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At least 181 records · Page 10

Fluid Physics and Macromolecular Crystal Growth in Microgravity

The molecular structure of biological macromolecules is important in understanding how these molecules work and has direct application to rational drug design for new medicines and for the improvement and development of industrial enzymes. In order to obtain the molecular structure, large, well formed, single macromolecule crystals are required. The growth of macromolecule crystals is a difficult task and is often hampered on the ground by fluid flows that result from the interaction of gravity with the crystal growth process. One such effect is the bulk movement of the crystal through the fluid due to sedimentation. A second is buoyancy driven convection close to the crystal surface. On the ground the crystallization process itself induces both of these flows. Buoyancy driven convection results from density differences between the bulk solution and fluid close to the crystal surface which has been depleted of macromolecules due to crystal growth. Schlieren photograph of a growing lysozyme crystal illustrating a 'growth plume' resulting from buoyancy driven convection. Both sedimentation and buoyancy driven convection have a negative effect on crystal growth and microgravity is seen as a way to both greatly reduce sedimentation and provide greater stability for 'depletion zones' around growing crystals. Some current crystal growth hardware however such as those based on a vapor diffusion techniques, may also be introducing unwanted Marangoni convection which becomes more pronounced in microgravity. Negative effects of g-jitter on crystal growth have also been observed. To study the magnitude of fluid flows around growing crystals we have attached a number of different fluorescent probes to lysozyme molecules. At low concentrations, less than 40% of the total protein, the probes do not appear to effect the crystal growth process. By using these probes we expect to determine not only the effect of induced flows due to crystal growth hardware design but also hope to optimize crystallization hardware so that destructive flows are minimized both on the ground and in microgravity.

Pusey, M.↗

Crystal Growth of ZnSe by Physical Vapor Transport: A Modeling Study

Crystal growth from the vapor phase has various advantages over melt growth. The main advantage is from a lower processing temperature which makes the process more amenable in instances where the melting temperature of the crystal is high. Other benefits stem from the inherent purification mechanism in the process due to differences in the vapor pressures of the native elements and impurities, and the enhanced interfacial morphological stability during the growth process. Further, the implementation of Physical Vapor Transport (PVT) growth in closed ampoules affords experimental simplicity with minimal needs for complex process control which makes it an ideal candidate for space investigations in systems where gravity tends to have undesirable effects on the growth process. Bulk growth of wide band gap II-VI semiconductors by physical vapor transport has been developed and refined over the past several years at NASA MSFC. Results from a modeling study of PVT crystal growth of ZnSe arc reported in this paper. The PVI process is numerically investigated using both two-dimensional and fully three-dimensional formulation of the governing equations and associated boundary conditions. Both the incompressible Boussinesq approximation and the compressible model are tested to determine the influence of gravity on the process and to discern the differences between the two approaches. The influence of a residual gas is included in the models. The preliminary results show that both the incompressible and compressible approximations provide comparable results and the presence of a residual gas tends to measurably reduce the mass flux in the system. Detailed flow, thermal and concentration profiles will be provided in the final manuscript along with computed heat and mass transfer rates. Comparisons with the 1-D model will also be provided.

Ramachandran, Narayanan↗

Protein crystal growth in low gravity

The solubility and growth of the protein canavalin, and the application of the schlieren technique to study fluid flow in protein crystal growth systems were investigated. These studies have resulted in the proposal of a model to describe protein crystal growth and the preliminary plans for a long-term space flight experiment. Canavalin, which may be crystallized from a basic solution by the addition of hydrogen (H+) ions, was shown to have normal solubility characteristics over the range of temperatures (5 to 25 C) and pH (5 to 7.5) studies. The solubility data combined with growth rate data gathered from the seeded growth of canavalin crystals indicated that the growth rate limiting step is a screw dislocation mechanism. A schlieren apparatus was constructed and flow patterns were observed in Rochelle salt (sodium potassium tartrate), lysozyme, and canavalin. The critical parameters were identified as the change in density with concentration (dp/dc) and the change in index of refraction with concentration (dn/dc). Some of these values were measured for the materials listed. The data for lyrozyme showed non-linearities in plots of optical properties and density vs. concentration. In conjunction with with W. A. Tiller, a model based on colloid stability theory was proposed to describe protein crystallization. The model was used to explain observations made by ourselves and others. The results of this research has lead to the development for a preliminary design for a long-term, low-g experiment. The proposed apparatus is univeral and capable of operation under microprocessor control.

Feigelson, Robert S.↗

Crystal Growth Furnace - An overview of the system configuration and planned experiments on the first United States Microgravity Laboratory mission

Attention is given to the Crystal Growth Furnace (CGF) currently in the Level IV integration cycle at the Kennedy Space Center in preparation for its maiden flight on the first United States Microgravity Laboratory (USML-1) mission to be launched in May 1992. CGF was developed for NASA under the Microgravity Science and Application division programs at NASA Headquarters. An overview of the CGF system and the system configuration for the USML-1 mission are presented, and the planned on-orbit experiments are described. The four important scientific experiments selected from industry and educational institutions for the CGF USML-1 mission will enable a better understanding of the complex phenomena inherent in materials processing that will lead to the ultimate improvement of both processes and materials. Crystal growth by chemical vapor transport has resulted in improved growth conditions with crystal morphology, lower defect densities, and higher growth rates than terrestrially observed.

Srinivas, R.↗

Diagenetic Crystal Growth in the Murray Formation, Gale Crater, Mars

The Pahrump region (Gale Crater, Mars) marks a critical transition between sedimentary environments dominated by alluvial-to-fluvial materials associated with the Gale crater rim, and depositional environments fundamentally linked to the crater's central mound, Mount Sharp. At Pahrump, the Murray formation consists of an approximately 14-meter thick succession dominated by massive to finely laminated mudstone with occasional interbeds of cross-bedded sandstone, and is best interpreted as a dominantly lacustrine environment containing tongues of prograding fluvial material. Murray formation mudstones contain abundant evidence for early diagenetic mineral precipitation and its subsequent removal by later diagenetic processes. Lenticular mineral growth is particularly common within lacustrine mudstone deposits at the Pahrump locality. High-resolution MAHLI images taken by the Curiosity rover permit detailed morphological and spatial analysis of these features. Millimeter-scale lenticular features occur in massive to well-laminated mudstone lithologies and are interpreted as pseudomorphs after calcium sulfate. The distribution and orientation of lenticular features suggests deposition at or near the sediment-water (or sediment-air) interface. Retention of chemical signals similar to host rock suggests that original precipitation was likely poikilotopic, incorporating substantial amounts of the primary matrix. Although poikilotopic crystal growth is common in burial environments, it also occurs during early diagenetic crystal growth within unlithified sediment where high rates of crystal growth are common. Loss of original calcium sulfate mineralogy suggests dissolution by mildly acidic, later-diagenetic fluids. As with lenticular voids observed at Meridiani by the Opportunity Rover, these features indicate that calcium sulfate deposition may have been widespread on early Mars; dissolution of depositional and early diagenetic minerals is a likely source for both calcium and sulfate ion-enrichment in burial fluids that precipitated in ubiquitous late-stage hydrofracture veins

Kah, L. C.↗

Protein crystal growth and the International Space Station

Protein structural information plays a key role in understanding biological structure-function relationships and in the development of new pharmaceuticals for both chronic and infectious diseases. The Center for Macromolecular Crystallography (CMC) has devoted considerable effort studying the fundamental processes involved in macromolecular crystal growth both in a 1-g and microgravity environment. Results from experiments performed on more than 35 U.S. space shuttle flights have clearly indicated that microgravity can provide a beneficial environment for macromolecular crystal growth. This research has led to the development of a new generation of pharmaceuticals that are currently in preclinical or clinical trials for diseases such as cutaneous T-cell lymphoma, psoriasis, rheumatoid arthritis, AIDS, influenza, stroke and other cardiovascular complications. The International Space Station (ISS) provides an opportunity to have complete crystallographic capability on orbit, which was previously not possible with the space shuttle orbiter. As envisioned, the x-ray Crystallography Facility (XCF) will be a complete facility for growing protein crystals; selecting, harvesting, and mounting sample crystals for x-ray diffraction; cryo-freezing mounted crystals if necessary; performing x-ray diffraction studies; and downlinking the data for use by crystallographers on the ground. Other advantages of such a facility include crystal characterization so that iterations in the crystal growth conditions can be made, thereby optimizing the final crystals produced in a three month interval on the ISS.

STS Shuttle Project↗

Growing protein crystals in microgravity - The NASA Microgravity Science and Applications Division (MSAD) Protein Crystal Growth (PCG) program

In collaboration with a medical researcher at the University of Alabama at Birmingham, NASA's Marshall Space Flight Center in Huntsville, Alabama, under the sponsorship of the Microgravity Science and Applications Division (MSAD) at NASA Headquarters, is continuing a series of space experiments in protein crystal growth which could lead to innovative new drugs as well as basic science data on protein molecular structures. From 1985 through 1992, Protein Crystal Growth (PCG) experiments will have been flown on the Space Shuttle a total of 14 times. The first four hand-held experiments were used to test hardware concepts; later flights incorporated these concepts for vapor diffusion protein crystal growth with temperature control. This article provides an overview of the PCG program: its evolution, objectives, and plans for future experiments on NASA's Space Shuttle and Space Station Freedom.

Herren, B.↗

The Effect of a Rotating Magnetic Field on Flow Stability During Crystal Growth

The effect of a rotating magnetic field on the stability of flow in crystal growth configurations has been experimentally modeled using liquid gallium contained in a finite cylinder and heated from below. Several distinct flow regions were determined as a function of the Rayleigh and Hartmann numbers. At low values of the Rayleigh and Hartmann numbers, a region of stationary flow exists. As the rotating magnetic field is increased, the critical Rayleigh number bounding the stationary flow region can increase by a factor of 10. However, the rotating magnetic field itself induces an instability at a critical value of the Hartmann number independent of the Rayleigh number. In the stationary flow region, the rotating magnetic field can induce fluid motion with velocities several orders of magnitude larger than typical semiconductor crystal growth velocities. Thus, a rotating magnetic field can be used to achieve the benefits of forced convection without triggering deleterious instabilities.

Volz, Martin P.↗

Novel protein crystal growth technology: Proof of concept

A technology for crystal growth, which overcomes certain shortcomings of other techniques, is developed and its applicability to proteins is examined. There were several unknowns to be determined: the design of the apparatus for suspension of crystals of varying (growing) diameter, control of the temperature and supersaturation, the methods for seeding and/or controlling nucleation, the effect on protein solutions of the temperature oscillations arising from the circulation, and the effect of the fluid shear on the suspended crystals. Extensive effort was put forth to grow lysozyme crystals. Under conditions favorable to the growth of tetragonal lysozyme, spontaneous nucleation could be produced but the number of nuclei could not be controlled. Seed transfer techniques were developed and implemented. When conditions for the orthorhombic form were tried, a single crystal 1.5 x 0.5 x 0.2 mm was grown (after in situ nucleation) and successfully extracted. A mathematical model was developed to predict the flow velocity as a function of the geometry and the operating temperatures. The model can also be used to scaleup the apparatus for growing larger crystals of other materials such as water soluble non-linear optical materials. This crystal suspension technology also shows promise for high quality solution growth of optical materials such as TGS and KDP.

Nyce, Thomas A.↗

High-Precision Temperature Control of a Crystal Growth Furnace at 1,500 C

For crystal growth of semiconductor materials a short-term temperature stability of 0.1 C at 1500 C is one of the essential parameters to be addressed for achieving high-quality crystals. Hence, for temperature monitoring and control with high precision in a floating zone furnace two sets of thermo-sensors, type B thermocouples and optical fibre thermometers, have been implemented and successfully operated in the furnace for more than 2000 h. The optical fibre thermometers consist of an optical system made of sapphire (two fibres plus a prism in between for deflection) and transmit the infra-red radiation of the heater to the outside of the hot core of the furnace for pyrometric temperature measurement. A dedicated control algorithm has been set up which controlled the power settings to the individual heaters. Both sensor types showed no degradation after this period and yielded a short-term stability at 1200 C of 0.05 C (optical fibre thermometers), respectively 0.08 C (thermocouples).

Stenzel, Ch.↗

Convection analysis on various crystal growth systems

Specific work done during an indicated contract period was reviewed. An extensive survey of crystal growth literature and related topics was accomplished during this time. Specific attention was given to those areas dealing with the effects of transport phenomena on crystal growth. Critical evaluations of growth techniques were made. Techniques studied included closed tube vapor growth, open reactor vapor growth, melt growth and solution growth.

Source record↗

Ground-based research of crystal growth of II-VI compound semiconductors by physical vapor transport

Ground-based investigation of the crystal growth of II-VI semiconductor compounds, including CdTe, CdS, ZnTe, and ZnSe, by physical vapor transport in closed ampoules was performed. The crystal growth experimental process and supporting activities--preparation and heat treatment of starting materials, vapor partial pressure measurements, and transport rate measurements are reported. The results of crystal characterization, including microscopy, microstructure, optical transmission photoluminescence, synchrotron radiation topography, and chemical analysis by spark source mass spectrography, are also discussed.

Volz, M. P.↗

Quantitative determination of zero-gravity effects on electronic materials processing germanium crystal growth with simultaneous interface demarcation. Experiment MA-060

Experiment MA-060 was designed to establish the crystal growth and segregation characteristics of a melt in a directional solidification configuration under near zero-g conditions. The interface demarcation technique was incorporated into the experiment since it constitutes a unique tool for recording the morphology of the growth rate throughout solidification, and for establishing an absolute time reference framework for all stages of the solidification process. An extensive study was performed of the germanium crystals grown during the Apollo-Soyuz Test Project mission. It was found that single crystal growth was achieved and that the interface demarcation functioned successfully. There was no indication that convection driven by thermal or surface tension gradients was present in the melt. The gallium segregation, in the absence of gravity, was found to be fundamentally different in its initial and its subsequent stages from that of the ground-based tests. None of the existing theoretical models for growth and segregation can account for the observed segregation behavior in the absence of gravity.

Gatos, H. C.↗

The effect of aspect ratio and fluid flow on crystal growth

Supersaturated solutions were conditioned at different aspect ratios before crystal growth. The conditioned solutions were poured out into a dish to initiate crystal nucleation and growth. The rate of growth was measured microscopically and found to depend upon the aspect ratio. Secondly, the number and size of crystals formed was found to depend upon the aspect ratio. The data support the above conclusion, but do not prove it.

Barber, Patrick G.↗

Effects of Kinetic Roughening and Liquid-Liquid Phase Transition on Lysozyme Crystal Growth Velocities

We measured the growth velocities of the (110) face of tetragonal lysozyme, V (centimeters per second), at four different concentrations, c (milligrams per milliliter), as the solution temperature, T (Centigrade), was reduced. For a broad range of T dependent on c, we find that the growth velocities increased as the solution temperature was reduced. The initial increase in V is well characterized by the 2D nucleation model for crystal growth, yielding the magnitude of an effective barrier for growth, gamma(sub s) = 1.2 plus or minus 0.1 x 10(exp -13) erg/molecule. Below certain temperatures, T(sub cr), dependent on c, however, a kinetic roughening hypothesis that considers the continuous addition of molecules anywhere on the crystal surface better describes the observed growth velocities. The application of the continuous growth model, up to the solution cloud-point temperatures, T(sub cl), enabled the determinations of the crossover concentration, c(sub r), from estimated values of T(sub cr). For all conditions presented, we find that the crossover from growth by 2D nucleation to continuous addition occurs at a supersaturation, sigma (sub c), = 2.0 plus or minus 0.1. Moreover, we find the energy barrier for the continuous addition, E(sub c), within the temperature range T(sub cl) less than T less than T less than T (sub cr), to be 6 plus or minus 1 x 10(exp -13) erg/molecule. Further reduction of T below approximately 2-3 C of T(sub cl), also revealed a rapid slowing of crystal growth velocities. From quasi-elastic light scattering investigations, we find that the rapid diminishment of crystal growth velocities can be accounted for by the phase behavior of lysozyme solutions. Namely, we find the reversible formation of dense fluid proto-droplets comprised of lysozyme molecules to occur below approximately 0.3 C of T(sub cl). Hence, the rapid slowing of growth velocities may occur as a result of the sudden depletion of "mobile" molecules within crystal growth solutions as dense fluid proto-droplets form.

Gorti, Sridhar↗

Characterization of the Bridgman crystal growth process by radiographic imaging

Elemental (Ge) and alloy (PbSnTe) crystal growth that is monitored via radiography to reveal both the interface position and the shape in real time is discussed for both seeded and unseeded growth. It is concluded that the interface position and the actual growth rate of a Bridgman grown crystal is dependent on the growth conditions. The actual growth rate which is a strong function of the degree of supercooling exceeded the pull rate by a factor of greater than two. The interface shape changed from concave to flat to convex during the growth.

Fripp, Archibald L.↗

Mechanism of shape symmetry breaking in surfactant-mediated crystal growth

We present a dynamical model of crystal growth, in which it is possible to reliably achieve asymmetric products, beginning from symmetric initial conditions and growing within an isotropic environment. The asymmetric growth is the result of a positive feedback mechanism that amplifies the effect of thermal fluctuations in the coverage of surfactants on the growing crystalline facets. Within our simple model, we are able to understand the kinetic and thermodynamic factors involved in both the onset of symmetry breaking and the persistence of anisotropic growth. We demonstrate that the mechanism is general by studying models with increasing complexity. We argue that this mechanism of symmetry breaking underpins observations of colloidal, seed-mediated syntheses of single crystalline metal nanorods capped with strongly interacting surfactants. The parameters within our model are related to experimental observables such as the concentration, hydrophobicity, and binding strength of the surfactants, which suggests a potential route to optimize the yield of asymmetric products in colloidal nanoparticle syntheses.

Oaks-Leaf, Sam↗

Containerless protein crystal growth method

A method of growing protein crystals from levitated drops is introduced and unique features of containerless approach in 1-g and micro-G laboratories are discussed. Electrostatic multidrop levitation system which is capable of simultaneous four drop levitation is described. A method of controlling protein saturation level in a programmed way is introduced and discussed. Finally, some of the unique features of containerless approach of protein crystal growth in space are discussed and summarized.

Rhim, Won-Kyu↗