A subnanometric resolution method for studying the local atomic structure of interface and surface of low contrast multilayered nanoheterostructure thin films is applied to the Fe/Cr multilayer sample with GMR (Giant Magnetoresistance) effect. We consider combination of the X-ray reflectivity (XRR) and the Extended X-ray absorption Fine Structure (EXAFS) spectroscopy with angular resolution. The XRR experiment has been carried out according to standard procedure using a specialized X-ray diffractometer "Empyrean" at the Institute of Metal Physics (Ekaterinburg). We have applied a measurement method proposed earlier by V. P. Romanov et al. This approach allowed us to separate the diffuse and pure specular contributions. To determine the concentration depth-profile of element from XRR data, we have implemented the Levenberg-Marquardt (L-M) algorithm for nonlinear inverse problem. Thus, the phase problem for X-ray specular reflectivity has been solving. The EXAFS measurements has been performed using synchrotron facilities (National Research Centre "Kurchatov Institute"). {The Fe and Cr K absorption spectra} were recorded in fluorescence mode with angular resolution. The experimental results for depth-resolved local atomic structure of Fe/Cr multilayer with GMR effect has been obtained. A depth resolution of 2-3 angstrom was reached. Atomic structure of Fe and Cr atoms located at seven depth points including interface for the Al2O3/Cr(100 angstrom)/[Fe(8 angstrom)/Cr(10,5 angstrom)](2)/Cr(20 angstrom) multilayered sample was obtained. It was shown what chromium oxides were present on the surface of the sample.
The heterogeneous ferromagnetic–superconducting layered heterostructures V/Fe0.7V0.3/V/Fe0.7V0.3/Nb and Nb/Ni0.65(0.81)Cu0.35(0.19), which contain magnetic clusters and ferromagnetic domains, are studied. The magnetic and superconducting properties of the structures depend on the magnetic-layer thickness, the magnetic field, and the time elapsed from structure preparation. We detected the interaction of clusters with a domain structure, diamagnetism and magnetization reversal of the magnetic layer during the superconducting transition in a ferromagnetic–superconducting heterostructure, and a superconducting transition in the magnetic layer. The magnetic and resistive properties of the heterostructures changed in several weeks and months.
The features of the technique of resonant synchrotron-radiation (SR) diffraction are considered. The energy, angular, polarization, and temperature dependences of Bragg reflections at incident radiation energies that are close to the absorption edges of material atoms are studied using this technique. These dependences contain information about the electronic, magnetic, and structural features of the objects under study. The contribution of several scattering channels to the formation of the diffraction spectrum leads to the appearance of interference effects making it possible to obtain information about the scattered radiation phase. Results of some studies of resonant SR diffraction performed at the Kurchatov SR source are presented.
The dichroic effect (“rotated” polarization) in the reflectivity from a magnetically ordered sample is experimentally studied at the station PHASE of the Kurchatov Synchrotron Radiation Source. The experiments are performed for the Gd 0.23 Co 0.77 film, which has a compensation temperature T comp ≈ 433 K, using linearly polarized radiation of the photon energy of 7930 eV ( L 2 absorption edge of gadolinium) at room temperature. The developed theory of reflectivity accounted for the magnetic contributions to the scattering amplitude predicts the appearance of a peak for the orthogonal (to the incident polarization) polarization of the reflected radiation near the critical angle of the total external reflection. The experiment reveals the significant difficulties because of the incomplete σ polarization of the synchrotron beam, the beam instability, and so on. Therefore, a rotated-polarization peak has been detected near the critical angle but at the limits of the measurement accuracy. In principle, our experimental technique could be an alternative to circular polarization experiments, which are widely used at synchrotrons to study magnetic ordering. However, as we have shown, it makes high demands of the radiation source parameters.
The influence of superconductivity on ferromagnetism in the layered Ta/V/Fe 1– x V x /V/Fe 1– x V x /Nb/Si structures consisting of ferromagnetic and superconducting layers is studied using polarized neutron reflection and scattering. It is experimentally shown that magnetic structures with linear sizes from 5 nm to 30 μm are formed in these layered structures at low temperatures. The magnetization of the magnetic structures is suppressed by superconductivity at temperatures below the superconducting transition temperatures in the V and Nb layers. The magnetic states of the structures are shown to undergo relaxation over a wide magnetic-field range, which is caused by changes in the states of clusters, domains, and Abrikosov vortices.
Resonant diffraction of synchrotron radiation (SR) is a modern method of studying the structure and properties of condensed matter that can be implemented on third-generation synchrotrons. This method allows one to investigate local properties of media (including magnetic and electronic ones) and observe thermal vibrations, defects, and orbital and charge orderings. A brief review of the advance provided by SR resonant diffraction is presented, and the capabilities of this method for analyzing phase transitions are considered in more detail by the example of potassium dihydrogen phosphate and rubidium dihydrogen phosphate crystals. It is shown that the investigation of the temperature dependence of forbidden reflections not only makes it possible to observe the transition from para- to ferroelectric phase, but also gives information about the proton distribution at hydrogen bonds.
A new method for determining the concentration profiles of chemical elements in multilayer metallic nanoheterostructures from X-ray reflectometry data has been developed as applied to low-contrast systems. The method is based on the solution of the Fredholm integral equation of the first kind, which relates the reflection coefficient and the concentration profile of the chemical elements involved in the composition of the sample. The ill-posed inverse problem of the determination of the concentration profile is solved by the regularization method. The efficiency of the proposed method is confirmed by model calculations performed for a four-layer Cr/Gd/Fe/Cr//Si structure with high-contrast Cr/Gd pairs and low-contrast Fe/Cr pairs. The experimental results on the determination of the concentration profile of the surface layer of the epitaxial thin Cr films and three-layer Cr/Fe/Cr structure deposited on the Al 2 O 3 substrate are presented.
Resonant x-ray diffraction was used to study the proton jumps in hydrogen-bonded rubidium dihydrogen phosphate (RDP) crystals. In the paraelectric RDP phase, hydrogen is delocalized between two crystallographically equivalent positions. At lower temperatures, this symmetry can be broken, which defines the processes that lead to the para- to ferroelectric phase transition. We have measured the energy spectra of the forbidden reflections 006 and 550 at incident radiation energies close to the Rb K edge in a wide temperature range, down to the temperature of the ferroelectric phase transition. In the paraelectric phase, we observed a growth of integrated intensity for both forbidden reflections with temperature. This behavior is opposite to conventional nonresonant Bragg reflections, where intensity decreases in accordance with the Debye-Waller factor. The developed theoretical model explains this effect with the thermal motion induced (TMI) scattering mechanism and also confirms the adiabatic approximation stating that electrons instantly follow the nuclei movements. In the 550 energy spectra, we have observed an additional contribution to the resonant structure factor, which could be associated with the presence of transient Slater-type proton configurations (PC) in the half-filled hydrogen position.
An upgraded X-ray Topography and Microtomography (XRT-MT) station is described, the parameters of the optical schemes and detectors are given, and the experimental possibilities of the station are analyzed. Examples of tomographic reconstructions are reported which demonstrate spatial resolutions of 2.5 and 10 μm at fields of view of 2.5 and 10 mm, respectively.
The surface morphology and local structure of layers in the Ni-Ge and Ge-Ni-Ge-Ni-Ge films have been investigated. It has been shown that the surface of the films follows the roughnesses of the substrate surface, which have characteristic dimensions of 2–4 nm in height and ∼100 nm in plane. It has been found that an interface with the depth ranging from 9 to 18 nm is formed at the boundaries between the Ni and Ge layers. The data obtained have been used to explain the specific features of the magnetic properties of the studied films, such as the asymmetry of hysteresis loops at low temperatures and the difference between the temperature dependences of the magnetization of the samples for two cooling modes: in a magnetic field and without a magnetic field.
Results of the study of the structural and magnetic properties of periodic Fe/V heterostructures with periods D = 9.4nm and D = 6.3nm are present. The study has shown that ferromagnetic islands are formed on the interfaces of Fe and V. These islands have different magnetic properties as sub-layers of pure iron. Islands in the sample with the period D = 9.4 nm have anisotropic shape, which leads to the anisotropy of magnetic properties.
The effect of strain (either static or caused by long-wavelength acoustic oscillations) on the energy spectrum and the azimuthal dependence of the intensity of “forbidden” reflections in crystals at the energy of incident radiation close to the absorption edge is considered. It is shown that a strain causing a weak change in the unit-cell symmetry may additionally contribute to the tensor atomic factor. Examples of changes in the azimuthal dependence of forbidden-reflection intensity in zinc oxide ZnO and potassium dihydrogen phosphate KH 2 PO 4 are considered.
A crystal of the tetragonal modification of lysozyme grown under controlled conditions with in situ monitoring of the growth kinetics and morphology of the (110) face is studied by X-ray topography using synchrotron radiation. The choice of a diffraction reflection with optimal dispersion allows us to obtain an informative X-ray topographic image of the sample. It is found that the striations that are formed under changing supersaturation correspond to the type of zonality characteristic of crystals growing by the normal mechanism and differ from those observed in inorganic crystals growing by the layer-by-layer mechanism.