X-ray Phase Analysis Research Articles

USING THE ADVANTAGES OF NANOTECHNOLOGY FOR THE PRODUCTION OF COMPOSITE MATERIALS OF THE TYPE NGO/CERAMIC MATRIX

Using the advantages of nanotechnology, composite ceramic materials of the type of graphene oxide nanocolloid/ceramic matrix were obtained in two stages. First, finely porous corundum (1500ºC) and barium titanate (1300ºC)ceramic samples containing 2 mass % graphene structures nanoplatelets were synthesized. The next stage of the study involved the preparation of graphene oxide in nanocolloid form (2 mg/ml, dispersion in H2O) which was impregnated in the solid porous ceramic samples to obtain composite materials. For the characterization of the ceramic samples, mainly infrared spectroscopy, X-ray phase analysis, scanning electron microscopy and light microscopy were used. The results obtained from the studies carried out showed that with the introduction of small amount of graphene nanoplatelets in the initial blends followed by solid state sintering, part of the added graphene is burned out which imparts significant porosity to the ceramics obtained. On the other hand, the addition of graphene initiates the formation of well-shaped fine-grain structure of the ceramic samples, and they had sufficient porosity.

LOW-TEMPERATURE SYNTHESIS OF FINE-POROUS CORUNDUM BASED ON INCORPORATED GRAPHENE NANOSTRUCTURES

In the present paper, the effect of the addition of graphene nanostructures and 3 mass % TiO2 on the microstructure and properties of sintered corundum ceramics were studied. Fine-porous corundum ceramics were obtained by the method of solid-phase sintering at relatively low temperatures of 1450oC, by adding graphene nanostructures in an amount of 2 % or 20 %. To lower the synthesis temperature, 3 mass % TiO2 was added to the initial ceramic blends. As a result of the solid solution formed between Al2O3 and TiO2, a well-sintered corundum ceramic is obtained at synthesis temperature lower than that of pure corundum - 1450oС. For the characterization of the initial blends and the ceramic samples, the methods of X-ray phase analysis, infrared spectroscopy, SEM, TEM EDS and visual microscopy were used. Besides, the basic physicochemical properties of the samples synthesized based on corundum were determined, e.g. water absorption (WA, %), apparent density (AD, %) and apparent (open) porosity (Pa, %).

AUGITE-BASED CERAMICS OBTAINED BY SOLID-STATE SINTERING OF LOESS

Loess from the Danubian Plain (Bulgaria) was used as the raw material for the solid-state synthesis of ceramics.The mineral phase composition of the loess fraction used was determined by powder X-ray phase analysis, and the chemical composition by X-ray fluorescence analysis. The semi-quantitatively determined mineral phases are quartz, plagioclase, K-feldspar, mica, carbonates (calcite and dolomite), chlorite and amphibole. The major oxides of the chemical composition of loess fraction are (in wt. %): SiO2 - 53,61; Al2O3 - 12.57; Fe2O3 - 7.05; P2O5 - 0,23; TiO2 - 1.37; CaO - 19.36; and MgO - 1.48. Experiments were performed with sintering of pure loess without additives, and with addition of MgO and Na2O in order to obtain a composition corresponding to that of the pyroxene augite - (Ca,Na)(Mg,Fe,Al,Ti)(Si,Al)2O6. Ceramics were obtained at three temperatures: 1000, 1100 and 1200°C. The phase composition, spectral characteristics and colour coordinates of the obtained ceramics were determined. The results show that when magnesium and sodium are added to the loess raw material, the ceramics obtained after sintering at 1100 and 1200°C have a predominant content of augite and have a yellow-beige colour.

Structure and Properties of the Electroexplosive Coating of the TiB2-Ag System after Electron Beam Treatment

A coating of the TiB2-Ag system was formed through the use of sequential operations of electroexplosive spraying and electron beam processing. The values of electrical conductivity (62.0 MS/m), Vickers microhardness (0.251-0.265 GPa at the point of measurement on a silver matrix and 25-32 GPa at the point of measurement at inclusions of boride phases), nanohardness (4.48 ± 0.76 GPa) were determined), Young’s modulus (116±29 GPa), wear parameter under dry friction-sliding conditions (1.2 mm3/N • m) and friction coefficient (0.5). Switching wear resistance during accelerated tests was 7000 on and off cycles with an electrical resistance of 10.01 - 11.76 LiOhm. The thickness of the coatings is 100 microns. The coatings are formed by a silver matrix with inclusions of titanium borides located in it with three types of sizes: nanocrystalline, submicrocrystalline and microcrystalline. Quantitatively, in the structural composition among titanium borides, titanium diboride and silver (56 wt. %) are formed predominantly (41 wt. %), while other titanium borides account for 3 wt. %. Structural transformations are described using complementary methods of X-ray phase analysis, scanning and transmission electron microscopy.

Study of the Structure and Properties of Concrete Modified with Nanofibrils and Nanospheres

The application of modifying nanoadditives in the technology of cement composites is currently a relevant and widely researched topic in global materials science. The purpose of this study was to investigate new nanoadditives—nanofibrils made from synthesized wollastonite (NF) and nanospheres from corundum (NS)—produced by LLC NPK Nanosystems (Rostov-on-Don, Russia) as a modifying additive. During the experimental investigations, the mechanical properties of cement pastes and concrete were examined. This included an analysis of the density, compressive and bending strength, as well as water absorption of concrete that had been modified with NF and NS additives. X-ray phase and microstructural analyses of concrete were performed. It was established that modification of cement composites with NF and NS additives had a beneficial effect on their properties, and the optimal amount for both types of additives was 0.3% by binder weight. The highest recorded enhancements in compressive and flexural strength of concrete with 0.3% NF were 7.22% and 7.04%, respectively, accompanied by a decrease in water absorption by 4.70%. When modifying concrete with 0.3% NS, the increases in compressive and flexural strength were 2.71% and 2.48%, and water absorption decreased by 1.96%. Modification of concrete with NF and NS additives did not have a significant effect on the change in concrete density, which was no more than 1%. Based on the results of phase analysis, it was established that concrete with NF and NS additives were characterized by the presence of five main phases: quartz, portlandite, calcite, larnite, and olivine-Ca. It was found that compositions with 0.3% NF and NS differed from the control composition by the presence of such a phase as olivine-Ca. Microstructural analysis confirmed the effectiveness of NF and NS additives. The microstructure of the modified concretes was distinguished by the extensive occurrence of clusters composed of calcium silicate hydrate zones. The conducted studies prove the possibility of using NF and NS as modifying nanoadditives in the technology of cement composites. The addition of nanofibrils from synthesized wollastonite is the most effective and promising and is recommended for use in real construction practice.

Selective Reduction of Iron in High-Phosphorus Oolitic Ore from the Lisakovsk Deposit

Reduction of iron in high-phosphorus oolitic ore from the Lisakovsk deposit using solid carbon, carbon monoxide, and hydrogen. An X-ray phase analysis was used to determine the phase composition of the samples after reduction roasting. When reduced with carbon monoxide or hydrogen, α-iron appears in the samples, while phosphorus remains in the form of iron, calcium, and aluminum phosphates. After roasting with solid carbon, phosphorus is reduced from iron and calcium phosphates and migrates into the metal but remains in aluminum phosphate. A micro X-ray spectral analysis showed that at a temperature of 1000 °C and a holding time of 5 h, during reduction with solid carbon, the phosphorus content in the metallic phase reaches up to 7.1 at. %. When reduced with carbon monoxide under the same conditions, the metallic phase contains only iron, and phosphorus is found only in the oxide phase. When reduced with hydrogen at 800 °C, phosphorus is almost absent in the metallic phase, but at 900 °C, phosphorus is reduced and its content in the metallic phase reaches 2.1 at. %.

Investigation of the corrosion behavior of 29NC alloy in LiCl-KCl melt at 500 oC depending on the content of Li2O and LiOH from 0 to 2 mol. %

Molten chloride salt electrolytes are promising for use as a working medium for the implementation of high-temperature technologies. Alkali metal chlorides are an aggressive environment in relation to structural materials. One of the possible methods of reducing the corrosion damage of a structural material is the method of oxygen passivation of the surface of a metal or alloy by introducing a certain amount of oxygen-containing additives into the melt. The article considers the effect of oxygen-containing impurities (lithium oxide and lithium hydroxide) on the corrosive behavior of a metal material — an alloy of the composition iron–cobalt–nickel. To assess the corrosion resistance of materials, gravimetric analysis, micro-X-ray spectral analysis (XRSA) of the surface and cross-section sections, and X-ray phase analysis (XRF) of the sample surface were used. The dependences of the corrosion rate of the material on the concentration of oxygen-containing additives Li2O and LiOH are presented. Based on the data set of gravimetric, MRSA and XRF data, it was found that 29NC alloy samples in the LiCl–KCl–nLi2O salt melt are not susceptible to corrosion, but in the LiCl–KCl–nLiOH melt, the speed of the 29NC alloy increases significantly due to the interaction of the LiOH additive with the most electronegative component of the alloy — iron.

3D model of a stable triangle LiF–NaBr–KBr four-component reciprocal system Li+, Na+, K+ || F-, Вr-

A 3D model of the phase equilibrium states of the quasi-three-component system LiF–NaBr–KBr, which is a stable triangle of the four-component reciprocal system Li+, Na+, K+ || F-, Br-, has been constructed. Based on the 3D-model, polythermal, isothermal sections and the polytherm of phase crystallization were constructed for the first time. Two polythermal sections contain wide areas of boundary solid solutions based on sodium and potassium bromide. In an isothermal section at 650 оC, the fields of the liquid phase and the coexisting two and three phases are delimited. The crystallization polytherm is represented by three fields. In the crystallization field of lithium fluoride, the area of separation of two liquids is limited. The direction of the ion exchange reaction 2LiBr + NaF + KF = 2LiF + NaBr + KBr was confirmed by thermodynamic calculations at temperatures of 400, 600, 800, 1000K. The exothermic nature of the exchange reaction is confirmed by taking a DTA heating curve for a mixture of powders from 50% LiBr + 25% NaF + 25% KF, and the phase composition of the reaction products LiF + NaBr(OTR) + KBr(OTR) is confirmed by X-ray phase analysis data, where OTR is limited solid solution.

Nanowires made of ternary alloys – synthesis features and magnetic properties

Nanowires of FexCoyCu(100–x–y) and FexNiyCu(100–x–y) alloys have been studied. The features of obtaining such structures by the matrix synthesis method have been investigated. Elemental analysis of nanowires grown at sequentially increasing voltages revealed a significant decrease in the amount of copper, as well as a change in the ratio of the main magnetic elements. X-ray phase analysis showed that FeCoCu is a three-component solid solution, while FeNiCu contains three phases of solid solutions: FeCu with copper content up to 80%, FeNi with high iron content, and NiCu in an amorphous or fine-crystalline state with nickel content up to 80%. Mössbauer spectroscopy revealed that the addition of copper can lead to a change in the angle of magnetic moment misalignment in nanowires, which correlates with magnetometry data.

Sol-gel synthesis, structure and adsorption properties of LiMgxMn(2-x)O4 (0 ≤ x ≤ 0.7) Oxides

Lithium manganese оxides with a spinel structure LiMgxMn(2–x)O4, doped with Mg2+ ions in the range 0 ≤ x ≤ 0.7, were obtained by sol-gel synthesis. Phase composition and morphology of obtained оxides were studied by using X-ray phase analysis and scanning electron microscopy. It is shown, that in the studied range 0 ≤ x ≤ 0.7 Mg-doped lithium manganese оxides saved the structure of the original cubic spinel LiMn2O4, while an increase in parameter a was observed from 8.175 to 8.309 Å and average crystallite size practically unchanged (30–36 nm). Samples of the initial LiMn2O4 and Mg-doped spinels were represented by prismatic particles of submicron (0.1–0.2 µm) and micron (1.0–3.0 µm) sizes, respectively. The effect of the adsorbent dose (0.05–0.3 g/l) and pH (3.0–13.0) of the solution on the adsorption efficiency was studied. The adsorption isotherms of the LiMg0.3Mn1.7O4 samples were described by the Langmuir monomolecular adsorption equation. An increase in the temperature of the model solution from 25 to 45°C was accompanied by an increase in the maximum adsorption of the LiMg0.3Mn1.7O4 samples from 10.50 to 10.98 mmol/g, which indicates the endothermic nature of the adsorption process. The kinetics of adsorption was well described by a pseudo-second order equation, which indicates the occurrence of chemical interaction during the adsorption process.

Structural Changes in Copper Slags During Slow Cooling

The objects of the study were converter slags from the Balkhash copper plant in their initial state and after heat treatment. Using mineralogical and X-ray phase analysis, scanning electron microscopy (SEM), and electron probe microanalysis (EPMA), it was found that the initial converter slag and its thermally treated samples have identical matrices with almost complete coincidence in mineral and phase compositions. The distinguishing feature is the quantitative ratio of mineral components in the slag mass. Almost all of the iron is oxidized and present in the form of fayalite, magnetite, and magnetite, with other elements (silicon, copper, zinc, and aluminum) incorporated into its lattice. The structure of all slag samples indicates an association of sulfur exclusively with copper. Copper in the slags was identified in both metallic and sulfide forms. Slow cooling of the converter slag after its remelting contributes to the reduction in the sulfide–metal suspension in the volume of the melt and its coarsening. During slow cooling, structural changes occur not only in the main oxide part of the slag but also in the polymetallic globules.

Study of the structural and phase state of ceramics synthesized from 6YSZ - Al2O3 – HfO2 by semi–dry pressing followed by sintering in vacuum

The study investigates the properties of 6YSZ – Al2O3 – HfO2 powder mixture and the resulting ceramics obtained by semi-dry pressing followed by sintering in vacuum. X-ray fluorescence spectrometry revealed the primary constituents as zirconium (81%), aluminum (8.7%), yttrium (5.7%), and hafnium (3.5%). The average particle diameter was 0.5 μm, with specific surface area and bulk weight recorded at 18,535 cm2/g and 0.84 g/cm3, respectively. X-ray phase analysis indicated a predominance of monoclinic zirconium dioxide. Sintering at 1400-1600°C transformed the phase composition, enhancing density and microhardness, with values peaking at 5.8 g/cm3 and 12.1 GPa at 1600°C. This process also increased the tetragonal phase content to 63%. The ceramics exhibited the highest crack resistance at 1600°C, attributed to the stabilized tetragonal zirconium dioxide. Microstructural analysis confirmed the homogenous distribution of the elements and the presence of fine fractions influencing microstructural properties. 1600°C was found to be the optimal temperature for sintering the 6YSZ – Al2O3 – HfO2 ceramics.

Raw Materials in the Paste of Ceramics of the Kulaika Culture Surgut Variant (Based on Samples from Barsova Gora)

A multidisciplinary analysis of ceramics from six sites of the Surgut variant of the Kulaika culture at Barsova Gora was made. Technology was assessed using traceological, petrographic, and X-ray phase analyses. At all the sites, the potters used ferruginous clays tempered with grus, grog, sand, and organic material. Fragments in the clay were either rounded, as in sand, or coarse, as in grus. The sand was mainly represented by feldspar and quartz, suggesting that this type of raw material was extracted from nearby non-metallic mineral deposits. The grus consisted of fragments of basaltoids, amphiboles, and pyroxenes, evidencing that it came from igneous common rocks associated with the Surgut volcanic fi eld and spread over a large area. Rocks were probably mined near settlements, perhaps on the floodplain of the Ob. Grog in all the samples was similar to the basic clay in terms of its composition. Three groups of sites were identified, differing in the composition of the clay of which the ceramics were made. This may indicate the presence of several groups within the Iron Age Kulaika population, utilizing various sources of clay.

In the LiCl-KCl melt at 500<sup>о</sup>С depending on the content of Li<sub>2</sub>О и LiOH

Molten alkali metal chlorides used in pyrotechnologies are aggressive corrosive agents. The high operating temperature of the process, the heterogeneity of the environment, and the significant corrosion activity of the molten salt necessitate both the search for stable structural materials and the development of methods for protecting the structural elements of high-temperature technological devices. Corrosion loss reduction techniques traditionally used in low temperature environments are not applicable at high temperatures. The article examines the influence of oxygen-containing impurities (lithium oxide and hydroxide) on the corrosion behavior of metallic nickel (grade NP1) – the main component of candidate structural alloys, a thermodynamically and structurally stable material in the melt for the process of electrolytic refining of spent nuclear fuel. A method for preparing the LiCl–KCl salt electrolyte and obtaining lithium oxide by thermal decomposition of anhydrous lithium hydroxide under vacuum is described, and the concentrations of impurities in the electrolyte and the synthesized lithium oxide are determined. An installation for conducting corrosion tests in an inert atmosphere of a glove box is presented. To assess the corrosion resistance of the material, the following were used: gravimetric analysis, X-ray diffraction analysis of the surface and cross-sectional sections, and X-ray diffraction analysis of the surface of the samples. The dependences of the corrosion rate of the material on the concentration of oxygen-containing additives Li2O and LiOH were obtained. Based on a combination of gravimetric, X-ray microspectral and X-ray phase analysis data, it was established that metallic nickel samples demonstrate high corrosion resistance in the studied melts with the introduction of Li2O and LiOH additives.

SYNTHESIS AND PHYSICO-CHEMICAL PROPERTIES OF A NEW COMPLEX FERRITE

The article discusses the synthesis of new complex ferrite, radiographic and electron microscopic studies. The phase of complex ferrites was synthesized by the method of high-temperature sol-gel synthesis. For the first time, the structure of CrKFe2O5 Composite ferrite was studied by X-ray phase analysis and scanning electron microscope methods, the syngony type, elementary cell parameters, radiographic and pycnometric densities, and elemental analysis were determined. A comparative analysis of the relationship between the parameters of the Crystal cell of primary substances and the parameters of the obtained complex ferrite Crystal cell was carried out. Micro-samples were taken from different parts of the crystallite obtained through a scanning electron microscope, the elemental composition of the crystals was analyzed, and the general type of layer of the complex ferrite surface was demonstrated. As a result, the fact that the compound consists of two phases, the clarity of its construction was determined by the topography and chemical composition of the compound. As a result, it was found that the newly synthesized complex ferrite corresponds to the Formula CrKFe2O5. The particle size of the compounds formed is large (between 200 μm, 20.0 μm, 5.00 μm and 2.00 μm).

Variations of the elemental composition distribution over the thickness of YBa2Cu3O7-δ thin films obtained by pulsed laser deposition from one target

Epitaxial YBa2Cu3O7‒δ (YBCO) films 150-200 and 300 nm thick, respectively, were deposited on SrTiO3 (100) substrates by pulsed laser deposition at different conditions: with and without using the velocity filtration technique. The films have T(R=0) in the range of 77.4 - 87 R(T) depending on the conditions of deposition from one target with YBa2Cu3O6.8 composition. The films contain Zn, Sr, Pd, Ag and Ti impurity elements obtained from the target (a total of no more than 2 at. % ). Data of the film resistance temperature dependences, X-ray phase analysis, analysis of X-ray fluorescence (XRF) spectra and study of the surface relief by SEM methods revealed the nonuniform distributions of impurity and matrix Y, Ba, Cu elements over the film depth. Impurity concentrations near the surface lead to the formation of faceted spiral pyramids on the surface, which probably evolve into large elongated particles according to the Ostwald mechanism. This knowledge is practically important for optimizing pulsed laser deposition technologies and creating 2D instruments and devices for studying physical phenomena.

Structural and electromagnetic properties of 3D printed and electron beam sintered lithium ferrite ceramic

In this work, the structures and electromagnetic properties of lithium ferrite ceramics manufactured by the additive method, based on the extrusion deposition of ferrite samples with a binder and their subsequent heating with high-energy electron beam, were studied. Preliminary synthesis of ferrite powder was carried out by a solid-phase method using iron oxide and lithium carbonate. To prepare ferrite paste, a binder based on ethylcellulose and terpineol was used. The printed samples were sintered by heating with 1.4 MeV electron beam using an ELV-6 accelerator. Using X-ray phase analysis, it was established that the sintered ceramic consists mainly of an ordered α−Li0.5Fe2.5O4 phase and a certain amount of disordered β−Li0.5Fe2.5O4 phase. Ferrite ceramics are characterized by a relative density of 72.6–92.1%, specific saturation magnetization of 63–65 emu/g, Curie temperature of 628–630 °C, electrical resistivity of 108–106 Ω cm, depending on the thickness of the printed sample (200 and 400 μm) and sintering temperature (1100 and 1200 °С).

RESEARCH OF THE POSSIBILITY OF USING CHP ASH IN THE PRODUCTION OF FIRED ASH GRAVEL

The article presents a comparative analysis of the characteristics of the dump ash of the Kyzylorda CHP hydraulic removal. A huge amount of ash, slag waste is collected in the dumps of the CHP, their accumulation in the dumps leads to a violation of the ecology of the environment. The issue of ash, slag waste disposal is an urgent problem. The use of ash and slag not only solves the issue of availability of raw materials, but also allows to improve the quality of products while reducing their cost. One of the valuable components of ash and slag waste is hydraulic removal ash. Hydraulic removal ash as a raw material can be used for the manufacture of artificial concrete aggregates (ash, agglomerate gravel, etc.). Studies were conducted to study the physico-chemical composition, determine the specific effective activity of natural radionuclides, loss during calcination of two types of hydraulic removal ash samples from Kyzylorda CHP (black and gray), which differ in sampling sites from ash dump. When studying the properties of the ash, X-Ray phase analysis was carried out, with the help of which the phase composition of the ash was determined. Work was carried out on the X-Ray phase analysis of ash, determination of the specific effective activity of natural radionuclides, calcination losses, which showed the possibility of using ash for the production of building materials. The conducted studies have confirmed the expediency of using the ash of the Kyzylorda thermal power plant in the production of fired ash gravel.

Possibility of processing phosphogypsum to obtain an alkalizing reagent

Relevance. The need to develop a technology for the disposal of solid and liquid industrial waste to obtain organic-inorganic fertilizer. The growth of industrial production is accompanied by an increase in waste. In modern society, considerable attention is paid to the problem of processing man-made waste to obtain demanded products. Phosphogypsum is the main by-product of the production of fertilizers and phosphoric acid, it is a multi-tonnage waste, its storage leads to the withdrawal of vast territories from circulation. Liquid waste from pig farms also needs to be processed into organic fertilizers. Aim. To study the process of heat treatment of phosphogypsum in the presence of a reducing agent to obtain an alkalizing reagent. This will make it possible to further organize processing liquid and solid agricultural and industrial waste and produce domestic organic fertilizers Methods. Heat treatment of phosphogypsum in the presence of a reducing agent, followed by the preparation of an aqueous suspension to obtain an agent that reduces the acidity of livestock effluents. The samples of heat-treated phosphogypsum obtained during the study were characterized by X-ray phase analysis, electron microscopy. Suspensions with different pH values were obtained on their basis. Results and conclusions. The authors have studied heat treatment of large-tonnage inorganic waste of the chemical industry – phosphogypsum. It was found that the suspension of phosphogypsum heat-treated in the presence of a reducing agent has increased values of the hydrogen index, which can be used to obtain an alkalizing reagent for treating agricultural waste. The authors revealed the optimal technological modes of obtaining a reagent having the maximum pH value of the suspension: the amount of the introduced reducing agent is 0.16 mol/mol CaSO4, the heat treatment temperature is 1000 °C.

Binding properties of synthesized CS glasses activated by alkaline components

The paper presents the synthesis and evaluation of hydration and binding properties of individual minerals with glass-like structures in silicate systems, most often found in technogenic materials based on phosphorus and blast furnace slags. This work aims to determine the optimum composition of CS glasses to obtain binders with given properties, the hydration of glasses of different silicate and aluminosilicate compositions in the presence of solutions of soda, sodium hydroxide, and sodium metasilicate was investigated. The results of X-ray phase and differential-thermal analysis, and infrared spectrum are given, and the hydration structure of the calcium oxide-silicon oxide-alkali component system has been studied. The analysis of hydrate neoplasms of the studied binding systems shows that the most optimal conditions for the synthesis of stone strength with stable physical and mechanical properties are created in the presence of gel-like phase reinforced by hydrosilicates and hydroaluminosilicates of alkaline and alkaline-alkaline-earth composition, characterized by fiber-like structure and possessing the ability to epitaxial fusion with each other, as well as gel-like phase, which they reinforce.