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NASA NTRS2016

Macrosegregation and Grain Formation Caused by Convection Associated with Directional Solidification Through Cross-Section Increase

Cylindrical Al-7 wt% Silicon, Al-19 wt% Copper and Lead-6 wt% Antimony alloy samples were directionally solidified (DS) with liquid above, solid below, and gravity pointing down, in graphite crucibles having an abrupt cross-sectional increase. These alloys have similar solidification shrinkage but are expected to have different degrees of thermosolutal convection during solidification. Microstructures in the DS samples in the vicinity of the section change have been studied in order to examine the effect of convection associated with the combined influence of thermosolutal effects and solidification shrinkage. Extensive radial and axial macrosegregation associated with cross-section change is observed. It also appears that steepling and local primary alpha-phase remelting resulting from convection are responsible for stray grain formation at the reentrant corners. Preliminary results from a numerical model, which includes solidification shrinkage and thermosolutal convection in the mushy zone, indicate that these regions are prone to solutal remelting of dendrites.

Ghods, Masoud↗

DOE OSTI2025

Rapid Solidification Effects in Additively Manufactured Si and SiGe Compositions

SiGe alloys have a proven track record as robust high-temperature thermoelectric materials, powering NASA missions like SNAP-10A, LES-9, and Voyager 1 and 2. Enhancing thermoelectric efficiency hinges on minimizing thermal conductivity while preserving electrical conductivity. Rapid solidification via LPBF can generate microstructural features such as subgrain cellular boundaries and twinning, which may help reduce thermal conductivity while preserving semiconducting behavior. Here, this study investigates the potential of laser powder bed fusion (LPBF) additive manufacturing to fabricate nanostructured Si and SiGe thermoelectric materials. High cooling rates (10 5 to 10 7 K/s) rates inherent to the LPBF process are conducive to forming such nanostructures. Moreover, this fabrication technique could also be suitable for fabricating complex geometries needed to achieve improved device level performance. Process mapping of commercial Si powder with irregular morphology was first performed to understand the LPBF processing behavior of this semiconductor material. Subsequent studies included in-house synthesized B-doped (p-type) Si7 8 Ge 22 spherical powder that was produced via ultrasonic atomization. Scan strategies involved multiple laser exposures to mitigate solidification cracking: a high density of >98% was achieved, but solidification cracking could not be fully eliminated. Subsequently, a high electrical resistivity (i.e., low conductivity) was observed, but the measured Seebeck coefficient, ∼230 μV/K @ 500 °C, proved that good semiconductor material was being fabricated. A subgrain cellular structure (5–10 μm) was observed as defined by Ge segregation to the intercellular boundaries. The remelting strategies helped lower the cooling rates in processing SiGe, but this still resulted in high residual stresses, which induced a remarkably high density of twins (78–95%) to accommodate the deformation. This unique grain structure offers an avenue for phonon scattering and potential improvements in thermoelectric performance.

figure of merit↗

DOE OSTI2024

Solidification of SRPPF Aqueous Recovery Liquid: Process Disruptions

Savannah River National Laboratory has identified a magnesium oxysulfate grout formulation to solidify the liquid effluent from the Savannah River Plutonium Processing Facility (SRPPF) Aqueous Recovery System (ARS). The formulation uses reactive, light burnt MgO, anhydrous MgSO 4 , and dead burnt MgO and provides good mixability, similar density to the original Portland Cement-based mix, and a leachate pH of 9.39, within the assumed Waste Isolation Pilot Plant (WIPP) brine pH range. The formulation will solidify the effluent using a solid first, lost paddle design, within a 55-gallon drum. A series of seven different process disruptions, or irregular processing during the expected ARS liquid effluent solidification process, were completed to assess the severity of the impact of the process disruption and how the formulation behaves under these conditions. Seven process disruptions were investigated including: No Mixing, Partial Mixing, Compacted/Stratified, Sealed, Overfilled, Underfilled, and Undermixed. The impact on solidification, leachate pH, Er (a Pu/Am surrogate) distribution, and density of the resulting grout were established. Overall, four of the process disruptions, No Mixing, Partial Mixing, Compacted/Stratified, and Overfilled, resulted in basic, unabsorbed liquid that would require additional solidification to be acceptable for WIPP. Most solids generated in this testing met the expected WIPP leachate pH requirements. Solids from the Compacted/Stratified process disruption test, however, produced a leachate pH slightly above the assumed range in the WIPP performance assessment. The distribution of Er for most of the tests was relatively consistent. The No Mixing process disruption test, however, resulted in non-homogeneous Er distribution, indicating that radioactive material would not be evenly distributed throughout this solid’s matrix. The Overfilled test is the only mix with a density slightly below the acceptable value. The Sealed and Overmixed tests produced a solid closest to the standard mix with no unabsorbed liquid, expected leachate pH levels, consistent Er concentrations, and expected density, indicating these process disruptions do not have a negative impact on the final grout form. Based on the other process disruptions, it is critical to have premixed dry materials and a well-defined mixing process to produce a solid, homogeneous magnesium oxysulfate cement, with no unabsorbed liquid. These process disruption tests show that the lack of adequate mixing is fundamental to creating an improperly solidified material that may require remediation.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

NASA NTRS2023

Solidification Furnace for In Situ Observation of Bulk Transparent Systems and Image Analysis Methods

This paper aims to describe the experimental framework of the Directional Solidification Insert (DSI), installed onboard the International Space Station (ISS), dedicated to the in situ and real-time characterization of the dynamic selection of the solid-liquid interface morphology in bulk samples of transparent materials under diffusive growth conditions. The in situ observation of the solid-liquid interface is an invaluable tool for gaining knowledge on the time-evolution of the interface pattern because the initial morphological instability evolves nonlinearly and undergoes a reorganization process. The result of each experiment, characterized by the sample concentration, a thermal gradient and a pulling rate, is a large number of images. Interpretation of these images necessitates a robust identification of each cell/dendrite position and size during the entire solidification. Several image analysis methods have been developed to achieve this goal reliably despite varying contrast and noise levels, and are described in details. Typical solidification experiments are presented and the dynamics of the pattern formation are analyzed to illustrate the application of the image analysis methods.

Programming languages↗

NASA NTRS2025

Simulations of Large-Scale Zero Boiloff, Densification, and Solidification of Hydrogen

An Integrated Refrigeration and Storage (IRAS) experimental system called the Ground Operations and Demonstration Unit for Liquid Hydrogen (GODU-LH2) demonstrated the ability store cryogens in a zero boiloff (ZBO) process, and to densify liquid hydrogen by reducing the temperature and pressure down to the triple point resulting in solidification. The incompressible Navier-Stokes was utilized to simulate ZBO, densification, and solidification of liquid hydrogen (LH2) in the IRAS tank. The simulations were performed using a commercially available Computational Fluid Dynamics (CFD) pressure-based mass and momentum flow model and an enthalpy-porosity energy model. Results demonstrated the simulation’s ability to predict time-dependent flow and temperature fields and solid-liquid phase locations for hydrogen during ZBO, densification, and solidification. The simulations showed good agreement with experimental data, with errors within acceptable ranges for temperature and pressure predictions, provided detailed insights into natural convection and solid-liquid phase change dynamics. These findings are critical for the design of future cryogenic fluid management systems.

Computational Fluid Dynamics↗

DOE OSTI2025

Laser‐Powder Melt Pool Solidification Dynamics and Microstructural Engineering of Ti‐5553 Microlattices

The fine geometric and topological control afforded by additive manufacturing technologies has enabled the manufacture of architected materials across length scales, and enabling tunable mechanical performance as a function of local and global design. Progress has been made to tune the mechanical response of architected materials through geometry, but understanding how the geometry and processing conditions will inform the microstructure remains a challenge due to the rapid solidification in laser powder bed fusion. This study uses in situ X-ray imaging and electron backscatter diffraction microscopy to demonstrate that the melt pool size, microstructure morphology, and elastic strain distribution is influenced by a combination of lattice geometry and laser processing conditions. These results indicate that within larger melt pools the local thermal gradients are sufficient to enable a columnar-to-equiaxed transition across the melt pool. Furthermore, the solidification mechanisms producing these microstructures are examined across the first 5 ms of melting and solidification, described via in situ high-speed X-ray imaging and mirrored via multiphysics simulation.

additive manufacturing↗

DOE OSTI2026

Enhancing microsegregation during rapid directional solidification through ternary microalloying

The nano-cellular dendritic microstructure formed during rapid directional solidification in powder bed fusion additive manufacturing creates unique properties such as simultaneous improvement in strength and ductility. However, process control of microsegregation features remains challenging due to low sensitivity of critical solidification mechanisms to process parameters. This study leverages microalloying to achieve large changes in dendrite composition, microstructure, and interdendritic zone width during laser powder bed fusion without modifying process parameters. CALPHAD simulations predict that the addition of Zr significantly steepens the solidus line of the dilute Cu-Cr alloy system, leading to enhanced Cr rejection into the melt and greater than 95% reduction in solubility of Cr in the solidified Cu matrix. Experimental validation using time-of-flight secondary ion mass spectrometry and Kelvin probe force microscopy reveals that the ternary alloy containing 0.01 wt% Zr exhibited wider interdendritic regions compared to the binary, a significantly higher number of Cr-rich particles within interdendritic regions, near-complete ejection of oxygen impurities from the matrix, and greater nanoscale work function contrast. These features indicate more aggressive Cr segregation in the presence of Zr and a purer Cu matrix and provide a potentially robust method for engineering the nano-cellular dendritic solidification microstructure.

CALPHAD↗

DOE OSTI2026

Analytical model for balling defects in laser melting using rivulet theory and solidification

In laser welding and additive manufacturing communities, the balling (humping) defect is primarily attributed to the Plateau–Rayleigh fluid instability (PRI) with a few authors suggesting fluid jetting and volume conservation as alternative mechanisms. As analytical descriptions of these mechanisms are unavailable, combining them into a single formalism is unfeasible. We present a new model of PRI with higher accuracy, accounting for competition with solidification, to compare the expected behavior with known experimental trends when fluid jetting is neglected. We adapt a rivulet instability model from fluid physics to account for the stabilizing effects of the substrate, which the traditional cylindrical-jet geometry does not account for and estimate the instability growth rate. Our model yields a continuous transition from non-balling to balling hitherto lacking in current literature and predicts instability growth at higher wavelengths with strong sensitivity to the solidification front curvature. While the fluid surface is most unstable for shallow melt pools, the absolute magnitude of balling relevant to printing defects scales with melt pool depth and has a maximum for a given melt pool geometry. Synchrotron-based x-ray radiography of thin samples indicates that PRI growth rates and solidification can be comparable in magnitude and thus compete, as we find in this work. We predict that deviations between model predictions and our experimental results demonstrate the importance of fluid flows and heat transport in the balling process. Our experiments further demonstrate at least one mechanism by which the melt pool length and the balling wavelength are not equivalent, as commonly claimed.

Taylor, Z. [Stanford Univ., CA (United States); SL↗

NASA NTRS1972

Thermal modeling of phase change solidification in thermal control devices including natural convection effects

Natural convection effects in phase change thermal control devices were studied. A mathematical model was developed to evaluate natural convection effects in a phase change test cell undergoing solidification. Although natural convection effects are minimized in flight spacecraft, all phase change devices are ground tested. The mathematical approach to the problem was to first develop a transient two-dimensional conduction heat transfer model for the solidification of a normal paraffin of finite geometry. Next, a transient two-dimensional model was developed for the solidification of the same paraffin by a combined conduction-natural-convection heat transfer model. Throughout the study, n-hexadecane (n-C16H34) was used as the phase-change material in both the theoretical and the experimental work. The models were based on the transient two-dimensional finite difference solutions of the energy, continuity, and momentum equations.

Ukanwa, A. O.↗

NASA NTRS1974

Eutectic solidification

The possibilities of using the low-gravity space environment for the processing of directionally solidified materials in order to remove the limitations imposed by the L-g earth environment have led to a careful evaluation of the directional solidification process and the results commonly obtained. Defects in the regularity of the microstructure have been identified as one of the most important areas where present processing technology needs to be improved. One-g environment material processing must also be carefully characterized before it can be determined if zero-g processing will produce significant benefits in eutectic and off-eutectic solidification. It is suggested that a combination of experimental and analytical thermal studies will be required to optimize the solidification process in order to minimize the structural defects which occur due to present processing techniques.

Douglas, F. C.↗

NASA NTRS1973

Investigation of solidification in zero-gravity environment: M553 sphere forming experiment. Nickel-silver alloy evaluation

The processing of nickel-silver alloy specimens in space is discussed. Four specimens were melted only partially, while a fifth was melted completely and assumed after solidification a perfectly spherical shape. Growth of the solid was epitaxial on the unmelted material or on the retaining sting and occurred without undercooling. Solidification was dendritic in all cases with nonequilibrium silver particles forming monotectically between dendrite arms. Substantial loss of silver by evaporation took place. Evaporation of the silver within internal gas cavities on the melt was followed by surface condensation after completion of solidification and cooling, leading to a silver-rich lining in these cavities. The material gave no microstructural evidence of any reduction in liquid convection.

Kattamis, T. Z.↗

NASA NTRS1975

External field effects on diffusion and solidification derived from the free-volume model

Expressions for the diffusion coefficient and the solidification rate from the free-volume model of liquids developed by Turnbull and Cohen have been used to estimate the effects which microgravity and magnetic fields will have on these quantities. The mathematical formalism describing changes of the diffusion coefficient and the solidification rate is the same for both the microgravity and magnetic field cases, but the difference between the magnitudes of the two effects is quite large. The change in the two parameters is found to be less than .0001% for the microgravity case and on the order of 0.1 to 1.1% for the magnetic field case for four representative materials. The diffusion coefficient and the solidification rate are found to increase under the influence of an applied magnetic field, and this is in agreement with experimental observations.

Miller, R. I.↗

NASA NTRS1975

Research on metal solidification in zero-g state

The containerless solidification of several pure metals and metallic alloys was studied in a low gravity environment. The tests were performed in the MSFC 4.2 s drop tower using a rapid wire melting apparatus designed and built for this purpose. Pure iron and nickel, and alloys of iron-nickel, iron-carbon, nickel-aluminum and tungsten-rhenium were all melted and solidified at a gravity level of approximately 100.000/-4 g. Interpretation of the results has led to an appreciation of the factors controlling the successful execution of this drop test experiment and to a delineation of the limits of applicability of the apparatus. Preliminary metallurgical evaluations are presented of the overall shapes, lattice parameters, surface microstructure,, cross-sectional microstructures, solidification and transformation sequences, evaporative segregation, and localized solute redistribution observed in the low-gravity specimens. The effects of low gravity on metallic solidification are discussed with particular emphasis on observations of spontaneous undercooling and evaporative segregation in uncontained melts.

Papazian, J. M.↗

NASA NTRS1975

The solidification under zero gravity conditions of binary alloys exhibiting solid state immiscibility

The solidification behavior of gold-silicon alloys containing up to 25 at. % silicon was studied, and a mathematical model of gravity segregation during solidification was developed. A background of knowledge is provided which can be used in the design of zero gravity solidification experiments to be carried out in the 300-ft drop tower, in Aerobee rockets and in future space missions. Such experiments are needed to develop the basic scientific knowledge required for the design of economically viable space manufacturing processes. Some preliminary zero gravity experiments were carried out on a gold-25 at. % silicon alloy using the drop tower facility.

Johnson, A. A.↗

NASA NTRS1978

Analysis of solidification interface shape during continuous casting of a slab

An analysis was made of the two-dimensional interface shape of a slab ingot being cast continuously by withdrawing it from a mold. The sides of the ingot are being cooled and the upper boundary of the ingot is in contact with a pool of molten metal. The solidification interface shape was determined from the analysis of the heat flow, utilizing the condition that the solidification interface is at constant temperature and must be normal to the lines of heat flow carrying away latent heat of fusion from the interface. The analysis includes the effect of interface curvature which, for a constant rate of withdrawing the cast ingot from the mold, causes the solidification to be nonuniform along the interface. The analysis was carried out by a conformal mapping procedure.

Siegel, R.↗

NASA NTRS1980

Analysis and calculation of macrosegregation in a casting ingot. MPS solidification model. Volume 3: Operating manual

The operation of solidification model 1 is described. Model 1 calculates the macrosegregation in a rectangular ingot of a binary alloy as a result of horizontal axisymmetric bidirectional solidification. The calculation is restricted to steady-state solidification; there is no variation in final local average composition in the direction of isotherm movement. The physics of the model are given.

Maples, A. L.↗

NASA NTRS1981

Laser shadowgraph and schlieren studies of gravity-related flow during solidification

Shadowgraph and schlieren techniques were used to observe gravity-related flow arising during solidification. The purpose of these studies was to elucidate the results of previous low gravity solidification experiments. Shadowgraph and schlieren techniques were selected as most suitable for operation in the anticipated experimental environment. A laser shadowgraph/schlieren system was built and flown on KC-135 low gravity simulation flights. A solution of ammonium chloride and water was cooled during the experiment, causing solidification. Growth plumes in the solution were observed and photographed using shadowgraph and schlieren techniques. Results are presented and related to previous work.

Owen, R. B.↗

NASA NTRS1982

Rapid solidification of metallic particulates

In order to maximize the heat transfer coefficient the most important variable in rapid solidification is the powder particle size. The finer the particle size, the higher the solidification rate. Efforts to decrease the particle size diameter offer the greatest payoff in attained quench rate. The velocity of the liquid droplet in the atmosphere is the second most important variable. Unfortunately the choices of gas atmospheres are sharply limited both because of conductivity and cost. Nitrogen and argon stand out as the preferred gases, nitrogen where reactions are unimportant and argon where reaction with nitrogen may be important. In gas atomization, helium offers up to an order of magnitude increase in solidification rate over argon and nitrogen. By contrast, atomization in vacuum drops the quench rate several orders of magnitude.

Grant, N. J.↗