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At least 217 records · Page 12

Advanced protein crystal growth programmatic sensitivity study

The purpose of this study is to define the costs of various APCG (Advanced Protein Crystal Growth) program options and to determine the parameters which, if changed, impact the costs and goals of the programs and to what extent. This was accomplished by developing and evaluating several alternate programmatic scenarios for the microgravity Advanced Protein Crystal Growth program transitioning from the present shuttle activity to the man tended Space Station to the permanently manned Space Station. These scenarios include selected variations in such sensitivity parameters as development and operational costs, schedules, technology issues, and crystal growth methods. This final report provides information that will aid in planning the Advanced Protein Crystal Growth Program.

Source record↗

In-Situ Optical Determination of Thermomechanical Properties of ZnSe and ZnTe Crystals

At temperatures above 1/2 T(sub m), the generation and movement of dislocations may result due to the load created by the weight of the crystal itself The deformation may be expected to increase the line defect density and may result in generation of low angle grain boundaries, especially in the regions of the crystal attached to the ampule. It has often been suspected that elimination of this effect in space can improve crystallinity of crystals grown under microgravity conditions, however, a direct experimental proof of such relation is still missing. In this work we have designed and built a system of in-situ optical detection and measurement of the mechanical deformations of a crystal wafer under its own weight, and studied the deformation effects as a function of temperature. The results of the measurements for ZnSe and ZnTe crystal wafers will be presented.

Burger, A.↗

Potential Challenges in Near-Field Scanning Optical Microscopy for Space Applications

Near-field scanning optical microscopy is a relatively new but very powerful technique for obtaining several metrological parameters at nanometer range spatial resolution. It is logical to think deploying it into space applications like diagnostics of protein crystal growth under microgravity conditions. One may attempt to deploy existing instrumentation and expect some results. However, the existing technology and commercial instrumentation is tailored to ground based laboratory situations. Even in those laboratory conditions, the role of fluids (common in crystal growth), rough objects (such as a crystal under growth), etc. on the instrumentation is only recently being investigated. These aspects combined with effects of reduced gravity environment are going to make the problem more complex. These technological challenges must be tackled for meaningful system operation in space. Since the microscopy concept has not been attempted so far in space, all of the actual problems are unknown. Nevertheless, based on current literature, some possible problems and potential solutions are described here. One may use the discussion for system modification/optimization during initial use of this kind of microscopy in space.

Vikram, C. S.↗

Integration and use of Microgravity Research Facility: Lessons learned by the crystals by vapor transport experiment and Space Experiments Facility programs

The Crystals by Vapor Transport Experiment (CVTE) and Space Experiments Facility (SEF) are materials processing facilities designed and built for use on the Space Shuttle mid deck. The CVTE was built as a commercial facility owned by the Boeing Company. The SEF was built under contract to the UAH Center for Commercial Development of Space (CCDS). Both facilities include up to three furnaces capable of reaching 850 C minimum, stand-alone electronics and software, and independent cooling control. In addition, the CVTE includes a dedicated stowage locker for cameras, a laptop computer, and other ancillary equipment. Both systems are designed to fly in a Middeck Accommodations Rack (MAR), though the SEF is currently being integrated into a Spacehab rack. The CVTE hardware includes two transparent furnaces capable of achieving temperatures in the 850 to 870 C range. The transparent feature allows scientists/astronauts to directly observe and affect crystal growth both on the ground and in space. Cameras mounted to the rack provide photodocumentation of the crystal growth. The basic design of the furnace allows for modification to accommodate techniques other than vapor crystal growth. Early in the CVTE program, the decision was made to assign a principal scientist to develop the experiment plan, affect the hardware/software design, run the ground and flight research effort, and interface with the scientific community. The principal scientist is responsible to the program manager and is a critical member of the engineering development team. As a result of this decision, the hardware/experiment requirements were established in such a way as to balance the engineering and science demands on the equipment. Program schedules for hardware development, experiment definition and material selection, flight operations development and crew training, both ground support and astronauts, were all planned and carried out with the understanding that the success of the program science was as important as the hardware functionality. How the CVTE payload was designed and what it is capable of, the philosophy of including the scientists in design and operations decisions, and the lessons learned during the integration process are descussed.

Heizer, Barbara L.↗

Experiment 2: Vapor Transport Crystal Growth of Mercury Cadmium Telluride in Microgravity- USML-2

The new epitaxial growth experiments of Hg(l-x)Cd(x)Te on (100) CdTe substrates by chemical vapor transport (CVT), using HgI2 as a transport agent, were performed in the transient growth regime of this ternary, heteroepitaxial system at normal and reduced gravity during the USML-2 flight. The surface and interface morphology, the compositional and structural uniformity, and carrier mobility of the epitaxial layer and islands grown in microgravity are measurably improved relative to ground specimens. These observations demonstrate the effects of convective flow on the transport, deposition, and growth processes of this solid-vapor system even in the transient growth regime. The properties of the Hg(l-x)Cd(x)Te layer grown in a microgravity environment compare quite favorably to those of layers obtained by other techniques.

Wiedemeier, H.↗

Protein crystal growth aboard the U.S. Space Shuttle flights STS-31 and STS-32

Results obtained from the Shuttle flight STS-32 flown in January 1990, and preliminary results from the most recent Shuttle flight, STS-31, flown in April 1990, are presented. Crystals grown in microgravity environment include Canavalin, isocitrate lyase, human serum albumin, and Anti-HPr Fab. It is concluded that about 20 percent of proteins flown exhibit better morphologies or better quality data than their earth-grown counterparts. About 40 percent do not yield crystals at all and the remaining 40 percent yield crystals that are either too small for X-ray analysis or produce data of poorer quality than the best earth-grown crystals.

Delucas, Lawrence J.↗

Reciprocal Space Mapping of Macromolecular Crystals in the Laboratory

The technique of reciprocal space mapping applied to the physical measurement of macromolecular crystals will be described. This technique uses a triple axis diffractometer setup whereby the monochromator is the first crystal, the sample is the second and the third crystal (of the same material as the monochromator) analyzes the diffracted beam. The geometry is such that it is possible to separate mosaic volume effects from lattice strain effects. The deconvolution of the instrument parameters will also be addressed. Results from measurements at Brookhaven National Synchrotron Radiation Source carried out on microgravity and ground-grown crystals will be presented. The required beam characteristics for reciprocal space mapping are also ideal for topographic studies and the first topographs ever recorded from microgravity protein crystal samples will be shown. We are now working on a system which will enable reciprocal space mapping, mosaicity and topography studies to be carried out in the home laboratory. This system uses a rotating anode X-ray source to provide an intense beam then a Bartels double crystal, four reflection monochromator to provide the spectral and geometric beam conditioning necessary such that the instrument characteristics do not mask the measurement. This is coupled to a high precision diffractometer and sensitive detector. Commissioning data and first results from the system will be presented.

Snell, Edward H.↗

Crystal growth in a low gravity environment

Crystal growth in microgravity possesses several distinct technological advantages over earth-bound processes; containerless handling and reduction of density gradient driven as well as sedimentation flows. Experiments performed in space to date have been basically reproductions of processes currently used on earth and the results have clarified our understanding of crystal growth dynamics. In addition, both unresolved problems and areas requiring further study on earth have been identified. Future work in space processing of materials must address these areas of study as soon as possible if the full potential of a space environment to develop new techniques and materials is to be realized.

Carruthers, J. R.↗

Growing Single Crystals of Compound Semiconductors

Defect reduced by preventing melt/furnace contact and suppressing convention. Large crystals of compound semiconductors with few defects grown by proposed new method. Such materials as gallium arsenide and cadmium telluride produced, with quality suitable for very-large-scale integrated circuits or for large focal-plane arrays of photodetectors. Method used on small scale in Earth gravity, but needs microgravity to provide crystals large enough for industrial use.

Naumann, Robert J.↗

Investigation of the Influence of Microgravity on Transport Mechanisms in a Virtual Spaceflight Chamber: A Ground Based Program

In January 1992, the IML-1 FES experiment produced a set of classic experimental data and a 40 hour holographic "movie" of an ensemble of spheres in a fluid in microgravity. Because the data are in the form of holograms, we can study the three-dimensional distribution of particles with unprecedented detail by a variety of methods and for a wide variety of interests. The possession of the holographic movie is tantamount to having a complex experiment in space while working in an easily accessible laboratory on earth. The movie contains a vast amount of useful data, including residual g, g-jitter, convection and transport data, and particle fluid interaction data. The information content in the movie is so great that we have scarcely begun to tap into the data that is actually available in the more than 1000 holograms, each containing as much as 1000 megabytes of information. This ground-based project is exploiting this data and the concept of holographic storage of spaceflight data to provide an understanding of the effects of microgravity in materials processing. This paper provides the foundation, objectives, and status of the ground based project. The primary objective of this project is to advance the understanding of microgravity effects on crystal growth, convection in materials processing in the space environment, and complex transport phenomena at low Reynolds numbers. This objective is being achieved both experimentally and theoretically. Experiments are making use of existing holographic data recorded during the IML- I spaceflight. A parallel theoretical effort is providing the models for understanding the particle fields and their physics in the microgravity environment.

Trolinger, James D.↗

Experiment 1: Orbital Processing of High-Quality Zn-Alloyed CdTe Compound Semiconductors

Zinc-alloyed cadmium telluride (Zn:CdTe) crystals were grown in unit gravity and in microgravity for comparative analysis. Two crystals were grown on USML-1/STS-50 in 1992, and two additional crystals were grown on USML-2/STS-73 in 1995. The Crystal Growth Furnace (CGF) in the seeded Bridgman-Stockbarger crystal growth geometry was utilized on both missions. Crystals grown on USML-1/STS-50 were found to have solidified with partial wall contact due to the near-absence of the hydrostatic pressure in microgravity, a residual g-vector that was not axial, and the nonwetting sample/ampoule wetting conditions. Crystals grown on USML-2/STS-73 included: a sample/ampoule identical to the USML-1/STS-73 sample/ampoule, with the addition of a restraining spring to simulate hydrostatic pressure internally, and a tapered ampoule which accomplished 2.2 cm of crystal growth without wall contact. Infrared transmission of all ground and flight samples was found to be 63-66 percent, very close to the theoretical 66 percent, suggesting good stoichiometric control. Infrared microscopy confirmed that the primary precipitates were Te and their size (1-10 microns) and density suggested that the flight- and ground-base samples experienced similar thermal histories. Longitudinal macrosegregation, calculated using scaling analysis, was predicted to be low. Nearly diffusion controlled growth was achieved even in unit gravity and macrosegregation data could be fit with a diffusion controlled model. Radial segregation was monitored and was found to vary with fraction solidified, particularly through the shoulder region, where the sample cross section was varying significantly. It was also disturbed in the flight samples in regions where asymmetric wall contact was noted. In regions where a steady state was established, the radial segregation was invariant within our experimental measurement error. Flight samples were found to be much higher in structural perfection than samples processed in unit gravity under identical growth conditions. In regions where solidification had occurred without wall contact, the free surfaces evidenced virtually no twinning, although twins appeared in the flight samples in regions of wall contact and were pervasive in the ground samples. These results were confirmed using optical microscopy and synchrotron x-ray white beam topography. Full-width half-maximum rocking curve widths (FWHM), recorded in arc-seconds, were significantly reduced from 20 a-s (1 g) to 9 a-s (micro-g) for the best regions of the crystals. The 9 a-s (FWHM) rocking curve value in the unconfined flight samples equals the best value reported terrestrially for this material. The ground samples exhibited a fully developed (111)[110] dislocation mosaic structure, whereas dislocations within the flight samples were discrete and no mosaic structure was evident. The defect density was quantitatively reduced from 75,000 (1 g) to 800 (micro-g) +/-50 percent. Dislocation etch pit density results were confirmed using transmission synchrotron white beam and monochromated beam topography. The low defect density is thought to have resulted from the near absence of hydrostatic pressure, which allowed the molten boule to solidify with little or no wall contact. This minimized the transfer of hoop stresses during solidification and post-solidification processing.

Larson, D. J., Jr.↗

Multiple experiment processing furnace crystal growth facility (MEPF-CGF)

The Multiple Experiment Processing Furnace - Crystal Growth Facility (MEPF-CGF) will be an improved modular version of earlier generation directional solidification furnaces having the capability for processing larger samples, for on-orbit exchange of samples by a crew member, and for pre-mission reconfiguration to accommodate a variety of user requirements. The MEPF-CGF will provide the capability for crystal growth in the microgravity environment and will satisfy the processing requirements of the crystal growth community. The MEPF-CGF will be accommodated in the pressurized Spacelab Module (manned environment) on board the Space Shuttle Orbiter. The system will permit operation of the furnace with crew interaction and will utilize Spacelab/Shuttle resources such as experiment mounting provisions, electrical power, data, communication, heat rejection, and crew time.

Srinivas, R.↗

Simulation-Aided Design and Interpretation of Results of Microgravity-Based Solidification Experiments

The preparation and interpretation of microgravity experiments conducted on the International Space Station (ISS) can be challenging because of the remote location of the equipment. Although a “ground unit” is typically available on Earth, it is not located in the laboratory of the principal investigator. Furthermore, test experiments in the ground unit cannot fully duplicate heat transfer conditions of the weightless environment, and thus be a reliable reference for experiment design. Under such conditions, numerical simulations are a valuable tool both for preparing the experiments and interpreting the results obtained under terrestrial and micro-gravity conditions. In this work, we developed a detailed 3D model of the “SUBSA” furnace located at the ISS, and demonstrate its use in our present investigation which includes melt growth and vapor growth of InI crystals on the ISS. In 2002, the SUBSA furnace was designed and built for the growth of InSb crystals in the Microgravity Science Glovebox (MSG) at the ISS. The SUBSA furnace features a transparent section without heating elements, where the axial temperature gradient is high. In our present investigation, we have used the same furnace to grow four InI crystals from the melt, and two InI crystals from the vapor phase (2018-2021). InI crystals have ~20 times lower thermal conductivity than InSb crystals. As a result, during melt growth, the InI crystals were exposed to extremely high temperature gradients. To reduce the axial temperature gradient, we added external jackets made from high thermal conductivity material to the growth ampoules. The SUBSA furnace could not be modeled as asymmetric because of its rectangular shape and right-angled transparent section, which contains a convoluted geometry. The rectangular shape of the transparent section further complicates modelling of radiative heat transfer, which dominates in the zone. At present, numerical simulations are being conducted to resolve an apparent discrepancy between the readings of the 5 thermocouples located in the SUBSA furnace, and the observed position of the solid and molten material. The 3D simulation will be presented, along with the calibration and growth experiment results conducted in microgravity and in the SUBSA ground unit. The developed model should be useful for upcoming microgravity investigations planned to be conducted in the SUBSA facility.

V Riabov↗

Non-linear resonance of fluids in a crystal growth cavity

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

Wang, Francis C.↗

Microgravity science experiment integration - When the PI and the PED differ

This paper addresses issues related to the integration of principal investigators (PIs) and payload-element developers (PEDs) for conducting effective microgravity experiments. The Crystal Growth Furnace (CGF) is used as an example to demonstrate the key issues related to the integration of a PI's sample into a facility run by a different organization. Attention is given to the typical preflight timeline, documentation required for experimental implementation, and hardware deliverables. A flow chart delineates the payload-integration process flow, and PI inputs required for an experiment include equipment and procedure definitions, detailed design and fabrication of the experiment-specific equipment, and specifications of the contract-end item. The present analysis is of interest to the coordination of effective microgravity experiments on the Space Station Freedom that incorporate PIs and PEDs from different organizations.

Baer-Peckham, M. S.↗

Microgravity and Macromolecular Crystallography

Macromolecular crystal growth has been seen as an ideal experiment to make use of the reduced acceleration environment provided by an orbiting spacecraft. The experiments are small, simply operated and have a high potential scientific and economic impact. In this review we examine the theoretical reasons why microgravity should be a beneficial environment for crystal growth and survey the history of experiments on the Space Shuttle Orbiter, on unmanned spacecraft, and on the Mir space station. Finally we outline the direction for optimizing the future use of orbiting platforms.

Kundrot, Craig E.↗

Development of Optical Diagnostic Techniques for Microgravity Materials Processing

Materials processing including crystal growth, either under a gravity environment on ground or a microgravity environment in space, involves complicated phenomena of fluid motions in gas or liquid phases as well as interaction of various species. To obtain important physical insight, it is very necessary to provide gross-field optical diagnostics for monitoring various physical properties. Materials processing inhibits easy access by ordinary instruments and thus characterizing gross-field physical properties is very challenging. Typical properties of importance can be fluid velocity, temperature, and species concentration for fluids, and surface topology and defects for solids. Observing surface grow rate during crystal growth is also important. Material microstructures, i.e., integrity of crystal structures, is strongly influenced by the existence of thermally-induced flow as well as local nucleation of particles during solidification, which may act in many detrimental ways. In both ground-based and microgravity experiments, the nature of product property changes resulting from three-dimensional fluid or particle motions need be characterized. Gross-field diagnostics is thus required to identify their effects on product defects and process deficiencies. The quantitative visualization techniques can also be used for validation of numerical modeling. For optical nonintrusive gross-field diagnostic techniques, two approaches were developed as summer projects. One optical approach allows us to provide information of species concentration and temperature for monitoring in real time. The other approach, that is, the concept which is formulated for detection of surface topography measurement can provide unprecedented spatial resolution during crystal growth.

Cha, Soyoung Stephen↗

Physics of Hard Spheres Experiment (PhaSE) or "Making Jello in Space"

The Physics of Hard Spheres Experiment (PHaSE) is a highly successful experiment that flew aboard two shuttle missions to study the transitions involved in the formation of jellolike colloidal crystals in a microgravity environment. A colloidal suspension, or colloid, consists of fine particles, often having complex interactions, suspended in a liquid. Paint, ink, and milk are examples of colloids found in everyday life. In low Earth orbit, the effective force of gravity is thousands of times less than at the Earth's surface. This provides researchers a way to conduct experiments that cannot be adequately performed in an Earth-gravity environment. In microgravity, colloidal particles freely interact without the complications of settling that occur in normal gravity on Earth. If the particle interactions within these colloidal suspensions could be predicted and accurately modeled, they could provide the key to understanding fundamental problems in condensed matter physics and could help make possible the development of wonderful new "designer" materials. Industries that make semiconductors, electro-optics, ceramics, and composites are just a few that may benefit from this knowledge. Atomic interactions determine the physical properties (e.g., weight, color, and hardness) of ordinary matter. PHaSE uses colloidal suspensions of microscopic solid plastic spheres to model the behavior of atomic interactions. When uniformly sized hard spheres suspended in a fluid reach a certain concentration (volume fraction), the particle-fluid mixture changes from a disordered fluid state, in which the spheres are randomly organized, to an ordered "crystalline" state, in which they are structured periodically. The thermal energy of the spheres causes them to form ordered arrays, analogous to crystals. Seven of the eight PHaSE samples ranged in volume fraction from 0.483 to 0.624 to cover the range of interest, while one sample, having a concentration of 0.019, was included for instrument calibration.

Ling, Jerri S.↗