Phase Composition Research Articles

Simulation of the Evolution of Phase Composition and Austenite Grain Size upon Multi-Pass Hot Deformationof Low-Alloy Steels

The paper presents a model for predicting the structural characteristics and phase composition of low-alloy steels upon hot rolling in the multi-pass deformation mode. The model considers recovery, dynamic, primary, dynamic and static recrystallization of grains, and the normal grain growth, as well as nucleation (including accelerated nucleation during deformation), growth or dissolution, and coarsening of carbonitride particles. The comparison between the calculated results and the experimental data available in the publications shows a satisfactory agreement.

Influence of Low-Energy High-Current Electron Beam Exposure on the Phase Composition and Corrosion Resistance of the AM60 Magnesium Alloy

The surface of an AM60 (Al – 5.5, Zn – 0.2, Cu – 0.009, Fe – 0.005, Si – 0.1; Ni – 0.002, Mn – 0.3 wt.%, Mg – the rest) magnesium alloy was exposed to a low-energy high-current electron beam. After the irradiation, the content of the β-phase (Mg17Al12) decreases and the aluminum content increases in the alloy surface layer. After the exposure to the electron beam, the corrosion resistance of the alloy in a 1-molar NaCl solution increases significantly compared to the initial state. The physical reason for the increase in the alloy corrosion resistance after exposure to the electron beam is the higher corrosion resistance of the oxide film formed on the alloy surface due to the increased aluminum content.

A Study on Metallurgical Artifacts Excavated from Luojiaba Site H235 in the Eastern Sichuan Region during the Eastern Han Dynasty

Currently, research remains limited on ironworking workshops in China and even throughout East Asia. The discovery of Luojiaba Site H235 in 2021 provides significant new material on this issue. This paper comprehensively organized the metallurgical artifacts and employed technological methods such as XRF and SEM-EDS to analyze the slag and hammerscale excavated from Luojiaba Site H235. First, the chemical composition and microstructural phases of the slag were analyzed, with an examination of the hammerscale. Second, the processes leading to the formation of slag and hammerscale are discussed. Third, based on the scale of the site, the chemical composition, and the characteristic shapes of the slag, combined with Serneels’ theoretical framework for quantitative analysis of forging slag, the slag unearthed from Luojiaba Site H235 was tentatively categorized as forging slag. This suggests that the workshop primarily produced or repaired iron objects through forging. Finally, considering the furnace shapes observed at contemporary sites and discussions on the potential sources of iron materials at the Luojiaba site, speculations are made regarding the furnace structure at the Luojiaba site and the possible origin of its iron materials. Unlike ironworking workshops at other contemporary sites, the location of the forging workshop at Luojiaba Site H235 presents a distinctly different choice, situated within a village or town during the Eastern Han Dynasty. This choice of location may reflect a phenomenon closer to consumer proximity. Therefore, analyzing metallurgical artifacts unearthed from Luojiaba contributes to understanding the operation of ironworking workshops and the distribution of resources in village-level settlements in the eastern Sichuan region during the Eastern Han Dynasty.

Performance Assessment of a Novel Green Concrete Using Coffee Grounds Biochar Waste

An actual scientific problem in current concrete science is poor knowledge of the problem of modifying concrete with plant waste. At the same time, plant waste benefits from other types of waste because it is a recycled raw material. A promising technological approach to modifying concrete with plant waste is the introduction of components based on the processing of coffee production waste into concrete. This study aims to investigate the use of biochar additives from spent coffee grounds (biochar spent coffee grounds—BSCG) in the technology of cement composites and to identify rational formulations. A biochar-modifying additive was produced from waste coffee grounds by heat treatment of these wastes and additional mechanical grinding after pyrolysis. The phase composition of the manufactured BSCG additive was determined, which is characterized by the presence of phases such as quartz, cristobalite, and amorphous carbon. The results showed that the use of BSCG increases the water demand for cement pastes and reduces the cone slump of concrete mixtures. Rational dosages of BSCG have been determined to improve the properties of cement pastes and concrete. As a result of the tests, it was determined that the ideal situation is for the BSCG ratio to be at a maximum of 8% in the concrete and not to exceed this rate. For cement pastes, the most effective BSCG content was 3% for concrete (3%–4%). The compressive and flexural strengths of the cement pastes were 6.06% and 6.32%, respectively. Concrete’s compressive strength increased by 5.85%, and water absorption decreased by 6.58%. The obtained results prove the feasibility of using BSCG in cement composite technology to reduce cement consumption and solve the environmental problem of recycling plant waste.

Fatigue Resistance of the Sheets of Heat-Resistant Titanium Alloys

The results of a study of the resistance to fatigue fracture of sheets made of heat-resistant titanium alloys VT18U (Ti–6.5Al–4.3Zr–2.4Sn–0.8Nb–0.7Mo–0.1Si, wt.%), VT8 (Ti–6.4Al–3.4Mo–0.3Si, wt.%), and VT25U (Ti–6.51Al–3.76Zr–1.71Sn–3.94Mo–0.5W–0.13Si, wt.%) has been presented. Fatigue curves have been obtained in the initial state and in the oxidized one after isothermal annealing at a temperature of 560 °C for 1000 h in air. It has been established that after annealing, the fatigue resistance of all oxidized alloys in the low-cycle region decreases by an order of magnitude. The fatigue limit of the oxidized alloys VT18U and VT25U does not change and is about 320 MPa. The high-cycle fatigue limit of the VT8 alloy decreases from 300 MPa in the initial state to 230 MPa in the oxidized state. It has been established that after annealing, the phase composition of an oxide of 250 nm in thickness on the surface of the alloys is different and contains the phases of anatase and rutile for the VT18U and VT25U alloys and contains predominantly rutile for the VT8 alloys, which is why the fatigue limit of the oxidized alloys differs.

The Impact of Thermal Treatment on the Structural, Optical and Electrochemical Characteristics of Tin Sulfide Films

The development of eco-friendly, cost-effective, and naturally abundant electrode materials for supercapacitors is gaining critical importance in current energy storage research. This study focuses on the synthesis of tin sulfide (SnSx) films via the eco-friendly successive ionic layer adsorption and reaction (SILAR) method, employing varying quantities of L-ascorbic acid (0.8 and 1.0 g) as a reducing agent. Tin sulfide films were deposited on fluorine-doped tin oxide (FTO) glass substrates and subsequently annealed in an inert atmosphere at temperatures ranging from 200 to 400 °C, resulting in thin films of varying thicknesses (100–420 nm). The structural and compositional characteristics of the films were thoroughly analyzed using Raman spectroscopy to confirm the purity and spectroscopic signatures of the sulfides. Further characterization was performed to assess the films’ morphology (scanning electron microscopy, SEM), phase composition (X-ray diffraction, XRD), surface chemical states (X-ray photoelectron spectroscopy, XPS), optical properties (UV–Vis spectroscopy), and electrical properties (Hall measurements). The gathered data were then used to evaluate the potential of tin sulfide films as electrode materials in supercapacitors, highlighting their suitability for sustainable energy storage applications.

Development of the High‐Temperature Knudsen Effusion Mass Spectrometry in the Nordic Countries

In this article, a brief review of the development of the Knudsen effusion mass spectrometric (KEMS) approach in the Theoretical Metallurgy Department of the KTH Royal Institute of Technology and in the in the Laboratory of Metallurgy of the Helsinki University of Technology and modifications of quadrupole model QMG420 mass spectrometers, is presented. The thermodynamic data obtained from vaporization of standards, such as NaCl, CsCl, B2O3, and Ag, and of the B2O3–Al2O3 and ZnO–P2O5 systems is compared with the data obtained using a magnetic MS1301 mass spectrometer. For the first time, composition of the vapor phase over the Dy2O3–DyF3, CaO–CaCl2, and Cu–Mg systems and the partial pressures of components at high temperatures are investigated. The experimental data obtained for the investigated systems are used for prediction of the vaporization processes and modeling of thermodynamic properties and high‐temperature phase equilibria in the multicomponent systems used in metallurgy. An account is given of the detailed studies of the vaporization processes and thermodynamic properties of some multicomponent systems composed of oxides, fluorides, and carbonates forming mold powders for continuous casting of steel. Some new directions of the ongoing studies by the KEMS method are summarized.

Microstructural Study of Medieval Crucible Steels from Archaeological Sites in Central and Northwest Asia: Identifying the Bulat

The microstructure of 9th–15th century artifacts made of crucible steel, found at sites in Central and Northwest Asia, is described. Metallographic study of items from settlements and burials with precise data on chronology, location, and accompanying artifacts is important for reconstructing the history of bulat steel and the technology of melting and processing ultra-high-carbon crucible steel. The study of the macro- and microstructure, and the chemical analysis of such items indicate an extremely high content of carbon—1.7–2.1 %. The characteristic feature of their microstructure is a dark matrix with white inclusions of ledeburite and iron carbides. The combination of structural components is reflected in the patterned structure of the metal. These properties suggest that such metal is identical to bulat steel. Findings of macrostructural analysis extend our knowledge of the varieties of this metal, its structural features, phase composition of separate groups of ultra-high-carbon crucible steel, smelting technology, plastic and thermal treatment, and physical properties.

Influences of Sr(OH)2 on the Structure and Corrosion Resistance of Micro‐Arc Oxidation Coatings Formed on TC4 Titanium Alloy

ABSTRACTIn order to improve the comprehensive properties of TC4 titanium alloy, micro‐arc oxidation (MAO) coating is prepared on the surface of a TC4 substrate in a basic electrolyte with varying concentrations of Sr(OH)2. The surface morphology, phase composition, element distribution, and corrosion resistance of MAO coatings are analyzed by scanning electron microscopy, X‐ray diffraction, an energy‐dispersive spectrometer, the electrochemical test, and the erosion–corrosion test. The results show that the voltage of the MAO process increases and then decreases; the surface morphology and density of the coatings are greatly improved after doping Sr(OH)2. When the concentration of Sr(OH)2 is 0.6 g L−1, the thickness, hardness, and adhesion strength of the coating reach the maximum values of 37.04 μm, 836.2 HV, and 21.8 N, respectively. At this time, the wear resistance and corrosion resistance are the best, and the friction coefficient and the corrosion rate are the lowest: 0.3352 and 1.04 × 10−10 mm a−1, respectively.

Refining of Secondary Pb with Retention of Sn Using Al and Ca Additions

AbstractLead grid from spent lead-acid batteries contains significant amounts of tin and antimony. In classical pyro-refining processes of lead, tin oxidizes and is transferred to dross, making its recovery problematic and expensive. This paper presents an innovative method of pyro-refining lead using metallic aluminum and calcium to purify the lead from contaminants while retaining a higher amount of tin than in the traditional process. The changes in the chemical composition of an impure lead alloy containing tin, under the influence of refining by adding Al and/or Ca, are discussed based on laboratory-scale studies. Microanalysis of the metallic dross formed during the process was conducted. Analyses of the metallic dross microstructures showed that lead impurities, such as Sb, As, Cu, Se, and Te, tend to accumulate in areas containing Al or Ca. The amount and form of dross produced in industrial practice indicate that its removal would be challenging. Therefore, in the second part of the study, the metallic dross was subjected to a reduction process, and the resulting products were analyzed for their chemical and phase composition. The analyses indicate that the degree of impurities return to the lead during reduction varied significantly depending on the method used.

Purification effect of pyrolyzed filler on the flammability of polylactide matrix

Abstract Research efforts are underway around the world to develop efficient recycling of the continuous phase of polymer composites toward reuse. It has already been demonstrated that pyrolyzed filler (PF) can be successfully used as a flame retardant for synthetic polyesters, including recycled ones. Therefore, the purpose of this work was to test the effect of PF on the flammability and thermal properties of the biopolyester phase. For this purpose, the pyrolysis technique was used, which yields a valuable solid phase in addition to the gas and liquid phases. To effectively give it a second life, a proprietary method of modifying the filler recovered by pyrolysis was developed to effectively separate and remove an organic part in the form of a layer of amorphous carbon (a-C), which acts as a universal sorbent. For this purpose, the a-C phase was extracted using binary solvent and replaced it using three types of salts: ammonium salt of benzyl phosphite, 1-butyl-3-methylimidazolium chloride (BMIC), and methyldodecylbenzyl trimethyl ammonium chloride (BMAC). Using a high-temperature processing technique, polylactide composites containing 5% (by weight) additive were obtained. The results of thermal (TGA, DSC) and flammability (PCFC, UL94, LOI) analysis studies show that the use of BMIC and BMAC salts for the intended purpose is particularly promising. The thermal stability of PLA composites containing SF-BMIC and SF-BMAC increased by 30 K and the flammability decreased by 23%. These promising results have opened up new avenues of research toward the synthesis of bio-flame retardants dedicated specifically to polylactide. Graphical abstract

Electrochemical production of zirconium silicides from KCl–K<sub>2</sub>SiF<sub>6</sub>–ZrO<sub>2</sub> melt

The unique properties of zirconium silicides attract the attention of a large number of authors from various scientific fields. Expansion of application methods also poses the challenge of developing new, more environmentally friendly and affordable methods of production. The most environmentally friendly method without equipment requirements is the electrolysis of the molten salt. The work proposes a method for producing zirconium silicides by electrolysis of the KCl–K2SiF6–ZrO2 melt. In order to substantiate the electrolysis parameters, the kinetics of cathodic reduction was studied and the limiting stage of the process was determined. The structure and phase composition of the cathode deposit were studied using X-ray diffraction and electron scanning microscopy. In the course of the work, conclusions were drawn about the change in the content of the ZrO2 additives on the morphology of the sediment, and it was also suggested that it was possible to obtain zirconium silicides from more accessible raw materials, such as zircon.

Preparation and performance study of modified diatomite based PCM for construction

Phase change energy storage technology provides a good solution to the spatial and temporal mismatch of energy use in buildings, but organic solid–liquid phase change materials suitable for the building sector limit their application due to leakage problems. To mitigate the effects of the above problems, diatomite (DME) is designed as the carrier for encapsulation in this experiment. Adsorption performance of DME is improved through double effects of 600°C high-temperature calcination and hydrochloric acid modification. The binary low eutectic mixture was prepared by co-melting of lauric acid (LA) and octadecyl alcohol (OD) with mass ratio of 70:30. Shape-stabilized composite phase change material (SSCPCM) was prepared by vacuum adsorption method with LA-OD and DME with a mass ratio of 35:65 and the melting temperature and latent heat of SSCPCM are 39.10°C and 54.02 J/g. It was experimentally evaluated that the surface impurities of modified DME under microscopic conditions were removed and LA-OD was uniformly embedded in the micropores of DME, and the prepared SSCPCM was able to maintain a thermal inertia of 39°C with good thermal properties and thermal stability, thus SSCPCM could be used as a building energy-saving material to reduce building energy consumption, in addition to expanding the utilization of inorganic mineral materials.

Microcrystalline and nanocrystalline structure of diamond films grown by MPCVD with nitrogen additions: Study of transitional synthesis conditions

This research explores the complex influence of nitrogen concentration and substrate temperature on the resultant properties of polycrystalline diamond (PCD) films grown by microwave plasma chemical vapor deposition (CVD). In particular, we investigated the growth parameters to find the exact conditions for changing the morphology of the resulting film from microcrystalline (MCD) to nanocrystalline (NCD). A series of 2 µm-thick polycrystalline diamond films was grown on Si substrates in methane-hydrogen–nitrogen gas mixtures with varied: (i) nitrogen concentration (0–2 %) and (ii) substrate temperature (700–1050 °C). Comprehensive characterization techniques, including scanning electron microscopy (SEM), micro-Raman spectroscopy, and X-ray diffraction, were employed to assess the morphological, structural, and spectroscopic properties of the films. The study reveals that even minor additions of nitrogen significantly modulate secondary nucleation, impacting both film morphology and phase composition. Furthermore, substrate temperature emerges as another critical parameter, influencing the growth kinetics and crystallite size. The comparison of the characteristics of grown PCD films allowed us to find conditions for the formation of NCD films with minimal surface roughness and maximal growth rate: nitrogen concentration [N2] ≈ 0.2–0.5 % and temperature T ≈ 850–900 °C. These findings can be used to optimize the CVD synthesis parameters of PCD films for applications as protective or friction-reducing layers, as well as for superhard cutting tools and optical devices.

Investigation of the Influence of the Oxygen Flow Rate on the Mechanical, Structural and Operational Properties of 86WC-10Co-4Cr Coatings, as Determined Using the High-Velocity Oxyfuel Spraying Method

The structural-phase composition and tribological and performance properties of coatings based on an 86WC-10Co-4Cr composition obtained by the HVOF method at varying (150 L/min, 170 L/min, 190 L/min) oxygen flow rates were studied. The results showed that the coefficient of friction of coatings in gear oil remained almost unchanged with the variation in oxygen flow rate. However, microhardness increased significantly with an increasing oxygen flow rate, reaching a maximum at 190 L/min. An increasing oxygen flow rate was also accompanied by an increase in roughness and coating thickness, with a decrease in porosity, particularly notable at 190 L/min. Adhesion strength reached the maximum values for the A2 and A3 coatings under high loads. The phase composition of the coatings included WC, W2C and CoO phases irrespective of the oxygen flow rate, and their microstructure was characterized by a more homogeneous and dense structure. Thus, this study confirmed that the optimal oxygen flow rate for achieving an improved performance and tribological characteristics of 86WC-10Co-4Cr coatings is 190 L/min.

Effect of Cr content on the high temperature oxidation behavior of FeCoNiMnCrx porous high-entropy alloys

FeCoNiMnCr porous high-entropy alloys were prepared using the activation reaction sintering method with Fe, Co, Ni, Mn, and Cr as raw materials. The oxidation behaviors of FeCoNiMnCrx porous high-entropy alloys with different Cr contents, such as pore structure, the surface oxide film phase composition, structure, and morphology, were characterized by X-ray diffraction (XRD), electron probe micro analysis (EPMA), energy dispersive X-ray spectroscopy (EDS), and pore tester after high-temperature oxidation at 800–1000 °C. The results indicate that the initial porous high-entropy alloy comprises a single FCC solid solution phase. With the increase in Cr content, the average pore diameter, average porosity, and air permeability of the porous high-entropy alloy also increase. The oxidation kinetics of the porous high-entropy alloy after exposure to temperatures between 800 °C and 1000 °C follows a single-stage parabolic evolution law. At the same oxidation temperature, With the increase of Cr content, the oxidation gains gradually increased, at the same Cr content at different temperatures, the antioxidant performance of 1000 °C was the weakest, followed by 800 °C, and 900 °C showed excellent antioxidant performance. The oxidation products are mainly Mn2O3, Mn3O4, (Mn, Cr)3O4, Cr2O3and Fe2O3.

Synergistic modulation of SrTiO3-TiO2 colossal permittivity system by internal lattice defects and phase composition: Experimental and theoretical investigations

The SrTiO3–TiO2 composite ceramics with different contents of La doping were fabricated by traditional solid-state sintering methods. The performance of the colossal permittivity ceramics was enhanced by the synergistic design of the internal defect structure and phase composition. When the doping content is 2%, SrTiO3–TiO2 composite ceramics possessed a colossal permittivity (ԑr ∼ 1.1 × 105), low dielectric loss (tanδ ∼ 0.050) and favorable thermal stability (−70 °C-150 °C, ΔC/C25°C ≤ ±15%). Phase structure analysis suggested that a TiO2 secondary phase was induced at the grain boundaries of SrTiO3 phase with the addition of La3+ ions. XPS and dielectric behavior analyses revealed that oxygen vacancies and lattice defects formed by inhomogeneous ion-doping act to modulate the dielectric behavior in ceramics. The IBLC interfacial effects in relation to semiconductor grains and insulation grain boundaries are the main contributors to the colossal permittivity (CP) properties of ceramics, and the contribution of the IBLC effects becomes more prominent with increasing doping content. On the basis of first-principles analysis, the ceramic lattice undergoes severe deformation when the La content is increased, and the gathering of electrons at oxygen vacancies and defects is evident. As a result, it leads to enhanced grain semiconducting properties and interfacial effects, which facilitate colossal permittivity and low dielectric loss for ceramics. The results are prospective in the application of CP ceramics.

Coloring Multilayer Zirconia May Affect Its Optical and Mechanical Properties.

The coloring process of monolithic dental zirconia caused considerable debate on the possible effects of different coloring methods. The main objective of this study was to investigate the influence of pigments in 3 multilayer 5-mol% yttria partially stabilized zirconia (5Y-PSZ) disks (Lava Esthetic A2 [Zr-AGG_A2] and Bleach [Zr-AGG_BL], both 3M Oral Care, and Katana STML A2 [Zr-NoAGG], Kuraray Noritake). The influence of pigment addition on the translucency parameter (TP00), fracture toughness, Vickers hardness, biaxial strength, and hydrothermal stability was assessed and correlated with the microstructure and phase composition. The pigment composition and distribution were evaluated by light and fluorescence microscopy, electron probe microanalysis, and nano-scanning electron microscopy. The chemical and phase composition and aging behavior were assessed using X-ray fluorescence and X-ray diffraction, respectively, while the aging sensitivity of the pigments was evaluated using micro-Raman spectroscopy. In contrast to Zr-NoAGG, possessing a typical 5Y-PSZ microstructure, the pigment additions in both Zr-AGG_A2/BL zirconia resulted in large yellow and blue fluorescent Er-, Hf-, and Al-containing agglomerates composed of small grains (0.57 µm and 0.38 µm, respectively, vs. 0.92 µm for the surrounding grains) with lower Y2O3 content. Zr-AGG_A2 had the lowest aging resistance, with transformation degradation occurring exclusively within the pigment agglomerates. All zirconia grades had a high Y2O3 content (4.2%-5.7 mol%) tetragonal ZrO2 phase and a high (42%-55 wt%) cubic ZrO2 phase content. Although no statistical differences were measured for hardness and toughness, Zr-NoAGG had a significantly higher TP00, higher flexural strength, and lower mechanical reliability compared to both Zr-AGG_A2/BL zirconia. The rare-earth oxide-containing zirconia agglomerates that were added as pigments to the multilayered monolithic Zr-AGG_A2/BL zirconia are the cause for their lower optical and mechanical properties and reduced aging resistance.

Structure and properties of powders obtained by electrodispersion of pure Nickel metal waste in distilled water

Purpose. Investigation of the composition, structure and properties of powder materials obtained by electrodispersion of nickel waste of the PNK-0T1 brand in an oxygen-containing medium – distilled water.Methods. To determine the composition, structure and properties of powder materials, samples of powders obtained from waste nickel grade PNK-0T1 were studied. The powder material was obtained by electroerosive dispersion in distilled water. Microanalysis of powder particles was carried out using a scanning electron microscope, an analysis of the size distribution of powder particles was obtained using a particle size analyzer, an X-ray spectral microanalysis of powder particles was carried out using an energy-dispersive X-ray analyzer embedded in a scanning electron microscope, an analysis of the phase composition of powder particles was carried out using X-ray diffraction on the diffractometer.Results. During the study, it was revealed that the shape of the particles obtained from nickel powders is spherical and elliptical, and agglomerates of smaller particles are also noted on the increase. Oxygen and nickel are present in the composition of powder materials. The phases of pure nickel and nickel oxide NiO are marked in the phase composition. From the analysis of the granulometric histogram, it follows that the particle size spread varies in the range of 0.26...18.62 microns, the average volume diameter of the particles was 5.2 microns.Conclusion. The obtained research results can be used to develop a new heavy pseudo-alloy using metal waste from expensive raw materials by the method of electroerosive dispersion, followed by improvement and optimization of the composition and structure of the alloy.

Effect of calcination temperature on the activity of basalt tailings for the lightweight geopolymer from microwave curing

Basalt, the most widely distributed alumino-silicate volcanic rock on Earth, is commonly utilized in construction aggregate area. The challenge lies in how to utilize the tailings produced during mining processes to create high-value products through energy-efficient and environmentally-friendly means. A previous study has already shown the use of basalt tail powder as raw material for lightweight geopolymer materials supported microwave curing, without an extensive focus on mechanical properties, in turn known to be significantly affected by the reactivity of constituents. Here, calcination operations are discussed in their impact on the activity of basalt for lightweight geopolymer from microwave curing. Additionally, the thermal characteristics of basalt during temperature were analyzed using differential scanning calorimetry, scanning electron microscopy, Fourier transform infrared spectroscopy, and X-ray diffraction analyses were employed to examine the micromorphology, chemical structure, phase compositions, and reaction degree of basalt and its alkali activated products. The results prove that basalt is a sustainable raw material for geopolymers, with properties already optimized without calcination, in turn determining a slight increase only at 750 °C (resulting in compressive strength >7 MPa, with a porosity of 30 %). The effect mechanism of calcination temperature on the activity of basalt tailings for the lightweight geopolymer from microwave curing is also discussed.