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At least 91 records · Page 5

Laser-Heated Floating Zone Production of Single-Crystal Fibers

This report describes how a laser-heated floating zone apparatus can be used to investigate single-crystal fibers of various compositions. A feedrod with a stoichiometric composition of high-purity powders was connected to a pedestal and fed into a laser scan where it combined with a single-crystal fiber seed. A molten zone was formed at this junction. As the feedrod was continuously fed into the laser scan, a single-crystal fiber of a prescribed orientation was withdrawn from the melt. The resultant fibers, whose diameters ranged from 100 to 250 gm, could then be evaluated on the basis of their growth behavior, physical properties, mechanical properties, and fiber perfection.

Ritzert, Frank↗

Growth of semiconductor compound single crystal InSb by floating zone method (M-3)

Floating zone methods have potential applications in growing single high-quality semi-conductor crystals. In this method, melts can be sustained without containers and, therefore, are free from contamination from the containers. The main objective of this project is to use the Image Furnace to study a large diameter, (20 mm) single crystal of InSb under microgravity conditions. The behavior of the liquid column is recorded on the VTR tapes and is compared with what is expected theoretically. The single crystal grown in space is characterized by comparing it with single crystals grown on the ground with respect to crystallographic and electronic properties. The goal of this project is to confirm the effects of the microgravity on the single crystals.

Nakatani, I.↗

Microgravity accelerometer characterization on Columbia STS-32 mission

The Honeywell In-Space Accelerometer (HISA) is a three-axis microgravity accelerometer instrument package recently developed by Honeywell Systems and Research Center (SRC) to monitor oscillatory and transient accelerations onboard spacecraft and spaceborne structures. The HISA was designed to be co-located with materials and life sciences experiments to record real-time accelerometer event data, sampling time, and temperature. The HISA was originally developed to monitor the microgravity disturbances associated with a polymer morphology experiment developed by 3M Company in Minneapolis, Minnesota. The HISA was first flight tested with the 3M experiment on the Space Shuttle Atlantis STS-34 in October 1989. The HISA was successfully flown on a second shuttle mission (Columbia STS-32 in January 1990) in support of the NASA JSC-sponsored Microgravity Disturbances Experiment (MDE), which focused on the effects of microgravity disturbances on the growth of high-quality Indium crystals. The primary objective of the STS-32 MDE experiment was to investigate the effects of crew-induced gravity disturbances on the microstructure (crystal defects and uniformity of impurity distribution) of float-zone-grown crystals. The float-zone technique involves establishing a suspended molten zone between two cylindrical samples a pure, single-crystal sample and an impure, polycrystalline sample. Microgravity disturbances due to crew treadmill activity and orbiter maneuvering system thruster firings were sensed and recorded by the HISA to understand their effects on the stability of the float zone. The principle of operation of the HISA, the flight configuration of the HISA supporting the MDE experiment, and the characterization of STS-32 treadmill disturbance data are summarized.

Schoess, Jeff↗

Structural and Improper Ferroelectric Properties of TbInO 3 Single Crystal Grown by Laser Floating Zone

The honeycomb TbInO 3 has attracted wide research attention due to its fascinating physical properties. However, TbInO 3 single crystal was difficult to grow owing to the high melting point and serious volatilization of indium during the crystal growth. In this study, the volatilization of the indium element was effectively suppressed by controlling the growth atmosphere and pressure. The excess ratio of indium oxide was determined, and pure hexagonal TbInO 3 crystal was obtained by the laser floating zone method. Systematic studies on the crystal structure and optical and ferroelectric properties were carried out. The structure distortion resulted in the improper geometric ferroelectric revealed by single crystal diffraction and Raman spectrum measurements. The topological vortex domains and P-E hysteresis loop demonstrated the presence of ferroelectricity. TbInO 3 crystal has great potential application in vortex memory.

36 MATERIALS SCIENCE↗

Space-based crystal growth and thermocapillary flow

The demand for larger crystals is increasing especially in applications associated with the electronic industry, where large and pure electronic crystals (notably silicon) are the essential material to make high-performance computer chips. Crystal growth under weightless conditions has been considered an ideal way to produce bigger and hopefully better crystals. One technique which may benefit from a microgravity environment is the float-zone crystal-growth process, a containerless method for producing high-quality electronic material. In this method, a rod of material to be refined is moved slowly through a heating device which melts a portion of it. Ideally, as the melt resolidifies it does so as a single crystal which is then used as substrate for building microelectronic devices. The possibility of contamination by contact with other material is reduced because of the 'float' configuration. However, since the weight of the material contained in the zone is supported by the surface-tension force, the size of the resulting crystal is limited in Earth-based productions; in fact, some materials have properties which prevent this process from being used to manufacture crystals of reasonable size. Consequently, there has been a great deal of interest in exploiting the microgravity environment of space to grow larger size crystals of electronic material using the float-zone method. In addition to allowing larger crystals to be grown, a microgravity environment would also significantly reduce the magnitude of convection induced by buoyancy forces during the melting state. This type of convection was once thought to be at least partially responsible for the presence of undesirable nonuniformities--called striations--in material properties observed in float-zone material. However, past experiments on crystal growth under weightless conditions found that even with the absence of gravity, the float-zone method sometimes still results striations. It is believed that another mechanism is playing a dominant role in the microgravity environment.

Shen, Yong-Hong↗

Direct Visualization of an Impurity Depletion Zone

When a crystal incorporates more impurity per unit of its volume than the impurity concentration in solution, the solution in vicinity of the growing crystal is depleted with respect to the impurity I,2. With a stagnant solution, e. g. in microgravity or gels, an impurity depletion zone expands as the crystal grows and results in greater purity in most of the outer portion of the crystal than in the core. Crystallization in gel provides an opportunity to mimic microgravity conditions and visualize the impurity depletion zone. Colorless, transparent apoferritin (M congruent to 450 KDa) crystals were grown in the presence of red holoferritin dimer as a microheterogeneous impurity (M congruent to 900 KDa) within agarose gel by counterdiffusion with Cd(2+) precipitant. Preferential trapping of dimers, (distribution coefficient K = 4 (exp 1,2)) results in weaker red color around the crystals grown in the left tube in the figure as compared to the control middle tube without crystals. The left and the middle tubes contain colored ferritin dimers, the right tube contains colored trimers. The meniscus in the left tube separate gel (below) and liquid solution containing Cd(2+) (above). Similar solutions, though without precipitants, were present on top of the middle and right tube allowing diffusion of dimers and trimers. The area of weaker color intensity around crystals directly demonstrates overlapped impurity depletion zones.

Chernov, Alex A.↗

Nanoscale trace-element zoning in pyrite framboids and implications for paleoproxy applications

Pyrite framboids (spherical masses of nanoscale pyrite) are among the earliest textures of pyrite to form in sediments. It has been proposed that their trace-element (TE) contents can be used to track the TE composition of the water column in which they formed. However, it is not clear how these TEs are associated with the framboidal pyrite grains. For instance, it is important to know whether they are incorporated uniformly or are enriched in different regions of the framboid. Here, we used high-resolution scanning transmission electron microscopy to identify chemical zoning within pyrite framboids. We found that initial, nanoscale pyrite euhedral crystals, which make up the volumetric majority of the framboids, are covered/infilled by later pyrite that templates on the earlier pyrite. Further, this later pyrite is enriched in TEs, suggesting that many TEs are incorporated in pyrite relatively late (during early diagenesis; not in the water column). This observation suggests that although chemical analyses of pyrite framboids may provide ocean-water chemistry trends through time, the details are complex. Specifically, the TEs found in pyrite may be linked to adsorption onto organic matter, detrital material, and authigenic minerals such as Fe- and Mn-oxide phases followed by desorption in the sediments or release via dissolution and incorporation into pyrite as overgrowths on the initial nanoscale euhedral crystals that make up framboids. While the use of pyrite chemistry to understand past ocean conditions remains promising, and even diagenetic additions may not preclude the utility of pyrite for reconstructing ancient ocean conditions, care must be taken in interpretations because the end concentration may be influenced by diagenesis.

58 GEOSCIENCES↗

Melt segregation in plagioclase-poikilitic mesosiderites

The Budalan and Mincy mesosiderites contain a poikilitic-plagioclase matrix with orthopyroxene chadacrysts and interstitial-subophitic inverted pigeonite. Orthopyroxene chadacrysts in both mesosiderites are uniformly more aluminous than orthopyroxene clasts, suggesting that they were not derived from clasts by metamorphism. Interstitial inverted pigeonite is more ferroan than adjacent orthopyroxene in the matrix, consistent with the crystallization of a melt with the sequence orthopyroxene followed by pigeonite. The magnesium chadcrysts in Mincy could not have formed from a melt in equilibrium with the clasts but could have crystallized from impact melt. The most Mg chadacrysts are enclosed in large reversely zoned plagioclase crystals as a result of the undercooling in melt-lacking plagioclase clasts and associated nuclei. Mincy contains both plagioclase-poor and plagioclase-rich regions, explained by a separation of silicate melt into pools. Reckling Peak A80258, a plagioclase-poikilitic mesosiderite with a very high chadacryst/plagioclase ratio, resembles Mincy material from which melt has been extracted. It is suggested that the origin of the plagioclase-poikilitic mesosiderites is impact melting of a metal-silicate mixture.

Hewins, R. H.↗

Thermal Characterization of the Universal Multizone Crystallizator

The Universal Multizone Crystallizator (UMC) is a special apparatus for crystal growth under terrestrial and microgravity conditions. The use of twenty-five zones allows the, UMC to be used for several normal freezing growth techniques. The thermal profile is electronically translated along the stationary sample by systematically reducing the power to the control zones. Elimination of mechanical translation devices increases the systems reliability while simultaneously reducing the size and weight. This paper addresses the UMC furnace design, sample cartridge, typical thermal profiles and corresponding power requirements necessary for two normal freezing techniques: dynamic gradient freeze and zone melting crystal growth.

Watring, D. A.↗

Influence of Containment on the Growth of Silicon-Germanium: A Materials Science Flight Project

A series of Ge(1-x)Si(x) crystal growth experiments are planned to be conducted in the Low Gradient Furnace (LGF) onboard the International Space Station. The primary objective of the research is to determine the influence of containment on the processing-induced defects and impurity incorporation in germanium-silicon alloy crystals. A comparison will be made between crystals grown by the normal and "detached" Bridgman methods and the ground-based float zone technique. Crystals grown without being in contact with a container have superior quality to otherwise similar crystals grown in direct contact with a container, especially with respect to impurity incorporation, formation of dislocations, and residual stress in crystals. "Detached" or "dewetted" Bridgman growth is similar to regular Bridgman growth in that most of the melt is in contact with the crucible wall, but the crystal is separated from the wall by a small gap, typically of the order of 10-100 microns. Long duration reduced gravity is essential to test the proposed theory of detached growth. Detached growth requires the establishment of a meniscus between the crystal and the ampoule wall. The existence of this meniscus depends on the ratio of the strength of gravity to capillary forces. On Earth, this ratio is large and stable detached growth can only be obtained over limited conditions. Crystals grown detached on the ground exhibited superior structural quality as evidenced by measurements of etch pit density, synchrotron white beam X-ray topography and double axis X-ray diffraction. The plans for the flight experiments will be described.

Volz, M. P.↗

Influence of Containment on the Growth of Silicon-Germanium (ICESAGE): A Materials Science ISS Investigation

A series of Ge(1-x)Si(x) crystal growth experiments are planned to be conducted in the Low Gradient Furnace (LGF) onboard the International Space Station. The primary objective of the research is to determine the influence of containment on the processinginduced defects and impurity incorporation in germanium-silicon alloy crystals. A comparison will be made between crystals grown by the normal and "detached" Bridgman methods and the ground-based float zone technique. Crystals grown without being in contact with a container have superior quality to otherwise similar crystals grown in direct contact with a container, especially with respect to impurity incorporation, formation of dislocations, and residual stress in crystals. "Detached" or "dewetted" Bridgman growth is similar to regular Bridgman growth in that most of the melt is in contact with the crucible wall, but the crystal is separated from the wall by a small gap, typically of the order of 10-100 microns. Long duration reduced gravity is essential to test the proposed theory of detached growth. Detached growth requires the establishment of a meniscus between the crystal and the ampoule wall. The existence of this meniscus depends on the ratio of the strength of gravity to capillary forces. On Earth, this ratio is large and stable detached growth can only be obtained over limited conditions. Crystals grown detached on the ground exhibited superior structural quality as evidenced by measurements of etch pit density, synchrotron white beam X-ray topography and double axis X-ray diffraction. The plans for the flight experiments will be described.

Volz, M. P.↗

Influence of Containment on the Growth of Silicon-Germanium (ICESAGE): A Materials Science Investigation

A series of Ge Si crystal growth experiments are planned to be conducted in the Low 1-x x Gradient Furnace (LGF) onboard the International Space Station. The primary objective of the research is to determine the influence of containment on the processing-induced defects and impurity incorporation in germanium-silicon alloy crystals. A comparison will be made between crystals grown by the normal and "detached" Bridgman methods and the ground-based float zone technique. Crystals grown without being in contact with a container have superior quality to otherwise similar crystals grown in direct contact with a container, especially with respect to impurity incorporation, formation of dislocations, and residual stress in crystals. "Detached" or "dewetted" Bridgman growth is similar to regular Bridgman growth in that most of the melt is in contact with the crucible wall, but the crystal is separated from the wall by a small gap, typically of the order of 10-100 microns. Long duration reduced gravity is essential to test the proposed theory of detached growth. Detached growth requires the establishment of a meniscus between the crystal and the ampoule wall. The existence of this meniscus depends on the ratio of the strength of gravity to capillary forces. On Earth, this ratio is large and stable detached growth can only be obtained over limited conditions. Crystals grown detached on the ground exhibited superior structural quality as evidenced by measurements of etch pit density, synchrotron white beam X-ray topography and double axis X-ray diffraction.

Volz, M. P.↗

Crystal Growth of Germanium-Silicon Alloys on the ISS

A series of Ge(1-x)Si(x) crystal growth experiments are planned to be conducted in the Low Gradient Furnace (LGF) onboard the International Space Station. The experiments are part of the investigation "Influence of Containment on the Growth of Silicon-Germanium" (ICESAGE). The primary objective of the research is to determine the influence of containment on the processing-induced defects and impurity incorporation in germanium-silicon alloy crystals. A comparison will be made between crystals grown by the normal and "detached" Bridgman methods and the ground-based float zone technique. Crystals grown without being in contact with a container have superior quality to otherwise similar crystals grown in direct contact with a container, especially with respect to impurity incorporation, formation of dislocations, and residual stress in crystals. "Detached" or "dewetted" Bridgman growth is similar to regular Bridgman growth in that most of the melt is in contact with the crucible wall, but the crystal is separated from the wall by a small gap, typically of the order of 10-100 microns. Long duration reduced gravity is essential to test the proposed theory of detached growth. Detached growth requires the establishment of a meniscus between the crystal and the ampoule wall. This meniscus can exist over a much larger range of processing parameters in microgravity and the meniscus is more stable under microgravity conditions. The plans for the flight experiments will be described.

Volz, M. P.↗

Detached Solidification of Germanium-Silicon Crystals on the ISS

A series of Ge(sub 1-x) Si(sub x) crystal growth experiments are planned to be conducted in the Low Gradient Furnace (LGF) onboard the International Space Station. The primary objective of the research is to determine the influence of containment on the processing-induced defects and impurity incorporation in germanium-silicon alloy crystals. A comparison will be made between crystals grown by the normal and "detached" Bridgman methods and the ground-based float zone technique. Crystals grown without being in contact with a container have superior quality to otherwise similar crystals grown in direct contact with a container, especially with respect to impurity incorporation, formation of dislocations, and residual stress in crystals. "Detached" or "dewetted" Bridgman growth is similar to regular Bridgman growth in that most of the melt is in contact with the crucible wall, but the crystal is separated from the wall by a small gap, typically of the order of 10-100 microns. Long duration reduced gravity is essential to test the proposed theory of detached growth. Detached growth requires the establishment of a meniscus between the crystal and the ampoule wall. The existence of this meniscus depends on the ratio of the strength of gravity to capillary forces. On Earth, this ratio is large and stable detached growth can only be obtained over limited conditions. Crystals grown detached on the ground exhibited superior structural quality as evidenced by measurements of etch pit density, synchrotron white beam X-ray topography and double axis X-ray diffraction.

Volz, M. P.↗

Detached Solidification of Germanium-Silicon Crystals on the ISS

A series of Ge(sub 1-x) Si(sub x) crystal growth experiments are planned to be conducted in the Low Gradient Furnace (LGF) onboard the International Space Station. The primary objective of the research is to determine the influence of containment on the processing-induced defects and impurity incorporation in germanium-silicon alloy crystals. A comparison will be made between crystals grown by the normal and "detached" Bridgman methods and the ground-based float zone technique. Crystals grown without being in contact with a container have superior quality to otherwise similar crystals grown in direct contact with a container, especially with respect to impurity incorporation, formation of dislocations, and residual stress in crystals. "Detached" or "dewetted" Bridgman growth is similar to regular Bridgman growth in that most of the melt is in contact with the crucible wall, but the crystal is separated from the wall by a small gap, typically of the order of 10-100 microns. Long duration reduced gravity is essential to test the proposed theory of detached growth. Detached growth requires the establishment of a meniscus between the crystal and the ampoule wall. The existence of this meniscus depends on the ratio of the strength of gravity to capillary forces. On Earth, this ratio is large and stable detached growth can only be obtained over limited conditions. Crystals grown detached on the ground exhibited superior structural quality as evidenced by measurements of etch pit density, synchrotron white beam X-ray topography and double axis X-ray diffraction.

Volz, M. P.↗

A Groundmass Composition for EET 79001A Using a Novel Microprobe Technique for Estimating Bulk Compositions. Lithology A as an Impact Melt?

Petrologic investigation of the shergottites has been hampered by the fact that most of these meteorites are partial cumulates. Two lines of inquiry have been used to evaluate the compositions of parental liquids: (i) perform melting experiments at different pressures and temperatures until the compositions of cumulate crystal cores are reproduced [e.g., 1]; and (ii) use point-counting techniques to reconstruct the compositions of intercumulus liquids [e.g., 2]. The second of these methods is hampered by the approximate nature of the technique. In effect, element maps are used to construct mineral modes; and average mineral compositions are then converted into bulk compositions. This method works well when the mineral phases are homogeneous [3]. However, when minerals are zoned, with narrow rims contributing disproportionately to the mineral volume, this method becomes problematic. Decisions need to be made about the average composition of the various zones within crystals. And, further, the proportions of those zones also need to be defined. We have developed a new microprobe technique to see whether the point-count method of determining intercumulus liquid composition is realistic. In our technique, the approximating decisions of earlier methods are unnecessary because each pixel of our x-ray maps is turned into a complete eleven-element quantitative analysis. The success or failure of our technique can then be determined by experimentation. As discussed earlier, experiments on our point-count composition can then be used to see whether experimental liquidus phases successfully reproduce natural mineral compositions. Regardless of our ultimate outcome in retrieving shergottite parent liquids, we believe our pixel-bypixel analysis technique represents a giant step forward in documenting thin-section modes and compositions. For a third time, we have analyzed the groundmass composition of EET 79001, 68 [Eg]. The first estimate of Eg was made by [4] and later modified by [5], to take phase diagram considerations into account. The Eg composition of [4] was too olivine normative to be the true Eg composition, because the ,68 groundmass contains no forsteritic olivine. A later mapping by [2] basically reconfirmed the modifications of [5]. However, even the modified composition of [5] has olivine on the liquidus for ~50 C before low-Ca pyroxene appears [6].

Jones, John H.↗

Fluid mechanics and mass transfer in melt crystal growth: Analysis of the floating zone and vertical Bridgman processes

This research program focuses on analysis of the transport mechanisms in solidification processes, especially one of interest to the Microgravity Sciences and Applications Program of NASA. Research during the last year has focused on analysis of the dynamics of the floating zone process for growth of small-scale crystals, on studies of the effect of applied magnetic fields on convection and solute segregation in directional solidification, and on the dynamics of microscopic cell formation in two-dimensional solidification of binary alloys. Significant findings are given.

Brown, R. A.↗