Root canal preparation in narrow, curved canals is a challenge even for experienced endodontists. Recently nickel-titanium (NiTi) hand files have played an important role in root canal preparation, particularly in curved root canals. Nickel-titanium endodontic instruments were first investigated in 1988 by Walia et al. who found that NiTi files have two to three times more elastic flexibility in bending and torsion, as well as superior resistance to torsional fracture compared with similar stainless steel files.

The successful use of Nickel-Titanium (Nitinol) in biomedical applications requires an accurate control of its unique mechanical properties. The purpose of this study is to analyze the effects of a wide range of heat treatments on the mechanical behavior of hot-rolled and cold-drawn Nitinol. Results comprise an understanding of the effect of heat treatment temperature and time variation on final material response which is imperative for optimization of material properties. Thirty-three heat treatment variations are tested by combining three durations, 10 minutes, 90 minutes, and 8 hours, with eleven different heat treatment temperatures between 200°C and 440°C. Following heat treatment, the Nitinol samples undergo tensile testing with upper plateau strength, lower plateau strength, ultimate tensile strength, strain to failure, and residual elongation compared for all test groups. Heat treatment "power" is used to describe the efficacy of different combinations of heat treatment temperature and duration. When using hot-rolled Nitinol, results show a low heat treatment power does not create significant precipitation hardening or a significant decrease in martensite transformation stress, resulting in a high upper plateau strength, high residual strain values, and evidence of plastic deformation upon unloading. Moderate power treatments lead to sufficient hardening of the material and a decrease in martensite transformation stress resulting in a pseudoelastic response. Increasing to a high treatment power further decreases the transformation stress and increases the martensite transformation temperature leading to a shape-memory response in hot rolled Nitinol. When using cold-drawn Nitinol, low and moderate heat treatment power levels result in the material exhibiting a pseudoelastic response. Increasing heat treatment power shows the same effects on martensite transformation stress and temperature as seen with the hot-rolled material resulting in a material response transition from pseudoelastic to shape memory.

Shape memory and superelastic applications of NiTi based alloys have typically been limited to near room temperature or to bulk length scales. The objective of this work is two-fold: first, to investigate shape memory behavior at low temperatures in the context of the R-phase transformation in NiTiFe alloys by recourse to arc-melting, differential scanning calorimetry (DSC), transmission electron microscopy (TEM) and mechanical testing at low temperatures; and second, to investigate superelasticity and two-way shape memory behavior at reduced length scales in the context of NiTi by recourse to micro-compression, micro-indentation and TEM studies. Selected compositions of ternary NiTiFe shape memory alloys were arc-melted and thermomechanically processed to investigate the influence of composition and processing parameters on the formation of the R-phase. The methodology used for the processing and characterization of the alloys was established and included microprobe analysis, DSC, TEM and mechanical testing. No phase transformation was observed in alloys with Fe content in excess of 4 at.%. Thermomechanical treatments facilitated the formation of the R-phase in Ni-rich alloys. The range of the transformation between the R-phase and austenite, and the hysteresis associated with it were influenced by the distribution and size of metastable Ni4Ti3 precipitates. The investigation of the microstructural, thermal and mechanical properties of the R-phase transformation in NiTiFe alloys revealed a complex dependence of these properties on processing parameters. The present work also highlighted the hitherto unexplored competition between the two inelastic deformation modes operating in the R-phase (detwinning and stress-induced transformation) and established the preference of one mode over the other in stress-temperature space. iv The complete micromechanical response of superelastic NiTi was examined by performing careful micro-compression experiments on single crystal pillars of known orientations using a nanoindenter tip. Specifically, the orientation dependence of the elastic deformation of austenite, the onset of its transformation to martensite, the gradient and the hysteresis in the stress-strain response during transformation, the elastic modulus of the stress-induced martensite and the onset of plasticity of the stress-induced martensite were analyzed in separate experiments. A majority of the results were explained by recourse to a quantitative determination of strains associated with austenite grains transforming to martensite variants or twinning in martensite. Microstructural studies were also performed on a micro-indentation trained NiTi shape memory alloy specimen to understand the mechanisms governing the two-way shape memory effect. In situ TEM studies at temperature on specimens obtained at different depths below the indent showed the presence of retained martensite along with the R-phase. Previously, while such twoway shape memory behavior has typically been associated with large dislocation densities, this work provides evidence of the role of retained martensite and the R-phase in cases with reduced dislocation densities. Funding support for this work from NSF (CAREER DMR-0239512), NASA (NAG3-2751) and SRI is acknowledged.

Thesis (Ph. D.)--Ohio State University, 2007. / Title from first page of PDF file. Includes bibliographical references (p. 162-169).

published_or_final_version / Dentistry / Master / Master of Dental Surgery

published_or_final_version / abstract / Orthopaedics and Traumatology / Master / Master of Philosophy

O presente estudo teve como objetivo avaliar a resistência à fadiga cíclica de dois diferentes sistemas rotatórios de níquel-titânio, K3 (Sybron Endo, EUA) e Endosequence (Brasseler, EUA), fundamentando-se no número de usos. Todas as limas rotatórias que foram selecionadas possuíam conicidade 0.04, 25 mm de comprimento e diâmetro de ponta 25, padrão ISO. Para tal logro, um dispositivo desenvolvido especificamente para executar ensaios dinâmicos foi utilizado. Cada grupo foi subdividido em quatro subgrupos em função do número de usos, sendo estabelecidos da seguinte maneira: grupos A0 e B0, instrumentos sem nenhum uso; grupos A1 e B1, instrumentos de um único uso; grupos A3 e B3, instrumentos de três usos e grupos A5 e B5, instrumentos de cinco usos. Cada subgrupo era composto por 12 limas, totalizando 96 instrumentos rotatórios entre K3 e Endosequence. A simulação foi realizada em canais artificiais de resina com curvatura de 40 graus e raio de 5 mm. Todas as limas foram submetidas a ensaios de fadiga cíclica realizados em um dispositivo experimental que permitiu que o instrumento reproduzisse uma instrumentação rotatória em canais curvos. Esse dispositivo possui um temporizador, que registra o tempo de avanços em segundos, desde o início do movimento até a fratura da lima e também um contador, que registra dentro do intervalo de tempo o número de ciclos realizados pelo cilindro pneumático até o momento da fratura. Foi utilizada uma peça de mão com contra-ângulo redutor de 16:1, acionado por motor elétrico na velocidade de 350 rpm e 2 Ncm de torque. O tempo foi registrado por meio do contador presente no dispositivo. Os valores foram transformados em segundos. Para análise estatística, empregou-se o teste de análise de variância (dois critérios) entre as amostras testadas e observou-se que não houve diferença estatisticamente significante em relação ao número de usos. Entretanto, o sistema K3 apresentou maior resistência à fadiga flexural em relação ao sistema Endosequence (p < 0,05). / The aim of this work was to evaluate the cyclic fatigue resistance of two different nickel-titanium rotary systems, K3 (Sybron Endo, EUA) and Endosequence (Brasseler, EUA), based on the number of uses. All rotary files which were selected had their conicity of 0,04, 25mm of length and tip diameter of 25, following ISO standardization. To reach the purposes, a specially developed apparatus to perform dynamic assays was employed. Each group was subdivided into 4 subgroups according to the number of uses, being established as follows: groups A0 and B0, instruments without any use; groups A1 and B1, instruments of a single use; groups A3 and B3, instruments of three uses and groups A5 and B5, instruments of five uses. Each subgroup was compound of 12 files, totalizing 96 rotary instruments between K3 and Endosequence. The simulation was conducted in resin artificial canals presenting curvature of 40 degrees and radius of 5 mm. All files were submitted to cyclic fatigue assays performed on an experimental apparatus where the instrument could reproduce a rotary instrumentation in curved canals. This equipment contains an timer, which records advance time per seconds, since the begin of movement until the file fracture, and also has a counter which registers, on a period of time, the cycle number accomplished by the pneumatic cylinder until the fracture time. A reducer contra-angle hand piece of 16:1 was used, activated by an electric motor on a speed of 350rpm and 2 Ncm of torque. Time was recorded by the counter coupled in the apparatus. Values were converted into seconds. The two-way analysis of variance was employed to statistical evaluation, among tested samples and we could observe that no statistical differences were found in relation to the number of uses. However, the K3 system showed higher resistance to flexural fatigue when compared to the Endosequence system (p < 0,01).

Thesis (M.D.S.)--University of Hong Kong, 2000. / Includes bibliographical references (leaves 119-130) Also available in print.

Thesis (Ph. D.)--Hong Kong University of Science and Technology, 2002. / Includes bibliographical references (leaves 155-160). Also available in electronic version. Access restricted to campus users.

Thesis (M. Phil.)--Hong Kong University of Science and Technology, 2003. / Includes bibliographical references (leaves 94-98). Also available in electronic version. Access restricted to campus users.