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At least 109 records · Page 6

Physical Vapor Transport of Mercurous Chloride Crystals: Design of a Microgravity Experiment

Flow field characteristics predicted from a computational model show that the dynamical state of the flow, for practical crystal growth conditions of mercurous chloride, can range from steady to unsteady. Evidence that the flow field can be strongly dominated by convection for ground-based conditions is provided by the prediction of asymmetric velocity profiles bv the model which show reasonable agreement with laser Doppler velocimetry experiments in both magnitude and planform. Unsteady flow is shown to be correlated with a degradation of crystal quality as quantified by light scattering pattern measurements, A microgravity experiment is designed to show that an experiment performed with parameters which yield an unsteady flow becomes steady (diffusive-advective) in a microgravity environment of 10(exp -3) g(sub 0) as predicted by the model, and hence yields crystals with optimal quality.

Duval, W, M. B.↗

Growth and Characteristics of Bulk Single Crystals Grown from Solution on Earth and in Microgravity

The growth of crystals has been of interest to physicists and engineers for a long time because of their unique properties. Single crystals are utilized in such diverse applications as pharmaceuticals, computers, infrared detectors, frequency measurements, piezoelectric devices, a variety of high technology devices and sensors. Solution crystal growth is one of the important techniques to grow a variety of crystals when the material decomposes at the melting point and a suitable solvent is available to make a saturated solution at a desired temperature. In this chapter an attempt is made to give some fundamentals of growing crystals from solution including improved designs of various crystallizers. Since the same solution crystal growth technique could not be used in microgravity, authors had proposed a new cooled sting technique to grow crystals in space. Authors? experiences of conducting two space shuttle experiments relating to solution crystal growth are also detailed in this work. The complexity of these solution growth experiments to grow crystals in space are discussed. These happen to be some of the early experiments performed in space, and various lessons learned are described. A brief discussion of protein crystal growth that also shares basic principles of solution growth technique is given along with some flight hardware information for its growth in microgravity.

Aggarwal, M. D.↗

Solution growth of Triglycine Sulfate (TGS) crystals on the International Microgravity Laboratory (IML-1)

An experiment was planned for the International Microgravity Laboratory (IML-1) to be launched around Feb. 1991. Crystals of triglycine sulfate (TGS) will be grown by low temperature solution crystal growth technique using a multiuser facility called Fluid Experiment System (FES). A special cooled sting technique of solution crystal growth will be used where heat is extracted from the seed crystal through a semi-insulating sting, thereby creating the desired supersaturation near the growing crystal. Also, a holocamera will be used to provide tomography of the three dimensional flow field and particle image displacement velocimetry to monitor the convective flows.

Lal, Ravi B.↗

Protein Crystal Movements and Fluid Flows During Microgravity Growth

The growth of protein crystals suitable for x-ray crystal structure analysis is an important topic. The quality (perfection) of protein crystals is now being evaluated by mosaicity analysis (rocking curves) and x-ray topographic images as well as the diffraction resolution limit and overall data quality. In yet another study, use of hanging drop vapour diffusion geometry on the IML-2 shuttle mission showed, again via CCD video monitoring, growing apocrustacyanin C(sub 1) protein crystal executing near cyclic movement, reminiscent of Marangoni convection flow of fluid, the crystals serving as "markers" of the fluid flow. A review is given here of existing results and experience over several microgravity missions. Some comment is given on gel protein crystal growth in attempts to 'mimic' the benefits of microgravity on Earth. Finally, the recent new results from our experiments on the shuttle mission LMS are described. These results include CCD video as well as interferometry during the mission, followed, on return to Earth, by reciprocal space mapping at the NSLS, Brookhaven, and full X-ray data collection on LMS and Earth control lysozyme crystals. Diffraction data recorded from LMS and ground control apocrustacyanin C(sub 1) crystals are also described.

Boggon, Titus J.↗

Growth of zinc selenide crystals by physical vapor transport in microgravity

The growth of single crystals of zinc selenide was carried out by both closed ampoule physical vapor transport and effusive ampoule physical vapor transport (EAPVT). The latter technique was shown to be a much more efficient method for the seeded growth of zinc selenide, resulting in higher transport rates. Furthermore, EAPVT work on CdTe has shown that growth onto /n11/ seeds is advantageous for obtaining reduced twinning and defect densities in II-VI sphalerite materials.

Rosenberger, Franz↗

Protein crystal growth results from the United States Microgravity Laboratory-1 mission

Protein crystal growth experiments have been performed by this laboratory on 18 Space Shuttle missions since April, 1985. In addition, a number of microgravity experiments also have been performed and reported by other investigators. These Space Shuttle missions have been used to grow crystals of a variety of proteins using vapor diffusion, liquid diffusion, and temperature-induced crystallization techniques. The United States Microgravity Laboratory - 1 mission (USML-1, June 25 - July 9, 1992) was a Spacelab mission dedicated to experiments involved in materials processing. New protein crystal growth hardware was developed to allow in orbit examination of initial crystal growth results, the knowledge from which was used on subsequent days to prepare new crystal growth experiments. In addition, new seeding hardware and techniques were tested as well as techniques that would prepare crystals for analysis by x-ray diffraction, a capability projected for the planned Space Station. Hardware that was specifically developed for the USML-1 mission will be discussed along with the experimental results from this mission.

Delucas, Lawrence J.↗

Preliminary Work in Obtaining Site-Directed Mutants of Hen Egg White Lysozyme

Protein crystal growth studies are recognized as a critical endeavor in the field of molecular biotechnology. The scientific applications of this field include the understanding of how enzymes function and the accumulation of accurate information of atomic structures, a key factor in the process of rational drug design. NASA has committed substantial investment and resources to the field of protein crystal growth and has conducted many microgravity protein crystal growth experiments aboard shuttle flights. Crystals grown in space tend to be larger, denser and have a more perfect habit and geometry. These improved properties gained in the microgravity environment of space result largely from the reduction of solutal convection, and the elimination of sedimentation at the growing crystal surface. Shuttle experiments have yielded many large, high quality crystals that are suitable for high resolution X-ray diffraction analysis. Examples of biologically important macromolecules which have been successfully crystallized during shuttle missions include: lysozyme, isocitrate lyase, gamma-interferon, insulin, human serum albumin and canavalin. Numerous other examples are also available. In addition to obtaining high quality crystals, investigators are also interested in learning the mechanisms by which the growth events take place. Crystallization experiments indicate that for the enzyme HEWL, measured growth rates do not follow mathematical models for 2D nucleation and dislocation-led growth of tetragonal protein crystals. As has been suggested by the laboratory of Marc L. Pusey, a possible explanation for the disagreement between observation and data is that HEWL tetraconal crystals form by aggregated units of lysozyme in supersaturated solutions. Surface measurement data was shown to fit very well with a model using an octamer unit cell as the growth unit. According to this model, the aggregation pathway and subsequent crystal growth is described by: monomer < ------ > dimer < ------- > tetramer < ------ > octamer < ------ > higher order. It is believed that multimer aggregation of lysozyme occurs by interaction at specific binding sites on the surface of the protein crystals. If the presence of discrete binding sites and the aggregation hypothesis is true, then it follows that the alteration of the binding site(s) should have significant effect on the measurements obtained during growth experiments. Site-directed mutagenesis allows the specific alteration of proteins by replacement, deletion or addition of specific amino acid residues. This report outlines the approach for this strategy and the progress made thus far toward that end.

Holmes, Leonard D.↗

Using Magnetic Fields to Control Convection during Protein Crystallization: Analysis and Validation Studies

The effect of convection during the crystallization of proteins is not very well understood. In a gravitational field, convection is caused by crystal sedimentation and by solutal buoyancy induced flow and these can lead to crystal imperfections. While crystallization in microgravity can approach diffusion limited growth conditions (no convection), terrestrially strong magnetic fields can be used to control fluid flow and sedimentation effects. In this work, we develop the analysis for magnetic flow control and test the predictions using analog experiments. Specifically, experiments on solutal convection in a paramagnetic fluid were conducted in a strong magnetic field gradient using a dilute solution of Manganese Chloride. The observed flows indicate that the magnetic field can completely counter the settling effects of gravity locally and are consistent with the theoretical predictions presented. This phenomenon suggests that magnetic fields may be useful in mimicking the microgravity environment of space for some crystal growth ana biological applications where fluid convection is undesirable.

Ramachandran, N.↗

Recent results and new hardware developments for protein crystal growth in microactivity

Protein crystal growth experiments have been performed on 16 space shuttle missions since April, 1985. The initial experiments utilized vapor diffusion crystallization techniques similar to those used in laboratories for earth-based experiments. More recent experiments have utilized temperature induced crystallization as an alternative method for growing high quality protein crystals in microgravity. Results from both vapor diffusion and temperature induced crystallization experiments indicate that proteins grown in microgravity may be larger, display more uniform morphologies, and yield diffraction data to significantly higher resolutions than the best crystals of these proteins grown on earth.

Delucas, L. J.↗

Growth of InSb and InI Crystals on Earth and in Microgravity

During the past 40 years, dozens of semiconductor crystal growth experiments have been conducted in space laboratories. The subsequent analysis of the space-grown crystals revealed (i) that weak convection existed in virtually all melt-growth experiments, (ii) de-wetting significantly reduced the level of stress-induced defects, and (iii) particularly encouraging results were obtained in vapor-growth experiments. In 2002, following a decade of ground based research in growing doped Ge and GaSb crystals, a series of crystal growth experiments was performed at the ISS, within the SUBSA (Solidification Using a Baffle in Sealed Ampoules) investigation. Te- and Zn-doped InSb crystals were grown from the melt. The specially designed furnace provided a side-view of the melt and precise seeding measurement of the growth rate. At present, under sponsorship of CASIS (Center for the Advancement of Science in Space, www.iss-casis.org), we are conducting ground-based experiments with indium mono-iodide (InI) in preparation for the "SUBSA II" ISS investigation, planned for 2017. The experiments include: i) Horizontal Bridgman (HB) growth and ii) Vapor Transport (VT) growth. Finite element modeling will also be conducted, to optimize the design of the flight ampoules, for vapor and melt growth.

Ostrogorsky, A. G.↗

Synchrotron X-Ray Reciprocal Space Mapping, Topography and Diffraction Resolution Studies of Macromolecular Crystal Quality

A comprehensive study of microgravity and ground grown chicken egg white lysozyme crystals is presented using synchrotron X-ray reciprocal space mapping, topography techniques and diffraction resolution. Microgravity crystals displayed, on average, reduced intrinsic mosaicities but no differences in terms of stress over their earth grown counterparts. Topographic analysis revealed that in the microgravity case the majority of the crystal was contributing to the peak of the reflection at the appropriate Bragg angle. In the earth case at the diffraction peak only a small volume of the crystal contributed to the intensity. The techniques prove to be highly complementary with the reciprocal space mapping providing a quantitative measure of the crystal mosaicity and stress (or variation in lattice spacing) and topography providing a qualitative overall assessment of the crystal in terms of its X-ray diffraction properties. Structural data collection was also carried out both at the synchrotron and in the laboratory.

Boggon, T. J.↗

Physical and Structural Studies on the Cryo-cooling of Insulin Crystals

Reflection profiles were analyzed from microgravity-(mg) and earth-grown insulin crystals to measure mosaicity (h) and to reveal mosaic domain structure and composition. The effects of cryocooling on single and multi-domain crystals were compared. The effects of cryocooling on insulin structure were also re-examined. Microgravity crystals were larger, more homogeneous, and more perfect than earth crystals. Several mg crystals contained primarily a single mosaic domain with havg of 0.005deg. The earth crystals varied in quality and all contained multiple domains with havg of 0.031deg. Cryocooling caused a 43-fold increase in h for mg crystals (havg=0.217deg) and an %fold increase for earth crystals (havg=0.246deg). These results indicate that very well-ordered crystals are not completely protected from the stresses associated with cryocooling, especially when structural perturbations occur. However, there were differences in the reflection profiles. For multi-mosaic domain crystals, each domain individually broadened and separated from the other domains upon cryo-cooling. Cryo-cooling did not cause an increase in the number of domains. A crystal composed of a single domain retained this domain structure and the reflection profiles simply broadened. Therefore, an improved signal-to-noise ratio for each reflection was measured from cryo-cooled single domain crystals relative to cryo-cooled multi-domain crystals. This improved signal, along with the increase in crystal size, facilitated the measurement of the weaker high- resolution reflections. The observed broadening of reflection profiles indicates increased variation in unit cell dimensions which may be linked to cryo-cooling-associated structural changes and disorder.

Lovelace, J.↗

A study of TRIGLYCINE SULFATE (TGS) crystals from the International Microgravity Laboratory Mission (IML-1)

Preliminary evaluation of the data was made during the hologram processing procedure. A few representative holograms were selected and reconstructed in the HGS; photographs of sample particle images were made to illustrate the resolution of all three particle sizes. Based on these evaluations slight modifications were requested in the hologram processing procedure to optimize the hologram exposure in the vicinity of the crystal. Preliminary looks at the data showed that we are able to see and track all three sizes of particles throughout the chamber. Because of the vast amount of data available in the holograms, it was recommended that we produce a detailed data reduction plan with prioritization on the different types of data which can be extracted from the holograms.

Lal, R. B.↗

Nucleation of Crystals From Solution in Microgravity (USML-1 Glovebox (GBX) Investigation)

A new method for initiating nucleation from solutions in microgravity which avoids nucleation on container walls and other surfaces is described. This method consists of injecting a small quantity of highly concentrated, heated solution into the interior of a lightly supersaturated, cooler host gowth solution. It was tested successfully on USML-I, producing a large number of LAP crystals whose longest dimension averaged 1 mm.

Kroes, Roger L.↗

Protein crystal growth; Proceedings of the First International Conference, Stanford University, CA, August 14-16, 1985

Papers are presented on mechanisms of nucleation and growth of protein crystals, the role of purification in the crystallization of proteins and nucleic acids, and the effect of chemical impurities in polyethylene glycol on macromolecular crystallization. Also considered are growth kinetics of tetragonal lysozyme crystals, thermodynamic and kinetic considerations for crystal growth of complex molecules from solution, protein single-crystal growth under microgravity, and growth of organic crystals in a microgravity environment. Papers are also presented on preliminary investigations of protein crystal growth using the Space Shuttle, convective diffusion in protein crystal growth, and the growth and characterization of membrane protein crystals.

Feigelson, R. S.↗

Structural Biology of Proteins of the Multi-enzyme Assembly Human Pyruvate Dehydrogenase Complex

Objectives and research challenges of this effort include: 1. Need to establish Human Pyruvate Dehydrogenase Complex protein crystals; 2. Need to test value of microgravity for improving crystal quality of Human Pyruvate Dehydrogenase Complex protein crystals; 3. Need to improve flight hardware in order to control and understand the effects of microgravity on crystallization of Human Pyruvate Dehydrogenase Complex proteins; 4. Need to integrate sets of national collaborations with the restricted and specific requirements of flight experiments; 5. Need to establish a highly controlled experiment in microgravity with a rigor not yet obtained; 6. Need to communicate both the rigor of microgravity experiments and the scientific value of results obtained from microgravity experiments to the national community; and 7. Need to advance the understanding of Human Pyruvate Dehydrogenase Complex structures so that scientific and commercial advance is identified for these proteins.

Source record↗

Crystallization of Hard Sphere Colloids in Microgravity: Results of the Colloidal Disorder-Order Transition, CDOT on USML-2

Classical hard spheres have long served as a paradigm for our understanding of the structure of liquids, crystals, and glasses and the transitions between these phases. Ground-based experiments have demonstrated that suspensions of uniform polymer colloids are near-ideal physical realizations of hard spheres. However, gravity appears to play a significant and unexpected role in the formation and structure of these colloidal crystals. In the microgravity environment of the Space Shuttle, crystals grow purely via random stacking of hexagonal close-packed planes, lacking any of the face-centered cubic (FCC) component evident in crystals grown in 1 g beyond melting and allowed some time to settle. Gravity also masks 33-539 the natural growth instabilities of the hard sphere crystals which exhibit striking dendritic arms when grown in microgravity. Finally, high volume fraction "glass" samples which fail to crystallize after more than a year in 1 g begin nucleation after several days and fully crystallize in less than 2 weeks on the Space Shuttle.

Zhu, Ji-Xiang↗