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At least 343 records · Page 19

Undercooling, Remelting, and Coarsening

Solidification of metal alloys with initial high undercoolings occurs with rapid recalescence due to rapid heat release of the latent heat of fusion. The recalescence temperature is usually higher than the solidus and/or the thermodynamic T sub o temperature of the alloy, depending on the initial undercooling and alloy composition. The rapid heating during recalescence alters the initially solidified structures, in ways that must include partial remelting, ripening, coarsening, and decomposition of the rapidly solidified primary metastable or supersaturated phases. New ways to study the solidification and remelting phenomena associated with the rapid heating during recalescence of undercooled alloys were developed. The phenomena are studied by using: (1) emulsions of iron and nickel base alloys in viscous liquid carriers; and (2) rapid heating of metal samples by electric discharge, using a technique similar to the exploding wire process (EWP), except with less power input. Experimental results are combined with theoretical analyses to better understand the solidification of levitated metal droplets with high undercooling, which relates to the solidification process.

Flemings, M. C.↗

Cooling dynamics of two titanium alloys during laser powder bed fusion probed with in situ X-ray imaging and diffraction

Metal parts produced by laser powder bed fusion (LPBF) additive manufacturing exhibit characteristic microstructures comparable to those observed in laser welding. The primary cause of this characteristic microstructure is rapid, localized heating and cooling cycles, which result in extreme thermal gradients where material solidification is followed by fast cooling in the solid state. The final microstructure and mechanical performance are also influenced by pore formation caused by melt pool fluid dynamics. Here, we use high speed, in situ X-ray diffraction to probe the kinetics of cooling and solid-solid phase transitions after laser melting in two aerospace titanium alloys: Ti-6Al-4V, an α + β alloy; and Ti-5Al-5V-5Mo-3Cr, a near-β alloy. We complement these diffraction studies with in situ X-ray imaging to probe melt pool dynamics and pore formation. From these two complementary probes, we quantify pore formation during melting and the subsequent microstructural evolution as the material rapidly cools after solidification. These results are critical for understanding defect formation and residual stress development in different titanium alloys under LPBF conditions and can help inform process models to predict final part performance.

36 MATERIALS SCIENCE↗

Physics and Chemistry of Te and HgTe-based Ternary Melts

Historically, the theoretical treatment of the liquid phases has always been more difficult and complicated than that for solid and gas phases. A liquid has no lattice structure as crystalline solids and the atoms/molecules in the liquid can migrate through it relatively rapidly. On the other hand, it is also interacting with many other atoms/molecules so that the simplifications of the kinetic theory of gases cannot be employed. For more complicated liquids, such as the liquids of high ionicity and those containing hydrogen bonds and electric dipoles, the understanding is far from complete. At the same time, accurate information on the physics and chemistry of semiconductor melts is needed for the quantitative descriptions of the process of crystal growth from melt. The pre-crystallization phenomena in the liquid phase are critical because the properties of the grown crystals depend on the state and structure of the melt as well as the thermal history of the melt during solidification process. However, the data on the liquid phase, such as thermophysical properties of semiconductor melts are scarce, especially for the HgTe-based II-VI ternary compound semiconductors because of their high vapor pressure and extreme toxicity. Analysis of the thermophysical properties of the melt can provide information about structural transitions of the melt during the solidification process. From a broader point of view, the structure of liquids is much more complicated than the crystalline solids, especially the relaxation behavior through different thermal histories. The theory of hetero-phase fluctuations of liquids is applicable to any many-body systems including condensed-matter physics, field theory, physics of nuclear-matter, cosmology, biology and even sociology. This book summarizes the physics and chemistry from the experimental measurements and theoretical analyses of phase diagram, thermodynamic properties, density, thermal conductivity, viscosity, and electrical conductivity on the binary, pseudo-binary and ternary melts of the most advanced IR-detector material systems of HgCdTe and HgZnTe as well as the analyses of these results. The main objectives of this study are: (1) to provide the phase diagrams and thermodynamic properties of Hg-Cd-Te and Hg-Zn-Te systems through quantitatively fitting the experimental data by assuming an associated solution model for the liquid phase, (2) to experimentally measure the thermophysical properties of the Hg-Cd-Te and Hg-Zn-Te melts, including density, viscosity, electrical conductivity and thermal conductivity as functions of temperature and composition and (3) to enhance the fundamental knowledge of hetero-phase fluctuations and relaxation phenomena in the melts and extend our understanding of the solidification process in order to interpret the experimental results of crystal growth so as to improve the melt growth processes of the compound semiconductor. The physics and chemistry of Te and HgTe-based ternary melts were explored through the studies of the structural transformation during melting, the supercooling during solidification, the relaxation phenomena after rapid cooling of the melts and the metal-semiconductor transition in the melts through the analyses of electrical conductivity and Lorenz number. An in-depth study on the thermophysical properties and their time-dependent structural dynamic processes taking place in the vicinity of the solid-liquid phase transition of the narrow homogeneity range HgTe-based ternary semiconductors as well as the analysis of the homogenization process in the melt will also be presented.

Thermophysical properties↗

Radiative cooling of a solidifying droplet layer including absorption and scattering

A simple solution for the transient cooling of a solidifying layer filled with drops that can emit and scatter radiation is discussed, with application to a liquid drop radiator proposed for the Space Station (Mattick and Hertzberg, 1981). The layer remains at uniform temperature during solidification, and the outer portions rapidly lose heat, producing a variation along the length of the layer in the distribution of liquid concentration across the layer. The analysis is used to obtain both the amount of energy dissipated by the two-phase system at uniform temperature and the velocity distribution necessary to maintain a uniform liquid fraction across the entire layer at all locations along the layer length.

Siegel, Robert↗

In-Operando Study of Shape Retention and Microstructure Development in a Hydrolyzing Sol–Gel Ink during 3D-Printing

3D printing of amorphous and crystalline ceramics is of paramount importance for the fabrication of a wide range of devices with applications across different technology fields. Printed ceramics are remarkably enabled by the sol-gel synthesis method in conjunction with continuous filament direct ink writing. During printing, multiple processes contribute to the evolution of inks including shape retention, chemical conversion, solidification, and microstructure formation. Traditionally, depending on the ink composition and printing environment, several mechanisms have been associated with the shape retention and solidification of 3D printed structures: gelation, rapid solvent evaporation, energy-driven phase transformation, and chemical-driven phase transformation. Understanding the fundamental differences between these mechanisms becomes key since they strongly influence the spatiotemporal evolution of the materials, as the out-of-equilibrium processes inherent to the extrusion, relaxation, and solidification of printed materials have significant effects on the materials properties. Herein, we investigate the shape retention mechanism and the hydrolysis-induced material conversion and microstructure formation during the 3D printing of a water reactive sol-gel ink that transforms into titanium dioxide-based ceramic. This study aims at identifying characteristic mechanisms associated with the material transformation, establishing connections between the microstructure development and the timescales associated with solidification under operando 3D-printing conditions. The investigation of this material's out-of-equilibrium pathways under processing conditions is enabled by time-resolved coherent X-ray scattering, providing simultaneous access to temporospatially resolved microstructural and dynamics information. Furthermore, we explore X-ray speckle tracking as a tool to resolve deformations of the microstructure in a printed filament associated with the deposition of consecutive filaments. Through this work, we aim at providing a fundamental understanding of the relationships behind these transformative processes in 3D printing and their timescales as the basis for achieving unprecedented control over printed materials microstructure.

36 MATERIALS SCIENCE↗

Experimental Investigation of Melting and Solidification Processes of Phase Change Material Heat Exchanger

Rapid development and validation of PCM embedded heat exchangers (PCM-HX) concepts warrant a purpose-built test bench. This paper describes a test facility built for testing various PCM-HX configurations and phase change temperatures that will serve to validate the performance of novel PCM-HX designs. The entire test rig is placed in a temperature-controlled environmental chamber. Inside the PCM-HX containers, up to 48 T-type thermocouples can be spatially distributed on and around the tubes depending on the HX type to capture the phase change process over time. In this paper, a straight tube embedded in PCM having a phase change temperature of 37°C in cylindrical containers is tested. The PCM-HX uses water as an in-tube working fluid. Based on the measured data, the energy balance is analyzed, and its temperature distribution is presented. Here, the maximum deviation between the predicted stored energy and the energy stored calculated from experimental measurements is less than 5%.

36 MATERIALS SCIENCE↗

Primary solidification of ternary compounds in Al-rich Al–Ce–Mn alloys

Primary solidification of ternary compounds Al 20 Mn 2 Ce and Al 10 Mn 2 Ce were analyzed through the coupling of the thermodynamic modeling and classic nucleation theory. Thermodynamic models of Al 20 Mn 2 Ce and Al 10 Mn 2 Ce were developed using the CALPHAD approach based on first-principles calculated enthalpy of formation and experimental data obtained from this work and the literature. The analysis suggested that despite the larger thermodynamic driving force for nucleation of Al 10 Mn 2 Ce, nucleation is preferred for the Al 20 Mn 2 Ce phase in the highly undercooled liquid due to its smaller interfacial energy. Therefore, manufacturing methods with rapid cooling rates will favor primary solidification of Al 20 Mn 2 Ce for Al-rich Al–Ce–Mn alloys.

36 MATERIALS SCIENCE↗

Numerical Modeling of Liquid-Vapor Phase Change

We implemented a two- and three-dimensional finite difference/front tracking technique to solve liquid-vapor phase change problems. The mathematical and the numerical features of the method were explained in great detail in our previous reports, Briefly, we used a single formula representation which incorporated jump conditions into the governing equations. The interfacial terms were distributed as singular terms using delta functions so that the governing equations would be the same as conventional conservation equations away from the interface and in the vicinity of the interface they would provide correct jump conditions. We used a fixed staggered grid to discretize these equations and an unstructured grid to explicitly track the front. While in two dimensions the front was simply a connection of small line segments, in three dimensions it was represented by a connection of small triangular elements. The equations were written in conservative forms and during the course of computations we used regriding to control the size of the elements of the unstructured grid. Moreover, we implemented a coalescence in two dimensions which allowed the merging of different fronts or two segments of the same front when they were sufficiently close. We used our code to study thermocapillary migration of bubbles, burst of bubbles at a free surface, buoyancy-driven interactions of bubbles, evaporation of drops, rapid evaporation of an interface, planar solidification of an undercooled melt, dendritic solidification, and a host of other problems cited in the reference.

Esmaeeli, Asghar↗

Size-dependent microstructures in rapidly solidified uranium-niobium powder particles

The microstructures of rapidly solidified U-6wt%Nb powder particles synthesized by centrifugal atomization were characterized using scanning electron microscopy and transmission electron microscopy. Observed variations in microstructure are related to particle sizes. All of the powder particles exhibited a two-zone microstructure. The formation of this two-zone microstructure is described by a transition from solidification controlled by internal heat flow and high solidification rate during recalescence (micro-segregation-free or partitionless growth) to solidification controlled by external heat flow with slower solidification rates (dendritic growth with solute redistribution). The extent of partitionless solidification increased with decreasing particle size due to larger undercoolings in smaller particles prior to solidification. The metastable phases that formed are related to variations in Nb concentration across the particles. Lastly, the microstructures of the powders were heavily twinned.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

Materials processing in low gravity

Several NASA facilities are available for low gravity experimentation: the Drop Facilities at NASA Marshall and the KC-135 at NASA Johnson. The use of these facilities allows for a rather inexpensive method of determining whether or not particular experiments will be worthwhile candidates for space experiments. Equipment currently available include various furnaces for the Drop Tube, the Drop Tower, and the KC-135. The furnaces for the Drop Tube include both an electron beam and electromagnetic levitation furnace. A vacuum furnace is used for the Drop Tower. Several furnaces used in performing KC-135 solidification experiments include the Automated Directional Solidification Furnace, the Isothermal Casting Furnace, the Rapid Melt/Rapid Quench and the Polymer/Video Furnaces.

Workman, Gary L.↗

Grain Refinement by Authigenic Inoculation Inherited from the Medium-Range Order Structure of Ni-Cr-W Superalloy

The combination of liquidus casting and thermal control solidification furnace was applied to obtain a fine-grained ingot. A rapid quenching method and x-ray diffraction measurement were used to investigate the effect of authigenic inoculation on grain refinement. The structure factor S(Q) of liquid Ni-Cr-W superalloy at 1400 °C (Liquidus temperature) and bright-field image of the microstructures quenched from 1400 °C have been measured by the high-temperature x-ray diffractometer and the transmission electron microscopy (TEM), respectively. The results show that a pre-peak exists on a S(Q) curve at the liquidus temperature. The clusters of atom in rapidly quenched microstructures obtained by isothermal heat treatment at 1400 °C were studied using TEM. Meanwhile, the effect of isothermal different temperatures on rapidly quenched microstructures was studied. The results also show that there are only the globular, equiaxed grains distributed in the solidification structure. These particles are inherited from the medium-range order structure, which is beneficial for grain refinement. The normalized work-hardening rate-strain curve indicates the work-hardening rate of fine grain is higher than that of conventional grain at the same temperature and the same deformation.

36 MATERIALS SCIENCE↗

Analysis of Radial Segregation in Directionally Solidified Hg(0.89)Mn(0.11)Te

Bridgman growth experiments were performed on Hg(0.89)Mn(0.11)Te (MMT) to determine the extent of radial Manganese segregation during directional solidification. MMT crystals were directionally solidified at rates of 0.09 and 0.18 p d s and in axial thermal gradients of 83 and 68"C/cm. Wavelength Dispersive Spectroscopy (WDS) and Fourier Transform Infra-Red (FTIR) analytical techniques were used to determine the radial homogeneity in all boules and the deflection of the solid-liquid interface (SLI) in two boules that were rapidly quenched after 5 to 6 cm of directional solidification. For all growth runs, the measured radial coinpositional variations were on the order of 0.01 molar percent MnTe in the steady state region of growth. Comparison of the measured radial compositional results of the crystals to predicted values in the diffusion-limited regime indicate a strong influence of convection near the solid-liquid interface. This conclusion is supported by the weak influence of the translation rates and axial thermal gradients utilized in this study upon radial compositional homogeneity.

Price, M. W.↗

Numerical investigation of electromagnetic pulse welded interfaces between dissimilar metals

The quality of an electromagnetic pulse weld is strongly affected by a variety of interacting physical phenomena including large plastic deformation, materials mixing, localised heating and rapid cooling, and possible localised melting and interfacial cracks and void. In the present study, a thermomechanically coupled dynamic model has been developed to quantitatively resolve the high speed impact joining interface characteristics as well as the process induced interface temperature evolution, defect formation and possible microstructural composition variations. Reasonably good agreement has been obtained between the predicted results and the experimental measurements in terms of interfacial morphology characteristics. The modelling framework is expected to provide further understanding of the hierarchical interfacial features of the non-equilibrium material joining process and the weld formation mechanisms.

Xu, W.↗

Site specific control of crystallographic grain orientation through electron beam additive manufacturing

Site specific control of the crystallographic orientation of grains within metal components has been unachievable prior to the advent of metals additive manufacturing (AM) technologies. To demonstrate the capability, the growth of highly misoriented micron-scale grains outlining the letters D, O, and E, through the thickness of a 25.4 mm tall bulk block comprised of primarily columnar [001] oriented grains made of the nickel-base superalloy Inconel 718 was promoted. To accomplish this, electron beam scan strategies were developed based on principles of columnar to equiaxed transitions during solidification. Through changes in scan strategy, the electron beam heat source can rapidly change between point and line heat source modes to promote steady state and/or transient thermal gradients and liquid-solid interface velocity. With this approach, an equiaxed-solidification in the regions bounding the letters D, O, and E was achieved. The through thickness existence of the equiaxed grain structure outlining the letters within a highly columnar [001] oriented bulk was confirmed through characterizing the bulk specimen with energy-selective neutron radiography and confirming with a electron backscatter detection (EBSD). Here, this demonstration promotes the ability to build metal components with site-specific control on crystallographic orientation of grains using electron beam melting process.

36 MATERIALS SCIENCE↗

Microstructures and properties of rapidly solidified alloys

The microstructure and properties of rapidly solidified aluminum alloys were researched. The effects of powder and flake chemistry and morphology and alternative consolidation processing parameters are being conducted. Samples of the powders being utilized were obtained for comprehensive metallurgical characterization. Seven aluminum alloys in the form of thin foils were studied by a variety of techniques including optical metallography, scanning electron microscope, and transmission electron microscope. Details of the microstructural characteristics are presented along with a discussion of the solidification process. A better understanding of the microstructure of the rapidly solidified aluminum alloys prepared by a variety of techniques such as roller quenching, the vacuum atomized procedure, ultrasonically atomized in inert atmospheres, and atomized in flue gas was provided.

Shechtman, D.↗

Laser weld-induced formation of amorphous Mn–Si precipitate in 304 stainless steel

In this paper, we report the formation of partially amorphous Mn-Si precipitates due to laser welding of face centered cubic (fcc) 304 stainless steel. Transmission electron microscopy and precession electron diffraction studies in the heat affected zone (HAZ) of the weldment indicate the formation of these precipitates in grain interiors. Precipitates have MnSi stoichiometry and the partially crystalline regions have a lattice constant of 0.45 nm. It is surmised that the rapid cooling rates during the laser weld melt pool solidification process may be sufficient to inhibit the complete crystallization of these precipitates.

304 stainless steel↗

Three-dimensional characterization of modifications in sapphire exposed to laser-induced damage using multimodal spectral microimaging

Sapphire (Al 2 O 3 ) is a commonly used dielectric material with many applications in lasers and optical systems. Owing to its high resistivity to laser induced damage, it is particularly suitable for use in high power laser systems. This work focuses on developing techniques to characterize material modifications in sapphire. These techniques were applied following localized laser induced ablation, commonly referred to as laser-damage, resulting from exposure to single 100-ps and 6-ns pulses. Measurements of fluorescence-based piezospectroscopy and confocal Raman microscopy were performed with spatial resolution on the order of 1 μ m. Raman microscopy reveals that the relaxation of material exposed to the rapid laser heating, elastic and viscoplastic deformation, melting, and solidification leads to the formation of a polycrystalline material phase. In addition, narrowband fluorescence lines, referred to as R 1 and R 2 , exhibit pressure-sensitive changes to their spectral profiles, allowing 3D internal stresses to be recorded with spatial resolution of the order of a few micrometers.

Laser-damage↗