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Vol 55, No 7 (2019)

Article

Effect of Hydrobromic Acid Concentration on the Chemical Etching Behavior of PbTe and Pb1 –xSnxTe Single Crystals in Aqueous H2O2–HBr–Ethylene Glycol Solutions

Malanych G.P., Tomashyk V.N.

Abstract

We have studied the effect of HBr concentration in (H2O2–HBr–EG)/EG etching mixtures on chemical–mechanical polishing (CMP) and dynamic chemical polishing (DCP) of single-crystal PbTe and Pb1 –xSnxTe solid solutions. The CMP and DCP rates have been measured as functions of solution composition, and the effect of initial HBr concentration on the composition range of polishing etchants, surface quality, and surface condition after polishing has been assessed by measuring surface roughness. We have optimized the composition of polishing mixtures and processing conditions for obtaining high-quality polished surfaces.

Inorganic Materials. 2019;55(7):641-647
pages 641-647 views

Defect Structure and Photogenerated Carrier Loss Processes in Cu1 –x(In0.7Ga0.3)Se2 (0 ≤ x ≤ 0.30) Chalcopyrite Solid Solutions

Gapanovich M.V., Odin I.N., Rabenok E.V., Orishina P.S., Novikov G.F.

Abstract

Cu1 –x(In0.7Ga0.3)Se2 (0 ≤ x ≤ 0.30) copper-deficient solid solutions with the chalcopyrite structure have been synthesized and their unit-cell parameters have been determined as functions of composition. Their 78-K cathodoluminescence spectra show a band centered at 1.13 eV, which is most likely due to Cu2+VCu defect associates. Microwave photoconductivity data demonstrate that the defect associates act as electron traps, considerably reducing the lifetime of photogenerated current carriers.

Inorganic Materials. 2019;55(7):648-652
pages 648-652 views

Interaction of the RNi1 –xSix (R = Dy, Gd; x = 0.05, 0.02) Compounds with Hydrogen

Lushnikov S.A., Movlaev E.A., Verbetsky V.N.

Abstract

This paper reports the synthesis of RNi1 –xSix-based (R = Dy, Gd; x = 0.05, 0.02) intermetallic hydrides. The amount of absorbed hydrogen in the hydride phases is three to four atoms per formula unit. According to X-ray diffraction data, the synthesized hydrides have a crystal lattice with the FeB structure (sp. gr. Pnma, no. 62) at R = Dy and the CrB structure (sp. gr. Cmcm, no. 63) at R = Gd.

Inorganic Materials. 2019;55(7):653-655
pages 653-655 views

Preparation and Properties of Graphite Nitrate-Modified Composite Electrochemical Coatings Based on a Nickel–Chromium Alloy

Tseluikin V.N.

Abstract

We have prepared graphite nitrate-modified composite electrochemical coatings based on a nickel–chromium alloy. The electrodeposition process used to grow the coatings has been studied in potentiodynamic mode. We have assessed the influence of disperse-phase concentration and cathode current density on the microhardness of the nickel–chromium–graphite nitrate coatings.

Inorganic Materials. 2019;55(7):656-658
pages 656-658 views

Heat Treatment- and Lamp Processing-Induced Structural Transformations of an Amorphous Fe77B7Nb2.1Si13Cu0.9 Alloy and Nonmonotonic Behavior of Its Mechanical Properties

Ievlev V.M., Kannykin S.V., Il’inova T.N., Vavilova V.V., Kushchev S.B., Serikov D.V., Baikin A.S.

Abstract

Using a variety of characterization techniques (differential scanning calorimetry, X-ray diffraction, high-resolution transmission electron microscopy, resistivity measurements, nanoindentation, and uniaxial tension testing), we have studied structural changes produced in the amorphous phase of the Fe77B7Nb2.1Si13Cu0.9 alloy by heating in vacuum to 750°C and lamp processing (LP) with the use of pulsed xenon lamps to a fluence F = 120 J/cm2 on the sample surface. Increasing the temperature or fluence leads to three stages of structural transformations: structural relaxation of the amorphous phase below 450°C and two stages of crystallization, which show up as nonmonotonic behavior of the hardness and local plasticity of the samples. With a common character of the structural changes, the effect of LP shows up as an increase in crystallization rate (the processing time is 200 times shorter). In both cases, the fraction of plastic strain in indentation work in amorphous and crystallized samples is 25% larger than that in amorphous–crystalline composites. It has been shown that irreversible deformation of amorphous samples by uniaxial tension leads to structural relaxation and an increase in the size of the relaxation zone.

Inorganic Materials. 2019;55(7):659-668
pages 659-668 views

Erbium–Ytterbium Upconversion in Polyvinyl Chloride Films

Rasmagin S.I., Kryshtob V.I., Novikov I.K.

Abstract

We have prepared a series of polyvinyl chloride–yttrium oxysulfide composites doped with ytterbium and erbium ions and measured their upconversion photoluminescence spectra and volume resistivity. The results demonstrate that the green photoluminescence intensity in the composites is considerably higher than that in yttrium oxysulfide doped with erbium and ytterbium. The resistivity of the composites drops by eight orders of magnitude on heating. Besides, with increasing erbium–ytterbium ion pair concentration, the upconversion photoluminescence intensity in the red and green spectral regions rises, and additional photoluminescence peaks emerge, two in the green and one in the red, owing to the Stark splitting of the erbium terms under the effect of the chlorine present in the polyvinyl chloride. On heating, the PVC–Y2O2S:Yb3+/Er3+ composite passes into a semiconducting state.

Inorganic Materials. 2019;55(7):669-672
pages 669-672 views

Synthesis, Structure, and Magnetic Characteristics of Mesoporous Fe2O3–SiO2 Composites

Kondrashova N.B., Lebedev A.I., Lysenko S.N., Valtsifer V.A., Strelnikov V.N.

Abstract

In this paper, we examine processes for producing mesoporous Fe2O3–SiO2 silica-matrix composites with different fractions of ferric oxide and demonstrate the effect of the synthesis procedure on the structure, textural characteristics, particle size, and magnetic properties of the materials. We assess the thermal stability of the composites. A ferric-oxide-rich material (Fe : Si = 0.6 : 1) prepared by hydrothermal synthesis (THS) exhibits ferrimagnetic properties after high-temperature holding (t = 1000°C) for 3 h.

Inorganic Materials. 2019;55(7):673-680
pages 673-680 views

Thermally Controlled Formation of WO3 Nano- and Microcrystals on the Surface of Coatings Produced on Titanium by Plasma Electrolytic Oxidation

Rudnev V.S., Vasilyeva M.S., Lukiyanchuk I.V.

Abstract

We demonstrate that air annealing of oxide layers produced on titanium by plasma electrolytic oxidation and containing WO3, MnWO4, and ZnWO4 leads to the surface growth of nano- and microcrystals consisting predominantly of WO3. The crystals are initially formed around the perimeter of the coating pores. The size, composition, and number of crystals depend on the annealing temperature. We discuss possible causes and mechanisms of crystal growth.

Inorganic Materials. 2019;55(7):681-686
pages 681-686 views

Effect of Bismuth Content on the Stability of (R,Bi)3(Fe,M)5O12 (R = Ln, Y; M = Ga, Al) Garnet Solid Solutions

Smirnova M.N., Nipan G.D.

Abstract

Published experimental data are used to assess the feasibility of adding bismuth to (R,Bi)3(Fe,M)5O12 (R = Ln, Y; M = Ga, Al) multicomponent solid solutions with the garnet structure using various synthesis techniques. We demonstrate that the existing approaches for producing (R,Bi)3(Fe,M)5O12 films and coatings are incapable of ensuring reproducibility of their chemical composition and phase stability.

Inorganic Materials. 2019;55(7):687-691
pages 687-691 views

Ordered Defect Lattice in Lithium Niobate Crystals

Aleshina L.A., Sidorova O.V., Kadetova A.V., Sidorov N.V., Teplyakova N.A., Palatnikov M.N.

Abstract

Nominally undoped and doped LiNbO3 crystals have been studied using full-profile analysis of X‑ray diffraction data and Raman spectroscopy. The X-ray diffraction patterns and Raman spectra of the crystals contain weak superstructure lines forbidden for space group R3c. The observed superstructure lines are not reflections from a second phase. The intensity distribution and position of the additional reflections are essentially independent of nonstoichiometry and dopant concentration. The additional lines in the Raman spectra and X-ray diffraction patterns of the crystals can result from the formation of an ordered hexagonal defect superstructure sublattice with a doubled a cell parameter relative to the fundamental unit cell.

Inorganic Materials. 2019;55(7):692-697
pages 692-697 views

Defect Structure of Zinc-Doped LiNbO3 Crystals in a Wide Range of Dopant Concentrations

Sidorov N.V., Bobreva L.A., Palatnikov M.N., Makarova O.V.

Abstract

IR absorption spectra of zinc-doped LiNbO3 crystals in the stretching region of OH groups, Raman spectra of the crystals, and their optical absorption spectra provide evidence of drastic changes in the mechanism responsible for the incorporation of Zn into the structure of the crystals and the nature of hydrogen bonds and the corresponding proton-containing charged defect complexes (\(V_{{{\text{Li}}}}^{ - }\)–OH, NbLi–OH, and \({\text{Zn}}_{{{\text{Nb}}}}^{{{\text{3}} - }}\)–OH) near a concentration threshold at ≈6.76 mol % ZnO in the melt.

Inorganic Materials. 2019;55(7):698-703
pages 698-703 views

Specific Absorption Coefficient of Cr3+ Ions in (TeO2)0.70(ZnO)0.30 Glass

Zamyatin O.A., Churbanov M.F., Zamyatina E.V.

Abstract

(TeO2)0.70(ZnO)0.30 tellurite glasses doped with Cr3+ ions in the concentration range 80 to 2500 ppm have been prepared via melt solidification using orthotelluric acid and zinc nitrate, and their optical transmission has been measured in the wavelength range 0.3 to 2.7 μm. Transmission spectra of the glasses have been shown to contain two strong absorption bands, peaking at 460 and 650 nm. Using a series of glasses differing in chromium content, we have evaluated the spectral dependence of the specific absorption coefficient for the glasses, which has been shown to be 142 ± 2 cm–1/wt % at the maximum of the 650-nm absorption band.

Inorganic Materials. 2019;55(7):704-709
pages 704-709 views

EPR Spectra and Distribution of Manganese Ions in Modified Fluorozirconate Glasses

Brekhovskikh M.N., Solodovnikov S.P., Moiseeva L.V., Zhidkova I.A., Denisov G.L., Fedorov V.A.

Abstract

We have studied EPR spectra of MnO2-activated fluorozirconate and fluorohafnate glasses in order to determine the oxidation state and distribution of the manganese ions. The effect of activator concentration on the ratio of the percentage of free Mn4+ ions to that of ions in clusters in the glasses has been investigated for the first time. The results demonstrate that, at high activator concentrations, the manganese ions in the glasses are clustered, and only a small fraction of them are present as isolated ions. Reducing the manganese concentration leads to an increase in the percentage of free Mn4+ ions. Devitrification is accompanied by dissociation of the clusters and a transition of the ions to an isolated state.

Inorganic Materials. 2019;55(7):710-714
pages 710-714 views

Structure and Thermal Stability of Lithium-Substituted Hydroxyapatite Ceramics

Obolkina T.O., Konovalov A.A., Leonov A.V., Smirnov V.V., Barinov S.M., Smirnov S.V., Krylov A.I., Antonova O.S., Goldberg M.A.

Abstract

We have studied the effect of doping with lithium cations on the phase composition, lattice parameters, and crystallite size of hydroxyapatite at different heat treatment temperatures (900, 1200, and 1400°C). The results demonstrate that, at high degrees of substitution (20 mol %) and heat treatment temperatures of 1200 and 1400°C, lithium cations contribute to conversion of apatite into lithium-substituted tricalcium phosphate. At degrees of substitution of 1, 5, and 10 mol %, the addition of lithium causes no destabilization of the apatite structure even at a temperature of 1400°C.

Inorganic Materials. 2019;55(7):715-723
pages 715-723 views

Phase Transformations in the Surface Layer of Compact Zirconium Nitride-Based Ceramics

Kovalev I.A., Shokodko A.V., Ogarkov A.I., Shevtsov S.V., Konovalov A.A., Kannykin S.V., Ashmarin A.A., Kolomiets T.Y., Chernyavskii A.S., Solntsev K.A.

Abstract

We have studied structural, morphological, and phase transformations in the surface layer of compact zirconium nitride-based ceramics during high-temperature annealing in vacuum, nitrogen, and air. The formation of oxygen-containing phases during heat treatment of ZrN is controlled by bulk and grain-boundary oxygen diffusion. At the beginning of the process, oxygen is supplied by an amorphous surface layer, which always forms during the ceramic preparation process. In air, the process is driven by oxygen indiffusion from the gas phase across an initially forming porous oxide layer. Grain-boundary oxygen diffusion leads to the formation of a crystalline zirconium oxide layer on grain boundaries and crack nucleation.

Inorganic Materials. 2019;55(7):724-729
pages 724-729 views

Thermal Expansion of Scheelite-Like Molybdate Powders and Ceramics

Tokarev M.G., Potanina E.A., Orlova A.I., Khainakov S.A., Boldin M.S., Lantsev E.A., Sakharov N.V., Murashov A.A., Garcia-Granda S., Nokhrin A.V., Chuvil’deev V.N.

Abstract

NaxSr1 – 2xNdxMoO4 (x = 0–0.5, Δx = 0.1) solid solutions with the scheelite structure have been synthesized for the first time and their crystallographic parameters have been determined as functions of composition and temperature. Their thermal expansion coefficients have been determined in the temperature range 25–1000°C: αa = (12.9–14.9) × 10–6 °C–1 and αc = (24.9–25.9) × 10–6 °C–1. Using spark plasma sintering at tmax ≈ 872–985°C and τ ≈ 650–750 s, we have prepared ceramics with relative densities in the range 97–99%.

Inorganic Materials. 2019;55(7):730-736
pages 730-736 views

Phase Composition and Microstructure of Crystallization Products of Molten Bi2O3 ⋅ GeO2 under Various Cooling Conditions

Zhereb V.P., Bermeshev T.V., Kargin Y.F., Mazurova E.V., Denisov V.M.

Abstract

We have studied the influence of melt heat treatment, initial cooling temperature (tcooling 0), and cooling schedule for a melt containing 50 mol % Bi2O3 and 50 mol % GeO2 on the phase composition, macrostructure, and microstructure of crystallizing solid phases. According to X-ray diffraction, optical microscopy, and scanning electron microscopy data, the phase composition of the crystallization products is represented by either the metastable bismuth germanate Bi2GeO5 or a mixture of metastable and stable phases, depending on melt cooling conditions. The crystallization behavior of phase-pure Bi2GeO5 under identical cooling conditions has been shown to be influenced by not only tcooling 0 but also isothermal preholding of the melt for 1 h at a temperature of 1160°C.

Inorganic Materials. 2019;55(7):737-747
pages 737-747 views

Structural, Mechanical, and Transport Properties of Scandia and Yttria Partially Stabilized Zirconia Crystals

Agarkova E.A., Borik M.A., Kulebyakin A.V., Kuritsyna I.E., Lomonova E.E., Milovich F.O., Myzina V.A., Osiko V.V., Tabachkova N.Y.

Abstract

Crystals of (ZrO2)1 –x – y(Sc2O3)x(Y2O3)y (x = 0.003–0.045, y = 0.005–0.03) solid solutions have been grown by directional solidification in a cold crucible. All of the crystals consist of a mixture of two tetragonal phases of zirconia, t and t', differing in the degree of tetragonality (c/\(\sqrt 2 a\)): 1.014–1.015 and 1.004–1.005 for the t- and t'-phases, respectively. All of the crystals have high microhardness (13.5–15.0 GPa) and high fracture toughness (on the order of 6–7 MPa m1/2). Their fracture toughness decreases with an increase in the total content of the stabilizing oxides, which is well consistent with the associated changes in phase composition, namely, with the increase in the percentage of the (transformable) t-phase. All of the crystals are similar in electrical conductivity: on the order of 0.04 S/cm at a temperature of 1173 K.

Inorganic Materials. 2019;55(7):748-753
pages 748-753 views