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16 records
All sourcesNASA NTRSDOE OSTI
DOE OSTI2026

Beyond the eutectic paradigm: nanolamellar patterns in a rapidly solidified peritectic alloy

Peritectic transformations are central to many structural alloys, yet pattern formation remains poorly understood due to complex growth dynamics and limited three-dimensional data. Here, we report an unusual two-phase microstructure in a Zn–Ag peritectic alloy subjected to rapid solidification by laser surface remelting. Synchrotron X-ray nanotomography reveals a lamellar structure of primary 𝜀-AgZn 3 and peritectic Zn with ∼700 nm spacing. Although resembling a eutectic morphology, this pattern forms without a eutectic reaction through non-steady coupled growth from the liquid. SEM and TEM-EDS confirm interface shapes and phase compositions. These findings expand the design space of peritectics for refined microstructural control.

36 MATERIALS SCIENCE↗
NASA NTRS1992

Microstructural development during directional solidification of peritectic alloys

Despite the widespread commercial use of peritectic alloys (e.g., steels, brass, bronze, intermetallic compounds, Co based superalloys and A3B type superconductors), the characterization of the microstructural development during directional solidification of peritectics has historically lagged behind similar efforts directed towards other types of binary invariant reactions such as eutectic or monotectic. A wide variety of possible microstructures has been shown to form in peritectics depending upon the imposed temperature gradient, G, the solidification velocity, V, as well as the presence or absence of convection in the melt. This has important technological implications since many commercially important alloys exhibit peritectics and processing methods such as casting and welding often involve widely changing conditions. It has been the aim of this project to examine, in a systematic fashion, both experimentally and theoretically, the influence of gravitationally driven convection on segregation and microstructural development during solidification in peritectic systems under terrestrial conditions. The scientific results of the project will be used to establish ground based data in support of a meaningful microgravity flight experiment.

Lograsso, Thomas A.↗
NASA NTRS1987

Growth of Metastable Peritectic Alloys

Effects of directional solidification on microstructural, compositional, and magnetic properties studied. Two reports describe experiments to determine effects of directional solidification on peritectic alloys. Of particular interest were effects of gravitationally driven convection.

Larson, David J., Jr.↗
NASA NTRS1996

Microstructural Development during Directional Solidification of Peritectic Alloys

A thorough understanding of the microstructures produced through solidification in peritectic systems has yet to be achieved, even though a large number of industrially and scientifically significant materials are in this class. One type of microstructure frequently observed during directional solidification consists of alternating layers of primary solid and peritectic solid oriented perpendicular to the growth direction. This layer formation is usually reported for alloy compositions within the two-phase region of the peritectic isotherm and for temperature gradient and growth rate conditions that result in a planar solid-liquid interface. Layered growth in peritectic alloys has not previously been characterized on a quantitative basis, nor has a mechanism for its formation been verified. The mechanisms that have been proposed for layer formation can be categorized as either extrinsic or intrinsic to the alloy system. The extrinsic mechanisms rely on externally induced perturbations to the system for layer formation, such as temperature oscillations, growth velocity variations, or vibrations. The intrinsic mechanisms approach layer formation as an alternative type of two phase growth that is inherent for certain peritectic systems and solidification conditions. Convective mixing of the liquid is an additional variable which can strongly influence the development and appearance of layers due to the requisite slow growth rate. The first quantitative description of layer formation is a model recently developed by Trivedi based on the intrinsic mechanism of cyclic accumulation and depiction of solute in the liquid ahead of the interface, linked to repeated nucleation events in the absence of convection. The objective of this research is to characterize the layered microstructures developed during ground-based experiments in which external influences have been minimized as much as possible and to compare these results to the current the model. Also, the differences between intrinsic and externally influenced layer formation were explored. The choice of alloy system is critical to a study of the formation of layered microstructures. The ideal system would have a well-characterized phase diagram, equal densities of both elements in the liquid state to minimize compositionally-driven convective flows, a low peritectic temperature to simplify directional solidification and the achievement of a high temperature gradient in the liquid, a broad composition range for the peritectic reaction, and a reasonable hardness at room temperature to facilitate handling and metallographic preparation. The In-Sn system was selected initially due to a very low peritectic temperature and the nearly equal densities of In and Sn in the liquid state. Since the In-rich peritectic reaction had apparently not been utilized previously for solidification research, experiments were conducted to check the phase diagram in the region of interest. The alloys in this system proved to be difficult to handle and prepare in bulk form with the equipment available, so experiments were initiated with the Sn-Cd system. Layered microstructures had been observed previously in Sn-Cd.

Lograsso, Thomas A.↗
NASA NTRS1984

The growth of metastable peritectic compounds

The influence of gravitationally driven convection on the directional solidification of peritectic alloys was evaluated. The Pb-Bi peritectic was studied as a model solidification system. Analyses of directionally solidified Pb-Bi peritectic samples indicate that appreciable macrosegregation occurs due to thermosolutal convection and/or Soret diffusion. The macrosegregation results in sequantial change of phase and morphology as solidification progresses down the length of the sample. Banding was eliminated when furnace conditions were selected which resulted in a planar solidification interface. The directional solidification that occurs in the vicinity of the Pb-Bi peritectic isothermal was found to be isocompositional and to consist solely of the equilibrium terminal solid solution and peritectic phases on an extremely fine scale. Evidence was found to support the peritectic supercooling mechanism, but not the proposed peritectic superheat mechanism.

Larson, D. J., Jr.↗
NASA NTRS1981

The growth of metastable peritectic compounds

The influence of gravitationally driven thermosolutal convection on the directional solidification of peritectic alloys is considered as well as the relationships between the solidification processing conditions, and the microstructure, chemistry, and magnetic properties of such alloys. Analysis of directionally solidified Pb-Bi peritectic samples indicates that appreciable macrosegregation occurs due to thermosolutal convection and/or Soret diffusion. A peritectic solidification model which accounts for partial mixing in the liquid ahead of the planar solidification interface and describes macrosegregation has been developed. Two-phase dendritic and banded microstructures were grown in the Pb-Bi peritectic system, refined two-phase microstructures have were observed, and candidate formation mechanisms proposed. Material handling, containment, casting, microstructural and magnetic characterization techniques were developed for the Sm-Co system. Alloys produced with these procedures are homogeneous.

Larson, D. J., Jr.↗
NASA NTRS1999

Role of Dynamic Nucleation at Moving Boundaries in Phase and Microstructure Selection

Solidification microstructures that form under steady-state growth conditions (cells, dendrites, regular eutectics, etc.) are reasonably well understood in comparison to other, more complex microstructures, which form under intrinsically non-steady-state growth conditions due to the competition between the nucleation and growth of several phases. Some important practical examples in this latter class include microstructures forming in peritectic systems in highly undercooled droplets, and in strip cast stainless steels. Prediction of phase and microstructure selection in these systems has been traditionally based on (1) heterogeneous nucleation on a static interface, and (2) comparing the relative growth rate of different phase/microstructures under steady-state growth conditions. The formation of new phases, however, occurs via nucleation on, or ahead of, a moving boundary. In addition, the actual selection process is controlled by a complex interaction between the nucleation process and the growth competition between the nuclei and the pre-existing phase under non-steady-state conditions. As a result, it is often difficult to predict which microstructure will form and which phases will be selected under prescribed processing conditions. This research addresses this critical role of nucleation at moving boundaries in the selection of phases and solidification microstructures through quantitative experiments and numerical modeling in peritectic systems. In order to create a well characterized system in which to study this problem, we focus on the directional solidification of hypo- and hyper-peritectic alloys in the two-phase region, imposing a large enough ratio of temperature gradient/growth rate (G/V(sub p)) to suppress the morphological instability of both the parent (alpha) and peritectic (Beta) phases, i.e. each phase alone would grow as a planar front. Our combined experimental and theoretical results show that, already in this simplified case, the growth competition of these two phases leads to a rich variety of microstructures that depend sensitively upon the relative importance of nucleation, diffusion, and convection.

Karma, Alain↗
NASA NTRS1984

The growth of metastable peritectic compounds

The effects of directional solidification processing on the microstructural, compositional, and magnetic properties of high-melting-temperature, commercially important alloys which form from the liquid state via peritectic or eutectic type reactions were determined. Emphasis was placed on ferromagnetic compounds of the commercially important Co-Sm and Al-Mn systems. The primary dendrite spacing for eutectic Sm2Co17/Co scaled with negative square root of V and varied from approximately 50 microns for V 20 cm/h to hundreds of microns for V 10 cm/h. Since the crystal growth mechanism was dendritic rather than cooperative, the assoicated permanent magnet properties were rather poor. Magnetization as a function of sample orientation indicates that the easy axis of magnetization was primarily along the direction of solidification for the eutectic Sm2Co17/Co and peritectic SmCo5/Sm2Co17 compositions. For the Al-Mn case, magnetization and microstructural characterization suggest isotropic, polycrystalling growth for all solidification velocities studied.

Pirich, R. G.↗
NASA NTRS1984

Containerless drop tube solidification and grain refinement of NiAl3

The possibility of undercooling Ni-Al alloys below the liquidus in order to produce a single phase peritectic structure by containerless drop tube solidification was studied. Containerless process is a technique for both high purity contamination free studies as well as for investigating the undercooling and rapid solidification of alloys by suppression of heterogeneous nucleation on container walls. In order to achieve large undercoolings one must avoid heterogeneous nucleation of crystallization. It was shown that the Marshall Space Flight Center drop tubes ae unique facilities for containerless solidification experiments and large undercoolings are possible with some alloys. The original goal of undercooling the liquid metal well below the liquidus to the peritectic temperature during containerless free to form primarily NiAl3 was achieved. The microstructures were interesting from another point of view. The microstructure from small diameter samples is greatly refined. Small dendrite arm spacings such as these could greatly facilitate the annealing and solid state transformation of the alloy to nearly 10% NiAl3 by reducing the distance over which diffusion needs to occur. This could minimize annealing time and might make it economically feasible to produce NiAl3 alloy.

Ethridge, E. C.↗
NASA NTRS2012

Microstructure Formations in the Two-Phase Region of the Binary Peritectic Organic System TRIS-NPG

In order to prepare for an onboard experiment on the International Space Station (ISS), systematic directional solidification experiments with transparent hypoperitectic alloys were carried out at different solidification rates around the critical velocity for morphological stability of both solid phases. The investigations were done in the peritectic region of the binary transparent organic TRIS-NPG system where the formation of layered structures is expected to occur. The transparent appearance of the liquid and solid phase enables real time observations of the dynamic of pattern formation during solidification. The investigations show that frequently occurring nucleation events govern the peritectic solidification morphology which occurs at the limit of morphological stability. As a consequence, banded structures lead to coupled growth even if the lateral growth is much faster compared to the growth in pulling direction.

Mogeritsch, Johann↗
DOE OSTI2021

Thermodynamic properties of Gd-Bi alloys determined by emf measurements in LiCl-KCl-GdCl 3 electrolyte

Thermodynamic properties of binary Gd-Bi alloys (mole fraction, x Gd = 0.02–0.35) were determined using electromotive force (emf) measurements in molten LiCl-KCl-GdCl 3 electrolyte in complement with structural, microstructural, and thermal characterization. X-ray diffractometry (XRD) and scanning electron microscopy (SEM) identified the phase constituents of Gd-Bi alloys (x Gd = 0.02–0.35) as Bi matrix and GdBi compound. According to differential scanning calorimetry (DSC) measurements up to 1250 K, a eutectic transition [L = Bi + GdBi] was observed at 543 K but the reported peritectic transition [L + GdBi = GdBi 2 ] was not detected, suggesting the absence of the GdBi 2 compound. Based on structural, microstructural, and thermal characterization of Gd-Bi alloys (x Gd = 0.02–0.35), the GdBi 2 compound was not detected, and its thermodynamic stability is questionable. The emf of Gd-Bi alloy (x Gd = 0.16) at 700–1048 K relative to Gd(s) was measured by electrodepositing pure Gd metal at 25 K increments. Further, the emf values of Gd-Bi alloys were determined via coulometric titration of Gd into liquid Bi using a two-phase [L + GdBi] alloy as a reference electrode at 773–973 K. The solubility of Gd in liquid Bi was also estimated to be 0.50 mol% (773 K), 0.99 mol% (873 K), and 2.21 mol% (973 K) and the excess partial molar Gibbs energy (Δ$\mathrm{\bar{G}^{ex}_{Gd}}$) of liquid Gd-Bi alloys was as low as 65 kJ mol –1 , indicating strong chemical interactions between Gd and Bi.

36 MATERIALS SCIENCE↗
NASA NTRS1993

Flow of ices in the Ammonia-Water System

We have fabricated in the laboratory and subsequently deformed crystalline hydrates and partial melts of the water-rich end of the NH3-H2O system, with the aim of improving our understanding of physical processes occurring in icy moons of the outer solar system. Deformation experiments were carried out at constant strain rate. The range of experimental variables are given. Phase relationships in the NH3-H2O system indicate that water ice and ammonia dihydrate, NH3-2H2O, are the stable phases under our experiment conditions. X-ray diffraction of our samples usually revealed these as the dominant phases, but we have also observed an amorphous phase (in unpressurized samples only) and occasionally significant ammonia monohydrate, NH3-H2O. The onset of partial melting at the peritectic temperature at about 176 K appeared as a sharp transition in strength observed in samples of x(sub NH3) = 0.05 and 0.01, the effect of melt was less pronounced. For any given water ice + dihydrate alloy in the subsolidus region, we observed one rheological law over the entire temperature range from 175 K to about 140 K. Below 140 K, a shear instability similar to that occurring in pure water ice under the same conditions limited our ability to measure ductile flow. The rheological laws for the several alloys vary systematically from that of pure ice to that of dihydrate. Pure dihydrate is about 4 orders of magnitude less viscous than water ice just below the peritectic temperature, but because of a very pronounced temperature dependence in dihydrate (100 kJ/mol versus 43 kJ/mol for water ice) the viscosity of dihydrate equals or exceeds that of water ice at T less than 140 K. The large variation in viscosity of dihydrate with relatively small changes in temperature may be helpful in explaining the rich variety of tectonic and volcanic features seen on the surfaces of icy moons in the outer solar system.

Durham, W. B.↗
DOE OSTI2021

Thermodynamic properties of the Nd-Bi system via emf measurements, $\mathrm{DFT}$ calculations, machine learning, and $\mathrm{CALPHAD}$ modeling

Thermodynamic properties of the Nd-Bi system were investigated using a combination of experimental measurements, first-principles calculations based on density functional theory (DFT), data mining and machine learning (DM + ML) predictions, and calculation of phase diagrams (CALPHAD) modeling. The electromotive force (emf) of Nd-Bi alloys in molten LiCl-KCl-NdCl 3 at 773–973 K was measured via coulometric titration of Nd into Bi for the determination of thermochemical properties such as activity coefficients and solubilities of Nd in Bi. A new peritectic reaction of [liquid + NdBi 2 = Nd 3 Bi 7 ] at 774 K was confirmed using differential scanning calorimetry, structural (X-ray diffraction), and microstructural (scanning electron microscopy) analyses. The unknown crystal structure of NdBi2 was suggested to be a mixture of the anti-La 2 Sb configuration and the La 2 Te-type configuration based on ML predictions for over 26,000 data-mined AB 2 -type configurations together with DFT-based verifications. Using the newly acquired experimental data and DFT-based calculations, the thermodynamic description of the Nd-Bi system was remodeled, and a more complete Nd-Bi phase diagram was calculated, including the Nd 3 Bi 7 compound, invariant transition reactions, and liquidus temperatures.

36 MATERIALS SCIENCE↗
NASA NTRS1998

Orbital Processing of Eutectic Rod-Like Arrays

The eutectic is one of only three solidification classes that exist. The others are isostructural and peritectic-class reactions, respectively. Simplistically, in a binaryeutectic phase diagram, a single liquid phase isothermally decomposes to two solid phases in a cooperative manner. The melting point minimum at the eutectic composition, isothermal solidification temperature, near-isocompositional solidification and refined solidification microstructure lend themselves naturally to such applications as brazing and soldering; industries that eutectic alloys dominate. Interest in direct process control of microstructures has led, more recently, to in-situ eutectic directional solidification with applications in electro-magnetics and electro-optics. In these cases, controlled structural refinement and the high aspect ratio and regularity of the distributed eutectic phases is highly significant to the fabrication and application of these in-situ natural composites. The natural pattern formation and scaling of the dispersed phase on a sub-micron scale has enormous potential application, since fabricating bulk materials on this scale mechanically has proven to be particularly difficult. It is thus of obvious importance to understand the solidification of eutectic materials since they are of great commercial significance. The dominant theory that describes eutectic solidification was derived for diffusion-controlled growth of alloys where both solid eutectic phases solidify metallically, i.e. without faceting at the solidification interface. Both high volume fraction (lamellar) and low volume fraction (rod-like) regular metallic arrays are treated by this theory. Many of the useful solders and brazements, however, and most of the regular in-situ composites are characterized by solidification reactions that are faceted/non-faceted in nature, rather than doubly non-faceted (metallic). Further, diffusion-controlled growth conditions are atypical terrestrially since gravitationally-driven convection is pervasive. As a consequence, it is important to determine whether these faceted/non-faceted composites behave in the same manner as their doubly non-faceted counterparts, particularly in the presence of convection. Prior analytical convective sensitivity testing of this theory predicted insensitivity. Prior experimental testing of this theory offered broad-based agreement between theory and experiment, though most results were for high volume fraction lamellar eutectics that solidified without faceting at the solidification interface. Directional solidification experiments of low volume fraction rod eutectics under damped (microgravity or magnetic field) conditions, however, have demonstrated significant sensitivity, challenging this fundamental theory. More recent theories have been proposed which introduce kinetic undercooling, faceting, fluid shear of the solute redistribution zone and the possibility that the interface composition is not the same as the bulk liquid composition. This program tests the established and proposed analytical theories and addresses the origins of discrepancies between the experimental and analytical results.

Larson, David J., Jr.↗
NASA NTRS1991

Containerless processing and rapid solidification of Nb-Si alloys of hypereutectic composition

A combination of bulk undercooling in an electromagnetic levitation apparatus and splat quenching between two copper plates is used to process Nb-Si alloys in order to maximize rapid solidification conditions and minimize the effects of recalescence, with emphasis on the solidification of characteristics of alloys in the 21 to 27 at. pct Si range of composition. SEM and TEM as well as X-ray diffraction are used to characterize the microstructures of the processed samples. In the range of compositions studied, the splat-quenched drops always formed the tetragonal Nb3Si phase directly from the liquid. Drops solidified in the coil were characterized by the presence of the primary intermetallic Nb5Si3 and the absence of both peritectic Nb3Si and the equilibrium eutectic. In these cases, a metastable alpha-Nb + beta-Nb5Si3 eutectic formed. The results are discussed in terms of possible metastable configurations of the Nb-Si phase diagram as well as concepts of nucleation and growth kinetics applied to the Nb3Si and Nb5Si3 intermetallics.

Hofmeister, W. H.↗
DOE OSTI2023

Re-investigation of high-temperature phase equilibria in Fe-rich Sm–Fe–Ti alloys

Recently renewed attempts to develop high-performance rare-earth-lean permanent magnets based on the Sm(Fe,Ti) 12 compound have drawn attention to the limited knowledge about the high-temperature phase equilibria in the Sm–Fe–Ti system. Experimental investigation of equilibrated alloys with electron probe microanalysis, X-ray diffraction and thermomagnetic analysis revealed several inaccuracies in the currently accepted phase relations at 1000°C and allowed for a revision of the Fe-rich corner of the Sm–Fe–Ti phase diagram. The Sm(Fe,Ti) 12 and Sm 3 (Fe,Ti) 29 phases were found to have more extended Ti ranges of 5.1–9.7 at% and 2.8–6.9 at%, respectively. With increasing of the Ti content, the Curie temperature of the Sm(Fe,Ti) 12 remains nearly constant at 306–312°C, whereas that of the Sm 3 (Fe,Ti) 29 increases from 188°C to 207°C. The low-titanium Sm 3 (Fe,Ti) 29 phase equilibrates not only with the Sm(Fe,Ti) 12 and Sm2(Fe,Ti) 17 phases, but also with (α-Fe) solid solution. Newly demonstrated equilibrium between Sm 2 (Fe,Ti) 17 and TiFe 2 phases makes impossible the earlier reported equilibrium between the Sm 3 (Fe,Ti) 29 and Sm(Fe,Ti) 11 phases. Because of an invariant reaction at 1000 °C, the revised phase diagram also features a class II four-phase equilibrium Sm 3 (Fe,Ti) 29 + TiFe 2 + Sm(Fe,Ti) 12 + Sm 2 (Fe,Ti) 17 . Peritectic decomposition of the Sm(Fe,Ti) 11 phase, which occurs either at 1075°C or at 1087°C, was found to have among its products the Sm(Fe,Ti) 12 phase. Although no such equilibration was attempted, it must be possible to obtain above 1087°C a two-phase state composed of the Sm(Fe,Ti) 12 phase and a liquid – which is important for manufacturing of the Sm(Fe,Ti) 12 - based permanent magnets via the liquid-phase sintering.

36 MATERIALS SCIENCE↗