La thèse résulte d'une collaboration entre le laboratoire académique G2Elab et les entreprises Aperam Amilly et Aperam Imphy.Les matériaux magnétiques nanocristallins de type Finemet sont constitués d'une phase nanocristalline et d'une phase amorphe. Cette structure singulière leur confère des anisotropies magnéto-cristalline et magnéto-élastique évanescentes. On peut alors induire, par le biais de recuits adaptés, une anisotropie contrôlée conditionnant la forme du cycle d’Hystérésis et la perméabilité. D’un point de vue applicatif, il s’agit d’une aptitude capitale puisque les caractéristiques du circuit magnétique peuvent être adaptées pour répondre à des cahiers des charges spécifiques. La mise au point des protocoles de recuit mis en œuvre industriellement est cependant empirique.Le sujet de la thèse porte donc sur la mise au point d'un modèle capable de prédire l'amplitude K_u de l'anisotropie induite sur ces matériaux en fonction des paramètres du recuit sous champ (température T_re, champ appliqué H_re) et des caractéristiques structurales (fraction cristalline f_c, taille moyenne D des nanograins, composition y de la phase cristalline Fe1-ySiy). / This thesis is the result of a collaboration between Grenoble Electrical Engineering laboratory, Aperam Alloys Amilly and Aperam Alloys Imphy manufactories.The magnetic materials nanocrystalline Finemet are made of Fe-Si nanocrystallites embedded in a residual amorphous phase. This unconventional crystallographic structure features vanishing magnetocristalline and magnetoelastic anisotropies. As a result, it is possible to induce a cohenrent magnetic anisotropy in such material by suitable annealing treatments, allowing to control the shape of the hysteretic loop and permeability. In view of applications in electronic devices, this attract a great interest, the magnetic circuit characteristics being could be easily adapted by this way to satisfy the requirement of the regarded sensor or actuator.However, the optimization of annealing parameters (temperature, duration, amplitude of applied field…) to fit the desired properties is focused on time and resources consuming, which are based on empirical experience at present.As a result, the aim of this work is to build a model which will be able to predict the magnitude of induced anisotropy according to the field annealing parameters and the structural ones (crystalline fraction f_c, size of nanograins D, and composition of FeSi phase).

Many modern technologies are enabled by the use of thin films and/or nanostructured composite materials. For example, many thermoelectric devices, solar cells, power electronics, thermal barrier coatings, and hard disk drives contain nanostructured materials where the thermal conductivity of the material is a critical parameter for the device performance. At the nanoscale, the mean free path and wavelength of heat carriers may become comparable to or smaller than the size of a nanostructured material and/or device. For nanostructured materials made from semiconductors and insulators, the additional phonon scattering mechanisms associated with the high density of interfaces and boundaries introduces additional resistances that can significantly change the thermal conductivity of the material as compared to a macroscale counterpart. Thus, better understanding and control of nanoscale heat conduction in solids is important scientifically and for the engineering applications mentioned above. In this dissertation, I discuss my work in two areas dealing with nanoscale thermal transport: (1) I describe my development and advancement of important thermal characterization tools for measurements of thermal and thermoelectric properties of a variety of materials from thin films to nanostructured bulk systems, and (2) I discuss my measurements on several materials systems done with these characterization tools. First, I describe the development, assembly, and modification of a time-domain thermoreflectance (TDTR) system that we use to measure the thermal conductivity and the interface thermal conductance of a variety of samples including nanocrystalline alloys of Ni-Fe and Co-P, bulk metallic glasses, and other thin films. Next, a unique thermoelectric measurement system was designed and assembled for measurements of electrical resistivity and thermopower of thermoelectric materials in the temperature range of 20 to 350 °C. Finally, a commercial Anter Flashline 3000 thermal diffusivity measurement system is used to measure the thermal diffusivitiy and heat capacity of bulk materials at high temperatures. With regards to the specific experiments, I examine the thermal conductivity and interface thermal conductance of two different types of nanocrystalline metallic alloys of nickel-iron and cobalt-phosphorus. I find that the thermal conductivity of the nanocrystalline alloys is reduced by a factor of approximately two from the thermal conductivity measured on metallic alloys with larger grain sizes. With subsequent molecular dynamics simulations performed by a collaborator, and my own electrical conductivity measurements, we determine that this strong reduction in thermal conductivity is the result of increased electron scattering at the grain boundaries, and that the phonon component of the thermal conductivity is largely unchanged by the grain boundaries. We also examine four complex bulk metallic glass (BMG) materials with compositions of Zr₅₀Cu₄₀Al₁₀, Cu_46.25Zr_44.25Al_7.5Er₂, Fe₄₈Cr₁₅Mo₁₄C₁₅B₆Er₂, and Ti_41.5Zr_2.5Hf₅Cu_42.5Ni_7.5Si₁. From these measurements, I find that the addition of even a small percentage of heavy atoms (i.e. Hf and Er) into complex disordered BMG structures can create a significant reduction in the phonon thermal conductivity of these materials. This work also indicates that the addition of these heavy atoms does not disrupt electron transport to the degree with which thermal transport is reduced. / Ph. D.

La thèse s'inscrit dans le cadre du projet GENOME « Gestion Optimisée de l'Energie » dont l'enjeu majeur est la conception d'un avion plus électrique. L'augmentation de l'efficacité énergétique et de la compacité des systèmes électriques de ces avions entraîne de fortes sollicitations en température. Ces sollicitations sont liées à la compacité des systèmes (réduction de masse et de volume) ainsi qu'à leur localisation par rapport aux sources chaudes (réacteur d'avion par exemple). De ce fait, les matériaux magnétiques des nouveaux convertisseurs électriques doivent pouvoir fonctionner sous des conditions de hautes températures, supérieures à 200°C. Il s'agit du polycristallin FeCoV dédié à la fabrication des tôles du stator et du rotor des génératrices rapides (situées à proximité des réacteurs) et le nanocristallin FeCuNuSiB dédié à la conception des inductances et transformateurs des convertisseurs statiques. Ce manuscrit s'intéresse à l'étude du vieillissement thermique de ces deux familles de matériaux magnétiques. Ces matériaux, fournis par la société APERAM, se déclinent sous plusieurs nuances et finitions. L'étude du vieillissement consiste en l'application de plusieurs essais de vieillissement continus sous différentes températures (jusqu'à 300 °C pour les FeCoV et 240 °C pour les nanocristallins). Plusieurs grandeurs macroscopiques magnétiques, électriques et mécaniques (pour les FeCoV) sont mesurées à chaque intervalle de vieillissement. Grâce à ces mesures macroscopiques et à des mesures complémentaires effectuées à l'échelle microscopique, des analyses sont faites et des hypothèses sont proposées afin d'expliquer les mécanismes de vieillissement de ces deux familles de matériaux et dans le but de proposer des modèles phénoménologiques fiables / The thesis takes part of the project GENOME “Gestion Optimisée de l’Energie” whose major issue is the design of the more electrical aircraft. The increase in the energy efficiency and the compactness of the electrical systems of these aircrafts lead to high temperature stresses. These thermal stresses are related to the compactness of the systems (reduction of mass and volume) as well as their location with respect to the hot sources (aircraft engine for example). Thus, the magnetic materials of the new electrical converters must be able to operate under conditions of high temperatures, above 200 °C. Typically, the FeCoV polycrystalline materials are dedicated to the fabrication of the stator and rotor sheets of the fast generators (located near the aircraft engine) and the FeCuNbSiB nanocrystalline materials are dedicated to the design of inductors and transformers of the static converters.This manuscript concerns the thermal ageing study of these two magnetic material families. These materials, supplied by the company APERAM, are available in several shades. The ageing study consists on applying several continuous ageing treatments at different temperatures (up to 300 °C for FeCoV and 240 °C for FeCuNbSiB). At each ageing step, several macroscopic properties namely: magnetic, electrical and mechanical (for the FeCoV materials) properties are measured. Using these macroscopic properties and complementary measurements carried out on a microscopic scale, analyses are made and hypotheses are proposed in order to explain the ageing mechanisms of these magnetic material families. The understanding of the magnetic ageing mechanisms is necessary towards establishing of phenomenological ageing models

Plastic deformation of metals and alloys are invariably accompanied by the development of texture. The origin of texture is attributed to the deformation micro-mechanisms associated with processing. The face-centered cubic (FCC) metals and alloys are known to exhibit two distinct types of textures when subjected to large strain rolling deformation, namely, (i) Cu-type texture, commonly seen in high/medium stacking fault energy (SFE) materials, (ii) Bs-type texture in low SFE materials. The circumstances that could result in the formation of Bs-type texture in low SFE materials still remains an open question and no definite mechanism has been uniquely agreed upon. Apart from the SFE, grain size could also influence the deformation mechanism and hence the deformation texture. It is well known that in materials with grain sizes less than 100 nm (referred to as nano-crystalline materials), the microstructures contain large fraction of grain boundaries. This subsequently introduces a variety of deformation mechanisms in the microstructure involving grain boundary-mediated processes such as grain boundary sliding and grain rotation, in addition to slip and twinning. A clear understanding of texture evolution in nano-crystalline materials, particularly at large strains, is a topic that remains largely unexplored. The present work is an attempt to address the aforementioned issues pertaining to the evolution of deformation texture, namely, (i) the effect of SFE and (ii) the effect of grain size, in FCC metals and alloys. Nickel-cobalt alloys are chosen as the model system for the present investigation. The addition of cobalt to nickel leads to a systematic reduction of SFE as a function of cobalt content. In this thesis, three alloys of Ni-Co system have been considered, namely, nickel – 20 wt.% cobalt, nickel – 40 wt.% cobalt and nickel – 60 wt.% cobalt. For a comparison, pure nickel has also been subjected to similar study. Chapter 1 of the thesis presents a detailed survey of literature pertaining to the evolution of rolling textures in FCC metals and alloys, and chapter 2 includes the details of the experimental techniques and characterization procedures, which are commonly employed for the entire work. Chapter 3 addresses the effect of stacking fault energy on the evolution of rolling texture. The materials subjected to study in this chapter are microcrystalline Ni-Co alloys. The texture evolution in Ni-20Co is very similar to pure Ni, and a characteristic Cu-type rolling texture is observed. The evolution of texture in these materials is primarily attributed to the intense dislocation activity throughout the deformation stages. In Ni-40Co, a medium SFE material, the rolling texture was predominantly Cu-type up to a strain of ε = 3 (95% thickness reduction). However, beyond this strain level, namely at ε = 4 (98%), the texture gets transformed to Bs-type with orientations maxima predominantly close to Goss ({110} <001>) position. Simultaneously, the Cu component which was dominant until 95% reduction has completely disappeared. The analysis of microstructures indicate that deformation is mostly accommodated by dislocation slip up to 95%, however, at ε > 3, Cu-type shear bands get initiated, preferably in the Cu-oriented ({112} <111>) grains. The sub-grains within the shear bands show preferred orientation towards Goss, which indicates that the Cu component should have undergone transformation and resulted in high fraction of Goss component. In Ni-60Co alloy, Bs-type texture forms in the early stages of deformation (ε ~ 0.5) itself and further deformation results in strengthening of the texture with an important difference that the maximum in orientation distribution has been observed at a location close to Goss component, rather than at exact Bs-location. The development of Bs-type texture is accompanied by the complete absence of Cu and S components. Extensive EBSD analyses show that the deformation twinning gets initiated beyond 10% reduction and was found extensively in most of the grains up to 50% reduction. At higher strains, tendency for twinning ceases and extensive shear banding is observed. A non-random distribution of orientations close to Goss orientation was found within the shear bands. The near-Goss component in the Ni-60Co alloy can be explained on the basis of deformation twinning and shear banding. Thus, a reasonable understanding of the deformation texture transition in the extreme SFE range has been developed. In chapter 4, the effect of fine grain size on the evolution of rolling texture has been addressed. Nanocrystalline (nc) nickel-cobalt alloys with a mean grain size of ~20 nm have been prepared by pulse electro-deposition method. For a comparison, nc Nickel (without cobalt) with similar grain size has also been deposited. For all the materials, a weakening of the initial fiber texture is observed in the early stage of room temperature rolling (ε ~ 0.22). A combination of equiaxed grain microstructure and texture weakening suggests grain boundary sliding as an operative mechanism in the early stage of rolling. At large strain (ε = 1.2), Ni-20Co develops a Cu-type texture with high fractions of S and Cu components, similar to pure Ni. The texture evolution in Ni-40Co and Ni-60Co alloys is more towards Bs-type. However, the texture maximum occurs at a location 10° away from the Goss. The evolution of Cu and S components in nc Ni-60Co alloy takes place simultaneously along with the α-fiber components during rolling. Microstructural investigation by TEM indicates deformation twinning to be more active in all the materials up to 40% reduction. However, no correlation could be drawn between the texture evolution and the density of twins. The deformation of nc Ni-20Co alloy, is also accompanied by significant grain growth at all the stages of rolling. The increase in grain size, subsequently, renders the texture to be of Cu-type. However, Ni-40Co and Ni-60Co alloys show high grain stability. The absence of strain heterogeneities such as shear bands, and the lack of significant fraction of deformation twins indicate that the observed Bs-type texture could be due to planar slip. The increase in deformation beyond 70% reduction caused a modest reduction in the intensity of deformation texture. The microstructural observation indicates the occurrence of restoration mechanisms such as recovery/ recrystallization at large strains. The overall findings of the investigation have been summarized in chapter 5. The deformation mechanism maps relating stacking fault energy with amount of strain and with grain size are proposed for micro- and nano- crystalline materials respectively.