforming. Para melhor entender os fenómenos presentes nesta liga foi feito um paralelismo com outras duas ligas de Ni‑Ti: (i) equiatómica com EMF acima da temperatura ambiente e (ii) rica em Ni superelástica (SE) à temperatura ambiente. Com o intuito de uma análise completa das transformações de fases foram utilizadas durante ciclos térmicos diversas técnicas de caracterização: Calorimetria Diferencial de Varrimento (DSC), Resistividade Eléctrica (RE), Dilatometria (DT) e Difracção de Raios‑X (DRX) convencional e por radiação sincrotrão – rotina e textura. Foram também utilizadas outras técnicas à temperatura ambiente com o intuito de observar características microestruturais (Microscopia Óptica (MO) e Electrónica de Varrimento (SEM)) e mecânicas (Microdureza e Ultra‑Microdureza Vickers, e Tracção). A liga de Ni‑Ti rica em Ti tem as suas transformações directa e inversa fortemente afectadas pelos tratamentos termomecânicos, devido à formação de fase‑R durante a transformação directa em duas (B2®R®B19’) ou em múltiplas etapas (B2®R, B2®B19’ e R®B19’). Os tratamentos termomecânicos conducentes à sequência de transformação B2®R®B19’ decrescem a temperatura de fim da formação de B19’ para próximo da temperatura ambiente e apresentam maior estabilidade nas temperaturas e histereses de transformação.

In-situ X-ray diffraction studies during growth of Ni-Ti shape memory alloy films and their complementary ex-situ characterization

Shape Memory Alloy (SMA) Ni-Ti films have attracted much interest as functional and smart materials due to their unique properties. However, there are still important issues unresolved like formation of film texture and its control as well as substrate effects. Thus, the main challenge is not only the control of the microstructure, including stoichiometry and precipitates, but also the identification and control of the preferential orientation since it is a crucial factor in determining the shape memory behaviour. The aim of this PhD thesis is to study the optimisation of the deposition conditions of films of Ni-Ti in order to obtain the material fully crystallized at the end of the deposition, and to establish a clear relationship between the substrates and texture development. In order to achieve this objective, a two-magnetron sputter deposition chamber has been used allowing to heat and to apply a bias voltage to the substrate. It can be mounted into the six-circle diffractometer of the Rossendorf Beamline (ROBL) at the European Synchrotron Radiation Facility (ESRF), Grenoble, France, enabling an in-situ characterization by X-ray diffraction(XRD) of the films during their growth and annealing. The in-situ studies enable us to identify the different steps of the structural evolution during deposition with a set of parameters as well as to evaluate the effect of changing parameters on the structural characteristics of the deposited film. Besides the in-situ studies, other complementary ex-situ characterization techniques such as XRD at a laboratory source, Rutherford backscattering spectroscopy(RBS), Auger electron spectroscopy (AES), cross-sectional transmission electron microscopy (X-TEM), scanning electron microscopy (SEM), and electrical resistivity (ER) measurements during temperature cycling have been used for a fine structural characterization. In this study, mainly naturally and thermally oxidized Si(100) substrates, TiN buffer layers with different thicknesses (i.e. the TiN topmost layer crystallographic orientation is thickness dependent) and MgO(100) single crystals were used as substrates. The chosen experimental procedure led to a controlled composition and preferential orientation of the films. The type of substrate plays an important role for the texture of the sputtered Ni-Ti films and according to the ER results, the distinct crystallographic orientations of the Ni-Ti films influence their phase transformation characteristics.

The Effect of Residence Time on the Tensile Properties of Superelastic and Thermal Activated Ni-Ti Orthodontic Wires

Since the 1980s, different devices based on superelastic alloys have been developed to fulfill orthodontic applications. Particularly in the last decades several researches have been carried out to evaluate the mechanical behavior of Ni-Ti alloys, including their tensile, torsion and fatigue properties. However, studies regarding the dependence of elastic properties on residence time of Ni-Ti wires in the oral cavity are scarce. Such approach is essential since metallic alloys are submitted to mechanical stresses during orthodontic treatment as well as pH and temperature fluctuations. The goal of the present contribution is to provide elastic stress-strain results to guide the orthodontic choice between martensitic thermal activated and austenitic superelastic Ni-Ti alloys. From the point of view of an orthodontist, the selection of appropriate materials and the correct maintenance of the orthodontic apparatus are essential needs during clinical treatment. The present work evaluated the elastic behavior of Ni-Ti alloy wires with diameters varying from 0.014 to 0.020 inches, submitted to hysteresis tensile tests with 8% strain. Tensile tests were performed after periods of use of 1, 2 and 3 months in the oral cavity of patients submitted to orthodontic treatment. The results from the hysteresis tests allowed to exam the strain range covered by isostress lines upon loading and unloading, as well as the residual strain after unloading for both superelastic and thermal activated Ni-Ti wires. Superelastic Ni-Ti wires exhibited higher load isostress values compared to thermal activated wires. It was found that such differences in the load isostress values can increase with increasing residence time.

Preparation of Ni-Ti-Mo and Ni-Ti-Mo-Zr Alloys by High-Energy Ball Milling and Subsequent Hot Pressing

This work discusses on the preparation of Ni-45Ti-5Mo, Ni-40Ti-10Mo and Ni-46Ti-2Mo-2Zr (at-%) alloys by high-energy ball milling and hot pressing, which are potentially attractive for dental and medical applications. The milling process was performed in stainless steel balls (19mm diameter) and vials (225 mL) using a rotary speed of 300rpm and a ball-to-powder weight ratio of 10:1. Hot pressing under vacuum was performed in a BN-coated graphite crucible at 900 degrees C for 1 h using a load of 20 MPa. The milled and hot-pressed materials were characterized by X-ray diffraction, electron scanning microscopy, and electron dispersive spectrometry. Peaks of B2-NiTi and Ni4Ti3 were identified in XRD patterns of Ni-45Ti-5Mo, Ni-40Ti-10Mo and Ni-46Ti-2Mo-2Zr powders milled for 1h. The NiTi compound dissolved small Mo amounts lower than 4 at%, which were measured by EDS analysis. Moreover, it was identified the existence of an unknown Mo-rich phase in microstructures of the hot-pressed Ni-Ti-Mo alloys.

Caracterização das ligas Ni-Ti-Mo, Ni-Ti-Ta e Ni-Ti-Mo-Zr obtidas por moagem de alta energia e prensagem a quente

Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)

Comparação da razão carga/deflexão entre fios ortodônticos de Ni-Ti termoativados 0,014”x0,025” e 0,016”x0,022”

The knowledge of the mechanical properties of nickel-titanium (NiTi) termoactives of the more accessible of the domestic market is still limited. Given this, the objective of this study was to evaluate and compare through deflection tests in brackets NiTi wires 03 term rectangular gauge 0.014 '' enabled x 0.025 '' and 0.016 '' x 0.022 '' of different brands (MORELLI (R), ORMCO (R) ORTHOSOURCE (R), ORTHOMETRIC (R), EURODONTO (R) and ADITEK (R)). All tests were carried out on universal testing machine EMIC DL 2000 under identical conditions and controlled at a temperature of 36 degrees C +/- 0.5 degrees C. Five measurements (N= 5) were performed for each thickness/wire tag that was deflected up to a limit of 4.0mm at a speed of 1.0mm/min. Each 0.2mm (round trip) of corresponding strength measured deflection for the construction of the graph of force x deflection at Tesc program version 3.04. Each graphic was evaluated according to the following variables: beginning of the Martensitic transformation (cN and mm), maximum strength (cN), the beginning and end of the plateau of deactivation (cN and mm) and length (mm) plateau. The average and standard deviation were calculated for all variables and statistical analysis was made by ANOVA tests 2 criteria and Turkey or Kruskal-Wallis and Dunn, a 5% level of significance. The results showed that the tests of 0.014 '' x0.025 '' ORTHOMETRIC (R) brands and ORMCO (R) showed the best results, as well as the wires of the MORELLI (R) and ORTHOSOURCE (R) to wires 0.016 '' x0.022 ''. In General, the gauge wires 0.014 '' x0.025 '' showed strength levels on the plateau of deactivation to 6 x smaller than 0.016 '' x0.022 '' caliber.

The Effect of Residence Time on the Tensile Properties of Superelastic and Thermal Activated Ni-Ti Orthodontic Wires

Since the 1980s, different devices based on superelastic alloys have been developed to fulfill orthodontic applications. Particularly in the last decades several researches have been carried out to evaluate the mechanical behavior of Ni-Ti alloys, including their tensile, torsion and fatigue properties. However, studies regarding the dependence of elastic properties on residence time of Ni-Ti wires in the oral cavity are scarce. Such approach is essential since metallic alloys are submitted to mechanical stresses during orthodontic treatment as well as pH and temperature fluctuations. The goal of the present contribution is to provide elastic stress-strain results to guide the orthodontic choice between martensitic thermal activated and austenitic superelastic Ni-Ti alloys. From the point of view of an orthodontist, the selection of appropriate materials and the correct maintenance of the orthodontic apparatus are essential needs during clinical treatment. The present work evaluated the elastic behavior of Ni-Ti alloy wires with diameters varying from 0.014 to 0.020 inches, submitted to hysteresis tensile tests with 8% strain. Tensile tests were performed after periods of use of 1, 2 and 3 months in the oral cavity of patients submitted to orthodontic treatment. The results from the hysteresis tests allowed to exam the strain range covered by isostress lines upon loading and unloading, as well as the residual strain after unloading for both superelastic and thermal activated Ni-Ti wires. Superelastic Ni-Ti wires exhibited higher load isostress values compared to thermal activated wires. It was found that such differences in the load isostress values can increase with increasing residence time.

The Effect of Residence Time on the Tensile Properties of Superelastic and Thermal Activated Ni-Ti Orthodontic Wires

Since the 1980s, different devices based on superelastic alloys have been developed to fulfill orthodontic applications. Particularly in the last decades several researches have been carried out to evaluate the mechanical behavior of Ni-Ti alloys, including their tensile, torsion and fatigue properties. However, studies regarding the dependence of elastic properties on residence time of Ni-Ti wires in the oral cavity are scarce. Such approach is essential since metallic alloys are submitted to mechanical stresses during orthodontic treatment as well as pH and temperature fluctuations. The goal of the present contribution is to provide elastic stress-strain results to guide the orthodontic choice between martensitic thermal activated and austenitic superelastic Ni-Ti alloys. From the point of view of an orthodontist, the selection of appropriate materials and the correct maintenance of the orthodontic apparatus are essential needs during clinical treatment. The present work evaluated the elastic behavior of Ni-Ti alloy wires with diameters varying from 0.014 to 0.020 inches, submitted to hysteresis tensile tests with 8% strain. Tensile tests were performed after periods of use of 1, 2 and 3 months in the oral cavity of patients submitted to orthodontic treatment. The results from the hysteresis tests allowed to exam the strain range covered by isostress lines upon loading and unloading, as well as the residual strain after unloading for both superelastic and thermal activated Ni-Ti wires. Superelastic Ni-Ti wires exhibited higher load isostress values compared to thermal activated wires. It was found that such differences in the load isostress values can increase with increasing residence time.

Avaliação da vida à fadiga de instrumentos endodônticos submetidos a movimento reciprocante

Dissertação para obtenção do Grau de Mestre em Engenharia Mecânica

Avaliação da resistência à fadiga de instrumentos endodônticos sujeitos a polimento electrolítico e a tratamento térmico específico

Esta dissertação teve como principais objectivos determinar a resistência à fadiga de instrumentos endodônticos de Níquel-Titânio sujeitos a polimento electrolítico e tratamento térmicopor autoclave, assim como estudar o comportamento estrutural dos instrumentos, através de análise numérica pelo método dos elementos finitos, quando sujeitos à curvatura em três regiões distintas. Vinte e dois instrumentos Hyflex (Coltene, Switzerland), com dois tamanhos diferentes (.04/20 e .06/20), foram divididos em 3 grupos: Grupo I, 4 instrumentos (dois de cada tamanho) sem qualquer tipo de tratamento térmico ou superficial; Grupo II, 12 instrumentos (seis de cada tamanho) submetidos a polimento electrolítico; Grupo III, 6 instrumentos (três de cada tamanho) submetidos a polimento electrolítico e tratamento térmico por autoclave. Todos os instrumentos foram sujeitos a testes de fadiga por flexão rotativa. Os instrumentos foram polidos, aplicando uma potência de 30 V, durante 3 segundos, a uma taxa de escoamento da solução electrolítica igual a 1. O tratamento térmico em autoclave foi realizado a uma temperatura e pressão de 134ºC e 2,16 bar, respectivamente, durante 30 minutos. O raio e ângulo de curvatura impostos durante os ensaios experimentais foram de 4,7 mm e 45º, respectivamente. A velocidade de rotação utilizada para testar os instrumentos foi de 500 rpm. O tempo até à fractura foi registado e o número de ciclos à fractura foi calculado. Calculou-se a área circular equivalente do instrumento Hyflex .06/20, em 3 regiões diferentes do mesmo (apical, central e coronal), na secção do instrumento correspondente a metade do comprimento do arco imposto pela curvatura do canal. Os valores de extensão teóricos foram calculados com o objectivo de comparar com a distribuição de tensão e extensão obtida pelo método dos elementos finitos. Os valores calculados analiticamente estão coerentes com os valores obtidos pelo método dos elementos finitos. Existe um grande risco de fractura do instrumento durante o tratamento endodôntico de canais radiculares que imponham curvaturas coronais aos instrumentos. Analisando os resultados obtidos experimentalmente, verifica-se que existem diferenças significativas, na duração e no número de ciclos à fadiga, entre os instrumentos polidos e não polidos e entre os instrumentos com e sem tratamento térmico por autoclave. Conclui-se que o polimento electrolítico tem uma influência significativa na vida à fadiga dos instrumentos Hyflex .04/20 e .06/20. O tratamento térmico por autoclave tem uma influência negativa nos instrumentos Hyflex .04/20 e uma influência positiva nos instrumentos Hyflex .06/20.

Avaliação das características superficiais de instrumentos reciprocantes por meio de icroscopia eletrônica de varredura antes e após o uso

Pós-graduação em Odontologia - FOAR

Sistema de instrumentação mecanizada Hyflex EDM

A Endodontia é uma área em constante evolução. Consideráveis desenvolvimentos nos materiais e técnicas têm sido essenciais para o melhoramento dos resultados nos tratamentos realizados. É exemplo disso mesmo a constituição dos instrumentos Endodônticos primordiais, construídos em cordas de piano, com evolução para aço de carbono, material este que sofria corrosão provocado pelo cloro presente no hipoclorito de sódio. O aço de carbono evoluiu para aço inoxidável e deste as limas endodônticas passaram a ser feitas em níquel-titânio, conferindo-lhes melhor flexibilidade e efeito de memória de forma. Mesmo com todas estas melhorias significativas, fraturas de instrumentos e erros durante a instrumentação continuam a acontecer e com eles veio a necessidade da pesquisa de possíveis melhorias da constituição das limas em NiTi. Como resultado surgiram ligas como o M-wire, fase-R e CM-wire, criadas a partir de tratamentos térmicos, que trouxeram às limas Endodônticas maior flexibilidade e resistência à fratura que os instrumentos feitos em NiTi convencional. A mais recente evolução das limas Ni-Ti, desenvolvida pela Coltene Whaldent (Allstätten, Suiça), são as limas Hyflex EDM, limas para canais radiculares de 5ª geração. O seu processo de fabrico por eletroerosão cria uma superfície única fazendo com que estas limas sejam mais duras e resistam mais à quebra, aliado à sua alta flexibilidade. É possível assim reduzir o número de limas para a limpeza e modelagem dos canais durante os tratamentos endodônticos sem comprometer a preservação da anatomia dos canais. As limas Hyflex EDM possuem, tal como as limas Hyflex CM, o efeito de controle de memória (CM), o que confere propriedades muito similares entre os dois sistemas.

Dendritic Arm Spacing Affecting Mechanical Properties and Wear Behavior of Al-Sn and Al-Si Alloys Directionally Solidified under Unsteady-State Conditions

Alloys of Al-Sn and Al-Si are widely used in tribological applications such as cylinder liners and journal bearings. Studies of the influence of the as-cast microstructures of these alloys on the final mechanical properties and wear resistance can be very useful for planning solidification conditions in order to permit a desired level of final properties to be achieved. The aim of the present study was to contribute to a better understanding about the relationship between the scale of the dendritic network and the corresponding mechanical properties and wear behavior. The Al-Sn (15 and 20 wt pct Sn) and Al-Si (3 and 5 wt pct Si) alloys were directionally solidified under unsteady-state heat flow conditions in water-cooled molds in order to permit samples with a wide range of dendritic spacings to be obtained. These samples were subjected to tensile and wear tests, and experimental quantitative expressions correlating the ultimate tensile strength (UTS), yield tensile strength, elongation, and wear volume to the primary dendritic arm spacing (DAS) have been determined. The wear resistance was shown to be significantly affected by the scale of primary dendrite arm spacing. For Al-Si alloys, the refinement of the dendritic array improved the wear resistance, while for the Al-Sn alloys, an opposite effect was observed, i.e., the increase in primary dendrite arm spacing improved the wear resistance. The effect of inverse segregation, which is observed for Al-Sn alloys, on the wear resistance is also discussed.

Histological evaluation of the effectiveness of increased apical enlargement for cleaning the apical third of curved canals

P>Objective To evaluate the influence of apical size on cleaning of the apical third of curved canals prepared with rotary instruments. Methodology Forty-four mesiobuccal canals of maxillary molars teeth were instrumented to different apical sizes (30, 0.02; 35, 0.02; 40, 0.02; 45, 0.02) using a crown-down technique. After canal preparation, the apical thirds of the roots were submitted to histological processing and examination. The specimens were analysed at 40x magnification and the images were submitted to morphometric analysis with an integration grid to evaluate the percentage of debris and uninstrumented root canal walls. The action of the instruments on the root canal walls was assessed based on the surface regularity, abrupt change on the continuity of root canal walls, and partial or total pre-dentine removal. The results were statistically compared using one-way anova with post hoc Tukey test. Pearson`s correlation was performed to identify potential correlations between values. Results The percentage of uninstrumented root canal dentine was higher when apical enlargement was performed with instruments 30, 0.02 taper (55.64 +/- 4.62%) and 35, 0.02 taper (49.03 +/- 5.70%) than with instruments 40, 0.02 taper (38.08 +/- 10.44%) and 45, 0.02 taper (32.65 +/- 8.51%) (P < 0.05). More debris were observed when apical enlargement was performed with instruments 30, 0.02 taper (34.62 +/- 9.49%) and 35, 0.02 taper (25.33 +/- 7.37%) (P < 0.05). There was a significant correlation between the amount of remaining debris and the perimeter of uninstrumented root canal dentine (r = 0.9130, P < 0.001). Conclusion No apical enlargement size allowed the root canal walls to be prepared completely. Apical third cleanliness could be predicted by instrument diameter.