Inclusion Detection in Aluminum Alloys <Emphasis Type="Italic">Via</Emphasis> Laser-Induced Breakdown Spectroscopy

Laser-induced breakdown spectroscopy (LIBS) has shown promise as a technique to quickly determine molten metal chemistry in real time. Because of its characteristics, LIBS could also be used as a technique to sense for unwanted inclusions and impurities. Simulated Al₂O₃ inclusions were added to molten aluminum via a metal-matrix composite. LIBS was performed in situ to determine whether particles could be detected. Outlier analysis on oxygen signal was performed on LIBS data and compared to oxide volume fraction measured through metallography. It was determined that LIBS could differentiate between melts with different amounts of inclusions by monitoring the fluctuations in signal for elements of interest. LIBS shows promise as an enabling tool for monitoring metal cleanliness.     

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.     

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.     

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.     

<Emphasis Type="Italic">In situ</Emphasis> Weak Magnetic-Assisted Thermal Stress Field Reduction Effect in Laser Welding

For decades, post-welding magnetic treatment has been used to reduce residual stress of welds by improving the crystal structure of solid-state welds. In this paper, we propose a new magnetic treatment method, which can reduce the time-dependent thermal stress field in situ and reduce the final residual stress of welds by simply exerting an assisted weak magnetic field perpendicular to the welding direction and workpiece during laser welding. A new finite-element model is developed to understand the thermal–mechanical physical process of the magnetic-assisted laser welding. For the widely used 304 austenite stainless steel, we theoretically observed that this method can reduce around 10 pct of the time-dependent thermal stress field, and finally reduce approximately 20 MPa of residual stress near the heat-affected zone with a 415-mT magnetic field for typical welding process parameters. A new mechanism based on magneto-fluid dynamics is proposed to explain the theoretical predications by combining high-speed imaging experiments of the transient laser welding process. The developed method is very simple but surprisingly effective, which opens new avenues for thermal stress reduction in laser welding of metals, particularly heat-sensitive metallic materials.     

Slip-System-Related Dislocation Study from <Emphasis Type="Italic">In-Situ</Emphasis> Neutron Measurements

A combined experimental/computational approach is employed to study slip-system-related dislocation-substructure formation during uniaxial tension of a single-phase, face-centered-cubic (fcc), nickel-based alloy. In-situ neutron-diffraction measurements were conducted to monitor the peak-intensity, peak-position, and peak-broadening evolution during a displacement-controlled, monotonic-tension experiment at room temperature. The measured lattice-strain evolution and the macrostress/macrostrain curves were used to obtain the material parameters required for simulating the texture development by a visco-plastic self-consistent (VPSC) model. The simulated texture compared favorably with experimentally-determined texture results over a range of 0 to 30 pct engineering strain. The grain-orientation-dependent input into the Debye-intensity ring was considered. Grains favorably oriented relative to the two detector banks in the geometry of the neutron experiment were indicated. For the favorably oriented grains, the simulated slip-system activity was used to calculate the slip-system-dependent, dislocation-contrast factor. The combination of the calculated contrast factor with the experimentally-measured peak broadening allows the assessment of the parameters of the dislocation arrangement within the specifically oriented grains, which has a quantitative agreement with the transmission-electron-microscopy results. This article is based on a presentation given in the symposium entitled “Neutron and X-Ray Studies for Probing Materials Behavior,” which occurred during the TMS Spring Meeting in New Orleans, LA, March 9–13, 2008, under the auspices of the National Science Foundation, TMS, the TMS Structural Materials Division, and the TMS Advanced Characterization, Testing, and Simulation Committee.

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<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.     

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.     

<Emphasis Type="Italic">In Situ</Emphasis> Observation of Phase Transformation in Low-Carbon,Boron-Treated Steels

It is known that adding the appropriate amount of boron to steels dramatically increases their hardness and toughness as a result of the transition of the microstructure from grain boundary nucleation to intragranular nucleation. In this study, precipitation and phase transformation kinetics in heat-affected zones of low-carbon, boron-treated steels are observed directly by high-temperature laser scanning confocal microscopy. The effects of boron content and austenite grain size on the phase transformation process are investigated systematically by quantifying the transformation product, the transformation start temperature, the average length of the ferrite plates, and the average number of potent nucleation sites. Finally, detailed methods for controlling and optimizing the microstructure in the heat-affected zones of low-carbon, boron-treated steels are discussed.     

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.     

Functionally Graded Al Alloy Matrix <Emphasis Type="Italic">In-Situ</Emphasis> Composites

In the present work, functionally graded (FG) aluminum alloy matrix in-situ composites (FG-AMCs) with TiB₂ and TiC reinforcements were synthesized using the horizontal centrifugal casting process. A commercial Al-Si alloy (A356) and an Al-Cu alloy were used as matrices in the present study. The material parameters (such as matrix and reinforcement type) and process parameters (such as mold temperature, mold speed, and melt stirring) were found to influence the gradient in the FG-AMCs. Detailed microstructural analysis of the composites in different processing conditions revealed that the gradients in the reinforcement modify the microstructure and hardness of the Al alloy. The segregated in-situ formed TiB₂ and TiC particles change the morphology of Si particles during the solidification of Al-Si alloy. A maximum of 20 vol pct of reinforcement at the surface was achieved by this process in the Al-4Cu-TiB₂ system. The stirring of the melt before pouring causes the reinforcement particles to segregate at the periphery of the casting, while in the absence of such stirring, the particles are segregated at the interior of the casting.     

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.     

<Emphasis Type="Italic">In-Situ</Emphasis> Investigation of Local Boundary Migration During Recrystallization

A combination of electron channeling contrast (ECC) and electron backscatter diffraction pattern (EBSP) techniques has been used to follow in situ the migration during annealing at 323 K (50 °C) of a recrystallizing boundary through the deformed matrix of high-purity aluminum rolled to 86 pct reduction in thickness. The combination of ECC and EBSP techniques allows both detailed measurements of crystallographic orientations to be made, as well as tracking of the boundary migration with good temporal resolution. The measured boundary velocity and the local boundary morphology are analyzed based on calculations of local values for the stored energy of deformation. It is found that the migration of the investigated boundary is very complex with significant spatial and temporal variations in its movement, which cannot directly be explained by the variations in stored energies, but that these variations relate closely to local variations within the deformed microstructure ahead of the boundary, and are found related to the local spatial arrangements and misorientations of the dislocation boundaries. The results of the investigation suggest that local analysis, on the micrometer length scale, is necessary for the further understanding of recrystallization boundary migration mechanisms.     

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.     

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.     

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.     

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.     

<Emphasis Type="Italic">In Situ</Emphasis> Micromechanical Testing for Single Crystal Property Characterization

An in situ method to fully characterize the single crystal properties for polycrystalline alloys is developed using microscale experimental and analysis techniques. The developed method can be applied to metallic engineering alloys that do not exist in single crystal form. Thus using this technique, testing and analysis on polycrystalline samples can yield the single crystal elastic and plastic properties required as input to micro- and mesoscale computational models such as those which rely on crystal plasticity theory. Compression and shear experiments are conducted on single crystal specimens of various crystallographic orientations. Analytical and numerical analysis of the experimental results yields a set of equations that can be solved for the single crystal elastic parameters. This novel methodology is demonstrated to produce reasonable elastic property prediction results for an aerospace aluminum lithium alloy, AA2070. Details regarding the experiments and analysis are provided to facilitate application of the technique to a wide range of polycrystalline material systems and properties.