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Vol 53, No 2 (2017)

Article

Solubility limits of manganese in InSb under equilibrium and nonequilibrium synthesis conditions

Sanygin V.P., Pashkova O.N., Izotov A.D.

Abstract

We demonstrate that, in the case of InSb〈Mn〉 synthesis through quenching from the liquid state, a second phase in InSb precipitates at higher manganese concentrations than in the case of Czochralski growth. The observed concentration delay of second-phase precipitation can be accounted for in terms of both the complex, multistep formation of Lomer–Cottrell sessile dislocations, accompanying the crystallization of III–V compound semiconductors, and diffusion hindrances to dopant motion to dislocations, associated with the high quenching rate and the presence of other lattice defects.

Inorganic Materials. 2017;53(2):135-141
pages 135-141 views

Fine purification of monoisotopic 32S and 34S

Sukhanov M.V., Storozheva T.I., Evdokimov I.I., Pimenov V.G., Sozin A.Y., Kotereva T.V.

Abstract

We have proposed and tested a combined process for ultrapurification of monoisotopic 32S and 34S sulfur, which comprises thermochemical treatment of sulfur vapor on silica and ceria packing, melting with aluminum, and distillation. The impurity composition of the purified sulfur has been determined by atomic emission and IR spectroscopy. We have obtained monoisotopic 32S and 34S sulfur samples comparable in chemical purity to high-purity sulfur of natural isotopic composition.

Inorganic Materials. 2017;53(2):142-147
pages 142-147 views

Chemical vapor deposition of carbon nanotube layers on aluminum foil

Red’kin A.N., Kipin V.A., Sedlovets D.M., Knyazev M.A.

Abstract

A novel technique has been demonstrated for direct chemical vapor deposition of carbon nanotubes (CNTs) on aluminum foil. It has been shown that the foil surface acquires catalytic properties after being held in an aqueous nickel nitrate solution for a certain time. CNTs were deposited by the catalytic pyrolysis of ethanol vapor. The hybrid materials thus prepared have the form of aluminum foil coated with “carbon wool” from CNTs on both sides. The layers have good adhesion to the aluminum substrate, which allows it to be deformed without causing the CNT layer to peel off. Such material is potentially attractive, in particular, for the fabrication of supercapacitors.

Inorganic Materials. 2017;53(2):148-153
pages 148-153 views

Graphitization and preparation of diamond in an amorphous carbon material at high pressures and temperatures

Varfolomeeva T.D., Lyapin A.G., Brazhkin V.V., Lyapin S.G., Borovikov N.F.

Abstract

Structural transformations of a carbynoid amorphous carbon material after high-temperature, high-pressure processing at different rates of isobaric heating have been studied by scanning electron microscopy and Raman spectroscopy. Using the 6 GPa data as an example, we demonstrate that slow heating leads to gradual graphitization of the material at temperatures above 600°C, in perfect agreement with previous measurements, in which graphitization was observed up to 8 GPa. At the same time, increasing the heating rate to 50°C/s at a sufficiently high pressure (8 GPa) leads to significant changes in the nature of the transformations. Whereas heating to temperatures from 1100 to 1200°C also leads to the formation of graphite-like phases, rapid heating to 1300°C ensures the formation of considerable amount of diamond in the absence of catalysts.

Inorganic Materials. 2017;53(2):154-159
pages 154-159 views

Exothermic synthesis of cast nickel aluminide alloys with tungsten and molybdenum carbides

Gostishchev V.V., Astapov I.A., Khimukhin S.N.

Abstract

Cast NiAl–Mo2C and NiAl–WC alloys have been prepared by self-propagating high-temperature synthesis involving the reduction of starting metal oxides. Synthesis conditions have been found experimentally. The elemental and phase compositions of the alloys have been determined and their microstructure has been studied. The composites have been shown to have higher microhardness than do NiAl intermetallic alloys containing Mo and W inclusions.

Inorganic Materials. 2017;53(2):160-163
pages 160-163 views

Paramagnetism in CoxZn1–xCr2S4 solid solutions

Aminov T.G., Shabunina G.G., Busheva E.V., Novotortsev V.M.

Abstract

The magnetic properties of CoxZn1–xCr2S4 solid solutions have been studied at temperatures from 5 to 300 K in static magnetic fields of 7.96 × 103 and 3.58 × 106 A/m. We have determined the Curie temperatures, Curie–Weiss constants, and effective magnetic moments of the solid solutions. The experimental data are discussed with allowance for the magnetic phase diagram of the system.

Inorganic Materials. 2017;53(2):164-170
pages 164-170 views

Effect of silver additions on the structural properties and phase composition of TiO2/Ag composites

Vakhrushev A.Y., Boitsova T.B., Gorbunova V.V., Stozharov V.M.

Abstract

We have studied the effect of silver nitrate additions on the anatase–rutile transformation of titanium dioxide in TiO2/Ag composites at low temperature (500°C). The structure and phase composition of the composites with different Ag(I) concentrations have been determined by X-ray diffraction and transmission electron microscopy. The results demonstrate that the percentage of rutile increases with increasing Ag(I) ion concentration, reaching 60 wt %. A mechanism of the anatase–rutile transformation in the composites has been proposed.

Inorganic Materials. 2017;53(2):171-175
pages 171-175 views

Role of iron and chromium in the photocatalytic activity of titanium dioxide films on stainless steel

Denisov N.M., Baglov A.V., Borisenko V.E.

Abstract

Photocatalytically active titanium dioxide films have been formed on stainless steel grids via sol–gel process followed by heat treatment in the temperature range of 450–550°C. During UV irradiation of the films in an aqueous solution of the Rhodamine B dye and in distilled water we have detected iron and chromium dissolution from uncoated grid regions and the deposition of iron and chromium compounds onto the titanium dioxide surface. The deposition rate of these compounds increases with annealing temperature, which leads to a decrease in the photocatalytic activity of the films.

Inorganic Materials. 2017;53(2):176-180
pages 176-180 views

Effect of supercritical drying parameters on the electrochemical properties of vanadium oxide-based aerogels

Balakhonov S.V., Vatsadze S.Z., Churagulov B.R.

Abstract

This paper examines the effect of supercritical drying parameters (including the nature of the solvent) on the electrochemical properties of vanadium oxide-based aerogels. It is shown that, among vanadium oxide-based aerogels prepared using different solvents (supercritical CO2, n-hexane, and n-octane), the material obtained in n-hexane is superior in discharge capacity characteristics: its capacity is 350 to 250 mAh/g in the first seven cycles. The aerogel obtained in supercritical CO2 has a far lower capacity: 80–105 mAh/g.

Inorganic Materials. 2017;53(2):181-184
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Electroconductive properties of zirconia/carbon nanotube aerogel composite

Lyapunova E.A., Morozov I.A., Naimark O.B.

Abstract

Electroconductive properties of zirconia/multiwalled carbon nanotube aerogel composite are investigated. The composite exhibits bulk percolation cluster-like conductivity at wide range of spatial scales. Conductive atomic force microscopy reveals the localized nature of conductive properties of the composite on the micro(nano)scopic scale and the uniformity of current distribution in all conductive areas independently of their size. The presence of unlinked conductive chains and the possibility of their linking by dissociating ions are demonstrated in experiments on registration of I–V curves during the evacuation of the composite impregnated with distilled water. The experimental data make it possible to describe the electrical properties of the composite as the properties of a circuit formed by the parallel connections of numerous voltage dividers arranged in a bulk porous structure. These features make the synthesized composite a promising candidate for use in catalysis and water vapor sensors.

Inorganic Materials. 2017;53(2):185-189
pages 185-189 views

High- and low-temperature X-ray diffraction studies of aluminate spinels in the CoAl2O4–NiAl2O4 system

Knyazev A.V., Demidov D.N., Knyazeva S.S.

Abstract

CoxNi1–xAl2O4 (x = 0, 0.25, 0.5, 0.75, 1) aluminate spinels have been prepared by solid-state reactions and their crystal structures have been refined by the Rietveld method. We have analyzed whether the results are consistent with theoretical relationships stemming from the hard sphere model. Using high- and low-temperature X-ray diffraction measurements, we have obtained the temperature dependences of the unit-cell parameters for the synthesized compounds and determined their thermal expansion coefficients. The rate of cation exchange reactions has been shown to be very slow at temperatures below 200°C.

Inorganic Materials. 2017;53(2):190-199
pages 190-199 views

Synthesis and upconversion luminescence spectra of (Y1–xyYbxEry)2O2S solid solutions

Andreev P.O., Sal’nikova E.I., Andreev O.V., Denisenko Y.G., Kovenskii I.M.

Abstract

Sequentially exposing coprecipitated yttrium, ytterbium, and erbium sulfates to flowing H2 at 500–600°C for 6 h and then to flowing H2S at 1000°C for ≤7 h, we obtained single-phase samples of the following solid solutions: (1) (Y0.97Er0.02Yb0.01)2O2S (а = 3.779 Å, с = 6.579 Å), (2) (Y0.94Er0.05Yb0.01)2O2S (а = 3.783 Å, с = 6.572 Å), (3) (Y0.91Er0.07Yb0.02)2O2S (а = 3.775 Å, с = 6.568 Å), (4) (Y0.87Er0.10Yb0.03)2O2S (а = 3.772 Å, с = 6.559 Å), (5) (Y0.82Er0.15Yb0.03)2O2S (а = 3.770 Å, с = 6.545 Å), and (6) (Y0.96Yb0.03-Er0.01)2O2S (a = 3.780 Å, c = 6.580 Å). The observed chemical transformations were accompanied by a transition from powder particles 2–25 μm in size to agglomerates 30–50 μm in size. The upconversion luminescence intensity in the samples was found to have a maximum: 400 (1), 3750 (2), 2100 (3), 1100 (4), and 150 arb. units (5). The presence of (Y0.96Yb0.03Er0.01)2O3 and (Y0.96Yb0.03Er0.01)2S3 as impurity phases in the samples was shown to considerably reduce the luminescence intensity.

Inorganic Materials. 2017;53(2):200-206
pages 200-206 views

Composites based on triethylammonium dodecahydro-closo-Dodecaborate ((Et3NH)2[B12H12]) and sodium silicate water glass

Skachkova V.K., Goeva L.V., Grachev A.V., Kochneva I.K., Malinina E.A., Shaulov A.Y., Berlin A.A., Kuznetsov N.T.

Abstract

The [B12H12]2– anion, a three-dimensional aromatic system with a uniform electron density distribution over its boron skeleton, has been shown to react with sodium silicate water glass (WG) to form a supramolecular structure. The WG/[B12H12]2– system has both short-range and weaker, long-range contacts, which influences the chemistry of the thermolysis process and, as a consequence, the thermal and thermomechanical properties of the composites. At 60% (Et3NH)2[B12H12] in the starting mixture, the reaction products contain ~6.6% [B12H11NEt3]2–, a substituted derivative that has a plasticizing effect in the case of thermomechanical processing. At an optimal ratio of the starting reagents, the thermo-oxidative stability of the [B12H12]2– anion and the deformation resistance of the WG/[B12H12]2– system persist up to 600°C.

Inorganic Materials. 2017;53(2):207-211
pages 207-211 views

Octacalcium phosphate as a precursor for the fabrication of composite bioceramics

Kukueva E.V., Putlyaev V.I., Tikhonov A.A., Safronova T.V.

Abstract

We have studied the formation of octacalcium phosphate (OCP) in various buffer solutions. Brushite hydrolysis in acetate and succinate buffer solutions at 60°C and pH 5.75 ensures rapid synthesis of pure OCP and substituted OCP (sOCP), which allows a rather large amount of this phosphate (at least 10 g in a single synthesis run) to be obtained in 50–60 min. The observed differences in phase composition between the OCP and sOCP thermolysis products make it possible to obtain biphasic ceramic composites of various kinds: β-TCP/β-CPP (Ca/P = 1.33) in the case of OCP and β-TCP/HA (Ca/P = 1.54) in the case of sOCP. Ceramics with a density of 80% of theoretical density and higher produced using the OCP precursors synthesized in this study have a uniform microstructure, possess the desired microporosity, and are potentially attractive for further advances in the field of bioresorbable osteoplastic materials.

Inorganic Materials. 2017;53(2):212-219
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Hot-pressed ceramic SiC–YAG materials

Perevislov S.N., Lysenkov A.S., Titov D.D., Tomkovich M.V.

Abstract

Dense SiC-based ceramic materials containing yttrium aluminum garnet (YAG) as an oxide sintering aid have been prepared by hot pressing in the temperature range 1750–1850°C. As a result of melting, the oxides fill spaces between the SiC particles, contributing to the densification of the material and mass transport during the hot pressing process. The present results demonstrate that relatively small amounts of the oxides (≤5 wt %) are needed to ensure a high degree of densification of the SiC–YAG materials. The best physicomechanical properties are offered by the SiC + 3 wt % YAG material sintered at a temperature of 1850°C: ρ = 3.24 ± 0.01 g/cm3, П = 1.1 ± 0.1%, σb = 640 ± 10 MPa; KIc = 6.4 ± 0.2 MPa m1/2, Еel = 410 ± 20 GPa, and HV = 26.0 ± 0.2 GPa. This material experiences predominantly intercrystalline fracture.

Inorganic Materials. 2017;53(2):220-225
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Crystal structure of lead zirconate titanate ceramics prepared using ultrasonic processing

Savchuk G.K., Letko A.K.

Abstract

We have studied how the duration of ultrasonic processing of presynthesized lead zirconate titanate powders influences the crystal structure and physical properties of ceramics produced from such powders. The effect of the ultrasonication time on the sintering temperature, the formation of crystalline phases in the ceramics, and their Curie temperature has been assessed.

Inorganic Materials. 2017;53(2):226-232
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Impurity composition of the samples in the exhibition–collection of extrapure substances: I. samples of elemental substances received in 2007–2015

Lazukina O.P., Malyshev K.K., Volkova E.N., Churbanov M.F.

Abstract

Data are presented on the purity of the samples of elemental substances, including isotopically enriched samples, received by the Exhibition–Collection of Extrapure Substances in 2007–2015. During this time period, the permanent exhibition received 26 samples of elemental substances from 11 institutes and research and production centers of Russia. The first samples of high-purity isotopically enriched silicon, germanium, sulfur, and selenium were provided. The total impurity concentration in the best samples is 3 × 10–5 to n × 10–4 at %. More than half of the new samples compare well to the current world level.

Inorganic Materials. 2017;53(2):233-241
pages 233-241 views