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At least 127 records · Page 7

Characterization of Dendritic Spatially Extended 3D Patterns in Directional Solidification: Microgravity Experiments in DECLIC-DSI onboard ISS and 3D Phase-field Simulations

To clarify and characterize the fundamental physical mechanisms active in the dynamical formation of three-dimensional (3D) arrays of dendrites under diffusive growth conditions, in situ monitoring of series of experiments on transparent model alloy succinonitrile – 0.46 wt% camphor was carried out under low gravity in the DECLIC Directional Solidification Insert onboard the International Space Station. These experiments offer the very unique opportunity to observe in situ and characterize the dynamics of the microstructure formation and evolution in extended 3D patterns under microgravity environment. The analyses of the dendritic patterns for a broad range of growth velocities displaying different levels of sidebranching will be presented. Especially, the time evolution of primary spacing, in case of solidifications at constant pulling rate as well as for experiments with pulling rate jump, will be compared to 3D phase-field simulations, and the results will be discussed in terms of stable spacing range.

Kaihua Ji

Characterization of Dendritic Spatially Extended 3D Patterns in Directional Solidification: Microgravity Experiments in DECLIC-DSI Onboard ISS and 3D Phase-field Simulations

To clarify and characterize the fundamental physical mechanisms active in the dynamical formation of three-dimensional (3D) arrays of dendrites under diffusive growth conditions, in situ monitoring of series of experiments on transparent model alloy succinonitrile – 0.46 wt% camphor was carried out under low gravity in the DECLIC Directional Solidification Insert onboard the International Space Station. These experiments offer the very unique opportunity to observe in situ and characterize the dynamics of the microstructure formation and evolution in extended 3D patterns under microgravity environment. The analyses of the dendritic patterns for a broad range of growth velocities displaying different levels of sidebranching will be presented. Especially, the time evolution of primary spacing, in case of solidifications at constant pulling rate as well as for experiments with pulling rate jump, will be compared to 3D phase-field simulations, and the results will be discussed in terms of stable spacing range.

Kaihua Ji

Conditions Of Directional Solidification Affect Superalloy

Report describes experiments to determine effects of gradient of temperature and rate of solidification on microstructure and fatigue properties of nickel-based superalloy MAR-M246(Hf). Enhancement of properties extends lifespans of objects, including turbo-pump blades of Space Shuttle Main Engines. Results indicate significant improvements in fatigue properties derived through manipulation of parameters of directional solidification. Particularly MAR-M246(Hf) for turbine blades contains small, well-dispersed blocky carbide and microstructure with small distances between dendrite arms, and without eutectic phase.

Schmidt, D. D.

From irregular to regular eutectic growth in the Al-Al 3 Ni system: In situ observations during directional solidification

Here we investigate the irregular eutectic growth dynamics of the Al-Al 3 Ni alloy, in which one of the solid phases (Al 3 Ni) grows faceted from the liquid. Leveraging in situ optical microscopy and synchrotron transmission x-ray microscopy, we address the question of the degree of coupling between Al and Al 3 Ni at the growth front and that of the shape of the microstructures left behind in the bulk solid during directional solidification. Real-time optical observations bring evidence for a morphological transition from a eutectic-grain dependent, irregular eutectic growth at low solidification velocity V (typically 1 μm s -1 ), to a weakly anisotropic, regular growth at higher V ( reaching 10 μm s -1 ). Unprecedented x-ray nano-imaging of the solid–liquid interface, and 3D characterization of the growth patterns, were made possible by a new DS setup at Brookhaven National Laboratory’s NSLS-II. At low V, the leading tips of partly faceted Al 3 Ni crystals are observed to grow not far ahead of the Al growth front. Correlating in situ images and postmortem 3D tomographic reconstructions reveals that the presence of faceted and non-faceted regions of Al 3 Ni crystals in the solid is a direct consequence of coupling and decoupling during DS, respectively. Upon increasing V, the lead distance of Al 3 Ni vanishes, and the shape of Al 3 Ni ceases to be governed by faceted growth. These observations cast light onto the basic mechanisms (faceted growth, diffusive coupling, and the dynamics of trijunctions) governing a faceted to rod-like transition upon increasing V in the Al 3 Ni system, with broad implications to a large class of irregular eutectics.

36 MATERIALS SCIENCE

Characterization of the general purpose research furnace for low-G directional solidification experiments

Preliminary tests have shown that it is possible to control the temperature settings in NASA's General Purpose Research Furnace in such a manner as to obtain a constant rate of movement of a high temperature isotherm down the length of the furnace. These tests also showed that a temperature gradient on the order of 40 deg cm could be obtained in the furnace while moving the particular isotherm of interest, i.e., 900 C. This provides the possibility of performing directional solidification experiments in the furnace on a MEA flight in the low gravity environment provided by the Shuttle. A functional dependency of growth rate on perturbations during the the growth has been derived and shows the importance of avoiding non-steady growth rates and changing temperature gradients.

Crouch, R. K.

Directional Solidification of Mercury Cadmium Telluride During the Second United States Microgravity Payload Mission (USMP-2)

As a solid solution semiconductor having, a large separation between liquidus and solidus, mercury cadmium telluride (MCT) presents a formidable challenge to crystal growers desiring an alloy of high compositional uniformity. To avoid constitutional supercooling during Bridgman crystal growth it is necessary to solidify slowly in a high temperature gradient region. The necessary translation rate of less than 1 mm/hr results in a situation where fluid flow induced by gravity on earth is a significant factor in material transport. The Advanced Automated Directional Solidification Furnace (AADSF) is equipped to provide the stable thermal environment with a high gradient, and the required slow translation rate needed. Ground based experiments in AADSF show clearly the dominance of flow driven transport. The first flight of AADSF in low gravity on USMP-2 provided an opportunity to test theories of fluid flow in MCT and showed several solidification regimes which are very different from those observed on earth. Residual acceleration vectors in the orbiter during the mission were measured by the Orbital Acceleration Research Experiment (OARE), and correlated well with observed compositional differences in the samples.

Gillies, D. C.

Modeling of Ultrasonically Generated Liquid-Liquid Dispersions During Controlled Directional Solidification

There are innumerable two-component systems in which two very different liquid phases co-exist in equilibrium over a range of temperature and composition, e.g., oil and water, salt fluxes and solders, aluminum and lead. Often it is of practical concern to fabricate a solid component consisting of a uniform dispersion of one phase in the other. Unfortunately, uniform microstructural development during solidification of two immiscible liquids is hampered by inherent, often large, density differences between the phases that lead to severe segregation. Uniformity is also compromised by preferential wetting and coalescence phenomena. It is, however, well known that ultrasonic energy can initiate and maintain a fine liquid-liquid dispersion. The work presented here extends that observation by application of ultrasonic energy to promote uniform phase incorporation during controlled directional solidification. To this end experiments with the transparent organic, immiscible, succinonitrile-glycerol system were conducted and the numerous processing parameters associated with this technique were evaluated in view of optimizing dispersion uniformity. In view of the initial experimental results a model that predicts the dispersed liquid droplet size as a function of material properties, sample geometry, and applied energy has been developed. In the mathematical model we consider the ultrasonic field in an experimental ampoule of length L and diameter D induced by a probe having a vibration frequency of f=2OKhz (circular frequency omega = 2 pi f). The amplitude is adjustable from A=65 to 13Omicrons. The probe tip diameter is d, the liquid has a density of p, in which the speed of sound and surface tension are, respectively, c and sigma. The mathematical model and numerical investigation for the experiments [1] is done using the following assumptions: (i) The droplet size is small in comparison to the sound wave length; (ii) The forces between droplets are neglected (relative concentration is small); (iii) The droplet is stable if the kinetic energy, E(sub K), of the liquid motion due to ultrasonic field influence is less then the binding energy, E(sub S), due to the surface tension (it is easy to show that the surface energy of two droplets resulting from one is larger by about a factor of two.); (iv) The stability limit is characterized by E(sub S) to approx. E(sub K).

Grugel, R. N.

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.

Three-Dimensional Stereoscopic Tracking Velocimetry and Experimental/Numerical Comparison of Directional Solidification

Measurement of three-dimensional (3-D) three-component velocity fields is of great importance in both ground and space experiments for understanding materials processing and fluid physics. The experiments in these fields most likely inhibit the application of conventional planar probes for observing 3-D phenomena. Here, we present the investigation results of stereoscopic tracking velocimetry (STV) for measuring 3-D velocity fields, which include diagnostic technology development, experimental velocity measurement, and comparison with analytical and numerical computation. STV is advantageous in system simplicity for building compact hardware and in software efficiency for continual near-real-time monitoring. It has great freedom in illuminating and observing volumetric fields from arbitrary directions. STV is based on stereoscopic observation of particles-Seeded in a flow by CCD sensors. In the approach, part of the individual particle images that provide data points is likely to be lost or cause errors when their images overlap and crisscross each other especially under a high particle density. In order to maximize the valid recovery of data points, neural networks are implemented for these two important processes. For the step of particle overlap decomposition, the back propagation neural network is utilized because of its ability in pattern recognition with pertinent particle image feature parameters. For the step of particle tracking, the Hopfield neural network is employed to find appropriate particle tracks based on global optimization. Our investigation indicates that the neural networks are very efficient and useful for stereoscopically tracking particles. As an initial assessment of the diagnostic technology performance, laminar water jets with and without pulsation are measured. The jet tip velocity profiles are in good agreement with analytical predictions. Finally, for testing in material processing applications, a simple directional solidification apparatus is built for experimenting with a metal analog of succinonitrile. Its 3-D velocity field at the liquid phase is then measured to be compared with those from numerical computation. Our theoretical, numerical, and experimental investigations have proven STV to be a viable candidate for reliably measuring 3-D flow velocities. With current activities are focused on further improving the processing efficiency, overall accuracy, and automation, the eventual efforts of broad experimental applications and concurrent numerical modeling validation will be vital to many areas in fluid flow and materials processing.

Lee, David

Analysis of Residual Acceleration Effects on Transport and Segregation During Directional Solidification of Tin-Bismuth in the MEPHISTO Furnace Facility

The research accomplishments summarized in this Final Report during the period from 3/95 to 3/98, which included a 12 months no-cost extension granted at the end of the nominal 2 year period of performance. The report has 5 sections, in section 1 the objectives are presented, a task description is given and the background and significance of the work is outlined. In section 2 the research accomplishments are summarized. In section 3 publications and presentations are listed. Student participation is listed in 4. The work is summarized in section 5. and references for sections 1 and 2 are supplied in section 6. The object of this work, is to approach the problem of determining the transport conditions (and effects of residual acceleration) during the plane-front directional solidification of a tin-bismuth alloy under low gravity conditions. The work involved using a combination of 2- and 3-D numerical models, scaling analyses, ID models and the results of ground-based and low-gravity experiments. The experiments conducted in the MEPHISTO furnace facility during the USW-3 space flight which took place between February 22 through March 6, 199). This experiment represents an unprecedented opportunity to make a quantitative correlation between residual accelerations and the response of an actual experimental solidification

Alexander, J. Iwan D.

Growth of CdZnTe Crystals for Radiation Detector Applications by Directional Solidification

Advances in Cadmium Zinc Telluride (Cd(sub 1-x)Zn(sub x)Te) growth techniques are needed for the production of large-scale arrays of gamma and x-ray astronomy. The research objective is to develop crystal growth recipes and techniques to obtain large, high quality CdZnTe single crystal with reduced defects, such as charge trapping, twinning, and tellurium precipitates, which degrade the performance of CdZnTe and, at the same time, to increase the yield of usable material from the CdZnTe ingot. A low gravity material experiment, "Crystal Growth of Ternary Compound Semiconductors in Low Gravity Environment", will be performed in the Material Science Research Rack (MSRR) on International Space Station (ISS). One section of the flight experiment is the melt growth of CdZnTe ternary compounds. This talk will focus on the ground-based studies on the growth of Cd(sub 0.80)Zn(sub 0.20)Te crystals for radiation detector applications by directional solidification. In this investigation, we have improved the properties that are most critical for the detector applications (electrical properties and crystalline quality): a) Electrical resistivity: use high purity starting materials (with reproducible impurity levels) and controlled Cd over pressure during growth to reproducibly balance the impurity levels and Cd vacancy concentration b) Crystalline quality: use ultra-clean growth ampoule (no wetting after growth), optimized thermal profile and ampoule design, as well as a technique for supercool reduction to growth large single crystal with high crystalline quality

Su, Ching-Hua

Morphological Evolution of Directional Solidification Interfaces in Microgravity: An Analysis of Model Experiments Performed on the International Space Station

A series of experiments performed using the Pore Formation and Mobility Investigation (PFMI) apparatus within the glovebox facility (GBX) on board the International Space Station (ISS) has provided video images of the morphological evolution of a three-dimensional interface in a diffusion controlled regime. The experimental samples were prepared on ground by filling glass tubes, 1 cm ID and approximately 30 cm in length, with "alloys" of succinonitrile (SCN) and water in an atmosphere of nitrogen at 450 millibar pressure. The compositions of the samples processed and analyzed are 0.25,0.5 and 1.0 wt% water. Experimental processing parameters of temperature gradient and translation speed, as well as camera settings, were remotely monitored and manipulated from the ground Telescience Center (TSC) at the Marshall !3pace Flight Center. During the experiments, the sample was first subjected to a unidirectional melt back, generally at 10 microns per second, with a constant temperature gradient ahead of the melting interface. Following the melt back, the interface was allowed to stabilize before translation is initiated. The temperatures in the sample were monitored by six in situ thermocouples and the position is monitored by an optical linear encoder. For the experiments performed and analyzed, the gradients ranged from 2.5 - 3.3 K/mm and the initial pulling velocities ranged from 0.7 micron per second to 1 micron per second with subsequent transition velocities of up to 100 microns per second. The data provided by the PFMI for analysis includes near-real-time (NRT) video captured on the ground during the experiment runs, ISS Video Tape Recorder (VTR) data dumped from the VTR at the end of the experiment run and recorded on the ground, telemetry data including temperature and position measurements, and limited flight HI-8 tapes in 2 camera views of experiment runs for which tapes have been returned to the investigators from ISS. Because of limited down mass from the ISS, the majority of the initial analysis has been performed using the NRT and VTR video data but will be supplemented with the HI-8 video as it becomes available. hardware and procedures required to prepare samples for correlation to flight samples is described. Using this ground-based system, a series of experiments have been performed for direct comparison with the flight data. The results of these comparisons as well as implications to future microgravity experiments are presented and discussed. A ground-based thin-sample directional solidification system as well as all associated

Strutzenberg, Louise L.

Highly Ordered Eutectic Mesostructures via Template‐Directed Solidification within Thermally Engineered Templates

Template-directed self-assembly of solidifying eutectics results in emergence of unique microstructures due to diffusion constraints and thermal gradients imposed by the template. Here, the importance of selecting the template material based on its conductivity to control heat transfer between the template and the solidifying eutectic, and thus the thermal gradients near the solidification front, is demonstrated. Simulations elucidate the relationship between the thermal properties of the eutectic and template and the resultant microstructure. The overarching finding is that templates with low thermal conductivities are generally advantageous for forming highly organized microstructures. When electrochemically porosified silicon pillars (thermal conductivity < 0.3 Wm −1 K −1 ) are used as the template into which an AgCl-KCl eutectic is solidified, 99% of the unit cells in the solidified structure exhibit the same pattern. In contrast, when higher thermal conductivity crystalline silicon pillars (≈100 Wm −1 K −1 ) are utilized, the expected pattern is only present in 50% of the unit cells. The thermally engineered template results in mesostructures with tunable optical properties and reflectances nearly identical to the simulated reflectances of perfect structures, indicating highly ordered patterns are formed over large areas. This work highlights the importance of controlling heat flows in template-directed self-assembly of eutectics.

36 MATERIALS SCIENCE

The influence of a microgravity environment on the dendritic morphology during directional solidification of hypoeutectic Al-Si alloys

NASA grant NAGW-2540 provided the opportunity to evaluate and extend ongoing studies of directionally solidified Al-Si alloys. Microstructural development was further characterized in terms of solidification processing parameters; novel relationships between processing and development of dendrite trunk diameters and tertiary dendrite arm spacings were found. This has resulted in three publications (one in print, one in press, and one in review). Microstructural development under conditions of controlled acceleration during directional solidification has been investigated; this has culminated in a Master's degree and will be submitted for publication. The above work not only contributes to our understanding of solidification phenomena but also defines the processing parameters for a successful microgravity experiment while providing a data base to which mu g samples can be unequivocally compared and evaluated.

Grugel, Richard N.

Effects of an Applied Magnetic Field on the Directional Solidification of Hg(1-x)Zn(x)Se Alloys

Directionally solidified Hg(0.9)Zn(0.1)Se alloys were studied as an alternative to HgCdTe for the detection of electromagnetic radiation because of predicted improvements in lattice stability. Several boules were grown using a modified Bridgman-Stockbarger method and in an applied magnetic field. Axial compositional profiles showed mass transfer was primarily diffusion controlled. Radial compositional variations were greatly reduced when solidification occurred in an applied magnetic field. Microstructural characteristics and dislocation etch pit densities were greatly improved over HgTe based alloys. The extreme importance of processing conditions on defect generation was illustrated by comparing ampoule configurations and thermal profiles.

Cobb, S. D.

SPAR VI Technical Report for Experiment 76-22: Directional Solidification of Magnetic Composites

Samples of eutectic Bi/MnBi were directionally solidified during a low-g interval aboard the SPAR 6 flight and in a l-g environment under identical furnace velocity and thermal conditions. The Bi/MnBi eutectic is characterized by a regular rod eutectic whose morphology may be sensitive to thermo-solutal convection and by its components, MnBi, which is ferromagnetic. Morphological analyses on samples show statistically smaller interrod spacings and rod diameters with respect to samples grown under identical solidification furnace conditions in l-g. An adjustment between the interrod spacing, growth velocity, and total undercooling at the solidification interface is proposed. Morphological analyses on samples grown in l-g indicate little difference between results for different growth orientations with respect to the gravity vector. The magnetic properties are significantly affected, however, by the presence of a nonequilibrium magnetic phase and the nonequilibrium phase transforms to the equilibrium ferromagnetic phase during isothermal heat treatment.

Pirich, R. G.

Observation of an Aligned Gas - Solid "Eutectic" during Controlled Directional Solidification Aboard the International Space Station - Comparison with Ground-based Studies

Direct observation of the controlled melting and solidification of succinonitrile was conducted in the glovebox facility of the International Space Station (ISS). The experimental samples were prepared on ground by filling glass tubes, 1 cm ID and approximately 30 cm in length, with pure succinonitrile (SCN) in an atmosphere of nitrogen at 450 millibar pressure for eventual processing in the Pore Formation and Mobility Investigation (PFMI) apparatus in the glovebox facility (GBX) on board the ISS. Real time visualization during controlled directional melt back of the sample showed nitrogen bubbles emerging from the interface and moving through the liquid up the imposed temperature gradient. Over a period of time these bubbles disappear by dissolving into the melt. Translation is stopped after melting back of about 9 cm of the sample, with an equilibrium solid-liquid interface established. During controlled re-solidification, aligned tubes of gas were seen growing perpendicular to the planar solid/liquid interface, inferring that the nitrogen previously dissolved into the liquid SCN was now coming out at the solid/liquid interface and forming the little studied liquid = solid + gas eutectic-type reaction. The observed structure is evaluated in terms of spacing dimensions, interface undercooling, and mechanisms for spacing adjustments. Finally, the significance of processing in a microgravity environment is ascertained in view of ground-based results.

Grugel, R. N.

Superalloy microstructural variations induced by gravity level during directional solidification

The Ni-base superalloy MAR-M246 (Hf) was directionally solidified during low gravity maneuvers aboard a NASA KC-135 aircraft. Gravity force variations during this process yielded a concomitant variation in microstructure and microsegregation. Secondary dendrite arm spacings are noted to be larger in the low-g portion; this, in turn, decreases the extent of interdendritic segregation. The amount of Hf in both the carbides and interdendritic eutectic increases as the gravity force diminishes. Fewer carbides are present in the low-g regions.

Johnston, M. H.