The main focus of this research is the transformation induced fatigue behavior of shape memory alloy (SMA) actuators undergoing thermally induced martensitic phase transformation. The recent development of aerospace applications employing shape memory alloys (SMAs) has expanded the need for fatigue life characterization and modeling. Lightweight, compact and with a great work output, SMAs are ideal materials for actuated structural components. However, fatigue life becomes a key factor in applications such as commercial airplanes. Therefore, it is necessary to not only perform fatigue testing but also to investigate the causes of fatigue failure. As a new class of materials, SMAs have unique characteristics and require novel test methodologies to conduct repeatable and reliable fatigue testing. For this research, two materials are being investigated: TiNiCu and Ni-rich NiTi. The experiments performed on the first selected alloy, i.e. TiNiCu SMA, explore three major parameters: the applied stress level, the amount of actuation, and the corrosive nature of the environment. Experimental results show that SMAs undergoing transformation induced fatigue exhibit a low-cycle fatigue behavior and the measurement of the accumulated plastic strain at failure is associated to a Manson-Coffin type failure criterion. Investigations conducted on the post-mortem microstructure showed evidence of a multiphysical coupling between corrosion and cyclic phase transformation, from which a novel cyclic damage mechanism is proposed and explained using the micromechanical shear lag model accounting for actuation and accumulated plastic strains. Thereafter, based upon the identified failure mechanism and considering damage accumulation through crack formation, a stress renormalization procedure is proposed in combination with the Miner’s rule to predict the reduction of number of cycles to failure due to cyclic phase transformation and corrosion. A direct method is first presented and the predictions show good agreement with experimental results. However, both corrosion and corrosion-free fatigue data are required. Therefore, a new approach is proposed: the inverse Miner’s rule, which requires corrosion fatigue data only to predict corrosion-free life. The new and attractive properties of the selected second alloy, i.e. Ni-rich NiTi SMA, have revived the motivation of the aerospace industry to design SMA actuators. One particular property is cyclic stability generated by precipitation hardening mechanism using precipitates. However, are also precipitates due to high Nickel content (60 wt.% or 55 at.%). Parameters such as processing, heat treatments, size effects, surface quality and environment are investigated. Thermomechanical response and fatigue life are discussed and the greatest impact is found to come from specimen surface quality. Finally, a detailed fractography presents the different microstructural aspects of the fatigue damage and concludes to a precipitation driven fatigue failure mechanism cause by precipitates.

NiTi based shape memory alloys (SMA) cover most of the commercially produced shape memory devices and components. The reversible martensitic transformation between the phases B2 (austenite) and B19′ (martensite) is responsible for the shape memory effect in these alloys. The amount of strain which can be regained after a permanent deformation through thermal activation, known as the recoverable strain, is a strong function of crystallographic texture and microstructure. Texture influences the activation of a specific martensite variant during stress induced martensitic (SIM) transformation and also the re-orientation of twinned variants during further deformation. The variant selection decides the amount of recoverable strain. Since the NiTi based shape memory alloys inevitably undergo thermo-mechanical processing in the course of component design, the consequent evolution of texture and microstructure regulate the shape memory behavior. The present thesis is aimed to address this issue in some NiTi alloys that are technologically important for different applications, namely a binary Ni-rich NiTi alloy, a copper containing NiTi alloy and a hafnium containing NiTi alloy. The Ni rich NiTi alloy displays pseudoelastic behavior that can be used for couplings, the NiTiCu alloy provides a controlled thermal hysteresis suitable for actuator applications and the NiTiHf alloy can be used for high temperature applications. The first Chapter of the thesis provides a detailed overview of the existing knowledge related to evolution of microstructure and texture during processing, the transformation texture and its role on the shape memory behavior in NiTi alloys. The second chapter includes the experimental procedure followed to generate different textures, namely unidirectional and cross rolling with and without a subsequent annealing and also the details of the techniques used to characterize the structure, microstructure, texture and mechanical properties. The evolution of texture during thermo-mechanical processing of a Ni rich NiTi alloy and its impact on shape memory behavior is addressed in Chapter 3. The two modes of rolling employed at higher temperature led to the formation of different textures. The texture of unidirectionally rolled samples was characterized by a strong <111>||ND fiber, while a strong Goss {100}<110> component along with <111>||ND fiber was observed in the texture of the cross rolled samples. Annealing of the unidirectionally rolled samples generated a strong <100>||ND fiber, and a weak <111>||ND fiber was observed for the cross rolled samples. Microtexture analyses indicated that dynamically recrystallized grains had significantly different texture compared to the statically annealed material. One of the salient features of this study is the analysis of different twin boundaries with coincident site lattice (CSL) relations that has been observed in the hot rolled material. The origin of these twins has been attributed to deformation. The evolution of twin boundaries with CSL relation has strong influence on texture formation. A few of the important texture components have been found to have CSL relation amongst them. The origin of different texture components were found using intra-grain misorientation parameters. In-situ transformation studies in a scanning electron microscope have confirmed the formation of different types of twins at very low amount of strain in the Ni rich NiTi alloy. A Schmid factor based criterion was used to identify the activation of a particular variant. Trace analysis of the surface relief due to SIM transformation was utilized to confirm the theoretically predicted variant. Schmid criterion has been found to be valid in all the cases. Modulus variation with temperature and strain was studied using dynamical mechanical analysis. Microstructural changes during thermal and thermo-mechanical cycling revealed higher orientation gradient along grain boundaries compared to grain interior. The compatibility condition at the grain boundaries were attributed to higher misorientation development. Misorientation development during cycling loading process is also found to be a strong function of texture. Processing condition and texture has a strong influence on the recoverable strain. Particularly, the strength of <111>||ND fiber is influential in deciding the recoverable strain. Study of microstructure and texture evolution in the TiNiCu SMA and subsequent study on its impact on recoverable strain is presented in Chapter 4. Convincing evidences for the mechanisms operating during different dynamic restoration processes have been presented through microstructural investigation. Texture analysis of the austenite phase showed the formation of <111>||ND fiber. Despite the weakening of texture at larger strain, strength of certain deformation texture components like S {123}<634> and Cu {112}<111> increased, which suggested that texture evolution in TiNiCu alloy deviates from the texture of binary NiTi at large strains. Transformation texture analysis was carried out through electron back scattered diffraction technique, using an in-situ heating stage. The analysis of the results showed predominant activation of <011> type II as well as {11 1 } type I twins. A comparison of martensite and austenite pole figures indicated strong variant selection during phase transformation. Like the binary NiTi alloy, cross rolling of TiNiCu alloy also showed ample changes in the texture of martensite phase through the formation of different texture components. Annealing of both unidirectionally and cross rolled samples led to the weakening of texture. The change in volume fraction of Ti2NiCu precipitates, resulting from different processing conditions, influenced the transformation temperature. In this case also, texture and large intra-grain misorientation governed the recoverable strain. Chapter 5 is dedicated to the study of high temperature NiTiHf alloy. X-ray diffraction and differential scanning calorimetric studies confirmed a two step martensitic transformation, a B19` monoclinic and rhombohedral R-phase martensite in the studied alloy (Ni49.4Ti38.6Hf12). Microstructural investigations showed the formation of dendritic (Ti,Hf)2Ni precipitates along the grain boundary. Evolution of R-phase martensite was always observed along with (Ti,Hf)2Ni precipitates, irrespective of the processing condition. Dissolution of (Ti,Hf)2Ni precipitates by solution treatment suppressed the R phase formation. Strong texture of R-phase martensite confirmed variant selection during martensitic transformation. On the contrary, texture of B19` martensite was always weak, suggesting no preference for variant selection. Rolled material with a relatively strong texture exhibited higher recoverable strain compared to annealed material. Finally, all the significant outcomes of the present investigation are summarized in Chapter 6. Based on the conclusions, suggestions for future work have been mentioned.

Ce travail décrit une étude expérimentale sur des tôles en Ni-Ti à température ambiante en cisaillement plan simple, et pour des vitesses de déformation de 10-4 à 103/s. En quasi-statique (10-4-10-2/s), la mesure optique du champ de déplacement est indispensable à cause du faible déplacement (0.3mm). Des essais à vitesse de déformation intermédiaire (10-1-101/s) ont été réalisés avec la Machine MTS modifiée, capable d'aller à 300mm/s. Une caméra rapide est nécessaire pour suivre ces tests. Enfin, des barres de Hopkinson sont utilisées pour les essais à haute vitesse (102-103/s).Les efforts se sont concentrés sur la méthodologie afin d'explorer les limites expérimentales. Au niveau mécanique, des efforts ont été apportés sur la conception des montages des mors pour combiner des exigences contradictoires. Au niveau mesure, des caméras optiques fonctionnant jusqu'à 5M images/s ont été utilisées. La texture des images, la peinture, la lumière, la taille d'élément et l'incertitude sont analysées. De plus, la caméra infrarouge est utilisée pour confirmer l'observation optique sous faibles vitesses de déformation.Finalement, des essais ont été réalisés pour 7 ordres de grandeurs de la vitesse de déformation, avec identification de la relation contrainte-déformation et observation de l'évolution de la bande de transformation. On observe : (i) Une augmentation de la contrainte avec la vitesse de déformation. (ii) Un champ de déformation non homogène, même en faible vitesse, avec une bande à 10 degrés par rapport à la direction de cisaillement. (iii) Deux bandes séparées à haute vitesse (102/s), ce qui indique que la bande de localisation dépend de la vitesse de chargement. / This work describes an experimental study on a NiTi alloy at the ambient temperature (Pseudoelastic behavior) under the double in-plane shear loading over strain rates from 10-4 to 103/s. Under quasi-static loadings (10-4-10-2/s), the optical full-field measurement is necessary because of the very small displacement (0.3mm). The intermediate loading rates (10-1-101/s) are realized with a modified MTS machine able to load at 300mm/s. Moreover, a high-speed camera is needed to follow such tests. Finally, the Split Hopkinson bars are used to perform tests at impact loading rates (102-103/s).The main effort has been made on the methodological study to explore the experimental possibility. For the mechanical level, the attention has been paid on the design of the clamping system to cope with the contradictory requirements. For the measuring level, different optical cameras with sampling rate till to 5M frames/second are used. The texture, the painting, the lightening, the element size and the uncertainty are analyzed. Furthermore, an infrared camera was used at lower loading rates to confirm the DIC measurement.The tests are continually performed over 7 decades of the strain rate. The nominal stress-strain curves and the detailed observation of the transformation band evolution are measured. The main findings are as follows: (i) Regular stress increase with the strain rate; (ii) an inhomogeneous strain field under in-plane shear condition, even at very low strain rates, with a band at 10 degrees from the shear direction under lower strain rates. (iii) Two separated bands at the strain rate of 102/s, which suggests that the localized transformation bands are rate dependent.

NiTiCu is a shape memory alloy that regains its original shape after large amount of shape changing deformation when heated above a critical temperature called reverse martensitic trans-formation temperature( Af). When external load is applied on the sample in twinned martensite phase at low temperature, it deforms by detwinning, accommodating large amount of strains. When it is heated above Af, the shape recovers by transformation of the martensite to austenite phase. However, the amount of shape recovery degrades over time due to internal factors such as precipitates, residual strains and thermal history as well as external factors such as stresses. Severe localized stresses induced by contacts result in plastic deformation that affect the reverse martensitic transformation and hence the shape recovery. In this work, we study how varying levels of contact stresses induced in NiTiCu thin film affect its shape recovery. NiTiCu thin films of six different compositions are deposited on Si(100) wafer by co-sputtering from elemental targets. After deposition, the films are annealed at 500 C for 4 h to make them crystalline. The composition of the films varied linearly with applied power to the targets. Uniformity in composition over a 4 inch substrate area is achieved by substrate rotation. All the films show ne grain microstructure after annealing. The subsurface of the Ni-rich films is columnar. Ni-rich films have annealing cracks and the crack width increases with Ni composition in the films. The roughness of as-deposited films is found to be more for Ni-rich films compared to Ti-rich films. The roughness of the Ni-rich and Ti-rich films increased after annealing. From the X-ray diffraction studies, it was observed that the films are nanocrystalline. Indentation is carried out using a Berkovich diamond indenter with spherical apex, at nine different locations with loads ranging from 0.25 mN to 25 mN. A predefined array is chosen for indentation such that the larger indents act as a guide to precisely locate minute indents generated at lower loads, with residual depth as small as 10 nm, for imaging in high-resolution microscopes like Scanning Electron Microscope as well as in Atomic Force Microscope . In Ti60 (a Ti-rich) lm, the residual indents generated at loads greater than 10 mN show radial cracks originating at corners. Average crack length increases with the maximum load used for generating the indent. Sequential sectioning of Ti48 (a Ni-rich) lm using Focused Ion Beam microscope, revealed that the cracks originate at the lm-substrate interface and reach the surface. In Ti48 lm, residual indents do not show any indentation cracks. The indentation stresses are accommodated by breaking of the columnar structure and the voids between them. Delamination of the film from the substrate is observed on either sides of the indent in both the Ti60 and Ti48 films. The hardness of the films is high at low loads and decrease as the load increases. The deformation by indentation at lower loads is mainly due to detwinning as only the apex of the indenter, which is nearly spherical, is in contact with the sample and the resulting stresses are low. As the load increases, the deformation starts getting accommodated through dislocations along with detwinning as the stress beneath the indenter increases. Spherical cavity model extended to SMA shows that inner hemisphere near the tip contains dislocations where stresses are very high, surrounded by detwinned region with stresses that are relatively low. When the sample is heated above reverse martensitic transformation temperature to induce shape recovery in the indents, only the detwinned region recovers to the original shape. Recovery ratio, quantification of shape recovery, is calculated from the depth of the indents before and after heating. Recovery ratio in Ti60 films is found to be large at low loads and decreases with increase in load. The decrease in shape recovery in Ti60 is attributed to the increase in the amount of plastic deformation at the expense of detwinning. Three-dimensional mapping of the surfaces shows that the recovery ratio is high at the apex of the indent at the maximum depth and reduces towards the edges of the indent. There is no evident recovery in Ti48 films. The shape recovery of SMAs can be achieved by Joule heating. When electric current is passed through the material, it heats up by Joule heating because of the intrinsic resistivity. The resistivity and hence the resistance would get effected by the dislocation based plastic deformation induced by the contact. This might result in shape recovery through resistive heating. Towards understanding this, the effect of contact stresses on electrical contact resistance is studied. Experimental setup is designed, developed and calibrated for studying the variation of electrical contact resistance of the NiTiCu thin films as a function of load. Electrical contact resistance is found to decrease with increase in applied load. Contact stresses in sub-micron NiTiCu thin films are simulated by carrying out nanoindentation at different loads. The recovery ratio is high when the stresses induced by the contact is less, at lower loads. The shape recovery ratio is reduced when the induced contact stresses in-creases. There is no shape recovery at the sharp edges of the indentation where contact stresses are very high. Hence, by carefully designing the features to reduce the stress concentrations, the performance of the device can be improved.

No description available.

PROPOSIÇÃO: O objetivo desta pesquisa foi apresentar a magnitude e a constância das forças liberadas por fios ortodônticos de níquel-titânio, usados para a correção dos apinhamentos dentários. Outro objetivo foi comparar os dois meios mais utilizados de avaliação da deflexão elástica destes fios: o teste de 3 pontos e o dispositivo de simulação clínica. MATERIAL E MÉTODOS: Foram avaliados 11 grupos de fios de liga predominantemente de níquel-titânio, calibre 0,014, de 6 marcas diferentes (Abzil convencional e termoativado; GAC convencional e termoativado; Morelli convencional e termoativado; Ormco CuNiTi; Orthometric convencional e termoativado e Orthosource convencional e termoativado), em teste de deflexão elástica, nas deflexões de 0,5; 1; 2 e 3mm. Uma máquina de ensaio universal INSTRON 3342, com célula de carga de 10N foi utilizada e, como protocolo, foi seguida a norma ISO 15.841. Para a análise estatística dos resultados foram utilizados os testes: Kolmogorov-Smirnov, para conferir se havia normalidade; teste t independente, para comparação dos resultados do teste de 3 pontos e dos resultados do dispositivo; e o teste ANOVA seguido do teste de Tukey, para comparações entre grupos. RESULTADOS: Houve diferença estatística entre os resultados gerados pelo teste de 3 pontos e os gerados pelo dispositivo. Por ser o teste indicado pela norma ISO citada, somente os resultados do teste de 3 pontos foram considerados. Todos os fios estudados apresentaram pseudoelasticidade em uma faixa de variação de força de até 40cN. Os grupos Abzil convencional, GAC convencional, Morelli termoativado, Ormco CuNiTi e Orthometric convencional apresentaram força dentro de uma faixa considerada ótima para a indução da movimentação dentária (50cN-100cN). Os fios termoativados liberaram forças mais leves que seus pares convencionais. CONCLUSÕES: Dentre os grupos estudados, aqueles que apresentaram pseudoelasticidade, forças dentro de uma faixa considerada ótima e homogeneidade de amostra, foram os grupos Morelli termoativado e Ormco CuNiTi. / OBJECTIVE: The purpose of this study was to present the magnitude and the constancy of the forces released by nickel-titanium orthodontic wires, used to treat dental crowding. Another purpose was to compare the most usual types of bending tests used to evaluate these wires: 3-point test and clinical simulation device. MATERIAL AND METHODS: Eleven groups of orthodontic nickel-titanium wires, caliber 0.014, of 6 different brands (Abzil conventional and heat-activated; GAC conventional and heat-activated; Morelli conventional and heat-activated; Ormco CuNiTi; Orthometric conventional and heat-activated and Orthosource conventional and heat-activated) were tested by bending test, at deflections of 0.5; 1; 2 and 3mm. A universal testing machine INSTRON 3342 with a 10N load cell was used and, in order to standardize the tests, the ISO 15.841 regulation was followed. Statistical analysis was performed using the subsequent tests: Kolmogorov-Smirnov to verify normality; independent t test to compare the results of the 3-point test and the results derived from the device, and ANOVA followed by the Tukey test for intergroup comparisons. RESULTS: There were significant differences between the results of the 3-point test and the device. As indicated by the ISO regulation, only the results from the 3-point bending test were considered. All groups were classified as pseudoelastic, within a load range of 40cN, at maximum. The groups Abzil conventional, GAC conventional, Morelli heat-activated, Ormco CuNiTi and Orthometric conventional released load within optimum range (50cN-100cN). Heatactivated wires released lower load compared to conventional wire of the same brand. CONCLUSIONS: Among the groups evaluated those that presented pseudoelasticity, load within a range considered optimal, in a homogeneous manner, were Morelli heat-activated and Ormco CuNiTi.

No description available.

Deformation phenomena in shape memory alloys involve stress-, temperature-induced phase transformations and crystallographic variant conversion or reorientation, equivalent to a twinning operation. In near equiatomic NiTi, Ti rich compositions can exist near room temperature as a monoclinic B19' martensitic phase, which when deformed undergoes twinning resulting in strains as large as 8%. Upon heating, the martensite transforms to a cubic B2 austenitic phase, thereby recovering the strain and exhibiting the shape memory effect. Ni rich compositions on the other hand can exist near room temperature in the austenitic phase and undergo a reversible martensitic transformation on application of stress. Associated with this reversible martensitic transformation are macroscopic strains, again as large as 8%, which are also recovered and resulting in superelasticity. This work primarily focuses on neutron diffraction measurements during loading at the Los Alamos Neutron Science Center at Los Alamos National Laboratory. Three phenomena were investigated: First, the phenomena of hysteresis reduction and increase in linearity with increasing plastic deformation in superelastic NiTi. There is usually a hysteresis associated with the forward and reverse transformations in superelastic NiTi which translates to a hysteresis in the stress-strain curve during loading and unloading. This hysteresis is reduced in cold-worked NiTi and the macroscopic stress-strain response is more linear. This work reports on measurements during loading and unloading in plastically deformed (up to 11%) and cycled NiTi. Second, the tension-compression stress-strain asymmetry in martensitic NiTi. This work reports on measurements during tensile and compressive loading of polycrystalline shape-memory martensitic NiTi with no starting texture. Third, a heterogeneous stress-induced phase transformation in superelastic NiTi. Measurements were performed on a NiTi disc specimen loaded laterally in compression and associated with a macroscopically heterogeneous stress state. For the case of superelastic NiTi, the experiments related the macroscopic stress-strain behavior (from an extensometer or an analytical approach) with the texture, phase volume fraction and strain evolution (from neutron diffraction spectra). For the case of shape memory NiTi, the macroscopic connection was made with the texture and strain evolution due to twinning and elastic deformation in martensitic NiTi. In all cases, this work provided for the first time insight into atomic-scale phenomena such as mismatch accommodation and martensite variant selection. The aforementioned technique of neutron diffraction for mechanical characterization was also extended to engineering components and focused mainly on the determination of residual strains. Two samples were investigated and presented in this work; first, a welded INCONEL 718 NASA space shuttle flow liner was studied at 135 K and second, Ti-6Al-4V turbine blade components were investigated for Siemens Westinghouse Power Corporation. Lastly, also reported in this dissertation is a refinement of the methodology established in the author's masters thesis at UCF that used synchrotron x-ray diffraction during loading to study superelastic NiTi. The Los Alamos Neutron Science Center is a national user facility funded by the United States Department of Energy, Office of Basic Energy Sciences, under Contract No. W-7405-ENG-36. The work reported here was made possible by grants to UCF from NASA (NAG3-2751), NSF CAREER (DMR-0239512), Siemens Westinghouse Power Corporation and the Space Research Initiative.

No description available.

This thesis presents methods for the wafer-level integration of shape memory alloy (SMA) and electrostatic actuators to functionalize MEMS devices. The integration methods are based on heterogeneous integration, which is the integration of different materials and technologies. Background information about the actuators and the integration method is provided. SMA microactuators offer the highest work density of all MEMS actuators, however, they are not yet a standard MEMS material, partially due to the lack of proper wafer-level integration methods. This thesis presents methods for the wafer-level heterogeneous integration of bulk SMA sheets and wires with silicon microstructures. First concepts and experiments are presented for integrating SMA actuators with knife gate microvalves, which are introduced in this thesis. These microvalves feature a gate moving out-of-plane to regulate a gas flow and first measurements indicate outstanding pneumatic performance in relation to the consumed silicon footprint area. This part of the work also includes a novel technique for the footprint and thickness independent selective release of Au-Si eutectically bonded microstructures based on localized electrochemical etching. Electrostatic actuators are presented to functionalize MEMS crossbar switches, which are intended for the automated reconfiguration of copper-wire telecommunication networks and must allow to interconnect a number of input lines to a number of output lines in any combination desired. Following the concepts of heterogeneous integration, the device is divided into two parts which are fabricated separately and then assembled. One part contains an array of double-pole single-throw S-shaped actuator MEMS switches. The other part contains a signal line routing network which is interconnected by the switches after assembly of the two parts. The assembly is based on patterned adhesive wafer bonding and results in wafer-level encapsulation of the switch array. During operation, the switches in these arrays must be individually addressable. Instead of controlling each element with individual control lines, this thesis investigates a row/column addressing scheme to individually pull in or pull out single electrostatic actuators in the array with maximum operational reliability, determined by the statistical parameters of the pull-in and pull-out characteristics of the actuators. / QC20100729