Vol 62, No 1 (2017)

The evolution of structural-phase states during the α → γ transformation upon slow heating of metastable Fe–32 at % Ni alloy has been studied. Experimental evidences in favor of the mechanism of dynamic γ → α → γ transformations as plastic relaxation of internal elastic stress, providing lattice reorientation and leading to the formation of a fine-grained structure, are found.

Possible combinations of the electronic polarizability tensor components for oxygen and tantalum ions have been established based on the analysis of the refraction coefficients of LiТаO₃ crystal in the far-IR region. The local electric field on structurally nonequivalent ions in the LiТаO₃ unit cell was calculated within the modified point-multipole model. A combination of the electronic polarizability tensor components for oxygen and tantalum ions and their effective charges is established, which provides a good correspondence of the calculation results with the experimental data on LiТаO₃ crystals obtained by ⁷Li nuclear magnetic resonance and ¹⁸¹Та nuclear quadrupole resonance and with the known value of the crystal spontaneous polarization.

The state switching in an extended quasi-one-dimensional material is modeled by the stochastic formation of local new-state nuclei and their subsequent growth along the system axis. An analytical approach is developed to describe the influence of defects, dividing a sample into an ensemble of finite-length segments, on its state switching kinetics. As applied to magnetic systems, the method makes it possible to calculate magnetization curves for different defect concentrations and parameters of material.

The investigation of phonon dispersion in crystalline materials and collective atom motions in disordered matter such as liquids and glasses by inelastic X-ray scattering has attracted a diversified user community with the advent of 3^rd generation synchrotron sources. The present article provides a short historical account of the research field and discusses selected highlights of research performed on the ESRF inelastic scattering beamlines ID16 and ID28 in the past ten years.

The propagation of wave packets in media with polarizability frequency dispersion is analyzed based on asymptotic expansions.

The choice of beryllium-based material for the use in X-ray optics has been substantiated based on electron microscopy and X-ray diffraction data. The first results of applying refraction lenses made of this material are reported.

The crystal and magnetic structures of a solid solution of double perovskite Ba_{2 – x}Sr_xFeMoO₆ (x = 0–1.6) have been investigated by neutron diffraction. The high-resolution diffraction patterns have provided precise information about the changes in the crystal and magnetic structures with an increase in the strontium content and data on the behavior of the sample microstructure. Replacement of barium with strontium leads to a change in the lattice symmetry from cubic (x = 0, sp. gr. Fm3̄m)) to tetragonal (x = 0.4, sp. gr. I4/m). At x = 1.0, the symmetry is either tetragonal (sp. gr. I4/m) or orthorhombic (sp. gr. Fmmm), and at x = 1.6 the symmetry becomes again tetragonal (sp. gr. I4/m). The values of the Curie temperature and microstrain increase with an increase in the strontium content.

Specific stereochemical features of silicon in oxygen-containing compounds, including hybrid silicates with all oxygen atoms of SiO_n groups (_n = 4, 5, or 6) entering into the composition of organic anions or molecules, are described by characteristics of Voronoi—Dirichlet polyhedra. It is found that in rutile-like stishovite and post-stishovite phases with the structures similar to those of СаСl₂, α-PbO₂, or pyrite FeS₂, the volume of Voronoi—Dirichlet polyhedra of silicon and oxygen atoms decreases linearly with pressure increasing to 268 GPa. Based on these results, the possibility of formation of new post-stishovite phases is shown, namely, the fluorite-like structure (transition predicted at ~400 GPa) and a body-centered cubic lattice with statistical arrangement of silicon and oxygen atoms (~900 GPa).

The crystal structure of ilyukhinite, a new mineral of the eudialyte group, is studied by X-ray diffraction. The mineral found in pegmatite bodies of the Kukisvumchorr Mountain (Khibiny alkaline complex) is characterized by low sodium content, high degree of hydration, and predominance of manganese over iron. The trigonal cell has the following parameters: a = 14.1695(6) and c = 31.026(1) Å; space group R3m. The structure is refined to final R = 0.046 in the anisotropic approximation of atomic displacements using 1527F > 3σF. The idealized formula of ilyukhinite (Z = 3) is written as (H₃O,Na)₁₄Ca₆Mn₂Zr₃Si₂₆O₇₂(OH)₂ · 3H₂O. The new mineral differs from other representatives of the eudialyte group by the predominance of both oxonium in the N positions of extra-framework cations and manganese in the М2 position centering the tetragonal pyramid.

Phosphoribosylpyrophosphate synthetases (PRPP synthetases) are among the key enzymes essential for vital functions of organisms and are involved in the biosynthesis of purine and pyrimidine nucleotides, coenzymes, and the amino acids histidine and tryptophan. These enzymes are used in biotechnology for the combined chemoenzymatic synthesis of natural nucleotide analogs. Recombinant phosphoribosylpyrophosphate synthetase I from the thermophilic strain HB27 of the bacterium Thermus thermophilus (T. th HB27) has high thermal stability and shows maximum activity at 75°С, due to which this enzyme holds promise for biotechnological applications. In order to grow crystals and study them by X-ray crystallography, an enzyme sample, which was produced using a highly efficient producer strain, was purified by affinity and gel-filtration chromatography. The screening of crystallization conditions was performed by the vapor-diffusion technique. The crystals of the enzyme suitable for X-ray diffraction were grown by the counter-diffusion method through a gel layer. These crystals were used to collect the X-ray diffraction data set at the SPring-8 synchrotron radiation facility (Japan) to 3-Å resolution. The crystals belong to sp. gr. P2₁ and have the following unitcell parameters: a = 107.7 Å, b = 112.6 Å, c = 110.2 Å, α = γ = 90°, β = 116.6°. The X-ray diffraction data set is suitable for determining the three-dimensional structure of the enzyme at 3.0-Å resolution.

The influence of arsenic flow in a growth chamber on the crystal structure of GaAs grown by molecular-beam epitaxy at a temperature of 240°C on GaAs (100) and (111)A substrates has been investigated. The flow ratio γ of arsenic As4 and gallium was varied in the range from 16 to 50. GaAs films were either undoped, or homogeneously doped with silicon, or contained three equidistantly spaced silicon δ-layers. The structural quality of the annealed samples has been investigated by transmission electron microscopy. It is established for the first time that silicon δ-layers in “low-temperature” GaAs serve as formation centers of arsenic precipitates. Their average size, concentration, and spatial distribution are estimated. The dependence of the film structural quality on γ is analyzed. Regions 100–150 nm in size have been revealed in some samples and identified (by X-ray microanalysis) as pores. It is found that, in the entire range of γ under consideration, GaAs films on (111)A substrates have a poorer structural quality and become polycrystalline beginning with a thickness of 150–200 nm.

The (001) cleavage surface of vanadium pentoxide (V₂O₅) crystal has been studied by scanning tunneling spectroscopy (STM). It is shown that the surface is not reconstructed; the STM image allows geometric lattice parameters to be determined with high accuracy. The nanostructure formed on the (001) cleavage surface of crystal consists of atomically smooth steps with a height multiple of unit-cell parameter с = 4.37 Å. The V₂O₅ crystal cleavages can be used as references in calibration of a scanning tunneling microscope under atmospheric conditions both along the (х, y) surface and normally to the sample surface (along the z axis). It is found that the terrace surface is not perfectly atomically smooth; its roughness is estimated to be ~0.5 Å. This circumstance may introduce an additional error into the microscope calibration along the z coordinate.

The processes of gas-phase clusterization of zinc during dc magnetron sputtering of a zinc target in an argon atmosphere have been investigated. The influence of the working gas pressure and magnetron discharge current on the morphology and structure of the precipitates formed on substrates previously cooled to–50°С is studied. It is shown that dense textured (002)Zn layers with a columnar structure are formed at relatively low argon pressures in the chamber (P = 0.5 Pa) and low discharge currents (100 mA). X-ray amorphous deposits with a fractal coral-like structure arise on substrates at an extremely high argon pressure in the chamber (P = 5 Pa). An increase in the magnetron discharge current at an operating gas pressure of 5 Pa leads to the formation of polycrystalline layers on substrates; the intensity of the XRD peaks related to crystalline zinc increases with an increase in the discharge current. Possible mechanisms of the structural transformation of Zn deposits are considered.

ZnO–Zn сermet composite powder with a nanocrystalline structure has been obtained by grinding a mixture of initial powders in a ball mill under inert atmosphere conditions. A study of the transformation of the structural state of this powder as a result of long-term mechanical activation has shown the formation of a cermet composite, in which ZnO nanocrystallites with an average size less than 50 nm are incorporated into an almost completely amorphous metallic matrix.

Lysozyme crystal growth was studied using reagents of different purity of three trademarks— Seikagaku Corporation (sixfold recrystallized lysozyme), Sigma-Aldrich (threefold recrystallized lysozyme), and Hampton Research (threefold recrystallized lysozyme). Solutions of these reagents were investigated by small-angle X-ray scattering, dynamic light scattering (DLS), ultracentrifugation, and electrophoresis. It was found that crystal-growth and oligomerization processes are more intense in solutions of the reagent of higher purity. The dependences of the fraction of lysozyme oligomers on the supersaturation and purity of the solution are analyzed.

A VecDec4SAS program has been developed to provide a fast and easy description of the dynamics of any process occurring in a nanoparticle solution observed by the small-angle scattering technique. The process should be characterized by the some conditional initial and final stages, in fractions of which all intermediate data are expanded. The program makes it possible to estimate the adequacy of two-basis approximation and indicate the presence of an additional process introducing a systematic error into the initial data. Scattering curves for human serum albumin protein in solutions with pH 7.4 and 3.0 and a concentration of 20 mg/mL, obtained on the DICSY station at the National Research Centre “Kurchatov Institute” in the solution temperature range from 25 to 70°C, were taken to be initial data to illustrate the potential of the program.