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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 NTRS1977

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↗

NASA NTRS1999

Ground Based Program for the Physical Analysis of Macromolecular Crystal Growth

In a reported period in situ atomic force microscopy was utilized in our laboratory to study mechanisms of growth and kinetics of crystallization of ten protein and virus crystals. These included canavalin, thaumatin, apoferritin, lipase, catalase, t-RNA, lysozyme, xylanase, turnip yellow mosaic virus (TYMV) and satellite tobacco mosaic virus (STMV). We have also designed and constructed in our laboratory both in situ conventional two-beam Michelson and phase shift Mach-Zenhder interferometers. Computer software for the processing of the interferometric images was developed as well. Interferometric techniques were applied for studies of growth kinetics and transport phenomena in crystallization of several macromolecular crystals. As a result of this work we have published 21 papers and have given many presentations at international and national meetings. A list of these publications and conference presentations is attached.

Malkin, Alexander J.↗

NASA NTRS2014

Ice Crystal Icing Engine Testing in the NASA Glenn Research Center's Propulsion Systems Laboratory: Altitude Investigation

The National Aeronautics and Space Administration (NASA) conducted a full scale ice crystal icing turbofan engine test using an obsolete Allied Signal ALF502-R5 engine in the Propulsion Systems Laboratory (PSL) at NASA Glenn Research Center. The test article used was the exact engine that experienced a loss of power event after the ingestion of ice crystals while operating at high altitude during a 1997 Honeywell flight test campaign investigating the turbofan engine ice crystal icing phenomena. The test plan included test points conducted at the known flight test campaign field event pressure altitude and at various pressure altitudes ranging from low to high throughout the engine operating envelope. The test article experienced a loss of power event at each of the altitudes tested. For each pressure altitude test point conducted the ambient static temperature was predicted using a NASA engine icing risk computer model for the given ambient static pressure while maintaining the engine speed.

Altitude Testing↗

NASA NTRS1976

Float-zone processing in a weightless environment

The results were reported of investigations to: (1) test the validity of analyses which set maximum practical diameters for Si crystals that can be processed by the float zone method in a near weightless environment, (2) determine the convective flow patterns induced in a typical float zone, Si melt under conditions perceived to be advantageous to the crystal growth process using flow visualization techniques applied to a dimensionally scaled model of the Si melt, (3) revise the estimates of the economic impact of space produced Si crystal by the float zone method on the U.S. electronics industry, and (4) devise a rational plan for future work related to crystal growth phenomena wherein low gravity conditions available in a space site can be used to maximum benefit to the U.S. electronics industry.

Fowle, A. A.↗

NASA NTRS1979

Anomalous growth of single ice crystals in solution

It is shown that major discrepancies exist between experiments and theory for ice crystal growth from solution. Accurate data, taken in a microgravity environment, approximate analytical models, and exact (probably numerical) models all are needed to advance our understanding of ice crystal growth phenomena. A new approximate semi-empirical theory is presented which predicts that a relatively sharp transition from natural convection control to diffusion control for ice growth in pure water occurs at a subcooling of about 10 C (a reduced temperature difference of about 0.125). No reliable data exist to test this prediction. The theory also predicts qualitatively the growth of ice in NaCl solution in which maxima in the growth rates are observed at various levels of subcooling.

Gill, W. N.↗

NASA NTRS1984

Hot stage and sample cell design for the solidification of transparent materials with and without forced convection

A temperature gradient stage design for optical microscopy is described. Exceptional thermal stability is the major feature. The stage is used to study crystal growth phenomena occurring at the solid-liquid interface. The apparatus is designed to use transparent organic solutions as models for the study of metal-like solidification. The stage provides a controlled thermal environment for unidirectional solidification of low melting temperature materials. Freezing rate is regulated by mechanically sliding in the stage a thin glass cell containing the materials being studied. Two cell assemblies are described. One type is used for convection-free and the other for controlled forced convection studies of the solidification interface.

Kaukler, W. F.↗

NASA NTRS1986

Vapor transport processes of Ge-chalcogenides under normal and reduced gravity conditions

Experimental and theoretical studies of the GeSe-GeI4 system revealed the multicomponent, multireaction nature of this system and the existence of a diffusion boundary layer; they also yielded equations for the prediction of diffusion limited mass transport rates. Vapor transport and crystal growth experiments of the GeSe-GeI4 and GeSe-Xe systems on earth and in a microgravity environment demonstrated the effects of convection and of microgravity on mass flux and crystal morphology. The surface and bulk morphology of GeSe crystals obtained for both systems in microgravity is considerably improved relative to ground-based specimens. Unexpected crystal growth phenomena were observed for the GeSe-Xenon system on recent Shuttle flights.

Wiedemeier, H.↗

NASA NTRS1975

The study of single crystals for space processing and the effect of zero gravity

A study was undertaken to analyze different growth techniques affected by a space environment. Literature on crystal growth from melt, vapor phase and float zone was reviewed and the physical phenomena important for crystal growth in zero-gravity environment was analyzed. Recommendations for potential areas of crystal growth feasible for space missions are presented and a bibliography of articles in the area of crystal growth in general is listed.

Lal, R. B.↗

NASA NTRS2000

Protein Crystals Grow Purer in Space: Physics of Phenomena

This presentation will summarize the quantitative experimental and theoretical results obtained by B.R. Thomas, P.G. Vekilov, D.C. Carter, A.M. Holmes, W.K. Widierow and the Author, the team with expertise in physics, biochemistry, crystallography and engineering. Impurities inhomogeneously trapped by a growing crystal - e.g., producing sectorial structure and/or striations - may induce macroscopic internal stress in it if an impurity molecule has slightly (less than 10%) different shape or volume than the regular one(s) they replace. We tested for the first time plasticity and measured Young modulus E of the triclinic, not cross-linked lysozyme by triple point bending technique. Triclinic lysozyme crystals are purely elastic with E similar or equal to 1/5 (raised dot) 10 (exp 9) partial derivative yn/sq cm. The strength limit, sigma (sub c) similar or equal to 10 (exp -3)E similar or equal to Epsilon (sub c), where sigma (sub c) and epsilon (sub c) are critical stress and strain, respectively. Scaling E and sigma (sub c) with the lattice spacing suggests similar binding stiffness in inorganic and biomolecular crystals. The inhomogeneous internal stress may be resolved in these brittle crystals either by cracking or by creation of misoriented mosaic blocks during, not after growth. If each impurity molecule induces in the lattice elementary strain epsilon (sub 0) similar or equal to 3 (raised dot) 10 (exp -2) (this is maximal elementary strain that can arise at the supersaturation DELTA mu/kT similar or equal to 2 and macroscopic molecular concentration difference between subsequent macrolayers or growth sectors is partial derivativeC similar or equal to 5 (raised dot) 10 (exp -3), the internal strain epsilon similar or equal to epsilon (sub 0) partial derivative C similar or equal to 10 (exp -4). Mosaic misorientation resolving such strain is approximately 30 arcsec. Tenfold increase of impurity concentration may cause cracking. Estimates of stress in an isometric sectorial crystal show that lysozyme crystals can tolerate the stress till the size of 0.5mm. Dissolving mosaic lysozyme crystal shows that the mosaicity, indeed, is absent below that size.

Chernov, Alex A.↗

NASA NTRS1961

Neutralization of Hydroxide Ion in Melt-Grown NaCl Crystals

Many recent studies of solid-state phenomena, particularly in the area of crystal imperfections, have involved the use of melt-grown NaCl single crystals. Quite often trace impurities in these materials have had a prominent effect on these phenomena. Trace amounts of hydroxide ion have been found in melt-grown NaCl crystals. This paper describes a nondestructive method of neutralizing the hydroxide ion in such crystals. Crystals of similar hydroxide content are maintained at an elevated temperature below the melting point of NaCl in a flowing atmosphere containing. dry hydrogen chloride. Heat treatment is continued until an analysis of the test specimens shows no excess hydroxide ion. A colorimetric method previously described4 is used for this analysis.

Otterson, Dumas A.↗

NASA NTRS1985

Simulation of the temperature distribution in crystals grown by Czochralski method

Production of perfect crystals, free of residual strain and dislocations and with prescribed dopant concentration, by the Czochralski method is possible only if the complex, interacting phenomena that affect crystal growth in a Cz-puller are fully understood and quantified. Natural and forced convection in the melt, thermocapillary effect and heat transfer in and around the crystal affect its growth rate, the shape of the crystal-melt interface and the temperature gradients in the crystal. The heat transfer problem in the crystal and between the crystal and all other surfaces present in the crystal pulling apparatus are discussed at length. A simulation and computer algorithm are used, based on the following assumptions: (1) only conduction occurs in the crystal (experimentally determined conductivity as a function of temperature is used), (2) melt temperature and the melt-crystal heat transfer coefficient are available (either as constant values or functions of radial position), (3) pseudo-steady state is achieved with respect to temperature gradients, (4) crystal radius is fixed, and (5) both direct and reflected radiation exchange occurs among all surfaces at various temperatures in the crystal puller enclosure.

Dudokovic, M. P.↗

NASA NTRS1993

Transport phenomena of growth-in-gel zeolite crystallization in microgravity

Secondary nucleation (SN) due to crystal sedimentation has been believed to be one of the major effects that causes smaller sizes of final zeolite crystals. The present investigation indicates that, in a reactor, this gravity-induced SN occurs only within a white opaque column termed the gel portion. Under normal gravity this portion shrinks to the bottom of the hydrothermal reactor, leaving a clear portion of solution at the top, due to depletion of the flocculated gel particles. Solution phase nucleation and crystallization is assumed and a correlation for the shrinkage is therefore derived, which shows good agreement with experimental observations. A non-dimensional parameter is suggested as a criterion for the occurrence of SN. Based on the parameter whether or not microgravity is beneficial to zeolite growth is discussed. Also, the growth mechanism and the transport phenomena in the absence of gravity are discussed.

Zhang, H.↗

NASA NTRS1993

Diffusion on Cu surfaces

Understanding surface diffusion is essential in understanding surface phenomena, such as crystal growth, thin film growth, corrosion, physisorption, and chemisorption. Because of its importance, various experimental and theoretical efforts have been directed to understand this phenomena. The Field Ion Microscope (FIM) has been the major experimental tool for studying surface diffusion. FIM have been employed by various research groups to study surface diffusion of adatoms. Because of limitations of the FIM, such studies are only limited to a few surfaces: nickel, platinum, aluminum, iridium, tungsten, and rhodium. From the theoretical standpoint, various atomistic simulations are performed to study surface diffusion. In most of these calculations the Embedded Atom Method (EAM) along with the molecular static (MS) simulation are utilized. The EAM is a semi-empirical approach for modeling the interatomic interactions. The MS simulation is a technique for minimizing the total energy of a system of particles with respect to the positions of its particles. One of the objectives of this work is to develop the EAM functions for Cu and use them in conjunction with the molecular static (MS) simulation to study diffusion of a Cu atom on a perfect as well as stepped Cu(100) surfaces. This will provide a test of the validity of the EAM functions on Cu(100) surface and near the stepped environments. In particular, we construct a terrace-ledge-kink (TLK) model and calculate the migration energies of an atom on a terrace, near a ledge site, near a kink site, and going over a descending step. We have also calculated formation energies of an atom on the bare surface, a vacancy in the surface, a stepped surface, and a stepped-kink surface. Our results are compared with the available experimental and theoretical results.

Karimi, Majid↗

NASA NTRS2003

Crystal Growth Rate Dispersion: A Predictor of Crystal Quality in Microgravity?

In theory macromolecular crystals grow through a process involving at least two transport phenomena of solute to the crystal surface: diffusion and convection. In absence of standard gravitational forces, the ratio of these two phenomena can change and explain why crystal growth in microgravity is different from that on Earth. Experimental evidence clearly shows, however, that crystal growth of various systems is not equally sensitive to reduction in gravitational forces, leading to quality improvement in microgravity for some crystals but not for others. We hypothesize that the differences in final crystal quality are related to crystal growth rate dispersion. If growth rate dispersion exists on Earth, decreases in microgravity, and coincides with crystal quality improvements then this dispersion is a predictor for crystal quality improvement. In order to test this hypothesis, we will measure growth rate dispersion both in microgravity and on Earth and will correlate the data with previously established data on crystal quality differences for the two environments. We present here the first crystal growth rate measurement data for three proteins (lysozyme, xylose isomerase and human recombinant insulin), collected on Earth, using hardware identical to the hardware to be used in microgravity and show how these data correlate with crystal quality improvements established in microgravity.

Kephart, Richard D.↗

NASA NTRS1992

Study of FES/CAST/HGS

The microgravity materials processing program has been instrumental in providing the crystal growth community with an experimental environment to better understand the phenomena associated with the growing of crystals. In many applications one may pursue the growth of large single crystals which cannot be grown on earth due to convective driven flows. A microgravity environment is characterized by neither convection of buoyancy. Consequently superior crystals are able to be grown in space. On the other hand, since neither convection nor buoyancy dominates the fluid flow in a microgravity environment, then lesser dominating phenomena can affect crystal growth, such as surface driven flows or diffusion limited solidification. In the case of experiments that are to be flown in space using the Fluid Experiments System (FES), diffusion limited growth should be the dominating phenomenon. The use of holographic and Schlieren optical techniques for studying the concentration gradients in solidification processes has been used by several investigators over the years. The Holographic Ground System (HGS) facility at MSFC has been a primary resource in researching this capability. Consequently scientific personnel have been able to utilize these techniques in both ground based research and in space experiments. An important event in the scientific utilization of the HGS facilities was the TGS (triglycine sulfate) Crystal Growth and the Casting and Solidification Technology (CAST) experiments that were flown on the International Microgravity Lab (IML) mission in March of this year. The preparation and processing of these space observations are the primary experiments reported in this work. This project provides some ground-based studies to optimize on the holographic techniques used to acquire information about the crystal growth processes flown on IML. Since the ground-based studies will be compared with the space-based experimental results, it is necessary to conduct sufficient ground based studies to best determine how the experiment in space worked. The current capabilities in computer based systems for image processing and numerical computation have certainly assisted in those efforts. As anticipated, this study has certainly shown that these advanced computing capabilities are helpful in the data analysis of such experiments.

Workman, Gary L.↗

NASA NTRS1978

Proceedings of the Workshop on an Electromagnetic Positioning System in Space

A workshop was convened to help determine if sufficient justification existed to proceed with the design of an electromagnetic (EM) positioning device for use in space. Those in attendance included experts in crystal growth, nucleation phenomena, containerless processing techniques, properties of materials, metallurgical techniques, and glass technology. Specific areas mentioned included the study of metallic glasses and investigations of the properties of high temperature materials.

Oran, W. A.↗

NASA NTRS1997

Experimental Program to Stimulate Competitive Research (EPSCoR)

Report includes: (1) CLUSTER: "Studies in Macromolecular Behavior in Microgravity Environment": The Role of Protein Oligomers in Protein Crystallization; Phase Separation Phenomena in Microgravity; Traveling Front Polymerizations; Investigating Mechanisms Affecting Phase Transition Response and Changes in Thermal Transport Properties in ER-Fluids under Normal and Microgravity Conditions. (2) CLUSTER: "Computational/Parallel Processing Studies": Flows in Local Chemical Equilibrium; A Computational Method for Solving Very Large Problems; Modeling of Cavitating Flows.

Dingerson, Michael R.↗