The diploma thesis deals with the switching of spin vortices in magnetic nanodisks. First, the basic concepts of (micro)magnetism are defined and existing theoretical and experimental achievements in the field of switching of the two basic characteristics (chirality and polarity) of magnetic vortex are summarized. Then the principle of dynamic switching of magnetic vortex chirality using in-plane magnetic field pulse with a well defined amplitude and duration is presented. There is no need to use a certain shape of nanodisks or asymmetry in magnetic field distribution. Nanostructures were prepared by the multi-step electron beam lithography and ion beam sputtering. Individual steps of sample preparation and optimization for the magnetization dynamics measurements are described. Finally, the experimental measurements of the dynamic switching of chirality on prepared samples obtained by transmission x-ray microscopy at the synchrotron Advanced Light Source at Berkeley, USA are presented and discussed.

<p>Magnetotactic bacteria (MTB) are ubiquitous, multi-phylogenetic bacteria that actively synthesize chains of magnetic, membrane bound; single domain magnetite (Fe₃O₄) or greigite (Fe₃S₄) crystals, termed magnetosomes in order to better navigate to their preferred chemical environment using the Earth’s magnetic field. Discovered in 1963, the field is now focused on understanding magnetosome chain formation and associated processes through genetic studies as well as analytical techniques such as Transmission Electron Microscopy (TEM) and Scanning Transmission X-ray Microscopy – X-ray Magnetic Circular Dichroism (STXM-XMCD).</p> <p>This thesis performed studies on <em>Candidatus Magnetovibrio blakemorei</em> strain MV-1 using STXM at the C 1s, O 1s, Ca 2p and Fe 2p edges. STXM-XMCD was used to determine the magnetism of individual magnetosomes and quantitatively determine magnetic properties such as the magnetic moment of individual chains. A sub-population of MV-1 cells was identified as having anomalous magnetic orientations of magnetosome sub-chains when separated spatial gaps. The frequency of this event and the underlying implications to magnetosome formation are discussed.</p> / Master of Science (MSc)

The nano-contact spin torque oscillator (NC-STO) is an emerging device for highly tunable microwave frequency generation in the range from 0.1 GHz to above 65 GHz with an on-chip footprint on the scale of a few μm. The frequency is inherent to the magnetic material of the NC-STO and is excited by an electrical DC current by means of the spin torque transfer effect. Although the general operation is well understood, more detailed aspects such as a generally nonlinear frequency versus current relationship, mode-jumping and high device-to-device variability represent open questions. Further application-oriented questions are related to increasing the electrical output power through synchronization of multiple NC-STOs and integration with CMOS integrated circuits. This thesis consists of an experimental part and a simulation part. Experimentally, for the frequency stability it is found that the slow but strong 1/f-type frequency fluctuations are related to the degree of nonlinearity and the presence of perturbing, unexcited modes. It is also found that the NC-STO can exhibit up to three propagating spin wave oscillation modes with different frequencies and can randomly jump between them. These findings were made possible through the development of a specialized microwave time-domain measurement circuit. Another instrumental achievement was made with synchrotron X-rays, where we image dynamically the magnetic internals of an operating NC-STO device and reveal a spin wave mode structure with a complexity significantly higher than the one predicted by the present theory. In the simulations, we are able to reproduce the nonlinear current dependence by including spin wave-reflecting barriers in the nm-thick metallic, magnetic free layer. A physical model for the barriers is introduced in the form of metal grain boundaries with reduced magnetic exchange coupling. Using the experimentally measured average grain size of 30 nm, the spin wave mode structure resulting from the grain model is able to reproduce the experimentally found device nonlinearity and high device-to-device variability. In conclusion, the results point out microscopic material grains in the metallic free layer as the reason behind the nonlinear frequency versus current behavior and multiple propagating spin wave modes and thereby as a source of device-to-device variability and frequency instability. / Dagens snabba utveckling inom informationsteknik drivs på av ständigt växande informationsmängder och deras samhällsanvändning inom allt från resursoptimering till underhållning. Utvecklingen möjliggörs till stor del hårdvarumässigt av miniatyrisering och integrering av elektroniska komponenter samt trådlös kommunikation med allt större bandbredd och högre överföringshastighet. Det senare uppnås främst genom utnyttjande av högre radiofrekvenser i teknologiskt tidigare oåtkomliga delar av spektrumet. Frekvensutnyttjandet har det senaste årtiondet ökat markant i mikrovågsområdet med typiska frekvenser runt 2.4 GHz och 5.2-5.8 GHz. I den spinntroniska oscillatorn (STO:n) möjliggörs frekvensgenerering i det breda området från 0.1 GHz upp till över 65 GHz av en komponent med mikrometerstorlek som kan integreras direkt i CMOS-mikrochip. Till skillnad från i konventionella radiokretsar med oscillatorer konstruerade av integrerade transistorer och spolar, genereras mikrovågsfrekvensen direkt i STO:ns magnetiska material och omvandlas därefter till en elektrisk signal genom komponentens magnetoresistans. Dessa materialegenskaper möjliggör ett tillgängligt frekvensband med extrem bredd i en och samma STO, som därtill kan frekvensmoduleras direkt genom sin styrström och på så sätt förenklar konstruktionen av sändarsystem. STO:ns icke-linjära egenskaper kan potentiellt också användas för att i en och samma komponent blanda ned mottagna mikrovågssignaler och på så sätt förenkla konstruktionen även av mikrovågsmottagare. STO:ns signalegenskaper bestäms av det magnetiska materialets fysik i form av magnetiseringsdynamik driven av elektriskt genererade spinnströmmar. I denna avhandling studeras denna dynamik experimentellt med särskilt fokus på frekvensstabiliteten i den hittills mest stabila STO-typen; nanokontakts-STO:n. Genom mätningar i tidsdomän av STO:ns elektriska signaler runt 25 GHz har frekvensstabiliteten funnits hänga samman med den typ av icke-linjärt beteende som också funnits vara utmärkande för tillverkningsvariationen i komponenterna. Mikroskopiska undersökningar av materialet visar att en trolig källa till denna variation är den magnetiska metallens uppbyggnad i form av korn i storleksordningen 30 nm, och datorsimuleringar av en sådan materialstruktur har visats kunna reproducera de experimentella resultaten. Därtill har en metod utvecklats för att med röntgenstrålning direkt mäta de små, magnetiska mikrovågsrörelserna i materialet. Denna röntgenteknik möjliggör detaljerade experimentella studier av magnetiseringsdynamiken och kan användas för att verifiera och vidareutveckla den existerande teorin för mikrovågsspinntronik. Sammantaget förs STO-teknologin genom denna studie ett steg närmare sina tänkbara samhällsbreda tillämpningar inom snabb, trådlös kommunikation för massproducerade produkter med integrerad sensor- och datorfunktionalitet. / <p>QC 20160620</p>

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.

La popularité des schémas d'homogénéisation classiques, basés sur la solution d'Eshelby du problème de l'inhomogénéité, tient à leur robustesse (des contrastes infinis entre les raideurs des différentes phases sont permis) et leur adaptabilité (les problèmes linéaires aussi bien que non-linéaires peuvent être abordés), la complexité des calculs mis en jeu restant limitée. Le fait qu'ils ne prennent en compte de façon quantitative qu'une quantité restreinte d'informations morphologiques constitue leur principale faiblesse. Ainsi, des problèmes tels que l'influence de la distribution de taille des pores ou l'orientation locale d'inclusions anisotropes leur sont inaccessibles. A l'heure actuelle, seuls de longs calculs complets (par éléments finis/de frontière) permettent d'aborder ces questions. L'objet de ce travail est de mettre au point de nouvelles méthodes d'homogénéisation, de mise en oe uvre plus légère que les éléments finis/de frontière, tout en rendant compte de plus de détails de la microstructure que les techniques basées sur la solution d'Eshelby. Le principe variationnel de Hashin et Shtrikman fournit le cadre mathématique rigoureux dans lequel sont développées deux méthodes. La méthode des inclusions polarisées, tout d'abord, dont le but est le calcul de milieux hétérogènes constitués d'inclusions, plongées dans une matrice homogène. Pour un calcul complet d'une microstructure donnée, il est connu que les méthodes numériques d'homogénéisation par transformée de Fourier rapide (FFT) sont de sérieux compétiteurs des méthodes d'éléments finis/de frontière. Le principe de Hashin et Shtrikman permet de jeter un éclairage nouveau sur ces techniques, et un schéma numérique original d'homogénéisation par FFT est proposé dans un second temps ; il s'avère plus rapide et plus robuste que les schémas existants. L'industrie du ciment pourrait certainement tirer parti de tels schémas d'homogénéisation avancés, puisqu'il est connu que les propriétés macroscopiques des pâtes de ciment dépendent fortement des détails les plus fins (à l'échelle sub-micronique) du réseau poreux (dans la phase CSH{}). Une partie de ce travail est consacrée à la caractérisation de ce réseau à l'aide de deux techniques expérimentales : la diffusion des rayons X aux petits angles, et la microscopie X. L'accent a été placé sur l'interprétation emph{quantitative} de ces expériences, en vue d'améliorer les prédictions des estimations des propriétés mécaniques macroscopiques. Une connexion est établie entre ces deux approches. Cette tentative, encore perfectible, montre que les modèles classiques du CSH{} ne peuvent rendre compte de ces données expérimentales / Classical homogenization schemes, based on the solution to Eshelby's inhomogeneity problem, draw their popularity from the fact that they are both robust (even infinite contrast of the mechanical phases is allowed) and versatile (linear- as well as non-linear mechanical problems can be addressed), while the computations involved are very limited. Their flaw lies in the fact that they incorporate very little morphological information: problems such as the influence of the pore-size distribution, or the local orientation of anisotropic inclusions is out of their reach. Presently, only lengthy full-field calculations (FEM, BEM) can address such issues. The aim of this work is to devise new homogenization techniques, which are not as computationally involved as FEM or BEM calculations, while capturing more details of the microstructure than Eshelby-based techniques. Two methods are developed within the framework of the variational principle of Hashin and Shtrikman, which provides sound mathematical ground. The polarized inclusion method, on the one hand, aims to address composites with inclusions embedded in a homogeneous matrix. On the other hand, FFT-based homogenization techniques are known to alleviate the burden of a full-field calculation carried out with FEM or BEM. With the help of the Hashin and Shtrikman principle, new light is shed on these techniques, and a new, faster and more robust, FFT-based scheme is proposed. The cement industry would certainly benefit from such advanced homogenization schemes, since the macroscopic properties of cement pastes are known to heavily rely on the finest details (at sub-micron length-scales) of the porous network (within the CSH{} phase). Part of this work is devoted to the characterization of this network using two experimental techniques, namely small-angle X-ray scattering and tomography with soft X-ray microscopy. Attempts are made at quantifying the microstructure of CSH{}, in order to improve the estimates of its mechanical properties. A link between these two approaches is established. This attempt, perfectible, shows that popular models for CSH{} cannot account for these experimental data

Soft x-ray microscopes routinely perform high-resolution 3D imaging of biological cells in their near-native environment with short exposure times at synchrotron radiation facilities. Some laboratory-sized microscopes are aiming to make this imaging technique more accessible to a wider scientific community. However, these systems have been hampered by source instabilities hindering routine imaging of biological samples with short exposure times. This Thesis presents work performed on the Stockholm laboratory x-ray microscope. A novel heat control system has been implemented, improving the stability of the laser-produced plasma source. In combination with recent upgrades to the imaging system and an improved cryofixation method, the microscope now has the capability to routinely produce images with 10-second exposure time of cryofixed biological samples. This has allowed for tomographic imaging of cell autophagy and cell-cell interactions. Furthermore, a numerical 3D image formation model is presented as well as a novel reconstruction approach dealing with the limited depth of focus in x-ray microscopes. / <p>QC 20170505</p>

In dieser Arbeit werden elektrodynamische Untersuchungen von diffraktiven Röntgenoptiken mit hohen Aspektverhältnissen - sog. Volumenzonenplatten - für hochauflösende Röntgenmikroskopie im Photonenenergiebereich von 0.1-10 keV behandelt. Des Weiteren werden Verfahren zur Realisierung solcher Optiken dargestellt. Das Auflösungsvermögen von Röntgenmikroskopen ist weitgehend durch die numerische Apertur der verwendeten Objektive bestimmt. Die Apertur hängt von der äußeren Zonenbreite der Zonenplatte und der gewählten Beugungsordnung ab. Eine Auflösungssteigerung kann nur durch Verringerung der äußeren Zonenbreiten oder Abbildung in hohen Ordnungen erzielt werden. Neben hoher Ortsauflösung ist ein hinreichender Beugungswirkungsgrad die Grundlage für röntgenmikroskopische Abbildungen. Elektrodynamische Rechnungen zeigen, dass geneigte Zonenstrukturen mit hohen Aspektverhältnissen zum signifikanten Anstieg der Effizienz in hohen Beugungsordnungen führen. Diese Volumenbeugungseffekte an Zonenplatten werden mit Hilfe der rigorosen Theorie gekoppelter Wellen untersucht. Praktisch können dreidimensionale, geneigte Nanostrukturen aufgrund der extremen nanotechnologischen Anforderungen nur durch Approximierung des Neigungswinkels realisiert werden. Zur Herstellung von Zonenplatten mit hohen Aspektverhältnissen und geneigten Zonen wird ein sog. Stack-Prozess eingeführt, der auf der Überlagerung von einzelnen Zonenplattenlagen basiert. Um den Neigungswinkel der Zonen anzunähern, werden die Zonenradien dabei mit jeder Lage verringert. Die erfolgreiche Realisierung der erforderlichen Nanotechnologien führt erstmalig zur Herstellung von Multi-Lagen-Zonenplatten mit minimalen Zonenbreiten bis zu 25 nm. Multi-Lagen- und Volumenzonenplatten bieten zukünftig das Potential für gesteigerte Auflösungsvermögen im sub-10 nm Bereich für die Mikroskopie im weichen Röntgenbereich und für die Fokussierung von harter Röntgenstrahlung auf bis zu 20 nm bei gleichzeitig hohen Beugungseffizienzen. / In this thesis, electrodynamical calculations of diffractive x-ray optics with high aspect ratios – so-called volume zone plates – for high resolution x-ray microscopy in the photon energy range from 0.1 - 10 keV are presented. In addition, methods for the realization of this optics are described. The resolution of an x-ray microscope is limited by the numerical aperture of the objective. Thereby the aperture depends on the outermost zone width of the zone plate and the diffraction order which is used for imaging. Hence, the resolution can only be increased by decreasing the minimum zone width or imaging in high orders of diffraction. Besides the resolving power, the diffraction efficiency needs to be sufficiently high for zone plate based x-ray microscopy. Electrodynamical calculations show that tilted zone structures with high aspect ratios significantly increase the diffraction efficiency in selected high orders. These volume diffraction effects on zone plates were investigated by the rigorous coupled wave theory. Due to very high nanotechnological requirements, such three-dimensional, tilted nanostructures can only be realized by multiple-step zone plates. For the fabrication of zone plates with high aspect ratios and tilted zones the so-called stack process is introduced in this thesis, which is based on a superposition of single zone plate layers. For an approximation of the tilt angle of the structures the zone radii are thereby decreased with each layer. For the first time multilayer zone plates with minimum zone widths down to 25 nm were fabricated by the successful realization of the stack process in this thesis. In the future, multilayer and volume zone plates have the potential for an increased spatial resolution in the sub-10 nm range for soft x-ray microscopy and for focusing hard x-rays down to 20 nm with high diffraction efficiencies.

Soft x-ray microscopy in the water-window (λ = 2.28 nm – 4.36 nm) is based on zone-plate optics and allows high-resolution imaging of, e.g., cells and soils in their natural or near-natural environment. Three-dimensional imaging is provided via tomographic techniques, soft x-ray cryo tomography. However, soft x-ray microscopes with such capabilities have been based on large-scale synchrotron x‑ray facilities, thereby limiting their accessibility for a wider scientific community. This Thesis describes the development of the Stockholm laboratory soft x-ray microscope to three-dimensional cryo tomography and to new optics-based contrast mechanisms. The microscope relies on a methanol or nitrogen liquid-jet laser-plasma source, normal-incidence multilayer or zone-plate condenser optics, in-house fabricated zone-plate objectives, and allows operation at two wavelengths in the water-window, λ = 2.48 nm and λ = 2.48 nm. With the implementation of a new state-of-the-art normal-incidence multilayer condenser for operation at λ = 2.48 nm and a tiltable cryogenic sample stage the microscope now allows imaging of dry, wet or cryo-fixed samples. This arrangement was used for the first demonstration of laboratory soft x-ray cryo microscopy and tomography. The performance of the microscope has been demonstrated in a number of experiments described in this Thesis, including, tomographic imaging with a resolution of 140 nm, cryo microscopy and tomography of various cells and parasites, and for studies of aqueous soils and clays. The Thesis also describes the development and implementation of single-element differential-interference and Zernike phase-contrast zone-plate objectives. The enhanced contrast provided by these optics reduce exposure times or lowers the dose in samples and are of major importance for harder x-ray microscopy. The implementation of a high-resolution 50 nm compound zone-plate objective for sub-25-nm resolution imaging is also described. All experiments are supported by extensive numerical modelling for improved understanding of partially coherent image formation and stray light in soft x-ray microscopes. The models are useful tools for studying effects of zone plate optics or optical design of the microscope on image formation and quantitative accuracy in soft x-ray tomography. / QC 20110221

Diffractive zone-plate lenses are widely used as optics in high-resolution x-ray microscopes. The achievable resolution in such microscopes is presently not limited by the x-ray wavelength but by limitations in zone-plate nanofabrication. Thus, for the advance of high-resolution x-ray microscopy, progress in zone-plate nanofabrication methods are needed.   This Thesis describes the development of new nanofabrication processes for improved x-ray zone-plate optics. Cold development of the electron-beam resist ZEP7000 is applied to improve the resolution of soft x-ray Ni zone plates. The influence of developer temperature on resist contrast, resolution, and pattern quality is investigated. With an optimized process, Ni zone plates with outermost zone widths down to 13 nm are demonstrated. To enhance the diffraction efficiency of Ni zone plates, the concept of Ni-Ge zone plates is introduced. The applicability of Ni-Ge zone plates is first demonstrated in a proof-of-principle experiment, and then extended to cold-developed Ni zone plates with outermost zone widths down to 13 nm. For 15-nm Ni-Ge zone plates a diffraction efficiency of 4.3% at a wavelength of 2.88 nm is achieved, which is about twice the efficiency of state-of-the-art 15-nm Ni zone plates. To further increase both resolution and diffraction efficiency of soft x-ray zone plates, a novel fabrication process for W zone plates is developed. High resolution is provided by salty development of the inorganic electron-beam resist HSQ, and cryogenic RIE in a SF6 plasma is investigated for high-aspect-ratio W structuring. We demonstrate W zone plates with 12-nm outermost zone width and a W height of 90 nm, resulting in a 30% increase in theoretical diffraction efficiency compared to 13-nm efficiency-enhanced Ni-Ge zone plates. In addition to soft x-ray zone plates, some lenses for hard x-ray free-electron-laser applications were also fabricated during this Thesis work. Fabrication processes for the materials W, diamond, and Pt were developed. We demonstrate Pt and W-diamond zone plates with 100-nm outermost zone width and respective diffraction efficiencies of 8.2% and 14.5% at a photon energy of 8 keV. / QC 20111114

abstract: Aluminum alloys are ubiquitously used in almost all structural applications due to their high strength-to-weight ratio. Their superior mechanical performance can be attributed to complex dispersions of nanoscale intermetallic particles that precipitate out from the alloy’s solid solution and offer resistance to deformation. Although they have been extensively investigated in the last century, the traditional approaches employed in the past haven’t rendered an authoritative microstructural understanding in such materials. The effect of the precipitates’ inherent complex morphology and their three-dimensional (3D) spatial distribution on evolution and deformation behavior have often been precluded. In this study, for the first time, synchrotron-based hard X-ray nano-tomography has been implemented in Al-Cu alloys to measure growth kinetics of different nanoscale phases in 3D and reveal mechanistic insights behind some of the observed novel phase transformation reactions occurring at high temperatures. The experimental results were reconciled with coarsening models from the LSW theory to an unprecedented extent, thereby establishing a new paradigm for thermodynamic analysis of precipitate assemblies. By using a unique correlative approach, a non-destructive means of estimating precipitation-strengthening in such alloys has been introduced. Limitations of using existing mechanical strengthening models in such alloys have been discussed and a means to quantify individual contributions from different strengthening mechanisms has been established. The current rapid pace of technological progress necessitates the demand for more resilient and high-performance alloys. To achieve this, a thorough understanding of the relationships between material properties and its structure is indispensable. To establish this correlation and achieve desired properties from structural alloys, microstructural response to mechanical stimuli needs to be understood in three-dimensions (3D). To that effect, in situ tests were conducted at the synchrotron (Advanced Photon Source) using Transmission X-Ray Microscopy as well as in a scanning electron microscope (SEM) to study real-time damage evolution in such alloys. Findings of precipitate size-dependent transition in deformation behavior from these tests have inspired a novel resilient aluminum alloy design. / Dissertation/Thesis / Doctoral Dissertation Materials Science and Engineering 2017