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No 9 (2023)

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Articles

Investigation of the Biodistribution of Gd0.5La0.5F3:Eu Nanoparticles in the Internal Tissues of Laboratory Mice Using X-Ray Computed Tomography and X-Ray Fluorescence Analysis

Polozhentsev O.E., Khodakova D.V., Goncharova A.S., Pankin I.A., Soldatov A.V.

Abstract

The biodistribution of Gd0.5La0.5F3:Eu(15%) X-ray phosphor nanoparticles in the body and tissues of internal organs of balb/c laboratory mice was studied. Gd0.5La0.5F3:Eu(15%) nanoparticles were obtained by the hydrothermal synthesis at 250°C for 24 h. Using X-ray powder diffraction, transmission electron microscopy, and dynamic light scattering, it was shown that a hexagonal phase was formed in the resulting sample, and the average size of nanoparticles varied in the range 30–40 nm. In vivo experiments have shown that intravenous administration of an aqueous solution of nanoparticles accumulates the sample mainly in the liver and spleen, with the maximum concentration being reached during the first day. According to the results of post-mortem analysis of tissues by micro-CT, it was shown that these nanoparticles formed conglomerates, their distribution over the volume of the organ was homogeneous. X-ray fluorescent analysis of liver and spleen tissue fragments allowed for elemental analysis and mapping. Distribution maps of heavy elements in the composition of nanoparticles (Gd, La, Eu) were similar to Fe distribution maps, which indicated the uniform distribution of Gd0.5La0.5F3:Eu(15%) nanoparticles in the pulp of the internal tissues of the liver and spleen.

Poverhnostʹ. Rentgenovskie, sinhrotronnye i nejtronnye issledovaniâ. 2023;(9):3-10
pages 3-10 views

Surface Crystallization and Magnetization Reversal Processes in Amorphous Microwires

Aksenov O.I., Fuks A.A., Abrosimova G.E., Matveev D.V., Aronin A.S.

Abstract

The bulk-inhomogeneous crystallization of amorphous microwires of composition Fe73.8Cu1Nb3.1B9.1Si13 has been studied. An assumption was put forward about the influence of the non-uniform distribution of tensile and compressive stresses in the bulk of microwires on their crystallization. It has been established that at the initial stages of crystallization the crystallization occurs in the near-surface region of a microwire with a thickness of about 2.5 μm. It has been established that the sizes of nanocrystals in the surface region of microwire are about 10 nm. It was found that the formation of an amorphous nanocrystalline layer on the microwire surface leads to an increase in the Mr/MS ratio (ratio of remanent magnetization to saturation magnetization), which is associated with a decrease in the magnetic anisotropy due to a decrease in the stress level during heat treatment and nanocrystallization. Chemical etching of annealed microwires leads to a significant increase in the Mr/MS ratio, which is due to an increase in the relative volume of the central domain layer. The results obtained indicate the potential for creating composite amorphous-nanocrystalline structures based on microwires. In the case of microwires of Fe73.8Cu1Nb3.1B9.1Si13 composition, the predominant crystallization of the surface layer can increase the effect of the giant magnetic impedance. Such objects may have potential applications in sensorics, in particular, in magnetic field and strain sensors.

Poverhnostʹ. Rentgenovskie, sinhrotronnye i nejtronnye issledovaniâ. 2023;(9):11-17
pages 11-17 views

Investigation of the Corrosion Properties of Bulk Amorphous Metal Alloys Based on Zirconium

Yakovlev A.V., Balybin D.V., Fedorov V.A., Pluzhnikova T.N., Fedotov D.Y., Shlykova A.A.

Abstract

Corrosion resistance of zirconium-based amorphous alloys in simulating a biological fluid, as well as in aqueous solutions of hydrochloric acid (with HCl concentration 0.1, 0.2, 0.4 mol/L) was studied in this work. When studying the effect of simulating a biological fluid, the samples were exposed to the environment in two ways. In the first case, the sample was completely immersed in a corrosive liquid. In the second case, the sample was subjected to local action of a drop of biological fluid deposited on the surface. It has been established that prolonged exposure to the medium leads to the dissolution of the surface layer of the sample, while the local impact of drops practically does not affect the surface. Preliminary ion implantation of argon and nitrogen ions leads to a decrease in the effect of the biological fluid on the samples. Polarization curves are obtained for all investigated alloys. On the curves obtained during measurements on alloys in simulating a biological fluid, the cathode and anode branches have a standard form. It has been established that the polarization curves for zirconium-based alloys in an aqueous solutions (with HCl concentration 0.1, 0.2, 0.4 mol/l) depend on the elemental composition of the alloys. It has been established that in a sample without copper, the corrosion potential at different concentrations of HCl changes insignificantly. For a sample with a copper content of 15%, the corrosion potential shifts to the cathodic region with an increase in the concentration of hydrochloric acid. The polarization curves of the sample with a higher copper content of 45% are qualitatively different from the curves of the other samples. It is noted that, as in the previous sample, with an increase in the concentration of hydrochloric acid, the corrosion potential shifts to the negative region. It has been established that the corrosion resistance of amorphous alloys based on zirconium, which is the basis of the alloys under study, in the studied solutions increases in comparison with the crystalline one, which is due to the amorphous structure of the electrode material, which complicates the transition of the metal to the ionic state.

Poverhnostʹ. Rentgenovskie, sinhrotronnye i nejtronnye issledovaniâ. 2023;(9):18-24
pages 18-24 views

Multilayer ZrO2/Cr Coating for Protection of E110 Zirconium Alloy from High-Temperature Oxidation

Sidelev D.V., Ruchkin S.E., Syrtanov M.S., Pirozhkov A.V., Maximov P.N.

Abstract

Cr coatings with multilayer barrier composed of alternating ZrO2 and Cr layers with an individual thickness of each layer of 50 and 250 nm were prepared onto substrates made from zirconium E110 alloy using magnetron sputtering. The protective multilayer ZrO2/Cr coating on zirconium E110 alloy were studied under high-temperature oxidation in air at a temperature of 1100°C for 10, 20, 30 and 40 min. The lower rate of change in weight gain of samples having ZrO2/Cr barriers was found in comparison with samples coated by chromium during long-term oxidation tests. Diffraction measurements of samples were done under linear heating (50°С/min) in a range of temperature of 25–1250°С and next isothermal treatment for 20 min under high vacuum (10–3 Pa) using the in situ diffraction. It was found that the mutual diffusion of Cr-Zr at the interface between the protective coating having the multilayer barrier composed of alternating ZrO2 and Cr layers and zirconium alloy can be slowed down. This results in the retention of high content of α-Cr phase in the coating and, as a result, in the increase of the duration of the protective state of E110 alloy under the high-temperature oxidation in air.

Poverhnostʹ. Rentgenovskie, sinhrotronnye i nejtronnye issledovaniâ. 2023;(9):25-29
pages 25-29 views

Mechanism of Solid Solution Hardening: Quasilocalisation of Dislocation Kinks

Petukhov B.V.

Abstract

The sensitivity of the mechanical properties of materials to violations of the translational invariance of the crystal lattice makes it possible to manipulate these properties in the desired direction by doping or creating solid solutions. The paper theoretically studies the mechanisms of such manipulation in relation to materials in which the mobility of dislocations is controlled mainly by the potential relief of the crystal lattice – the so-called Peierls relief. Due to the concentration of alloying atoms in dislocation nuclei, which play the role of traps for these atoms, the dynamic properties of dislocations change, which also leads to modification of the macroscopic mechanical properties of the material. The theory of the effect of doping on the kink mechanism of overcoming the Peierls barriers is constructed taking into account the disordered content of solution atoms in dislocation nuclei. Correspondingly, the direct description of the kinetics of elementary processes characteristic of kinks has been replaced by a statistical description. The multidirectional effect of fluctuations in the solutes distribution, which increase the rate of formation of pairs of kinks, but inhibit the propagation of kinks along dislocation lines, is considered. Inhibition of kinks can lead to an anomalous nature of their mobility, so-called quasilocalisation. The conditions for the predominance of the accelerating or inhibiting factor corresponding in macroscopic terms to the hardening or softening of the material are found.

Poverhnostʹ. Rentgenovskie, sinhrotronnye i nejtronnye issledovaniâ. 2023;(9):30-36
pages 30-36 views

Сomposites with a Matrix Based on Niobium and Molybdenum Reinforced with Sapphire Fibers

Kiiko V.M., Korzhov V.P., Kurlov V.N.

Abstract

Single-crystal sapphire fibers were obtained by the Stepanov method/EFG – Edge defined Film-fed Growth. The procedure for obtaining them is described. Mechanical testings of the fibers were carried out according to the presented scheme, and the dependences of the ultimate deformation and strength of the fibers on the length were determined. The dependences are power-law, and decrease with the length of the fibers. The strength of the obtained fibers corresponds to the world level and meets the conditions for their use as reinforcing for high-temperature composite materials. From workpieces containing layer-by-layer unidirectionally arranged sapphire fibers, niobium powder, metal foils of molybdenum and aluminum, layered-fibrous composites were obtained by solid-phase diffusion welding under load. Using scanning electron microscopy with X-ray analysis, the structure of the composites was studied, it was found that, in addition to the initial components, it includes intermetallic compounds of niobium, molybdenum and aluminum, as well as solid solutions of these metals formed in the technological process. As a result of mechanical testing of composite samples, deformation curves of load-deflection dependences were obtained, which, together with developed fracture surfaces, indicate the non-brittle nature of the fracture of composites containing brittle components. The dependences of the strength of composites on temperature in the range of 20–1400°C are obtained, which meet the requirements for high-temperature structural materials of this kind.

Poverhnostʹ. Rentgenovskie, sinhrotronnye i nejtronnye issledovaniâ. 2023;(9):37-43
pages 37-43 views

Layered Composite Materials Based on Ti/Ta/Hf/Ceramic to Solve Tasks under Extreme Conditions

Kamynina O.K., Vadchenko S.G., Kovalev I.D., Prokhorov D.V.

Abstract

Layered composite materials Ti/Ta/Hf/ ceramic were produced via self-propagating high-temperature synthesis (SHS) of pre-structured samples using metal foils (Ti, Hf, Ta, Ni) and reaction tapes (Ti + 0.65C), (Ti + 1.7B) and (5Ti + 3Si). Reaction tapes were prepared by cold rolling from powder mixtures. The microstructure, elemental and phase compositions of the synthesized multilayer composite materials were characterized by Scanning Electron Microscopy (SEM) and X-ray analysis. Their flexural strength was determined according to the scheme of three-point loading at temperatures of 25 and 1100°С. The microstructure analysis of produced materials showed that the joining in the combustion mode of metal foils and reaction tapes is provided due to reaction diffusion, mutual impregnation and chemical reactions occurring in reaction tapes and on the surface of metal foils. The formation of thin intermediate layers in the form of cermets and eutectic solutions provides the synthesized multilayer materials with good strength properties (up to 275 MPa at 25°С, up to 72 MPa at 1100°С). These results are of interest for the development of construction materials operating under extreme conditions.

Poverhnostʹ. Rentgenovskie, sinhrotronnye i nejtronnye issledovaniâ. 2023;(9):44-51
pages 44-51 views

On the Radiation Stability of ZnO Powders Modified with Own Nanoparticles

Mikhailov M.M., Yuryev S.A., Lapin A.N., Goronchko V.A.

Abstract

Changes in the diffuse reflectance spectra (∆ρλ) and integral absorption coefficient (Δаs) in the range of 0.2–2.5 µm were studied after modification of zinc oxide powders with few µm particles (mZnO) via own nZnO nanoparticles of various concentrations in the range of 0.1–10.0 wt %. A decrease in the reflection coefficient (ρ) in the range of 0.4–1.0 µm and its increase in the range of 1.0–2.5 µm in the modified mZnO/nZnO powders was established. Electron irradiation (Е = 30 keV, F = 2 × 1016 cm–2) of mZnO, nZnO, and mZnO/nZnO powders with different concentrations of nanoparticles showed that the optimal concentration of nanoparticles is 5 wt %. The radiation stability of the modified powder at this concentration increased by a factor of 2.95, the radiation stability of a nanopowder is more than 2 times higher than that of a powder with particles a few microns in size. When irradiated with electrons all three types of powders form their own point defects, which absorb in the visible region, and free electrons, which absorb in the near-IR region.

Poverhnostʹ. Rentgenovskie, sinhrotronnye i nejtronnye issledovaniâ. 2023;(9):52-57
pages 52-57 views

Determining the Collimation Degree for a Coherent X-Ray Beam Using a Planar Multilens Interferometer

Zverev D.A., Yunkin V.A., Kuznetsov S.M., Barannikov A.A., Sorokovikov M.N., Voevodina .A., Snigirev A.A.

Abstract

A method is proposed for determining the degree of collimation of a coherent X-ray beam using a planar multilens interferometer. The method is based on analyzing Talbot images, which are periodic patterns of interference fringes formed by the interferometer at appropriate distances. The high sensitivity of the position and period of the interference fringes to the shape of the X-ray beam wave front makes it possible to determine the degree of its collimation, as well as to evaluate the coherent properties of the radiation. The effectiveness of the proposed approach has been experimentally demonstrated at the ID15B beamline of the ESRF synchrotron radiation source. A theoretical study has been carried out, and the corresponding results of computer simulation have been presented. The experimentally data obtained fully correspond to the theoretical estimates.

Poverhnostʹ. Rentgenovskie, sinhrotronnye i nejtronnye issledovaniâ. 2023;(9):58-64
pages 58-64 views

Kinetics of Hydrogen Evolution during Amminborane Hydrolysis with Cobalt-Based Catalysts

Dyankova N.Y., Lapin N.V., Grinko V.V., Vyatkin A.F.

Abstract

The kinetics of hydrogen evolution during the hydrolysis reaction of aqueous solutions of amminborane with cobalt-based catalysts deposited on various substrates – Co3O4/ZnO, Co/ZnO, Co3O4/zeolite, Co/zeolite, as well as Co(OH)2 powder, was studied. In each case, the reaction order, the rate constants and apparent activation energy of the reaction, and the rate of hydrogen evolution during hydrolysis in the temperature range 35–80°C were determined. In all cases, an amminborane solution with a concentration of 0.078 M was used. The amount of the active part of the catalysts was determined by the chemical method and was 7.5–10% of the total weight of the catalyst. For low-temperature Co–B and Co(OH)2 catalysts, the kinetic dependences corresponded to the zero or close to zero reaction order. When using the catalysts Co3O4/ZnO, Co/ZnO, Co3O4/zeolite, Co/zeolite, the first order of the reaction was observed. The maximum rate of hydrogen evolution at 80°C was 3125 mL H2 · (g-cat–1) · min–1 for Co/ZnO catalyst (turnover frequency TOF = 8.2 min–1) and 3750 mL H2 · (g-cat–1) · min–1 for Co–B catalyst (TOF = 11.7 min–1), respectively. The values of the apparent activation energy of the reaction of catalytic hydrolysis of amminborane were calculated for the catalysts: Co3O4/ZnO – 26.0, LT Co–B – 44.8, Co(OH)2 black – 43.4, Co(OH)2 blue – 47.4 kJ/mol, respectively.

Poverhnostʹ. Rentgenovskie, sinhrotronnye i nejtronnye issledovaniâ. 2023;(9):65-73
pages 65-73 views

Properties of Deformable Medium Element as a Factor of Superplasticity of Metallic Materials

Solov’eva Y.V., Lipatnikova Y.D., Vovnova I.G., Starenchenko V.A.

Abstract

Theoretical study of the phenomenon of superplasticity of metallic materials has been carried out. Numerical calculations were performed on the basis of a two-level finite element model of an elastoplastic medium. The plastic properties of the deformable medium element determining the deformation by uniaxial tension in superplasticity mode were found. It was shown that depending on the shape of the stress-strain curve (σ–ε) of the medium element, the various types of plastic flow localizations were observed at the macroscale level. The nonmonotonic dependence σ–ε of the deformable medium element having single maximum was determined as the condition for the appearance of a stable fracture neck. In the case when the dependence σ–ε characterized by the strengthening of the elementary volumes with two maxima, a propagating (running) neck was observed, then a second (counter) neck appeared, while further tension led to the appearance of the third stable neck in which fracture occurred. In the case of more complex oscillating shape of σ–ε curve the multiple running necks were observed. The movement of the multiple necks propagating along the sample leads, ultimately, to a uniform picture of the deformation and made it possible to achieve the strain values observed in superplasticity mode.

Poverhnostʹ. Rentgenovskie, sinhrotronnye i nejtronnye issledovaniâ. 2023;(9):74-81
pages 74-81 views

On Influence of the Parameters of a Layered Target and Electron Beam on Diffracted Transition and Parametric X-Ray

Blazhevich S.V., Shevchuk O.Y., Noskov A.V., Fedoseev A.E.

Abstract

The paper considers parametric X-ray radiation (PXR) and diffracted transition radiation (DTR) of a beam of relativistic electrons crossing a target with a periodic layered structure in the Bragg scattering geometry. The general case of asymmetric electron reflection relative to the target surface is considered, that is, when the target layers occupy a place at right angles to its surface. Within the framework of the two-wave approximation of the dynamic theory of diffraction expressions are obtained that describe the angular densities of PXR, DTR and their interference. Computational calculations of the angular densities are carried out for various values of the target parameters and a variety of quantities. The density-to-flow ratio depends on the density and on the thickness-to-thickness ratio of the periodic structure. At a large electron value, the angular dependence of the DTR on the consumed mass increases.

Poverhnostʹ. Rentgenovskie, sinhrotronnye i nejtronnye issledovaniâ. 2023;(9):82-88
pages 82-88 views

Some Methods for Improving the Quality of Magnetic Force Microscopy Images

Temiryazev A.G., Temiryazeva M.P.

Abstract

Some factors affecting the quality of magnetic force microscopy images are considered. The main attention is paid to the deterioration of the quality of scans caused by contamination of the probe. It is shown that contamination can occur both during scanning and during storage of the probe. These two different sources of contamination show up differently in images, and different methods must be used to eliminate them. A likely source of probe contamination is the gel used in probe storage and shipping boxes. The magnetic coating of cantilevers can be a catalyst for a chemical reaction leading to the formation of liquid hydrocarbons. The liquid contaminants act as probe functionalizers. When the probe is moved away from the surface, mechanical bonds can be maintained between them due to the molecular chains adsorbed on the probe. Depending on the degree of pollution, the presence of such a connection can lead either to the appearance of stripes in the image of the magnetic structure, or to the complete disappearance of the magnetic contrast. A modification of the standard procedure for magnetic measurements, i.e., the introduction of an additional bounce into the two-pass technique (lift mode), makes it possible to completely eliminate the parasitic influence of this effect.

Poverhnostʹ. Rentgenovskie, sinhrotronnye i nejtronnye issledovaniâ. 2023;(9):89-95
pages 89-95 views

Use of Special Devices for X-Ray Interferometric Investigation of Structural Imperfections in Single Crystals

Drmeyan H.R., Vasilyan M.S.

Abstract

A universal device for X-ray interferometric study of structural defects in single crystals has been designed, manufactured and tested. The device can serve both for scratching the surface of the interferometer crystal blocks and for bending it. A technology for generating dislocation in an interferometer block is also proposed. It has been experimentally proved that the moiré topographic patterns obtained using a double X-ray interferometer depend on the orientation of the reflection planes relative to the defect (dislocation). It is shown that multiple interferometers make it possible to simultaneously observe images of various structural imperfections. The results obtained make it possible to judge the spatial orientation of defects and the distribution of strain fields caused by these defects, i.e., strain fields can be visualized as X-ray moiré patterns. The results obtained in the work can form the basis for solving the inverse task, namely, the restoration of mechanical tension fields in the interferometer crystal blocks using the decoding of moiré patterns.

Poverhnostʹ. Rentgenovskie, sinhrotronnye i nejtronnye issledovaniâ. 2023;(9):96-102
pages 96-102 views

Neutron Irradiation Effect on the Spectral Characteristics of InxGa1 – xN LEDs

Tkachev O.V., Dubrovskikh S.M., Koksharova K.D., Fedorets A.V.

Abstract

The results of studying the neutron irradiation effect on the spectral characteristics of InxGa1 – xN LEDs are presented. The mechanism responsible for the shift of the emission spectra maximum of LEDs under the neutron influence has been determined. The coherence is shown between the radiation sensitivity of the spectral characteristics of the sample active layers and the composition of InxGa1 – xN solid solution. An analytical calculation has been carried out to estimate the possible maximum shift of the luminescence spectrum of InxGa1 – xN LEDs after neutron exposure.

Poverhnostʹ. Rentgenovskie, sinhrotronnye i nejtronnye issledovaniâ. 2023;(9):103-109
pages 103-109 views

On the Possibility of Observing the Effect of Quantization of the Orbital Momentum, during the Passage of Laser Radiation through an Optical Fiber

Kalashnikov N.P., Olchak A.S.

Abstract

The speed of propagation of optical radiation in an optical fiber is noticeably lower than the speed of light in vacuum. This fact opens the possibility to consider the propagation of light in fiber in the so-called comoving frame of reference. This type of consideration proved to be very useful and helping, for example, in studying the motion of ultrarelativistic charged particles and gamma rays in ordered media (channeling effect). This type of consideration makes it possible to notice some simple, albeit rather unexpected, macroscopic quantum effects that can manifest themselves when laser radiation passes through optical fibers. In particular, when photons propagate along an optical fiber twisted into a helix, at certain parameters of the helix, the effect of quantization of the moment of the photon momentum should reveal itself. Attracting attention to the possibility of such an effect is the goal of this note, which contains the formulation of the conditions and estimates of the parameters under which the effect of quantization of the angular momentum of photons moving along a spiral trajectory should be observed.

Poverhnostʹ. Rentgenovskie, sinhrotronnye i nejtronnye issledovaniâ. 2023;(9):110-112
pages 110-112 views

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