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NASA NTRS1992

An examination of anticipated g-jitter on Space Station and its effects on materials processes

Information on anticipated g-jitter on Space Station Freedom and the effect of the jitter on materials processes is given in viewgraph form. It was concluded that g-jitter will dominate the acceleration environment; that it is a 3D multifrequency phenomenon; and that it varies dramatically in orientation. Information is given on calculated or measured sources of residual acceleration, aerodynamic drag, Shuttle acceleration measurements, the Space Station environment, tolerable g-levels as a function of frequency, directional solidification, vapor crystal growth, protein crystal growth, float zones, and liquid bridges.

Nelson, Emily↗

NASA NTRS1997

Lithium-ion drifting: Application to the study of point defects in floating-zone silicon

The use of lithium-ion (Li(+)) drifting to study the properties of point defects in p-type Floating-Zone (FZ) silicon crystals is reported. The Li(+) drift technique is used to detect the presence of vacancy-related defects (D defects) in certain p-type FZ silicon crystals. SUPREM-IV modeling suggests that the silicon point defect diffusivities are considerably higher than those commonly accepted, but are in reasonable agreement with values recently proposed. These results demonstrate the utility of Li(+) drifting in the study of silicon point defect properties in p-type FZ crystals. Finally, a straightforward measurement of the Li(+) compensation depth is shown to yield estimates of the vacancy-related defect concentration in p-type FZ crystals.

Silicon↗

NASA NTRS2015

REE Partitioning in Lunar Minerals

Rare earth elements (REE) are an extremely useful tool in modeling lunar magmatic processes. Here we present the first experimentally derived plagioclase/melt partition coefficients in lunar compositions covering the entire suite of REE. Positive europium anomalies are ubiquitous in the plagioclase-rich rocks of the lunar highlands, and complementary negative Eu anomalies are found in most lunar basalts. These features are taken as evidence of a large-scale differentiation event, with crystallization of a global-scale lunar magma ocean (LMO) resulting in a plagioclase flotation crust and a mafic lunar interior from which mare basalts were subsequently derived. However, the extent of the Eu anomaly in lunar rocks is variable. Fagan and Neal [1] reported highly anorthitic plagioclase grains in lunar impact melt rock 60635,19 that displayed negative Eu anomalies as well as the more usual positive anomalies. Indeed some grains in the sample are reported to display both positive and negative anomalies. Judging from cathodoluminescence images, these anomalies do not appear to be associated with crystal overgrowths or zones.

Rapp, J. F.↗

NASA NTRS1982

Bread board float zone experiment system for high purity silicon

A breadboard float zone experimental system has been established at Westech Systems for use by NASA in the float zone experimental area. A used zoner of suitable size and flexibility was acquired and installed with the necessary utilities. Repairs, alignments and modifications were made to provide for dislocation free zoning of silicon. The zoner is capable of studying process parameters used in growing silicon in gravity and is flexible to allow trying of new features that will test concepts of zoning in microgravity. Characterizing the state of the art molten zones of a growing silicon crystal will establish the data base against which improvements of zoning in gravity or growing in microgravity can be compared. 25 mm diameter was chosen as the reference size, since growth in microgravity will be at that diameter or smaller for about the next 6 years. Dislocation free crystals were growtn in the 100 and 111 orientations, using a wide set of growth conditions. The zone shape at one set of conditions was measured, by simultaneously aluminum doping and freezing the zone, lengthwise slabbing and delineating by etching. The whole set of crystals, grown under various conditions, were slabbed, polished and striation etched, revealing the growth interface shape and the periodic and aperiodic natures of the striations.

Kern, E. L.↗

NASA NTRS2011

SiC growth by Solvent-Laser Heated Floating Zone

In an effort to grow single crystal SiC fibers for seed crystals the following two growth methods have been coupled in this work: traveling solvent and laser heated floating zone to create the solvent-laser heated floating zone (Solvent-LHFZ) crystal growth method. This paper discusses the results of these initial experiments, which includes: source material, laser heating, and analysis of the first ever Solvent-LHFZ SiC crystals (synchrotron white beam x-ray topography confirmed).

Woodworth, Andrew A.↗

NASA NTRS1995

Introduction of artificial pinning centres in Bi2Sr2CaCu2O8 ceramics

Considering the phase equilibrium diagram of the system Bi203-SrO-CaO-CuO, single phase 'Bi2Sr2CaCu208' ceramics have been transformed by a simple annealing procedure into multiphase samples. The transformation results in the formation of second phases and in an increase of the intra-grain critical current density at 1 T of five times. This increase is believed to express improved pinning properties of the superconducting crystals. The prepared pinning centers are believed to be e.g. coherent precipitates (Guinier-Preston-zones) within the superconducting crystals.

Majewski, P.↗

NASA NTRS1999

Identification of Gravity-Related Effects on Crystal Growth From Melts With an Immiscibility Gap

This work involves an experimental-numerical approach to study the effects of natural and Marangoni convections on solidification of single crystals from a silicate melt with a liquid-liquid immiscibility gap. Industrial use of crystals grown from silicate melts is becoming increasingly important in electronic, optical, and high temperature structural applications. Even the simplest silicate systems like Al203-SiO2 have had, and will continue to have, a significant role in the development of traditional and advanced ceramics. A unique feature of crystals grown from the silicate systems is their outstanding linear electro-optic properties. They also exhibit exceptionally high optical rotativity. As a result, these crystals are attractive materials for dielectric, optical, and microwave applications. Experimental work in our laboratory has indicated that directional solidification of a single crystal mullite appears to be preceded by liquid-liquid phase separation in the melt. Disruption of the immiscible state results in crystallization of a two phase structure. There is also evidence that mixing in the melt caused by density-driven convection can significantly affect the stability of the immiscible liquid layers and result in poly-crystalline growth. On earth, the immiscible state has only been observed for small diameter crystals grown in float zone systems where natural convection is almost negligible. Therefore, it is anticipated that growth of large single crystals from silicate melts would benefit from microgravity conditions because of the reduction of the natural convective mixing. The main objective of this research is to determine the effects of transport processes on the phase separation in the melt during growth of a single crystal while addressing the following issues: (1) When do the immiscible layers form and are they real?; (2) What are the main physical characteristics of the immiscible liquids?; and (3) How mixing by natural or Marangoni convection affects the stability of the phase separated melt.

Kassemi, M.↗

NASA NTRS2003

Reduction of Defects in Germanium-Silicon

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 the crystals. In addition to float-zone processing, detached Bridgman growth, although not a completely crucible-free method, is a promising tool to improve crystal quality. It does not suffer from the size limitations of float zoning and the impact of thermocapillary convection on heat and mass transport is expected to be negligible. Detached growth has been observed frequently during g experiments. Considerable improvements in crystalline quality have been reported for these cases. However, neither a thorough understanding of the process nor a quantitative assessment of the quality of these improvements exists. This project will determine the means to reproducibly grow GeSi alloys in a detached mode and seeks to compare processing-induced defects in Bridgman, detached-Bridgman, and floating-zone growth configurations in GeSi crystals (Si less than or equal to 10 at%) up to 20mm in diameter. Specific objectives include: measurement of the relevant material parameters such as contact angle, growth angle, surface tension, and wetting behavior of the GeSi-melt on potential crucible materials; determination of the mechanism of detached growth including the role of convection; quantitative determination of the differences in defects and impurities for crystals grown using normal Bridgman, detached Bridgman, and floating zone (FZ) methods; investigation of the influence of a defined flow imposed by a rotating magnetic field on the characteristics of detached growth; control of time-dependent Marangoni convection in the case of FZ growth by the use of a rotating magnetic field to examine the influence on the curvature of the solid-liquid interface and the heat and mass transport; and growth of benchmark quality GeSi-single crystals.

Szofran, Frank R.↗

NASA NTRS2007

Al, Ti, and Cr: Complex Zoning in Synthetic and Natural Nakhlite Pyroxenes

Nakhlites are olivine-bearing clinopyroxene cumulates. The cumulus pyroxenes have cores that are relatively homogeneous in Fe, Mg, and Ca, but show complex zoning of minor elements, especially Al, Ti, and Cr. Zoning patterns contain information about crystallization history parent magma compositions. But it has proven difficult to decipher this information and translate the zoning patterns into petrogenetic processes. This abstract reports results of high-precision Electron Probe MicroAnalysis (EPMA) analysis of synthetic nakhlite pyroxenes run at fO2 from IW to QFM. It compares these with concurrent analyses of natural nakhlite MIL03346 (MIL), and with standardprecision analyses of Y000593 (Y593) collected earlier. Results suggest that (1) different processes are responsible for the zoning of MIL and other more slowly-cooled nakhlites such as Y593, and (2) changes in oxidation conditions during MIL crystallization are not responsible for the unusual Cr zoning pattern

McKay, G.↗

NASA NTRS2013

Can Solution Supersaturation Affect Protein Crystal Quality?

The formation of large protein crystals of "high quality" is considered a characteristic manifestation of microgravity. The physical processes that predict the formation of large, high quality protein crystals in the microgravity environment of space are considered rooted in the existence of a "depletion zone" in the vicinity of crystal. Namely, it is considered reasonable that crystal quality suffers in earth-grown crystals as a result of the incorporation of large aggregates, micro-crystals and/or large molecular weight "impurities", processes which are aided by density driven convective flow or mixing at the crystal-liquid interface. Sedimentation and density driven convection produce unfavorable solution conditions in the vicinity of the crystal surface, which promotes rapid crystal growth to the detriment of crystal size and quality. In this effort, we shall further present the hypothesis that the solution supersaturatoin at the crystal surface determines the growth mechanism, or mode, by which protein crystals grow. It is further hypothesized that protein crystal quality is affected by the mechanism or mode of crystal growth. Hence the formation of a depletion zone in microgravity environment is beneficial due to inhibition of impurity incorporatoin as well as preventing a kinetic roughening transition. It should be noted that for many proteins the magnitude of neither protein crystal growth rates nor solution supersaturation are predictors of a kinetic roughening transition. That is, the kinetic roughening transition supersaturation must be dtermined for each individual protein.

Gorti, Sridhar↗

NASA NTRS1981

Relict grains in chondrules

Attention is given to the fact that a significant fraction of the chondrules from ordinary chondrites contain silicate grains that survived the chondrule formation process without melting. Typically, these grains consist of coarse olivine, rarely orthopyroxene, crystals located in the core of chondrules and displaying a zoning that is inconsistent with crystallization from a silicate melt. It is noted that the relict grains still preserve the imprint of processes that occurred in the solar nebula and, in some cases, may include the isotopic record of interstellar grains. Information is presented on the chondrule precursor materials and the process of chondrule formation which was acquired by a compositional and textural study of three of the most unequilibrated type 3 ordinary chondrites.

Rambaldi, E. R.↗

NASA NTRS1996

The Advanced Automated Directional Solidification Furnace

The Advanced Automated Directional Solidification Furnace (AADSF) is a five zone tubular furnace designed for Bridgman-Stockbarger, other techniques of crystal growth involving multiple temperature zones such as vapor transport experiments and other materials science experiments. The five zones are primarily designed to produce uniform hot and cold temperature regions separated by an adiabatic region constructed of a heat extraction plate and an insert to reduce radiation from the hot to the cold zone. The hot and cold zone temperatures are designed to reach 1600 C and 1100 C, respectively. AADSF operates on a Multi-Purpose Experiment Support Structure (MPESS) within the cargo bay of the Space Shuttle on the United States Microgravity Payload (USMP) missions. Two successful flights, both employing the directional solidification or Bridgman Stockbarger technique for crystal growth have been made, and crystals of HgCdTe and PbSnTe grown in microgravity have been produced on USMP-2 and USMP-3, respectively. The addition of a Sample Exchange Mechanism (SEM) will enable three different samples to be processed on future flights including the USMP-4 mission.

Gillies, D. C.↗

NASA NTRS1992

Numerical simulations of inductive-heated float-zone growth

The present work provides an improved fluid flow and heat-transfer modeling of float-zone growth by introducing a RF heating model so that an ad hoc heating temperature profile is not necessary. Numerical simulations were carried out to study the high-temperature float-zone growth of titanium carbide single crystal. The numerical results showed that the thermocapillary convection occurring inside the molten zone tends to increase the convexity of the melt-crystal interface and decrease the maximum temperature of the molten zone, while the natural convection tends to reduce the stability of the molten zone by increasing its height. It was found that the increase of induced heating due to the increase of applied RF voltage is reduced by the decrease of zone diameter. Surface tension plays an important role in controlling the amount of induced heating. Finally, a comparison of the computed shape of the free surface with a digital image obtained during a growth run showed adequate agreement.

Chan, Y. T.↗

NASA NTRS1991

Quantitative determination of the mineral distribution in different collagen zones of calcifying tendon using high voltage electron microscopic tomography

High voltage electron microscopic tomography was used to make the first quantitative determination of the distribution of mineral between different regions of collagen fibrils undergoing early calcification in normal leg tendons of the domestic turkey, Meleagris gallopavo. The tomographic 3-D reconstruction was computed from a tilt series of 61 different views spanning an angular range of +/- 60 degrees in 2 degrees intervals. Successive applications of an interactive computer operation were used to mask the collagen banding pattern of either hole or overlap zones into separate versions of the reconstruction. In such 3-D volumes, regions specified by the mask retained their original image density while the remaining volume was set to background levels. This approach was also applied to the mineral crystals present in the same volumes to yield versions of the 3-D reconstructions that were masked for both the crystal mass and the respective collagen zones. Density profiles from these volumes contained a distinct peak corresponding only to the crystal mass. A comparison of the integrated density of this peak from each profile established that 64% of the crystals observed were located in the collagen hole zones and 36% were found in the overlap zones. If no changes in crystal stability occur once crystals are formed, this result suggests the possibilities that nucleation of mineral is preferentially and initially associated with the hole zones, nucleation occurs more frequently in the hole zones, the rate of crystal growth is more rapid in the hole zones, or a combination of these alternatives. All lead to the conclusion that the overall accumulation of mineral mass is predominant in the collagen hole zones compared to overlap zones during early collagen fibril calcification.

NASA Program Space Biology↗

NASA NTRS2001

Reduction of Defects in Germanium-Silicon

Szofran, Frank R.↗

NASA NTRS1998

The Role of Marangoni Convection for the FZ-Growth of Silicon

In growing crystals by the floating zone (FZ) technique under microgravity, the size restriction we have under earth conditions because of the hydrostatic pressure are avoided. Further, buoyancy related convection is eliminated to a high degree. But in the case of silicon, the gravity independent thermocapillary (Marangoni) convection is time-dependent even for small zone geometries. This has been demonstrated in several Technische Experimente unter Schwerelosigkeit (TEXUS) - technical experiments under reduced gravity) flights. Thus, to really take advantage of microgravity with respect to improve crystal quality, tools are required to control Marangoni convection in space facilities. Applying magnetic fields, convection can be influenced; fluid flow can either be damped (static magnetic fields) or overlaid by a regular flow regime (rotating magnetic fields). In floating zones of 8-10mm diameter and height (Ma approximately equals 6 x 10(exp 3)), a static magnetic field of about 2OOmT is sufficient to suppress time-dependent Marangoni convection to a high degree, but in dependence on the kind and the concentration of the added dopant, a new type of strongly pronounced dopant inhomogeneities have been detected. They are originated by thermoelectromagnetic convection. This can be avoided as well as detrimental effects on the radial dopant distribution by using rotating magnetic fields instead of static ones. Applying 75mT/50Hz to the FZ, the intensity of the dopant fluctuations is reduced to a high degree. Considering the rather low power consumption of rotating magnetic fields, this will be a useful tool for control or elimination of time-dependent Marangoni convection under microgravity. The strong time dependent character of thermocapillary flow and its influence on the temperature field has been measured in silicon half-zones for Marangoni numbers of Ma is approximately equal to 1-1.5 x 10(exp 4): temperature fluctuations up to 4C have been determined. Their frequency range was 0.1 and 0.4 Hz. Between certain thermocouple or sensor pairs, strong correlation has been detected.

Dold, P.↗

NASA NTRS1999

The Role of Marangoni Convection for the FZ-Growth of Silicon

Growing crystals by the floating zone (FZ) technique under microgravity avoids the size restriction we have under earth conditions due to hydrostatic pressure. Further, buoyancy related convection is eliminated to a great degree. But in the case of silicon, the gravity independent thermocapillary (Marangoni) convection is time-dependent even for small zone geometries. This has been demonstrated in several Technische Experimente unter Schwerelosigkeit (TEXUS) technical experiments under reduced gravity flights. Thus, to really take advantage of microgravity with respect to improved crystal quality, tools are required to control Marangoni convection in space facilities. With the application of magnetic fields, convection can be influenced; fluid flow can either be damped (static magnetic fields) or overlaid by a regular flow regime (rotating magnetic fields). In floating zones of 8-10 mm diameter and height (i.e., Ma is much greater than 6X 10(exp 3), a static magnetic field of about 2OOmT is sufficient to suppress time-dependent Marangoni convection to a high degree, but in dependence on the kind and the concentration of the added dopant, a new type of strongly pronounced dopant inhomogeneities have been detected. They are originated by thermoelectromagnetic convection. This can be avoided as well as detrimental effects on the radial dopant distribution by using rotating magnetic fields instead of static ones. Applying 7.5mT/5OHz to the FZ, the intensity of the dopant fluctuations is reduced to a high degree. Considering the rather low power consumption of rotating magnetic fields, this will be a useful tool for control or elimination of time-dependent Marangoni convection under microgravity. The strong time-dependent character of thermocapillary flow and its influence on the temperature field has been measured in silicon half-zones for Marangoni numbers of Ma is much greater than l - 1.5 X 10(exp 4): temperature fluctuations up to 4C have been determined, their frequency range was 0.4 and 0.4Hz. Between certain thermocouple or sensor pairs, strong correlation has been detected.

Dold, P.↗

NASA NTRS1990

Growth and characterization of CdS crystals

A growth method for the physical vapor transport of compound semiconductors in closed ampoules is described. With the unique techniques applied in the heat treatment of the starting materials and the temperature profiles provided by the three-zone translational furnace, large crystals of CdS have been grown successfully by the method at lower temperatures than previously used. Both unseeded and seeded growth have been investigated. The CdS crystals were examined using optical and scanning electron microscopies (SEM) to study the microstructure and the dislocation etch-pits. The crystals were further characterized by infrared (IR) and ultraviolet (UV) transmission measurements.

Su, Ching-Hua↗