De nombreuses avancées ont été réalisées en termes de géométries instrumentales, mouvements de travail et procédés de fabrication des limes endodontiques. Cependant, peu de recherches se sont tournées vers l’utilisation d’alliages à mémoire de forme (AMF) autres que le Nickel-Titane (NiTi). Ce travail se propose de développer un instrument endodontique constitué d’un nouvel AMF aux propriétés mécaniques et antimicrobiennes très prometteuses : le CuAlBe monocristallin. Après une première analyse par éléments finis des paramètres géométriques adéquats pour une lime endodontique en AMF monocristallin à base de CuAlBe, plusieurs prototypes ont été fabriqués puis testés en rotation continue selon un protocole de pénétration / retrait (P/R) dans des canaux artificiels. Des limes endodontiques en NiTi, déjà commercialisées, ont été également testées avec le même protocole. L’objectif de ces recherches était de montrer que les instruments endodontiques en CuAlBe monocristallin présentaient des performances mécaniques équivalentes à ceux en NiTi, en plus de leurs propriétés antimicrobiennes / Many advances have been made in terms of instrumental geometry, working motion and manufacturing processes of endodontic files. However, since the discovery of Nickel-Titanium (NiTi) shape memory alloys (SMA), few research has been carried out on new SMAs. In this context, this work aims to develop an endodontic instrument machined from a new SMA with very promising mechanical and antimicrobial properties: the single crystal CuAlBe. Following a finite element analysis in order to determine adequate geometric parameters for a single crystal CuAlBe SMA endodontic instrument, prototypes were machined and tested following a continuous rotation penetration / removal (P/R) protocol in artificial canals. Endodontic files made of NiTi SMA, already commercialized, were also tested with the same protocol. The aim of this researches is to show that CuAlBe endodontic instruments could lead equivalent mechanical performances to NiTi instruments in addition of their antimicrobial properties

Submitted by Maria Medeiros (maria.dilva1@ufcg.edu.br) on 2018-07-09T12:28:39Z No. of bitstreams: 1 MATHEUS JOSÉ CUNHA DE OLIVEIRA - DISSERTAÇÃO (PPGCEMat) 2016.pdf: 9296942 bytes, checksum: a273053730345dafcd282de1fc0bf6f1 (MD5) / Made available in DSpace on 2018-07-09T12:28:39Z (GMT). No. of bitstreams: 1 MATHEUS JOSÉ CUNHA DE OLIVEIRA - DISSERTAÇÃO (PPGCEMat) 2016.pdf: 9296942 bytes, checksum: a273053730345dafcd282de1fc0bf6f1 (MD5) Previous issue date: 2016-02-16 / CNPq / As Ligas com Memória de Forma (LMF) foram descobertas nos anos 60 e o desenvolvimento de vários sistemas (NiTi, CuAlNi, CuAlBe, CuZnAl) vem sendo explorado desde então, sendo aquelas do sistema NiTi as mais utilizadas. Devido às suas excelentes propriedades mecânicas, ótima resistência a corrosão e biocompatibilidade, além de apresentarem as melhores propriedades funcionais de efeito de memória de forma e superelasticidade, as LMF NiTi e suas variações ternárias passaram a ser objeto de estudos para várias aplicações nas mais diferentes áreas. Um dos maiores problemas das LMF NiTi ainda está relacionado a dificuldades de conformação mecânica e usinagem. Por esse motivo, o processo de soldagem pode ser uma boa ferramenta alternativa para se conseguir obter peças de geometrias mais complexas, envolvendo a união das LMF NiTi com metais convencionais, como o aço inoxidável. O aço inoxidável é uma opção importante de união com LMF NiTi pois possui igualmente propriedades desejadas de resistência mecânica, biocompatibilidade e resistência a corrosão. A união por soldagem destas duas ligas encontra barreiras diversas, sendo a principal delas a formação de intermetálicos frágeis na junta soldada limitando sua resistência mecânica e consequente aplicação. Nesse contexto, o presente trabalho teve como objetivo geral avaliar a soldabilidade de chapas finas (espessura de 1 mm) de uma LMF NiTi com aço inoxidável (INOX) AISI 304 utilizando o processo micro GTAW e compreender a metalurgia da soldagem na variação das propriedades mecânicas e metalúrgicas das juntas. O processo GTAW foi escolhido por ser mais econômico que os processos usuais de soldagem para estas ligas NiTi, como a soldagem a laser (LBW). As juntas dissimilares NiTi-SS obtidas foram caracterizadas pelas técnicas de MO, MEV, EDS, DSC, ensaios de tração à ruptura e de dureza Vickers. Estas juntas foram soldadas utilizando a própria LMF NiTi e também o Inconel 625 como metais de adição. No geral, constatou-se que as juntas apresentam comportamento frágil, porém ao se utilizar camada intermediária de Inconel 625 na união entre os metais dissimilares e após tratamento térmico para alívio de tensões, é possível aumentar a resistência mecânica da junta para valores da ordem de 150MPa. As juntas apresentaram uma poça de fusão heterogênea devido a formação de elementos fragilizantes ao longo do metal de solda. Observou-se a formação de uma zona parcialmente diluída (ZPD) correlacionada a um aumento excessivo da dureza nesta região e composição química distinta. / Shape Memory Alloys (SMA) were discovered in the 60s and the development of various systems (NiTi, CuAlNi, CuAlBe, CuZnAl) has been explored since then, with those of the NiTi system the most commonly used. Due to its excellent mechanical properties, good corrosion resistance and biocompatibility, in addition to having the best functional properties of shape memory effect and superelasticity, the NiTi SMA and its ternary variations have become the subject of studies for various applications in different areas. One of the main problems of NiTi SMA is also related to difficulties in forming and machining. For this reason, the welding process can be a good alternative tool to achieve more complex geometry parts, involving the union of NiTi SMA with conventional metals, such as stainless steel. Stainless steel is an important option for union with NiTi SMA, since it also has desired properties of mechanical strength, biocompatibility and corrosion resistance. The union by welding between these two alloys find various barriers, the main one being the formation of brittle intermetallic compounds on the welded joint, limiting its mechanical strength and consistent application. In this context, this study aimed to assess the weldability of thin sheet metal (1 mm thick) of a NiTi SMA with AISI 304 stainless steel (SS) using the micro process GTAW, and study the influence of welding metallurgy in mechanical and metallurgical properties of the joints. The GTAW process was chosen because it is more economical than the usual welding processes for these NiTi alloys such as the laser beam welding (LBW). The NiTi-SS dissimilar joints obtained were characterized by optical microscopy techniques, SEM, EDS, DSC, tensile test to rupture and Vickers hardness. These joints were welded using NiTi SMA and also the Inconel 625 as filler metals. Overall, it was found that the joints have brittle behavior, but when using an intermediate layer of Inconel 625 at the junction between dissimilar metals and after heat treatment for stress relief, it is possible to increase the mechanical strength of the joint for values in the order of 150MPa. The joints exhibited a heterogeneous molten weld pool due to formation of elements along the embrittlement of the weld metal. It was observed the formation of a partially diluted zone (PDZ) correlated to an excessive increase of the hardness in that region and different chemical composition.

Submitted by Renata Lopes (renatasil82@gmail.com) on 2016-06-08T13:51:53Z No. of bitstreams: 1 douglasmartinsvieiradasilva.pdf: 9760300 bytes, checksum: 76f54b4635afbf189d4c45e3c3a06ab7 (MD5) / Approved for entry into archive by Adriana Oliveira (adriana.oliveira@ufjf.edu.br) on 2016-06-08T13:53:47Z (GMT) No. of bitstreams: 1 douglasmartinsvieiradasilva.pdf: 9760300 bytes, checksum: 76f54b4635afbf189d4c45e3c3a06ab7 (MD5) / Made available in DSpace on 2016-06-08T13:53:47Z (GMT). No. of bitstreams: 1 douglasmartinsvieiradasilva.pdf: 9760300 bytes, checksum: 76f54b4635afbf189d4c45e3c3a06ab7 (MD5) Previous issue date: 2016-02-24 / CAPES - Coordenação de Aperfeiçoamento de Pessoal de Nível Superior / NiTi (nitinol) é uma liga com efeito memória de forma (EMF), o EMF é um termo utilizado para descrever a capacidade de certos materiais, depois de deformados plasticamente, voltarem às suas formas originais por aquecimento. Ligas com essa propriedade são empregadas em vários setores da indústria metalúrgica, que vão desde aeroespacial, eletrônica, construção, Robótica e Bioengenharia. Podem ser utilizadas em conectores, sensores, dispositivos de segurança e muitas outras aplicações. Este trabalho foi divido em duas partes: utilizando os parâmetros do potencial TBSMA, energia de coesão, parâmetros de rede em T=0K, para a fase B2 NiTi, retirados do trabalho do Liu e colaboradores, estudamos a formação de nano os com simulações via Dinâmica Molecular (DM) em duas fases especí cas da liga de NiTi: a fase de alta temperatura B2 cúbica (austenítica) e a fase de baixa temperatura B19 monocíclica (martensítica), alongando o sistema em diferentes direções cristalográ cas; ajustamos os parâmetros do potencial TB-SMA para a liga NiTi na fase B19', calculando (via método de Parrinello- Rahman) a variação do volume e da entalpia do sistema com a temperatura, obtendo a temperatura de fusão com ótima concordância com valor experimental e comprovando a e cácia do potencial utilizado. Apresentamos resultados das energias do estado fundamental e a estabilidade mecânica relativa as fases B2, B19, B19' e BCO, bem como as transições de fase ocorridas sob tensão mecânica e os parâmetros de rede para cada uma dessas fases. Vimos que é necessário uma tensão xz = 0.38 GPa para estabilizar a fase B19'. Também determinamos as constantes elásticas e os parâmetros elásticos macroscó- picos (módulos de bulk, limites de Reuss e Voigt) para a fase B19' de NiTi. Os resultados estão em ótima concordância com dados experimentais. / NiTi (Nitinol) is an alloy with shape memory e ect (SMA), the SMA is a term used to describe the ability of some materials after having been deformed plastically, back to its original shape by heating. Metallic materials that have this interesting property are employed in various sectors of the metallurgical industry, ranging from aerospace, electronics, construction, Robotics and Bioengineering. This type of material can be used in connectors, sensors, safety devices, and many other applications. This study was divided into two parts: using the parameters the potential TB-SMA, energy choesion, lattice parameters at T=0K, for the phase B2 NiTi, removed from Liu et al work, we studied the formation of nanowires with means molecular dynamics (MD) simulations at two speci c stages of NiTi alloy: a high-temperature phase B2 cubic (austenitic) and phase B19 monocyclic low temperature (martensite), extending the system in di erent crystallographic directions; adjust the TB-SMA potential parameters for the NiTi alloy in B19' phase, calculating (by method Parrinello-Rahman) the volume variation and the enthalpy of the system to temperature, obtaining the melting temperature with excellent agreement with experimental value and proving the e ectiveness of potential use. We present results of the energy of the ground state and the mechanical stability relative B2, B19, B19' and BCO phases, as well as phase transitions observed under mechanical tension and the network parameters for each of these phases. We saw that a voltage is necessary xz = 0.38 GPa to stabilize the B19' phase. Also determine the elastic constants and the macroscopic elastic parameters (bulk modules, limits Reuss and Voigt) for phase B19' of NiTi. The results are in excellent agreement with experimental data.

[pt] Limas de NiTi Profile® 25/.04 após sua usinagem não recebem tratamento superficial de polimento gerando pontos concentradores de tensão conseqüente áreas de trinca e fraturas. Avaliou-se o efeito de diferentes condições superficiais de limas endodônticas na resistência à torção. Foram avaliadas e caracterizadas por Microscopia Eletrônica de Varredura dezoito limas rotatórias de NiTi Profile® 25/.04. Utilizou-se 6 limas que não foram submetidas a tratamento químico (Grupo I), 6 limas tratadas com Ácido Nítrico 8% e Ácido Fluorídrico 4% em solução durante 2 minutos (Grupo II) e 6 limas tratadas com a mesma solução porém em tempo de 2 minutos e trinta segundos (Grupo III). Analisaram-se as limas com e sem tratamento superficial carregadas em ensaio de torção e suas fractografias em Microscopia Eletrônica de Varredura. As variáveis avaliadas foram torque aplicado no momento da fratura e ângulo máximo de rotação até a fratura. Os valores obtidos nos ensaios mecânicos referentes ao ângulo máximo de rotação e torque máximo foram analisados estatisticamente através do teste estatístico T-student. Os resultados obtidos permitem concluir que houve diferença estatisticamente significante quanto aos valores de torque máximo entre o Grupo II e Grupo III e ângulo máximo entre os Grupos I e III. / [en] NiTi Profile® 25/.04 files do not undergo surface polishing treatments after machining, and therefore exhibit local stress concentrators and, consequently, areas of cracking and fractures. The effect of different surface conditions on the torsional strength of endodontic files were evaluated. 18 NiTi Profile® 25/.04 rotary files were examined by scanning electron. A group of 6 files (Group I) were not subjected to any chemical treatment, another group of 6 (Group II) were treated for 2 minutes using a solution of 8% Nitric Acid, 4% Flouridic Acid, and a further 6 (Group III) were treated with the same solution fot 2.5 minutes. All the file, with and without treatment, were loaded in a torsion test and fractography of the samples was undertaken by scanning electron microscopy. The variables investigated were, torque at fracture and maximum angle of rotation at fracture. The results obtained in these mechanical tests were subjected to a statistical analysis utilizing the T-Student test. It can be concluded from these results that there was a statistically significant difference between the maximum torque results for groups II and III, and between the maximum angle results for groups I and III.

The synthesis of in-situ bulk metallic glass composites (BMGCs) with crystals that undergo a martensitic transformation under loading is possibly the most effective method to improve the plasticity of metallic glasses at room temperature. These martensitic or shape memory BMGCs are typically fabricated via solidification of glass-forming melts, which requires the meticulous selection of the chemical composition and the proper choice of the processing parameters (particularly the cooling rate) in order to ensure that the glassy matrix coexists with the desired amount of austenitic phase having suitable morphology and characteristics. Unfortunately, a relatively limited number of alloy systems, where austenite and glassy matrix coexist over a wide range of compositions, is available. Additionally, the necessity for rapid heat extraction and the corresponding high cooling rates essential for glass formation by melt solidification set an inherent limit to the achievable dimensions of BMGs and BMGCs specimens. The aim of this thesis is to study the effectiveness of powder metallurgy as an alternative to solidification for the synthesis of shape memory BMGCs. Ni50.6Ti49.4 and Zr48Cu36Al8Ag8 metallic glass powders were selected as the constituents of the composites because they have been extensively investigated and represent well the characteristic behavior of metallic glass and shape memory phases. BMGCs with different volume fractions of NiTi phase were fabricated using pressure-assisted sintering via hot pressing and their microstructure, mechanical properties and deformation mechanism were investigated. Particular focus was placed upon identifying the individual contributions of the martensitic transformation and shear band formation to plasticity as well as their mutual interaction at different length scales using a multidisciplinary approach involving experiments and simulations. BMG composites were synthesized by hot pressing of powder mixtures consisting of Zr48Cu36Al8Ag8 metallic glass and different amounts of Ni50.6Ti49.4 particles (10, 20, 40 and 60 vol.%) using the optimized consolidation parameters (temperature-time-pressure) determined for the monolithic BMG. All composites are characterized by a relatively uniform particle distribution and good interface bonding without any sign of reaction between the metallic glass and NiTi. The NiTi particles are progressively less isolated with increasing volume fraction of NiTi up to 40 % and, for the BMGC with 60 vol.% NiTi, the glassy particles are no longer connected and the NiTi phase becomes the continuous matrix. This is not a trivial achievement as the change of matrix while maintaining the structure of the constituent phases would not be easily obtained by solidification of melts with such different compositions. The size of the samples (10 mm diameter and 9 - 11 mm height) is larger than the characteristic BMGCs synthesized by casting and can, in principle, be scaled up to larger dimensions, demonstrating the effectiveness of this approach for overcoming the size limitation inherent to glass formation via solidification. In contrast to the monolithic BMG, which does not show any sign of plasticity, the BMGCs exhibit macroscopic plastic deformation that progressively increases with increasing NiTi content along with distinct strain-hardening. The BMG composites have similar fracture strength, which is comparable with the monolithic BMG, and exhibit a distinct double yield behavior, similar to shape memory BMGCs fabricated by casting. The deformed BMGCs exhibit a high density of shear bands, again in agreement with what observed for similar BMGCs fabricated by casting. These findings not only demonstrate that BMGCs with tunable microstructures and thus with optimized deformability can be synthesized by pressure-assisted sintering but, thanks to the phase stability of the components across such a wide range of compositions, also offer an excellent platform to examine fundamental aspects in the field of martensitic BMGCs. The confining stress exerted by the surrounding glassy matrix was quantified at the macroscale via a hybrid Voigt-Reuss mixture, which considers intermediate weighted combinations of stiff and compliant behaviors. In this way, the macroscopic stress required to initiate the martensitic transformation from B2 to B19´ can be described with rather good accuracy. The confining effect was further investigated by in-situ high-energy X-ray diffraction to have access to the strain tensor of the B2 phase as a function of loading. The results indicate that the confining stress along the direction perpendicular to the loading axis is particularly strong because the expansion of the B2 phase is constrained by the elastic matrix. A mechanism responsible for shear band formation in shape memory BMGCs is proposed. The stress field generated by the martensitic transformation in the contiguous glass would activate the adjacent shear transformation zone (STZ, the elementary units of plasticity in BMGs). The stress field induced by the activated STZ in the surrounding material then triggers the activation of the following STZs along the path of a potential shear band, in an autocatalytic process resembling the domino effect. The shear band formed in this way propagates through the glassy phase and, when impinging a B2 particle, the associated stress field would locally trigger the martensitic transformation, starting again the process. Molecular dynamics (MD) simulations of a martensitic BMGC show that the structural perturbation generated by the martensitic transformation is indeed transmitted to the adjacent glassy matrix and, in turn, to the developing shear band, in agreement with the proposed mechanism. The individual contribution of the glassy phase to the residual strain after each loading-unloading cycle was quantified assuming that the NiTi phase behaves in the same manner across the different specimens. The glass contribution was then correlated to the shear band density to obtain the plastic strain resulting from shear banding for a given amount of NiTi phase, a quantity that could be effectively used in the design of plastically-deformable BMGCs with shape memory particles. The martensitic transformation in the composites becomes progressively more irreversible with increasing strain. A large contribution to the martensite stabilization may come from the residual stress induced by the shear bands, in accordance with the finite element method (FEM) simulations, showing that residual stresses in the composites suppress the reverse transformation after unloading. These finding corroborates the hypothesis that the residual elastic stress field generated by the shear bands may be fundamental for stabilizing the martensitic phase by restraining the atoms at the glass-crystal interface from rearranging back to form austenite. This process can be reversed by proper heat treatment. The findings presented in this thesis offer the opportunity to synthesize shape memory BMG composites with enhanced plasticity and strain-hardening capability along with larger dimensions than those typically achieved by solidification. The powder metallurgy approach provides the necessary versatility in materials design and resulting properties of the composites via the control over the fundamental microstructural features, such as volume fraction, size, morphology and distribution of the second phase. Additionally, materials processing in the solid state gives a virtually infinite choice among the possible composite components, a degree of freedom not usually given when processing via solidification.:Abstract iii Kurzfassung vii Motivation and objectives xi 1 Theoretical background and state-of-the-art 1 1.1 Bulk metallic glasses (BMGs) 1 1.1.1 Formation of metallic glasses 2 1.1.2 Mechanical properties of BMGs 5 1.1.3 Shear bands in metallic glasses 8 1.2 Bulk metallic glass matrix composites 19 1.2.1 Fabrication of BMG composites 20 1.2.2 In-situ BMG composites 27 1.2.3 Ex-situ BMG composites 43 2 Experiments and simulations 57 2.1 Sample preparation 57 2.1.1 Starting materials 57 2.1.2 Powder mixing 59 2.1.3 Powder consolidation 60 2.2 Materials characterization 61 2.2.1 Composition analysis 61 2.2.2 Laboratory X-ray diffraction 61 2.2.3 High-energy X-ray diffraction and strain analysis 62 2.2.4 Viscosity measurements 63 2.2.5 Differential scanning calorimetry 64 2.2.6 Density measurements 64 2.2.7 X-ray computed tomography 65 2.2.8 Optical microscopy and scanning electron microscopy 65 2.2.9 Transmission electron microscopy 66 2.2.10 Elastic constants measurements 66 2.2.11 Mechanical tests 67 2.3 Molecular dynamic simulations 67 2.4 Finite element simulations 68 3 Pressure-assisted sintering of single-phase Zr48Cu36Al8Ag8 metallic glass and Ni50.6Ti49.4 powders 73 3.1 Synthesis and properties of single-phase Zr48Cu36Al8Ag8 bulk metallic glass 73 3.2 Synthesis and properties of single-phase Ni50.6Ti49.4 shape memory alloy 80 4 Pressure-assisted sintering of BMG composites with shape memory crystals: Microstructure and mechanical properties 87 4.1 Microstructure of BMG composites 87 4.2 Effect of NiTi volume fraction on mechanical properties 90 4.3 Effect of confinement of the glassy phase on the martensitic transformation 95 5 Deformation mechanism of shape memory BMG composites 101 5.1 Martensitic transformation and shear band formation 101 5.2 Mechanism of shear band formation in shape memory BMG composites 107 6 Reversibility of the martensitic transformation in shape memory BMG composites 113 6.1 Martensite stabilization in NiTi alloy and BMG composites 113 6.2 Simulation of the martensite stabilization effect in BMG composites 119 6.3 Effect of heat treatment on the martensitic reverse transformation 121 7 Summary and outlook 125 References 131 Acknowledgements 155 Publications 157 Erklärung 159

This work is focused on study of mechanical properties of NiTi alloy which shows pseudoelastic and shape memory behaviour. Functional and structural fatigue of the material is examined. The main aim of this work was to perform and to evaluate a series of fatigue tests. The material was supplied in the form of wire which was gripped in the machine using special grips. In the first part of the experiment, tensile tests are evaluated and the reproducibility of measurements is demonstrated. Then, a series of cyclic tests was performed. Results were analysed together with previous measurements. One part of discussion concerned changes of the hysteresis loops during cycling and their dependence on strain rate. The fatigue life curves were plotted. It was found that these curves have non-standard shapes. The reasons for this are explained in the work.

Formgedächtnislegierungen wie Nickel-Titan (NiTi) können sich nach einer plastischen Verformung und anschließendem Aufheizen an ihre ursprüngliche Form „erinnern“ und diese wieder einnehmen. Als meistverwendete Formgedächtnislegierung kann NiTi als Aktor, zur Dämpfung und zur elastokalorischen Kühlen verwendet werden und kommt von der Medizintechnik bis hin zur Luft- und Raumfahrt zum Einsatz. Der Formgedächtniseffekt basiert auf der martensitischen Phasenumwandlung, einer diffusionslosen Strukturänderung, bei der sich die Kristallsymmetrie ändert. Bei NiTi mit etwa 50 At.-% Ni wandelt die kubische Hochtemperaturphase (Austenit) in die monokline Tieftemperaturphase (Martensit) um. Während dieser Umwandlung entsteht eine Vielzahl an Grenzflächen, wodurch sich ein komplexes martensitisches Gefüge – eine Art dreidimensionales „Puzzle“ bildet. Um NiTi-Formgedächtnislegierungen auf verschiedene Anwendungen zuzuschneiden und deren Eigenschaften zu verbessern, ist es wichtig, das Gefüge zu verstehen. Die häufig eingesetzten polykristallinen NiTi-Schichten haben dabei den Nachteil, dass die enthaltenen Korngrenzen einen zusätzlichen Parameter darstellen, der Gefügeuntersuchungen erschwert. Dagegen werden epitaktische Schichten bereits für andere magnetische Formgedächtnislegierungen als Modellsystem eingesetzt und tragen zu einem besseren Verständnis der martensitischen Umwandlung bei. Epitaktische Schichten sind einkristallin, sodass der Einfluss von Korngrenzen ausgeklammert werden kann. Außerdem dient das Substrat, das die Orientierung der Schicht vorgibt, als festes Referenzsystem. In dieser Arbeit wurden epitaktische NiTi-Schichten mit Magnetron-Sputterdeposition hergestellt, die bei Raumtemperatur martensitisch sind. Dabei wurde der Einfluss von Parametern wie Herstellungstemperatur, chemische Zusammensetzung, Wärmebehandlungsszenarien und Pufferschichten auf das Wachstum und die Eigenschaften der Schichten untersucht. So konnten Schichten in zwei unterschiedlichen Orientierungen, (100) und (111), hergestellt werden. Die so optimierten Schichten wurden anschließend dafür genutzt, das martensitische Gefüge skalenübergreifend zu untersuchen. Mit einer Kombination von Mikroskopie- und Röntgenbeugungsmethoden wurden die auftretenden Zwillingsgrenzen, Habitusebenen und Variantenorientierungen analysiert. So lässt sich feststellen, welche Martensitcluster entstehen, wie sie nukleieren und wachsen und welche Grenzflächen auftreten. Dabei ließ sich ein hierarchischer Aufbau des martensitischen Gefüges feststellen, wobei drei Zwillingsgrenzen auf unterschiedlichen Längenskalen für die Beschreibung des Gefüges nötig sind. Die auftretenden Zwillingsgrenzen sind aus Massivmaterialien bekannt, was zeigt, dass sich die Schichten gut als Modellsystem eignen. Das identifizierte, dreidimensionale Modell des Gefüges wurde mit Röntgenmethoden global bestätigt. Dazu wurden die experimentellen Ergebnisse mit zwei unterschiedlichen Martensittheorien, der phänomenologischen Martensittheorie (PTMC) und der Korrespondenztheorie (CT) verglichen. Der hierarchische Aufbau des Gefüges lässt sich zum Großteil mit den Theorien beschreiben. Die Schichten zeigen aber auch die Limitierungen der bisherigen Theorien und bieten so eine Möglichkeit für deren Weiterentwicklung.

New insight into the temperature dependent evolution of internal strain in the austenite phase during the martensitic phase transformation in NiTi shape memory alloys is provided via classical molecular dynamics simulations that employ well-established interatomic potentials for NiTi. It is shown, for the first time, that the developed strain tensor in the austenite phase is tetragonal in nature, with exponential temperature-dependence. Equally importantly, it is found that the developed internal strain (parallel to the habit plane) in the austenite varies linearly with the evolving martensite phase fraction. Interestingly, the Richard’s equation is found to describe the temperature dependence of the martensite phase fraction as well as the internal strain components parallel to the habit plane in the austenite phase. An analysis of the temperature dependent phonon dispersion of strained austenite revealed the competition between phonon softening of the TA2 branch and internal strain that leads to stabilization of the austenite phase in the two phase regime.

Thermally induced phase transformation in NiTi shape memory alloys (SMA) shows strong size and shape, collectively termed length scale effects, at the nano to micrometer scales, and that has important implications for the design and use of devices and structures at such scales. This paper, based on a recently developed multiscale model that utilizes molecular dynamics (MD) simulations at small scales and MD-verified phase field (PhF) simulations at larger scales, reports results on specific length scale effects, i.e. length scale effects in martensite phase fraction evolution, transformation temperatures (martensite and austenite start and finish) and in the thermally cyclic transformation between austenitic and martensitic phase. The multiscale study identifies saturation points for length scale effects and studies, for the first time, the length scale effect on the kinetics (i.e. developed internal strains) in the B19 phase during phase transformation. The major part of the work addresses small scale single crystals in specific orientations. However, the multiscale method is used in a unique and novel way to indirectly study length scale and grain size effects on evolution kinetics in polycrystalline NiTi, and to compare the simulation results to experiments. The interplay of the grain size and the length scale effect on the thermally induced martensite phase fraction (MPF) evolution is also shown in this present study. Finally, the multiscale coupling results are employed to improve phenomenological material models for NiTi SMA.

Martensitic phase transformation in NiTi shape memory alloys (SMA) occurs over a hierarchy of spatial scales, as evidenced from observed multiscale patterns of the martensitic phase fraction, which depend on the material microstructure and on the size of the SMA specimen. This paper presents a methodology for the multiscale tracking of the thermally induced martensitic phase transformation process in NiTi SMA. Fine scale stochastic phase field simulations are coupled to macroscale experimental measurements through the compound wavelet matrix method (CWM). A novel process for obtaining CWM fine scale wavelet coefficients is used that enhances the effectiveness of the method in transferring uncertainties from fine to coarse scales, and also ensures the preservation of spatial correlations in the phase fraction pattern. Size effects, well-documented in the literature, play an important role in designing the multiscale tracking methodology. Molecular dynamics (MD) simulations are employed to verify the phase field simulations in terms of different statistical measures and to demonstrate size effects at the nanometer scale. The effects of thermally induced martensite phase fraction uncertainties on the constitutive response of NiTi SMA is demonstrated.