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DOE OSTI2026

Emergence of complex-regular eutectic patterns in Al–Ge: Observations from correlative nano-imaging

Eutectic solidification exemplifies nonequilibrium pattern formation, making it a well-studied moving boundary problem. Yet the mechanisms behind the formation of complex-regular microstructures – particularly in highly anisotropic systems with a significant volume fraction of a faceted phase – remain poorly understood. Our understanding of such systems is made complicated by the nonlinear interface kinetics and unique growth dynamics characteristic of faceted phases. To address these challenges, we investigate a model Al–Ge eutectic system, where the faceted Ge phase constitutes a substantial volume fraction (~0.35) and where the two solid phases arrange into so-called “fishbone” or “feather” complex-regular patterns. Using synchrotron-based x-ray nano-imaging and nanotomography with high spatial resolution (22 nm per pixel), we capture in real-time the evolution of the solid–liquid interfaces and the resulting three-dimensional microstructures in this faceted/non-faceted eutectic system. By integrating these observations with electron backscattered diffraction, we elucidate the crystallographic biases on the solidification process and the mechanisms driving the formation of such complex-regular microstructures. These findings inform a new growth model for irregular eutectics in (near-)symmetrical phase diagrams, offering insight on advanced microstructural design and processing strategies. More broadly, we demonstrate how interfacial curvature is generated in irregular eutectic alloys and how it depends on the volume fraction of the faceted phase.

36 MATERIALS SCIENCE↗

DOE OSTI2024

Systematic discovery of new nano-scale metastable intermetallic eutectic phases in laser rapid solidified Aluminum-Germanium alloy

Laser surface remelting of as-cast Al-Ge eutectic alloy is shown to produce ultrafine lamellar eutectic morphology with interlamellar spacing refined up to ∼60 nm and composed of FCC Al solid solution and unusual Al x Ge y intermetallic phases that do not form during near-equilibrium solidification. The microstructures are characterized and analyzed using a combination of selected area electron diffraction, high-resolution scanning transmission electron microscopy, energy dispersive X-ray spectroscopy to obtain high-resolution elemental maps, and atomistic modeling using density functional theory followed by atomic-scale image simulation. Depending on the local solidification conditions, the crystallography of the Al x Ge y intermetallic phases in the eutectic microstructure is either monoclinic (C 2/c) or monoclinic (P 2 1 ), with high densities of defects in both cases. This is in sharp contrast to the as-cast alloys that showed nominally pure Al and Ge phases with significant solute partitioning and equilibrium FCC and diamond cubic crystal structures, respectively. Corresponding kinetic phase diagrams are proposed to interpret the evolution of nano-lamellar eutectic morphologies with equilibrium Al and metastable Al x Ge y phases, and to explain increased solid solubility in the Al phases manifested by precipitation of ultrafine clusters of Ge. Furthermore, the reasons for the formation of these metastable eutectics under laser rapid solidification are discussed from the perspective of the competitive growth criterion.

Al-Ge eutectic↗

DOE OSTI2025

Tuning Solvation Dynamics of Electrolytes at Their Eutectic Point Through Halide Identity

Deep eutectic solvents (DESs) are regarded as highly promising solvent systems for redox flow batteries. DESs, composed of choline halides (ChX, X = F − , Cl − , Br − , I − ) and ethylene glycol (EG), exhibit distinct physicochemical properties at their eutectic points, including halide-dependent phase behavior, viscosity, polarity, conductivity, and solvation dynamics. In this study, we investigate the effects of the halide identity on the solvation properties of ChX:EG mixtures at varying mol % of ChX salt content. The solvatochromic polarity based on ET(30) measurements indicates higher polarity for larger halides (I − > Br − ) than for smaller halides (Cl − > F − ), which exhibit larger compensating solvation shells. The ionic conductivity follows the trend of the solvent fluidity (the inverse of the viscosity), namely ChCl > ChBr > ChI > ChF, influenced by the ion mobility and solvodynamic radii. Measurements of the liquidus temperatures (T L ) reveal that the system with ChCl exhibits the deepest eutectic point (at ~20 mol % ChCl), while ChBr and ChI have shallower minima at ~10 mol % ChBr and ~3 mol % ChI, respectively. ChF does not display a eutectic transition but instead appears to readily supercool at salt concentrations above 30 mol % ChF. Consistent with the phase transition measurements, femtosecond transient absorption spectroscopy shows that in the ChCl system, the solvation dynamics become faster with an increasing salt concentration up to ~16.67 mol %, after which the dynamics slow down with further increases in the salt content. The ChF-based system exhibits similar behavior, though with slower dynamics. In contrast, the solvation dynamics of the systems containing ChBr and ChI monotonously slow down with an increasing salt concentration, in agreement with the phase transition measurements, which show that the eutectic points occur at low salt concentrations. These measurements suggest that the solvent composition and, in particular, the identity of the halide anion play a significant role in the solvation behavior of these ethylene-glycol-based DESs, offering a foundation for tuning the DES properties for specific applications.

Biochemistry & Molecular Biology↗

NASA NTRS1975

Directionally solidified pseudo-binary eutectics of Ni-Cr-/Hf,Zr/

This report is concerned with the experimental determination of pseudo binary eutectic compositions and the directional solidification of the Ni-Cr-Hf,Zr, and Ni-Cr-Zr eutectic alloys. To determine unknown eutectics, chemical analyses were made of material bled from near eutectic ingots during incipient melting. Nominal compositions in weight per cent of Ni-18.6Cr-24.0Hf, Ni-19.6Cr-12.8Zr-2.8Hf, and Ni-19.2Cr-14.8Zr formed aligned pseudo-binary eutectic structures. The melting points were about 1270 C. The reinforcing intermetallic phases were identified as noncubic (Ni,Cr)7Hf2 and (Ni,Cr)7(Hf,Zr)2, and face centered cubic (Ni,Cr)5Zr. The volume fraction of the reinforcing phases were about 0.5.

Kim, Y. G.↗

NASA NTRS1981

A quantitative study of factors influencing lamellar eutectic morphology during solidification

The factors that influence the shape of the solid-liquid interface of a lamellar binary eutectic alloy are evaluated. Alloys of carbon tetrabromide and hexachloroethane which serve as a transparent analogue of lamellar metallic eutectics are used. The observed interface shapes are analyzed by computer-aided methods. The solid-liquid interfacial free energies of each of the individual phases comprising the eutectic system are measured as a function of composition using a 'grain boundary groove' technique. The solid-liquid interfacial free energy of the two phases are evaluated directly from the eutectic interface. The phase diagram for the system, the heat of fusion as a function of composition, and the density as a function of composition are measured. The shape of the eutectic interface is controlled mainly by the solid-liquid and solid-solid interfacial free energy relationships at the interface and by the temperature gradient present, rather than by interlamellar diffusion in the liquid at the interface, over the range of growth rates studied.

Kaukler, W. F. S.↗

NASA NTRS1985

Study of Eutectic Formation

The objectives of this program are to determine the influence of convection on the microstructure of eutectics and to develop a technique for revealing the longitudinal microstructure of the MnBi-Bi eutectic. Both objectives aim at trying to explain the observed influence of space processing on the microstructure of MnBi-Bi. A computer program was developed and used to determine the concentration field in front of a growing lamellar eutectic. From this the deviation of the interfacial concentration from the eutectic composition was calculated as a function of eutectic composition, freezing rate, convection, and lamellar spacing.

Wilcox, W. R.↗

NASA NTRS1986

Microstructural variations induced by gravity level during directional solidification of near-eutectic iron-carbon type alloys

The effects of gravity on the microstructure of directionally solidified near-eutectic cast irons are studied, using a Bridgman-type automatic directional solidification furnace aboard a NASA KC-135 aircraft which flies parabolic arcs and generates alternating periods of low-g (0.01 to 0.001 g, 30 seconds long) and high-g (1.8 g, 1.5 minutes long). Results show a refinement of the interlamellar spacing of the eutectic during low-g processing of metastable Fe-C eutectic alloys. Low-g processing of stable Fe-C-Si eutectic alloys (lamellar or spheroidal graphic) results in a coarsening of the eutectic grain structure. Secondary dendrite arm spacing of austenite increases in low-g and decreases in high-g. The effectiveness of low-gravity in the removal of buoyancy-driven graphite phase segregation is demonstrated.

Stefanescu, Doru M.↗

NASA NTRS1988

Microstructure Of MnBi/Bi Eutectic Alloy

Collection of three reports describes studies of directional solidification of MnBi/Bi eutectic alloy. Two of the reports, "Influence of Convection on Lamellar Spacing of Eutectics" and "Influence of Convection on Eutectic Microstructure," establish theoretical foundation for remaining document. Reports seek to quantify effect of convection on concentration field of growing lamellar eutectic. Remaining report, "Study of Eutectic Formation," begins by continuing theoretical developments. New technique under development by one of the authors helps to reveal three-dimensional microstructures of alloys.

Wilcox, William R.↗

NASA NTRS1995

Deformation and fracture of a directionally solidified NiAl-28Cr-6Mo eutectic alloy

A directionally solidified alloy based on the NiAl-(Cr, Mo) eutectic was examined by transmission and scanning electron microscopy to characterize the microstructure and room temperature deformation and fracture behavior. The microstructure consisted of a lamellar morphology with a group of zone axes (111) growth direction for both the NiAl and (Cr, Mo) phases. The interphase boundary between the eutectic phases was semicoherent and composed of a well-defined dislocation network. In addition, a fine array of coherent NiAl precipitates was dispersed throughout the (Cr, Mo) phase. The eutectic morphology was stable at 1300 K with only coarsening of the NiAl precipitates occurring after heat treatment for 1.8 ks (500 h). Fracture of the aligned eutectic is characterized primarily by a crack bridging/renucleation mechanism and is controlled by the strength of the semicoherent interface between the two phases. However, contributions to the toughness of the eutectic may arise from plastic deformation of the NiAl phase and the geometry associated with the fracture surface.

Chen, X. F.↗

NASA NTRS2003

A Comparison between Growth Morphology of "Eutectic" Cells/Dendrites and Single-Phase Cells/Dendrites

Directionally solidified (DS) intermetallic and ceramic-based eutectic alloys with an in-situ composite microstructure containing finely distributed, long aspect ratio, fiber, or plate reinforcements are being seriously examined for several advanced aero-propulsion applications. In designing these alloys, additional solutes need to be added to the base eutectic composition in order to improve heir high-temperature strength, and provide for adequate toughness and resistance to environmental degradation. Solute addition, however, promotes instability at the planar liquid-solid interface resulting in the formation of two-phase eutectic "colonies." Because morphology of eutectic colonies is very similar to the single-phase cells and dendrites, the stability analysis of Mullins and Sekerka has been extended to describe their formation. Onset of their formation shows a good agreement with this approach; however, unlike the single-phase cells and dendrites, there is limited examination of their growth speed dependence of spacing, morphology, and spatial distribution. The purpose of this study is to compare the growth speed dependence of the morphology, spacing, and spatial distribution of eutectic cells and dendrites with that for the single-phase cells and dendrites.

Tewari, S. N.↗

DOE OSTI2026

Fuel-Cladding Eutectic Study of Legacy Fast Flux Test Facility (FFTF) MFF HT9/U-10Zr Metallic Fuel

This report presents the first systematic investigation of fuel-cladding eutectic interaction (FCEI) in irradiated HT9/U-10Zr metallic fuel from the Fast Flux Test Facility (FFTF) Materials Fuels Form (MFF) program, using differential scanning calorimetry (DSC) coupled with scanning electron microscopy (SEM) and energy dispersive X-ray spectroscopy (EDS). Two irradiated fuel cross-sections, MNT07H (9.5 at% burnup, x/L = 0.78) and MNT08H (7.0 at% burnup, x/L = 0.93), were subjected to three successive isothermal annealing rounds (R1–R3) at 820°C for 20 minutes each, yielding a cumulative transient duration of one hour. This study directly addresses a recognized gap in the existing FCEI database, which previously lacked irradiated HT9/U-10Zr data at burnup levels above 8 at%. Two principal findings emerge from the study. First, for both samples, FCEI remained spatially confined within the pre-existing fuel-cladding chemical interaction (FCCI) zone boundaries after R3, with no measurable eutectic penetration into unaffected cladding beyond the original FCCI layer. This self-limiting behavior is consistent with historical Fuel Behavior Test Apparatus (FBTA) results and is attributed to the near-eutectic phase composition of the FCCI zone, which rapidly absorb the available eutectic-forming constituents and then stall penetration once the FCCI zone is consumed. A comparison with unirradiated surrogate data further supports this mechanism: whereas a U–34 at.% Fe sample would be expected to show ~176 µm of iron penetration under comparable conditions, the irradiated samples exhibited only ~20 µm, a discrepancy attributed to irradiation-induced interfacial porosity and pre-existing FCCI composition gradients. Second, for MNT08H, FCEI was observed exclusively on the half of the cladding circumference where pre-existing steady-state FCCI was present, with no detectable FCEI on the opposite half. Three hypotheses are proposed to explain this asymmetry: the inhibiting role of a zirconium-rich rind at the fuel-cladding interface; the chemical sequestration of iron by redistributed zirconium within the fuel matrix; and the persistence of fuel-cladding gaps on the FCEI-free half that preclude direct contact. All three hypotheses require further experimental investigation. The results extend the empirical FCEI database into higher-burnup territory and demonstrate the viability of DSC-based testing as a substitute for the no-longer-available FBTA apparatus. Future work will include additional cross-section testing, compilation of the full FCEI dataset, model evaluation, and DSC testing of ternary fuel compositions to broaden the experimental basis for safety assessment of sodium-cooled fast reactor systems.

11 - NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

DOE OSTI2024

From irregular to regular eutectic growth in the Al-Al 3 Ni system: In situ observations during directional solidification

Here we investigate the irregular eutectic growth dynamics of the Al-Al 3 Ni alloy, in which one of the solid phases (Al 3 Ni) grows faceted from the liquid. Leveraging in situ optical microscopy and synchrotron transmission x-ray microscopy, we address the question of the degree of coupling between Al and Al 3 Ni at the growth front and that of the shape of the microstructures left behind in the bulk solid during directional solidification. Real-time optical observations bring evidence for a morphological transition from a eutectic-grain dependent, irregular eutectic growth at low solidification velocity V (typically 1 μm s -1 ), to a weakly anisotropic, regular growth at higher V ( reaching 10 μm s -1 ). Unprecedented x-ray nano-imaging of the solid–liquid interface, and 3D characterization of the growth patterns, were made possible by a new DS setup at Brookhaven National Laboratory’s NSLS-II. At low V, the leading tips of partly faceted Al 3 Ni crystals are observed to grow not far ahead of the Al growth front. Correlating in situ images and postmortem 3D tomographic reconstructions reveals that the presence of faceted and non-faceted regions of Al 3 Ni crystals in the solid is a direct consequence of coupling and decoupling during DS, respectively. Upon increasing V, the lead distance of Al 3 Ni vanishes, and the shape of Al 3 Ni ceases to be governed by faceted growth. These observations cast light onto the basic mechanisms (faceted growth, diffusive coupling, and the dynamics of trijunctions) governing a faceted to rod-like transition upon increasing V in the Al 3 Ni system, with broad implications to a large class of irregular eutectics.

36 MATERIALS SCIENCE↗

DOE OSTI2025

Mechanisms and Energetics of CO 2 Chemisorption in Choline-Based Eutectic Solvents

Understanding the influences of proton sharing and hydrogen transfer in amine and hydroxyl functionalized eutectic solvents is important for tuning CO 2 binding as they relate to the chemisorption capacity and energetics of solvent regeneration in carbon capture. In this study, we examine how the CO 2 binding mechanism and energetics vary in eutectic solvents composed of choline-based hydrogen-bond acceptors (HBAs) with amine and hydroxyl moieties and ethylene glycol (EG), propylene glycol (PG), 1,2-butanediol (BD), and monoethanolamine (MEA)-type hydrogen-bond donors (HBDs), through absorption–desorption experiments and spectral analysis, supported with density functional theory (DFT) calculations. While the HBD-CO 2 complex is the major and the thermodynamically more favored product of absorption in all of the examined eutectic solvents, this complexation is only possible proceeding a proton transfer from HBD to the HBA in diol-based systems (EG, PG, BD). The interplay between HBA-CO 2 and HBD-CO 2 speciation is governed by the HBD concentration, basicity, and steric effects, with increased HBD-CO 2 interactions in the presence of smaller HBDs (size: BD > PG > EG). On the other hand, in MEA-based systems, CO 2 readily binds to the amine followed by a proton transfer from the amine to the HBA as confirmed by DFT calculations. In this way, the MEA-CO 2 chemisorption capacities exceeded that of the conventional amine (up to 0.93 mol of CO 2 per mol of MEA versus 0.5). Furthermore, the increase in CO 2 capacities and enhanced binding in eutectics including MEA or the more basic HBAs also resulted in regeneration temperatures of 70 to 60 °C with calculated reaction energies of −82 to −57 kJ/mol, compared to 50 °C for others with weaker binding, following CO 2 absorption at 25 °C.

absorption↗

DOE OSTI2025

Unravelling Microstructure Selection in an Additively Manufactured Eutectic High‐Entropy Alloy

High-entropy alloys (HEAs) are promising candidates for advanced structural applications due to their excellent mechanical properties. Additive manufacturing (AM), with its rapid solidification conditions, enables the creation of unique nonequilibrium microstructures. To fully leverage the synergy between AM and HEAs, understanding how processing affects structure and properties is essential. Here, how solidification rate influences microstructure evolution and phase transformation pathway in laser additively manufactured AlCrFe2Ni2 eutectic HEAs is investigated. By increasing the laser scan speed and hence the solidification rate, distinct solidification modes evolving from coupled eutectic to anomalous eutectic and eventually to single-phase solidification are revealed. These transitions result in distinct microstructures and a wide range of mechanical properties. Thermodynamic modeling and molecular dynamics simulations reveal that low cooling rates allow for sufficient atomic diffusion and phase separation, facilitating coupled eutectic growth. In contrast, rapid cooling suppresses diffusion and destabilizes the solid–liquid interface, promoting anomalous or single-phase solidification. This integrated experimental and computational approach provides a multiscale understanding of solidification mechanisms in HEAs and underscores how kinetic effects can over-ride thermodynamic predictions under nonequilibrium conditions. Furthermore, these results demonstrate that AM can serve as a powerful tool to design HEAs with tailored microstructures and properties.

36 MATERIALS SCIENCE↗

DOE OSTI2026

Evaluation of high-temperature properties of binary, eutectic Ni-X alloys (X = B, Ca, Ce, La, Y, Zr)

We investigated the high-temperature behavior of binary eutectic nickel-base alloys with low-solubility elements, towards developing alloys with new combinations of structural and functional (e.g. thermal or corrosion) properties. Based on thermodynamic screening, we cast binary near-eutectic Ni-B, Ni-Ca, Ni-Ce, Ni-La, Ni-Y, and Ni-Zr alloys and characterized their microstructure and high-temperature properties. All alloys (except Ni-Ca) contain a fine eutectic microstructure, containing submicron alternating lamellae of γ-Ni and continuous intermetallic phases. The eutectic microstructure did not significantly coarsen at 700°C (except for Ni-B), but measurably coarsened in all alloys at 900°C, most quickly in Ni-B, followed by Ni-Ce, Ni-La, Ni-Y, and Ni-Zr. Coarsening in these alloys occurs by fault migration; diffusion within the intermetallic, and its interfacial energy, likely influence coarsening kinetics. At room-temperature, all alloys possess negligible ductility due to the continuous, brittle intermetallic. At 700 and 900°C, the Ni-Zr alloy showed the best combination of strength and ductility. Oxidation experiments at 900°C on Ni-Zr and Ni-Ce revealed heavy internal oxidation of the continuous intermetallic phase. Overall, the Ni-Zr alloy showed good high-temperature coarsening resistance and strength, though ductility and oxidation resistance require improvement for use in structural applications. Possible routes for improving alloy properties via additive manufacturing are discussed.

Ekaputra, Clement [ORNL] (ORCID:0000000307166479)↗

DOE OSTI2026

Influence of Nd(II) and Nd(III) Ions on the Speciation and Kinetic Dynamics of Radiolytic Transients in Molten LiCl-KCl Eutectic Salt Mixtures

In the pyrochemical reprocessing of used nuclear fuel, understanding the effects of ionizing radiation on the chemical behavior of fission products in molten chloride eutectic salt is crucial. Here, this study investigates the impact of radiation on the chemical and kinetic speciation of Nd ions in molten LiCl-KCl eutectic, which are challenging to separate due to their multivalent oxidation states and comproportionation reactions. Electron pulse radiolysis techniques were used to determine transient absorption spectra, chemical kinetics, and activation parameters for the reaction of Nd ions with the primary products of molten LiCl-KCl eutectic radiolysis: the solvated electron (e S - ) and dichlorine radical anion (Cl 2 •- ). Initially, Nd(III) reacted rapidly with e S - , forming Nd(II) with a second-order rate coefficient of k = (4.54 ± 0.07) × 10 10 M -1 s -1 at 673 K. The resulting Nd(II) ions then reacted slowly with Cl 2 •- , regenerating Nd(III) with an estimated rate of k = (1.72 ± 0.04) × 10 10 M -1 s -1 at 673 K. Additionally, the comproportionation reaction of Nd(III) and Nd(s) to form Nd(II) was monitored chemically and electrochemically. This work suggests that the comproportionation reaction of Nd(III) with Nd(s) to form Nd(II) is unstable in molten LiCl-KCl eutectic.

36 - MATERIALS SCIENCE↗

DOE OSTI2024

Ab-initio molecular dynamics study of eutectic chloride salt: MgCl2–NaCl–KCl

Ionic liquid materials are viable candidates as a heat transfer fluid (HTF) in a wide range of applications, notably within concentrated solar power (CSP) technology and molten salt reactors (MSRs). For next-generation CSP and MSR technologies that strive for higher power generation efficiency, a HTF with wide liquid phase range and energy storage capabilities is crucial. Studies have shown that eutectic chloride salts exhibit thermal stability at high temperatures, high heat storage capacity, and are less expensive than nitrate and carbonate salts. However, the experimental data needed to fully evaluate the potential of eutectic chloride salts as a HTF contender are scarce and entail large uncertainties. Considering the high cost and potential hazards associated with the experimental methods used to determine the properties of ionic liquids, molecular modeling can be used as a viable alternative resource. In this study, the eutectic ternary chloride salt MgCl 2 –NaCl–KCl is modeled using ab-initio molecular dynamics simulations (AIMDs) in the liquid phase. Using the simulated data, the thermophysical and transport properties of eutectic chloride salt can be calculated: density, viscosity, heat capacity, diffusion coefficient, and ionic conductivity. For an initial model validation, experimental pair-distribution function data were obtained from X-ray total scattering techniques and compared to the theoretical pair-distribution function. Additionally, theoretical viscosity values are compared to experimental viscosity values for a similar system. The results provide a starting foundation for a MgCl 2 –NaCl–KCl model that can be extended to predict other fundamental properties.

38 RADIATION CHEMISTRY, RADIOCHEMISTRY, AND NUCLEA↗

NASA NTRS1973

Evaluation of magnesium-aluminum eutectic to improve combustion efficiency in low burning rate propellants

A previous investigation indicated that combustion efficiency of low burning-rate propellants could be improved if the aluminum fuel was replaced by aluminum particles coated with a magnesium-aluminum eutectic alloy (ALCAL). The purpose of the present investigation was to evaluate the possibility of improving the combustion efficiency of these propellants by admixing the eutectic with the aluminum rather than coating the aluminum. Tests of three propellants similar in every respect except for the metal fuel were conducted in test motors with 4.54 kg (10 lbm) of propellant. The first propellant used aluminum fuel; the second contained aluminum admixed with magnesium-aluminum eutectic; the third used ALCAL. The test results show the the admixed fuel gave better low burning-rate combustion efficiency than the other two. The test results also showed that the ALCAL was deficient in that much, if not all, of the coating material could be found as the fine particles in a bimodal mix of aluminum and eutectic. The combustion efficiency of low burning-rate aluminized propellants can be significantly improved by mixing a small amount of magnesium-aluminum alloy with the aluminum fuel.

Northam, B. G.↗