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At least 721 records · Page 40
All sourcesNASA NTRSDOE OSTI
NASA NTRS1999

Modeling of Macroscopic/Microscopic Transport and Growth Phenomena in Zeolite Crystal Solutions Under Microgravity Conditions

Crystals grown from liquid solutions have important industrial applications. Zeolites, for instance, a class of crystalline aluminosilicate materials, form the backbone of the chemical process industry worldwide, as they are used as adsorbents and catalysts. Many of the phenomena associated with crystal growth processes are not well understood due to complex microscopic and macroscopic interactions. Microgravity could help elucidate these phenomena and allow the control of defect locations, concentration, as well as size of crystals. Microgravity in an orbiting spacecraft could help isolate the possible effects of natural convection (which affects defect formation) and minimize sedimentation. In addition, crystals will stay essentially suspended in the nutrient pool under a diffusion-limited growth condition. This is expected to promote larger crystals by allowing a longer residence time in a high-concentration nutrient field. Among other factors, the crystal size distribution depends on the nucleation rate and crystallization. These two are also related to the "gel" polymerization/depolymerization rate. Macroscopic bulk mass and flow transport and especially gravity, force the crystals down to the bottom of the reactor, thus forming a sedimentation layer. In this layer, the growth rate of the crystals slows down as crystals compete for a limited amount of nutrients. The macroscopic transport phenomena under certain conditions can, however, enhance the nutrient supply and therefore, accelerate crystal growth. Several zeolite experiments have been performed in space with mixed results. The results from our laboratory have indicated an enhancement in size of 30 to 70 percent compared to the best ground based controls, and a reduction of lattice defects in many of the space grown crystals. Such experiments are difficult to interpret, and cannot be easily used to derive empirical or other laws since many physical parameters are simultaneously involved in the process. At the same time, however, there is increased urgency to develop such an understanding in order to more accurately quantify the process. In order to better understand the results obtained from our prior space experiments, and design future experiments, a detailed fluid dynamic model simulating the crystal growth mechanism is required. This will not only add to the fundamental knowledge on the crystallization of zeolites, but also be useful in predicting the limits of size and growth of these important industrial materials. Our objective is to develop macro/microscopic theoretical and computational models to study the effect of transport phenomena in the growth of crystals grown in solutions. Our effort has concentrated so far in the development of separate macroscopic and microscopic models. The major highlights of our accomplishments are described.

Gatsonis, Nikos A.↗
NASA NTRS2002

A Model for Tetragonal Lysozyme Crystal Nucleation and Growth

Macromolecular crystallization is a complex process, involving a system that typically has 5 or more components (macromolecule, water, buffer + counter ion, and precipitant). Whereas small molecules have only a few contacts in the crystal lattice, macromolecules generally have 10's or even 100's of contacts between molecules. These can range from hydrogen bonds (direct or water-mediated), through van der Waals, hydrophobic, salt bridges, and ion-mediated contacts. The latter interactions are stronger and require some specificity in the molecular alignment, while the others are weaker, more prevalent, and more promiscuous, i.e., can be readily broken and reformed between other sites. Formation of a consistent, ordered, 3D structure may be difficult or impossible in the absence of any or presence of too many strong interactions. Further complicating the process is the inherent structural asymmetry of monomeric (single chain) macromolecules. The process of crystal nucleation and growth involves the ordered assembly of growth units into a defined 3D lattice. We suggest that for many macromolecules, particularly those that are monomeric, this involves a preliminary solution-phase assembly process into a growth unit having some symmetry prior to addition to the lattice, recapitulating the initial stages of the nucleation process. If this model is correct then fluids and crystal growth models assuming a strictly monodisperse nutrient solution need to be revised. This model has been developed from experimental evidence based upon face growth rate, AFM, and fluorescence energy transfer data for the nucleation and growth of tetragonal lysozyme crystals.

Pusey, Marc L.↗
NASA NTRS1989

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.↗
NASA NTRS2004

The Nucleation and Growth of Protein Crystals

Obtaining crystals of suitable size and high quality continues to be a major bottleneck in macromolecular crystallography. Currently, structural genomics efforts are achieving on average about a 10% success rate in going from purified protein to a deposited crystal structure. Growth of crystals in microgravity was proposed as a means of overcoming size and quality problems, which subsequently led to a major NASA effort in microgravity crystal growth, with the agency also funding research into understanding the process. Studies of the macromolecule crystal nucleation and growth process were carried out in a number of labs in an effort to understand what affected the resultant crystal quality on Earth, and how microgravity improved the process. Based upon experimental evidence, as well as simple starting assumptions, we have proposed that crystal nucleation occurs by a series of discrete self assembly steps, which 'set' the underlying crystal symmetry. This talk will review the model developed, and its origins, in our laboratory for how crystals nucleate and grow, and will then present, along with preliminary data, how we propose to use this model to improve the success rate for obtaining crystals from a given protein.

Pusey, Marc↗
NASA NTRS1972

Development of single crystal membranes

The design and construction of a high pressure crystal growth chamber was accomplished which would allow the growth of crystals under inert gas pressures of 2 MN/sq m (300 psi). A novel crystal growth technique called EFG was used to grow tubes and rods of the hollandite compounds, BaMgTi7O16, K2MgTi7O16, and tubes of sodium beta-alumina, sodium magnesium-alumina, and potassium beta-alumina. Rods and tubes grown are characterized using metallographic and X-ray diffraction techniques. The hollandite compounds are found to be two or three-phase, composed of coarse grained orientated crystallites. Single crystal c-axis tubes of sodium beta-alumina were grown from melts containing excess sodium oxide. Additional experiments demonstrated that crystals of magnesia doped beta-alumina and potassium beta-alumina also can be achieved by this EFG technique.

Stormont, R. W.↗
NASA NTRS1979

The processing of semiconductor materials

Five experiments involving the processing of semiconductor materials were performed during the Skylab mission. After discussions on semiconductors and their unique electronic properties, and techniques of crystal growth, these five experiments are presented. Four melt growth experiments were attempted: (1) steady state growth and segregation under zero gravity (InSb); (2) seeded, containerless solidification of InSb; (3) influence of gravity-free solidification on microsegregation; and (4) directional solidification of InSb-GaSb alloys. One vapor growth experiment, crystal growth by vapor transport, was attempted.

Source record↗
NASA NTRS1985

Variable-Temperature-Gradient Device for Solidification Research

Device for research in solidification and crystal growth allows crystallization of melt observed as occurs. Temperature gradient across melt specimen increased or decreased rapidly while solidification front proceeds at constant speed across sample. Device moves sample at same speed, thereby holding position of liquid/solid interface stationary within field of optical microscope. Device, variabletemperature-gradient microscope stage, used to study crystal growth at constant rate while thermal driving force is varied.

Kaukler, W. F.↗
NASA NTRS1992

An examination of anticipated g-jitter on Space Station and its effects on materials processes

Information on anticipated g-jitter on Space Station Freedom and the effect of the jitter on materials processes is given in viewgraph form. It was concluded that g-jitter will dominate the acceleration environment; that it is a 3D multifrequency phenomenon; and that it varies dramatically in orientation. Information is given on calculated or measured sources of residual acceleration, aerodynamic drag, Shuttle acceleration measurements, the Space Station environment, tolerable g-levels as a function of frequency, directional solidification, vapor crystal growth, protein crystal growth, float zones, and liquid bridges.

Nelson, Emily↗
NASA NTRS2000

Magnetic Susceptibility Effects and Lorentz Damping in Diamagnetic Fluids

A great number of crystals (semi-conductor and protein) grown in space are plagued by convective motions which contribute to structural flaws. The character of these instabilities is not well understood but is associated with density variations in the presence of residual gravity and g-jitter. Both static and dynamic (rotating or travelling wave) magnetic fields can be used to reduce the effects of convection in materials processing. In semi-conductor melts, due to their relatively high electrical conductivity, the induced Lorentz force can be effectively used to curtail convective effects. In melts/solutions with reduced electrical conductivity, such as aqueous solutions used in solution crystal growth, protein crystal growth and/or model fluid experiments for simulating melt growth, however, the variation of the magnetic susceptibility with temperature and/or concentration can be utilized to better damp fluid convection than the Lorentz force method. This paper presents a comprehensive, comparative numerical study of the relative damping effects using static magnetic fields and gradients in a simple geometry subjected to a thermal gradient. The governing equations are formulated in general terms and then simplified for the numerical calculations. Operational regimes, based on the best damping technique for different melts/solutions are identified based on fluid properties. Comparisons are provided between the numerical results and available results from experiments in surveyed literature.

Ramachandran, Narayanan↗
NASA NTRS1983

Technique for Crystal-Ribbon Growth

Single-crystal ribbon of silicon or other material is grown by pulling at low angle from shallow melt. By pulling crystal at small angle, technique prevents overflow problem experienced with horizontal growth. Also creates meniscus that minimizes growth defects in main portion of ribbon. Use of shallow pool prevents convection problems.

Jewett, D. N.↗
NASA NTRS1982

Influence of diffusion and convective transport on dendritic growth in dilute alloys

Experimentation has been carried out in which the kinetics and morphology of dendritic growth were measured as a function of thermal supercooling, solute concentration, and spatial orientation of the dendritic growth axis. The crystal growth system studied is succinonitrile, NC(CH2)2CN, with additions of argon (up to 0.1 mole percent). This system is especially useful as a model for alloy studies because kinetic data are available for high purity (7-9's) succinonitrile. The influence of the solute, at fixed thermal supercooling, is to increase the growth velocity and correspondingly decrease intrinsic crystal dimensions. Morphological measurements are described in detail relating tip size, perturbation wavelength, supercooling, and solute concentration. The analysis of these effects based on morphological stability theory is also discussed, and experiments permitting the separation of convective and diffusive heat transport during crystal growth of succinonitrile are described. The studies underscore the importance of gravitationally-induced buoyancy effects on crystal growth.

Glicksman, M. E.↗
NASA NTRS1985

Comparison of theory with experiment in convectionless growth of crystals from solution

Wilcox's computer program for predicting the growth rates of crystals in convectionless supersaturated solution is used to model experiments to measure the crystal growth experiments of Simon (1978) and of Nerad and Shlichta (1984), and the results are compared with the experimental data. The predictions of Wilcox's model are found to be in remarkably good agreement with the results of Simon. The data of Nerad and Shlichta are 30 to 90 percent higher than the predictions of the Wilcox model for a certain range of temperature dependence, consistent with the observation of occasional low-level convection in these experiments. These comparisons indicate that the Wilcox model can be used to make reliable order-of-magnitude predictions of growth rates in the absence of convection.

Schlom, D. G.↗
NASA NTRS1998

New AFM Techniques for Investigating Molecular Growth Mechanisms of Protein Crystals

Atomic Force Microscopy (AFM) has emerged as a powerful technique for investigating protein crystal growth. Earlier AFM studies were among the first to demonstrate that these crystals grew by dislocation and 2D nucleation growth mechanisms [1]. These investigations were restricted to the micron range where only surface features, such as dislocation hillocks and 2D islands are visible. Most AFM instruments can scan at higher resolutions and have the potential to resolve individual protein molecules at nanometer ranges. Such scans are essential for determining the molecular packing arrangements on crystal faces and for probing the growth process at the molecular level. However, at this resolution the AFM tip influences the image produced, with the resulting image being a convolution of the tip shape and the surface morphology [2]. In most studies this problem is resolved by deconvoluting the image to obtain the true surface morphology. Although deconvolution routines work reasonably well for simple one- dimensional shapes, for complex surfaces this approach does not produce accurate results. In this study we devised a new approach which takes advantage of the precise molecular order of crystal surfaces, combined with the knowledge of individual molecular shapes from the crystallographic data of the protein and the AFM tip shape. This information is used to construct expected theoretical AFM images by convoluting the tip shape with the constructed crystal surface shape for a given surface packing arrangement. By comparing the images from actual AFM scans with the constructed ones for different possible surface packing arrangements, the correct packing arrangement can be conclusively determined. This approach was used in this study to determine the correct one from two possible packing arrangements on (I 10) faces of tetragonal lysozyme crystals. Another novel AFM technique was also devised to measure the dimension of individual growth units of the crystal faces. Measuring these units was not attempted before and most studies have assumed that the growth unit consisted of individual protein molecules. The linescan mode of AFM instruments allows the crystal surface to be scanned along a single line. By scanning across a growth step an image showing the motion of the step is obtained. Normally such an image shows a straight line for continuous and constant step velocity. In this study by increasing the scan rate and by decreasing the step velocity (by decreasing the supersaturation), we were able to capture images of individual growth events, shown by jump discontinuities in the step line. By suitable integration of the image the growth unit dimension in the scanned direction can be obtained. Since multiple units can be involved in the growth process it is necessary to collect a statistically relevant sample before drawing conclusions about the growth mechanism. This technique was successfully employed to obtain the dimensions of growth units for the (110) face, showing that they consisted of various aggregates corresponding to the 43 helices in the crystal structure.

Li, Huayu↗
NASA NTRS1985

Vapor Growth of Alloy-Type Semiconductor Crystals

The present effort is part of a continuing research program directed towards the investigation of basic vapor transport phenomena and of crystal growth properties of electronic materials. The primary purpose of ground-based studies is the development and definition of optimum experimental parameters for flight experiments. The ground-based effort includes the investigation of gravity-driven convection effects on mass transport rates and on crystal morphology for different orientations of the density gradient with respect to the gravity vector, and as a function of pressure and of temperature. In addition to the experimental tasks, theoretical efforts involve the quantitative thermodynamic analysis of the systems under investigation, the computation of fluid dynamic parameters, and the consideration of other possible effects on fluid flow under vertical, stabilizing and microgravity conditions. The specific experiments to be performed in a microgravity environment include the investigation of vapor transport and crystal growth phenomena of the GeSe-Xenon system and of the mass flux and growth of bulk and layer-type crystals of Hg sub (1-x) Cd sub x Te using HgI as a transport agent.

Wiedemeier, H.↗
NASA NTRS1992

Mass-Transport Properties In Growth Of Crystals From Vapors

Brief report summarizes results of experimental and theoretical studies of mass-transport properties of GeSe/Gel4 and Hg0.8Cd0.2Te systems in connection with growth of crystals in closed ampoules. Primary emphasis in studies was on thermochemical analyses, on development of mathematical models to predict diffusion-limited mass transport, and on comparison of theoretically predicted with experimental fluxes. Results applied to design, preparation, performance, and analysis of crystal-growth experiments of semiconducting materials on Earth and in outer space. Model extended to predict mass flux and overall composition of transport products of Hg0.8Cd0.2Te transport system.

Wiedemeier, H.↗
NASA NTRS1997

Growth of Bulk Wide Bandgap Semiconductor Crystals and Their Potential Applications

Developments in bulk crystal growth research for electro-optical devices in the Center for Photonic Materials and Devices since its establishment have been reviewed. Purification processes and single crystal growth systems employing physical vapor transport and Bridgman methods were assembled and used to produce high purity and superior quality wide bandgap materials such as heavy metal halides and II-VI compound semiconductors. Comprehensive material characterization techniques have been employed to reveal the optical, electrical and thermodynamic properties of crystals, and the results were used to establish improved material processing procedures. Postgrowth treatments such as passivation, oxidation, chemical etching and metal contacting during the X-ray and gamma-ray device fabrication process have also been investigated and low noise threshold with improved energy resolution has been achieved.

Chen, Kuo-Tong↗
NASA NTRS1999

Characterization of Optical Lenses to be Considered for the Imaging of Crystal Dendrite Growth

Dynamic fracture is a phenomenon that is extremely sensitive to small perturbations in system parameters. This phenomenon is, in some ways, similar to that of dendritic crystal growth, although it is governed by different physical principles. Crystal dendrite growth patterns are affected by parameters such as temperature, pressure, and gravity. By studying the behavior of crystal dendrites in a controlled, microgravity environment, a greater understanding of dynamic fracture could be revealed. A sealed cubical container contains four stingers, which facilitate the growth of crystal dendrites. The container has five windows and is emersed in a liquid, for thermal isolation. The tip of a dendrite can advance in any direction, therefore three-dimensional images of the process are desired. Furthermore, because of the rapid growth rate, a fast image frame rate is required for accurate tracking of dendrite tip velocity. In addition, optical parameters such as field of view, depth of focus, and resolution are examined, as well as the working distance between a lens and the target of observation.

Wing, Frank M.↗