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NASA NTRS1997

Colloids and Nucleation

The objectives of the work funded under this grant were to develop a microphotographic technique and use it to monitor the nucleation and growth of crystals of hard colloidal spheres. Special attention is given to the possible need for microgravity studies in future experiments. A number of persons have been involved in this work. A masters student, Keith Davis, began the project and developed a sheet illumination apparatus and an image processing system for detection and analysis. His work on a segmentation program for image processing was sufficient for his master's research and has been published. A post doctoral student Bernie Olivier and a graduate student Yueming He, who originally suggested the sheet illumination, were funded by another source but along with Keith made photographic series of several samples (that had been made by Keith Davis). Data extraction has been done by Keith, Bernie, Yueming and two undergraduates employed on the grant. Results are published in Langmuir. These results describe the sheet lighting technique as one which illuminates not only the Bragg scattering crystal, but all the crystals. Thus, accurate crystal counts can be made for nucleation rate measurements. The strange crystal length scale reduction, observed in small angle light scattering (SALS) studies, following the initial nucleation and growth period, has been observed directly. The Bragg scattering (and dark) crystal size decreases in the crossover region. This could be an effect due to gravitational forces or due to over- compression of the crystal during growth. Direct observations indicate a complex morphology for the resulting hard sphere crystals. The crystal edges are fairly sharp but the crystals have a large degree of internal structure. This structure is a result of (unstable) growth and not aggregation. As yet unpublished work compares growth exponents data with data obtained by SALS. The nucleation rate density is determined over a broad volume fraction range (0.505 to 0.575) and compared to classical nucleation rate calculations. The experimental nucleation rate density varies with volume fraction more slowly than expected theoretically. Gravity may influence nucleation because crystal nuclei are more dense than the surrounding fluid and may be gravitationally convected. The largest observed crystal size was near volume fraction 0.52. Near the freezing point, crystals should grow to large size because nuclei are sparse and there is plenty of room to grow without contacting other crystals. Near melting the opposite is true, with crystals growing into one another shortly after nucleation. The maximum crystal size seen near 0.52 volume fraction suggests that gravitational stresses are limiting crystal growth near freezing.

Ackerson, Bruce↗

NASA NTRS1994

Effects of vibration (G-jitters) on convection in micro-gravity

To obtain high quality crystals, it is desirable to maintain a diffusion-limited transport process in a planar solidification surface between the solid and the melt during the crystal growth process. Due to the presence of buoyancy-driven convection, however, this situation is difficult to maintain on Earth. The microgravity environment of an orbiting space laboratory presents an alternative worth pursuing. With reduced gravity, convections very much suppressed in a space laboratory, making the environment more conducive for growing crystals with better quality. However, a space laboratory is not immune from any undesirable disturbances. Nonuniform and transient accelerations such as vibrations, g-jitters, and impulsive accelerations exist as a result of crew activities, space maneuvering, and the operations of on-board equipment. Measurements conducted on-board a U.S. Spacelab mission showed the existence of vibrations in the frequency range of 1 to 100 Hz. It was reported that a dominant mode of 17 Hz and harmonics of 54 Hz were observed and these were attributed to antenna operations. The vibration is not limited to any single plane but exists in all directions. Some data from the Russian MIR space station indicates the existence of vibration also at this frequency range.

Wang, Francis C.↗

NASA NTRS2001

First Protein Crystallization Experiments on The International Space Station: Sweet Success in Space With Thaumatin

We determined the room temperature 1.2 A structure of thaumatin using a crystal grown in the first protein crystallization experiment conducted aboard the International Space Station (ISS). The crystals were grown in the Enhanced Gaseous Nitrogen Dewar (EGN) developed by Alexander McPherson and co-workers. EGN transports frozen solutions contained in tygon tubing in a liquid nitrogen Dewar to ISS where the tubes then thaw. Batch, free interface diffusion (FID), or vapor diffusion crystallization occurs after thawing. EGN was flown to the ISS on STS-106 on September 8, 2000. This was a "risk mitigation" flight that tested EGN performance and the process of conducting experiments on ISS. We focused on how to map a hanging drop crystallization recipe to the EGN FID method. Thaumatin was chosen as the test system. Three series of crystallization recipes were set-up. Each series tested different volume ratios of protein-rich solution to precipitant-rich solution. The series differed from each other by fixing either the protein concentration or the amount of protein in the solutions. Upon return of the samples to Earth on October 24 by STS-92, bubbles that spanned the diameter of the tubing were observed in all tubes. Such bubbles interrupt liquid-liquid diffusion and force vapor diffusion equilibration to occur instead. Nonetheless, crystals grew in 9 of 30 tubes. Many large crystals were grown, the largest being 2.0 x 1.1 x 1.0 cubic mm. The largest crystal was used to collect data at room temperature on beamline 7-1 of the Stanford Synchrotron Radiation Source to a maximum resolution of 1.2 A. The structure was refined anisotropically using SHELX with a data to parameter ratio of 4.5 to give an R(sub factor) of 15.8% (R(sub free) = 18.2%) for ail reflections without generated hydrogens. This refinement is proceeding. Comparisons of this 1.2 A microgravity structure to previous reports of the thaumatin structure at 1.75 A and to ground control crystals will be presented.

Kundrot, Craig E.↗

NASA NTRS1983

International aspects of commercial space activities

Attention is given to problems in international cooperation that will arise if NASA proceeds with a Space Station. The rise in space budgets in many countries is cited as an indication of the growing importance being placed on space activities. It is also pointed out that these nations are emphasizing areas which hold promise for eventual commercial payoff. Developing countries are also paying greater attention to space. As part of the European Space Agency's development program, it is underwriting the development of up to six multiuser facilities dedicated to microgravity research; these include furnaces and thermostats for processing metallurgical samples and for crystal growth and botanical investigations. Competition from Europe is seen as a spur to efficiency. Attention is also given to the question whether international cooperation will interfere with research carried out by the US for military purposes.

Pedersen, K. S.↗

NASA NTRS1984

Material research in microgravity

A popular discussion is given of microgravity effects in engineering and medicine gained from Skylab experience. Areas covered include crystal growing, liquid surface properties, diffusion, ferromagnetism, and emulsions.

Langbein, D.↗

NASA NTRS1985

Summary results of the Industry Conference on the Commercial Use of Space

The future intentions of the Federal Republic of Germany in the area of the commercialization of space are presented. It is shown that significant advances in microgravity research, particulary in the areas of materials science, composite materials, physical chemistry, crystal growth, biology, and process engineering will have an effect on future plans for establishing sponsoring organizations to guide commercial interests in German space research. An organizational and functional outline of a proposed sponsoring organization to promote space commercialization under German supervision, including the objectives, the target group to be served, and the administrative structure, is presented. The role of the DFVLR (German Aerospace Research Establishment) and the BMFT (German Ministry for Research and Technology) as sponsoring organizations representing the interests of the German government is shown.

REUSE↗

NASA NTRS1991

A materials scientist in space - 1990 MRS Fall Meeting Plenary Address

An edited version of astronaut Bonnie J. Dunbar's Plenary Address at the 1990 MRS Fall Meeting is presented. The Shuttle program is briefly reviewed with emphasis on the microgravity environment experiments conducted aboard the Columbia in January 1991. In particular, protein crystal growth experiments resulted in growing morphologically uniform crystals with sizes in the 400-500 micron range are discussed. The Long-Duration Exposure Facility intended to study the effects of atomic oxygen and the ultraviolet light environment in low earth orbit on materials has been successfully retrieved. Some research areas of future flights are noted.

Dunbar, Bonnie J.↗

NASA NTRS1992

Space Station Furnace Facility Core. Requirements definition and conceptual design study. Volume 2: Technical report. Appendix 6: Technical summary reports

The Space Station Furnace Facility (SSFF) is a modular facility for materials research in the microgravity environment of the Space Station Freedom (SSF). The SSFF is designed for crystal growth and solidification research in the fields of electronic and photonic materials, metals and alloys, and glasses and ceramics and will allow for experimental determination of the role of gravitational forces in the solidification process. The facility will provide a capability for basic scientific research and will evaluate the commercial viability of low-gravity processing of selected technologically important materials. The facility is designed to support a complement of furnace modules as outlined in the Science Capabilities Requirements Document (SCRD). The SSFF is a three rack facility that provides the functions, interfaces, and equipment necessary for the processing of the furnaces and consists of two main parts: the SSFF Core Rack and the two Experiment Racks. The facility is designed to accommodate two experimenter-provided furnace modules housed within the two experiment racks, and is designed to operate these two furnace modules simultaneously. The SCRD specifies a wide range of furnace requirements and serves as the basis for the SSFF conceptual design. SSFF will support automated processing during the man-tended operations and is also designed for crew interface during the permanently manned configuration. The facility is modular in design and facilitates changes as required, so the SSFF is adept to modifications, maintenance, reconfiguration, and technology evolution.

Source record↗

NASA NTRS1992

Space Station Furnace Facility. Volume 2: Summary of technical reports

The Space Station Furnace Facility (SSFF) is a modular facility for materials research in the microgravity environment of the Space Station Freedom (SSF). The SSFF is designed for crystal growth and solidification research in the fields of electronic and photonic materials, metals and alloys, and glasses and ceramics, and will allow for experimental determination of the role of gravitational forces in the solidification process. The facility will provide a capability for basic scientific research and will evaluate the commercial viability of low-gravity processing of selected technologically important materials. In order to accommodate the furnace modules with the resources required to operate, SSFF developed a design that meets the needs of the wide range of furnaces that are planned for the SSFF. The system design is divided into subsystems which provide the functions of interfacing to the SSF services, conditioning and control for furnace module use, providing the controlled services to the furnace modules, and interfacing to and acquiring data from the furnace modules. The subsystems, described in detail, are as follows: Power Conditioning and Distribution Subsystem; Data Management Subsystem; Software; Gas Distribution Subsystem; Thermal Control Subsystem; and Mechanical Structures Subsystem.

Source record↗

NASA NTRS2003

In-Situ Pressure Measurements During the Detached Growth of Germanium

Crystal growth by the vertical Bridgman method in which there is little or no contact between the wall and the crystal has been termed detached solidification. Detachment has been observed frequently in previous microgravity experiments, and has been reported under some terrestrial conditions as well. It is expected that detachment can be conditioned by establishing an appropriate pressure difference below and above the melt. To test this hypothesis, an experimental technique has been developed to measure this pressure difference during the growth of germanium by the vertical Bridgman method. The apparatus allows for both monitoring the pressures and actively controlling them during growth. For a given melt height, there is a maximum pressure difference attainable before gas bubbles up through the melt. This maximum pressure increases with increasing melt height. As the melt height approaches zero, the maximum pressure difference, about 20 mbar in these experiments, is determined by the surface tension and gap width of the meniscus at the bottom of the melt.

Volz, M. P.↗

NASA NTRS1998

SAMS Acceleration Measurements on Mir (NASA Increment 4)

During NASA Increment 4 (January to May 1997), about 5 gigabytes of acceleration data were collected by the Space Acceleration Measurements System (SAMS) onboard the Russian Space Station, Mir. The data were recorded on 28 optical disks which were returned to Earth on STS-84. During this increment, SAMS data were collected in the Priroda module to support the Mir Structural Dynamics Experiment (MiSDE), the Binary Colloidal Alloy Tests (BCAT), Angular Liquid Bridge (ALB), Candle Flames in Microgravity (CFM), Diffusion Controlled Apparatus Module (DCAM), Enhanced Dynamic Load Sensors (EDLS), Forced Flow Flame Spreading Test (FFFr), Liquid Metal Diffusion (LMD), Protein Crystal Growth in Dewar (PCG/Dewar), Queen's University Experiments in Liquid Diffusion (QUELD), and Technical Evaluation of MIM (TEM). This report points out some of the salient features of the microgravity environment to which these experiments were exposed. Also documented are mission events of interest such as the docked phase of STS-84 operations, a Progress engine bum, Soyuz vehicle docking and undocking, and Progress vehicle docking. This report presents an overview of the SAMS acceleration measurements recorded by 10 Hz and 100 Hz sensor heads. The analyses included herein complement those presented in previous summary reports prepared by the Principal Investigator Microgravity Services (PIMS) group.

DeLombard, Richard↗

NASA NTRS1998

SAMS Acceleration Measurements on Mir From January to May 1997 (NASA Increment 4)

During NASA Increment 4 (January to May 1997), about 5 gigabytes of acceleration data were collected by the Space Acceleration Measurements System (SAMS) onboard the Russian Space Station, Mir. The data were recorded on 28 optical disks which were returned to Earth on STS-84. During this increment, SAMS data were collected in the Priroda module to support the Mir Structural Dynamics Experiment (MiSDE), the Binary Colloidal Alloy Tests (BCAT), Angular Liquid Bridge (ALB), Candle Flames in Microgravity (CFM), Diffusion Controlled Apparatus Module (DCAM), Enhanced Dynamic Load Sensors (EDLS), Forced Flow Flame Spreading Test (FFFT), Liquid Metal Diffusion (LMD), Protein Crystal Growth in Dewar (PCG/Dewar), Queen's University Experiments in Liquid Diffusion (QUELD), and Technical Evaluation of MIM (TEM). This report points out some of the salient features of the microgravity environment to which these experiments were exposed. Also documented are mission events of interest such as the docked phase of STS-84 operations, a Progress engine burn, Soyuz vehicle docking and undocking, and Progress vehicle docking. This report presents an overview of the SAMS acceleration measurements recorded by 10 Hz and 100 Hz sensor heads. The analyses included herein complement those presented in previous summary reports prepared by the Principal Investigator Microgravity Services (PIMS) group.

DeLombard, Richard↗

NASA NTRS1996

Local and Global Bifurcations of Flow Fields During Physical Vapor Transport: Application to a Microgravity Experiment

The local bifurcation of the flow field, during physical vapor transport for a parametric range of experimental interest, shows that its dynamical state ranges from steady to aperiodic. Comparison of computationally predicted velocity profiles with laser doppler velocimetry measurements shows reasonable agreement in both magnitude and planform. Correlation of experimentally measured crystal quality with the predicted dynamical state of the flow field shows a degradation of quality with an increase in Rayleigh number. The global bifurcation of the flow field corresponding to low crystal quality indicates the presence of a traveling wave for Ra = 1.09 x 10(exp 5). For this Rayleigh number threshold a chaotic transport state occurs. However, a microgravity environment for this case effectively stabilizes the flow to diffusive-advective and provides the setting to grow crystals with optimal quality.

Duval, W. M. B.↗

NASA NTRS1998

Second United States Microgravity Laboratory: One Year Report

This document reports the one year science results for the important and highly successful Second United States Microgravity Laboratory (USML-2). The USML-2 mission consisted of a pressurized Spacelab module where the crew performed experiments. The mission also included a Glovebox where the crew performed additional experiments for the investigators. Together, about 36 major scientific experiments were performed, advancing the state of knowledge in fields such as fluid physics, solidification of metals, alloys, and semiconductors, combustion, and the growth of protein crystals. The results demonstrate the range of quality science that can be conducted utilizing orbital laboratories in microgravity and provide a look forward to a highly productive Space Station era.

Vlasse, M.↗

NASA NTRS1998

Second United States Microgravity Laboratory: One Year Report

Vlasse, M↗

NASA NTRS1998

Damping Mechanisms for Microgravity Vibration Isolation (MSFC Center Director's Discretionary Fund Final Report, Project No. 94-07)

As a research facility for microgravity science, the International Space Station (ISS) will be used for numerous investigations such as protein crystal growth, combustion, and fluid mechanics experiments which require a quiescent acceleration environment across a broad spectrum of frequencies. These experiments are most sensitive to low-frequency accelerations and can tolerate much higher accelerations at higher frequency. However, the anticipated acceleration environment on ISS significantly exceeds the required acceleration level. The ubiquity and difficulty in characterization of the disturbance sources precludes source isolation, requiring vibration isolation to attenuate the anticipated disturbances to an acceptable level. This memorandum reports the results of research in active control methods for microgravity vibration isolation.

Whorton, M. S.↗

NASA NTRS1979

Crystal growth of sulfide materials from alkali polysulfide liquids

The fluids experiment system was designed for low temperature solution growth, nominally aqueous solution growth. The alkali polysulfides, compositions in the systems Na2S-S and K2S-S form liquids in the temperature range of 190 C to 400 C. These can be used as solvents for other important classes of materials such as transition metal and other sulfides which are not soluble in aqueous media. Among these materials are luminescent and electroluminescent crystals whose physical properties are sensitive functions of crystal perfection and which could, therefore, serve as test materials for perfection improvement under microgravity conditions.

White, W. B.↗

NASA NTRS1982

Segregation effects during growth of pseudo-binary system with large liquidus-solidus separation

Results are reported for an experimental study of the seeded growth, of PbSnTe single crystals in a vertical Bridgman-Stockbarger (B-S) furnace. Profiles of axial and radial segregation of Sn are presented for crystal growth from melts with aspect ratios of 15 and 6.8; the profiles indicate intense convective mixing. A one-dimensional model of heat and mass transfer in an idealized B-S furnace with diffusion control is used to examine the importance of liquidus-solidus separation in determining growth-rate and composition transients in a pseudobinary system. It is shown that the coupling of heat and mass transfer in a pseudobinary system with a large liquidus-solidus separation causes the transient behavior in a nondilute system to differ markedly from such behavior in a dilute system and that PbSnTe crystals with a reasonable diameter can be grown under nearly convectionless conditions in a microgravity environment.

Bourret, E. D.↗