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A 2014 study by the US Department of Energy conducted at Lawrence Berkeley National Laboratory estimated that U.S. data centers consumed 70 billion kWh of electricity[1]. This represents about 1.8% of the total U.S. electricity consumption. Putting this in perspective 70 billion kWh of electricity is the equivalent of roughly 8 big nuclear reactors, or around double the nation's solar panel output[2]. Developing new memory technologies capable of reducing this power consumption would be greatly beneficial as our demand for connectivity increases in the future. One newly emerging candidate for an information carrier in low power memory devices is the magnetic skyrmion. This magnetic texture is characterized by its specific non-trivial topology, giving it particle-like characteristics. Recent experimental work has shown that these skyrmions can be stabilized at room temperature and moved with extremely low electrical current densities. This rapidly developing field requires new measurement techniques capable of determining the topology of these textures at greater speed than previous approaches. In this dissertation, I give a brief introduction to the magnetic structures found in Fe/Gd multilayered systems. I then present newly developed techniques that streamline the analysis of Lorentz Transmission Electron Microscopy (LTEM) data. These techniques are then applied to further the understanding of the magnetic properties of these Fe/Gd based multilayered systems. This dissertation includes previously published and unpublished co-authored material.

Les nouvelles technologies numériques sont très avides en capacité de stockage, ainsi qu’en efficacité (rapidité et bas coût énergétique) de transport d’information. Les dispositifs d’aujourd’hui atteignant leurs limites, la recherche de nouvelles solutions de stockage est primordiale.L’utilisation de parois magnétiques comme brique élémentaire au codage de l’information a été proposée il y a quelques années, dans l’optique de réaliser un enregistrement tridimensionnel et ainsi d’augmenter considérablement les capacités de stockage.Depuis, un nouvel objet magnétique plus robuste et moins sensible aux perturbations extérieures a été découvert : le skyrmion. Il est récemment devenu un sujet d’étude très actif et a été observé expérimentalement dans deux types de systèmes. Le premier est basé sur les matériaux hélimagnétiques, dont la structure cristalline est non centrosymétrique. Le FeGe est l’un d’eux, avec la température de transition magnétique observée la plus élevée. Le skyrmion a également été observé à l’interface entre un métal lourd à fort couplage spin-orbite et un matériau ferromagnétique. En particulier, les systèmes de multicouches à interfaces non symétriques ont montré leur fort potentiel pour la manipulation de skyrmions à température ambiante.Les deux principales difficultés rencontrées aujourd’hui sont la réalisation de systèmes avec des techniques d’élaboration intégrables à des dispositifs industriels, ainsi que la détection fiable de la présence de skyrmions. Cette thèse est donc séparée en deux problématiques, appliquées aux deux types de systèmes. Un protocole de croissance de couches minces de FeGe hélimagnétique par pulvérisation cathodique a été développé en s’appuyant principalement sur des caractérisations structurales par diffraction de rayons X. L’élaboration de multicouches à interfaces non symétriques du type [métal lourd 1/matériau ferromagnétique/métal lourd 2]n a également été étudiée. Ces deux systèmes ont ensuite été caractérisés magnétiquement par diverses techniques basées sur de l’imagerie magnétique, des mesures de magnéto-transport et de la spectroscopie magnétique. / New technology needs huge storage capacity together with high speed and low-cost transport of information. Current devices meeting their limits, research on new storage solutions is needed.One of them, proposed a few years ago, consists in using magnetic domain walls. Aligning them in nanowires and using the thickness of the layers could enable the realization of a tridimensional recording device and then improve the storage capacity.A new object more robust and less sensitive to perturbations has been discovered since. Skyrmion is now widely studied. It has been experimentally observed in two kinds of systems. The first one is helimagnet, with non centrosymmetric crystal structure. FeGe is one of them, with the highest critical temperature observed yet. Skyrmion has been observed as well at the interface between a heavy metal with strong spin-orbit coupling and a ferromagnet. In particular, multilayers with non-symmetric interfaces are very promising systems for manipulation of skyrmions at room temperature.Nevertheless, the elaboration of systems for industrial devices and reliable detection of skyrmions is still challenging. These two problematics are explored in this thesis, applied to two different systems. A protocol to grow helimagnetic FeGe thin films was first established, thanks to structural characterization mainly based on X-ray diffraction. Growth of multilayers with non symmetrical interfaces [heavy metal 1/ferromagnet/heavy metal 2]n was studied as well. These systems were then magnetically characterized, using numerous techniques such as magnetic imaging, magneto transport measurements and magnetic spectroscopy.

Low-temperature magnetic force microscopy was used to study the phase diagram of a La1/3Pr1/3Ca1/3MnO3 thin film grown on a (110) NdGaO3 (NGO) substrate by pulsed laser deposition. Traditionally, one can observe the phase change at the nanoscale level as the sample is cooled from room temperature through the transition temperature to liquid nitrogen temperatures, but in this case a fixed voltage ranging from 0 V to 31 V was applied before each cooling cycle. From in and ex situ transport measurements, it is observed that the temperature of the peak of the transition increases with applied field; however, the MFM images show that the magnetic transition begins at a lower temperature with the same increase in field. Thus, this dissertation shows that a new voltage control exists for the phase transition in certain manganites. / text

State-of-the art Fourier transform holography (FTH) techniques use x-ray magnetic circular dichroism (XMCD) as a contrast mechanism for element-specfi c imaging of magnetic domains. With the soft x-ray Nanoscience beamline at Diamond Light Source in the UK, and the Dragon beamline at the European Synchrotron Radiation Facility (ESRF) in France, the possibility of new methods to study nanostructured magnetic systems has been demonstrated. The ability to record images without the use of lenses, in varying magnetic fi elds and with high spatial resolution down to 30 nm has been used to study in-plane magnetism of 50 nm thin permalloy (NiFe alloy) nanoelements. The holographic technique used extended reference objects rather than conventional pinhole references, which allowed a high flexibility on the direction of magnetisation that is probed. The element specific nature of the imaging, with the additional choice in the directions of magnetisation that are probed has been used to study dipolar interactions in a hard/Ta/soft [Co/Pt]30/Ta/Py multi-layered system. Images of the out-of-plane magnetised domains of [Co/Pt]30 were found to bare strong spatial resemblance to the in-plane domains of the permalloy. The domain structure is thought to be magnetostatically imprinted into permalloy during the growth stage of the lm, where stray elds generated by the adjacent Co/Pt multilayer influence the formation of domains in the permalloy. Strong resemblance between the two layers could be found at remanence within a pristine sample, however the similarities disappear after the sample was exposed to a saturating magnetic field. This disagreed with micromagnetic simulations performed in The Object Oriented MicroMagnetic Framework (OOMMF) program, and an explanation for the observations has been sought in the growth process of the multi-layered fi lm, with conditions that are diffi cult to recreate in the model. Optical holography has been used for preliminary insight into implementing a method of FTH in a reflective geometry at soft x-rays wavelength. With scattering chambers at BESSY II in Germany and at the Stanford Synchrotron Radiation Lightsource (SSRL) in California the possibility of reducing scattered noise in a hologram recorded in a reflective geometry has been investigated. Studies into specular and dif use reflections have been performed optically however the use of extended references alone may alleviate the current problem at x-ray wavelengths which lie in the weak signal given by a reflective point-like reference source.

Au cours de ces travaux de thèse, nous avons étudié par microscopie magnétique à émission d’électrons balistiques (BEMM) les propriétés de magnétotransport d’électrons chauds de la vanne de spin Fe/Au/Fe épitaxiée sur GaAs(001). Dans ces expériences, la pointe d’un microscope à effet tunnel (STM) injecte localement un courant d’électrons chauds à la surface de la vanne de spin. La mesure sous champ magnétique du courant d’électrons balistiques collecté à l’arrière de l’échantillon donne accès aux propriétés locales de magnétoconductance de l’échantillon. Nous avons dans un premier temps étudié les propriétés de magnétotransport de vannes de spin planaires. Les mesures BEMM démontrent un magnétocourant d’électrons chauds pouvant atteindre 500 % à température ambiante. Ces forts effets de magnétoconductance ne sont que très faiblement dépendants des épaisseurs des électrodes de fer et ne peuvent donc être dus à l’asymétrie en spin de la longueur d’atténuation des électrons chauds dans les couches de fer. Dans cette structure épitaxiée, la polarisation en spin du faisceau d’électrons chauds s’acquiert principalement aux interfaces via des effets de structure électronique. L’électron traversant les couches minces métalliques se propage comme un état de Bloch. Sa transmission aux différentes interfaces se fait en conservant d’une part la composante transverse k║ du vecteur d’onde électronique, et d’autre part, la symétrie de la fonction d’onde. Au-dessus de la barrière Schottky, les électrons chauds sont collectés dans la vallée Г du GaAs se projetant à l’interface dans la direction k║=0. Dans cette direction k║=0, la conservation de la symétrie de la fonction d’onde à l’interface Fe/Au conduit au filtrage des états de Bloch de symétrie Δ1 du fer. Ces états de symétrie Δ1, totalement polarisés en spin, sont responsables des forts magnétocourants d’électrons chauds observés. Cette analyse est confirmée expérimentalement par l’observation d’une corrélation entre amplitude du magnétocourant et masse effective du substrat semiconducteur. En augmentant la masse effective du semiconducteur, on ouvre le collimateur filtrant le courant d’électrons chauds autour de la direction k║=0, et le magnétocourant diminue sans modifier la vanne de spin. Dans un second temps, tirant partie de la résolution latérale du microscope et de sa sensibilité au magnétisme, des microstructures de fer préparées sous ultra-vide par évaporation à travers un masque (méthode du nanostencil) ont été étudiées. Dans ces structures, la modulation du courant collecté par la structure locale en domaines magnétiques a permis la réalisation d’images magnétiques avec une haute résolution spatiale. Les contrastes observés sur ces microstructures sont en excellent accord avec les images BEMM calculées à partir de simulations micromagnétiques ouvrant la voie à une microscopie magnétique quantitative à forte sensibilité et résolution latérale nanométrique. / During this thesis work, we studied by ballistic electron magnetic microscopy (BEMM) the hot electron magnetotransport properties of epitaxial Fe/Au/Fe/GaAs(001) heterostructures. In these experiments, hot electrons are injected from an STM tip through the metallic base. The measurement of the ballistic electron current collected at the back of the substrate under magnetic field gives access to the local magnetoconductance properties of the sample. The first part of this work consists in the study of a planar heterostructures. BEMM measurements on epitaxial Fe/Au/Fe/GaAs(001) samples demonstrate hot electron magnetocurrent as high as 500% at room temperature. This high magnetocurrent value is observed to be almost independent of the Fe layers thickness, and thus can not be explained by the spin asymmetry of the electron attenuation length in the iron layers. In this epitaxial heterostructure, the hot electron beam is mainly spin-polarized at the interfaces due to band structure effects. In the metallic thin films, electrons propagate as Bloch states. The electron wave function transmission at the interfaces should satisfy two selection rules: the transverse momentum (k║) of the electron wave vector and the symmetry of the electron wave function should be conserved. Above the Schottky barrier height, hot-electrons are collected in the Г valley of GaAs selecting thus only electrons with a transverse momentum (k║) close to zero. Among these k|| ≈ 0 states, conservation of the electron wave-function symmetry at the Fe/Au epitaxial interfaces additionally selects electrons with the Δ1 symmetry. These Δ1 states are fully spin-polarized and are responsible for the observed high magnetocurrent in these heterostructures. This analysis is experimentally confirmed by the observation of a correlation between the magnetocurrent value and the semiconductor effective mass. By increasing the semiconductor effective mass, we open the collimator which filters the electronic states around k║=0 and the magnetocurrent value decreases. To take advantage of the lateral resolution of the microscope and of its high sensitivity to magnetism, the second part of this work was devoted to the study of sub-micrometric iron structures prepared under UHV by evaporation through a nanostencil. In these structures, the modulation of the collected current by the local magnetic domain structure in the Fe dots allows magnetic imaging with a high spatial resolution. The experimental magnetocontrasts observed on these sub-micrometric Fe dots are in excellent agreement with BEMM current maps calculated from micromagnetic simulation results. This opens the way to a quantitative magnetic microscopy with high contrast and nanometric lateral resolution.

Le centre coloré azote-lacune du diamant, appelé centre NV, est comparable à un atome piégé à l’état solide. Ses propriétés de spin, conservées à température ambiante, permettent la détection de résonances magnétiques par voie purement optique. Le travail décrit dans cette thèse est centré sur l’utilisation d’ensembles de centres NV pour répondre à des problématiques à la fois scientifiques et industrielles. Nous avons réalisé un microscope de photoluminescence permettant d’exploiter les propriétés d’une couche nanométrique de centres NV. Les images obtenues ont une résolution spatiale de 500 nm et les fluctuations du signal sont limitées par le bruit de photons. En soumettant les centres NV à un signal hyperfréquence connu, nous pouvons reconstituer la cartographie à l’échelle microscopique des trois composantes d’espace d’un champ magnétique : par exemple, celui produit par un conducteur parcouru par un courant. La sensibilité associée à une surface d’intégration de 1 µm² de la couche de centres NV est de l’ordre du microtesla par racine de hertz. Notre dispositif d’imagerie permet également d’analyser le spectre d’un signal hyperfréquence. En soumettant les centres NV à un gradient de champ magnétique connu, l’information spectrale est transformée en information spatiale. Des résultats préliminaires montrent l’analyse simultanée d’une bande de fréquences de 700 MHz associée à une résolution de 7 MHz et à un taux de rafraîchissement de 4 ms. Ces travaux illustrent les perspectives prometteuses du centre NV du diamant, notamment pour le contrôle de circuits électroniques et l’analyse en temps réel de spectres hyperfréquences pris dans leur ensemble. / The nitrogen-vacancy color center of diamond, called NV center, is an atom like system trapped in a solid lattice. Its spin properties, kept at room temperature, allow the detection of magnetic resonances by purely optical means. The work described in this thesis is focused on the use of NV centers’ ensembles targeting both scientific and industrial issues. We realized a photoluminescence microscope that exploits the properties of a nanoscale layer of NV centers. The spatial resolution of the resulting image is around 500 nm and the fluctuations of the signal is limited by the shot-noise. When the NV centers are submitted to a microwave signal witch frequency is known, the cartography of the three spatial components of the magnetic field, the one produced by a conductor carrying a current for example, can be determined at the microscopic scale. The sensitivity associated to an integration surface on the NV center layer of 1 µm² is in the order of the microtesla per square root of hertz. Our imaging device also leads to the spectral analysis of a microwave signal. When the NV centers are submitted to a known magnetic field gradient, the spectral information is transformed into spatial information. Preliminary results show the simultaneous analysis of a 700 MHz frequency band associated to a resolution of 7 MHz and a refresh rate of 4 ms. These works illustrate promising perspectives for the NV center of diamond, especially for the control of electronic circuits and the real time analysis of a whole microwave spectrum.

L'auteur n'a pas fourni de résumé en français / The epitaxial growth condition and the superconducting properties of nanostructured devices made of rhenium (superconducting below T=1.7 K) on sapphire were explored. Epitaxial growth of rhenium thin films onto a single crystal α-Al2O3(001) substrate was realised using molecular beam epitaxy. The cleanness of the substrate was verified using XPS, and the growth of rhenium was monitored using RHEED. The orientations of the two crystals are (0001)Al2O3//(0001)Re and <2110>Al2O3//<0110>Re, which was confirmed using X-ray diffraction. The in-plane misfit between the lattices is -0.43% at room temperature, which allows us to estimate the critical thickness of rhenium to be between 10 nm and 15 nm.For deposition, rhenium was heated using an electron beam. Substrates were heated during growth using either a Joule-heated W filament located behind the sample or electron bombardment. Generally deposition temperatures of 800◦C and 900◦C gave reproducible results.The effect of deposition temperature was studied on samples that had the same thickness but were deposited at different temperatures. Three thickness groups were selected: 25 nm, 50 nm and 100 nm. Every sample was dominated by the (001) epitaxial orientation. Orientations (110), (100), (101) were present, but their intensities were small and decreased with increasing deposition temperature. AFM imaging was used to observe the morphology of the films. The 25 nm thick films were decorated with grains. The diameter of the grains (∼ 50 nm) did not vary significantly on the 25 nm thick sample, however, they became more uniform with increasing deposition temperature, and the surface became smoother. On the 50 nm and 100 nm thick films spirals and holes can be observed. Diameter of spirals on the 50 nm thick film increased from 100 nm to 500 nm when the temperature of the deposition was increased from 800◦C to 900◦C. XRD rocking curves measured on all samples got narrower with increasing deposition temperatures, indicating lower mosaicity of the (001) crystals. High-resolution θ-2θ scans evidenced a disorder in the 50 nm thick film, corresponding to strain values in the range of 0.01. Deposition temperature of 1000◦C lead to the dewetting of a 50 nm thick sample, islands with atomically flat surfaces were formed.The frequently observed spirals are most likely the result of screw dislocations. The origin of the holes that accompany the spirals is a dewetting process that starts when the thickness of the film reaches ~10 nm. We quantified the temperature evolution of the film during growth taking into account emission, reflection and transmission between all surfaces. This thermal model confirmed that the temperature of the film increases as the thickness of the rhenium film grows. The dewetting was studied using Mullins’ theory of thermal grooving. A surface diffusion coefficient of 4E−12 cm2/s was obtained, which is consistent with the observed dimensions of the surface topography.Wires with widths ranging from 100 nm to 3 μm and SQUIDs were fabricated from the rhenium films. Transport measurements confirmed that the lithography process does not affect the superconducting properties of rhenium. Critical temperatures between 1.43 K and 1.96 K were measured. We could correlate the superconducting transition temperature with the topography and the crystallinity of the films. Mean free path of electrons, and the superconducting coherence length were obtained, for two of the films both mean free path and effective coherence length were over 100 nm. These two films were in the clean limit, but the fabricated wires were in the dirty limit.On one film SQUIDs of 1 um diameter with 50 nm and 20 nm wide nanobridges acting as Josephson junctions were fabricated. The SQUIDs were cooled down using a dilution refrigerator. Critical current oscillations were measured. The flux noise values obtained were as low as 2.6E−5 Φ0/Hz1/2.

L'objectif de cette thèse a été d'étudier la dynamique de parois de domaines dans des couches minces magnétiques ayant anisotropie perpendiculaire, dans un empilement non-centrosymétrique. Dans ce type de système la compétition entre l'interaction d'échange de Heisenberg et un terme d'échange antisymétrique appelé interaction Dzyaloshinskii-Moriya interfaciale, favorise des textures magnétiques non colinéaires avec une chiralité définie, comme les parois de Néel chirales et les skyrmions. Dans ce travail nous nous sommes intéressés à la dynamique induite par un champ magnétique ou un courant électrique de parois Néel chirales dans une tricouches constituée d'une fine couche de cobalt déposée sur du platine, et recouverte par un oxyde.Nous avons démontré que la structure statique et la dynamique des parois est fortement impactée par la présence de la DMI. La DMI favorise une structure Néel avec une chiralité bien définie (plutôt que la structure de Bloch trouvé en général dans des systèmes symétriques). En comparant des parois dans Pt/Co/Pt (DMI=0) et Pt/Co/AlOx (DMI forte) nous avons montré que en la présence de DMI les parois de domaines peuvent être déplacées plus efficacement avec un champ magnétique. La stabilisation de la structure interne de la paroi par la DMI déplace le régime precessionnel à de plus hauts champs magnétiques et permet d'obtenir des vitesses importantes.En opposition à ce que prédisent les modèles 1D, nous montrons que en la présence de fort DMI la vitesse de paroi sature après le champ de Walker, et que la vitesse de saturation est proportionnelle au rapport entre la force de la DMI et l'aimantation à saturation (D/Ms). L'augmentation de la vitesse de saturation dans des systèmes avec faible Ms a été démontrée en comparant la dynamique de parois dans Pt/Co/GdOx et Pt/Co/Gd. Ceci implique aussi que en connaissant Ms, la mesure de la vitesse de saturation fournit une méthode originale pour quantifier l'interaction Dzyaloshinskii-Moriya interfaciale, comme nous montrons dans ce travail. Cette méthode a été utilisée pour mesurer la DMI dans des tricouches Pt/Co/AlOx avec oxydation variable de l'interface supérieure du Co. Nous montrons que en plus de la forte DMI de l'interface Pt/Co, l'interaction Co/oxyde contribue avec une DMI du même signe, la force de laquelle dépend du dégrée d'oxydation de l'interface. Nous observons aussi que cette DMI est proportionnelle à l'anisotropie magnétique perpendiculaire, ce qui suggère que les deux effets ont une origine commune. Pour finir, nous avons montré des résultats préliminaires de dynamique de parois induite par champ et courant dans des systèmes ferrimagnétiques GdCo. Si d'une part près de la compensation les parois de domaines dans des tricouches Pt/GdCo/Ta peuvent être déplacées seulement avec des champs très forts, d'autre part le courant est très efficace et les courants de dépiégeage très faibles. Nous avons attribué cet effet à la dépendance en 1/Ms du couple de spin-orbite qui agit sur l'aimantation. / The aim of this thesis has been to study domain wall dynamics in magnetic thin films with perpendicular magnetic anisotropy embedded in a non centrosymmetric stack. In this kind of system the competition between the symmetric Heisenberg exchange and an antisymmetric exchange term, called the interfacial Dzyaloshinskii-Moriya interaction (DMI), favours non collinear magnetic textures with a fixed chirality, like chiral Néel domain walls and skyrmions. In this work we have been interested in the field and current-driven dynamics of chiral Néel walls in trilayer stacks, typically consisting of a thin Co film deposited on Pt and capped with an oxide.We have shown that the statics and dynamics of a domain wall (DW) is strongly affected by the DMI. The DMI favours Néel internal structure (rather than the Bloch structure usually found in symmetric systems) with a fixed chirality. By comparing DWs in Pt/Co/Pt (no DMI) and Pt/Co/AlOx (strong DMI), we have shown that in the presence of DMI, DWs can be moved more efficiently by a magnetic field. The stabilization of the internal DW structure by the DMI allows the precessional regime to be pushed to large magnetic fields and large velocities to be reached.Opposite to what is predicted by 1D models we show that in the presence of DMI, the DW velocity saturates after the Walker field, and that the saturation velocity is proportional to the ratio of the DMI strength and the saturation magnetization (D/Ms). The enhancement of the saturation velocity in systems with reduced Ms is shown by comparing DW dynamics in Pt/Co/GdOx and Pt/Co/Gd stacks. This also means that, knowing Ms, measuring the DW saturation velocity provides an original method to quantify the interfacial Dzyaloshinskii-Moriya interaction, as we show in this work.This method has been used to measure the DMI interaction in Pt/Co/AlOx trilayers in which the top Co interface presents a varying degree of oxidation. We show that besides the strong DMI at the Pt/Co interface, the Co/oxide interface also provides a DMI contribution of the same sign, whose strength depends on the degree of oxidation of the Co/AlOx interface. We also observe that this DMI scales with the perpendicular magnetic anisotropy, which suggest a common origin for the two effects. Finally we have shown preliminary results of field- and current-driven dynamics of DWs in a ferrimagnetic system (GdCo). While close to the compensation composition domain walls in Pt/GdCo/Ta trilayers can be moved to high velocities only by very high magnetic fields, the current driven dynamics is very efficient and depinning currents low. This effect is attributed to the 1/ Ms dependence of the spin-orbit torque acting on the DW magnetization.