Cette thèse porte sur l’influence des transformations de phases solide-solide sur la propagation de fissure. On souhaite ainsi mieux comprendre les variations de ténacité en cours de soudage par exemple, ou bien pendant la réparation d’une fissure. Dans ce travail, la ténacité est obtenue à partir de l’intégrale J. Il existe de nombreuses méthodes expérimentales permettant d’obtenir la ténacité critique JIC mais qui sont difficilement applicables pour des essais se déroulant pendant une transformation de phase. C’est pourquoi nous avons proposé une méthode couplant essai mécanique et mesure par corrélation d’images avec de la simulation par éléments finis. Les essais sont réalisés sur de simples éprouvettes plates pré fissurées, faciles à usiner et simple à chauffer par induction. Les essais sont conduits pour différentes températures et jusqu’à rupture. En sus des mesures d’efforts et déplacements de traverse, la corrélation d’images nous fourni également les champs de déplacement sur chaque face de l’éprouvette. Chaque essai est ensuite simulé par éléments finis où la ténacité critique est calculée par la méthode G-Theta au maximum de la charge supportée par l’éprouvette. Les simulations précédentes intègrent les conditions aux limites obtenues par corrélation et le comportement mécanique considéré est celui que nous avons identifié sur des essais de caractérisation. Deux nuances de matériau ont été étudiées avec cette méthode ; l’acier inoxydale 15-5PH ainsi que l’acier ferritique 16MND5. Pour ces deux matériaux, différentes températures d’essai ont été choisies avant, pendant et après la transformation pour effectuer les essais de rupture ainsi que de caractérisation du comportement mécanique. Les résultats de cette étude montrent que la transformation de phase peut avoir un impact non négligeable sur la ténacité. Ainsi, pour le 15-5PH, le taux d’austénite résiduel est un facteur important et les essais pendant la transformation martensitiques montrent que la ténacité critique peut être inférieure pendant celle ci à celle du matériau purement austénitique. Dans le cas du 16MND5, la ténacité est beaucoup plus faible à 600°C (et bainitique) qu’à température ambiante ce qui est assez logique. Par contre, lors du refroidissement, depuis 600° (austénitique) jusqu’à la température ambiante (bainitique), nous avons obtenu une ténacité critique relativement constante. En conclusion, cette étude apporte une solution quant à la mesure de la ténacité critique de matériau pendant des transformations de phases, ce que ne permettent pas forcément les essais normalisés. Pour le 15-5PH, la ténacité critique semble évoluer pendant la transformation martensitique et est assez dépendante du taux d’austénite résiduelle. Il semble par contre que pour le 16MND5, la ténacité critique soit assez peu dépendante de la fraction volumique d’austénite et la valeur obtenue varie peu au cours du refroidissement du matériau depuis 600°C. / Ou study focuses on the effects of phase transformations on crack propagation. We want to understand the changes of fracture toughness during welding. In this work, fracture toughness is expressed by J-integral. There are many experimental methods to obtain the critical toughness JIC but they are impractical for our investigation during phase transformation. That is the reason why we have proposed a method coupling mechanical tests, digital image correlation and finite element simulation. The fracture tests are implemented on pre-cracked single edge notched plate sample which is easy for machining and heat conduct during phase transformation. The tests are conducted at different temperatures until rupture. Digital image correlation gives us the displacement information on every sample. Each test is then simulated by finite element where the fracture toughness is evaluated by the method G-Theta at the crack propagation starting moment found by potential drop method and digital image correlation technical. Two materials have been studied, 15Cr-5Ni martensitic precipitation hardening stainless steel and 16MND5 ferritic low carbon steel. For these two materials, different test temperatures were chosen before, during and after phase transformation for testing and failure characterization of the mechanical behavior. Investigation result shows that metallurgical phase transformation has an influence on fracture toughness and further crack propagation. For 15-5PH, the result of J1C shows that the as received 15-5PH has higher fracture toughness than the one at 200°C. The toughness is also higher than the original material after one cycle heat treatment probably due to some residual austenite. Meanwhile, pure austenite 15-5PH at 200°C has higher fracture toughness than pure martensitic 15-5PH at 200°C. For 16MND5, the result also proves that the phase transformation affects fracture toughness. The as received material has bigger J1C than the situation where it was heated to 600°C. On the other hand, the material at 600°C just before isothermal bainite transformation after the austenitization during cooling process also has higher fracture toughness than the one at 600°C before austenitization. These two conclusions are consistent well with the result of 15-5PH. But the final situation of 16MND5 after one cycle heat treatment has a slightly smaller J1C than the receiving situation. It means that one cycle heat treatment hasn't an significant influence on 16MND5fracture toughness. Conclusions show that one should pay attention to the heating period before austenitization of the substrate material when people do the welding as the higher temperature will bring the lower fracture toughness during this process. While during cooling period, the fracture toughness doesn't change a lot during, before or after the cooling induced phase transformation. Even for 15-5PH, it has a better fracture toughness after the martensite transformation than before.

<p align='justify'>This thesis is devoted to the micromechanical study of the size-dependent strengthening in Transformation Induced Plasticity (TRIP) steels. Such grades of advanced high-strength steels are compelling for the automotive industry, due to their improved mechanical properties. Among others, they combine a good strength versus ductility balance. In this context, many research works have been carried out to study these grades of steels. In particular, from a numerical point of view, earlier studies within the framework of classical plasticity do not properly reproduce the strengthening levels characterizing TRIP steels and obtained experimentally.</p> <p><p align='justify'>In this study, the strain gradient plasticity theory presented by Fleck and Hutchinson (2001) is chosen to account for the strengthening effect resulting from the phase transformation. A two-dimensional embedded cell model of a simplified microstructure composed of small cylindrical metastable austenitic inclusions, partially undergoing the phase transformation, within a ferritic matrix is used.</p><p><p align='justify'>First, the single-parameter version of the strain gradient plasticity theory under small strain assumption is used for the simulations. The impact of the higher order boundary conditions is assessed. It is shown that, when the plastic flow is unconstrained at the elasto-plastic boundaries, the transformation strain has no significant impact on the overall strengthening. The strengthening is essentially coming from the composite effect with a marked inclusion size effect resulting from the appearance during deformation of new boundaries (at the interface between parent and product phases) constraining the plastic flow.</p><p><p align='justify'>Second, the multi-parameter version of the strain gradient plasticity theory, incorporating separately the rotational and extensional gradients in the formulation, is employed under small strain assumption. The effect of the plastic strain gradients resulting from the transformation strain is better captured. In particular, the results show a significant influence of the shear component of the transformation strain. An implicit confinement effect is revealed at the elasto-plastic boundaries which is partly responsible for the transformation strain effect. Size effects on the overall strengthening are also revealed, due to a combined size dependent effect of the transformation strain and of the evolving composite structure.</p><p align='justify'>Third, the extension of the strain gradient plasticity theory to a finite strain description is applied. A significant effect of the transformation strain is obtained with the multi-parameter version of the theory as well as an optimal austenite grain size improving the damage resistance of the martensite, in agreement with the typical grain size of the current TRIP-assisted steels (Jacques et al. 2007).</p> / Doctorat en Sciences de l'ingénieur / info:eu-repo/semantics/nonPublished

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.

PhD thesis focuses the field of textile application of modern functional materials, namely metallic shape memory alloys with unique thermomechanical properties deriving from martensitic transformation in solid state. Particularly, it deals with the development of a nonconventional thermomechanical treatment of thin NiTi filaments via Joule heating by electric current and related basic research involving thermomechanical testing and modeling of functional properties of the filaments, investigation of martensitic transformations and deformation processes in NiTi and investigation of the fast recovery and recrystallization processes in metals heated by short pulses of controlled electric power. The method was developed and called FTMT-EC. In contrast to conventional heat treatment of metallic filaments in environmental furnaces, this method allows for precise control of the raise of the filament temperature and filament stress during the fast heating (rate ~50 000 °C/s). As a consequence, it is possible to precisely control the progress of the fast recovery and recrystallization processes in heat treated filaments. In this way it is possible to prepare filaments with desired nanostructured microstructure and related functional properties. A prototype equipment for application of the method for heat treatment of continuous SMA filaments during respooling in textile processing was designed and built. Comparing to the conventional heat treatment of SMA filaments in tubular environmental furnaces, this approach is faster, saves energy and allows for preparation of filaments with special functional properties. International patent application was filed on the method. It is currently utilized in the research and development of smart textiles for medical applications.

Η ανάπτυξη ευφυών υλικών, ή καλύτερα ευφυών συστημάτων, βασίζεται στην αξιοποίηση των λειτουργικών ιδιοτήτων μιας σειράς υλικών με κυριότερους εκπροσώπους τα υλικά με μνήμη σχήματος, τα ηλεκτρορεολογικά αιωρήματα και τα πιεζο/σιδηροηλεκτρικά στοιχεία. Το επιστημονικό και τεχνολογικό πεδίο των «ευφυών υλικών» επιχειρεί να αναπτύξει συστήματα υλικών των οποίων η επιτυχία δε θα βασίζεται στην εκπλήρωση πολύ υψηλών και σταθερών προδιαγραφών, αλλά στη δυνατότητα ελεγχόμενης μεταβολής της συμπεριφοράς τους. Η εργασία αυτή αναφέρεται σε κράματα με μνήμη σχήματος και στη μελέτη των συντελούμενων σε αυτά κρυσταλλογραφικών μετασχηματισμών, με τη μέθοδο της διαφορικής θερμιδομετρίας σάρωσης και τη μέθοδο της δυναμικής μηχανικής ανάλυσης. Στόχος της παρούσας εργασίας ήταν η μελέτη των μετασχηματισμών φάσεων προτανυσμένων συρμάτων SMA που είναι ενσωματωμένα στο εσωτερικό πολυμερικής μήτρας. Για λόγους αναφοράς εξετάσθηκε και η θερμική απόκριση των συνιστωσών υλικών. Το πρώτο μέρος της εργασίας προσφέρει μια βιβλιογραφική επισκόπηση του αντίστοιχου επιστημονικού πεδίου και το δεύτερο μέρος αναφέρεται στην πειραματική μελέτη του ίδιου θέματος. Στη συνέχεια δίνεται μια συνοπτική περιγραφή της διάρθρωσης της παρούσης εργασίας. Στο πρώτο κεφάλαιο γίνεται λόγος για τα ευφυή υλικά. Ως ευφυή υλικά αναφέρονται συστήματα που έχουν την ικανότητα να μεταβάλλουν τη συμπεριφορά τους ή ορισμένα χαρακτηριστικά τους (σχήμα, ιδιοσυχνότητα, συντελεστή απόσβεσης δονήσεων και άλλα) με δεδομένο και ελεγχόμενο τρόπο, εξ’ αιτίας μιας διέγερσης. Τα συστήματα αυτά ενσωματώνουν αισθητήρες και ενεργοποιητές, οι οποίοι συνδέονται μεταξύ τους με έναν κατάλληλο βρόχο ελέγχου. Στο ίδιο κεφάλαιο αναφέρονται τα υλικά που μπορούν να χρησιμοποιηθούν ως αισθητήρες και ενεργοποιητές και οι τύποι τους, τα είδη ελέγχου που έχουν επιτευχθεί, καθώς και εφαρμογές των ευφυών συστημάτων. Στο δεύτερο κεφάλαιο γίνεται αναφορά στα σύνθετα υλικά. Ως σύνθετο υλικό χαρακτηρίζεται ένα σύστημα δύο ή περισσότερων, διαφορετικών σε σύσταση και χημική δομή, υλικών τα οποία είναι φυσικά συνδεδεμένα μεταξύ τους. Τα σύνθετα υλικά αποτελούνται από μια συνεχή φάση, που λέγεται «μήτρα», ενισχυμένη με κάποιο υλικό που συνήθως αποκαλείται «ενισχυτικό ή πληρωτικό μέσο» και μια τρίτη φάση τη «διεπιφάνεια». Στο κεφάλαιο αυτό αναφέρονται οι κατηγορίες των σύνθετων υλικών, τα είδη μήτρας και εγκλεισμάτων, καθώς και τα χαρακτηριστικά της διεπιφάνειας. Στο τρίτο κεφάλαιο παρουσιάζονται τα ευφυή σύνθετα υλικά με ενσωματωμένα σύρματα με μνήμη σχήματος. Τα κράματα με μνήμη σχήματος εμφανίζουν την ικανότητα να μεταβάλλουν αντιστρεπτά ορισμένες φυσικές ιδιότητες του υλικού καθώς και το σχήμα τους. Εδώ αναλύεται ο ευθύς και αντίστροφος μαρτενσιτικός μετασχηματισμός, το φαινόμενο μνήμης σχήματος, τα κυριότερα κράματα μνήμης σχήματος που χρησιμοποιούνται και οι μηχανικές τους ιδιότητες, ενώ γίνεται αναφορά στις δυνατότητες και στους περιορισμούς των κραμάτων στις διάφορες εφαρμογές. Στο τέταρτο κεφάλαιο αναφέρονται τα υλικά που χρησιμοποιήθηκαν για την παρασκευή των ευφυών συστημάτων στην παρούσα εργασία. Αρχικά γίνεται λόγος για τη χημική δομή, τη θερμική κατεργασία και τις εφαρμογές εποξειδικών ρητινών. Στη συνέχεια αναφέρονται οι ίνες Kevlar® και αναλύεται η χημική δομή τους, τα είδη των ινών Kevlar® που υπάρχουν και οι εφαρμογές τους. Στο κεφάλαιο αυτό παρουσιάζονται και τα σύρματα με μνήμη σχήματος. Στο πέμπτο κεφάλαιο περιγράφεται ο τρόπος με τον οποίο παρασκευάστηκαν τα σύνθετα με ενσωματωμένα σύρματα με μνήμη σχήματος. Στο έκτο κεφάλαιο αναφέρονται οι πειραματικές τεχνικές που χρησιμοποιήθηκαν για τη μελέτη των δοκιμίων. Εδώ αναφέρονται σε συντομία γενικά στοιχεία για τη μέθοδο της διαφορικής θερμιδομετρίας σάρωσης (DSC) και για τη μέθοδο της δυναμικής μηχανικής ανάλυσης (DMA). Επίσης, περιγράφονται οι συσκευές της διαφορικής θερμιδομετρίας σάρωσης και της δυναμικής μηχανικής ανάλυσης που χρησιμοποιήθηκαν για τη μελέτη της θερμικής και μηχανικής απόκρισης των δοκιμίων. Στο έβδομο κεφάλαιο παρατίθενται τα πειραματικά αποτελέσματα για δοκίμια Ni-Ti, Ni-Ti-Cu με 6% σε Cu, Ni-Ti-Cu με 12% σε Cu και για σύνθετα δοκίμια NiTi με προτάνυση 3%, NiTiCu (6% Cu) με προτάνυση 2%, NiTiCu (12% Cu) με προτάνυση 3%, που μελετήθηκαν με τη διάταξη της διαφορικής θερμιδομετρίας σάρωσης (DSC). Επιπλέον, παρουσιάζονται τα πειραματικά αποτελέσματα για σύρματα Ni-Ti-Cu με 12% σε Cu και Ni-Ti, καθώς και για σύνθετα Ni-Ti-Cu (12% Cu) με 3% προτάνυση και για ρητίνη με ίνες Kevlar 29®, που μελετήθηκαν με διάταξη δυναμικής μηχανικής ανάλυσης (DMA). Στο επόμενο κεφάλαιο σχολιάζονται τα αποτελέσματα αυτά, ενώ στο τελευταίο κεφάλαιο αναφέρονται τα συμπεράσματα που προκύπτουν από τη μελέτη των αποτελεσμάτων. / Exploiting the functional properties of materials such as shape memory alloys, electrorheological suspensions and piezo/ferroelectric elements results in the development of smart materials or systems. In the scientific and technological field of smart materials the major achievement is not related to the values of specific physical properties but to the “adopted” ability to control their own behaviour. The subject of the present work concerns the crystallographic transformations of Shape Memory Alloys (SMA) under constrained conditions. The occurring transitions are studied experimentally by means of Differential Scanning Calorimetry (DSC) and Dynamic Mechanical Analysis (DMA). The first part of this work is a bibliographical review of the field, while the second one is the experimental study of the same subject. In the following lines, a short description, of the present thesis is given. The first chapter gives an introduction to smart materials. Composite systems, which under the influence of an external cause, can vary their behaviour or some characteristics (shape, natural vibration frequency, damping coefficient etc) in a specific and controllable way, are referred as smart materials. These systems incorporate sensors and actuators, which in turn are connected by a suitable control loop. Suitable materials for being employed as sensors and actuators, as well as the types of the, up to now, achieved control are also discussed. Chapter two covers briefly, fundamental aspects of composite materials. A system of two or more different, in composition and chemical structure, materials physically bonded between of them is characterised as a composite material. Composite materials are consisted from a continuous phase, often called “matrix”, and a discrete phase, called “reinforcing or filling phase”. Composite materials exhibit always a third phase, namely interface, between matrix and reinforcement. In this chapter the types of composites, matrices, fillers and the characteristics of interface are referred. Chapter three presents smart composite systems with embedded shape memory alloys (SMA). Shape memory alloys have the ability to change, reversibly, a number of characteristics, including their own shape. In this chapter direct and reverse martensitic transformation, shape memory effect, important shape memory alloys and their mechanical properties, as well as a short description of the manufacturing procedure of smart systems with embedded shape memory alloys, is presented. In the fourth chapter the employed materials for the production of the smart systems are discussed. The chemical structure, the curing procedure and the applications of epoxy resins are referred. Aramid fibres, such as Kevlar® fibres are also discussed, connecting their reinforcing role with their microstructure. Chapter five describes analytically the preparation procedure of the specimens. Next chapter describes the main characteristics of differential scanning calorimetry, dynamic mechanical analysis, as well and the devices used to study the thermal and mechanical response of the specimens. Chapters seven and eight present the experimental results of all the examined specimens and the resulting discussion respectively. Finally, concluding remarks and possible future work are included in chapter nine.

L’entraînement par application d’un champ externe s'est révélé être un moyen efficace d'améliorer la déformation induite par champ magnétique (Magnetic-Field-Induced Strain MFIS) dans les alliages Heusler de type Ni-Mn-Ga, en éliminant les variantes défavorables. Pour guider la procédure de l’entraînement, les mécanismes de l’entraînement des alliages à martensite 5M ou NM ont été étudiés, alors que ceux des alliages à martensite 7M ne sont pas entièrement clarifiés. Dans ce travail, les mécanismes de l’entraînement mécanique et thermomécanique ont été étudiés en analysant l'évolution de la microstructure et de l'orientation cristallographique au cours de ces processus. Tout d'abord, des caractérisations de microstructure et d'orientation cristallographique ont été réalisées dans l'état recuit sur l'alliage Ni50Mn30Ga20 préparé par solidification directionnelle. Cinq colonies transformées à partir d'un grain parent d'austénite ont été observées avec chaque colonie consistant en quatre variantes avec les relations d’orientation de Type-I, Type-II et composé transformation (TrF)-macle rapports. En supposant une charge de compression appliquée le long de la direction de solidification (SD), les cinq colonies pourraient être divisées en deux groupes par rapport au facteur de Schmid (Schmid Factor SF) des systèmes de démaclage de Type-I/Type-II TrF-macle des variantes dans la colonie : trois d'entre eux ont des SF élevés et désignés comme des colonies élevées de SF et les deux autres colonies de SF inférieurs. Ensuite, une compression unidirectionnelle a été effectuée sur l'alliage avec la charge appliquée le long de SD. En caractérisant l'évolution de la microstructure et le changement d'orientation cristallographique, les mécanismes de déformation ont été analysés. La déformation au stade précoce était principalement située dans certaines bandes initiées à partir des colonies de SF élevés et traversant les colonies de SF inférieurs. Le démaclage de Type-II/Type-I TrF-macle s'est produit principalement dans des colonies de SF élevés, ce qui a entraîné l'épaississement des variantes 7M favorables au détriment des variantes adjacentes. Les systèmes de maclage de Type-I/Type-II déformation (DeF)-macle et de réarrangement des variantes dans les colonies de SF inférieurs ont été activés, ce qui a entraîné la formation de nouvelles variantes 7M et NM. Les déformations correspondantes dans les colonies de SF inférieurs sont fortement coordonnées avec celles des colonies de SF élevés permettant la formation des bandes de déformation et l'accommodation de la déformation macroscopique. Au cours du stade avancé, le maclage de Type-I/Type-II DeF-macle et le réarrangement ont progressé pour coordonner la déformation macroscopique. Le processus de réarrangement inverse a été activé pour accommoder la déformation locale. Les nombres de colonies et de variantes sont considérablement réduits. Le chemin et le produit de la transformation martensitique ont également été fortement influencés par la déformation macroscopique imposée. Sous une petite charge, l'austénite transformée en martensite 5M suit à la fois l’OR Pitsch et une nouvelle OR plutôt que le martensite 7M auto-accommodée sous l’OR Pitsch. Avec l'augmentation de la charge appliquée, l'austénite s'est transformée presque simultanément en martensite 7M sous une nouvelle OR et en martensite 5M. Après la transformation martensitique, 5M s’est ensuite transformé en martensite 7M avec la diminution de la température sous la charge appliquée. La transformation martensitique a été modifiée par la contrainte externe en termes de produit de la transformation et de chemin de transformation pour accommoder la déformation macroscopique imposée. Ce travail offre de nouvelles idées sur les mécanismes de déformation des alliages Ni-Mn-Ga [...] / External field training is proven to be an effective way to improve the magnetic-field-induced strain (MFIS) in Ni-Mn-Ga Heusler type alloys by eliminating the unfavorable variants. To guide the training procedure, the training mechanisms of alloys with 5M or NM martensite have been investigated, whereas those for alloys with 7M martensite are not fully clarified. In this work, the mechanisms of mechanical and thermo-mechanical training were studied by analyzing the microstructure and crystallographic orientation evolution during these processes.Firstly, microstructure and crystallographic characterizations were performed on the as-annealed Ni50Mn30Ga20 alloy. 5 colonies transformed from one parent austenite grain were observed with each colony consisting of four variants with Type-I, Type-II and compound Transformation (TrF)-twin relations. By assuming an applied compressive load along the solidification direction (SD), 5 colonies could be divided into two groups with respect of the Schmid factor (SF) of detwinning systems of Type-I/Type-II TrF-twin of the in-colony variants: three of them have high SF and referred to as high SF colonies and the other two low SF colonies.Then unidirectional compression was performed on the alloy with the load applied along the SD. By characterizing the microstructure evolution and crystallographic orientation change, the deformation mechanisms were analyzed. The deformation in the early stage was mainly located in some band regions initiated from the high SF colonies and going through the low SF colonies. The detwinning of Type-II/Type-I TrF-twin occurred primarily in high SF colonies, resulting in the thickening of the favorable 7M variants at the expense of the adjacent variants. The twinning of Type-I/Type-II Deformation (DeF)-twin and shuffling systems of the variants in low SF colonies were activated, leading to the formation of new 7M variants and NM. The corresponding strains in the low SF colonies were highly coordinated with those in the high SF colonies allowing the formation of the deformation bands and the accommodation of the macroscopic strain. During the late stage, twinning of Type-I/Type-II DeF-twin and shuffling further progressed to coordinate the macroscopic strain. Reverse shuffling process was activated to accommodate the local deformation. The numbers of colony and variant were greatly reduced.The path and the product of martensitic transformation were also strongly affected by the imposed macroscopic deformation. Under a small load, austenite transformed to 5M martensite following both the Pitsch and a new OR rather than the self-accommodated 7M martensite under the Pitsch OR. With the increase of the applied load, austenite transformed almost simultaneously to 7M martensite under a new OR and 5M martensite. After the martensitic transformation, 5M further transformed to 7M martensite with the decrease of the temperature under the applied load. The martensitic transformation was modified by the external stress in terms of the transformation product and the transformation strain path to accommodate the imposed macroscopic deformation.This work offers new insights into the deformation mechanisms of the Ni-Mn-Ga alloys under unidirectional compression that are useful for the design of effective training procedures and provides new perspectives on further investigations of external field training on Ni-Mn-Ga alloys

Les alliages à base de Ni-Mn-In ont attiré une attention considérable en raison de leurs propriétés multifonctionnelles depuis leur découverte en 2004, telles que l’effet de mémoire de forme métamagnétique (Metamagnetic shape memory effect MMSME), l'effet magnétocalorique (MCE) et l'effet de magnétorésistance (MR). Cependant, certaines connaissances fondamentales sur ces alliages manquent toujours jusqu'à présent, telles que la structure cristalline de la martensite, les caractéristiques cristallographiques de microstructure et de transition magnétostructurale. Dans cette thèse, les caractéristiques cristallographiques, les comportements mécaniques et les propriétés magnétiques des alliages Ni-Mn-In base ont été étudiés théoriquement et expérimentalement. Tout d'abord, les structures cristallines des alliages Ni-Mn-In ont été déterminées avec précision par la méthode de Rietveld dans le cadre de la théorie du superespace. Ensuite, la microstructure de la martensite, notamment l'organisation et l'interface des variantes, ainsi que les caractéristiques cristallographiques de la transformation martensitique, telles que les relations d'orientation (OR), le chemin de déformation de la transformation et la compatibilité géométrique entre l'austénite et la martensite, ont été systématiquement étudiés. Enfin, avec cette connaissance fondamentale sur les alliages Ni-Mn-In, les comportements et les mécanismes de sélection /réarrangement des variantes de martensite sous deux types de stratégies de chargement mécanique, à savoir le chargement à l'état martensitique et le chargement durant la transition structurelle, et les effets du recuit sur l'effet MCE et les pertes d'hystérésis associées ont été explorées. Les principaux résultats sont les suivants. La martensite modulé a une structure cristalline incommensurable avec la structure cristalline 6M et le groupe de superespace I2/m(α0γ)00 qui peut être approximée par un modèle de superstructure de multiplicité 3 dans l'espace à tridimensionnel. La microstructure de martensite est en forme de plaques et auto-organisée en colonies. Chaque colonie a quatre variantes d'orientations distinctes. Le maximum de 6 colonies distinctes et 24 variantes peut être généré à l'intérieur d'un grain austénitique. Bien que jusqu'à 14 types de relations de maclage sont proposées dans le cadre des théories cristallographiques de transformation martensitique, seuls trois types de relations de maclage sont généralement observés, à savoir des macles de type I, type II et composées. Les interfaces des variantes sont définies à l'échelle mésoscopique par leur plan de maclage K1 correspondant. Cependant, à l'échelle atomique, la macle de type I a une interface cohérente, alors que celles de type-II et les macles composées ont des interfaces étagées. Les deux relations d'orientations K-S et Pitsch sont appropriés pour décrire la correspondance de réseau entre austénite et martensite dans les alliages Ni-Mn-In. Cependant, le chemin de déformation lié à la relation de Pitsch est mis en évidence pour être efficace pour la déformation de la structure. Avec le chemin de transformation déterminé, le mécanisme sous-jacent de l'organisation des variantes est révélé. À travers la transformation martensitique, en dépit de l'existence d'une relativement large couche contrainte (de l'ordre de 20 nm), le plan d'habitat est bordé par une variante de martensite simple avec l'austénite plutôt que la structure généralement observée "en sandwich", ce qui suggère une relativement bonne compatibilité géométrique entre les phases correspondantes. Pour le chargement en compression à l'état martensitique, l'arrangement des variantes est réalisé par des processus de démaclage. Il est démontré que l'état de variante unique dans certaines colonies pourrait être obtenu lorsque l'orientation de chargement est située dans la zone de Facteur de Schmid (SF) positif commune pour les trois systèmes de démaclage. [...] / Ni-Mn-In based alloys have attracted considerable attention due to their multifunctional properties since its discovery in 2004, such as metamagnetic shape memory effect (MMSME), magnetocaloric effect (MCE) and magnetoresistance (MR) effect. However, some fundenmental knowledge on these alloys is still missing until now, such as crystal structure of martensite, crystallographic features of microstructure and magnetostructural transition. In this dissertation, the crystallographic features, mechanical behaviors and magnetic properties of Ni-Mn-In based alloys were studied theoretically and experimentally. First, the crystal structures of Ni-Mn-In alloys were accurately determined by Rietveld method in the frame of superspace theory (Chapter 3). Then, the microstructure of martensite (Chapter 4), such as variant organization and interface structure, and the crystallographic features of martensitic transformation, such as orientation relationship (OR), transformation strain path and geometrical compatibility between austenite and martensite, were systematically studied (Chapter 5). Finally, with this fundamental knowledge on Ni-Mn-In alloys, the behaviors and mechanisms of martensite variant rearrangement/ selection under two kinds of mechanical loading strategies, i.e. loading at martensite state and loading across the structural transition, and the effects of annealing on MCE and its related hysteresis loss were explored (Chapter 6). The main results are as follows. The modulated martensite has an incommensurate 6M crystal structure with superspace group I2/m(α0γ)00 that can be approximated by a three-fold superstructure model in the three-dimensional space. The microstructure of martensite is in plate shape and self-organized in colonies. Each colony has four distinct orientation variants. The maximum of 6 distinct colonies and 24 variants can be generated within one austenite grain. Although as many as 14 kinds of twin relations are suggested in the frame of crystallographic theories of martensitic transformation, only three types of twin relations are generally detected, i.e. type-I, type-II and compound twin. Variant interfaces are defined by their corresponding twinning plane K1 at mesoscopic scale. However, at atomic scale, the type-I twin has a coherent interface, whereas type-II and compound twins have “stepped” interfaces. Both the K-S and Pitsch ORs are appropriate to describe the lattice correspondence between austenite and martensite in Ni-Mn-In alloys. However, the strain path related to the Pitsch relation is evidenced to be the effective for the structural distortion. With the determined transformation path, the underlying mechanism of variant organization is revealed. Across the martensitic transformation, despite the existence of a relative wide stressed layer (around 20 nm), the habit plane is bordered by single martensite variant with austenite rather than the generally observed “sandwich-like” structure, implying a relative good geometrical compatibility between the corresponding phases. For compressive loading at martensite, variant arrangement is realized by the detwinning process. It is evidenced that a single variant state in some colonies can be obtained when the loading orientation is located in the common positive Schmid factor (SF) zone of the three detwinning systems. For loading across the structural transition, the prestrain is obtained by variant selection in which the number of colonies is significantly reduced and the variant organization within colony is greatly changed. The SF for transformation strain path is introduced to evaluate the possible selection of variants. Heat treatment can significantly enhance the magnetic entropy change ΔSM but simultaneously increase the magnetic hysteresis loss. For ΔSM, the chemical ordered degree should play a prominent role [...]

Pseudoelastic NiTi shape memory alloys exhibit different stress–strain curves and modes of deformation in tension vs. compression. We have recently shown that under a combination of compression and shear, heterogeneous deformation can occur. In the present study, we use digital image correlation to systematically analyze how characteristic features of the nominally uniaxial engineering stress–strain curves (particularly the martensite nucleation peak and the plateau length) are affected by extensometer parameters in tension, compression, and the novel load case of shear-compression. By post-experimental analysis of full surface strain field data, the effect of the placement of various virtual extensometers at different locations (with respect to the nucleation site of martensite bands or inhomogeneously deforming regions) and with different gauge lengths is documented. By positioning an extensometer directly on the region corresponding to the nucleating martensite band, we, for the first time, directly record the strain-softening nature of the material—a specific softening behavior that is, for instance, important for the modeling community. Our results show that the stress–strain curves, which are often used as a basis for constitutive modeling, are affected considerably by the choice of extensometer, particularly under tensile loading, that leads to a distinct mode of localized deformation/transformation. Under compression-shear loading, inhomogeneous deformation (without lateral growth of martensite bands) is observed. The effects of extensometer gauge length are thus less pronounced than in tension, yet systematic—they are rationalized by considering the relative impact of differently deforming regions.

PhD thesis focuses the field of textile application of modern functional materials, namely metallic shape memory alloys with unique thermomechanical properties deriving from martensitic transformation in solid state. Particularly, it deals with the development of a nonconventional thermomechanical treatment of thin NiTi filaments via Joule heating by electric current and related basic research involving thermomechanical testing and modeling of functional properties of the filaments, investigation of martensitic transformations and deformation processes in NiTi and investigation of the fast recovery and recrystallization processes in metals heated by short pulses of controlled electric power. The method was developed and called FTMT-EC. In contrast to conventional heat treatment of metallic filaments in environmental furnaces, this method allows for precise control of the raise of the filament temperature and filament stress during the fast heating (rate ~50 000 °C/s). As a consequence, it is possible to precisely control the progress of the fast recovery and recrystallization processes in heat treated filaments. In this way it is possible to prepare filaments with desired nanostructured microstructure and related functional properties. A prototype equipment for application of the method for heat treatment of continuous SMA filaments during respooling in textile processing was designed and built. Comparing to the conventional heat treatment of SMA filaments in tubular environmental furnaces, this approach is faster, saves energy and allows for preparation of filaments with special functional properties. International patent application was filed on the method. It is currently utilized in the research and development of smart textiles for medical applications.

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