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All sourcesNASA NTRSDOE OSTI
NASA NTRS1995

Directional Solidification and Mechanical Properties of NiAl-NiAlTa Alloys

Directional solidification of eutectic alloys is a promising technique for producing in-situ composite materials exhibiting a balance of properties. Consequently, the microstructure, creep strength and fracture toughness of directionally solidified NiAl-NiAlTa alloys were investigated. Directional solidification was performed by containerless processing techniques to minimize alloy contamination. The eutectic composition was found to be NiAl-15.5 at% Ta and well-aligned microstructures were produced at this composition. A near-eutectic alloy of NiAl-14.5Ta was also investigated. Directional solidification of the near-eutectic composition resulted in microstructures consisting of NiAl dendrites surrounded by aligned eutectic regions. The off-eutectic alloy exhibited promising compressive creep strengths compared to other NiAl-based intermetallics, while preliminary testing indicated that the eutectic alloy was competitive with Ni-base single crystal superalloys. The room temperature toughness of these two-phase alloys was similar to that of polycrystalline NiAl even with the presence of the brittle Laves phase NiAlTa.

Johnson, D. R.↗
NASA NTRS1993

Solidification of eutectic system alloys in space (M-19)

It is well known that in the liquid state eutectic alloys are theoretically homogeneous under 1 g conditions. However, the homogeneous solidified structure of this alloy is not obtained because thermal convection and non-equilibrium solidification occur. The present investigators have clarified the solidification mechanisms of the eutectic system alloys under 1 g conditions by using the in situ observation method; in particular, the primary crystals of the eutectic system alloys never nucleated in the liquid, but instead did so on the mold wall, and the crystals separated from the mold wall by fluid motion caused by thermal convection. They also found that the equiaxed eutectic grains (eutectic cells) are formed on the primary crystals. In this case, the leading phase of the eutectic must agree with the phase of the primary crystals. In space, no thermal convection occurs so that primary crystals should not move from the mold wall and should not appear inside the solidified structure. Therefore no equiaxed eutectic grains will be formed under microgravity conditions. Past space experiments concerning eutectic alloys were classified into two types of experiments: one with respect to the solidification mechanisms of the eutectic alloys and the other to the unidirectional solidification of this alloy. The former type of experiment has the problem that the solidified structures between microgravity and 1 g conditions show little difference. This is why the flight samples were prepared by the ordinary cast techniques on Earth. Therefore it is impossible to ascertain whether or not the nucleation and growth of primary crystals in the melt occur and if primary crystals influence the formation of the equiaxed eutectic grains. In this experiment, hypo- and hyper-eutectic aluminum copper alloys which are near eutectic point are used. The chemical compositions of the samples are Al-32.4mass%Cu (Hypo-eutectic) and Al-33.5mass%Cu (hyper-eutectic). Long rods for the samples are cast by the Ohno Continuous Casting Process and they show the unidirectionally solidified structure. Each flight and ground sample was made of these same rods. The dimensions of all samples are 4.5 mm in diameter and 23.5 mm in length. Each sample is put in a graphite capsule and then vacuum sealed in a double silica ampoule. Then the ampoule is put in the tantalum cartridge and sealed by electron beam welding. For onbard experiments, a Continuous Heating Furnance (CHF) will be used for melting and solidifying samples under microgravity conditions. Six flight samples will be used. Four samples are hypo-eutectic and two are hyper-eutectic alloys. The surface of the two hypo-eutectic alloy samples are covered with aluminum oxide film to prevent Marangoni convection expected under microgravity conditions. Each sample will be heated to 700 C and held at that temperature for 5 min. After that the samples will be allowed to cool to 500 C in the furnace and they will be taken out of the furnace for He gas cooling. The heating and cooling diagrams for the flight experiments are shown. After collecting the flight samples, the solidified structures of the samples will be examined and the mechanisms of eutectic solidification under microgravity conditions will be determined. It is likely that successful flight experiment results will lead to production of high quality eutectic alloys and eutectic composite materials in space.

Ohno, Atsumi↗
DOE OSTI2026

Assessment of binary eutectic Ni alloys for high-temperature applications via laser remelting

It has been recently demonstrated that eutectic alloys processed by additive manufacturing have excellent high-temperature mechanical properties. We suggest that nickel-base eutectic alloys may enable new combinations of structural and functional properties. To this end, we investigate the processability, microstructure, and thermal stability of five, binary near-eutectic Ni-X (X = B, Ce, La, Y, and Zr) alloys processed via surface laser-remelting. The microstructure of all alloys contain a two-phase lamellar eutectic microstructure consisting of γ-Ni and intermetallic phases; this microstructure is significantly finer (100–200 nm lamellar spacing) in the laser-remelted alloys than in the cast substrate (0.5–1.0 µm lamellar spacing). The microhardness of the laser-remelted alloys (550–770 HV) is 35–50% higher than that of the cast alloys (370–570 HV) due to this finer eutectic spacing. An anomalous eutectic microstructure appears at the meltpool boundaries, containing globular and lamellar γ-Ni phases. The alloys contain a high volume fraction (>50 vol%) of intermetallic phase which forms a continuous network, causing brittleness. Following laser-remelting trials, the alloys showed a high density of solid-state cracks, except for the Ni-Zr alloy which processed well. During thermal exposure at 700 and 900°C for up to 500 h, the eutectic microstructure coarsens. Coarsening occurs heterogeneously and initiates at the meltpool boundaries. This process occurs more slowly in the Ni-Zr and Ni-Y alloys, and more rapidly in the remaining alloys, resulting in greater microhardness retention in the Ni-Zr and Ni-Y alloys following thermal exposure at 700°C. Thus, among the five alloys, the Ni-Zr system exhibits a good combination of high-temperature mechanical properties and processability. Here, we conclude with recommendations for future work on designing additively manufactured alloys based on these eutectic Ni systems.

Additive manufacturing↗
NASA NTRS2001

Experimental and Theoretical Investigations of the Solidification of Eutectic Al-Si Alloy

The eutectic alloys have a wide spectrum of applications due to their good castability and physical and mechanical properties. The interphase spacing resulting during solidification is an important microstructural feature that significantly influences the mechanical behavior of the material. Thus, knowledge of the evolution of the interphase spacing during solidification is necessary in order to properly design the solidification process and optimize the material properties. While the growth of regular eutectics is rather well understood, the irregular eutectics such as Al-Si or Fe-graphite exhibit undercoolings and lamellar spacings much larger than those theoretically predicted. Despite of a considerable amount of experimental and theoretical work a clear understanding of the true mechanism underlying the spacing selection in irregular eutectics is yet to be achieved. A new experimental study of the solidification of the eutectic Al-Si alloy will be reported in this paper. The measured interface undercoolings and lamellar spacing will be compared to those found in the literature in order to get more general information regarding the growth mechanism of irregular eutectics. A modification of the present theory of the eutectic growth is also proposed. The results of the modified mathematical model, accounting for a non-isothermal solid/liquid interface, will be compared to the experimental measurements.

Sen, S.↗
NASA NTRS1981

Heat storage in alloy transformations

The feasibility of using metal alloys as thermal energy storage media was determined. The following major elements were studied: (1) identification of congruently transforming alloys and thermochemical property measurements; (2) development of a precise and convenient method for measuring volume change during phase transformation and thermal expansion coefficients; (3) development of a numerical modeling routine for calculating heat flow in cylindrical heat exchangers containing phase change materials; and (4) identification of materials that could be used to contain the metal alloys. Several eutectic alloys and ternary intermetallic phases were determined. A method employing X-ray absorption techniques was developed to determine the coefficients of thermal expansion of both the solid and liquid phases and the volume change during phase transformation from data obtained during one continuous experimental test. The method and apparatus are discussed and the experimental results are presented. The development of the numerical modeling method is presented and results are discussed for both salt and metal alloy phase change media.

Birchenall, C. E.↗
DOE OSTI2023

3D Printed eutectic aluminum alloy has facility for site-specific properties

Additive manufacturing (AM) has the ability to print structures with site-specific properties. Existing AM approaches for site-specific properties are, however, based on complex processing-microstructure relationships in conventional alloys that were not designed for this purpose. Here, in this work, we report a straightforward approach for achieving site-specific properties that takes advantage of eutectic solidification characteristics. We demonstrate that the yield strength of a eutectic Al-Cu-Ce-Zr alloy can be tuned by varying the laser scan speed in concert with hatch spacing in laser powder bed fusion AM. A faster speed increases solidification rate resulting in finer eutectic spacing and higher strength. The hatch spacing is reduced at faster speeds to ensure overlap between melt pools which become smaller with increasing scan speed. The yield strength and its anisotropy relative to build direction are further tunable with a heat treatment. The scan speed-eutectic spacing-strength relationship is successfully applied to print a complex pattern of site-specific hardness in the alloy. The generalized principle of using AM for a eutectic alloy to create site-specific properties and anisotropy in properties is demonstrated.

36 MATERIALS SCIENCE↗
NASA NTRS1991

Free energy change of off-eutectic binary alloys on solidification

A formula for the free energy difference between the undercooled liquid phase and the stable solid phase is derived for off-eutectic binary alloys in which the equilibrium solid/liquid transition takes place over a certain temperature range. The free energy change is then evaluated numerically for a Bi-25 at. pct Cd alloy modeled as a sub-subregular solution.

Ohsaka, K.↗
NASA NTRS1986

Directional solidification and characterization of near eutectic Sm2CO17/Co alloys

The effects of directional solidification processing on the microstructural, compositional, and magnetic properties of near eutectic Co-Sm alloys (about 9 at. pct Sm) have been studied. Initial investigations have been performed at modest thermal gradients in the liquid, G(L) less than 60 C/cm and over a range of furnace (solidification) velocities, V = 0.8 45.4 cm/h. The primary dendrite spacing for near eutectic Sm2Co17/Co scaled with 1/sq rt V and varied from about 50 microns for V greater than or equal to 20 cm/h to hundreds of microns for V less than 10 cm/h, while the rod eutectic diameter and interrod spacing were an order of magnitude smaller. For both dendritic and cooperative growth, the associated permanent magnet properties were rather poor, e.g., remanence less than 4 kG and coercive force less than 1 kOe for the smallest dendrite and rod diameter dimensions encountered, although the magnetic hardness for the rod eutetic was larger than for the dendritic microstructure. Magnetization as a function of sample orientation indicated that the easy axis of magnetization was primarily along the direction of solidification for both ferromagnetic phases.

Pirich, Ronald G.↗
NASA NTRS1987

Containerless processing of undercooled melts

Containerless drop tube processing allows for significant levels of liquid undercooling through control of parameters such as sample size, surface coating and cooling rate. A laboratory scale (3 m) drop tube has been developed which allows the undercooling and solidification behavior of powder samples to be evaluated under low gravity free-fall conditions. The level of undercooling obtained in an InSb-Sb eutectic alloy has been evaluated by comparing the eutectic spacing in drop tube samples with a spacing/undercooling relationship established using thermal analysis techniques. Undercoolings of 0.17 and 0.23 T(e) were produced by processing under vacuum and He gas conditions respectively. Alternatively, the formation of an amorphous phase in a Ni-Nb eutectic alloy indicates that undercooling levels of approximately 500 C were obtained by drop tube processing. The influence of droplet size and gas environment on undercooling behavior in the Ni-Nb eutectic was evaluated through their effect on the amorphous/crystalline phase ratio. To supplement the structural analysis, heat flow modeling has been developed to describe the undercooling history during drop tube processing, and the model has been tested experimentally.

Shong, D. S.↗
DOE OSTI2025

Unraveling Impurity-Dependent Morphological and Chemical Evolution of Ni–20Cr Alloy in Eutectic LiCl–KCl Molten Salt

Understanding the interfacial evolution of alloys in molten salt with different amounts of water (H 2 O) and oxygen (O 2 ) impurities is significant for applications in many fields, including concentrated solar power, molten salt reactors, and applications in pyrochemical reprocessing and electrorefining. Additionally, the impurity-driven corrosion mechanisms that lead to various morphological and chemical evolution characteristics at the interfaces of structural alloys and molten salts are not fully understood. In the present work, the three-dimensional (3D) morphological evolution of Ni-20Cr microwires in LiCl-KCl was studied at 500 °C under different moisture and oxygen conditions using in situ synchrotron transmission X-ray microscopy (TXM) and scanning transmission electron microscopy (STEM) techniques. No significant morphological changes were observed in Ni-20Cr microwires under vacuum conditions. However, the wires exhibited distinct morphological evolutions when exposed to molten salt containing H 2 O alone, as well as when both H 2 O and O 2 were present. Furthermore, Cr 2 O 3 precipitates were observed in the molten salt during corrosion with only H 2 O present, while Cr 6+ species were identified in the salt when O 2 was added. Further, these findings are crucial for understanding the corrosion mechanisms of molten salt with different amounts of H 2 O and O 2 contamination, providing insights for developing corrosion mitigation methods and improving the stability of containment alloys in molten salt applications.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
NASA NTRS1980

Heat storage in alloy transformations

The feasibility of using metal alloys as thermal energy storage media was investigated. The elements selected as candidate media were limited to aluminum, copper, magnesium, silicon, zinc, calcium, and phosphorus on the basis of low cost and latent heat of transformation. Several new eutectic alloys and ternary intermetallic phases were determined. A new method employing X-ray absorption techniques was developed to determine the coefficients of thermal expansion of both the solid and liquid phases and the volume change during phase transformation. The method and apparatus are discussed and the experimental results are presented for aluminum and two aluminum-eutectic alloys. Candidate materials were evaluated to determine suitable materials for containment of the metal alloys. Graphite was used to contain the alloys during the volume change measurements. Silicon carbide was identified as a promising containment material and surface-coated iron alloys were also evaluated. System considerations that are pertinent if alloy eutectics are used as thermal energy storage media are discussed. Potential applications to solar receivers and industrial furnaces are illustrated schematically.

Birchenall, C. E.↗
DOE OSTI2024

Thermal stability and coarsening of eutectic and near-eutectic Ni–Ce alloys

Ni–Ce alloys are currently being studied as a castable alternative to conventional Ni-based superalloys. To understand the evolution of microstructure and mechanical behavior at elevated temperatures, this study investigates the mechanism of coarsening behavior in eutectic and near eutectic Ni–Ce at 900 °C. The as-cast eutectic Ni–Ce consists of a combination of fine lamellar and rod eutectic colonies with coarser boundary regions. Upon annealing, continuous coarsening, via process of globularization, initiates at colony boundaries or primary dendrites where faults (termination and branches) in the lamellar structure are plentiful. Coarsening then proceeds by a combination of fault migration mechanism and lamellar boundary splitting, growing toward the center of the eutectic colonies with increasing annealing time. Coarsening near the center of a colony is extremely slow, indicating the eutectic microstructure itself is very stable. Here, the near-eutectic alloys containing primary dendrites coarsen and stabilize faster compared to the fully eutectic alloy. Moreover, an anomaly is observed in the hardness of the fully eutectic alloy after long exposure at elevated temperature compared to the near-eutectic alloys.

36 MATERIALS SCIENCE↗
NASA NTRS1976

Coatings for directional eutectics

Coatings developed to provide oxidation protection for the directionally-solidified eutectic alloy NiTaC-B (4.4 weight percent Cr) were evaluated. Of seven Co-, Fe- and Ni-base coatings that were initially investigated, best resistance to cyclic oxidation was demonstrated by duplex coatings fabricated by depositing a layer of NiCrAl(Y) by vacuum evaporation from an electron beam source followed by deposition of an Al overlayer using the pack cementation process. It was found that addition of carbon to the coating alloy substantially eliminated the problem of fiber denudation in TaC-type eutectic alloys. Burner rig cycled NiTaC-B samples coated with Ni-20Cr-5Al-0.1C-0.1Y+Al and rupture-tested at 1100 deg C performed as well as or better than uncoated, vacuum cycled and air-tested NiTaC-13; however, a slight degradation with respect to uncoated material was noted in air-stress rupture tests at 870 deg C for both cycled and uncycled samples.

Rairden, J. R.↗
NASA NTRS1975

Eutectic superalloys by edge-defined, film-fed growth

The feasibility of producing directionally solidified eutectic alloy composites by edge-defined, film-fed growth (EFG) was carried out. The three eutectic alloys which were investigated were gamma + delta, gamma/gamma prime + delta, and a Co-base TaC alloy containing Cr and Ni. Investigations into the compatibility and wettability of these metals with various carbides, borides, nitrides, and oxides disclosed that compounds with the largest (negative) heats of formation were most stable but poorest wetting. Nitrides and carbides had suitable stability and low contact angles but capillary rise was observed only with carbides. Oxides would not give capillary rise but would probably fulfill the other wetting requirements of EFG. Tantalum carbide was selected for most of the experimental portion of the program based on its exhibiting spontaneous capillary rise and satisfactory slow rate of degradation in the liquid metals. Samples of all three alloys were grown by EFG with the major experimental effort restricted to gamma + delta and gamma/gamma prime + delta alloys. In the standard, uncooled EFG apparatus, the thermal gradient was inferred from the growth speed and was 150 to 200 C/cm. This value may be compared to typical gradients of less than 100 C/cm normally achieved in a standard Bridgman-type apparatus. When a stream of helium was directed against the side of the bar during growth, the gradient was found to improve to about 250 C/cm. In comparison, a theoretical gradient of 700 C/cm should be possible under ideal conditions, without the use of chills. Methods for optimizing the gradient in EFG are discussed, and should allow attainment of close to the theoretical for a particular configuration.

Hurley, G. F.↗
NASA NTRS1990

Influence of convection on microstructure

In eutectic growth, as the solid phases grow they reject atoms to the liquid. This results in a variation of melt composition along the solid/liquid interface. In the past, mass transfer in eutectic solidification, in the absence of convection, was considered to be governed only by the diffusion induced by compositional gradients. However, mass transfer can also be generated by a temperature gradient. This is called thermotransport, thermomigration, thermal diffusion or the Soret effect. A theoretical model of the influence of the Soret effect on the growth of eutectic alloys is presented. A differential equation describing the compositional field near the interface during unidirectional solidification of a binary eutectic alloy was formulated by including the contributions of both compositional and thermal gradients in the liquid. A steady-state solution of the differential equation was obtained by applying appropriate boundary conditions and accounting for heat flow in the melt. Following that, the average interfacial composition was converted to a variation of undercooling at the interface, and consequently to microstructural parameters. The results obtained show that thermotransport can, under certain circumstances, be a parameter of paramount importance.

Wilcox, William R.↗
NASA NTRS1977

Method for attaching a fused-quartz mirror to a conductive metal substrate

A fused-quartz mirror is attached to a conductive metal substrate by the following steps: tinning one surface of a fused-quartz mirror with a solder of substantially pure indium; tinning a metallic substrate with an indium eutectic alloy consisting essentially of indium bismuth, lead and tin having a melting point substantially below that of indium; heating the eutectic alloy to a temperature substantially above its melting point, but below that of the solder; floating the mirror into place, and subsequently cooling the alloy to a temperature substantially below its melting point.

Sonnenschein, G.↗
NASA NTRS1999

Use of Microgravity to Control the Microstructure of Eutectics

The long term goal of this project is to be able to control the microstructure of directionally solidified eutectic alloys, through an improved understanding of the influence of convection. Prior experimental results on the influence of microgravity on the microstructure of fibrous eutectics have been contradictory. Theoretical work at Clarkson University showed that buoyancy-driven convection in the vertical Bridgman configuration is not vigorous enough to alter the concentration field in the melt sufficiently to cause a measurable change in microstructure when the eutectic grows at minimum supercooling. Currently, there are four other hypotheses that might explain the observed changes in microstructure of fibrous eutectics caused by convection: (1) Disturbance of the concentration boundary layer arising from an off-eutectic melt composition and growth at the extremum; (2) Disturbance of the concentration boundary layer of a habit-modifying impurity; (3) Disturbance of the concentration boundary layer arising from an off-eutectic interfacial composition due to non-extremum growth; and (4) A fluctuating freezing rate combined with differences in the kinetics of fiber termination and fiber formation. We favor the last of these hypotheses. Thus, the primary objective of the present grant is to determine experimentally and theoretically the influence of a periodically varying freezing rate on eutectic solidification. A secondary objective is to determine the influence of convection on the microstructure of at least one other eutectic alloy that might be suitable for flight experiments.

Wilcox, William R.↗
NASA NTRS1998

Use of Microgravity to Control the Microstructure of Eutectics

This grant began in June of 1996. Its long term goal is to be able to control the microstructure of directionally solidified eutectic alloys, through an improved understanding of the influence of convection. The primary objective of the present projects is to test hypotheses for the reported influence of microgravity on the microstructure of three fibrous eutectics (MnBi-Bi, InSb-NiSb, Al3Ni-Al). A secondary objective is to determine the influence of convection on the microstructure of other eutectic alloys. Two doctoral students and a masters student supported as a teaching assistant were recruited for this research. Techniques were developed for directional solidification of MnBi-Bi eutectics with periodic application of current pulses to produce an oscillatory freezing rate. Image analysis techniques were developed to obtain the variation in MnBi fiber spacing, which was found to be normally distributed. The mean and standard deviation of fiber spacing were obtained for several freezing conditions. Eighteen ampoules were prepared for use in the gradient freeze furnace QUELD developed at Queen's University for use in microgravity. Nine of these ampoules will be solidified soon at Queen's in a ground-based model. We hope to solidify the other nine in the QUELD that is mounted on the Canadian Microgravity Isolation Mount on MIR. Techniques are being developed for directional solidification of the Al-Si eutectic at different freezing rates, with and without application of accelerated crucible rotation to induce convection. For the first time, theoretical methods are being developed to analyze eutectic solidification with an oscillatory freezing rate. In a classical sharp-interface model, we found that an oscillatory freezing rate increases the deviation of the average interfacial composition from the eutectic, and increases the undercooling of the two phases by different amounts. This would be expected to change the volume fraction solidifying and the fiber spacing. Because of difficulties in tracking the freezing interfaces of the two solid phases, a phase-field model is also being developed. A paper demonstrating application of phase field methods to periodic structures has been submitted for publication.

Wilcox, William R.↗