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Vol 12, No 6 (2018)

Article

Mössbauer and Magnetic Studies of Doped Lanthanum Manganite La1 – xCaxMn0.98Fe0.02O3 + δ (x = 0.05, 0.10, 0.20): I. Nonstoichiometric Composition

Pchelina D.I., Medvetskaya I.Y., Chistyakova N.I., Rusakov V.S., Sedykh V.D., Alekhina Y.A.

Abstract

Mössbauer and magnetic studies of Ca-doped lanthanum manganites La1 – xCaxMn0.98Fe0.02O3 + δ (x = 0.05, 0.10, 0.20) of a nonstoichiometric composition are performed. An increase in the Ca concentration and a decrease in the interstitial oxygen quantity results in a decreasing electric-field gradient in the region of the Fe atomic nucleus due to the spatial rearrangement of the charge of surrounding atoms. The Mössbauer spectra of all studied lanthanum-manganite samples demonstrate a relaxation character at low temperatures, which can be associated with the presence of small-sized magnetic clusters. This finding correlates with the results of magnetic investigations. The values of the coercive force, saturation magnetization, and blocking temperature are determined.

Journal of Surface Investigation: X-ray, Synchrotron and Neutron Techniques. 2018;12(6):1047-1051
pages 1047-1051 views

Blistering in Molybdenum Foils under Exposure to the Glow Discharge of D2‒N2 Mixtures

Gorodetsky A.E., Bukhovets V.L., Zalavutdinov R.K., Markin A.V., Kazansky L.P., Arkhipushkin I.A., Rybkina T.V., Zakharov A.P., Voytitsky V.L., Mukhin E.E., Razdobarin A.G.

Abstract

The evolution of indestructible blistering in molybdenum foils with the Mo {100} texture is investigated in dc glow discharge in a D2–N2 mixture with a nitrogen molar fraction in the mixture varying from zero to unity at 100 V potential negative with respect to plasma, a total pressure of 15 Pa, and temperatures of 30–60°C. After the addition of 0.01N2 to the deuterium discharge, the surface area occupied by the blisters increases from 2 to 5% and reaches its maximum of 11% upon exposure to D2−0.04N2 mixture discharge (the fluence is 4 × 1019 cm–2). Afterward, the area decreases, and blistering is absent in the pure N2 discharge. The amount of deuterium desorbed from the samples upon heating also increases with the addition of nitrogen. In accordance with X-ray photoelectron spectroscopy data, a nitride layer about 5 nm thick is formed if small amounts of N2 are added to D2. This layer is assumed to slow both the recombination rate of atomic deuterium coming from the material bulk to the surface and the transfer of D2 molecules into the gas phase. At the same time, the nitride layer increases the diffusion flux of D atoms into the foil bulk, promoting blister growth.

Journal of Surface Investigation: X-ray, Synchrotron and Neutron Techniques. 2018;12(6):1052-1060
pages 1052-1060 views

Synthesis of Rhenium-Silicide Microcrystals in a Tin Melt

Solomkin F.Y., Orekhov A.S., Sharenkova N.V., Khavrov G.D., Isachenko G.N., Zaitseva N.V., Klechkovskaya V.V.

Abstract

The present work is aimed at discussing the possibility in principle of obtaining rhenium-silicide microcrystals in tin melt at temperatures of 200–250 K below those used in the synthesis of pure components. The formation of rhenium silicides is confirmed by X-ray diffraction and scanning electron microscopy data. According to phase diagrams, neither rhenium nor silicon is soluble in tin, which does not allow the process to be described in the context of classical solution-melt crystallization theory. In this case, Sn is assumed to be a catalyst in the high-temperature chemical reaction between rhenium and silicon, favoring a decrease in the silicide-formation temperature and opens up the possibility of producing polycrystalline layers of these materials with a temperature gradient.

Journal of Surface Investigation: X-ray, Synchrotron and Neutron Techniques. 2018;12(6):1061-1065
pages 1061-1065 views

In Situ Observation of the Phase Transition of a Ferroelectric Triglycine Sulfate Crystal by Piezoresponse Force Microscopy

Tolstikhina A.L., Gainutdinov R.V., Belugina N.V.

Abstract

The second-order phase transition in a ferroelectric triglycine sulfate crystal is studied in situ by piezoresponse force microscopy. For the first time, the formation of a metastable one-dimensional quasiperiodic polarized structure is observed in the critical region of the phase transition, within one degree near the Curie temperature. Via image processing, the temperature dependence of the parameters of the quasiperiodic structure is studied. At a temperature exceeding the phase-transition point by one degree or more, the usual domain structure is formed, the width of the domains and the spread of the widths with respect to their mean value increase significantly.

Journal of Surface Investigation: X-ray, Synchrotron and Neutron Techniques. 2018;12(6):1066-1072
pages 1066-1072 views

Study of the Structure of Polyphthalocyanines by Transmission Electron Microscopy

Sedlovets D.M., Korepanov V.I., Khodos I.I.

Abstract

Two-dimensional polymers are highly promising materials for microsystems technologies and fundamental science. Some of the most interesting, but relatively unstudied, materials of this kind are polyphthalocyanines. These are a unique class of organometallic polymers with a two-dimensional conjugated structure and variable electronic properties. Since polyphthalocyanines of a high degree of polymerization can be obtained only as thin films and not as a bulk crystal, their study and characterization is a complicated scientific challenge. In this work we demonstrate the potential of transmission electron microscopy as a key tool in characterizing thin films. In particular, transmission-electron-microscopy data provide a basis for interpreting the Raman spectra of polyphthalocyanines, and also make possible interpretation of the crystal structure of the two-dimensional polymer.

Journal of Surface Investigation: X-ray, Synchrotron and Neutron Techniques. 2018;12(6):1073-1076
pages 1073-1076 views

Influence of the Substrate Type on the Surface Morphology of Cu2ZnSnSe4 Thin Films

Baraishuk S.M., Tkachenko T.M., Stanchik A.V., Gremenok V.F., Bashkirov S.A., Wiertel M., Budzynski M., Turovets A.I., Yakovenko Y.S.

Abstract

Investigations into the influence of the substrate type (a glass substrate with a molybdenum sublayer, tantalum and molybdenum foils) on the surface morphology of Cu2ZnSnSe4 thin films obtained by selenization of electrochemically deposited and preliminary annealed metallic precursors are presented. Metal foils are attractive for use as substrates of solar cells in both ground and space objects due to their light weight, flexibility, and the possibility of using the commercial roll-to-roll technology of film fabrication, leading to a reduction in the cost. At different stages of Cu2ZnSnSe4 film preparation, their surface morphology is studied by atomic-force microscopy and scanning electron microscopy in combination with energy-dispersive spectrometry. The metal substrate morphology is demonstrated to have an insignificant effect on the surface morphology of Cu2ZnSnSe4 films, indicating that flexible-foil substrates are promising for the production of thin-film solar cells.

Journal of Surface Investigation: X-ray, Synchrotron and Neutron Techniques. 2018;12(6):1077-1081
pages 1077-1081 views

On the Surface Micromorphology and Structure of Stainless Steel Obtained via Selective Laser Melting

Afanasieva L.E., Ratkevich G.V., Ivanova A.I., Novoselova M.V., Zorenko D.A.

Abstract

The regularities of the formation of the surface micromorphology and structure in stainless steel prepared via the selective laser melting of CL20ES powder are investigated. It is demonstrated that samples with optimal microgeometric characteristics possess the largest values of the density and microhardness and a low level of imperfection.

Journal of Surface Investigation: X-ray, Synchrotron and Neutron Techniques. 2018;12(6):1082-1087
pages 1082-1087 views

On the Role of the Proton Component in the Evolution of the Morphology of K-208 Glass under Combined Electron–Proton Irradiation

Khasanshin R.H., Novikov L.S.

Abstract

By the methods of atomic force microscopy (AFM) we investigate the surfaces of samples of K-208 glass after separate and combined irradiation in a vacuum chamber with a residual pressure of pv = 10−4 Pa with protons and electrons with energies of 20 and 30 keV, respectively. At flux densities of protons φp and electrons φe from 1011 to 5 × 1012 cm–2 s–1, the fluences of the particles Φp and Φe vary in the range of 1014–5 × 1016 cm–2. The obtained results allow us to state the following: the character of changes in the morphology of the samples under the action of protons and electron–proton plasma for φp <5 × 1012 cm–2 s–1 at φe: φp < 3 coincides and is due to radiation-stimulated stresses, reorganization of the glass network and the formation of gas-filled bubbles; at φp ≥ 5 × 1012 cm–2 s–1, the change in the morphology of the glass is determined by the mass transfer caused by local heating of the near-surface layer. In the case of proton irradiation, a model is proposed that describes the process of the field migration of sodium ions, which plays a key role in restructuring of the glass microstructure and the release of atoms of non-bridging oxygen.

Journal of Surface Investigation: X-ray, Synchrotron and Neutron Techniques. 2018;12(6):1088-1098
pages 1088-1098 views

Investigation of Changes in the Structure and Adhesion Properties of the Surface of Tread Tire Rubber during Friction

Shcherbakova O.O., Zagorskiy D.L., Bukovskii P.O., Yusupov A.A., Morozov A.V., Muravyeva T.I., Gainutdinov R.V.

Abstract

Different types of tread rubbers used in pneumatic tires of different applications are studied in the present work. The influence of various rubbers used in manufacturing treads on the rubber surface structure and its tribological, mechanical, and adhesive properties is estimated. A study and comparative analysis of the results of tribological tests and microscopic studies are performed. Microscopy of the sample surfaces is performed both before and after the tribological tests. To visualize the surface, the methods of scanning electron microscopy (combined with elemental analysis) and scanning probe microscopy are used. The character of changes occurring on the surface during friction, which is simulated on a tribometer with a rubber ring–disk contact circuit, is studied using these microscopy methods. It is established that the worn surfaces of all elastomers under study have a close structure and typical surface microrelief, but have different adhesion and mechanical properties depending on the type of rubber used in the rubber base and the used fillers. It is noted that high values of the sliding-friction coefficient and similarity of the rubber surface structures prove that their abrasive wear mechanisms are identical. The performed tribological laboratory tests show that the friction coefficient of the tread rubbers at high temperatures decreases with an increase in the normal load, while the opposite trend is observed at low temperatures. It is established that the change in the relaxation properties of rubbers due to temperature changes greatly affects the dependence of the friction coefficient on the sliding speed, while the energy loss due to friction is maximal in the temperature range of 15–20°C.

Journal of Surface Investigation: X-ray, Synchrotron and Neutron Techniques. 2018;12(6):1099-1107
pages 1099-1107 views

Nanotribology of Aqueous Solutions of Monobasic Carboxylic Acids in a Copper Alloy‒Steel Tribological Assembly

Burlakova V.E., Milov A.A., Drogan E.G., Novikova A.A.

Abstract

The tribological properties of the “copper alloy–carboxylic acid‒steel” system are studied. It is found that the wear-free mode accompanied by an increase in the pH of lubricant solutions, a decrease in the electrical conductivity, and a variation in the friction-surface charge is implemented in the “copper alloy–valeric acid–steel” and “copper alloy–caproic acid–steel” tribosystems. With the help of quantum-chemical calculations via the UB3LYP/Lanl2DZ method, it is demonstrated that the total charge of a metal cluster, the local distribution of electron and spin densities at copper atoms, and the structure of hydrocarbon radicals of carboxylic acids affect the physicochemical properties of the system during the formation of servovite films.

Journal of Surface Investigation: X-ray, Synchrotron and Neutron Techniques. 2018;12(6):1108-1116
pages 1108-1116 views

Formation of Vortex Motion by Capillary Waves on the Surface of Water

Filatov S.V., Khramov D.A., Kravchenko I.V., Likhter A.M., Levchenko A.A.

Abstract

The processes of the formation and decay of vortex motion on the surface of water are studied experimentally. The vortex motion is formed by capillary waves, which are generated as a result of harmonic oscillations of a cell with water in the vertical direction. It is shown that, at oscillation amplitudes smaller than the critical value, a vortex lattice with a period that is equal to the excitation wavelength is formed. The characteristic time of the formation and decay of vortex motion is close to the time of viscous damping of the pumping wave. At pumping amplitudes that are greater than the critical value, a vortex lattice is initially formed on the surface; then it is destroyed gradually by large-scale movements. The energy distribution over the wave vector can be described by a power function that is close to k–5/3. It is suggested that large-scale vortex motion arises as a result of the interaction of low-frequency waves appearing on the surface as a consequence of the nonlinear interaction of waves.

Journal of Surface Investigation: X-ray, Synchrotron and Neutron Techniques. 2018;12(6):1117-1123
pages 1117-1123 views

Mechanically Activated Mica as an Inert Filler for Heterogeneous Ion-Conducting Composites

Asvarov A.S., Akhmedov A.K., Amirov A.M., Rabadanova D.I., Muslimov A.E., Kanevsky V.M.

Abstract

It is demonstrated that mica-particle agglomerates disintegrate, its effective grinding occurs, and surface properties are modified under the condition that the mixture of muscovite and zinc powders is jointly mechanically activated in a ball grinder in an inert-gas atmosphere. Superfine muscovite extracted from the mechanically activated mixture by the chemical etching of a metal component can be used as a filler for heterogeneous ion-conducting nanocomposite systems.

Journal of Surface Investigation: X-ray, Synchrotron and Neutron Techniques. 2018;12(6):1124-1126
pages 1124-1126 views

Evolution of Foamed Liquids Structure

Tumachev D.D., Gavrilov S.A., Likhter A.M., Slavnetskov I.O., Yuvchenko S.A., Zymnyakov D.A.

Abstract

In this article the conducted experiments resulted in identifying a power nature of dependence of an average radius of bubbles in the model foam metastable samples on time with a value close to 0.5. The special experimental setup has been developed for studying the dependence of the average radius of gas bubbles in the model foam metastable samples on time. Within the assumption of a thermally-activated mechanism of the gas phase diffusion through bubble walls, the analysis of temperature influence on behavior of average radius dependences on time allowed to estimate molar energy of the process activation.

Journal of Surface Investigation: X-ray, Synchrotron and Neutron Techniques. 2018;12(6):1127-1129
pages 1127-1129 views

Microstructure and Microhardness of Rapidly Cooled Bi–38 wt % Sn, Additionally Doped with Lead

Shepelevich V.G.

Abstract

The results of investigating the microstructure and microhardness of rapidly cooled (BiSn)‒x wt % Pb (x = 0‒8) alloys are presented. Rapidly cooled foils consist of bismuth, β-tin, and the ε-phase. The textures \((10\bar {1}\bar {2})\) bismuth, \((100)\) β-tin and \((10\bar {1}0)\) ε-phase are formed in the foils. Changes in the foil microstructure and microhardness at room temperature are investigated.

Journal of Surface Investigation: X-ray, Synchrotron and Neutron Techniques. 2018;12(6):1130-1134
pages 1130-1134 views

Synthesis and X-ray Diffraction Studies of Cu2ZnGexSn1 – xSe4 Solid Solutions

Sheleg A.U., Hurtavy V.G., Chumak V.A.

Abstract

Quaternary compounds (Cu2ZnGeSe4 and Cu2ZnSnSe4) and solid solutions on their basis are prepared via single-temperature synthesis from Cu, Zn, Ge, Sn, and Se. The crystallographic characteristics of the synthesized compounds and Cu2ZnGexSn1 – xSe4 solid solutions are determined using the X-ray diffraction method at room temperature. It is found that parameters a and c reduce with increasing Ge concentration.

Journal of Surface Investigation: X-ray, Synchrotron and Neutron Techniques. 2018;12(6):1135-1137
pages 1135-1137 views

Exact Solution of the Problem of Bound Electronic States in Graphene

Belosludzev A.V., Savinsky S.S.

Abstract

In graphene with a gap in the electronic spectrum, the problem of bound states of an electron in the field of an impurity ion with the charge Z is considered. Parameter Z is the effective ion charge; it includes the permittivity of graphene. Analytical solution of the Schrödinger equation in the problem under consideration leads to a formula which contains two numbers determining the quantum state of the electron: the total pseudospin moment and the radial quantum number. The sign of the effective screening ion charge Z determines the positions of levels near the conduction or valence band of graphene. Accordingly, the energy levels can be interpreted as donor or acceptor electronic states in the gap.

Journal of Surface Investigation: X-ray, Synchrotron and Neutron Techniques. 2018;12(6):1138-1141
pages 1138-1141 views

On the Impact of Polyethylene Glycol on the Structure of Aqueous Micellar Solutions of Sodium Oleate According to Small-Angle Neutron Scattering

Artykulnyi O.P., Petrenko V.I., Bulavin L.A., Almasy L., Grigoryeva N.A., Avdeev M.V., Aksenov V.L.

Abstract

The impact of the addition of a polymer (polyethylene glycol) with a molecular weight of 20 kDa on the structure of micellar systems of an anionic surfactant (sodium oleate) in aqueous solutions is investigated via small-angle neutron scattering. The structure and interaction parameters of micelles (micelle aggregation number, degree of ionization, axial ratio, average diameter, charge, inverse screening length, and surface potential) are compared in a solution with and without the addition of the polymer. Using the concentration dependences of the experimental data on surface tension, parameters such as the critical micelle concentration, area per molecule, surface activity, surface excess, and critical aggregation concentration are determined in the case of complex solutions. The observed effect of the addition of the polymer on the behavior of a micellar solution of sodium oleate can be related to a change in the surface activity of the surfactant in the presence of the polymer. As a result of comparison with previous experimental data, it is concluded that the weight of the polymer significantly affects the structural properties of sodium oleate–polyethylene glycol mixed solutions.

Journal of Surface Investigation: X-ray, Synchrotron and Neutron Techniques. 2018;12(6):1142-1148
pages 1142-1148 views

Features of the Crystal Structure and Vibrational Spectra of Ba1.65Sr3.35Nb10O30–Ba4Na2Nb10O30 Barium-Strontium Niobates with the Structure of Tetragonal Tungsten Bronze

Kichanov S.E., Mehdiyeva R.Z., Dang N.T., Jabarov S.H., Kozlenko D.P., Dubrovinsky L.S., Mammadov A.I., Lukin E.V., Kurnosov A.V., Savenko B.N.

Abstract

The crystal structure and vibrational spectra of Ba1.65Sr3.35Nb10O30–Ba4Na2Nb10O30 barium-strontium niobates are investigated by neutron diffraction and Raman spectroscopy in the concentration range x = 0–1 with steps of 0.1 and 0.05. All compounds under study have a structure of the tetragonal tungsten-bronze type with the space group of P4mm symmetry. The concentration dependences of the crystal-cell parameters, interatomic bonds, and vibrational modes for a number of solid solutions of the (1–х)Ba1.65Sr3.35Nb10O30хBa4Na2Nb10O30 system are obtained. Anomalies in the behavior of the crystal parameters and vibrational modes are observed for the concentration dependences at x ~ 0.5. This may be due to a change in the nature of the sodium occupation of vacancies in various crystallographic positions of the tetragonal structure.

Journal of Surface Investigation: X-ray, Synchrotron and Neutron Techniques. 2018;12(6):1149-1154
pages 1149-1154 views

Magnetic Properties of Polycrystalline and Amorphous Cobalt- and Nickel-Ferrite Films

Kanevsky V.M., Butashin A.V., Muslimov A.E.

Abstract

The magnetic properties of polycrystalline and amorphous cobalt- and nickel-ferrite films obtained by solid-phase synthesis are studied. Polycrystalline nickel-ferrite films are shown to be characterized by significant coercive fields at room temperature in the direction normal to the substrate plane. Compressive stresses that arise in the films during solid-phase oxidation and synthesis are assumed to contribute to the enhancement of the coercive fields. In polycrystalline films, a magnetic anisotropy of the “easy plane” type, characteristic of two-dimensional layers, is found. X-ray amorphous films have only paramagnetic properties.

Journal of Surface Investigation: X-ray, Synchrotron and Neutron Techniques. 2018;12(6):1155-1158
pages 1155-1158 views

Obtainment of Stabilized Zirconium Dioxide via the High-Frequency Magnetron Sputtering of a Metallic Target

Valyukhov S.G., Stognei O.V., Filatov M.S.

Abstract

The influence of the yttrium concentration on the structure of coatings prepared via the high-frequency magnetron sputtering of a metal target is investigated. The results of coating deposition in pure argon and a mixed (Ar + O2), reactive medium are discussed. It is demonstrated that a nonequilibrium body-centered-cubic solid solution based on zirconium with an extended homogeneous region (up to 16 at % Y) is formed under the condition that a target is sputtered in pure argon. During reactive-coating deposition, the formation of cubic or tetragonal zirconium dioxide is generated depending on the yttrium concentration. The tetragonal structure is created if the yttrium concentration is 8 at %. It is found that the obtained tetragonal zirconium dioxide is thermally stable both in terms of structure and in morphology upon heat treatment in air at 1100°C for 11 h.

Journal of Surface Investigation: X-ray, Synchrotron and Neutron Techniques. 2018;12(6):1159-1164
pages 1159-1164 views

Structure and Phase Composition of Multilayer AlN/SiN Films Irradiated with Helium Ions

Uglov V.V., Shymanski V.I., Korenevski E.L., Remnev G.E., Kvasov N.T.

Abstract

The results of investigating the microstructure and phase composition of AlN/SiNx multilayer films with alternating nanocrystalline aluminum nitride (nc-AlN) and amorphous silicon nitride (a-SiNx) phases, which were formed via magnetron sputtering, are presented. The layer thickness varies from 2 to 10 nm, the total film thickness is 300 nm, and the grain size of the AlN phase corresponds to the nc-AlN layer thickness. By means of transmission electron microscopy, it is revealed that, due to 30-keV He+ ion irradiation with a dose of 5 × 1016 cm–2, gas pores with an average size of 2.0–2.4 nm and localized mainly in a-SiNx layers are generated within the projective range of helium ions. The appearance of such inclusions is due to the fact that implanted helium atoms migrate into the formed vacancy complexes. In this case, the structural state of AlN crystal layers remains unchanged.

Journal of Surface Investigation: X-ray, Synchrotron and Neutron Techniques. 2018;12(6):1165-1169
pages 1165-1169 views

On the Mechanism of Thermal Expansion of Orthorhombically Modified Copper Pyrovanadate

Rotermel M.V., Krasnenko T.I., Samigullina R.F.

Abstract

A set of X-ray diffraction data on the crystal-lattice transformations of the α-Cu2V2O7 phase demonstrates that, in regions with an anomalous negative and near-zero volumetric thermal expansion, both vanadium‒oxygen and copper‒oxygen sublattices are maximally deformed. The near-zero and negative volumetric thermal expansion of the α-Cu2V2O7 unit cell arises from the degeneration of zigzag copper‒oxygen columns at invariable distances between Cu–O sublattice layers.

Journal of Surface Investigation: X-ray, Synchrotron and Neutron Techniques. 2018;12(6):1170-1175
pages 1170-1175 views

Anomalous-Diffraction Method Applied to Studying the Structure of the Composite Oxide (Eu2Hf2O7)

Kolyshkin N.A., Veligzhanin A.A., Zubavichus Y.V., Popov V.V.

Abstract

The anomalous-diffraction method applied near the absorption edge of Hf is used to investigate the features of atomic ordering in the Eu2Hf2O7 structure. Structural parameterization describing a continuous transition between ideally disordered (fluorite) and ideally ordered (chalcolamprite) structures is proposed. A comparison between the calculated and experimental results demonstrates qualitative coincidence and confirms the hypothesis that the sample under study exists in the intermediate phase. The method is sensitive to cation ordering, but anion ordering of the suggested model is not described.

Journal of Surface Investigation: X-ray, Synchrotron and Neutron Techniques. 2018;12(6):1176-1181
pages 1176-1181 views

Determination of the Thickness of Nanofilms Using X-Ray Photoelectron Spectroscopy

Kaplya P.S., Efremenko D.S., Afanas’ev V.P.

Abstract

Determination of coating thicknesses whose dimensions lie in the nanometer range is an important analytical application of X-ray photoelectron spectroscopy (XPS). The coating thickness is determined as a result of comparing peak intensities measured using lines corresponding to the coating with those of characteristic substrate lines. It is shown that the error in determining thicknesses using a procedure that completely disregards processes of elastic electron scattering reaches 50%. At present, the influence of elastic scattering processes is taken into account by replacing the inelastic mean free path with the fitting parameter called the effective attenuation length. Physical phenomena occurring in the case of the inclusion of an elastic photoelectron scattering channel are analyzed in this paper. Two approaches to the description of XPS spectra are considered: the first one is implemented using invariant embedding methods, and the second one used the method of discrete ordinates with the matrix exponent. On the basis of the first method, the influence of multiple elastic-scattering events on the XPS energy spectra is studied. The second one shows a high effectiveness when calculating no loss peaks of photoelectrons emitted by multilayer samples.

Journal of Surface Investigation: X-ray, Synchrotron and Neutron Techniques. 2018;12(6):1182-1189
pages 1182-1189 views

Scanning Probe Microscopy Used to Estimate the Structural Asymmetry of Filters with Micro- and Nanopores

Bakulin V.N., Boshenyatov B.V., Valiev H.H., Karnet Y.N., Popov V.V., Snegireva N.S., Yumashev O.B.

Abstract

The features of the surface structure of nanoporous and microporous polymer-membrane films promising for use in cleanrooms during the manufacturing of microelectronics products are examined. The degrees of asymmetry of selective and supporting surfaces are determined via scanning probe microscopy. The hydrodynamic characteristics of the membranes under study are analyzed.

Journal of Surface Investigation: X-ray, Synchrotron and Neutron Techniques. 2018;12(6):1190-1193
pages 1190-1193 views

Depth Profiling Using Reflected Electron Spectroscopy

Afanas’ev V.P., Bodisko Y.N., Gryazev A.S., Kaplya P.S., Fedorovich S.D.

Abstract

Nondestructive depth profiling method based on reflected electron spectroscopy is presented. Large loss spectra of wide energy range is analyzed. Spectra analysis is performed using two approaches: boundary problem solution using invariant imbedding method and approximate interpretation based on Straight Line Approximation with correction coefficients, which depend on ration of evaporated layer thickness and transport mean free path. It is shown that the transport mean free path, not the inelastic mean free path, limits the information depth of the method in opposite of X-ray photoelectron spectroscopy, elastic peak electron spectroscopy. This fact significantly increase depths that can be analyzed using presented method. Thickness of the evaporated Nb layer on the Si substrate is determined.

Journal of Surface Investigation: X-ray, Synchrotron and Neutron Techniques. 2018;12(6):1194-1199
pages 1194-1199 views

Identification of Field-Emission Images as “Spotty Pictures”

Egorov N.V., Karpov A.G., Klemeshev V.A.

Abstract

In this work we propose and implement an algorithm for identifying field-emission images with the aim of determining the crystallographic orientation of an emitter and obtaining detailed information about the structural features of its surface. A threshold-type analysis of the brightness distribution in the image is found to be preferable for selecting information-containing areas and their contours. An original algorithm is proposed for selecting the mask of a “spot” of arbitrary shape. The proposed algorithm of processing the information area is also applicable to “skeletons”; however, the contour of an information fragment should not contain more than one gap. In contrast to the skeletons, the use of internal areas of emission “spots” by means of determining geometric moments improves the reliability of processing results due to an increase in sampled information.

Journal of Surface Investigation: X-ray, Synchrotron and Neutron Techniques. 2018;12(6):1200-1205
pages 1200-1205 views

A Comparative Analysis of the Size Dependence of the Melting and Crystallization Temperatures in Silver Nanoparticles via the Molecular Dynamics and Monte-Carlo Methods

Samsonov V.M., Sdobnyakov N.Y., Myasnichenko V.S., Talyzin I.V., Kulagin V.V., Vasilyev S.A., Bembel A.G., Kartoshkin A.Y., Sokolov D.N.

Abstract

The size dependences of the melting and crystallization temperatures of silver nanoparticles are obtained by two alternative atomistic simulation methods, such as the molecular dynamics and Monte-Carlo methods. The simulation results are analyzed and compared with available experimental values and a melting temperature calculated using the well-known Thomson formula. Atomistic simulation reveals good coincidence between the data and satisfactorily conforms to the Thomson formula. However, the melting temperatures predicted through atomistic simulations exceeds the available experimental data.

Journal of Surface Investigation: X-ray, Synchrotron and Neutron Techniques. 2018;12(6):1206-1209
pages 1206-1209 views

Study on the Electronic Structure of the Graphene–Iron–Nickel Interface

Dunaevskii S.M., Lobanova E.Y., Mikhailenko E.K., Pronin I.I.

Abstract

In the present study the evolution of the electronic structure of the graphene/Fe/Ni(111) interface with increasing number of intercalated iron atoms is investigated. The Eσ(k) dependences and full and partial densities of states are calculated within density functional theory. It is shown that an increase in the number of iron layers does not affect the electronic structure, but greatly affects the magnetic properties of the interface.

Journal of Surface Investigation: X-ray, Synchrotron and Neutron Techniques. 2018;12(6):1210-1214
pages 1210-1214 views

On the Phase Associations and Crystal-Chemical Inheritance of Be–Mg–Al Silicates during Subsolidus Crystallization

Mamontova S.G., Bogdanova L.A., Belozerova O.Y., Zelentcov S.Z.

Abstract

During the solid-phase synthesis of Be–Mg–Al silicates, i.e., beryllian indialite (BI), the crystal-chemical proximity is due to the transfer of elements of chemical and structural inheritance. BI crystallization from a gel is carried out via the structural adaptation of multicomponent metastable phases transforming into BI, which is implemented in two stages: diffusion and the formation of microcrystallites fed by a melt film. During the sintering of dry oxides, parageneses are transferred from a previous temperature stage to the subsequent one so that several phases of the former stage are retained and the fraction of stable phases increases because of the consumption of intermediate phases. Phase transformations whereby BI is crystalized in the subsolidus region are interpreted from the viewpoint of the evolutionary regularities of mineralogenesis.

Journal of Surface Investigation: X-ray, Synchrotron and Neutron Techniques. 2018;12(6):1215-1219
pages 1215-1219 views

Titanium-Carbide Formation in a Liquid Hydrocarbon Medium by Femtosecond Laser Irradiation

Kochuev D.A., Khorkov K.S., Abramov D.V., Arakelian S.M., Prokoshev V.G.

Abstract

A brief description of the properties of titanium carbide, its applications, and established methods for its industrial fabrication are provided. A novel procedure for creating titanium-carbide coatings by subjecting a titanium sample to ultrashort laser pulses in a liquid hydrocarbon medium is described. Details of the experimental procedure are provided and the used laser setup is described. The prepared samples are characterized by scanning electron microscopy and Raman spectroscopy. The specifics of titanium-carbide formation at the boundary of the area subjected to the irradiation of a femtosecond laser are investigated based on Raman-spectroscopy data, and a comparison with a sample of commercial titanium carbide is made.

Journal of Surface Investigation: X-ray, Synchrotron and Neutron Techniques. 2018;12(6):1220-1223
pages 1220-1223 views

Test Object for SEM Calibration: 2. Correlation Analysis of SEM Signals

Novikov Y.A.

Abstract

A method for correlation analysis of the coordinates of control points in scanning electron microscope signals obtained by recording slow secondary electrons is described. The method allows one to independently and quantitatively estimate the fabrication quality of the relief components of test objects with a trapezoidal profile and large inclination angles of the lateral walls, which are intended for the calibration of a scanning electron microscope, and to choose only the components or separate areas of components with a high quality of their fabrication for the purpose of calibration. Correlation analysis of the quality of fabrication of the MShPS-2.0Si test object is performed. Analysis shows that the used microscopes (with real and usually unknown drawbacks) allow one to investigate the advantages and disadvantages both of real test objects with a trapezoidal profile and large inclination angles of the lateral walls, and of real scanning electron microscopes.

Journal of Surface Investigation: X-ray, Synchrotron and Neutron Techniques. 2018;12(6):1224-1232
pages 1224-1232 views

Electromotive Force in a Layer of Finely Dispersed Spontaneously Polarized Semiconductor

Kharlamov V.F.

Abstract

The phenomenon of energy conversion by a thin layer of finely dispersed spontaneously polarized semiconductor sandwiched between two plane-parallel metallic electrodes (being in direct contact with them), upon exposure to hydrogen gas, is studied. When the device is incorporated in a closed electrical circuit, the powder layer acts as a source of direct current. We develop a theoretical model that presupposes that the heat absorbed by the powder layer from the surrounding environment is converted into electrical energy. The model is shown to be consistent with the experiment.

Journal of Surface Investigation: X-ray, Synchrotron and Neutron Techniques. 2018;12(6):1233-1236
pages 1233-1236 views

Fundamental Principles Employed for Ionization and Acceleration Layer Control in the Discharge of a Stationary Plasma Thruster

Kim V.P., Gnizdor R.Y., Grdlichko D.P., Merkuriev D.V., Mitrofanova O.A., Smirnov P.G., Shilov E.A., Zakharchenko V.S.

Abstract

The fundamental principles allowing control of the ionization and acceleration layer position and thickness in the discharge of a stationary plasma thruster (SPT) determining ion flows to the discharge chamber walls and the corresponding energy losses and wall erosion rate are considered in this work. These principles have allowed the development of modern SPTs with a long life life that have already been successfully used for many years in space technology. Some of these principles were formulated earlier on the basis of available data and were not fully verified from the physical point of view. To date some new investigations have been carried out. Using them, some new principles are formulated and the earlier ones are corrected in this paper. These principles can be used in the processes of new thruster development.

Journal of Surface Investigation: X-ray, Synchrotron and Neutron Techniques. 2018;12(6):1237-1247
pages 1237-1247 views

Application of Fractal-Geometry Approaches to Simulating Migration Processes in Soil

Sharapova T.V., Makin R.S.

Abstract

The migration processes occurring in soil are considered to be diffusion processes. At present, there is no sufficient information on the parameters of radionuclide migration processes in soils. This makes it difficult to solve issues of preventing the consequences of radioactive contamination. In existing models based on Gaussian (normal) distributions, a large number of important factors capable of affecting radionuclide migration in the soil is not taken into account. In turn, radionuclide migration processes occurring in the soil behave unusually. Hence, classical estimates can lead to significant differences from experimental data. Due to the application of nonstandard approaches to this issue, soil can be regarded to be an aggregate of fractal clusters with a characteristic property of self-similarity. The observed spatial and temporal correlations can lead to the appearance of memory effects and self-organization. The fractal and chaotic dynamics of radionuclide migration in soil must be understood as a unified holistic process of the formation of a fractal model. As a result, it is possible to eliminate the discrepancy between experimental data and theoretical models constructed according to classical laws.

Journal of Surface Investigation: X-ray, Synchrotron and Neutron Techniques. 2018;12(6):1248-1252
pages 1248-1252 views

Current State of Development of a Microscope Operating at a Wavelength of 3.37 nm at the Institute of Physics of Microstructures of the Russian Academy of Sciences

Malyshev I.V., Pestov A.E., Polkovnikov V.N., Salashchenko N.N., Toropov M.N., Chkhalo N.I.

Abstract

The study is devoted to the development of a microscope operating at a wavelength of 3.37 nm in the water window. A Schwarzschild lens with a multilayer coating is used as an image-forming objective lens. The microscope has a theoretical resolution of up to 13 nm and a field of view of 7.3–97.5 µm depending on the magnification. A low depth of focus (±37.5 nm) allows one to implement the z-tomography of samples. A schematic diagram of the microscope, the result of aspherizing the mirror collector, and the results of measuring the roughness of the mirror substrates are given. A three-point method for mounting the mirrors and also a magnetic damper operating on Foucault currents are described. The exposure time is estimated.

Journal of Surface Investigation: X-ray, Synchrotron and Neutron Techniques. 2018;12(6):1253-1263
pages 1253-1263 views

Action of the Pulses of Shock Waves on the Structure and Superconducting Parameters of MgB2 Tapes

Mikhailov B.P., Nikulin V.Y., Mikhailova A.B., Silin P.V., Borovitskaya I.V., Shavkin S.V., Serov A.A.

Abstract

The possibility of increasing the critical current of MgB2 tapes containing carbon and oxygen additives under the action of shock waves produced by pulsed plasma in a Plasma Focus setup is demonstrated. The microstructure of the tapes and the chemical composition of superconducting layers in the initial state and after impact at different distances between the samples and the anode of Plasma Focus installation (from 20 to 45 mm) and the number of shocks (from three to five) are investigated. The regularities of the change in the critical current as a function of the magnitude of transverse and longitudinal magnetic fields in the range of 2–9 T are studied at 4.2 K. It is established that as a result of the impact and thermal action of the plasma, the superconducting interlayers become denser, the grains are fragmented, the composition is homogenized, and the chemical composition is changed. This promotes an increase in the critical current by 50–80 A in transverse magnetic fields of 2–3 T.

Journal of Surface Investigation: X-ray, Synchrotron and Neutron Techniques. 2018;12(6):1264-1269
pages 1264-1269 views

Molecular Dynamics Simulation of Physical Sputtering of Nanoporous Silicon-Based Materials with Low Energy Argon

Sycheva A.A., Voronina E.N., Rakhimova T.V.

Abstract

The process of the physical sputtering of the (001) surface of continuous and nanoporous crystalline silicon by 100- and 200-eV Ar ions is simulated using the molecular dynamics method. The features of the process in porous materials are revealed. The dependences of the sputtering yield on the fluence and energies of incident ions are obtained. The structural changes under ion bombardment are described. The dissimilarity between the sputtering mechanisms for materials differing in pore radii and the degree of porosity is demonstrated.

Journal of Surface Investigation: X-ray, Synchrotron and Neutron Techniques. 2018;12(6):1270-1277
pages 1270-1277 views

Cold Metal Transfer (CMT) Based Wire and Arc Additive Manufacture (WAAM) System

Xizhang Chen ., Su C., Wang Y., Siddiquee A.N., Sergey K., Jayalakshmi S., Singh R.A.

Abstract

The forming system of wire and arc additive manufacture (WAAM) based on cold metal transfer (CMT) is a high build rate system for production of near-net shape components layer by layer, which is composed of industrial robot operation system and 3D path simulation software. In the 3D path simulation software, the working layout of the off-line virtual robot is carried for the imported three-dimensional model to screen the model wall thickness, correct process library, set process parameters, slice, layer, plan deposition path, form simulation and upload program to execution system. Among the whole system, the 3D path simulation software provides essential database for process control and an innovative planning path to coordinate industrial robot platform to build parts layer by layer. Furthermore, the experiment is also performed to study the stability of aluminum alloy forming using the WAAM-CMT system by establishing different experimental models and changing process parameters and process modes of industrial robot and Fronius digital welding machine embedded on robot operation platform.

Journal of Surface Investigation: X-ray, Synchrotron and Neutron Techniques. 2018;12(6):1278-1284
pages 1278-1284 views

Near-Field Defects Imaging in Thin DLC Coatings Using High-Frequency Scanning Acoustic Microscopy

Zinin P.V., Kutuza I.B., Titov S.A.

Abstract

A high-frequency scanning acoustic microscope (SAM) operating at 1–1.3 GHz was used to investigate subsurface defects in diamond-like carbon (DLC) films that were 2–3 μm thick. Because the wavelength of the longitudinal wave in the film was comparable to the film thickness, the acoustical images obtained were near-field images. To interpret the features in the acoustical images, a multidisciplinary approach was utilized through a combination of SAM with atomic force microscopy (AFM), a focused ion beam (FIB) technique, and optical microscopy. Simulations based on the rigorous theoretical approach better predict the depth of the defect than the ray optical approach. It is shown that scattering of the shear waves by subsurface defects is responsible for the acoustical contrast of the cavity.

Journal of Surface Investigation: X-ray, Synchrotron and Neutron Techniques. 2018;12(6):1285-1293
pages 1285-1293 views

Radiosensitivity Detection of Gamma Radiation by Using (In2O3)0.1(TeO2)0.9 Thin Films for Clinical Radio-Image

Chenjun Zhang ., Niu H., Wang L., Yang J.

Abstract

To study the detecting radiosensitvie of (In2O3)0.1(TeO2)0.9 thin films irradiated by gamma rays. Materials and Methods: The effects of gamma irradiation of various levels on the current-voltage characteristics for the (In2O3)0.1(TeO2)0.9 thin films, prepared by thermal evaporation in vacuum. The current increases linearly with the gamma radiation dose up to certain dose and decreases thereafter. The sensitivity of these thin films, at different applied voltages in the range 0–4.8 V, has been found to be in the range 35–190 mA/cm 2/Gy. Correspondingly, the minimum measurable dose has been found to be in the range 0.05–0.26 mGy. The values of the sensitivity are reasonably high in comparison to the commercially available gamma radiation dosimeters, revealing high scope for further developments.

Journal of Surface Investigation: X-ray, Synchrotron and Neutron Techniques. 2018;12(6):1294-1297
pages 1294-1297 views

Modulation Instability of a Gravity Wave and Generation of a Direct Cascade of Vortex Energy on the Surface of Water

Mezhov-Deglin L.P., Filatov S.V., Brazhnikov M.Y., Levchenko A.A.

Abstract

The development of instability of gravity-capillary waves on the surface of water excited by two perpendicular plungers has been experimentally observed. As a result of a four-wave process, waves with a frequency of 8 Hz scatter in pairs into waves with frequencies of 3.92 and 4.08 Hz, as well as 11.98 and 12.02 Hz. The amplitude of low-frequency waves increases exponentially with a characteristic time of about 90 s which exceeds the time of viscous wave damping almost by an order of magnitude. Along with the main pumping mode, the appeared low-frequency harmonics, propagating on the surface of water at an angle of 15° to each other, form large-scale vortex flows on the surface of water. The wave energy is transferred from the pumping region directly to vortices with a size comparable to the length of a bath wall. In a vortex system, a direct energy cascade with the energy distribution close to E(k) ~ k5/3 is formed from the region of low wave vectors.

Journal of Surface Investigation: X-ray, Synchrotron and Neutron Techniques. 2018;12(6):1298-1303
pages 1298-1303 views

Study of the Effect of Optical Illumination on Resistive Switching in ZrO2(Y) Films with Au Nanoparticles by Tunneling Atomic Force Microscopy

Novikov A.S., Filatov D.O., Antonov D.A., Antonov I.N., Shenina M.E., Gorshkov O.N.

Abstract

The effect of optical illumination on the resistive switching in ultrathin (~4 nm) ZrO2(Y) films with embedded single-layer Au nanoparticle arrays 2–3 nm in size is studied via tunneling atomic force microscopy. The ZrO2(Y) films with Au nanoparticles are grown by layerwise magnetron deposition onto glass substrates with a conductive indium-tin-oxide sublayer, followed by annealing at 450°C. An increase in hysteresis due to bipolar resistive switching in the ZrO2(Y) films is observed on the cyclic current–voltage curves of the microscope probe-to-sample contact. The effect is found to manifest itself in a dense Au nanoparticle array (~660 nm) when the contact area is photoexcited through a transparent substrate exposed to the radiation of a semiconductor laser at the plasmon-resonance wavelength. The effect is attributed to the photon-assisted field emission of electrons from Au nanoparticles to the conduction band of ZrO2(Y) in a strong electric field between the microscope probe and the indium-tin-oxide substrate under plasmon-resonance conditions.

Journal of Surface Investigation: X-ray, Synchrotron and Neutron Techniques. 2018;12(6):1304-1309
pages 1304-1309 views

Atomic Force Microscopy for Studies of Molecular Layering Products

Sosnov E.A., Kochetkova A.S.

Abstract

The products obtained via molecular layering on materials with a different chemical nature and structure are studied with atomic force microscopy. The atomic force microscopy of synthesis products is analyzed to control the structure and properties of coatings formed during molecular layering on matrices of various geometric shapes.

Journal of Surface Investigation: X-ray, Synchrotron and Neutron Techniques. 2018;12(6):1310-1322
pages 1310-1322 views

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