


Vol 59, No 2 (2023)
Articles
Microcrystalline Bi0.5Sb1.5Te3-Based Materials Prepared by Various Methods
Abstract
We have studied properties of p-type Bi0.5Sb1.5Te3 solid solution samples produced by hot pressing, extrusion, and spark plasma sintering of powders prepared by melt spinning and grinding the ingot in a jet mill to a particle size on the order of hundreds of microns or less than hundreds of nanometers (by mechanical activation). The powders and fracture surfaces of the samples have been examined on an optical and a scanning electron microscope. The powders prepared by melt spinning at disk rotation rates of 3000 and 5500 rpm had the form of platelets tens of microns in thickness, consisting of distinct regions ranging in thickness from a few to hundreds of nanometers. Microstructural analysis showed that all of the samples contained a small amount of tellurium, which was confirmed by X-ray microanalysis data. We have measured the thermoelectric parameters (Seebeck coefficient, electrical conductivity, and thermal conductivity) of the materials at room temperature and in the range 100–700 K and calculated their lattice thermal conductivity and thermoelectric figure of merit, ZT. The highest thermoelectric figure of merit, ZT = 1.0 ± 0.1 at 380 K, has been reached in the samples produced by spark plasma sintering and hot pressing of powders prepared by melt spinning and mechanical activation, respectively.



Structural Characteristics and Deformation Behavior of Porous Titanium Prepared by Sintering
Abstract
We have studied characteristic structural features of PTM-1 and PTS-1 titanium powders and related porous materials prepared by sintering the powders and determined quantitative characteristics of the pore system in the sintered materials. Macro- and microstructural features of the porous alloys have been shown to correlate with their deformation and strength parameters. The materials have been characterized by scanning electron microscopy, X-ray diffraction, and stereometric techniques, and their strength characteristics have been studied in compression tests. The porous material prepared by sintering the PTM-1 titanium powder has been found to have better principal strength and deformation characteristics owing to its lower porosity in comparison with the material obtained by sintering PTS-1 and to dispersion hardening by TiC particles in the structure formation process.



Phase Formation during Aluminothermic Reduction of Titanium from Its Oxides with the Anatase and Rutile Structures
Abstract
Low-temperature phase formation processes (below 1270–1450°C) underlying aluminothermic reduction of titanium from different TiO2 polymorphs—stable rutile and metastable anatase—have been studied during continuous heating and isothermal heat treatment. Interaction between the components has been investigated at TiO2/Al molar ratios of 0.23 and 0.43 using thermal analysis and X-ray diffraction. The results demonstrate that, in the case of continuous heating of anatase + aluminum powders with TiO2/Al = 0.43, the reduction process begins at a temperature of 943°C and does not reach completion up to 1270°C, resulting in the formation of the intermetallic phase Al3Ti, Al2O3, and intermediate titanium oxides (Ti0.78O0.937 and (Ti0.99Al0.01)2O3). Increasing the fraction of aluminum in the mixture (TiO2/Al = 0.23) increases the degree of reduction of titanium, which shows up as an increase in the amount of intermetallic phases (Al3Ti, Al2Ti, Al1.1Ti0.9, and AlTi3) in the reduction products and a decrease in the amount of intermediate titanium oxides. Rutile has been shown to have low reactivity: heating of rutile + aluminum mixtures to 1450°C leads to the formation of many intermediate titanium oxides along with a small amount of Al3Ti and AlTi3. The results have been confirmed by isothermal heat treatment (1400°C, 60 min) of mixtures of anatase and rutile with aluminum. The anatase-to-rutile polymorphic transformation during heating in flowing argon has been shown to occur in the range 622–913°C. During the reduction process, molten aluminum inhibits the phase transition of anatase, but its reactivity remains higher than that of rutile



Synthesis of Titanium Oxide/Manganese Oxide Composites and Their Physicochemical and Photocatalytic Properties
Abstract
We have synthesized photocatalytically active manganese-modified titanium dioxide-based materials and studied key features of the formation of the synthesized materials and their physicochemical and photocatalytic properties. Modification of TiO2 with manganese has been shown to ensure preparation of nanopowders (4.8–2550 nm) with a specific free surface area from 0.56 to 479 m2/g. The synthesized powders have high photocatalytic activity (PCA) under illumination with visible light, which exceeds the PCA of unmodified TiO2 of the same origin and that of Degussa P-25 commercially available titanium dioxide. An increased PCA level is offered by the manganese-modified materials containing both anatase and rutile, without separation of individual manganese phases.



Structure and Phase Formation in Arc PVD Zr–B–Si–C–Ti–(N) Coatings
Abstract
Zr–B–Si–C–Ti and Zr–B–Si–C–Ti–N coatings have been produced for the first time by an arc physical vapor deposition process in a residual argon + nitrogen atmosphere. The Zr–B–Si–C–Ti coating had an amorphous–nanocrystalline structure. Nanocrystallites were formed in the Ti–B–C system, and the amorphous component of the material was formed by Zr–B–C and Si–C phases. The coating of the latter system had a predominantly amorphous structure (amorphous content of ~85–93%) based on titanium nitride with Ti–B and Ti–C bonds, zirconium carboboronitride (Zrx(C,N,B)y), zirconium boride, and silicon carbonitride.



Preparation and Characterization of Lithium Niobate Single Crystals Doped with 4.02–5.38 mol % Zn
Abstract
Using homogeneous doping, a Nb2O5:4.5 mol % Zn precursor, and lithium carbonate, we have synthesized a single-phase LiNbO3:4.1 mol % Zn growth charge, which was then used to grow lithium niobate crystals by the Czochralski technique. High-speed optical quality evaluation results for the crystals and their calculated piezoelectric modulus d333 demonstrate that they have high optical quality. Photoinduced light scattering and laser conoscopy characterization results for homogeneously and directly doped crystals containing 4.02–5.38 mol % Zn confirm their high optical homogeneity and laser damage resistance. The crystals have absolutely no photorefractive response. Our results can be used in the growth of large LiNbO3:Zn crystals with a small coercive field, which are of interest for making laser light converters based on periodically poled structures.



Properties of Terbium Oxide Nanoparticles Synthesized via Laser Ablation in a Reducing Medium
Abstract
This paper reports on the synthesis of terbium sesquioxide (Tb2O3) nanoparticles via laser ablation of a solid target in a flowing 95% Ar + 5% H2 binary welding mixture with the use of an ytterbium-doped fiber laser with an average output power of 300 W. We have studied morphological and structural features of the synthesized powder, its thermal behavior, magnetic properties, and densification dynamics during heating to 1450°C in vacuum. The synthesized particles were nearly spherical in shape, with an average size of 13 nm, and had a monoclinic crystal structure, which irreversibly transformed into a cubic structure of
symmetry as a result of firing in argon or vacuum at temperatures near 750 and 1050°C, respectively. Using temperature-dependent specific magnetization measurements, we determined their paramagnetic Curie temperature (θp = –11.8 K), Curie constant (C = 11.74 K emu/(mol Oe)), and effective magnetic moment (μeff = 9.69μB/Tb). These data suggest that antiferromagnetic exchange interaction between the terbium ions prevails and that the content of Tb4+ ions in the nanopowder is negligible. We have demonstrated the feasibility of producing transparent Tb2O3 ceramics by consolidating presintered nanoparticles via hot isostatic pressing for 2 h at a temperature of 1450°C and pressure of 200 MPa.



Preparation and Properties of Glasses in the Tellurium Dioxide–Sodium Hexametaphosphate System
Abstract
New glasses in the TeO2–Na6P6O18 system have been prepared, their thermal behavior has been studied by differential scanning calorimetry in the range 25–580°C, and their heat capacity has been determined as a function of temperature in the range 25–400°C. We have evaluated characteristics of the devitrification process and glassy state, obtained analytical representations of the glass transition temperature and the thermodynamic characteristics of the glasses as functions of their composition at 80°C, and carried out a comparative analysis of the results together with those for previously studied TeO2-based binary systems. Optical transmission of the glasses has been measured in the UV, visible, and IR spectral regions. We have demonstrated the possibility of doping the glasses with rare-earth oxides and studied luminescence properties of the glass with the composition 0.89TeO2–0.08Na6P6O18–0.03Nd2O3.



Adhesion Strength of the Interface between Solid Phases in the GaxGe40–xS60–Quartz Glass System
Abstract
Using normal pull-off testing, we have studied adhesion contact strength in the GaxGe40–xS60–quartz glass system as a function of contact formation temperature, pull-off test temperature, and chalcogenide glass composition. The addition of 1 at % gallium to glass composition considerably reduces the adhesion strength. Further increasing the percentage of gallium, to 8 at %, causes only a slight drop in adhesion. The observed general relationships can be accounted for by partial glass crystallization on heating for adhesion contact formation and subsequent cooling to the pull-off test temperature. We have formulated recommendations concerning detachment of GaxGe40–xS60 glasses from the quartz reactor wall.



Electrothermal Atomic Absorption Determination of Platinum and Palladium in Glass Cloth Catalysts
Abstract
A technique has been proposed for electrothermal atomic absorption determination of Pt and Pd in glass cloth catalysts after dissolution of a sample in hydrofluoric acid, followed by treatment of the resultant solution with aqua regia. The analytical accuracy has been checked by the standard addition method. The detection limits for Pt and Pd in fiberglass catalysts are 5 × 10–5 and 3 × 10–5 wt %, respectively. The technique has been used to evaluate the content of active components in glass cloth catalysts at a level of 1.5–n × 10–3 wt %.



Preparation of Zirconium Carbide-Based Refractory Ceramics by Direct Zirconium Carburization
Abstract
Compact stoichiometric zirconium carbide (ZrC) with a tailored shape has been synthesized by direct carburization of rolled zirconium metal in an atmosphere of an argon + ethylene gas mixture. Ceramics have been produced by reacting zirconium metal with ethylene gas, through absorption of the carbon released on the reaction surface as a result of C2H6 pyrolysis. We have characterized the microstructure of the ceramics and assessed the mechanical and conductive properties of the synthesized ZrC.



Preparation, Structure, and Dielectric and Nonlinear Optical Properties of (K0.5Na0.5)NbO3–BaZrO3 Ceramics
Abstract
Single-phase (1 – x)(K0.5Na0.5)NbO3⋅xBaZrO3 (x = 0–0.06) ceramics with new compositions, including those modified with SiO2 and ZnO oxide additions, have been prepared and their crystal structure, microstructure, and dielectric and nonlinear optical properties have been studied. A phase with the perovskite structure and an orthorhombic unit cell has been shown to form in all of the synthesized materials. Partial replacement of cations of the basic composition by cations of the combined additive has been demonstrated to cause an increase in unit-cell volume. The ferroelectric phase transitions in the ceramics have been confirmed by dielectric spectroscopy and laser radiation second harmonic generation measurements. Doping with SiO2 and ZnO oxide additions has been shown to lower the temperatures of the transitions from the orthorhombic ferroelectric phase to a tetragonal ferroelectric one and then to a cubic paraelectric phase.



Stereolithographic Fabrication of Alumina Ceramics from Aluminum Chloride-Containing Polymerizable Precursors
Abstract
An approach has been proposed for preparing polymerizable precursors to alpha-alumina and aluminum oxynitride ceramics and using them in stereolithographic fabrication of aluminum-containing ceramics. With allowance for their homogeneity (optical transmission), photopolymerizability, and weight loss during thermolysis, three precursors based on aluminum chlorides (anhydrous and hexahydrate) and a basic aluminum chloride were chosen for characterization. We analyzed the behavior of the precursors during firing in an ammonia atmosphere for the preparation of oxynitride ceramics and during firing in air for the preparation of alpha-alumina ceramics from homogeneous precursors. Stereolithographic 3D printing of alpha-alumina ceramics was tested, in particular with the use of the proposed precursors in the form of photopolymerizable binders allowing the fraction of alumina in photosuspensions to be increased.



Granulated Materials Based on Calcium Silicate Hydrate, Poorly Crystallized Carbonated Hydroxyapatite, and Gelatin
Abstract
Spherical granules have been produced via suspension processing from synthetic ceramic powders consisting of calcium silicate hydrate and poorly crystallized carbonated hydroxyapatite in a wide range of ratios, using gelatin as a polymer binder. It has been shown that the experimental conditions of this study lead to the formation of polydisperse granules ranging in diameter from 500 μm to 5 mm and having open porosity on the order of 40–60%. The granulated materials contain 19–29 wt % gelatin and 60–75 wt % inorganic salts.



Frequency-Dependent Behavior of the Conductivity of a Polymer Composite of Ultrahigh Molecular Weight Polyethylene and Nano-NiO
Abstract
Electrical transport properties of a composite material based on ultrahigh molecular weight polyethylene having NiO nanoparticles deposited on its granules have been investigated using impedance spectroscopy. This has made it possible to study electrical engineering properties of an ensemble of nanoparticles uniformly distributed over a polymer matrix. We have evaluated the dielectric permittivity, capacitance, and dielectric loss tangent of the composite and found frequency dependences of the real and imaginary parts of its complex conductivity. The hopping conduction mechanism has been shown to prevail in the composite at frequencies of up to 1 MHz, giving way to a relaxation mechanism at higher frequencies. We discuss a correlation between structural features of the composite and charge transport processes.


