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Process modelling for materials preparation experiments

The main goals of the research under this grant consist of the development of mathematical tools and measurement techniques for transport properties necessary for high fidelity modelling of crystal growth from the melt and solution. Of the tasks described in detail in the original proposal, two remain to be worked on: development of a spectral code for moving boundary problems, and development of an expedient diffusivity measurement technique for concentrated and supersaturated solutions. We have focused on developing a code to solve for interface shape, heat and species transport during directional solidification. The work involved the computation of heat, mass and momentum transfer during Bridgman-Stockbarger solidification of compound semiconductors. Domain decomposition techniques and preconditioning methods were used in conjunction with Chebyshev spectral methods to accelerate convergence while retaining the high-order spectral accuracy. During the report period we have further improved our experimental setup. These improvements include: temperature control of the measurement cell to 0.1 C between 10 and 60 C; enclosure of the optical measurement path outside the ZYGO interferometer in a metal housing that is temperature controlled to the same temperature setting as the measurement cell; simultaneous dispensing and partial removal of the lower concentration (lighter) solution above the higher concentration (heavier) solution through independently motor-driven syringes; three-fold increase in data resolution by orientation of the interferometer with respect to diffusion direction; and increase of the optical path length in the solution cell to 12 mm.

Rosenberger, Franz↗

Preliminary flight results from the second U.S. Microgravity Payload (USMP-2)

The second U.S. Microgravity Payload (USMP-2) was flown on the Space Shuttle in March 1994. It carried four major microgravity experiments plus a sophisticated accelerometer system to record the microgravity environment during USMP-2 operations. The USMP program is designed to accommodate experiments requiring extensive resources short of a full Spacelab mission, and the experiments are remotely operated and monitored. Results are reviewed from the four experiments: the Advanced Automated Directional Solidification Facility (AADSF), the Isothermal Dendrite Growth Experiment (IDGE), the Materiel por Etude des Phenomenes Interessant la Soldification sur Terre et en Orbite (MEPHISTO), and the Critical Fluid Light Scattering Experiment (Zeno). AASDF grew what is expected to be the largest steady-state sample ever of HgCdTe during 240 hours of operation. IDGE provided 60 growth cycles over a wide range of supercooling conditions studying the dendritic solidification of succinonitrile. MEPHISTO achieved 55 melt-solidify cycles and grew over 1 m of Bi/Sn alloy. Zeno located the critical point temperature for liquid Xe to 0.00001 K. IDGE and Zeno also provided the most extensive demonstrations to date of telescience.

Curreri, Peter↗

The study of dopant segregation behavior during the growth of GaAs in microgravity

An investigation into the segregation behavior of selenium doped gallium arsenide during directional solidification in the microgravity environment was conducted using the Crystal Growth Furnace (CGF) aboard the first United States Microgravity Laboratory (USML-1). The two crystals grown were 1.5 cm in diameter and 16.5 cm in length with an initial melt length of 14 cm. Two translation periods were executed, the first at 2.5 microns/s and after a specified time, which was different between the two experiments, the translation rate was doubled to 5.0 microns/s. The translation was then stopped and the remaining sample melt was solidified using a gradient freeze technique in the first sample and a rapid solidification in the second experiment. Measurement of the selenium dopant distribution, using quantitative infrared transmission imaging, indicates that the first sample initially achieved diffusion controlled growth as desired. However, after about 1 cm of growth, the segregation behavior was driven from a diffusion controlled growth regime to a complete mixing regime. Measurements in the second flight sample indicated that the growth was always in a complete mixing regime. In both experiments, voids in the center line of the crystal, indicative of bubble entrapment, were found to correlate with the position in the crystal when the translation rates were doubled.

Matthiesen, David H.↗

AMCC casting development. Volume 1: Executive Summary

The Advanced Combustion Chamber Casting (AMCC) has been a technically challenging part due to its size, configuration, and alloy type. The height and weight of the wax pattern assembly necessitated the development of a hollow gating system to ensure structural integrity of the shell throughout the investment process. The complexity in the jacket area of the casting required the development of an innovative casting technology that PCC has termed 'TGC' or Thermal Gradient Control. This method, of setting up thermal gradients in the casting during solidification, represents a significant process improvement for PCC and has been successfully implemented on other programs. Metallurgical integrity of the final four castings was very good. Only the areas of the parts that utilized 'TGC Shape & Location System #2' showed any significant areas of microshrinkage when evaluated by non-destructive tests. Alumina oxides detected by FPI on the 'float' surfaces (top sid surfaces of the casting during solidification) of the part were almost entirely less than the acceptance criteria of .032 inches in diameter. Destructive chem mill of the castings was required to determine the effect of the process variables used during the processing of these last four parts (with the exception of the 'Shape & Location of TGC' variable).

Source record↗

Magnetic fields of the terrestrial planets

The four terrestrial planets, together with the Earth's Moon, provide a significant range of conditions under which dynamo action could occur. All five bodies have been visited by spacecraft, and from three of the five bodies (Earth, Moon and Mars) we have samples of planetary material upon which paleomagnetic studies have been undertaken. At the present time, only the Earth and Mercury appear to have a significant dipole magnetic field. However, the Moon, and possibly Mars, appear to have had ancient planetary dynamos. Venus does not now have a significant planetary magnetic field, and the high surface temperatures should have prevented the recording of evidence of any ancient magnetic field. Since the solidification of the solid inner core is thought to be the energy source for the terrestrial magnetic field, and since smaller bodies evolve thermally more rapidly than larger bodies, we conjecture that the terrestrial planets are today in three different phases of magnetic activity. Venus is in a predynamo phase, not having cooled to the point of core solidification. Mercury and the Earth are in the middle of their dynamo phase, with Mercury perhaps near the end of its activity. Mars and the Moon seem to be well past their dynamo phase. Much needs to be done in the study of the magnetism of the terrestrial planets. We need to characterize the multipole harmonic structure of the Mercury magnetic field plus its secular variation, and we need to analyze returned samples to attempt to unfold the long-term history of Mercury's dynamo. We need to more thoroughly map the magnetism of the lunar surface and to analyze samples obtained from a wider area of the lunar surface. We need a more complete survey of the present Martian magnetic field and samples from a range of different ages of Martian surface material. Finally, a better characterization of the secular variation of the terrestrial magnetic field is needed in order to unfold the workings of the terrestrial dynamo.

Russell, C. T.↗

Reply

Treiman (this issue) argues that the melting temperature of carbonatite used by Gregg and Greeley (1993) is too low, and that values presented for other thermophysical properties for carbonatite lava are more appropriate for carbonatite rock. With the exception of the mechanical solidification temperature, values presented by Gregg and Greeley (1993) were taken directly, or calculated, from values presented within the works by Dawson et al. (1990) and Keller and Krafft (1990). Because a mechanical solidification temperature for carbonatite lavas was not presented in those works, we estimated one based on extrusion temperature, Venusian surface pressure, and the temperatures measured in cooling carbonatite lava lakes. We have reexamined values shown for properties of carbonatite lavas used by Gregg and Greeley (1993), and concur that Treiman's arguments (Treiman, this issue) are valid. Here, we present results of analyses described in Gregg and Greeley 1993, using values for the properties of carbonatite lavas obtained from Treiman and Schedl (1983) and Norton and Pinkerton (1990).

Gregg, Tracy K. P.↗

Convective and morphological instabilities during crystal growth: Effect of gravity modulation

During directional solidification of a binary alloy at constant velocity in the vertical direction, morphological and convective instabilities may occur due to the temperature and solute gradients associated with the solidification process. The effect of time-periodic modulation (vibration) is studied by considering a vertical gravitational acceleration which is sinusoidal in time. The conditions for the onset of solutal convection are calculated numerically, employing two distinct computational procedures based on Floquet theory. In general, a stable state can be destabilized by modulation and an unstable state can be stabilized. In the limit of high frequency modulation, the method of averaging and multiple-scale asymptotic analysis can be used to simplify the calculations.

Coreill, S. R.↗

Non-linear resonance of fluids in a crystal growth cavity

In the microgravity environment, the effect of gravity on fluid motion is much reduced. Hence, secondary effects such as vibrations, jitters, surface tension, capillary effects, and electromagnetic forces become the dominant mechanism of fluid convection. Numerous studies have been conducted to investigate fluid behavior in microgravity with the ultimate goal of developing processes with minimal influence from convection. Industrial applications such as crystal growth from solidification of melt and protein growth for pharmatheutical application are just a few examples of the vast potential benefit that can be reaped from material processing in space. However, a space laboratory is not immune from all undesirable disturbances and it is imperative that such disturbances be well understood, quantifiable, and controlled. Non-uniform and transient accelerations such as vibrations, jitters, and impulsive accelerations exist as a result of crew activities, space vehicle maneuvering, and the operations of on-board equipment. Measurements conducted on-board a U.S. Spacelab showed the existence of vibrations in the frequency range of 1 to 100 Hz with a dominant mode of 17 Hz and harmonics of 54 Hz. The observed vibration is not limited to any coordinate plane but exists in all directions. Similar situation exists on-board the Russian MIR space station. Due to the large structure of its design, the future International Space Station will have its own characteristic vibration spectrum. It is well known that vibration can exert substantial influence on heat and mass transfer processes, thus hindering any attempts to achieve a diffusion-limited process. Experiments on vibration convection for a liquid-filled enclosure under one-g environment showed the existence of different flow regimes as vibration frequency and intensity changes. Results showed the existence of a resonant frequency, near which the enhancement is the strongest, and the existence of a high frequency asymptote. Numerical simulations of vibration convection have been conducted by Yurkov, Fu and Shieh, and by Wang. These analyses considered a two-dimensional air-filled cell under weightlessness condition and showed results similar to those of the experiments. It is not yet known whether resonance convection can be triggered by jitter alone or whether it requires the interaction of jitter with other convective forces in low gravity. An order of magnitude analysis, however, can be used to show the dependence of the resonance frequency on the fluid Prandtl number. Even though the onset of resonance convection may depend on other factors, results indicates that fluids with low Prandtl numbers are more susceptible to resonance than those with high Prandtl numbers. The current study is aimed at gaining additional insights to this problem using germanium as working fluid. Germanium was chosen for this analysis because of its common usage in solidification process and its relatively low Prandtl number (Pr = 0.02).

Wang, Francis C.↗

STS-75 Flight Day 1

On this first day of the STS-75 mission, the flight crew, Cmdr. Andrew Allen, Pilot Scott Horowitz, Payload Cmdr. Franklin Chang-Diaz, Payload Specialist Umberto Guidoni (Italy), and Mission Specialists Jeffrey Hoffman, Maurizio Cheli (ESA) and Claude Nicollier (ESA), were shown performing pre-launch and launching activities. This international space mission's primary objective is the deployment of the Tethered Satellite System Reflight (TSS-1R) to a 12 mile length from the shuttle, a variety of experiments, and the satellite retrieval. These experiments include: Research on Orbital Plasma Electrodynamics (ROPE); TSS Deployer Core Equipment and Satellite Core Equipment (DCORE/SCORE); Research on Electrodynamic Tether Effects (RETE); Magnetic Field Experiments for TSS Missions (TEMAG); Shuttle Electrodynamic Tether Systems (SETS); Shuttle Potential and Return Electron Experiment (SPREE); Tether Optical Phenomena Experiment (TOP); and Observations at the Earth's Surface of Electromagnetic Emissions by TSS (OESSE). The mission's secondary objectives were those experiments found in the United States Microgravity Payload-3 (USMP-3), which include: Advanced Automated Directional Solidification Furnace (AADSF); Material pour l'Etude des Phenomenes Interessant la Solidification sur Terre et en Orbite (MEPHISTO); Space Acceleration Measurement System (SAMS); Orbital Acceleration Research Experiment (OARE); Critical Fluid Scattering Experiment (ZENO); and Isothermal Dendritic Growth Experiment (IDGE).

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Shear Stabilization of a Solidifying Front

The manufacturing of multi-component single crystals with uniform material properties is frequently hampered by the presence of morphological instabilities during the solidification. We discuss the influence of shear flows on the linear and nonlinear stability of the solid/liquid interface during the directional solidification of binary alloys. The flows are generated by nonplanar harmonic translations of the crystal parallel to the mean interface position. Oscillations with physically realizable amplitudes and frequencies are found useful for stabilization purposes.

Davis, Stephen H.↗

Nonlinear Convection in Mushy Layers

When alloys solidify in a gravitational field there are complex interactions between solidification and natural, buoyancy-driven convection that can alter the composition and impair the structure of the solid product. The particular focus of this project has been the compositional convection within mushy layers that occurs in situations where the lighter component of the alloy is rejected into the melt during solidification by cooling from below. The linear stability of such a situation was previously described and has been further elucidated in a number of published articles. Here we describe some recent developments in the study of nonlinear evolution of convection in mushy layers.

Worster, M. Grae↗

NiAl-based Polyphase in situ Composites in the NiAl-Ta-X (X = Cr, Mo, or V) Systems

Polyphase in situ composites were generated by directional solidification of ternary eutectics. This work was performed to discover if a balance of properties could be produced by combining the NiAl-Laves phase and the NiAl-refractory metal phase eutectics. The systems investigated were the Ni-Al-Ta-X (X = Cr, Mo, or V) alloys. Ternary eutectics were found in each of these systems and the eutectic composition, temperature, and morphology were determined. The ternary eutectic systems examined were the NiAl-NiAlTa-(Mo, Ta), NiAl-(Cr, Al) NiTa-Cr, and the NiAl-NiAlTa-V systems. Each eutectic consists of NiAl, a C14 Laves phase, and a refractory metal phase. Directional solidification was performed by containerless processing techniques in a levitation zone refiner to minimize alloy contamination. Room temperature fracture toughness of these materials was determined by a four-point bend test. Preliminary creep behavior was determined by compression tests at elevated temperatures, 1100-l400 K. Of the ternary eutectics, the one in the NiAl-Ta-Cr system was found to be the most promising. The fracture toughness of the NiAl-(Cr, Al)NiTa-Cr eutectic was intermediate between the values of the NiAl-NiAlTa eutectic and the NiAl-Cr eutectic. The creep strength of this ternary eutectic was similar to or greater than that of the NiAl-Cr eutectic.

Johnson, D. R.↗

Design of a High Thermal Gradient Bridgman Furnace

The Advanced Automated Directional Solidification Furnace (AADSF) is a Bridgman-Stockbarger microgravity processing facility, designed and manifested to first fly aboard the second United States Microgravity Payload (USMP-2) Space Shuttle mission. The AADSF was principally designed to produce high axial thermal gradients, and is particularly suitable for metals solidification experiments, including non-dilute alloys. To accommodate a wider range of experimental conditions, the AADSF is equipped with a reconfigurable gradient zone. The overall design of the AADSF and the relationship between gradient zone design and furnace performance are described. Parametric thermal analysis was performed and used to select gradient zone design features that fulfill the high thermal gradient requirements of the USMP-2 experiment. The thermal model and analytical procedure, and parametric results leading to the first flight gradient zone configuration, are presented. Performance for the USMP-2 flight experiment is also predicted, and analysis results are compared to test data.

LeCroy, J. E.↗

Thermal Problems in Material processing of High-Temperature Materials

In this final report axial segregation in unsteady diffusion dominated directional solidification of a binary alloy with a planar solid-liquid interface profile is considered. The analysis is an extension of the work of Smith et al. to account for an arbitrary initial axial concentration profile. This situation is important in the experimental studies of growth of crystals in a microgravity environment in which the growth is from melts formed by re-melting crystals that have a known axial impurity profile. Three situations are discussed. There are the initial transient, a re-solidified crystal, and multipass solidification.

Korpela, Seppo A.↗

Advanced Gradient Heating Facility (AGHF)

This section of the publication includes papers entitled: (1) Coupled growth in hypermonotectics; (2) Directional solidification of refined Al-4 wt.% Cu alloys; (3) Effects of convection on interface curvature during growth of concentrated ternary compounds; (4) Directional solidification of Al-1.5 wt.% Ni alloys; (5) Interactive response of advancing phase boundaries to particles; (6) INTeractive Response of Advancing Phase boundaries to Particles-INTRAPP; and (7) Particle engulfment and pushing by solidifying interfaces.

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The Effect of Microgravity Direction on the Growth of PbSnTe

The Space Shuttle Columbia was launched as STS-75 at 2018 GMT (Greenwich Mean Time) on February 22, 1996. One of the two major experiment packages was the Third United States Microgravity Payload (USMP-3), and one of the principal instruments on the USMP was the Advanced Automated Directional Solidification Furnace (AADSF). The AADSF is a multizone directional solidification furnace, and at the time of the USMP-3 flight was capable of processing only one sample per Shuttle mission which, for that flight, was a lead tin telluride (PbSnTe) crystal growth experiment. In the one year since the flight experiment the sample has been retrieved from the spacecraft and analysis has begun. After presenting introductory material on why PbSnTe was chosen as a test material, why microgravity processing was expected to produce desired results, and what we expected to find in conducting these tests, this report discusses the results to date which are far from complete.

Fripp, A. L.↗

Adaptive-Grid Methods for Phase Field Models of Microstructure Development

In this work the authors show how the phase field model can be solved in a computationally efficient manner that opens a new large-scale simulational window on solidification physics. Our method uses a finite element, adaptive-grid formulation, and exploits the fact that the phase and temperature fields vary significantly only near the interface. We illustrate how our method allows efficient simulation of phase-field models in very large systems, and verify the predictions of solvability theory at intermediate undercooling. We then present new results at low undercoolings that suggest that solvability theory may not give the correct tip speed in that regime. We model solidification using the phase-field model used by Karma and Rappel.

Provatas, Nikolas↗

The Isothermal Dendritic Growth Experiment (IDGE)

The Isothermal Dendritic Growth Experiment (IDGE) constituted a series of three NASA-supported microgravity experiments, all of which flew aboard the space shuttle, Columbia. This experimental space flight series was designed and operated to grow and record dendrite solidification in the absence of gravity-induced convective heat transfer, and thereby produce a wealth of benchmark-quality data for testing solidification scaling laws. The data and analysis performed on the dendritic growth speed and tip size in Succinontrie (SCN) demonstrates that although the theory yields predictions that are reasonably in agreement with experiment, there are significant discrepancies. However, some of these discrepancies can be explained by accurately describing the diffusion of heat. The key finding involves recognition that the actual three-dimensional shape of dendrites includes time-dependent side-branching and a tip region that is not a paraboloid of revolution. Thus, the role of heat transfer in dendritic growth is validated, with the caveat that a more realistic model of the dendrite then a paraboloid is needed to account for heat flow in an experimentally observed dendrite. We are currently conducting additional analysis to further confirm and demonstrate these conclusions. The data and analyses for the growth selection physics remain much less definitive. From the first flight, the data indicated that the selection parameter, sigma*, is not exactly a constant, but exhibits a slight dependence on the supercooling. Additional data from the second flight are being examined to investigate the selection of a unique dendrite speed, tip size and shape. The IDGE flight series is now complete. We are currently completing analyses and moving towards final data archiving. It is gratifying to see that the IDGE published results and archived data sets are being used actively by other scientists and engineers. In addition, we are also pleased to report that the techniques and IDGE hardware system that the authors developed with NASA, are being currently employed on both designated flight experiments, like EDSE, and on flight definition experiments, like TDSE.

Glicksman, Martin E.↗