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No 11 (2023)

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Articles

Formation of Whisker-Like Morphology on the Surface of Carbon Fiber under Magnetron Sputtering

Andrianova N.N., Borisov A.M., Metel A.S., Ovchinnikov M.A., Sleptsov V.V., Tsyrkov R.A.

Abstract

The effect of irradiation with hydrogen, helium, nitrogen and neon ions with an average energy of 0.8 keV on the surface morphology under magnetron sputtering of a high-modular carbon fiber made of polyacrylonitrile was studied experimentally. In all cases, a whisker-like relief was formed on the surface. The greatest height of whiskers was obtained under irradiation with nitrogen and neon ions, the lowest height and lower density of whiskers was obtained under irradiation with hydrogen ions. Comparison with irradiation of polyacrylonitrile carbon fiber with noble gas and nitrogen ions with energies of 10–30 keV shows that the whisker-like morphology complements the variety of types of ion-induced fiber surface morphology. The results obtained are discussed within the framework of existing models of formation of ion-induced morphological elements on the surface of graphite-like materials. It is assumed that there is a threshold in the number of radiation displacements created in the surface layer, leading to the observed qualitative difference in ion-induced morphology at low and high energies. The evaluations of the displacement profiles for the case of irradiation with hydrogen ions show several-fold fewer displacements than for other ions, which correlates with the observed differences in whiskering by selected ions and whisker growth factors observed in the experiment performed.

Poverhnostʹ. Rentgenovskie, sinhrotronnye i nejtronnye issledovaniâ. 2023;(11):3-8
pages 3-8 views

Investigation of Factors Determining the Efficiency of Interaction of Aluminum Alloys Activated with the Ga–In Eutectic with Water in Hydrogen Cartridges

Nizovskii A.I., Shmakov A.N., Kulikov A.V., Suprun E.A., Bukhtiyarov V.I.

Abstract

Using high-resolution X-ray diffraction and synchrotron radiation, as well as and scanning electron microscopy, it has been shown that the observed high reactivity of commercial aluminum alloys activated with the Ga–In eutectic is associated with the formation of the Al–Ga–In eutectic along grain boundaries in the entire material volume. The loss of material activity during storage under atmospheric conditions is due to the oxidation of the eutectic components. Activation with pure gallium leads to formation of AlGax solid solution, which has low activity in the reaction with water under neutral pH.

Poverhnostʹ. Rentgenovskie, sinhrotronnye i nejtronnye issledovaniâ. 2023;(11):9-15
pages 9-15 views

The Influence of Ta Coating on the Crystallization of Deformed Fe78Si13B9 and Al87Ni8Gd5 Amorphous Alloys

Chirkova V.V., Abrosimova G.E., Pershina E.A., Volkov N.A., Aronin A.S.

Abstract

The influence of the free volume on the crystallization processes of Fe78Si13B9 and Al87Ni8Gd5 amorphous alloys was studied by X-ray diffraction. To study the influence of the free volume, two methods of amorphous alloys deformation were carried out: ultrasonic treatment and multiple rolling. After deformation, a protective coating was applied to the amorphous alloys. It is shown that the deposition of a protective coating with a higher vacancy formation energy compared to the vacancy formation energy in the amorphous alloys under study is an effective way to maintain the free volume in the amorphous phase, since it is thermodynamically unfavorable for the free volume to migrate from the amorphous phase into the coating material. Experimental data indicate that the preliminary deformation of amorphous alloys leads to an increase in the amount of free volume. An increase in the amount of free volume and its maintenance by protective coating contributes to a significant crystallization acceleration of Fe78Si13B9 and Al87Ni8Gd5 amorphous alloys. The results obtained expand the existing ideas about the processes of crystallization of amorphous alloys and indicate the possibility of developing materials with different structural characteristics and, consequently, with different physicochemical properties.

Poverhnostʹ. Rentgenovskie, sinhrotronnye i nejtronnye issledovaniâ. 2023;(11):16-23
pages 16-23 views

Influence of Aluminium on the Structure and Electrical Properties of Amorphous Diamond-Like Silicon-Carbon Films

Popov A.I., Presnyakov M.Y., Domashevskaya E.P., Terekhov V.A., Semenov-Shefov M.A., Afanas’ev V.P., Chukanova T.S., Zezin D.A., Yemets V.M., Barinov A.D., Shapetina M.A.

Abstract

This article studies the influence of aluminium, a weak-carbide-forming metal, on phase composition, structure, and electro physical properties of amorphous diamond-like silicon-carbon films. The results of this study are compared with the influence on the same characteristics of strong-carbide-forming transition metals – titanium and hafnium. It is shown that the effects of aluminium and transition metals on the structure and properties of silicon-carbon films are fundamentally different. The addition of aluminium in a wide range of concentrations, in contrast to transition metals, does not lead to formation of a nano-crystalline phase in the films. The dependence of electrical conductivity on the aluminium concentration is smooth and monotonic, but in the case of transition metals, it has a pronounced percolation form. In addition, the absolute values of changes in electrical conductivity differ by orders of magnitude. The performed studies allowed us to conclude that the reasons for these differences are due to the interaction of metals with different chemical elements of the film. Transition metal atoms interact mainly with carbon atoms to form nanocrystals of highly conductive carbides. In contrast, aluminium atoms mainly interact with oxygen atoms and form an amorphous phase of aluminium oxide.

Poverhnostʹ. Rentgenovskie, sinhrotronnye i nejtronnye issledovaniâ. 2023;(11):24-32
pages 24-32 views

Surface Preparation and Investigation of Ohmic Film Contacts Formed by Various Methods to Thermoelements

Shtern M.Y., Sherchenkov A.A., Shtern Y.I., Rogachev M.S., Korchagin E.P.

Abstract

Methods were proposed and criteria were established for surface preparation of nanostructured thermoelectric materials for deposition of thin and thick film ohmic contacts. The parameters of the mechanical and chemical methods of thermoelectric material surface treatment before the deposition of contacts were established. The roughness and morphology of the surface of thermoelectric material samples and the films obtained have been studied. Criteria and optimal values of surface roughness of thermoelectric materials were established. The conditions of obtaining thin and thick film contacts were determined. Thin film contacts (thickness up to 300 nm) were obtained by magnetron sputtering of Ni. Thick film contacts were formed by chemical and electrochemical deposition of Ni. The obtained films contained various amounts of Ni. The electrical resistivity of Ni films obtained by chemical deposition was significantly higher than that of Ni films obtained by electrochemical deposition. The specific contact resistance of the metal–thermoelectric material system in the case of deposition of Ni films by magnetron sputtering was the smallest among the considered samples. And in the case of forming contacts by chemical deposition, it is comparable to that for Ni films formed by electrochemical deposition. The adhesion strength of Ni films obtained by various methods has high values exceeding the industry standard for film coatings in microelectronics. All obtained ohmic contacts satisfy the requirements for the construction of the efficient thermoelements by the electrical properties and adhesive strength.

Poverhnostʹ. Rentgenovskie, sinhrotronnye i nejtronnye issledovaniâ. 2023;(11):33-43
pages 33-43 views

Modeling of Multilayer Structures with Tunable Optical Characteristics

Tolkach N.M., Vishnyakov N.V., Litvinov V.G., Sherchenkov A.A., Trusov E.P., Glukhenkaya V.B., Pepelyaev D.V.

Abstract

Phase transition materials, in particular chalcogenide glassy semiconductors and Ge–Sb–Te system materials are of interest for application in optical information processing technologies. The uniqueness of these materials lies in the fact that they have a low-energy, fast and reversible phase transition, leading to a significant change in the refractive index in the infrared region of the optical spectrum. The model calculations carried out in the work made it possible to investigate the transformation of optical properties in multilayer structures consisting of SiO2, Si, Si3N4 layers and an active layer of a phase transition material when its phase state changes. The aim of these studies was to fulfill the condition of the lowest optical losses during transmission and reflection of radiation of 1550 nm in such structures in the case of amorphous and crystalline states of the active layer, respectively. As a result, the nine-layer “SiO2//111 nm Si/277 nm SiO2/111 nm Si/251 nm SiO2/10 nm Ge2Sb2Se4Te/241 nm SiO2/110 nm Si/276 nm SiO2/112 nm Si//SiO2” structure that most satisfies the specified conditions was designed.

Poverhnostʹ. Rentgenovskie, sinhrotronnye i nejtronnye issledovaniâ. 2023;(11):44-52
pages 44-52 views

Determination of the Thicknesses of Monolayer Coatings Exposed to Ion Bombardment by X-Ray Photoelectron Spectroscopy

Afanas’ev V.P., Lobanova L.G., Selyakov D.N., Semenov-Shefov M.A.

Abstract

The samples of monocrystalline silicon coated with golden nanolayers were investigated. The samples were obtained by two methods, namely, gold sputtering using Xe+ beam with the initial energy of 7 keV and the method of thermal deposition. Preliminary analysis of samples based on the deciphering of energy spectra of reflected protons with an initial energy of 25 keV was performed. By methods of X-ray photoelectron spectroscopy with angular resolution (Angle Resolved XPS) thicknesses of gold coatings on silicon were determined. Analysis of samples using X-ray photoelectron spectroscopy was performed by comparing the intensities of Au 4f and Si 2p maxima measured at different angles of photoelectron detection. The calculations carried out by traditional methods indicate a marked dependence of the calculated gold coating thickness on the angle of sight for the case of monolayer and submonolayer coatings. It is shown that such discrepancy is possible if gold is deposited on silicon in the form of clusters forming islands rather than in the form of a continuous homogeneous coating. The possibility of gold islands moving relative to silicon in the upper silicon layers that have been subjected to proton bombardment at sliding angles to the surface is discussed.

Poverhnostʹ. Rentgenovskie, sinhrotronnye i nejtronnye issledovaniâ. 2023;(11):53-59
pages 53-59 views

Formation of Zn-Containing Clusters in Implanted Si3N4 Film

Tereshchenko A.N., Privezentsev V.V., Firsov A.A., Kulikauskas V.S., Zatekin V.V., Voronova M.I.

Abstract

The results of the synthesis and study of Zn-containing clusters at the interface of a Si3N4/Si film implanted with 64Zn+ ions with a dose of 5 × 1016 cm–2 and an energy of 40 are presented. The Si3N4 film was preliminarily deposited on a silicon substrate from chemical vapor. Then, the implanted samples 10 × 10 mm in size were annealed in an oxidizing atmosphere (in air) with a step of 100°C for 1 h at each step in the temperature range 400–800°C. To study the profiles of zinc during annealing, the Rutherford backscattering method was used. The structure and composition of the film were studied using scanning electron microscopy in combination with energy dispersive spectroscopy, as well as photoluminescence. After implantation, individual clusters of metallic zinc with a size of about 100 nm or less were recorded near the surface of the Si3N4 film. It has been established that, during annealing, Zn clusters grow in the sample and the phase of metallic Zn gradually transforms into phases of its oxide ZnO and then, presumably, Zn2SiO4 silicide. After annealing at a temperature of 700°C, which is the most optimal for obtaining the ZnO phase, zinc oxide сlusters about 100 nm in size are formed in the Si3N4 film. A peak appears in the photoluminescence spectrum at a wavelength of 370 nm due to exciton luminescence in zinc oxide. After annealing at 800°C, the ZnO phase degrades and, presumably, the zinc silicide phase Zn2SiO4 is formed.

Poverhnostʹ. Rentgenovskie, sinhrotronnye i nejtronnye issledovaniâ. 2023;(11):60-66
pages 60-66 views

The Size Dependence of the Adsorption Properties of Nickel Clusters on the Surface of Aluminum Oxide

Magkoev Т.Т., Nadimi E., Tvauri I.V., Zaalishvili V.B., Ashkhotov O.G., Ashkhotova I.B.

Abstract

Despite the recent activity in the field of research on the properties of systems formed by the adsorption of metal atoms on the surface of oxides, many fundamental issues remain open. Finding out the fundamental features of the behavior of systems of the type under consideration will improve the technological basis for the practical development and application of existing materials. In this regard, in this work, studies of the Ni/Al2O3/Mo(110) system were carried out in ultrahigh vacuum using surface diagnostics methods. Using X‑ray photoelectron and electron Auger spectroscopy, low-energy ion backscattering spectroscopy, and infrared Fourier spectroscopy, it is shown that electronic and adsorption properties of nanoscale nickel clusters on the surface of aluminum oxide significantly depend on the size of the cluster. The properties of clusters no larger than 2 nm are determined by the formation of a bond polarized towards the oxide substrate at the Ni/Al2O3 interface. With the growth of the cluster, depolarization of this connection occurs with the redistribution of electron density to lateral bonds between Ni atoms. Such a dimensional dependence makes it possible to program the properties of metal clusters and the metal oxide system as a whole, in particular, to achieve the required electronic and adsorption-reaction parameters.

Poverhnostʹ. Rentgenovskie, sinhrotronnye i nejtronnye issledovaniâ. 2023;(11):67-71
pages 67-71 views

Synthesis and Structure of the Nanosized Cobalt Coatings on Porous Aluminum Oxide

Valeev R.G., Alalykin A.S., Beltiukov A.N., Kriventsov V.V.

Abstract

The results of studies of the morphology and chemical structure of cobalt coatings deposited by magnetron sputtering on nanostructured surfaces of porous alumina with different morphologies are presented. The morphology of porous alumina was specified by the anodization voltage in solutions of sulfuric (25 V) and oxalic (40 and 120 V) acids. Using scanning electron and atomic force microscopy, it has been shown that the coatings have morphological features, which are hexagonally arranged nanoparticles formed at the boundaries between pores. With an increase in the size of nanopores on the surface of the substrates, the size and shape of the morphological features of the deposited coatings change. According to X-ray absorption fine structure spectroscopy and fine structure spectroscopy of the near region of the X-ray absorption edge, there are changes in the local atomic structure of cobalt, in particular, cobalt in a coating sample deposited on the surface of porous alumina obtained by anodizing at a voltage of 25 V in sulfuric acid, oxidized more strongly, which is associated with greater chemical activity due to the smaller sizes of the nanoparticles that make up the coating. The results obtained will allow in the future to make a directed change in the formation of structure-sensitive properties, such as chemical and electrochemical activity, magnetic sensitivity, of the resulting coatings.

Poverhnostʹ. Rentgenovskie, sinhrotronnye i nejtronnye issledovaniâ. 2023;(11):72-77
pages 72-77 views

Superconducting Solenoid (7 T) Indirectly Cooled by Cryocoolers for THz Radiation

Bragin A.V., Volkov A.A., Kubarev V.V., Mezentsev N.A., Tarasenko O.A., Khrushchev S.V., Tsukanov V.M., Shkaruba V.A.

Abstract

The test results and performance characteristics of an indirectly crycooled superconducting solenoid to be used at the THz spectroscopy experimental station of free-electron laser at the Institute of Nuclear Physics, are presented. The superconducting solenoid with a winding diameter of 102 mm and a length of 0.5 m was designed for a magnetic field of 6.5 T. The warm bore diameter of 80 mm is available for THz spectroscopy experiments. The superconducting wire Cu/NbTi = 1.4 was used. The design implements passive protection methods due to sectioning and secondary connected circuits in case of a sudden quench. The required field uniformity of 0.5% was ensured by using an iron yoke and additional side windings. The cryogenics of the solenoid is based on two Sumitomo HI cryocoolers. The solenoid and iron yoke are cooled by the second stage of the cryocooler via copper links. The manufacturing technology of the solenoid is described in detail. The solenoid was tested in a liquid helium bath and in its own cryostat. Its characteristics meet the requirements of the experimental station. The obtained filed of 7.5 T is greater than the designed one due to overcooling up to 3.6 K. The magnetic field was measured both in a bath cryostat and in a design cryostat; the results corresponded to the design calculations. The solenoid cooling time is 13 days. The quench happened only twice, at 5.6 and 7.5 T.

Poverhnostʹ. Rentgenovskie, sinhrotronnye i nejtronnye issledovaniâ. 2023;(11):78-83
pages 78-83 views

Scanning Synchrotron X-Ray Fluorescence Microanalysis for Tephrochronological Studies

Darin A.V., Darin F.A., Sorokoletov D.S., Rakshun Y.V., Rogozin D.Y.

Abstract

On the border of China and North Korea, there is the only active stratovolcano in the eastern part of Asia – Paektusan (other names are Baitoushan, Changbaishan). It is widely known for one of the largest eruptions in the historical era, which occurred in the 10th century AD. On a volcanic activity scale, the event is rated at seven points, this is the largest eruption in the last millennium. Modern research shows that the eruption of the Paektusan volcano occurred in late autumn–winter 946 AD. This dating is supported by data obtained from the study of an ice core from North Greenland, in which traces of volcanic ash were found. At a depth of 860 mm (the age according to the calculation of annual layers is 942 AD ± 26 years), a layer 2–3 mm thick was found, which differed sharply in color and texture from the rest of the core material. Using a module of confocal X-ray microscopy, an optical section containing an anomalous layer was studied. 2D scanning with a focused beam of synchrotron radiation 20 µm in diameter was carried out. A large amount of microparticles with a high content of zirconium and yttrium was found inside the layer. The possibility of finding traces of the eruption of the Paektusan volcano is discussed.

Poverhnostʹ. Rentgenovskie, sinhrotronnye i nejtronnye issledovaniâ. 2023;(11):84-89
pages 84-89 views

X-Ray Transfocators a Tunable X-Ray Focusing Apparatus Based on Compound Refractive Lenses

Narikovich A.S., Korotkov A.S., Medvedskaya P.N., Barannikov A.A., Sinitsyn А.V., Lushnikov A.A., Panormov I.B., Zverev D.A., Lyatun I.I., Snigirev A.A.

Abstract

This paper presents a new generation of ultra-compact and high-vacuum cooled X-ray refractive lens-based transfocators for collimation, transport, and focusing of hard X-rays. The transfocator is an optical device capable of changing the position of focus depending on the number of X-ray refractive lenses, which are exposed along the optical path of X-ray radiation. The design features of the device allow the individual optical elements to be controlled independently of each other, providing a more flexible adjustment of the focal distance for a wide range of applications. The small overall dimensions and light weight of the devices allow them to be integrated into any synchrotron radiation station.

Poverhnostʹ. Rentgenovskie, sinhrotronnye i nejtronnye issledovaniâ. 2023;(11):90-100
pages 90-100 views

Nuclear Stopping for DFT Potentials with Attraction Well

Babenko P.Y., Zinoviev A.N.

Abstract

Using the interaction potentials obtained in the framework of the density functional theory, the nuclear stopping powers are calculated for the H, D, T–Be, C, W, systems necessary for calculating the plasma–wall interaction in thermonuclear research, as well as for the Kr–Si, Kr–Ge, O–Si systems, used in ion implantation into semiconductors. In the collision energy range 10–1000 eV, the obtained data differ from the SRIM data by 15–70%. The presence of a potential well leads to the appearance of an additional peak in the nuclear stopping power at low energies. A comparison of the classical calculations of the transport cross section with the semiclassical ones showed their identity at energies up to 0.3 eV.

Poverhnostʹ. Rentgenovskie, sinhrotronnye i nejtronnye issledovaniâ. 2023;(11):101-106
pages 101-106 views

The SKIF X-Techno Beamline Project

Nazmov V.P., Goldenberg B.G.

Abstract

Beamlines nowadays installed at synchrotron radiation centers typically pose different and sometimes even incompatible requirements to X-ray beams being utilized. Some techniques require minimum attainable beam cross-sections in order to enable microbeam techniques with the sample mapping. To the contrary, relatively broad X-ray beams with the uniform intensity distribution are needed to address problems related to X-ray irradiation-based processing of materials or fabrication of components and devices with X-ray lithography approaches. The present paper describes the concept of a novel beamline named X-Techno proposed for the synchrotron radiation facility SKIF. It would use synchrotron beams as wide as 100 mm in the horizontal plane in different spectral ranges with either out of three experimental chambers to study materials and manufacture micro and nanostructures. The beamline will be specifically suitable for studies of physicochemical properties of materials under intense X-ray irradiation within the spectral range from 2 to 70 keV.

Poverhnostʹ. Rentgenovskie, sinhrotronnye i nejtronnye issledovaniâ. 2023;(11):107-112
pages 107-112 views

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