S.N. Yakunin

Short period La/B and LaN/B multilayer mirrors for ~6.8 nm wavelength.

In the first part of this article we experimentally show that contrast between the very thin layers of La and B enables close to theoretical reflectance. The reflectivity at 6.8 nm wavelength was measured from La/B multilayer mirrors with period thicknesses ranging from 3.5 to 7.2 nm at the appropriate angle for constructive interference. The difference between the measured reflectance and the reflectance calculated for a perfect multilayer structure decreases with increasing multilayer period. The reflectance of the multilayer with the largest period approaches the theoretical value, showing that the optical contrast between the very thin layers of these structures allows to experimentally access close to theoretical reflectance. In the second part of the article we discuss the structure of La/B and LaN/B multilayers. This set of multilayers is probed by hard X-rays (λ = 0.154 nm) and EUV radiation (λ = 6.8 nm). The structure is reconstructed based on a simultaneous fit of the grazing incidence hard X-ray reflectivity and the EUV reflectivity curves. The reflectivity analysis of the La/B and LaN/B multilayer mirrors shows that the lower reflectance of La/B mirrors compared to LaN/B mirrors can be explained by the presence of 5% of La atoms in the B layer and 63% of B in La layer. After multi-parametrical optimization of the LaN/B system, including the nitridation of La, the highest near normal incidence reflectivity of 57.3% at 6.6 nm wavelength has been measured from a multilayer mirror, containing 175 bi-layers. This is the highest value reported so far.

Combined EUV reflectance and X-ray reflectivity data analysis of periodic multilayer structures

We present a way to analyze the chemical composition of periodical multilayer structures using the simultaneous analysis of grazing incidence hard X-Ray reflectivity (GIXR) and normal incidence extreme ultraviolet reflectance (EUVR). This allows to combine the high sensitivity of GIXR data to layer and interface thicknesses with the sensitivity of EUVR to the layer densities and atomic compositions. This method was applied to the reconstruction of the layered structure of a LaN/B multilayer mirror with 3.5 nm periodicity. We have compared profiles obtained by simultaneous EUVR and GIXR and GIXR-only data analysis, both reconstructed profiles result in a similar description of the layered structure. However, the simultaneous analysis of both EUVR and GIXR by a single algorithm lead to a ∼ 2x increased accuracy of the reconstructed layered model, or a more narrow range of solutions, as compared to the GIXR analysis only. It also explains the inherent difficulty of accurately predicting EUV reflectivity from a GIXR-only analysis.

Structural coupling across the direct EuO/Si interface.

The ferromagnetic semiconductor EuO is believed to be an effective spin injector when directly integrated with silicon (Si). Injection through spin-selective ohmic contact requires superb structural quality of the interface EuO/Si. A recent breakthrough in manufacturing free-of-buffer-layer EuO/Si junctions calls for structural studies of the interface between the semiconductors. The synthesis of EuO employs an advanced protection of the Si substrate surface and a two-step growth protocol. It prevents unwanted chemical reactions at the interface. Ex situ high-resolution x-ray diffraction (XRD) and reflectivity (XRR) accompanied by in situ reflection high-energy electron diffraction reveal direct coupling at the interface. A combined analysis of XRD and XRR data provides a common structural model. The structural quality of the EuO/Si spin contact far exceeds that of previous reports and thus makes a step forward to the ultimate goals of spintronics.

Model independent X-ray standing wave analysis of periodic multilayer structures

We present a model independent approach for the reconstruction of the atomic concentration profile in a nanoscale layered structure, as measured using the X-ray fluorescence yield modulated by an X-ray standing wave (XSW). The approach is based on the direct regularized solution of the system of linear equations that characterizes the fluorescence yield. The suggested technique was optimized for, but not limited to, the analysis of periodic layered structures where the XSW is formed under Bragg conditions. The developed approach was applied to the reconstruction of the atomic concentration profiles for LaN/BN multilayers with 50 periods of 35 °A thick layers. The object is especially difficult to analyse with traditional methods, as the estimated thickness of the interface region between the constituent materials is comparable to the individual layer thicknesses. However, using the suggested technique it was possible to reconstruct the La atomic profile, showing that the La atoms stay localized within the LaN layers and interfaces and do not diffuse into the BN layer. The atomic distributions were found with an accuracy of 1 °A. The analysis of the Kr fluorescence yield showed that Kr atoms originating from the sputter gas are trapped in both the LaN-on-BN and the BN-on-LaN interfaces.

Reconstruction of interfaces of periodic multilayers from X-ray reflectivity using a free-form approach

Grazing-incidence X-ray reflectivity (GIXRR) is a widely used analysis method for thin films and multilayer structures. However, conventional so-called model-based approaches of structural reconstruction from GIXRR data lack flexibility when dealing with very thin structures (down to the nanometre scale), because a priori assumptions have to be made about the interface composition and structure. This makes it very difficult to extract reliable information about such structures. In this work, a custom free-form approach is presented, which solves this task without the need for a priori assumptions on layer or interface parameters. As a proof of principle, an optical constant profile reconstruction and GIXRR curve matching for simulated data are demonstrated. The developed approach is used to analyse the structures of multilayer LaN/B Bragg reflectors designed for the extreme UV range. The performed analysis allowed the difference in optical constant profiles of these structures produced with different processes to be revealed. The uncertainties of structural reconstruction are also discussed.

Possibilities of surface-sensitive X-ray methods for studying the molecular mechanisms of interaction of nanoparticles with model membranes

The processes of structural rearrangement in a model membrane, i.e., an arachic acid monolayer formed on a colloidal solution of cerium dioxide or magnetite, are studied in situ in real time by the methods of X-ray standing waves and 2D diffraction. It is shown that the character of the interaction of nanoparticles with the monolayer is determined by their nature and sizes and depends on the conditions of nanoparticle synthesis. In particular, the structure formation in the monolayer–particle system is greatly affected by the stabilizer (citric acid), which is introduced into the colloidal solution during synthesis.

Investigation of the thermal diffusion during the formation of a quasicrystalline phase in thin Al-Pd-Re films

The layer mixing during the formation of the Al70Pd20Re10 icosahedral quasicrystalline phase in thin (55 nm) Al-Pd-Re layered film systems subjected to vacuum annealing has been studied. It is shown that a combined layer of Pd and Al atoms (with the Al3Pd2 phase dominating) is formed in the first stage (at 350°C), while the rhenium layer remains invariable. In the second annealing stage (at 450°C), the β′-AlPd phase is formed and the Re layer is diffused. In the third stage (700°C), Pd and Re atoms are uniformly distributed throughout the film with the formation of a quasicrystalline phase.

Direct observation of anomalous Kossel lines

Anomalous Kossel lines corresponding to the yield of X rays from a germanium crystal under the conditions of strongly asymmetric diffraction have been observed in the simplest experimental scheme with the use of characteristic Mo Kα radiation and a germanium crystal analyzer. In agreement with the results of a previous theoretical analysis, such lines are narrow collimated beams of radiation in the form of a ridge in a narrow angular range near a given direction whose intensity is one or two orders of magnitude higher than the background with a divergence of about several seconds of arc in the diffraction plane and of about 10′ along the Kossel line. The possible applications of this effect, in particular, for solving the problems of X-ray holography, are discussed.

Studying the Molecular Mechanisms of Interaction of Nanoaerosol Particles with a Model Membrane

An X-ray study of the interaction of Langmuir monolayers with nanoparticles under the conditions when nanoparticles arrive at the monolayer from the side of the air medium has been performed for the first time. Measurements by the X-ray standing-wave method and two-dimensional diffraction have made it possible to investigate the transport of nanoaerosol particles through a lipid monolayer and observe the structural changes occurring in it. Nanoaerosol particles were formed by electrohydrodynamic sputtering of desalted solutions of ferritin. It was shown that nanoaerosol particles pass through the monolayer without disrupting the two-dimensional packing of lipid molecules. The ferritin molecules penetrating the aqueous subphase after sputtering are found to be adsorbed under the monolayer.

Investigation of the dynamics of the interaction of metal particles with a Langmuir single layer upon an increase in the surface pressure

X-ray studies of dipalmitoylphosphatidylcholine (DPPC) single layers on the surface of a liquid provide detailed information on the interaction of metal particles with a single layer upon an increase in the surface pressure up to the collapse. Two complementary X-ray methods are used: grazing incidence diffraction and the X-ray standing waves method. The experimental results obtained for a single layer formed on a colloidal solution of magnetite nanoparticles reveal that the increase in the surface pressure is accompanied by an increase in the concentration of nanoparticles near the surface. In a series of experiments where metal particles of submicron size are sputtered onto a DPPC single layer, a sharp decrease in the intensity of the fluorescence yield from metal atoms is observed while the single layer is compressed. These data suggest that metal particles deposited onto the surface of a single layer were extruded into the aqueous subphase.