Mechanochemical preparation of Ni<Subscript><Emphasis Type="Italic">x</Emphasis></Subscript>Al<Subscript><Emphasis Type="Italic">y</Emphasis></Subscript>/Al<Subscript>2</Subscript>O<Subscript>3</Subscript> nanocomposites

The mechanochemical preparation of nickel aluminide/corundum (Ni _x Al _y /Al₂O₃) powder nanocomposites is shown to be possible during the mechanochemical aluminum reduction of nickel oxide at various weight proportions of the components.     

Precipitation in Nb-Stabilized Ferritic Stainless Steel Investigated with <Emphasis Type="Italic">in-situ</Emphasis> and <Emphasis Type="Italic">ex-situ</Emphasis> Transmission Electron Microscopy

A Nb-stabilized Fe-15Cr-0.45Nb-0.010C-0.015N ferritic stainless steel is studied with transmission electron microscopy (TEM) to investigate the morphology and kinetics of precipitation. Nb_x(C,N)_y\hbox{Nb}_{x}\hbox{(C,N)}_y and MnS precipitates are present in the steel in the initial condition. Ex-situ TEM analysis is performed on samples heat treated at 973 K, 1073 K, 1173 K, and 1273 K (700 °C, 800 °C, 900 °C, and 1000 °C). Within this temperature range, both Fe₂Nb\hbox{Fe}_2\hbox{Nb} and Fe₃Nb₃X_x\hbox{Fe}_{3}\hbox{Nb}_{3}\hbox{X}_{x} (with X = C or N) precipitates form. Fe₂\hbox{Fe}_2Nb is observed at 1073 K (800 °C).   Fe₃Nb₃X_x\;\hbox{Fe}_{3}\hbox{Nb}_{3}\hbox{X}_{x} precipitates form at the grain boundaries between 973 K and 1273 K (700 °C and 1000 °C). Up to at least 1173 K (900 °C) their fraction increases with time and temperature, but at 1273 K (1000 °C) they lose stability with respect to Nb_x(C,N)_y.\hbox{Nb}_{x}\hbox{(C,N)}_{y}. With in-situ TEM, no phase transition is observed between room temperature and 1243 K (970 °C). At 1243 K (970 °C) the precipitation of Fe₃Nb₃X_x\hbox{Fe}_{3}\hbox{Nb}_{3}\hbox{X}_{x} is observed in the neighborhood of a dissolving Nb₂\hbox{Nb}_2(C,N) precipitate. For sections of grain boundaries where no Nb_x(C,N)_y\hbox{Nb}_x\hbox{(C,N)}_y precipitates are present, Fe₃Nb₃X_x\hbox{Fe}_3\hbox{Nb}_3\hbox{X}_{x} does not form. It is concluded that the precipitation of Fe₃Nb₃X_x\hbox{Fe}_{3}\hbox{Nb}_{3}\hbox{X}_x is directly related to the dissolution of Nb₂\hbox{Nb}_2(C,N) through the redistribution of C or N.     

Microstructure and Properties of Fe<Subscript>3</Subscript>Al-Fe<Subscript>3</Subscript>AlC<Subscript><Emphasis Type="Italic">x</Emphasis></Subscript> Composite Prepared by Reactive Liquid Processing

A Fe₃Al-Fe₃AlC _x composite was prepared using reactive liquid processing (RLP) through controlled mixture of carbon steel and aluminum in the liquid state. The microstructure and phases of the composite were assessed using X-ray diffraction, scanning electron microscopy, energy-dispersive X-ray spectroscopy, optical microscopy, and differential scanning calorimetry. In addition, the density, hardness, microhardness, and elastic modulus were evaluated. The Fe₃Al-Fe₃AlC _x composite consisted of 65 vol pct Fe₃Al and 35 vol pct Fe₃AlC _x (κ). The κ phase contained 10.62 at. pct C, resulting in the stoichiometry Fe₃AlC_0.475. The elastic modulus of the Fe₃Al-Fe₃AlC_0.475 composite followed the rule of mixtures. The RLP technique was shown to be capable of producing Fe₃Al-Fe₃AlC_0.475 with a microstructure and properties similar to those achieved using other processing techniques reported in the literature.     

Agglomeration of Non-metallic Inclusions at Steel/Ar Interface: <Emphasis Type="Italic">In</Emphasis>-<Emphasis Type="Italic">Situ</Emphasis> Observation Experiments and Model Validation

Better understanding of agglomeration behavior of nonmetallic inclusions in the steelmaking process is important to control the cleanliness of the steel. In this work, a revision on the Paunov simplified model has been made according to the original Kralchevsky–Paunov model. Thus, this model has been applied to quantitatively calculate the attractive capillary force on inclusions agglomerating at the liquid steel/gas interface. Moreover, the agglomeration behavior of Al₂O₃ inclusions at a low carbon steel/Ar interface has been observed in situ by high-temperature confocal laser scanning microscopy (CLSM). The velocity and acceleration of inclusions and attractive forces between Al₂O₃ inclusions of various sizes were calculated based on the CLSM video. The results calculated using the revised model offered a reasonable fit with the present experimental data for different inclusion sizes. Moreover, a quantitative comparison was made between calculations using the equivalent radius of a circle and those using the effective radius. It was found that the calculated capillary force using equivalent radius offered a better fit with the present experimental data because of the inclusion characteristics. Comparing these results with other studies in the literature allowed the authors to conclude that when applied in capillary force calculations, the equivalent radius is more suitable for inclusions with large size and irregular shape, and the effective radius is more appropriate for inclusions with small size or a large shape factor. Using this model, the effect of inclusion size on attractive capillary force has been investigated, demonstrating that larger inclusions are more strongly attracted.     

<Emphasis Type="Italic">In-Situ</Emphasis> Synthesis of Cu/Cr-Al<Subscript>2</Subscript>O<Subscript>3</Subscript> Nanocomposite by Mechanical Alloying and Heat Treatment

In this article, a novel method has been used to prepare a copper matrix nanocomposite containing Cu-10 wt pct Cr-10 wt pct Al₂O₃ by heat treatment of the mechanically activated Cu, Al, and Cr₂O₃ powder mixture. Structural evolutions were investigated using the X-ray diffraction (XRD) technique. The microstructure of samples was examined using scanning electron microscopy (SEM). It was found that during the milling process, Cu(Al) solid solution and Cu₉Al₄ phase were formed as the intermediate products, and therefore, Al activity was decreased. Hence, the reduction of Cr₂O₃ with Al was prevented during the ball milling stage. Further heat treatment carried out under argon atmosphere at 900 °C for 8 hours resulted in completion of Cr₂O₃ reduction by Al.     

Corrosion-Resistant Ti-<Emphasis Type="Italic">x</Emphasis>Nb-<Emphasis Type="Italic">x</Emphasis>Zr Alloys for Nitric Acid Applications in Spent Nuclear Fuel Reprocessing Plants

This article reports the development, microstructure, and corrosion behavior of two new alloys such as Ti-4Nb-4Zr and Ti-2Nb-2Zr in boiling nitric acid environment. The corrosion test was carried out in the liquid, vapor, and condensate phases of 11.5 M nitric acid, and the potentiodynamic anodic polarization studies were performed at room temperature for both alloys. The samples subjected to three-phase corrosion testing were characterized using scanning electron microscopy (SEM) and energy-dispersive X-ray microanalysis (EDAX). As Ti-2Nb-2Zr alloy exhibited inferior corrosion behavior in comparison to Ti-4Nb-4Zr in all three phases, weldability and heat treatment studies were carried out only on Ti-4Nb-4Zr alloy. The weldability of the new alloy was evaluated using tungsten inert gas (TIG) welding processes, and the welded specimen was thereafter tested for its corrosion behavior in all three phases. The results of the present investigation revealed that the newly developed near alpha Ti-4Nb-4Zr alloy possessed superior corrosion resistance in all three phases and excellent weldability compared to conventional alloys used for nitric acid application in spent nuclear reprocessing plants. Further, the corrosion resistance of the beta heat-treated Ti-4Nb-4Zr alloy was superior when compared to the sample heat treated in the alpha + beta phase.     

Kinetics of Reduction of CaO-FeO<Subscript><Emphasis Type="Italic">x</Emphasis></Subscript>-MgO-PbO-SiO<Subscript>2</Subscript> Slags by CO-CO<Subscript>2</Subscript> Gas Mixtures

Kinetics of the reaction of lead slags (PbO-CaO-SiO₂-FeO _x -MgO) with CO-CO₂ gas mixtures was studied by monitoring the changes in the slag composition when a stream of CO-CO₂ gas mixture was blown on the surface of thin layers of slags (3 to 10 mm) at temperatures in the range of 1453 K to 1593 K (1180 °C to 1320 °C). These measurements were carried out under conditions where mass transfer in the gas phase was not the rate-limiting step and the reduction rates were insensitive to factors affecting mass transfer in the slag phase. The results show simultaneous reduction of PbO and Fe₂O₃ in the slag. The measured specific rate of oxygen removal from the melts varied from about 1 × 10^?6 to 4 × 10^?5 mol O cm^?2 s^?1 and was strongly dependent on the slag chemistry and its oxidation state, partial pressure of CO in the reaction gas mixture, and temperature. The deduced apparent first-order rate constant increased with increasing iron oxide content, oxidation state of the slag, and temperature. The results indicate that under the employed experimental conditions, the rate of formation of CO₂ at the gas-slag interface is likely to be the rate-limiting step.     

Self-propagating high-temperature synthesis of ceramic materials based on the M<Subscript><Emphasis Type="Italic">n</Emphasis> + 1</Subscript>AX<Subscript><Emphasis Type="Italic">n</Emphasis></Subscript> phases in the Ti-Cr-Al-C system

Compact ceramic materials based on the M_{n + 1}AX _n phases in the Ti-Cr-Al-C system are produced by forced self-propagating high-temperature synthesis (SHS) compaction. The mechanisms of the structure and phase formation in synthetic products, as well as the combustion macrokinetics of the SHS mixture, are studied. Complex investigations of the structure, phase composition, and physical and mechanical properties of new Ti_{2 ? x} Cr _x AlC ceramic materials synthesized at different charging parameters (x = 0, 0.5, 1, 1.5, and 2) are performed. The highest content (96–98%) of the M_{n + 1}AX _n phase in the composition of synthetic products is found to be in samples where just one of the host elements (titanium (x = 0) or chromium (x = 2)) is present. The produced materials have a high heat resistance, and the increase in the chromium concentration is favorable to an appreciable growth in resistance to high-temperature oxidation.     

A Developed Method for Fabricating <Emphasis Type="Italic">In-Situ</Emphasis> TiC<Subscript><Emphasis Type="Italic">p</Emphasis></Subscript>/Mg Composites by Using Quick Preheating Treatment and Ultrasonic Vibration

Quick preheating treatment of the Al-Ti-C pellets and high-intensity ultrasonic vibration are introduced in the fabrication of in-situ TiC _p /Mg composites. Al-Ti-C pellets are preheated for about 130 seconds in the furnace at 1023 K (750 °C), in which magnesium is melted as well. In this process, plenty of heat can be accumulated due to the reactive diffusion between liquid aluminum and solid titanium in Al-Ti-C, and a small amount of Al₃Ti phase is formed as well. After adding the preheated Al-Ti-C into the molten magnesium, thermal explosion takes place in a few seconds. In the meantime, high-intensity ultrasonic vibration is applied into the melt to disperse in-situ formed TiC particles into the matrix and degas the melt as well. Microstructural characterization indicates that in-situ formed TiC particles are spherical in morphology and smaller than 2 μm in size. Furthermore, a homogeneous microstructure with low porosity of the magnesium composite is obtained due to the effect of ultrasonic vibration. A novel approach using the quick preheating treatment technique and high-intensity ultrasonic vibration to synthesize in-situ TiC _p /Mg composites is proposed in our research.     

Rare-earth metals (REMs) in nickel aluminide-based alloys: I. Physicochemical laws of interaction in the Ni-Al-REM and Ni<Subscript><Emphasis Type="Italic">x</Emphasis></Subscript>Al<Subscript><Emphasis Type="Italic">y</Emphasis></Subscript>-REM-AE (alloying element) systems

The data on the Ni-Al-R (R = REM Sc, Y, La, lanthanides) binary and ternary systems and the interactions of three rare-earth metals (yttrium, lanthanum, cerium) with the main alloying elements (Ti (Zr, Hf), Cr (Mo, W) that are introduced into Ni₃Al-based VKNA alloys are analyzed. The binary aluminides of REMs in the Ni-Al-R ternary systems are shown to be in equilibrium with neither NiAl nor Ni₃Al. The solid solution of aluminum in RNi₅, which penetrates deep into these ternary systems, is the most stable phase in equilibrium with Ni₃Al. In the NiAl (Ni₃Al)-AE-R systems, REM precipitation (segregation) on various defects and interfaces in nickel aluminides is likely to be the most probable, and REMs are thought to interact with the most active impurities in real alloys (C, O, N), since REMs have a large atomic radius and, thus, are virtually undissolved in nickel, aluminum, and nickel aluminides.     

Effects of test temperature and grain size on the charpy impact toughness and dynamic toughness (<Emphasis Type="Italic">K</Emphasis><Subscript><Emphasis Type="Italic">ID</Emphasis></Subscript>) of polycrystalline niobium

The effects of changes in test temperature (−196 °C to 25 °C) and grain size (40 to 165 μm) on the dynamic cleavage fracture toughness (K _ID ) and Charpy impact toughness of polycrystalline niobium (Nb) have been investigated. The ductile-to-brittle transition was found to be affected by both changes in grain size and the severity of stress concentration (i.e., notch vs fatigue-precrack). In addition to conducting impact tests on notched and fatigue-precracked Charpy specimens, extensive fracture surface analyses have been performed in order to determine the location of apparent cleavage nucleation sites and to rationalize the effects of changes in microstructure and experimental variables on fracture toughness. Existing finite element analyses and the stress field distributions ahead of stress concentrators are used to compare the experimental observations with the predictions of various fracture models. The dynamic cleavage fracture toughness, K _ID , was shown to be 37±4 MPa√m and relatively independent of grain size (i.e., 40 to 105 μm) and test temperature over the range −196 °C to 25 °C.     

Water Network in Room-Temperature Ionic Liquid: <Emphasis Type="Italic">N,N</Emphasis>-Diethyl-<Emphasis Type="Italic">N</Emphasis>-Methyl-<Emphasis Type="Italic">N</Emphasis>-2-Methoxyethyl Ammonium Tetrafluoroborate

Crystal structures of room-temperature ionic liquid (RTIL)-H₂O mixtures are determined by the X-ray diffraction method. The RTIL is N,N-diethyl-N-methyl-N-2-methoxyethyl ammonium tetrafluoroborate, [DEME][BF₄]. At 0.9 mol pct H₂O, two kinds of superstructures occur simultaneously without a strain. Also, the volume of the unit cell is very small only at 0.9 mol pct additives. This relates to the composite domain structure, including a twin-related one, as an elastic anomaly. At other water concentrations, such an extraordinary behavior is not observable. By assuming a sublattice having an equivalent lattice constant, a water network at 1 mol pct H₂O is simulated using a Monte Carlo (MC) method. The network develops over the medium range in the simulation box.     

Thermodynamics and Kinetics to Alloying Addition on <Emphasis Type="Italic">In-Situ</Emphasis> AlN/Mg Composites Synthesis <Emphasis Type="Italic">via</Emphasis> Displacement Reactions in Liquid Mg Melt

Based on the Wilson equation, extended Miedema model, and hard sphere theory, new models are developed theoretically only using the quantities of the pure component and are applied to investigate the thermodynamical and kinetic effect of alloying additions on in-situ AlN formation via displacement reaction in Mg-Al alloy melt. The results show that the alloying additions such as Si, Zn, and Cu can promote the formation of AlN in Mg-Al melt both in thermodynamics and kinetics. Meanwhile, other elements, including Mn, Nd, Ce, Ni, and La, must be matched properly in order to produce the desired reinforcement AlN in liquid Mg-Al melt.     

Estimation of the Ultimate Tensile Strength of Steel from Its <Emphasis Type="Italic">HB</Emphasis> and <Emphasis Type="Italic">HV</Emphasis> Hardness Numbers and Coercive Force

A formula is derived to accurately describe the tabulated relation between the Brinell (HB) and Vickers (HV) hardnesses of steel over the entire range of their possible variation. This formula and the formulas describing the relation between the HB hardness of chromium–molybdenum and chromium–nickel steels and their ultimate tensile strength σ_u are used to analyze the change in σ_u of 38KhNM steel upon quenching and tempering. The data that reveal a relation between σ_u of 38KhNM steel and its coercive force are obtained.     

Synthesis of Al-Zr Alloys <Emphasis Type="Italic">Via</Emphasis> ZrO<Subscript>2</Subscript> Aluminum-Thermal Reduction in KF-AlF<Subscript>3</Subscript>-Based Melts

Physical–chemical investigations of KF-AlF₃ melts were carried out in order to develop the scientific basis of the technology for Al-Zr alloy synthesis. The possibility of Al-Zr alloy synthesis via the aluminum-thermal method was shown. The liquidus temperatures of KF-AlF₃ and KF-NaF-AlF₃ melts with additions of Al₂O₃ and ZrO₂ were determined using the thermal analysis method in the temperature range from 873 K to 1173 K (600 °C to 900 °C). The dependency of the solubility of ZrO₂ in KF-AlF₃ and KF-NaF-AlF₃ melts on Al₂O₃ concentration was measured.     

Crystallization of Co<Subscript>100-<Emphasis Type="Italic">x</Emphasis></Subscript>Pt<Subscript><Emphasis Type="Italic">x</Emphasis></Subscript>B<Subscript>10</Subscript>Si<Subscript>12</Subscript> amorphous metallic alloys

Alloys of Co_78-x Pt _x B₁₀Si₁₂ were produced using the melt-spin process in order to study the crystallization behavior and ensuing magnetic properties of the Co-Pt amorphous alloys as a function of the Pt content. We showed that when x>15, well below its stoichiometric composition, CoPt intermetallic compound crystallized in the amorphous alloy. Below this composition, the main crystallization product was Co with Pt dissolved in its lattice. The nucleation of CoPt greatly altered the crystallized microstructures and magnetic properties of the Co-Pt amorphous alloys during annealing. In spite of the nucleation of CoPt with its high magnetic anisotropy, the highest coercivity was obtained when x was 15, free of the CoPt grains. It was also concluded that the Pt addition, in general, triggered crystallization to occur at a progressively lower temperature.     

<Emphasis Type="Italic">In situ</Emphasis> Observation of Calcium Oxide Treatment of Inclusions in Molten Steel by Confocal Microscopy

Calcium treatment of aluminum killed steel was observed in situ using high-temperature confocal scanning laser microscope (HT-CSLM). This technique along with a novel experimental design enables continuous observation of clustering behavior of inclusions before and after the calcium treatment. Results show that the increase in average inclusion size in non-calcium-treated condition was much faster compared to calcium-treated condition. Results also show that the magnitude of attractive capillary force between inclusion particles in non-treated condition was about 10^?15 N for larger particles (10 µm) and 10^?16 N for smaller particles (5 µm) and acting length of force was about 30 µm. In the case of calcium-treated condition, the magnitude and acting length of force was reduced to 10^?16 N and 10 µm, respectively, for particles of all sizes. This change in attractive capillary attractive force is due to change in inclusion morphology from solid alumina disks to liquid lens particles during calcium treatment.     

Reactive synthesis of <Emphasis Type="Italic">in-situ</Emphasis> ZrAl<Subscript>3</Subscript>-Al<Subscript>2</Subscript>O<Subscript>3</Subscript>-Al composites

In this work, a reactive synthesis process is proposed to obtain ZrAl₃-Al₂O₃ particulate-reinforced aluminum matrix composites. The process involves the in-situ formation of Al₂O₃ and ZrAl₃ from Al-ZrO₂ green compacts. Upon compact heating, it is found that reduction of ZrO₂ by molten aluminum occurs at temperatures above 750 °C, leading to the development of ZrAl₃ and Al₂O₃ phases. Thermodynamically, it is found that the reduction of zirconium oxide is driven mainly by the dissolution of Zr in molten aluminum. Because the solubility of Zr in liquid aluminum is extremely small, the formation of ZrAl₃ is favored after relatively small Zr dissolutions. The first Zr-Al intermetallics to form at the lowest temperatures seem to be metastable, as infered from the measured atom ratios for Al : Zr of 2.83 : 1. At increasing temperatures, the reaction comes into completion, resulting in the formation of equilibrium intermetallic ZrAl₃ phases. The results obtained from differential scanning calorimetry (DSC) indicate that by increasing the scanning rates, both the reaction temperature and the exothermic peak intensity also increase. Alternatively, it is found that by reducing the amount of ZrO₂ in the green compact, the in-situ reaction temperatures also shift toward higher values.     

<Emphasis Type="Italic">In Situ</Emphasis> Observation of Calcium Aluminate Inclusions Dissolution into Steelmaking Slag

The dissolution rate of calcium aluminate inclusions in CaO-SiO₂-Al₂O₃ slags has been studied using confocal scanning laser microscopy (CSLM) at elevated temperatures: 1773 K, 1823 K, and 1873 K (1500 °C, 1550 °C, and 1600 °C). The inclusion particles used in this experimental work were produced in our laboratory and their production technique is explained in detail. Even though the particles had irregular shapes, there was no rotation observed. Further, the total dissolution time decreased with increasing temperature and decreasing SiO₂ content in the slag. The rate limiting steps are discussed in terms of shrinking core models and diffusion into a stagnant fluid model. It is shown that the rate limiting step for dissolution is mass transfer in the slag at 1823 K and 1873 K (1550 °C and 1600 °C). Further investigations are required to determine the dissolution mechanism at 1773 K (1500 °C). The calculated diffusion coefficients were inversely proportional to the slag viscosity and the obtained values for the systems studied ranged between 5.64 × 10^?12 and 5.8 × 10^?10 m²/s.