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NASA NTRS1972

Directional solidification of eutectic composites in space environment

The Ni-Ni3Ta eutectic and a nickel-base alloy containing 30 wt pct Ta were solidified unidirectionally in an electron beam floating zone melting apparatus. It was found that the volume fraction of the Ni3Ta phase in the Ni-Ni3Ta eutectic mixture was increased from 7.6 to 36 volume pct in agreement with the theory as predicted. Tensile properties of the randomly solidified and unidirectionally solidified Ni-Ni3Ta eutectic were determined as function of solidification rate and temperature. It was found that the ultimate tensile strength decreased as both the test temperature and solidification rate increased. An elongation of 40 pct was obtained for a nickelbase alloy containing 30 wt at room temperature. This unusually large elongation was attributed to the superplastic behavior of the alloy. The critical currents versus the external fields at 2.5, 3.0, 3.5 and 4.2 deg for the unidirectionally solidified Pb-Sn eutectic were measured. The values of critical fields at zero critical currents were obtained by extrapolation.

Yue, A. S.↗

DOE OSTI2025

Compatibility of Zircaloy-4 in eutectic PbSn and PbBiSn liquid metals

Here, a novel nuclear fuel concept has been proposed, consisting of UO₂ particles suspended in a liquid metal alloy. To evaluate its feasibility, the compatibility of Zircaloy-4 cladding with candidate eutectic PbSn and PbBiSn alloys—as well as with pure Pb, Bi, and Sn—was investigated through 1000-hour exposures at 400 °C and 600 °C. Severe degradation of the Zircaloy-4 specimens was observed in eutectic PbSn at 600 °C, whereas oxidation and oxygen diffusion were evident after exposure at 400 °C. At 600 °C, the formation of Zr₃Fe precipitates at the oxide–alloy interface was identified in specimens exposed to Pb and PbBiSn. Thermodynamic analysis suggested that the observed intermetallic formation resulted from the destabilization of Laves phases due to oxygen ingress at elevated temperatures.

Bismuth↗

NASA NTRS1992

Mechanical properties of Haynes Alloy 188 after exposure to LiF-22CaF2, air, and vacuum at 1093 K for periods up to 10,000 hours

As part of a program to provide reassurance that the cobalt-base superalloy Haynes Alloy 188 can adequately contain a LiF-CaF2 eutectic thermal energy storage salt, 4900- and 10,000-hr exposures of Haynes Alloy 188 to LiF-22CaF2, its vapor, vacuum, and air at 1093 K have been undertaken. Following such exposures, the microstructure has been characterized and the 77 to 1200 K tensile properties measured. In addition, 1050 K vacuum creep-rupture testing of as-received and molten salt- and vacuum-exposed samples has been undertaken. Although slight degradation of the mechanical properties of Haynes Alloy 188 due to prior exposure was observed, basically none of the losses could be ascribed to a particular environment. Hence, observed decreases in properties are due to thermal aging effects, not corrosive attack. In view of these findings, Haynes Alloy 188 is still deemed to be suitable for containment of the eutectic LiF-CaF2 thermal energy storage media.

Whittenberger, J. D.↗

NASA NTRS1990

Crystal growing

One objective is to demonstrate the way crystals grow and how they affect the behavior of material. Another objective is to compare the growth of crystals in metals and nonmetals. The procedures, which involve a supersaturated solution of a salt that will separate into crystals on cooling and the pouring off of an eutectic solution to expose the crystals formed by a solid solution when an alloy of two metals forms a solid and eutectic solution on cooling, are described.

Neville, J. P.↗

DOE OSTI2025

Design and Analysis of a Mutual Inductance Level Sensor for Liquid Metals

Here, this article describes the design and analysis of an electromagnetic level sensor for use in high-temperature liquid metal systems. The mutual inductance level sensor (MILS) described in this work was fabricated using two single-conductor mineral insulated cables wrapped in a bifilar fashion around a stainless steel tube core and was housed in an isolating thimble that preserved the pressure boundary of the test vessel. Two sensor variations were fabricated that differ only in active length, 1016 and 1778 mm. Experimental data were collected using the 1016-mm sensor (MILS-MKII-040) that demonstrated a sensitivity of 9.2 μ V/mm in a room temperature testing stand that used solid aluminum as a surrogate for liquid metal. Experimental data were collected using the 1778-mm sensor (MILS-MKII-070) that demonstrated a sensitivity of 6.9 μ V/mm in the high-temperature (300 ° C) liquid sodium environment at the mechanisms engineering test loop (METL) of Argonne National Laboratory. The sensor performance was found to be repeatable over the course of several months, with roughly ±1% deviation from nominal output. Finite element models were developed in COMSOL Multiphysics that fully describe each test setup, and the models were validated using experimental data. The validated COMSOL models were used to perform an array of analyses that examined the performance of the sensor in differing environments. Maximizing the coil diameter inside the isolating thimble was found to maximize the signal and sensitivity of the sensor. An optimal operating frequency was found near 1000 Hz using both experimental data and COMSOL. The influence of a metallic thimble surrounding the sensor and a metallic sensor core was quantified and found to be negligible at the optimal operating frequency. The sensitivity of the sensor was quantified when monitoring the level of additional liquid metals. These include lead, lead-bismuth eutectic (LBE), sodium-potassium alloy (NaK), and lithium (in addition to sodium). The sensitivities were quantified using liquid metal properties at 350 ° C and 650 ° C. The geometry of the test stand model, all material properties used in the model, and the results are presented in a manner that allows the reader can replicate the model and perform additional analyses.

COMSOL↗

NASA NTRS1984

Bulk undercooling

Bulk undercooling methods and procedures will first be reviewed. Measurement of various parameters which are necessary to understand the solidification mechanism during and after recalescence will be discussed. During recalescence of levitated, glass-encased large droplets (5 to 8 mm diam) high speed temperature sensing devices coupled with a rapid response oscilloscope are now being used at MIT to measure local thermal behavior in hypoeutectic and eutectic binary Ni-Sn alloys. Dendrite tip velocities were measured by various investigators using thermal sensors or high speed cinematography. The confirmation of the validity of solidification models of bulk-undercooled melts is made difficult by the fineness of the final microstructure, the ultra-rapid evolution of the solidifying system which makes measurements very awkward, and the continuous modification of the microstructure which formed during recalescence because of precipitation, remelting and rapid coarsening.

Kattamis, T. Z.↗

NASA NTRS1987

Dendritic growth of undercooled nickel-tin. I, II

A comparison is made between high speed cinematography and optical temperature measurements of the solidification of an undercooled Ni-25 wt pct Sn alloy. The first part of this study notes that solidification during the recalescence period at all undercoolings studied occurred in the form of a dendritelike front moving across the sample surface, and that the growth velocities observed agree with calculation results for the dendrite growth model of Lipton et al. (1986); it is concluded that the coarse structure observed comprises an array of much finer, solute-controlled dendrites. In the second part, attention is given to the solidification of levitated metal samples within a transparent glass medium for the cases of two undercooled Ni-Sn alloys, one of which is eutectic and another hypoeutectic. The data obtained suggest a solidification model involving dendrites of very fine structure growing into the melt at temperatures near the bulk undercooling temperature.

Wu, Y.↗

NASA NTRS1977

Directionally solidified eutectic gamma-gamma nickel-base superalloys

A directionally solidified multivariant eutectic gamma-gamma prime nickel-base superalloy casting having improved high temperature properties was developed. The alloy is comprised of a two phase eutectic structure consisting essentially of on a weight percent base, 6.0 to 9.0 aluminum, 5.0 to 17.0 tantalum, 0-10 cobalt, 0-6 vanadium, 0-6 rhenium, 2.0-6.0 tungsten, and the balance being nickel, subject to the proviso that the sum of the atomic percentages of aluminum plus tantalum is within the range of from 19-22, and the ratio of atomic percentages of tantalum to aluminum plus tantalum is within the range of from 0.12 to 0.23. Embedded within the gamma nickel-base matrix are aligned eutectic gamma prime phase (primarily nickel-aluminum-tantalum) reinforcing fibers.

Jackson, M. R.↗

NASA NTRS1984

Structure and recalescence behavior of undercooled nickel-tin alloys

The effects of undercooling on the thermal behavior and structure of Ni-Sn alloys are investigated. Hypoeutectic (Ni-25 wt pct Sn) and eutectic (Ni-32.5 wt pct Sn) compositions of the Ni-Sn alloy were undercooled using a levitation melting with glass encasement technique, and the recalescence of these alloys was measured using a high speed temperature sensing device and a digital oscilloscope. It is observed that in both samples the total solidification and recalescence times decrease with increasing undercooling; the volume fraction of normal lamellar eutectic decreases with increasing undercooling; and in the hypoeutectic sample, the morphology of the primary phase changes from dendritic to spherical with increasing undercooling.

Wu, Yanzhong↗

NASA NTRS1987

Directional solidification of Bi-Mn alloys using an applied magnetic field

Off-eutectic compositions of Bi-Mn were directionally solidified in applied transverse magnetic fields up to 3 kG, to determine the effects on thermal and solutal convection. Plane front directional solidification of eutectic and near-eutectic Bi-Mn results in a two-phase rodlike morphology consisting of ferromagnetic MnBi rods in a Bi solid solution matrix. Compositions of either side of the eutectic were studied in growth orientations vertically up and down. Temperature gradient was monitored during growth by means of an in-situ thermocouple. For Bi-rich compositions, the magnetic field appeared to increase mixing as determined from thermal, morphological, chemical, and magnetic analyses. For Mn-rich compositions, morphological and chemical analyses suggest some reduction in mixing due to application of the magnetic force. The capability for carrying out directional solidification of Bi-Mn in high longitudinal magnetic fields was established.

Decarlo, J. L.↗

NASA NTRS1977

The promise of eutectics for aircraft turbines

Gas turbine blades and vanes for the 1980s call for new materials with higher operational temperature capabilities. The potential increase of from 40 to 110 C in operational temperature capabilities predicted for directionally solidified eutectics is a larger increment over currently available alloys than previously obtained in any new turbine blade alloy. The paper discusses the properties of gamma/gamma prime-delta and NiTaC-13 directionally solidified first-generation eutectics for use as gas turbine blade materials. A few of the more promising second-generation eutectics for blade applications (gamma/gamma prime-alpha, NiTaC 3-116A) and for vane applications (gamma-beta, COTAC 74) are also discussed. Attention is given to mechanical properties, such as transverse ductility and shear strength, that can be inherently critical in a directionally solidified eutectic. Further R&D requirements for properties, coatings, and lower cost processing technology are identified.

Gray, H. R.↗

NASA NTRS2003

Minimizing Segregation during the Controlled Directional Solidification of Dendric Alloys

Gravity-driven convection induced in the liquid by density gradients of temperature or composition disrupts uniform dendritic growth during controlled directional solidification and promotes severe macrosegregation. The solute-rich region about the dendrite tip appears to play a pivotal role in channel initiation. Allen and Hunt referred to this region as an "initial transient" or dynamic region constituting steep concentration gradients. Experimental investigation also point to the role the tip region plays in developing microstructure. Hellawell and co-workers showed that flow-through dendritic channels could be effectively disrupted, and segregation minimized, during the gradient freezing of bulk castings by rotating the melt through a slight angle with respect to Earth's gravity vector. Adapting this principle to controlled directional solidification, it has been shown" that segregation in dendritic alloys can be minimized, and properties improved, by processing the sample near horizontal in conjunction with a slow axial rotation of the crucible. It is postulated that the observed microstructural uniformity arises by maintaining the developing solute field about the dendrite tip. Solute rejected during vertical directional solidification will rise or sink parallel to the primary dendrite arms during axial rotation setting the stage for accumulation, instabilities, and segregation. In contrast, during horizontal growth, the rejected solute will sink or rise perpendicular to the primary dendrite. Now, in the presence of a slight axial rotation, solute that was initially sinking (or rising) will find itself above (or below) its parent dendrite, i.e., still about the tip region. The following is intended to experimentally demonstrate the viability of this concept in coordination with a model that gives predictive insight regarding solute distribution about growing dendrites. Alloys based on the lead-tin eutectic system were used in this study. The system is well characterized, the constituent metals are available in a very pure form, and the thermophysical properties are well known. During solidification of hypoeutectic alloys, e.g., 55 wt pct Pb, the primary dendrites reject the less dense tin, and for the hypereutectic alloys, e.g., 75 wt pct Sn, the primary dendrites reject denser lead. Alloys were prepared by melting appropriate amounts of lead and tin in a glass crucible after which the homogeneous liquid was sucked directly into 5-mm i.d. glass tubes. The sample tube, containing approximately 30 cm of alloy, was then mechanically driven into the directional solidification furnace assembly and positioned such that approx. 20 cm of the sample was remelted. Subsequently, directional solidification was initiated by withdrawing the sample through a water-cooled jacket at a constant growth velocity of 2 ,microns/s. After 5 to 6 cm of growth, the sample was quickly removed from the furnace and quenched in a water bath to preserve the solid-liquid interface. Samples were directionally solidified vertically upward, nearly horizontally, and some in conjunction with an applied axial rotation of the crucible. Temperature gradients at the solid-liquid interface were measured with an in-siru K-type thermocouple. Solidified samples were cut perpendicular and parallel to the growth direction and conventionally prepared for microscopic examination.

Grugel, Richard N.↗

DOE OSTI2024

Cathodic Decomposition Electrodes as Standard Reference Electrodes for Molten Salts: Example of the Lithium Eutectic Electrode for the LiCl-KCl Eutectic

Alternatives to the widely-used standard anodic decomposition reference electrodes in molten salts are necessary to enable more easily reproduced thermochemical and electrochemical data in molten salt electrolytes. The class of standard reference electrodes called cathodic decomposition electrodes (CDEs) are easily constructed and can be used to make thermochemical measurements in molten salts more directly compared to anodic decomposition electrodes. The lithium eutectic electrode (LEE) was chosen as a sample test case for validation and was applied to thermochemical measurements of electroactive species in molten LiCl-KCl eutectic. Transient measurements were made to measure the Li + /Li reduction potential at zero current in pure LiCl-KCl eutectic relative to a Li-alloy reference electrode to validate the reference potential of the LEE. Literature-reported electromotive force measurements against Li-alloy reference electrodes were used to generate a relationship between the LEE and the standard chlorine electrode and this relationship was used to evaluate measured and reported formal potential measurements for the LiCl-KCl-GdCl 3 system. This work demonstrates the general framework for defining CDEs for any molten salt system and a method for calibrating external reference electrodes against a CDE standard reference electrode, improving the ease of obtaining thermochemical and electrochemical measurements in any molten salt system.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

NASA NTRS1981

Space Shuttle - A new era in transportation

After a brief historical review of the economics of expendable-booster, commercial-payload operations to date, and a description of the Space Shuttle system's design, operational capabilities, and mission profile, the payload flight assignments, materials processing experiments, and Spacelab I material science experiment are detailed. Among the Materials Processing in Space (MPS) fields for investigation are crystal growth from vapor and solution, the production of magnetic composites and metal foams, laser host glasses and metallic glasses, non-buoyancy-driven convections, unidirectional solidification of eutectics, and the solidification of immiscible alloys. Emphasis is put on the long-term, commercial usefulness of such studies, with attention to historical precedents such as the Skylab, Apollo and Apollo-Soyuz programs.

Dunbar, B. J.↗

NASA NTRS1983

Scientific results from the materials processing in space program

Scientific experiments conducted in a low-gravity environment make it possible to study effects, such as surface tension-driven flows, which are often masked by buoyancy-driven flows. A summary is provided of several early experiments which demonstrate that unwanted convective flows can be effectively suppressed in experiments conducted in orbiting spacecraft. Possible applications of low-G processing are discussed, taking into account Bridgman growth of solid solution alloy-type semiconductors, Bridgman growth of eutectic systems, and float-zone crystal growth. The control of macrosegregation and phase separation in castings is considered, giving attention also to containerless melting and solidification. A description of experiment facilities and opportunities is provided.

Naumann, R.↗

NASA NTRS1993

Melt spinning study

Containerless processing of materials provides an excellent opportunity to study nucleation phenomena and produce unique materials, primarily through the formation of metastable phases and deep undercoolings. Deep undercoolings can be readily achieved in falling drops of molten material. Extended solute solubilities and greatly refined microstructures can also be obtained in containerless processing experiments. The Drop Tube Facility at Marshall Space Flight Center has played an important role in enhancing that area of research. Previous experiments performed in the Drop Tube with refractory metals has shown very interesting microstructural changes associated with deep undercoolings. It is apparent also that the microstructure of the deep undercooled species may be changing due to the release of the latent heat of fusion during recalescence. For scientific purposes, it is important to be able to differentiate between the microstructures of the two types of metallic species. A review of the literature shows that although significant advances have been made with respect to the engineering aspects of rapid solidification phenomena, there is still much to be learned in terms of understanding the basic phenomena. The two major ways in which rapid solidification processing provides improved structures and hence improved properties are: (1) production of refined structures such as fine dendrites and eutectics, and (2) production of new alloy compositions, microstructures, and phases through extended solid solubility, new phase reaction sequences, and the formation of metallic-glass microstructures. The objective of this work has been to determine the optimal methodology required to extract this excess energy without affecting the thermo-physical parameters of the under-cooled melt. In normal containerless processing experiments recalescence occurs as the melt returns toward the melting point in order to solidify. A new type of experiment is sought in which the resultant microstructure of the undercooled species is frozen in without going through the melting point regime and subsequent near equilibrium solidification of the remaining liquid. This experimental approach entails the design of an appropriate melt spinning system which is compatible with Drop Tube operations and processing constraints. That work is the goal of this study.

Workman, Gary L.↗

NASA NTRS2003

Investigation of Dynamic Oxygen Adsorption in Molten Solder Jetting Technology

Surface tension forces play a critical role in fluid dynamic phenomena that are important in materials processing. The surface tension of liquid metals has been shown to be very susceptible to small amounts of adsorbed oxygen. Consequently, the kinetics of oxygen adsorption can influence the capillary breakup of liquid-metal jets targeted for use in electronics assembly applications, where low-melting-point metals (such as tin-containing solders) are utilized as an attachment material for mounting of electronic components to substrates. By interpreting values of surface tension measured at various surface ages, adsorption and diffusion rates of oxygen on the surface of the melt can be estimated. This research program investigates the adsorption kinetics of oxygen on the surface of an atomizing molten-metal jet. A novel oscillating capillary jet method has been developed for the measurement of dynamic surface tension of liquids, and in particular, metal melts which are susceptible to rapid surface degradation caused by oxygen adsorption. The experimental technique captures the evolution of jet swells and necks continuously along the jet propagation axis and is used in conjunction with an existing linear, axisymmetric, constant-property model to determine the variation of the instability growth rate, and, in turn, surface tension of the liquid as a function of surface age measured from the exit orifice. The conditions investigated so far focus on a time window of 2-4ms from the jet orifice. The surface properties of the eutectic 63%Sn-37%Pb solder alloy have been investigated in terms of their variation due to O2 adsorption from a N2 atmosphere containing controlled amounts of oxygen (from 8 ppm to 1000 ppm). The method performed well for situations where the oxygen adsorption was low in that time window. The value of surface tension for the 63Sn-37Pb solder in pure nitrogen was found to be 0.49 N/m, in good agreement with previously published work. A characteristic time of O(1ms) or less was determined for the molten-metal surface to be saturated by oxygen at 1000 ppm concentration in N2.

Megaridis, Constantine M.↗

NASA NTRS2003

Effects of Traveling Magnetic Field on Dynamics of Solidification

The Lorentz body force induced in electrically conducting fluids can be utilized for a number of materials processing technologies. An application of strong static magnetic fields can be beneficial for damping convection present during solidification. On the other hand, alternating magnetic fields can be used to reduce as well as to enhance convection. However, only special types of time dependent magnetic fields can induce a non-zero time averaged Lorentz force needed for convection control. One example is the rotating magnetic field. This field configuration induces a swirling flow in circular containers. Another example of a magnetic field configuration is the traveling magnetic field (TMF). It utilizes axisymmetric magnetostatic waves. This type of field induces an axial recirculating flow that can be advantageous for controlling axial mass transport, such as during solidification in long cylindrical tubes. Incidentally, this is the common geometry for crystal growth research. The Lorentz force induced by TMF can potentially counter-balance the buoyancy force, diminishing natural convection, or even setting up the flow in reverse direction. Crystal growth process in presence of TMF can be then significantly modified. Such properties as the growth rate, interface shape and macro segregation can be affected and optimized. Melt homogenization is the other potential application of TMF. It is a necessary step prior to solidification. TMF can be attractive for this purpose, as it induces a basic flow along the axis of the ampoule. TMF can be a practical alloy mixing method especially suited for solidification research in space. In the theoretical part of this work, calculations of the induced Lorentz force in the whole frequency range have been completed. The basic flow characteristics for the finite cylinder geometry are completed and first results on stability analysis for higher Reynolds numbers are obtained. A theoretical model for TMF mixing is also developed. In the experimental part, measurements of flow induced by TMF in a column of mercury (Hg) are presented. Also, an alloy mixing of Bi-Sn of the eutectic composition is demonstrated. A traveling magnetic field of 4mT at 3kHz applied for 120 minutes is found to be sufficient to homogenize an alloy enclosed in a 1cm diameter and 12 cm long tube.

Source record↗