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Vol 54, No 12 (2018)

Article

Formation of Cobalt Impurity Microinclusions in Silicon Single Crystals

Turgunov N.A.

Abstract

The structure and chemical composition of cobalt impurity microinclusions in silicon have been studied by electron probe microanalysis using n- and p-type Si〈Co〉 samples prepared by diffusion doping and cooled at different rates after diffusion annealing. The cooling rate after diffusion annealing has been shown to have a significant effect on the structural parameters of the samples and the size of the forming impurity microinclusions. The size and shape of the impurity microinclusions determine their distribution over the bulk of the samples.

Inorganic Materials. 2018;54(12):1183-1186
pages 1183-1186 views

Effect of Particle Size on the Magnetostructural Transformation of a Manganese Monoarsenide-Based Phase in the ZnGeAs2–MnAs System

Marenkin S.F., Aronov A.N., Fedorchenko I.V., Zheludkevich A.L., Khoroshilov A.V., Kozlov V.V.

Abstract

We have studied the caloric and magnetic properties of alloys in the MnAs–ZnGeAs2 eutectic system. The results demonstrate that the heat effect and temperature range of the ferromagnetic-to-paramagnetic phase transformation depend on the crystallite size of manganese arsenide. Reducing the crystallite size to ≤60 nm causes the heat effect of the transformation to disappear, significantly changes the temperature range of the magnetic transition, and raises the Curie temperature of the alloy to 351 K.

Inorganic Materials. 2018;54(12):1187-1192
pages 1187-1192 views

Mechanical and Thermoelectric Properties of Bismuth Chalcogenide Solid Solutions Prepared through Melt Solidification in a Liquid

Ivanova L.D., Granatkina Y.V., Mal’chev A.G., Nikhezina I.Y., Emel’yanov M.V., Nikulin D.S.

Abstract

We have studied the mechanical and thermoelectric properties of samples of n-type Bi2Te3–Bi2Se3 solid solutions containing 8 and 20 mol % Bi2Se3; doped with excess tellurium, cadmium chloride, and antimony iodide; and prepared by hot-pressing and extruding granules produced through melt solidification in a liquid. The materials have been tested in compression at 300, 423, 523, and 623 K and in bending at 300 K. Their electrical conductivity, Seebeck coefficient, and thermal conductivity have been measured in the temperature range 100–700 K. We have obtained materials with a compressive strength of ~260 MPa and maximum thermoelectric figure of merit ZT ~ 0.9 in the range 320–390 K.

Inorganic Materials. 2018;54(12):1193-1198
pages 1193-1198 views

Phase Relations along the Cu2S(Sb2S3, PbSb2S4, Pb5Sb4S11)–PbCuSbS3 Joins in the Pseudoternary System Cu2S–PbS–Sb2S3 and Physical Properties of (Sb2S3)1 –x(PbCuSbS3)x Solid Solutions

Aliyev O.M., Ajdarova D.S., Agayeva R.M., Maksudova T.F., Mamedov S.H.

Abstract

Phase relations along the Cu2S(Sb2S3, PbSb2S4, Pb5Sb4S11)–PbCuSbS3 joins in the pseudoternary system Cu2S–PbS–Sb2S3 have been studied using a variety of physicochemical characterization techniques (differential thermal analysis, X-ray diffraction, microstructural analysis, microhardness tests, and immersion density measurements). All of the joins have been shown to be pseudobinary, with eutectic phase relations. We have investigated the electrical transport properties of (Sb2S3)1 – x(PbCuSbS3)x solid solutions, which have been shown to be p-type semiconductors.

Inorganic Materials. 2018;54(12):1199-1204
pages 1199-1204 views

Preparation of Graphene on Copper Substrates of Various Geometries by Chemical Vapor Deposition

Zaitsev E.V., Bocharov G.S., Chuprov P.N., Tkachev S.V., Kornilov D.Y., Gubin S.P., Eletskii A.V., Kurkina E.S.

Abstract

In this paper, we examine the key features of the preparation of graphene by chemical vapor deposition on copper substrates differing in geometry (foil and wire). Along with graphene, we analyze impurity structures forming on the surface of copper substrates as a result of graphene synthesis and discuss their origin and possible ways of eliminating them.

Inorganic Materials. 2018;54(12):1205-1215
pages 1205-1215 views

Preparation of Cast Mo2B5 by Self-Propagating High-Temperature Synthesis Metallurgy Methods

Gorshkov V.A., Sachkova N.V., Khomenko N.Y.

Abstract

This paper reports the preparation of cast dimolybdenum pentaboride by a self-propagating high-temperature synthesis (SHS) metallurgy method. Experiments were carried out in SHS reactors at an initial excess gas (Ar) pressure p0 = 5 MPa. In the experiments, we used thermite-type starting mixtures consisting of molybdenum oxide, aluminum, boron oxide, and elemental boron powders. The combustion of such mixtures yields two types of final product: Mo2B5 and Al2O3. The combustion temperatures of the starting mixtures used in our experiments have been shown to exceed the melting points of the final products, which are thus formed in a liquid (cast) state. Under the effect of gravity, the heavier phase Mo2B5 settles down to form a lower ingot, whereas the lighter phase Al2O3 forms an upper ingot. The synthesis products have been characterized by X-ray diffraction and local microstructural analysis. The results demonstrate that the composition and amount of the starting mixture have a significant effect on the synthesis parameters and the composition and microstructure of the Mo2B5. We have optimized conditions for the preparation of single-phase cast dimolybdenum pentaboride.

Inorganic Materials. 2018;54(12):1216-1222
pages 1216-1222 views

Synthesis and Physicochemical and Electrorheological Properties of Modified Nanodisperse Titanium Dioxide

Murashkevich A.N., Chechura K.M., Novitskaya M.S., Alisienok O.A., Korobko E.V., Novikova Z.A.

Abstract

Nanodisperse modified titanium dioxide ranging in specific surface from 70 to 130 m2/g has been prepared by a sol–gel process using Al(NO3)3 and H3PO4 as modifying components and dodecylamine and ammonium carbonate as structuring components. Microwave drying of an intermediate product and pulverization in a planetary mill have been shown for the first time to be effective in reducing the bulk density of the material and improving its electrorheological activity. The effect of filler concentration (10–40 wt %) on the shear load and leakage current density of electrorheological dispersions has been examined.

Inorganic Materials. 2018;54(12):1223-1230
pages 1223-1230 views

Composition and Thermal Stability of Al- and Zr-Containing Gels Prepared by a Sol–Gel Synthesis Using N,N-Dimethyloctylamine and Acetylacetone

Trusova E.A., Koshcheev A.P., Konovalov A.A., Chipkin P.I., Safronenko M.G., Fortalnova E.A., Khrustalev V.N.

Abstract

Al- and Zr-containing sols intended for producing Al2O3 and ZrO2 nanocoatings, respectively, were prepared by a sol–gel process using N,N-dimethyloctylamine (DMOA) and acetylacetone (acacH). Aluminum and zirconyl nitrates were used as metal precursors. The DMOA/Al and DMOA/Zr molar ratios were 1 and 2, respectively, and the acacH/DMOA molar ratio was 1.5 in both cases. The sols were synthesized at a temperature of 80–90°C and then were evaporated at 90–95°C to a gel state. The resultant gels were characterized by differential thermal analysis, differential scanning calorimetry, and electron impact mass spectrometry. Measurements in the temperature range 20–500°C in air and Ar showed that the Zr-containing material was more thermally stable (decomposition temperature of 304–308°C) than its Al-containing analog (decomposition temperature of 225–230°C). According to the mass spectrometry analysis data, the gels contained metals as acetylacetonate complexes having strong M–O bonds and coordinated molecular DMOA. The nature of the metal was shown to influence both the thermal stability of the gel in which it is present in a chemically bound state and the mechanisms of the processes involved in its thermolysis.

Inorganic Materials. 2018;54(12):1231-1237
pages 1231-1237 views

Thermolysis of Nanoparticulate Boehmite Prepared via Aluminum Isopropylate Hydrolysis

Posel’skaya Y.V., Belaya E.A., Zherebtsov D.A., Viktorov V.V., Tikhonov S.S., Ryabkov Y.I., Kovalev I.N., Vinnik D.A.

Abstract

Boehmite gel was prepared via hydrolysis of aluminum isopropylate in a water–alcohol solution. Electron-microscopic examination showed that the boehmite particles were highly uniform in diameter, at ~70 nm. X-ray fluorescence analysis demonstrated high purity of the material. The boehmite was heat-treated in air at 50, 165, 250, 400, 600, 800, 1000, and 1200°C and characterized by X-ray diffraction after each step. The crystallite size of the thermolysis products was found to increase from 1.1 to 3.6 nm in the range 50 to 1000°C. The gel sample dried at 50°C was characterized by simultaneous thermal analysis in combination with mass spectrometry of released gases. According to the thermal analysis results, the total weight loss in the sample was 45%. The mass spectrometry data allowed us to determine the overall formula of the synthesized gel. In the range 100–200°C, the gel lost the residual adsorbed isopropanol and isopropoxide groups, whereas water release continued up to 1000°C. We conclude that the degree of structural order, water content, and purity of the material influence the thermal stability of the metastable phases of aluminum oxide.

Inorganic Materials. 2018;54(12):1238-1244
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Heat Capacity of In2Ge2O7 and YInGe2O7 from 320 to 1000 K

Denisova L.T., Kargin Y.F., Irtyugo L.A., Belousova N.V., Beletskii V.V., Denisov V.M.

Abstract

Polycrystalline In2Ge2O7 and YInGe2O7 samples have been prepared by solid-state reactions, by sequentially firing stoichiometric mixtures of In2O3, Y2O3, and GeO2 at temperatures from 1273 to 1473 K. The molar heat capacity of the indium and yttrium indium pyrogermanates has been determined by differential scanning calorimetry in the range 320–1000 K. The experimental Cp(T) data have been used to evaluate the enthalpy increment, entropy change, and reduced Gibbs energy of In2Ge2O7 and YInGe2O7.

Inorganic Materials. 2018;54(12):1245-1249
pages 1245-1249 views

Raman Scattering in Nanocomposites Based on Synthetic Opal and Nanocrystalline Bi2TeO5

Moiseyenko V.N., Brynza N.P., Abu Sal B., Holze R., Gorelik V.S., Sverbil’ P.P.

Abstract

This paper presents a systematic Raman scattering study of novel nanostructured materials based on synthetic opal and Bi2TeO5 nanocrystals, which offer high photorefractive sensitivity. Bismuth tellurite was introduced into opal pores in a molten state. The crystal structure of the material in the opal pores was determined by Raman spectroscopy. Comparison of the measured Raman spectra of the opal–Bi2TeO5 nanocomposite and those of polycrystalline powders and single crystals made it possible to reveal a number of new bands and analyze their origin. The observed variation in the intensity of Raman bands from point to point on the sample surface can be interpreted as due to structural light focusing and excitation field localization at surface and volume defects of the photonic crystal structure of the material.

Inorganic Materials. 2018;54(12):1250-1255
pages 1250-1255 views

Purity of Natural Monoisotopic Substances

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

Abstract

In this paper, we discuss general aspects of the impurity composition of natural monoisotopic substances, which are exemplified by samples in the Permanent Exhibition–Collection of Extrapure Substances. The entire set of natural monoisotopes is divided into subsets belonging to sets of alkali and alkaline-earth metals, transition metals, rare-earth metals (REMs), and p-block elements. We estimate the average and total concentrations of elemental impurities in subsets of the purest samples of the natural monoisotopes. The purest monoisotopes are those of the p-block elements. Next are samples of the alkali and alkaline-earth metals, transition metals, and REMs. We estimate the contributions of individual impurity classes to the total impurity concentration, which enables more accurate characterization of the impurity composition of the natural monoisotopes and statistical characteristics of its description.

Inorganic Materials. 2018;54(12):1256-1266
pages 1256-1266 views

Preparation of NZP-Type Ca0.75 + 0.5xZr1.5Fe0.5(PO4)3 –x(SiO4)x Powders and Ceramic, Thermal Expansion Behavior

Savinykh D.O., Khainakov S.A., Boldin M.S., Orlova A.I., Aleksandrov A.A., Lantsev E.A., Sakharov N.V., Murashov A.A., Garcia-Granda S., Nokhrin A.V., Chuvil’deev V.N.

Abstract

Ca0.75 + 0.5xZr1.5Fe0.5(PO4)3 –x(SiO4)x (x = 0–0.5) solid solutions have been synthesized by a sol–gel process and characterized by X-ray diffraction, IR spectroscopy, and differential scanning calorimetry. As expected, the synthesized phosphatosilicates crystallize in a NaZr2(PO4)3-type structure (trigonal symmetry, sp. gr. R\(\bar {3}\)c). The thermal expansion of the solid solutions has been studied by high-temperature X-ray diffraction in the temperature range from 25 to 800°C. Their thermal expansion parameters have been calculated and analyzed as functions of composition. High-density ceramics based on the Ca0.875Zr1.5Fe0.5(PO4)2.75(SiO4)0.25 phosphatosilicate have been produced by spark plasma sintering and their structure and properties have been studied in detail.

Inorganic Materials. 2018;54(12):1267-1273
pages 1267-1273 views

Granular Inhomogeneity Formation during Quartz Glass Melting

Nasyrov R.S., Lunin B.S., Lopatin V.M.

Abstract

This paper examines the formation of fine-grain inhomogeneity in quartz glass. We demonstrate that this defect emerges during the melting of fine-particle crystalline raw materials and the formation of a three-dimensional intergranular network, which contains a high impurity concentration and has a disordered structure. The present results are inconsistent with the existing believe that incomplete melting of quartz grains is the main cause of the development of fine-grain inhomogeneity. In contrast, prolonged high-temperature heat treatment increases the intergranular impurity concentration and intensifies the effect.

Inorganic Materials. 2018;54(12):1274-1276
pages 1274-1276 views

Lead Zirconate Titanate/Modified Nickel Ferrite Magnetoelectric Composites Prepared from Submicron Precursors

Lisnevskaya I.V.

Abstract

We have studied the effects of the preparation procedure, connectivity pattern, and weight ratio of components on the phase composition and properties of particulate PZT–Ni0.9Co0.1Cu0.1Fe1.9O4 – δ magnetoelectric (ME) composites (where PZT stands for piezoelectric materials based on lead zirconate titanate of various industrial grades). The ME ceramics contain no foreign phases, but the use of fine piezoelectric powders leads to one-way doping of the piezoelectric with components of the ferrite. If macrocrystalline PZT is used, undesirable doping processes occur only on interfaces. The 0–3 connectivity composites with equal weight percentages of phases based on soft piezoelectric materials have improved piezoelectric parameters and high ME coupling efficiency (ΔEH = 110–140 mV/(cm Oe)), which exceeds that of the composites with the other connectivity patterns by at least a factor of 1.5. The use of hard piezoelectrics instead of the soft ones reduces ΔEH coefficients by a factor of 3 or more.

Inorganic Materials. 2018;54(12):1277-1290
pages 1277-1290 views

Preparation of Fine-Grained Y2.5Nd0.5Al5O12 + MgO composite ceramics for Inert Matrix Fuels by Spark Plasma Sintering

Golovkina L.S., Nokhrin A.V., Boldin M.S., Lantsev E.A., Orlova A.I., Chuvil’deev V.N., Murashov A.A., Sakharov N.V.

Abstract

We have studied the feasibility of preparing high-density (98.6–99.5%) Y2.5Nd0.5Al5O12 (YAG)–xMgO (x = 5, 10, 20 vol %) composite ceramics by spark plasma sintering. YAG–MgO powder materials have been prepared via MgO precipitation from an aqueous solution of magnesium nitrate, Mg(NO3)2, on the surface of garnet particles. The sintering rate of the YAG–MgO composites has been shown to be controlled by volume diffusion at low temperatures and by grain-boundary diffusion at elevated temperatures.

Inorganic Materials. 2018;54(12):1291-1298
pages 1291-1298 views

Solid-State Thermal Transformations in a Mixture of Palladium Tetraammine Dichloride with Ammonium Chromate

Fesik E.V., Buslaeva T.M., Mel’nikova T.I., Tarasova L.S.

Abstract

Solid-state transformations of a 3[Pd(NH3)4]Cl2 + (NH4)2CrO4 mixture at temperatures from 40 to 550°C in various media have been studied by thermal analysis and mass spectrometry. The results demonstrate that the solid thermolysis product obtained in an argon atmosphere consists of a single phase: palladium-based Pd1 – xCrx solid solution isostructural with palladium and having a unit-cell parameter a = 3.897(2) Å. Its formation proceeds through the formation of metallic Pd and Cr, as evidenced by the absence of chromium oxide phases in all of the solid intermediate thermolysis products. The solid thermolysis product obtained in air consists of the phases Pd and PdO. A model has been proposed for the transformations of the 3[Pd(NH3)4]Cl2 + (NH4)2CrO4 mixture through the formation of metallic palladium and chromium.

Inorganic Materials. 2018;54(12):1299-1307
pages 1299-1307 views

Evolution of the Structure and Properties of AK10M2N Silumin under Irradiation with a High-Intensity Pulsed Electron Beam

Gromov V.E., Ivanov I.F., Zagulyaev D.V., Petrikova E.A., Konovalov S.V., Teresov A.D., Rygina M.E.

Abstract

The structure of cast AK10M2N silumin has been studied by scanning electron microscopy. The results demonstrate that the silumin is a multiphase material containing silicon and intermetallic inclusions. Irradiation of silumin with a high-intensity electron beam has been shown to be accompanied by melting of the surface layer, dissolution of the silicon and intermetallic inclusions, formation of a cellular crystallization structure, and secondary precipitation of submicron- and nanometer-sized second-phase particles. Dispersion of the structure of the surface layer is accompanied by an improvement of the mechanical properties of the silumin.

Inorganic Materials. 2018;54(12):1308-1314
pages 1308-1314 views