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At least 145 records · Page 8

Non-contact temperature measurement of a falling drop

The 105 meter drop tube at NASA-Marshall has been used in a number of experiments to determine the effects of containerless, microgravity processing on the undercooling and solidification behavior of metals and alloys. These experiments have been limited, however, because direct temperature measurement of the falling drops has not been available. Undercooling and nucleation temperatures are calculated from thermophysical properties based on droplet cooling models. In most cases these properties are not well known, particularly in the undercooled state. This results in a large amount of uncertainty in the determination of nucleation temperatures. If temperature measurement can be accomplished then the thermal history of the drops could be well documented. This would lead to a better understanding of the thermophysical and thermal radiative properties of undercooled melts. An effort to measure the temperature of a falling drop is under way. The technique uses two color pyrometry and high speed data acquisition. The approach is presented along with some preliminary data from drop tube experiments. The results from droplet cooling models is compared with noncontact temperature measurements.

Hofmeister, William↗

Phase stability in binary Ti-Al

Binary Ti-Al samples containing from 46 to 54 at. pct Al were solidified while undercooled by various amounts using electromagnetic levitation techniques. A detailed thermal history of these samples was obtained with sampling rates as high as 500 KHz during recalescence. This very high sampling rate was essential to resolve the thermal events. Primary alpha solidification was observed in samples containing from 51 to 54 at. pct Al that were undercooled less than about 100 K at solidification. Primary beta solidification was found for all undercoolings tested in samples containing less than 51 at. pct Al and for undercoolings greater than about 100 K in samples containing 51 to 54 at. pct Al.

Anderson, C. D.↗

Dynamic Nucleation of Supercooled Melts and Measurement of the Surface Tension and Viscosity

We investigate the phenomenon of acoustic pressure-induced nucleation by using a novel approach involving the large amplitude resonant radial oscillations and collapse of a single bubble intentionally injected into a supercooled liquid. Using a combination of previously developed and proven techniques, the bubble is suspended in a fluid host by an ultrasonic field which supplies both the levitation capability as well as the forcing of the radial oscillations. We observe the effects of an increase in pressure (due to bubble collapse) in a region no larger than 100 microns within the supercooled melt to rigorously probe the hypothesis of pressure-induced nucleation of the solid phase. The use of single bubbles operating in narrow temporal and spatial scales will allow the direct and unambiguous correlation between the origin and location of the generation of the disturbance and the location and timing of the nucleation event. In a companion research effort, we are developing novel techniques for the non-contact measurements of the surface tension and viscosity of highly viscous supercooled liquids. Currently used non-invasive methods of surface tension measurement for the case of undercooled liquids generally rely of the quantitative determination of the resonance frequencies of drop shape oscillations, of the dynamics of surface capillary waves, or of the velocity of streaming flows. These methods become quickly ineffective when the liquid viscosity rises to a significant value. An alternate and accurate method which would be applicable to liquids of significant viscosity is therefore needed. We plan to develop such a capability by measuring the equilibrium shape of levitated undercooled melt droplets as they undergo solid-body rotation. The experimental measurement of the characteristic point of transition (bifurcation point) between axisymmetric and two-lobed shapes will be used to calculate the surface tension of the liquid. Such an approach has already been validated through the experimental verification of numerical modeling results. The experimental approach involves levitation, melting, and solidification of undercooled droplets using a hybrid ultrasonic-electrostatic technique in both a gaseous as well as a vacuum environment. A shape relaxation method will be investigated in order to derive a reliable method to measure the viscosity of undercooled melts. The analysis of the monotonic relaxation to equilibrium shape of a drastically deformed and super-critically damped free drop has been used to derive interfacial tension of immiscible liquid combinations where one of the component has high viscosity. A standard approach uses the initial elongation of a droplet through shear flows, but an equivalent method could involve the initial deformation of a drop levitated in a gas by ultrasonic radiation pressure, electric stresses, or even solid body rotation. The dynamic behavior of the free drop relaxing back to equilibrium shape will be modeled, and its characteristic time dependence should provide a quantitative means to evaluate the liquid viscosity.

Trinh, E. H.↗

Real Time Characterization of Solid/Liquid Interfaces During Directional Solidification

A X-Ray Transmission Microscope (XTM) has been developed to observe in real time and in-situ solidification phenomenon at the solid/liquid interface. Recent improvements in the horizontal Bridgman furnace design provides real-time magnification (during solidification) up to 12OX. The increased magnification has enabled for the first time the XTM imaging of real-time growth of fibers and particles with diameters of 3-6 micrometers. Further, morphological transitions from planar to cellular interfaces have also been imaged. Results from recent XTM studies on Al-Bi monotectic system, Al-Au eutectic system and interaction of insoluble particles with s/I interfaces in composite materials will be presented. An important parameter during directional solidification of molten metal is the interfacial undercooling. This parameter controls the morphology and composition at the s/I interface. Conventional probes such as thermocouples, due to their large bead size, do not have sufficient resolution for measuring undercooling at the s/I interface. Further, the intrusive nature of the thermocouples also distorts the thermal field at the s/I interface. To overcome these inherent problems we have recently developed a compact furnace which utilizes a non-intrusive technique (Seebeck) to measure undercooling at the S/I interface. Recent interfacial undercooling measurements obtained for the Pb-Sn system will be presented. The Seebeck measurement furnace in the future will be integrated with the XTM to provide the most comprehensive tool for real time characterization of s/I interfaces during solidification.

Sen, S.↗

A Real Time Investigation of Morphological Evolution During Solidification of Different Alloy Systems

Solidification phenomenon which occur at the solid/liquid (s/I) interface play a major role in the determination of structure and hence the technologically important properties of a casting. However, metals being opaque, conclusions related to several important phenomenon such as boundary layer thickness, morphological evolution, and eutectic and cell spacing are deduced from quenching experiments and subsequent post solidification metallographic analysis. Consequently, limited information is obtained about the dynamics of the process. This paper will discuss the recent efforts at the Space Science Laboratory, NASA Marshall Space Flight Center, to view and quantify in-situ and in real time the dynamics of the solidification process and to measure interfacial undercooling. First, a high resolution x-ray transmission microscope (XTM) has been developed to monitor fundamental interfacial phenomena during directional solidification of metals and alloys. The XTM operates in the range of 10-100 KeV and through projection is capable of achieving magnification of up to 16OX. Secondly, an innovative collapsible furnace has been designed to quantify interfacial undercooling by measuring the temperature of a moving s/I interface in reference to a fixed s/l interface. This measurement technique is non-intrusive in nature and is based on the Seebeck principle. In this paper real time results obtained to characterize the dynamics of irregular eutectic spacing will be presented. As an example fiber to lamella or plate transition in the Al-Al2Au eutectic system will be discussed. Further, a resolution limit of 25 micron has permitted viewing in real time morphological instability and cellular growth in Al-Au and Al-Ag systems. Simultaneously, a systematic investigation has been carried out to measure interfacial undercooling for Pb-1 wt.% Sn at and near the marginal stability regime. In conjunction with the XTM observations this study attempts to validate existing relationships between undercooling and growth velocity during plane front growth, marginal stability regime, and stable cellular growth.

Sen, S.↗

NASA MSFC Electrostatic Levitator (ESL) Rapid Quench System

Electrostatic levitation, a form of containerless processing, is an important tool in materials research. Levitated specimens are free from contact with a container; therefore, heterogeneous nucleation on container walls is not possible. This allows studies of deeply undercooled melts. Furthermore, studies of high‐temperature, highly reactive materials are also possible. Studies of the solidification and crystallization of undercooled melts is vital to the understanding of microstructure development, particularly the formation of alloys with unique properties by rapid solidification. The NASA Marshall Space Flight Center (MSFC) Electrostatic Levitator (ESL) lab has recently been upgraded to allow for rapid quenching of levitated materials. The ESL Rapid Quench System uses a small crucible‐like vessel that can be partially filled with a low melting point material, such as a Gallium alloy, as a quench medium. An undercooled sample can be dropped into the vessel to rapidly quench the sample. A carousel with nine vessels sits below the bottom electrode assembly. This system allows up to nine rapid quenches before having to break vacuum and remove the vessels. This new Rapid Quench System will allow materials science studies of undercooled materials and new materials development. In this presentation, the system is described and initial results are presented.

SanSoucie, Michael P.↗

The effect of phosphorus on the formation of the Widmanstaetten pattern in iron meteorites.

Use of a combination of a revised Fe-Ni-P phase diagram and laboratory cooling experiments on Fe-Ni-P alloys to determine the effect of P on the formation of the Widmanstaetten pattern. From the phase diagram results, two reaction paths were found for the formation of kamacite (1) gamma (taenite) yields alpha (kamacite) + gamma (taenite) and (2) gamma yields gamma + Ph /phosphide, (FeNi)3P/ yields alpha + gamma + Ph. The reaction path gamma yields alpha + gamma is preferred at low P contents, while at higher P contents and at Ni contents greater than 7.0 wt.%, the reaction path gamma yields gamma + Ph yields alpha + gamma + Ph controls the formation of kamacite. Above 7 wt.% Ni, the effect of P on the equilibrium nucleation temperature of kamacite is quite small, less than about plus or minus 30 C with respect to the Fe-Ni binary diagram. The addition of P (greater than 0.1 wt.%) to meteorites promotes nucleation of kamacite at higher temperatures and effectively lowers the amount of undercooling necessary to nucleate kamacite homogeneously. Ni has just the opposite effect, decreasing the temperature of nucleation and increasing the amount of undercooling. It is concluded that significant amounts of undercooling, 50 to 100 C, are necessary for the nucleation of the Widmanstaetten structure in meteorites, and that chemical equilibrium is maintained in the various phases of slowly cooled iron meteorites to 650 C and probably to 600 C.

Goldstein, J. I.↗

Containerless processing of Nb-Ge alloys in a long drop tube

The thirty-two meter drop tube at the Marshall Space Flight Center was used to study the effect of zero gravity containerless processing on the structure and properties of materials. The concept involves the suppression of heterogeneous nucleation of solid in liquid and, therefore, solidification accompanied by large degrees of undercooling. Under these conditions metastable phases can be formed or, at the very least, unique nonequilibrium microstructures (containing equilibrium phases) with unique properties can be produced. The drop tube solidification was applied to niobium base alloys with emphasis on the Nb-Ge binary system in an effort to produce metastable phases with high superconducting transition temperatures in bulk specimens. In the past, only lower Ge alloys (Nb-13 a/o, Nb-18 a/o, and Nb-22 a/o) could be undercooled. Higher Ge alloys (e.g., Nb-25 a/o Ge and Nb-27 a/o Ge) can now be undercooled on a routine basis.

Bayuzick, R. J.↗

A review of long drop tubes as a supplement/alternative to space experiments

A description of the 100-m drop tube at the Marshall Space Flight Center is presented, along with some undercooling observations and a discussion of some microstructural properties of deeply undercooled Nb-Ge alloys. The facility comprises two turbopumps which can evacuate the tube to 0.00001 torr, and three IR detectors at 15, 80, and 103-m levels which are sensitive to light in the range of 9660-2635 K (wavelength range of 0.2 to 1.1 microns), though recalescence events were detected at 1700 K. Finally, hypercooling regimes and maximum possible undercooling in vacuum are defined for several materials, including Al, Cu, Ni, Fe, Pt, and Nb.

Bayuzick, R. J.↗

Dendritic solidification. III - Some further refinements to the model for dendritic growth under an imposed thermal gradient

Some further refinements to a simple model for dendritic solidification in a binary alloy melt under an imposed positive thermal gradient are presented. Two new expressions for the dendrite tip undercooling have been obtained and shown to yield a limiting value of Delta T sub 0 and very small growth rates. Here Delta T sub 0 is the equilibrium solidification range of the alloy. At very large growth rates, all three tip undercooling expressions reach the same limiting value depending on the value of a dimensionless parameter lambda which is related to the effective diffusion distance ahead of the dendrite tip. The predicted tip undercoolings are, however, somewhat lower at intermediate growth rates. An improved calculation for the solute buildup at the dendrite tip due to curvature effects is also included.

Laxmanan, V.↗

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.↗