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At least 145 records · Page 8

Solidification of Nb-Ge alloys in long drop tubes

The 30-m and 100 m-long drop tubes at the Marshall Space Flight Center have been used to obtain large undercooling in Nb-Ge alloys. Electron beam melting has been used to obtain drops approximately 2.5 mm in diam. In the 30-m tube, many specimens fell the length of the tube without solidifying, and were ultimately liquid-quenched in oil. The amount of undercooling prior to the quench was usually around 0.13 T(m). In the 100-m tube, freezing generally initiated during free fall, and the maximum undercooling was around 0.22 T(m). Microstructures were characterized by a combination of X-ray diffraction, optical microscopy, and scanning electron microscopy with energy dispersive analysis by X-rays. A variety of interesting microstructures was observed.

Bayuzick, R. J.↗

Initial conditions implied by t exp 1/2 solidification of a sphere with capillarity and interfacial kinetics

The paper explores the initial conditions implied by t exp 1/2 growth of a spherical crystal solidifying from a pure, undercooled melt, including the effects of both capillarity and interface kinetics, and relates the findings to initial conditions that would be expected on the basis of classical nucleation theory. For crystal sizes near the nucleation radius, the calculated temperature profiles show a cold region ahead of the advancing interface that is even more undercooled than the undercooled bath. This cold region acts as a local heat sink that compensates for the reduced growth speed that would otherwise result from capillarity and kinetics, leading to precisely the same t exp 1/2 growth law that would have been obtained had both capillarity and kinetics been neglected.

Sekerka, R. F.↗

The glass transition, crystallization and melting in Au-Pb-Sb alloys

The glass transition, crystallization and melting of Au(55)Pb(22.5)Sb(22.5) alloys have been studied by differential scanning calorimetry DSC. Crystallization on heating above the glass transition temperature Tg (45 C) begins at 64 C. Further crystallization events are observed at 172 C and 205 C. These events were found to correspond to the formation of the intermetallic compounds AuSb2, Au2Pb, and possibly AuPb2, respectively. Isothermal DSC scans of the glassy alloy above Tg were used to monitor the kinetics of crystallization. The solidification behavior and heat capacity in the glass-forming composition range were determined with droplet samples. An undercooling level of 0.3T(L) below the liquidus temperature T(L) was achieved, resulting in crystallization of different stable and metastable phases. The heat capacity C(P) of the undercooled liquid was measured over an undercooling range of 145 C.

Lee, M. C.↗

Analysis of stability of a planar solid-liquid interface in a dilute binary alloy

This paper reconsiders the question of stability of a planar solid-liquid interface in an undercooled alloy melt without making the restrictive assumption of no heat flow in the solid (i.e., Gs = 0). The results of this analysis indicate that, provided the thermal gradient on the solid side of the interface, Gs, is positive, stability can be achieved in an undercooled alloy melt for growth rates R greater than Ra (where Ra is the absolute stability limit of Mullins and Sekerka, 1964). Thus, the absolute stability criterion for steady-state planar growth in an undercooled alloy melt is the same as derived earlier by Mullins and Sekerka for directional solidification. Relaxing the restrictive assumption of Gs = 0 also reveals that there is a regime of stability for low growth rates and low supercoolings.

Laxmanan, V.↗

Dual purpose pyrometer for temperature and solidification velocity measurement

A dual purpose pyrometer is described that allows both accurate radiance temperature measurement and fast temporal response. The system uses two silicon photodiodes with separate optical paths derived from a common spot on the sample. The optical bandwidths and response times of each detection circuit are tailored to the function of each radiometer. The radiance temperature of electromagnetically levitated metallic samples is measured over a narrow optical bandwidth with a high-gain silicon detector. The velocity of solidification of undercooled melts can be deduced from the rise time of the second silicon detector which samples a broad optical bandwidth and has a fast response time. Results from experiments on the undercooling and solidification behavior of electromagnetically levitated pure nickel show that the solidification velocity approaches 17 m/s at high undercooling.

Hofmeister, W. H.↗

Containerless Processing in Reduced Gravity Using the TEMPUS Facility

Containerless processing provides a high purity environment for the study of high-temperature, very reactive materials. It is an important method which provides access to the metastable state of an undercooled melt. In the absence of container walls, the nucleation rate is greatly reduced and undercooling up to (Tm-Tn)/Tm approx. 0.2 can be obtained, where Tm and Tn are the melting and nucleation temperatures, respectively. Electromagnetic levitation represents a method particularly well-suited for the study of metallic melts. The TEMPUS facility is a research instrument designed to perform electromagnetic levitation studies in reduced gravity. It provides temperatures up to 2600 C, levitation of several grams of material and access to the undercooled state for an extended period of time (up to hours).

Roger, Jan R.↗

Microgravity Processing of Oxide Superconductors

Considerable effort has been concentrated on the synthesis and characterization of high T(sub c) oxide superconducting materials. The YBaCuO system has received the most intense study, as this material has shown promise for the application of both thin film and bulk materials. There are many problems with the application of bulk materials- weak links, poor connectivity, small coherence length, oxygen content and control, environmental reactivity, phase stability, incongruent melting behavior, grain boundary contamination, brittle mechanical behavior, and flux creep. The extent to which these problems are intrinsic or associated with processing is the subject of controversy. This study seeks to understand solidification processing of these materials, and to use this knowledge for alternative processing strategies, which, at the very least, will improve the understanding of bulk material properties and deficiencies. In general, the phase diagram studies of the YBaCuO system have concentrated on solid state reactions and on the Y2BaCuO(x) + liquid yields YBa2Cu3O(7-delta) peritectic reaction. Little information is available on the complete melting relations, undercooling, and solidification behavior of these materials. In addition, rare earth substitutions such as Nd and Gd affect the liquidus and phase relations. These materials have promising applications, but lack of information on the high temperature phase relations has hampered research. In general, the understanding of undercooling and solidification of high temperature oxide systems lags behind the science of these phenomena in metallic systems. Therefore, this research investigates the fundamental melting relations, undercooling, and solidification behavior of oxide superconductors with an emphasis on improving ground based synthesis of these materials.

Olive, James R.↗

Mechanisms for the Crystallization of ZBLAN

A number of research teams have observed that glass forming melts that are solidified in low-g exhibit enhanced glass formation. This project will examine one of these glasses, the heavy metal fluoride glass ZBLAN. A four year ground based research program has been approved to examine the crystallization of ZBLAN glasses with the purpose of testing a theory for the crystallization of ZBLAN glass. The theory could explain the general observations of enhanced glass formation of other glasses melted and solidified in low-g. Fluid flow in 1-g results from buoyancy forces and surface tension driven convection. This fluid flow can introduce shear in undercooled liquids in 1-g. In low-g it is known that fluid flows are greatly reduced so that the shear rate in fluids in low-g are extremely low. It is believed that fluids may have some weak structure in the absence of flow. Even very small shear rates could cause this structure to collapse in response to the shear. A general result would be shear thinning of the fluid. The hypothesis of this research is that: Shear thinning in undercooled liquids increases the rate of nucleation and crystallization of glass forming melts. Shear of the melt can be reduced in low-g enhancing undercooling and glass formation. Samples will be melted and quenched in 1-g under quiescent conditions at a number of controlled cooling rates to determine times and temperatures of crystallization and heated at controlled heating rates to determine kinetic crystallization parameters. Experiments will also be performed on the materials while under controlled vibration conditions and compared with the quiescent experiments in order to evaluate the effect of shear in the liquid on crystallization kinetics. After the experimental parameters are well known, experiments will be repeated under low-g (and 2-g) conditions on the KC-135 aircraft during low-g parabolic maneuvers. The results will determine the effects of shear on crystallization. Our experimental setups will be designed with low-g experiments in mind and will be tested as breadboard low-g experiments. It is very likely that the thermal analysis instrumentation can be adapted to be run in the microgravity glovebox facilities. Critical space experiments may result to test the theory at longer low-g time experiments in space.

Ethridge, Edwin C.↗

Adaptive-Grid Methods for Phase Field Models of Microstructure Development

Modeling solidification microstructures has become an area of intense study in recent years. The properties of large scale cast products, ranging from automobile engine blocks to aircraft components and other industrial applications, are strongly dependent on the physics that occur at the mesoscopic and microscopic length scales during solidification. The predominant morphology found in solidification microstructures is the dendrite, a tree-like pattern of solid around which solidification proceeds. The microscopic properties of cast products are determined by the length scales of these dendrites, and their associated segregation profiles. For this reason understanding the mechanisms for pattern selection in dendritic growth has attracted a great deal of interest from the experimental and theoretical communities. In particular, a great deal of research has been undertaken to understand such issues as dendrite morphology, shape and growth speed. Experiments on dendrite evolution in pure materials by Glicksman and coworkers on succinonitrile (SCN), and more recently pivalic acid (PVA), as well as other transparent analogs of metals, have provided tests of theories for dendritic growth, and have stimulated considerable theoretical progress. These experiments have clearly demonstrated that in certain parameter ranges the physics of the dendrite tip can be characterized by a steady value for the dendrite tip velocity, radius of curvature and shape. Away from the tip, the time-dependent dendrite exhibits a characteristic sidebranching as it propagates, which is not yet well understood. These experiments are performed by observing individual dendrites growing into an undercooled melt. The experiments are characterized by the dimensionless undercooling. Most experiments are performed at low undercooling.

Dantzig, Jonathan A.↗

The Role of Convection and Growth Competition in Phase Selection in Microgravity: Controlled Convection in the Containerless Processing of Steel Alloys

Containerless processing using electromagnetic levitation (EML) is a powerful technique in the investigation of reactive molten metal systems. On ground, the power required to overcome the weight of the sample is sufficient to cause significant heating and induce substantial melt convection. In microgravity, the heating and positioning fields may be decoupled and the field strength may be varied to achieve the desired level of convection within the limits set by the geometry of the levitation coil and the sample size. From high-speed digital images of the double recalescence behavior of Fe-Cr-Ni alloys in ground-based testing and in reduced-gravity aboard the NASA KC-135 parabolic aircraft, we have shown that phase selection can be predicted based on a growth competition model. An important parameter in this model is the delay time between primary nucleation and subsequent nucleation of the stable solid within the liquid/metastable solid array. This delay time is a strong function of composition and a weak function of the undercooling of the melt below the metastable liquidus. From the results obtained during the first Microgravity Sciences Laboratory (MSL-1) mission, we also know that convection may significantly influence the delay time, especially at low undercoolings. Currently, it is unclear what mechanism controls the formation of a heterogeneous site that allows nucleation of the austenitic phase on the pre-existing ferrite skeleton. By examining the behavior of the delay time under different convective conditions, we hypothesize that we can differentiate between several of these mechanisms to gain an understanding of how to control microstructural. evolution. We will anchor these predictions by examining samples quenched at different times following primary recalescence in microgravity. A second important parameter in the growth competition model is the identification of the growth rate of the stable phase into the semi-solid array that formed during primary recalescence. Current dendritic growth theory is inadequate in predicting solidification behavior under these conditions as metallographic analyses show that stable phase growth proceeds along the interface between the metastable solid and residual liquid. Since growth velocity is independent of the initial undercooling relative to the metastable liquidus, we hypothesize that purely thermal effects can be separated from other important growth model parameters by careful selection of the liquid composition in a ternary system.

Matson, D. M.↗

The Connection Between Local Icosahedral Order in Metallic Liquids and the Nucleation of Ordered Phases

Over fifty years ago, David Turnbull showed that the temperature of many metallic liquids could be decreased far below their equilibrium melting temperature before crystallization occurred. To explain those surprising results, Charles Frank hypothesized that the local structures of undercooled metallic liquids are different from those of crystal phases, containing a significant degree of icosahedral order that is incompatible with extended periodicity. Such structural differences must create a barrier to the formation crystal phases, explaining the observed undercooling behavior. If true, the nucleation from the liquid of phases with extended icosahedral order should be easier. Icosahedral order is often favored in small clusters, as observed recently in liquid-like clusters of pure Pb on the (111) surface of Si(3), for example. However, it has never been shown that an increasing preference for icosahedral phase formation can be directly linked with the development of icosahedral order in the undercooled liquid. Owing to the combination of very recent advances in levitation techniques and the availability of synchrotron X-ray and high flux neutron facilities.

Kelton, K. F.↗

The Connection Between Local Icosahedral Order in Metallic Liquids and the Nucleation of Ordered Phases

Over fifty years ago, David Turnbull showed that the temperature of many metallic liquids could be decreased far below their equilibrium melting temperature before crystallization occurred. To explain those surprising results, Charles Frank hypothesized that the local structures of undercooled metallic liquids are different from those of crystal phases, containing a significant degree of icosahedral order that is incompatible with extended periodicity. Such structural differences must create a barrier to the formation crystal phases, explaining the observed undercooling behavior. If true, the nucleation from the liquid of phases with extended icosahedral order should be easier. Icosahedral order is often favored in small clusters, as observed recently in liquid-like clusters of pure Pb on the (111) surface of Si, for example. However, it has never been shown that an increasing preference for icosahedral phase formation can be directly linked with the development of icosahedral order in the undercooled liquid. Owing to the combination of very recent advances in levitation techniques and the availability of synchrotron x-ray and high flux neutron facilities, this is shown here.

Curreri, Peter A.↗

Dendritic Growth with Fluid Flow for Pure Materials

We have developed a three-dimensional, adaptive, parallel finite element code to examine solidification of pure materials under conditions of forced flow. We have examined the effect of undercooling, surface tension anisotropy and imposed flow velocity on the growth. The flow significantly alters the growth process, producing dendrites that grow faster, and with greater tip curvature, into the flow. The selection constant decreases slightly with flow velocity in our calculations. The results of the calculations agree well with the transport solution of Saville and Beaghton at high undercooling and high anisotropy. At low undercooling, significant deviations are found. We attribute this difference to the influence of other parts of the dendrite, removed from the tip, on the flow field.

Jeong, Jun-Ho↗

Mechanisms for the Crystallization of ZBLAN

The objective of this ground based study is to test the hypothesis that shear thinning (the non-Newtonian response of viscosity to shear rate) is a viable mechanism to explain the observation of enhanced glass formation in numerous low-g experiments. In 1-g, fluid motion results from buoyancy forces and surface tension driven convection. This fluid flow will introduce shear in undercooled liquids in 1-g. In low-g it is known that fluid flows are greatly reduced so that the shear rate in fluids can be extremely low. It is believed that some fluids may have weak structure in the absence of flow. Very small shear rates could cause this structure to collapse in response to shear resulting in a lowering of the viscosity of the fluid. The hypothesis of this research is that: Shear thinning in undercooled liquids decreases the viscosity, increasing the rate of nucleation and crystallization of glass forming melts. Shear in the melt can be reduced in low-g, thus enhancing undercooling and glass formation. The viscosity of a model glass (lithium di-silicate, L2S) often used for crystallization studies has been measured at very low shear rates using a dynamic mechanical thermal analyzer. Our results are consistent with increasing viscosity with a lowering of shear rates. The viscosity of L2S may vary as much as an order of magnitude depending on the shear rate in the temperature region of maximum nucleation and crystal growth. Classical equations for nucleation and crystal growth rates, are inversely related to the viscosity and viscosity to the third power respectively. An order of magnitude variation in viscosity (with shear) at a given temperature would have dramatic effects on glass crystallization Crystallization studies with the heavy metal fluoride glass ZBLAN (ZrF2-BaF2-LaF3-AlF3-NaF) to examine the effect of shear on crystallization are being initiated. Samples are to be melted and quenched under quiescent conditions at different shear rates to determine the effect on crystallization. The results from this study are expected to advance the current scientific understanding of glass formation in low-g and glass crystallization under glass molding conditions and will improve the scientific understanding of technological processes such as fiber pulling, bulk amorphous alloys, and glass fabrication processes.

Ethridge, Edwin C.↗

Flight Planning for the International Space Station - Levitation Observation of Dendrite Evolution in Steel Ternary Alloy Rapid Solidification (LODESTARS)

During rapid solidification, a molten sample is cooled below its equilibrium solidification temperature to form a metastable liquid. Once nucleation is initiated, growth of the solid phase proceeds and can be seen as a sudden rise in temperature. The heat of fusion is rejected ahead of the growing dendrites into the undercooled liquid in a process known as recalescence. Fe-Cr-Ni alloys may form several equilibrium phases and the hypoeutectic alloys, with compositions near the commercially important 316 stainless steel alloy, are observed to solidify by way of a two-step process known as double recalescence. During double recalescence, the first temperature rise is associated with formation of the metastable ferritic solid phase with subsequent conversion to the stable austenitic phase during the second temperature rise. Selection of which phase grows into the undercooled melt during primary solidification may be accomplished by choice of the appropriate nucleation trigger material or by control of the processing parameters during rapid solidification. Due to the highly reactive nature of the molten sample material and in order to avoid contamination of the undercooled melt, a containerless electromagnetic levitation (EML) processing technique is used. In ground-based EML, the same forces that support the weight of the sample against gravity also drive convection in the liquid sample. However, in microgravity, the force required to position the sample is greatly reduced, so convection may be controlled over a wide range of internal flows. Space Shuttle experiments have shown that the double recalescence behavior of Fe-Cr-Ni alloys changes between ground and space EML experiments. This program is aimed at understanding how melt convection influences phase selection and the evolution of rapid solidification microstructures.

Flemings, Merton C.↗

The Connection Between Local Icosahedral Order in Metallic Liquids and the Nucleation Behavior of Ordered Phases

Over fifty years ago, David Turnbull showed that the temperature of many metallic liquids could be decreased far below their equilibrium melting temperature before crystallization occurred. To explain those surprising results, Charles Frank hypothesized that the local structures of undercooled metallic liquids are different from those of crystal phases, containing a significant degree of icosahedral order that is incompatible with extended periodicity. Such structural differences must create a barrier to the formation crystal phases, explaining the observed undercooling behavior. If true, the nucleation from the liquid of phases with extended icosahedral order should be easier. Icosahedral order is often favored in small clusters, as observed recently in liquid-like clusters of pure Pb on the (111) surface of Si[3], for example. However, it has never been shown that an increasing preference for icosahedral phase formation can be directly linked with the development of icosahedral order in the undercooled liquid. Owing to the combination of very recent advances in levitation techniques and the availability of synchrotron x-ray and high flux neutron facilities, this is shown here.

Kelton, K. F.↗

Surface Tension and Viscosity of Quasicrystal-Forming Ti-Zr-Ni Alloys

The surface tension and viscosity of quasicrystal-forming Ti-Zr-Ni alloys were measured over a range of temperature, including both stable and undercooled liquids by an Electrostatic Levitation (ESL) technique. ESL is a containerless technique which allows processing of samples without contact, greatly reducing contamination and increasing access to the metastable undercooled liquid. The measured viscosity is typical of glass-forming alloys of similar composition to the quasicrystal-forming alloys studied here, while the surface tension shows an anomaly at deep undercoolings.

Hyers, R. W.↗

Containerless Measurement of Thermophysical Properties of Ti-Zr-Ni Alloys

The surface tension, viscosity, density, and thermal expansion of Ti-Zr-Ni alloys were measured for a number of compositions by electrostatic levitation methods. Containerless methods greatly reduce heterogeneous nucleation, increasing access to the undercooled liquid regime at finite cooling rates. The density and thermal expansion are measured optically, while the surface tension and viscosity are measured by the oscillating drop method. The measured alloys include compositions which form a metastable quasicrystal phase from the undercooled liquid, and alloys close to the composition of several multi-component bulk metallic glass-forming alloys. Measurements of surface tension show behavior typical of transition metals at high temperature, but a sudden decrease in the deeply undercooled liquid for alloys near the quasicrystal-forming composition range, but not for compositions which form the solid-solution phase first.

Hyers, Robert↗