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We present a general approach to thin bulk samples to transparency for experiments in the soft x-ray and extreme ultraviolet spectral range. The method relies on mechanical grinding followed by focused-ion-beam milling. It results in a uniformly thin area of high surface quality, suitable for nanoscale imaging in transmission. In a proof-of-principle experiment, nanoscale magnetic bits on a commercial hard drive glass disk are imaged with a spatial resolution below 30 nm by soft x-ray spectro-holography. Furthermore, we demonstrate imaging of a lithographically patterned test object via absorption contrast. Our approach is suitable for both amorphous and crystalline substrates and has been tested for a variety of common epitaxy growth substrates. Lateral thinning areas in excess of 100 μm2 and a remaining substrate thickness as thin as 150 nm are easily achievable. Our approach allows preserving a previously grown thin film, and from nanofocus electron diffraction, we find no evidence for morphological changes induced by the process, in agreement with numerical simulations of the ion implantation depth distributon. We expect our method to be widely applicable and especially useful for nanoscale imaging of epitaxial thin films. © 2017 Author(s).

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Department of Physics

Fulltext

Review of Scientific Instruments

A general approach to obtain soft x-ray transparency for thin films grown on bulk substrates

In this work, we take a step toward nanometer resolution magnetic tomography, demonstrating the use of resonant magnetic x-ray scattering for three-dimensional (3D) characterization of Co/Pd multilayers. Trading coherence for x-ray flux, we measured magnetic scattering out to full period resolutions of 20 nm for incidence angles up to 75 from normal incidence, which was sufficient for a semiquantitative analysis of the 3D magnetic domain structure of such films. For the analysis of such patterns, we developed a scattering model based upon multiple plane propagation of the beam through the sample, taking into account the effects of multiple scattering not accounted for with Born or Rytov approximation based models. Our results demonstrate that 3D statistical characterization of nanoscale magnetic features is currently possible, and it is expected that the advent of high brilliance sources such as MAX IV in Sweden and SIRIUS in Brazil will provide the coherent flux necessary to permit the generalization of this work to nanometer resolution magnetic tomography. © 2017 American Physical Society.

Physical Review B

Three-dimensional characterization of Co/Pd multilayer thin films using resonant soft x-ray scattering

We prepared monolayers of iron oxide nanoparticles via self-assembly on a bare silicon wafer and on a vanadium film sputter deposited onto a plane sapphire substrate. The magnetic configuration of nanoparticles in such a dense assembly was investigated by polarized neutron reflectivity. A theoretical model fit shows that the magnetic moments of nanoparticles form quasi domain-like configurations at remanence. This is attributed to the dipolar coupling amongst the nanoparticles. © 2015 IOP Publishing Ltd.

Journal of Physics Condensed Matter

Polarized neutron reflectivity from monolayers of self-assembled magnetic nanoparticles

We report on the fabrication and characterization of iron oxide nanoparticle thin film superlattices. The formation into different film morphologies is controlled by tuning the particle plus solvent-to-substrate interaction. It turns out that the wetting vs dewetting properties of the solvent before the self-assembly process during solvent evaporation plays a major role in determining the resulting film morphology. In addition to layerwise growth three-dimensional mesocrystalline growth is also evidenced. The understanding of the mechanisms ruling nanoparticle self-assembly represents an important step towards the fabrication of novel materials with tailored optical, magnetic or electrical transport properties. © 2014 IOP Publishing Ltd.

Nanotechnology

Growth modes of nanoparticle superlattice thin films

We have fabricated by e-beam lithography periodic arrays of rectangular shaped trenches of different widths into Si substrates. The trenches were filled with iron oxide nanoparticles, 20 nm in diameter, by spin-coating them onto the Si substrate. The trenches have the purpose to assist the self-assembly of the iron oxide nanoparticles. Using x-ray scattering techniques, we have analyzed the structure factor of the trenches before and after filling in order to determine the filling factor. We present a theoretical analysis of the x-ray scattering function within the distorted-wave Born approximation and we present a quantitative comparison between theory and experiment. © 2014 AIP Publishing LLC.

Journal of Applied Physics

Template assisted self-assembly of iron oxide nanoparticles: An x-ray structural analysis

We have investigated the structure and magnetism of self-assembled, 20nm diameter iron oxide nanoparticles covered by an oleic acid shell for scrutinizing their structural and magnetic correlations. The nanoparticles were spin-coated on an Si substrate as a single monolayer and as a stack of 5ML forming a multilayer. X-ray scattering (reflectivity and grazing incidence small-angle scattering) confirms high in-plane hexagonal correlation and a good layering property of the nanoparticles. Using polarized neutron reflectivity we have also determined the long range magnetic correlations parallel and perpendicular to the layers in addition to the structural ones. In a field of 5kOe we determine a magnetization value of about 80% of the saturation value. At remanence the global magnetization is close to zero. However, polarized neutron reflectivity reveals the existence of regions in which magnetic moments of nanoparticles are well aligned, while losing order over longer distances. These findings confirm that in the nanoparticle assembly the magnetic dipoledipole interaction is rather strong, dominating the collective magnetic properties at room temperature. © 2012 IOP Publishing Ltd.

Self-assembled iron oxide nanoparticle multilayer: X-ray and polarized neutron reflectivity

The deliberate control over the spatial arrangement of nanostructures is the desired goal for many applications such as, for example, in data storage, plasmonics or sensor arrays. Here we present a novel method to assist the self-assembly process of magnetic nanoparticles. The method makes use of nanostructured aluminum templates obtained after anodization of aluminum discs and the subsequent growth and removal of the newly formed alumina layer, resulting in a regular honeycomb-type array of hexagonally shaped valleys. The iron oxide nanoparticles, 20nm in diameter, are spin-coated onto the surface of honeycomb nanostructured Al templates. Depending on the size, each hexagon site can host up to 30 nanoparticles. These nanoparticles form clusters of different arrangements within the valleys, such as collars, chains and hexagonally closed islands. Ultimately, it is possible to isolate individual nanoparticles. The strengths of the magnetic interaction between particles in a cluster are probed using the memory effect known from the coupled state in superspin glass systems. © 2011 IOP Publishing Ltd.

Template-assisted self-assembly of individual and clusters of magnetic nanoparticles

Cobalt and magnetite nanoparticles were studied with small-angle x-ray and neutron scattering methods under grazing incidence for analyzing their structural and magnetic correlation on silicon substrates. The Co nanoparticles are in the ferromagnetic state while the iron oxide nanoparticles are superparamagnetic at room temperature. After spin-coating the iron oxide particles with a diameter of 20 nm and a very narrow size distribution of only 6 show very nice self-ordering on silicon substrates with nearly perfect six-fold symmetry as can be derived from scanning electron microscopy (SEM) images and from grazing incidence small angle x-ray scattering results. In contrast the dropcasted cobalt nanoparticles show a much higher roughness and less ordering. The corresponding SEM images and grazing incidence small angle neutron scattering maps with polarization of the incident beam reveal less pronounced structural and magnetic correlation. © 2011 American Institute of Physics.

Self organization of magnetic nanoparticles: A polarized grazing incidence small angle neutron scattering and grazing incidence small angle x-ray scattering study

We have studied the precessional dynamics of Co/Cu/Py (where Py Ni 81Fe19) trilayers by time-resolved x-ray resonant magnetic scattering at the synchrotron radiation facility BESSY II. We have found that the magnetic precessional decay time of Fe magnetic moments in Py layers decreases when changing the mutual orientation of the magnetization direction of Py and Co layers from parallel to antiparallel. The observed changes of the decay time can be associated with the spin pumping induced damping effect. © 2011 American Institute of Physics.

Applied Physics Letters

Precessional dynamics and damping in Co/Cu/Py spin valves

We report about a combined structural and magnetometric characterization of self-assembled magnetic nanoparticle arrays. Monodisperse iron oxide nanoparticles with a diameter of 20nm were synthesized by thermal decomposition. The nanoparticle suspension was spin-coated on Si substrates to achieve self-organized arrays of particles and subsequently annealed at various conditions. The samples were characterized by x-ray diffraction, and bright and dark field high resolution transmission electron microscopy. The structural analysis is compared to magnetization measurements obtained by superconducting quantum interference device magnetometry. We can identify either multi-phase FexO/γ-Fe2O3 or multi-phase Fe xO/Fe3O4 nanoparticles. The Fe xO/γ-Fe2O3 system shows a pronounced exchange bias effect which explains the peculiar magnetization data found for this system. © 2011 IOP Publishing Ltd.

Structural and magnetic characterization of self-assembled iron oxide nanoparticle arrays

Magnetic Γ-Fe 2O 3 nanoparticles with a mean diameter of 20 nm and size distribution of 7% were chemically synthesized and spin-coated on top of a Si-substrate. As a result, the particles self-assembled into a mono layer with hexagonal close-packed order. Subsequently, the nanoparticle array was coated with a Co layer of 20 nm thickness. The magnetic properties of this composite nanopar-ticle/thin film system were investigated by magnetometry and related to high-resolution transmission electron microscopy studies. Herein three systems were compared: i.e. a reference sample with only the particle monolayer, a composite system where the particle array was ion-milled prior to the deposition of a thin Co film on top, and a similar composite system but without ion-milling. The nanoparticle array showed a collective super-spin behavior due to dipolar interparticle coupling. In the composite system, we observed a decoupling into two nanoparticle subsystems. In the ion-milled system, the nanoparticle layer served as a magnetic flux guide as observed by magnetic force microscopy. Moreover, an exchange bias effect was found, which is likely to be due to oxygen exchange between the iron oxide and the Co layer, and thus forming of an antiferromagnetic CoO layer at the Γ-Fe 2O 3/Co interface. © 2010 Confalonieri et al.