Ce travail a porté sur l'étude des phases métastables de l'alliage à mémoire de forme CuAlBe sous différents types de sollicitations mécaniques et thermiques par diffraction des neutrons. Il a permis de définir un protocole expérimental de caractérisation des transformations des phases métastables caractéristiques de l'effet mémoire de forme et de la superélasticité. Après élaboration par filage à chaud suivi d'une trempe à l'eau, le matériau est entièrement austénitique β1. Sa microstructure est composée de grains de taille relativement importante, de l'ordre de 400 µm. Ce procédé de fabrication génère une texture cristallographique de type fibre partielle <001>. L'étude de la superélasticité lors d'un essai de traction à température ambiante a mis en évidence le comportement pseudoélastique de l'alliage. L'étude de l'évolution des microdéformations a permis de mettre en avant la forte hétérogénéité de comportement du plan (400). Le pic de diffraction de ce plan présente également un fort élargissement dû aux fautes d'empilements qui est directement à relier à la transformation de phase de l'austénite en martensite. La martensite β'1 de structure monoclinique 18R complexe a été affinée à l'aide d'un modèle de type 6M. Ce modèle permet de rendre compte au mieux de la faible périodicité des fautes d'empilement caractéristiques de cette phase métastable à notre échelle d'analyse caractéristique d'un volume de l'ordre du centimètre cube. Après déformation plastique, la texture cristallographique du matériau a fortement évoluée. Le laminage à froid fait disparaitre la fibre partielle <001>. Aux plus forts taux de déformation plastique par laminage à chaud, la fibre <111> apparait. Cette forte déformation affecte également l'orientation des lattes de martensite. D'autre part, les températures des transformations de phases ainsi que l'hystérésis sont modifiées. Cependant, la structure cristallographique de la martensite générée par déformation plastique est identique à celle obtenue par refroidissement pour notre échelle d'observation. L'étude du retour à l'équilibre des phases métastables après recuit à haute température suivi d'une trempe sur un échantillon déformé plastiquement a montré la disparition totale de la martensite et l'apparition des phases stables α et γ2 pour des températures de recuit entre 500°C et 600°C. Au-delà de 600°C, ces deux phases disparaissent au profit de la phase β. On observe alors un fort grossissement du grain. La texture cristallographique est de nouveau caractérisée par la fibre partielle <001>. / This work deals with the study of metastable phases of CuAlBe shape memory alloy under mechanical and thermal solicitations by neutron diffraction. It enables to define an experimental protocol of characterization of metastable phase transformation.The raw material is fully austenitic at room temperature. Its microstructure is composed by huge grain size, close to 400 µm. The crystallographic texture is characterized by a <001> partial fibber.The study of the superelasticity during a tensile test at room temperature demonstrated the pseudoelastic behaviour of this material. The evolution of microdeformations showed the heterogeneous behaviour, especially for the (400) plane in axial direction. The diffraction peak of this plane family also has an important increase of the width. This increase can be linked to the transformation of the austenite into martensite.The crystallographic structure of the monoclinic martensite β'1 has been refined using the 6M model. This model enables to report the relatively low periodicity of stacking faults characterizing the martensitic transformation.After plastic deformation, the crystallographic texture evolved. The <001> partial fibber disappears. For the larger deformation rates, the <111> fibber appears.This large deformation also affects the martensite variant orientation and modifies the temperature of phase transformation.The return into equilibrium of metastable phases after annealing treatments between 500°C and 600°C followed by a quenching at room temperature on a plastically deformed sample has shown the disappearance of martensite and the growth of α and γ2 stable phases. Beyond 600°C, the grains grow largely. The crystallographic texture is characterized by the <001> partial fibber.

Orientador: Paulo Roberto Mei / Dissertação (mestrado) - Universidade Estadual de Campinas, Faculdade de Engenharia Mecânica / Made available in DSpace on 2018-08-18T15:15:33Z (GMT). No. of bitstreams: 1 Bueno_JulianaCristina_M.pdf: 6612143 bytes, checksum: ff1f20ccef9c00e4455c0b43362c43ce (MD5) Previous issue date: 2005 / Resumo: Neste trabalho foi estudada uma liga inoxidável Fe-Mn-Si-Cr-Ni-Co com efeito de memória de forma (EMF) e os objetivos principais foram otimizar a técnica de coloração por ataque químico (color etching) para identificação e análise das fases presentes na microestrutura, o que permitiu a determinação da dureza da martensita-? e da austenita-? através da técnica de nanoindentação. O desenvolvimento deste processo também permitiu a quantificação das fases e e g por microscopia óptica. A técnica de coloração por ataque químico consiste na utilização de reagentes específicos que resultam em uma microestrutura composta por várias colorações, o que permite identificar fases por microscopia óptica. Os resultados de dureza obtidos por nanoindentação foram de 7,0 GPa para a martensita-? e de 3,0 GPa para a austenita-?. Já para a fração volumétrica da martensita-?, os resultados obtidos por microscopia óptica variaram de 33 a 40 % para amostras no estado deformado. Para amostras de tamanho de grão 123 ?m e 3º ciclo de treinamento, os resultados foram coerentes com os obtidos por difração de raios X de trabalhos anteriores para a mesma liga / Abstract: In this work a Fe-Mn-Si-Cr-Ni-Co stainless alloy with shape memory effect (SME) was studied and the main objectives were to optimize the technique of coloration by chemical attack (color etching) for identification and analysis of the phases in the microstructure, allowing the determination of the ?-martensite and the -austenite hardness by nanoindentation technique. The development of this process also allowed the quantification of the ?- and ?- phases by optical microscopy. The technique of coloration by chemical attack consists in the use of specific reagents to identify phases by color using optic microscopy. The hardness obtained was 7.0 GPa for ?-martensite and 3.0 GPa for ?-austenite. The volume fraction of the ?-martensite, measured with optical microscopy varied from 33 to 40 % for samples in the deformed state. For samples with grain size of 123 ?m and after the 3º training cycle, the results were coherent with the obtained by X ray diffraction of previous works for the same alloy / Mestrado / Materiais e Processos de Fabricação / Mestre em Engenharia Mecânica

The martensite and magnetic transformations in Ni-Fe-Ga ferromagnetic shape memory alloys are very sensitive to both alloy chemistry and thermal history. A series of Ni-Fe-Ga alloys near the prototype Heusler composition (X2YZ) were fabricated and homogenized at 1423 °K, and a Ni₅₃Fe₁₉Ga₂₈ alloy was subsequently annealed at various temperatures below and above the B2/L21 ordering temperature. Calorimetry and magnetometry were employed to measure the martensite transformation temperatures and Curie temperatures. Compositional variations of only a few atomic percent result in martensite start temperatures and Curie temperatures that differ by about 230 °K degrees and 35 °K degrees, respectively. Various one-hour anneals of the Ni₅₃Fe₁₉Ga₂₈ alloy shift the martensite start temperature and the Curie temperature by almost 70 °K degrees. Transmission electron microscopy investigations were conducted on the annealed Ni₅₃Fe₁₉Ga₂₈ alloy. The considerable variations in the martensite and magnetic transformations in these alloys are discussed in terms of microstructural differences resulting from alloy chemistry and heat treatments. The phase-field method has been successfully employed during the past ten years to simulate a wide variety of microstructural evolution in materials. Phase-field computational models describe the microstructure of a material by using a set of field variables whose evolution is governed by thermodynamic functionals and kinetic continuum equations. A two dimensional phase-field model that demonstrates the ferromagnetic shape memory effect in Ni2MnGa is presented. Free energy functionals are based on the phase-field microelasticity and micromagnetic theories; they account for energy contributions from martensite variant boundaries, elastic strain, applied stress, magnetocrystalline anisotropy, magnetic domain walls, magnetostatic potential, and applied magnetic fields. The time-dependent Ginzburg-Landau and Landau-Lifshitz kinetic continuum equations are employed to track the microstructural and magnetic responses in ferromagnetic shape memory alloys to applied stress and magnetic fields. The model results show expected microstructural responses to these applied fields and could be potentially utilized to generate quantitative predictions of the ferromagnetic shape memory effect in these alloys. / Ph. D.

Shape Memory Alloys (SMA’s) are intermetallic materials (chemical compounds of two or more elements) that are able to sustain a residual deformation after the application of a large stress, but they “remember” the original shape to which they creep back, without the application of any external force, after they are heated above a certain critical temperature. A general one-dimensional dynamic mathematical model is presented which accounts for thermal coupling, time-dependent distributed and boundary inputs and internal variables. Well-posedness is obtained using an abstract formulation in an appropriate Hilbert space and explicit decay rates for the associated linear semigroup are derived. Numerical experiments using finite-dimensional approximations are performed for the case in which the thermodynamic potential is given in the Landau-Devonshire form. The sensitivity of the solutions with respect to the model parameters is studied. Finally, an alternative approach to the stress-strain laws is presented which is able to capture the dependence on the strain history. / Ph. D.

In this thesis, the thermomechanical approach with internal variables has been thoroughly analyzed. This approach is based on the combination of thermodynamic principles and continuum mechanics. Therefore it reflects the physical essence of constitutive behavior of materials. Based on this approach, a one-dimensional constitutive model for the two-way shape memory effect and a one-dimensional constitutive model for piezoceramics have been developed, respectively. In modeling the two-way shape memory effect, a residual stress σ_re is introduced as a controlling parameter for the two-way shape memory effect. A further refinement of the transformation kinetics expression for two-way shape memory is derived. It is demonstrated that the material parameters required by this model can be calculated or measured using a standard materials testing apparatus. A numerical study is conducted and the effectiveness of this model is verified. In the constitutive modeling of piezoceramics, a new internal state variable is introduced to relate the macroscopic behavior of a piezoceramic with its micro-properties. A phenomenological formulation of polarization reversal is proposed, and then a fully-coupled thermo-electro-mechanical model is developed. It is shown that the theory developed can describe the electromechanical behavior of piezoceramics well. / Master of Science

Les Alliages à Mémoire de Forme (AMF) sont des matériaux actifs ayant des propriétés mécaniques spectaculaires comparées aux autres métaux : effets mémoire simple et double sens, pseudo-élasticité et amortissement. Les propriétés des AMF ont pour origine physique une transformation austénite – martensite pilotée par la température et le niveau de contrainte dans le matériau. Les phases austénite (A) et martensite (M) sont présentes respectivement à haute température et à base température. L’effet mémoire, quant à lui, réside dans la capacité du matériau à retrouver la forme austénitique initiale par élévation de température, après avoir été déformé de manière permanente à l’état martensitique à basse température. Le comportement mécanique des structures en béton est gouverné par le processus d’endommagement du matériau. Ce processus peut être retardé en appliquant un chargement uni ou multi-axial de compression, dans le but de contrer les contraintes locales de traction auxquelles le béton est peu résistant. Cette thèse porte sur l’utilisation d’alliages à mémoire de forme (AMF) pour la création d’états de précontrainte dans des composants en béton. Le travail repose sur deux approches : expérimentation et modélisation. Dans la première partie, des essais préliminaires concernent l’étude du comportement thermomécanique de l’AMF en Ni-Ti. Cette réponse complexe est étudiée de manière séparée à l’aide d’une machine de traction – compression uni-axiale couplée à des moyens de chauffage et de refroidissement. Ensuite, des fils d’AMF sont utilisés pour la création de précontraintes dans des poutrelles et de confinements dans des cylindres en béton. Les fils sont étirés à l’état martensitique avant d’être fixés à leurs extrémités sur des éprouvettes en béton. L’activation thermique de l’effet mémoire provoque la mise en contrainte du béton. Et puis, des essais d’écrasement des cylindres sont réalisés pour estimer l’amélioration des performances du béton confiné à l’aide de fils d’AMF. Les résultats montrent que l’effet de confinement permet d’améliorer fortement la performance mécanique en compression du béton. Dans la deuxième partie, un modèle thermomécanique est élaboré pour l’analyse du comportement de fils d’AMF sollicités en traction-compression alternée uni-axiale. Une procédure de calcul numérique pas-à-pas est développé pour la simulation du comportement de fils en AMF pour l’ensemble de la procédure de création d’effet de précontrainte. Cette simulation donne une description fine des mécanismes au sein du fil au cours des essais sur des composants en béton-AMF. L’interaction complexe entre le béton et l’AMF est précisément analysée grâce à l’utilisation du modèle thermomécanique de l’AMF. Enfin, les études de cette thèse confirment une possibilité du champ d’application des AMF dans la thématique du renforcement préventif des structures en béton. / Shape memory alloys (SMAs) are active materials that exhibit special properties such as pseudoelasticity and memory effect. These properties are resulting from austenite vs. martensite reversible transformations governed by temperature and mechanical stress states. The austenite phase (A) and the martensite phase (M) are present respectively at high and low temperature. The shape memory effect is the ability of the material to retain a deformation gained in the martensite phase, i.e. at low temperature, and then to recover its initial shape when it returns to the austenite phase upon temperature increase. The mechanical behaviour of structural concrete is governed by a process of damage. The damaging process can be delayed by applying a uni- or multiaxial compression in order to counterbalance local tensile stresses in the material. The present thesis deals with the use of shape memory alloys (SMAs) to create prestress states in concrete components. The work is based on two approaches: experimental and modelling. In the first part, preliminary tests concern the studies of the thermomechanical behaviour of Ni-Ti SMA. This complex response is studied singly by means of a MTS uniaxial testing machine and heating-cooling systems. Then, SMA wires are used to create prestress states in small-scale concrete beams as well as confinement states in concrete cylinders. They were given a prestrain in a martensitic state before being firmly fixed on concrete components. Thermal activation of the memory effect in the SMA wires caused their tensioning, which resulted in reaction in the creation of stresses in the concrete. Moreover, crush tests of concrete cylinders are performed in order to estimate the improvement of the mechanical performance of concrete confined by means of SMA wires. The test results show that the confinement effect can improve strongly the mechanical performance of concrete. In the second part, a thermomechanical model is performed to analyze the behaviour of SMA with an extension to allow for uniaxial traction-compression. A steps by steps process of the numerical simulation is developed for SMAs during the process of prestress creation. This simulation gives a detailed description of the mechanisms of SMA wires which lead to the process of experimental studies on the SMAs-concrete components. A complex interaction between the concrete and the SMAs is evidenced by means of the thermomechanical model of SMAs. Finally, studies presented in the present thesis confirm the possibility to use SMA as preventive reinforcement for application to civil engineering structures.

Šiame baigiamajame magistro darbe apžvelgti atmenieji lydiniai, pagrindinės jų savybės bei panaudojimo pavyzdžiai, atlikta literatūros nagrinėjama tematika apžvalga, pagrindiniai šių medžiagų panaudojimo privalumai ir trūkumai. Atlikus literatūrinos apžvalgą, remiantis teoriniais duomenimis ir charakteristikomis, suplanuotas ir atliktas eksperimentas — siekiant geriau išsiaiškinti pagrindines šių lydinių savybes bei charakteristikas, kurios reikalingos norint šias medžiagas panaudoti robotiškos srityje - robotų vykdikliams. Eksperimentiškai gauti duomenys pateikiami grafikų pavidalu, iš kurių nustatytos pagrindinės charakteristikos, kurios reikalingos norint sėkmingai šias medžiagas panaudoti projektuojant įvairius mechanizmus ir pavaras su šio lydinio vykdikliais. Eksperimento metu gauti duomenys panaudojami sudarant sistemos dinaminį modelį, kuris sumodeliuojamas skaitmeniniu būdu. Gaunamas sistemos atsakas, kuris patvirtina eksperimento metu gautus duomenis ir suteikia galimybę tolesnius eksperimento plėtojimo planus ir tyrimus vykdyti skaitmeniniais metodais. / This final master thesis contains an overview of shape memory alloys, their literature review, main characteristics, common sage examples as well as their advantages and disadvantages. After analyzing the literature review the experiment has been planed and made in purpose of researching the most basic characteristics of shape memory alloys. The experiment was made with a shape memory alloy spring. The main purpose of the research is to get the most of the characteristics that are mostly needed for the successful usage in the robotic actuators. The data that was taken from the experiment in included in this paper. Acording to this data the conclusions has been made. Based on the experiment data and theoretical data the system’s dynamic model has been made to confirm the results that were taken from the experiment. This thesis allows to use the data taken from the experiment to be used in digital modeling, so further experimenting and system’s designing can be done using digital methods.

NiTi is the most commonly used shape memory alloy (SMA) and has been widely used for bio-medical, electrical and mechanical applications. Nickel rich NiTi shape memory alloys are coming into prominence due to their distinct superelasticity and shape memory properties as compared to near equi-atomic NiTi shape memory alloys. Besides, their lower density and higher work output than steels makes these alloys an excellent candidate for aerospace and automotive industry. Shape memory properties and phase transformation behavior of high Ni-rich Ni54Ti46 (at.%) polycrystals and Ni-rich Ni51Ti49 (at.%) single-crystals are determined. Their properties are sensitive to heat treatments that affect the phase transformation behavior of these alloys. Phase transformation properties and microstructure were investigated in aged Ni54Ti46 alloys with differential scanning calorimetry (DSC) and transmission electron microscopy (TEM) to reveal the precipitation characteristics and R-phase formation. It was found that Ni54Ti46 has the ability to exhibit perfect superelasticity under high stress levels (~2 GPa) with 4% total strain after 550°C-3h aging. Stress independent R-phase transformation was found to be responsible for the change in shape memory behavior with stress. The shape memory responses of [001], [011] and [111] oriented Ni51Ti49 single-crystals alloy were reported under compression to reveal the orientation dependence of their shape memory behavior. It has been found that transformation strain, temperatures and hysteresis, Classius-Clapeyron slopes, critical stress for plastic deformation are highly orientation dependent. The effects of precipitation formation and compressive loading at selected temperatures on the two-way shape memory effect (TWSME) properties of a [111]-oriented Ni51Ti49 shape memory alloy were revealed. Additionally, aligned Ni4Ti3 precipitates were formed in a single crystal of Ni51Ti49 alloy by aging under applied compression stress along the [111] direction. Formation of a single family of Ni4Ti3 precipitates were exhibited significant TWSME without any training or deformation. When the homogenized and aged specimens were loaded in martensite, positive TWSME was observed. After loading at high temperature in austenite, the homogenized specimen did not show TWSME while the aged specimen revealed negative TWSME.

Submitted by Caroline Periotto (carol@ufscar.br) on 2016-10-10T12:55:43Z No. of bitstreams: 1 DissJMS.pdf: 4383574 bytes, checksum: 04172fa81fb0f3d2e00439bbeaf3cbd4 (MD5) / Approved for entry into archive by Marina Freitas (marinapf@ufscar.br) on 2016-10-20T19:49:46Z (GMT) No. of bitstreams: 1 DissJMS.pdf: 4383574 bytes, checksum: 04172fa81fb0f3d2e00439bbeaf3cbd4 (MD5) / Approved for entry into archive by Marina Freitas (marinapf@ufscar.br) on 2016-10-20T19:49:51Z (GMT) No. of bitstreams: 1 DissJMS.pdf: 4383574 bytes, checksum: 04172fa81fb0f3d2e00439bbeaf3cbd4 (MD5) / Made available in DSpace on 2016-10-20T19:49:57Z (GMT). No. of bitstreams: 1 DissJMS.pdf: 4383574 bytes, checksum: 04172fa81fb0f3d2e00439bbeaf3cbd4 (MD5) Previous issue date: 2015-12-16 / Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES) / The aim of the present work was the study of the viability of a manufacturing route of parts with the Cu-based Shape Memory Alloy (SMA) Cu- 11,3Al-3,2Ni-3Mn-0,5Zr through gas atomization followed by Selective Laser Melting (SLM) consolidation. The alloy was prepared from high purity elements in an induction furnace with a concentrate argon flow shield above the molten metal. The atomization was carried out using an induction furnace for melting and argon as atomizer gas. The atomized powder was sieved in 32-106 μm range particles sizes and consolidated by SLM 250 HL device settled at the Leibniz Institute for Solid State and Materials Research, Dresden, Germany. In the consolidation step the best combination of power (P in Watts) and velocity (V in mm/s) were selected through the visual aspect criteria. In the following step the hatching track percentage (S) guided by relative density criteria was included. The atomized powder and the consolidated samples were characterized by optical and electron microscopy, X-ray diffraction and differential scanning calorimetry. The composition and the powder morphology were suitable for the SLM processing. The parameters optimization point out that the best combinations were P310v740S40 and P310v740S50, their relative density were around 97 %. The β’ “zig-zag” martensite phase, the SMA effect cause, was prevailing in the consolidated samples microstructure, still, the microstructure although was not-uniform it was relatively grain refined, pointing out the effect of Zr addition. The consolidated samples transformation temperatures were As=172-174C, Af=194-197C, Ms=156-160C, Mf=132- 138C. The results point to a strong indicative of the viability of a manufacturing route of parts with Cu-based SMA through gas atomization followed by SLM consolidation. / O objetivo da dissertação foi o estudo da viabilidade de uma rota de fabricação de peças com liga Cu-11,3Al-3,2Ni-3Mn-0,5Zr a base de cobre com Efeito de Memória de Forma (EMF) por atomização a gás da liga, seguida pela consolidação por Fusão Seletiva por Laser (FSL). A liga foi elaborada a partir de elementos de alta pureza em forno de indução com proteção de fluxo de argônio concentrado acima do banho. As atomizações foram realizadas com fusão por indução e utilizando argônio como gás de atomização. Os pós, separados na faixa granulométrica 32-106 μm foram consolidados por FSL utilizando o equipamento SLM 250 HL do Leibniz Institute for Solid State and Materials Research, Dresden, Alemanha. Para consolidação foram selecionadas as melhores combinações de potência (P em W) e velocidade (V em mm/s) do feixe de laser pelo critério de aspecto visual das trilhas simples. Na etapa seguinte foi considerada a porcentagem de sobreposição de pistas (S) avaliada pelo critério de densidade relativa. O pó atomizado e os corpos consolidados por FSL foram caracterizados por microscopia ótica e eletrônica de varredura, difração de raios-X e por calorimetria diferencial de varredura. A composição e a morfologia do pó atomizado foram adequadas para o processo de FSL. A otimização dos parâmetros de processamento indicaram que as melhores combinações foram de P310v740S40 e P310v740S50, com densidade relativa alcançada em torno de 97%. A fase martensítica β’ “zigzag”, responsável pelo EMF, foi predominante nos corpos consolidados por FSL sendo que a microestrutura, embora não uniforme, foi relativamente refinada, indicando o efeito da adição de Zr na composição da liga. As temperaturas de transformação dos corpos consolidados foram de As=172- 174C, Af=194-197C, Ms=156-160C, Mf=132-138C. Os resultados indicam a viabilidade da rota de fabricação de peças em ligas a base de cobre com EMF por atomização a gás da liga, seguida pela consolidação por FSL.

Title: Martensite microstructures in thin films and monocrystals of Heusler alloys Ni-Mn-Ga Author: Kristýna Onderková Department: Department of Surface and Plasma Science Supervisor: Mgr. Ing. Oleg Heczko, Dr., Institute of Physics of the Czech Academy of Sciences Abstract: The submitted thesis examines mainly the first thin films from Ni-Mn-Ga Heusler alloy prepared by magnetron sputtering on the new equipment at Institute of Physics of Charles University. However, the work also analysed the thin films prepared in IFW Dresden and bulk material. The main focus of the work is primarily on the martensitic microstructures, because of the significant effect that their twin boundaries have on the magnetic shape memory phenomena. Microscopic techniques used for the research were mainly Scanning Electron Microscopy (SEM), but also Transmission Electron Microscopy (TEM) and Atomic Force Microscopy (AFM). As the Ni-Mn-Ga properties are stronly dependent on chemical composition, the composition was evaluated by two different methods (Electron Dispersive X-ray Spectroscopy and X-ray Fluorescence) and observed differences discussed. Finally the results were compared with X-ray diffraction (XRD) measurements and the films were further characterised by magnetic measurements using Vibrating Sample Magnetometer (VSM)....