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At least 757 records · Page 42

Results of the TTF-TCNQ- and the calcium carbonate-crystallization on the Long Duration Exposure Facility

Experiment AO139A on the Long Duration Exposure Facility (LDEF) carried four large containers into orbit for five years with crystal growth solutions for lead sulfide, calcium carbonate, and tetra thiafulvalene- tetra cyanoquino methane (TTF-TCNQ). The LDEF was in excellent condition after the long orbital stay, and although the temperature data was lost, the experiment program had been working since the valves in all containers were opened. All four experiments produced crystals; however, they were of varying quality. The calcium carbonate crystals had the best appearance. The TTF-TCNQ crystals were packed together near the valve openings of the container. When taken apart, the single crystals showed some unusual morphological properties. X-ray investigations as well as conductivity measurements on the long duration space grown TTF-TCNQ crystals are presented, and pictures of the calcium carbonate are shown. Comparisons are made with previous space solution growth experiments on the European Spacelab Mission and the Apollo-Soyuz Test Project.

Nielsen, Kjeld Flemming↗

Stratospheric ice crystals

In situ sampling of the crystals is described with a NASA high-altitude aircraft to characterize the presence of ice particles and their role in Antarctic ozone chemistry. A NASA wire impactor was employed to collect the crystals, and the device was modified to permit Formvar crystal replication. The size distributions of the columnar crystals show that at the highest altitude the the smallest crystals are collected. The crystals provide surface area for heterogeneous chemical reactions as well as the removal of moisture and particles from the stratosphere and its ozone-related components.

Goodman, Jindra↗

The effects of small ice crystals on the infrared radiative properties of cirrus clouds

To be successful in the development of satellite retrieval methodologies for the determination of cirrus cloud properties, we must have fundamental scattering and absorption data on nonspherical ice crystals that are found in cirrus clouds. Recent aircraft observations (Platt et al. 1989) reveal that there is a large amount of small ice particles, on the order of 10 micron, in cirrus clouds. Thus it is important to explore the potential differences in the scattering and absorption properties of ice crystals with respect to their sizes and shapes. In this study the effects of nonspherical small ice crystals on the infrared radiative properties of cirrus clouds are investigated using light scattering properties of spheroidal particles. In Section 2, using the anomalous diffraction theory for spheres and results from the exact spheroid scattering program, efficient parameterization equations are developed for calculations of the scattering and absorption properties for small ice crystals. Parameterization formulas are also developed for large ice crystals using results computed from the geometric ray-tracing technique and the Fraunhofer diffraction theory for spheroids and hexagonal crystals. This is presented in Section 3. Finally, applications to the satellite remote sensing are described in Section 4.

Takano, Y.↗

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.↗

Transport phenomena in the crystallization of lysozyme by osmotic dewatering and liquid-liquid diffusion in low gravity

Two methods of protein crystallization, osmotic dewatering and liquid-liquid diffusion, like the vapor diffusion (hanging-drop and sessile-drop) methods allow a gradual approach to supersaturation conditions. The crystallization of hen egg-white lysozyme, an extensively characterized protein crystal, in the presence of sodium chloride was used as an experimental model with which to compare these two methods in low gravity and in the laboratory. Comparisons of crystal growth rates by the two methods under the two conditions have, to date, indicated that the rate of crystal growth by osmotic dewatering is nearly the same in low gravity and on the ground, while much faster crystal growth rates can be achieved by the liquid-liquid diffusion method in low gravity.

Todd, Paul↗

Ground based experiments on the growth and characterization of L-Arginine Phosphate (LAP) crystals

L-Arginine Phosphate (LAP) is a new nonlinear optical material with higher efficiency for harmonic generation compared to KDP. Crystals of LAP were grown in the laboratory from supersaturated solutions by temperature lowering technique. Investigations revealed the presence of large dislocation densities inside the crystals which are observed to produce refractive index changes causing damage at high laser powers. This is a result of the convection during crystal growth from supersaturated solutions. It is proposed to grow these crystals in a diffusion controlled growth condition under microgravity environment and compare the crystals grown in space with those grown on ground. Physical properties of the solutions needed for modelling of crystal growth are also presented.

Rao, S. M.↗

Colorimetric qualification of shear sensitive liquid crystal coatings

The work that has been done to date on the Shear Sensitive Liquid Crystal Project demonstrated that cholesteric liquid crystal coatings respond to both the direction and magnitude of a shearing force. The response of the coating is to selectively scatter incident white light into a spectrum of colors. Discernible color changes at a fixed angle of observation and illumination are the result of an applied shear stress. The intention was to be able to convert these observable color patterns from a flow visualization technique into a quantitative tool. One of the earlier intentions was to be able to use liquid crystals in dynamic flow fields. This was assumed possible because liquid crystals had made it possible to visualize transients in surface shear forces. Although the transients were visualized by color changes to an order one micro second, the time response of a coating to align to a shearing force is dependent on the magnitude of the change between its initial and final states. Unfortunately, the response is not instantaneous. It is for this reason any future attempt at quantifying the magnitude and directions of a shearing force are limited to surface shear stress vector fields in three dimensional steady state flows. This limitation does not significantly detract from the utility of liquid crystal coatings. The measurement of skin friction in the study of transition on wings, prediction of drag forces, performance assessment, and the investigation of boundary layer behavior is of great importance in aerodynamics. There exist numerous examples of techniques for the measurement of surface shear stress. Most techniques require arduous calibrations and necessitate extensive preparation of the receiving surfaces. However, the main draw back of instruments such as Preston tubes, hot films, buried wire gages, and floating element balances is that they only provide a point measurement. The advantages of capturing global shear data would be appreciable when compared with conventional point measurement sensors. It has yet to be determined if a repeatable correlation exists between the measured color of a liquid crystal coating and the magnitude/directional components of a shear vector imposed onto it.

Muratore, Joseph J., Jr.↗

On line quantification of crystal surfaces by stereo imaging

The shape of an interface while a crystal is growing inside a crystal growth furnace is an important measurement to assess the crystal quality on-line. If the crystal surface can be visualized by video or x ray imaging, the interface shape can be determined by the stereo image processing techniques. This paper presents a methodology to determine the shape of the solid-melt interface by stereo based imaging techniques while the crystal is growing inside a transparent furnace. The methodology generates qualitative shape information provided that a good pair of stereo images of the interface can be captured. For a quantitative shape description, i.e., for the determination of interface points with respect to a fixed coordinate frame, both cameras must be calibrated. This paper illustrates the methodology for qualitative shape determination of lead bromide crystal interface.

Batur, Celal↗

Ifluence of crystallization and entrainment of cooler material on the emplacement of basaltic aa lava flows

A theoretical model is used to describe and investigate the effects of simultaneous crystallization, radiation loss, and entrainment of cooler material on the temperature of a well-mixed core of an active aa lava flow. Entrainment of crust, levee debris, and base material into the interior of active flows has been observed, but the degree of assimilation and the thermal consequences are difficult to quantify. The rate of entrainment can be constrained by supplementing the theoretical model with information on the crystallization along the path of the flow and estimation of the radiative loss from the flow interior. Application of the model is demonstrated with the 1984 Mauna Loa flow, which was erupted about 30 C undercooled. Without any entrainment of cooler material, the high crystallization rates would have driven temperatures in the core wall above temperatures measured by thermocouple and estimated from glass geothermometry. One plausible scenario for this flow, which agrees with available temperature and crystallinity measurements, has a high initial rate of entrainment during the first 8 hours of travel (a mass ratio of entrained material to fluid core of about 15% if the average temperature of the entrained material was 600 C), which counterbalances the latent heat from approximately 40% crystallization. In this scenario, the model suggests an additional 5% crystallization and a 5% entrainment mass ratio over the subsequent 16-hour period. Measurements of crystallization, radiative losses, and entrainment factors are necessary for understanding the detailed thermal histories of active lava flows.

Crisp, Joy↗

The Averaged Face Growth Rates of lysozyme Crystals: The Effect of Temperature

Measurements of the averaged or macroscopic face growth rates of lysozyme crystals are reported here for the (110) face of tetragonal lysozyme, at three sets of pH and salt concentrations, with temperatures over a 4-22 C range for several protein concentrations. The growth rate trends with supersaturation were similar to previous microscopic growth rate measurements. However, it was found that at high super-saturations the growth rates attain a maximum and then start decreasing. No 'dead zone' was observed but the growth rates were found to approach zero asymptotically at very low super-saturations. The growth rate data also displayed a dependence on pH and salt concentration which could not be characterized solely by the super-saturation. A complete mechanism for lysozyme crystal growth, involving the formation of an aggregate growth unit, mass transport of the growth unit to the crystal interface and faceted crystal growth by growth unit addition, is suggested. Such a mechanism may provide a more consistent explanation for the observed growth rate trends than those suggested by other investigators. The nutrient solution interactions leading to the formation of the aggregate growth unit may, thus, be as important as those occurring at the crystal interface and may account for the differences between small molecule and protein crystal growth.

Nadarajah, Arunan↗

A Simple Inexpensive Bridgman-Stockbarger Crystal Growth System for Organic Materials

Direct observation of solid-liquid interface is important for the directional solidification to determine the desired interface shape by controlling the growth parameters. To grow good quality single crystals of novel organic nonlinear optical materials, a simple inexpensive Bridgman-Stockbarger (BS) crystal growth system has been designed and fabricated. Two immiscible liquids have been utilized to create two zones for this crystal growth system. Bulk single crystals of benzil derivative and n-salicylidene-aniline have been successfully grown in this system. The optimum lowering rate has been found to be 0.1 mm/h for the flat interface. Results on the crystal growth and other parameters of the grown crystals are presented.

Choi, J.↗

Effects of Purification on the Crystallization of Lysozyme

We have additionally purified a commercial lysozyme preparation by cation exchange chromatography, followed by recrystallization. This material is 99.96% pure with respect to macromolecular impurities. At basic pH, the purified lysozyme gave only tetragonal crystals at 20 C. Protein used directly from the bottle, prepared by dialysis against distilled water, or which did not bind to the cation exchange column had considerably altered crystallization behavior. Lysozyme which did not bind to the cation exchange column was subsequently purified by size exclusion chromatography. This material gave predominately bundles of rod-shaped crystals with some small tetragonal crystals at lower pHs. The origin of the bundled rod habit was postulated to be a thermally dependent tetragonal- orthorhombic change in the protein structure. This was subsequently ruled out on the basis of crystallization behavior and growth rate experiments. This suggests that heterogeneous forms of lysozyme may be responsible. These results demonstrate three classes of impurities: (1) small molecules, which may be removed by dialysis; (2) macromolecules, which are removable by chromatographic techniques; and (3) heterogeneous forms of the protein, which can be removed in this case by cation exchange chromatography. Of these, heterogeneous forms of the lysozyme apparently have the greatest affect on its crystallization behavior.

Ewing, Felecia L.↗

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.↗

CCD Video Observation of Microgravity Crystallization of Lysozyme and Correlation with Accelerometer Data

Lysozyme has been crystallized using the ESA Advanced Protein Crystallization Facility onboard the NASA Space Shuttle Orbiter during the IML-2 mission. CCD video monitoring was used to follow the crystallization process and evaluate the growth rate. During the mission some tetragonal crystals were observed moving over distances of up to 200 micrometers. This was correlated with microgravity disturbances caused by firings of vernier jets on the Orbiter. Growth-rate measurement of a stationary crystal (which had nucleated on the growth reactor wall) showed spurts and lulls correlated with an onboard activity; astronaut exercise. The stepped growth rates may be responsible for the residual mosaic block structure seen in crystal mosaicity and topography measurements.

Snell, E. H.↗

Effects of Gravity on Crystallization of Fluorozircante Optical Fibers

ZBLAN (ZrF4-BaF2-LaF3-AlF3-NaF) optical fibers were flown on NASA's reduced gravity KC135 aircraft and Conquest I sub-orbital rocket. The purpose of these experiments was to determine the effects of gravity on the crystallization process of this material. Fiber samples encapsulated in evacuated quartz ampoules were heated to the crystallization temperature during flight in reduced gravity and on the ground in unit gravity. Scanning electron and transmission electron microscopy were utilized to study the crystallization behavior. Samples heated under unit gravity conditions exhibited significant crystallization, while fibers heated to the crystallization temperature in reduced gravity showed no signs of crystallization. A mechanism based on microcellular convection is proposed to explain these observed behaviors.

Tucker, D. S.↗

Snow Crystal Orientation Effects on the Scattering of Passive Microwave Radiation

For this study, consideration is given to the role crystal orientation plays in scattering and absorbing microwave radiation. A discrete dipole scattering model is used to measure the passive microwave radiation, at two polarizations (horizontal and vertical), scattered by snow crystals oriented in random and non random positions, having various sizes (ranging between 1 micrometers to 10,000 micrometers in radius), and shapes (including spheroids, cylinders, hexagons). The model results demonstrate that for the crystal sizes typically found in a snowpack, crystal orientation is insignificant compared to crystal size in terms of scattering microwave energy in the 8,100 gm (37 GHz) region of the spectrum. Therefore, the assumption used in radiative transfer approaches, where snow crystals are modeled as randomly oriented spheres, is adequate to account for the transfer of microwave energy emanating from the ground and passing through a snowpack.

Foster, J. L.↗

Characterization of ZnSe Single Crystals Grown by Physical Vapor Transport

ZnSe bulk crystals were grown by self-seeded physical vapor transport technique in horizontal and vertical configurations. The impurities and defects in the grown crystals were studied by glow discharge mass spectroscopy (GDMS) and low temperature photoluminescence (PL) measurements. The PL results on the starting material and the grown crystals are consistent with the low impurity levels measured by GDMS. The crystalline quality of the grown crystals were examined by synchrotron white beam X-ray topography (SWBXT) and high resolution triple X-ray diffraction (HRTXD). The SWBXT shows that, aside from twins, the overall crystalline quality of the vapor grown ZnSe crystals, especially in the contactless grown region, was quite high. The HRTXD results are in line with the SWBXT findings. The comparison between the HRTXD on a chemical-mechanically polished and a cleaved surface seems to indicate that polishing damage can obscure the true microstructure in the as-grown ZnSe crystals.

Su, Ching-Hua↗

X-Ray Diffraction Analysis of NLO Crystals: Traditional Applications and More New Opportunities

Single crystal X-ray diffraction analysis is one of the more important methods for the molecular and crystal structure determination of matter and therefore it has a great importance in material science including design and engineering of different compounds with non-linear optical (NLO) properties. It was shown in our previous publications that this method provides unique information about molecular structure of NLO compounds, their crystal symmetry and crystal packing arrays, molecular conformation and geometries and many other structural and electronic characteristics that are important for understanding the nature of NLO properties of solids. A very new application of the X-ray diffraction method is related to analysis of the electron density distribution p(r) in crystals and some of its characteristics (atomic and group charges, dipole and higher multipole moments, etc.), that may be obtained directly form the diffraction measurements. In the present work, we will discuss our preliminary low temperature high-resolution X-ray data for the m-nitroaniline (mNA) single crystal (VI). This is one of the "classical" organic NLO materials and electron density distribution analysis in this simple compound has a great scientific interest.

Antipin, Mikhail Yu.↗