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At least 325 records · Page 18

Anisotropy of nickel-base superalloy single crystals

The effects of crystal orientation on the mechanical properties of single crystals of the nickel-based superalloy Mar-M247 are investigated. Tensile tests at temperatures from 23 to 1093 C and stress rupture tests at temperatures from 760 to 1038 C were performed for 52 single crystals at various orientations. During tensile testing between 23 and 760 C, single crystals with high Schmid factors were found to be favorably oriented for slip and to exhibit lower strength and higher ductility than those with low Schmid factors. Crystals which required large rotations to become oriented for cross slip were observed to have the shortest stress rupture lives at 760 C, while those which required little or no rotation had the longest lives. In addition, stereographic triangles obtained for Mar-M247 and Mar-M200 single crystals reveal that crystals with orientations near the -111 had the highest lives, those near the 001 had high lives, and those near the 011 had low lives.

Mackay, R. A.↗

Electromigration process for the purification of molten silicon during crystal growth

A process for the purification of molten materials during crystal growth by electromigration of impurities to localized dirty zones. In the Czochralski crystal growing process, the impurities are electromigrated away from the crystallization interface by applying a direct electrical current to the molten silicon for electromigrating the charged impurities away from the crystal growth interface. The edge-defined film-fed crystal growth process, a direct electrical current is applied between the two faces which are used in forming the molten silicon into a ribbon. The impurities, migrated to one side only of the crystal ribbon, may be removed or left in place. If left in place, they will not adversely affect the ribbon when used in solar collectors. The migration of the impurity to one side only of the silicon ribbon is especially suitable for use with asymmetric dies which preferentially crystallize uncharged impurities along one side or face of the ribbon.

Shlichta, P. J.↗

Orientation dependence of the stress rupture properties of Nickel-base superalloy single crystals

The influence of orientation of the stress rupture behavior of Mar-M247 single crystals was studied. Stress rupture tests were performed at 724 MPa and 774 C where the effect of anisotropy is prominent. The mechanical behavior of the single crystals was rationalized on the basis of the Schmid factors for the operative slip systems and the lattice rotations which the crystals underwent during deformation. The stress rupture lives were found to be greatly influenced by the lattice rotations required to produce intersecting slip, because steady-state creep does not begin until after the onset of intersecting slip. Crystals which required large rotations to become oriented for intersecting slip exhibited a large primary creep strain, a large effective stress level at the onset of steady-state creep, and consequently a short stress rupture life. A unified analysis was attained for the stress rupture behavior of the Mar-M247 single crystals tested in this study at 774 C and that of the Mar-M200 single crystals tested in a prior study at 760 C. In this analysis, the standard 001-011-111 stereographic triangle was divided into several regions of crystallographic orientation which were rank ordered according to stress rupture life for this temperature regime. This plot indicates that those crystals having orientations within about 25 deg of the 001 exhibited significantly longer lives when their orientations were closer to the 001-011 boundary of the stereographic triangle than to the 001-111 boundary.

Mackay, R. A.↗

Method and apparatus for minimizing convection during crystal growth from solution

A method and apparatus are disclosed for growing in a gravitational field a microscopic crystal from a solution. The solution is held in a vertical chamber which is relatively thin, the thin being generally perpendicular to the vertical. There is a substrate crystal disposed at either the upper or lower end of the chamber and the crystal grows from this substrate crystal in one direction. The temperature conditions of the solution are controlled so that, as the crystal forms, the effects of buoyant convection within the solution are minimized. This is accomplished in two different ways depending upon whether the crystal is grown from the upper or lower end of the chamber. When grown from the upper end of the chamber, the temperature of the solution is controlled so that it remains essentially isothermal so that there is essentially no heat loss from the solution. When the crystal is grown from the lower end of the chamber, the temperature of the solution is controlled so that there is a differential in temperature throughout the solution which provides a positive thermal gradient within the chamber.

Shlichta, P. J.↗

Liquid encapsulated crystal growth

Low-defect crystals are grown in a closed ampoule under a layer of encapsulant. After crystal growth, the crystal is separated from the melt and moved into the layer of encapsulant and cooled to a first temperature at which crystal growth stops. The crystal is then moved into the inert gas ambient in the ampoule and further cooled. The crystal can be separated from the melt by decanting the melt into and adjacent reservoir or by rotating the ampoule to rotate the crystal into the encapsulant layer.

Morrison, Andrew D.↗

Protein-crystal growth experiment (planned)

To evaluate the effectiveness of a microgravity environment on protein crystal growth, a system was developed using 5 cubic feet Get Away Special payload canister. In the experiment, protein (myoglobin) will be simultaneously crystallized from an aqueous solution in 16 crystallization units using three types of crystallization methods, i.e., batch, vapor diffusion, and free interface diffusion. Each unit has two compartments: one for the protein solution and the other for the ammonium sulfate solution. Compartments are separated by thick acrylic or thin stainless steel plates. Crystallization will be started by sliding out the plates, then will be periodically recorded up to 120 hours by a still camera. The temperature will be passively controlled by a phase transition thermal storage component and recorded in IC memory throughout the experiment. Microgravity environment can then be evaluated for protein crystal growth by comparing crystallization in space with that on Earth.

Fujita, S.↗

Convection effects in protein crystal growth

Protein crystals for X-ray diffraction study are usually grown resting on the bottom of a hanging drop of a saturated protein solution, with slow evaporation to the air in a small enclosed cell. The evaporation rate is controlled by hanging the drop above a reservoir of water, with its saturation vapor pressure decreased by a low concentration of a passive solute. The drop has a lower solute concentration, and its volume shrinks by evaporation until the molecular concentrations match. Protein crystals can also be grown from a seed crystal suspended or supported in the interior of a supersaturated solution. The main analysis of this report concerns this case because it is less complicated than hanging-drop growth. Convection effects have been suggested as the reason for the apparent cessation of growth at a certain rather small crystal size. It seeems that as the crystal grows, the number of dislocations increases to a point where further growth is hindered. Growth in the microgravity environment of an orbiting space vehicle has been proposed as a method for obtaining larger crystals. Experimental observations of convection effects during the growth of protein crystals have been reported.

Roberts, Glyn O.↗

Protein crystal growth in a microgravity environment

Protein crystal growth is a major experimental problem and is the bottleneck in widespread applications of protein crystallography. Research efforts now being pursued and sponsored by NASA are making fundamental contributions to the understanding of the science of protein crystal growth. Microgravity environments offer the possibility of performing new types of experiments that may produce a better understanding of protein crystal growth processes and may permit growth environments that are more favorable for obtaining high quality protein crystals. A series of protein crystal growth experiments using the space shuttle was initiated. The first phase of these experiments was focused on the development of micro-methods for protein crystal growth by vapor diffusion techniques, using a space version of the hanging drop method. The preliminary space experiments were used to evolve prototype hardware that will form the basis for a more advanced system that can be used to evaluate effects of gravity on protein crystal growth.

Bugg, Charles E.↗

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.↗

Growth and characterization of large YBa2Cu3O(7-x) single crystals

Centimeter-sized crystal plates of YBa2Cu3O(7-x) have been obtained using a bulk composition and method described by Schneemeyer at al. (1987) modified for growth in a pure oxygen atmosphere. A porous MgO crucible and long soak time promote large crystals. Mg was not detectable in the crystals. Electron microbeam analysis using a 60 A monochromator crystal for the oxygen determination gave the composition Y(1.05)Ba(2.02)Cu(2.94)O(6.52 + or - 0.06). As-grown crystals from the melt surface exhibit a fairly sharp Tc with zero resistance at 80 K, and show complex twinning and crack patterns. Optical micrographs of a lightly polished surface normal to the c-axis of a 3-mm crystal delineate twinning and fine scale microcracking; this crystal surface now has a zero resistance at 68 K. Microhardness measurements and microfracture observations indicate intrinsic properties that may inhibit or impede large scale manufacture of electronic ceramics.

Keester, Kenneth L.↗

Hydrogen induced fracture characteristics of single crystal nickel-based superalloys

A stereoscopic method for use with x ray energy dispersive spectroscopy of rough surfaces was adapted and applied to the fracture surfaces single crystals of PWA 1480E to permit rapid orientation determinations of small cleavage planes. The method uses a mathematical treatment of stereo pair photomicrographs to measure the angle between the electron beam and the surface normal. One reference crystal orientation corresponding to the electron beam direction (crystal growth direction) is required to perform this trace analysis. The microstructure of PWA 1480E was characterized before fracture analysis was performed. The fracture behavior of single crystals of the PWA 1480E nickel-based superalloy was studied. The hydrogen-induced fracture behavior of single crystals of the PWA 1480E nickel-based superalloy was also studied. In order to understand the temperature dependence of hydrogen-induced embrittlement, notched single crystals with three different crystal growth orientations near zone axes (100), (110), and (111) were tensile tested at 871 C (1600 F) in both helium and hydrogen atmospheres at 34 MPa. Results and conclusions are given.

Chen, Po-Shou↗

Protein crystal growth in low gravity

The effect of low gravity on the growth of protein crystals and those parameters which will affect growth and crystal quality was studied. The proper design of the flight hardware and experimental protocols are highly dependent on understanding the factors which influence the nucleation and growth of crystals of biological macromolecules. Thus, those factors are investigated and the body of knowledge which has been built up for small molecule crystallization. These data also provide a basis of comparison for the results obtained from low-g experiments. The flows around growing crystals are detailed. The preliminary study of the growth of isocitrate lyase, the crystal morphologies found and the preliminary x ray results are discussed. The design of two apparatus for protein crystal growth by temperature control are presented along with preliminary results.

Feigelson, Robert S.↗

Glass formation and crystallization in high-temperature glass-ceramics and Si3N4

The softening of glassy grain boundaries in ceramic matrix composites and Si3N4 at high temperatures reduces mechanical strength and the upper-use temperature. By crystallizing this glass to a more refractory crystalline phase, a material which performs at higher temperatures may result. Three systems were examined: a cordierite composition with ZrO2 as a nucleating agent; celsian compositions; and yttrium silicate glasses both in bulk and intergranular in Si3N4. For the cordierite compositions, a series of metastable phases was obtained. The crystallization of these compositions was summarized in terms of metastable ternary isothermal sections. Zircon formed at the expense of ZrO2 and spinel. In SiC composites, the transformations were slower. In celsian, two polymorphs were crystallized. One phase, hexacelsian, which always crystallized, even when metastable, had an undesirable volume change. The other phase, celsian, was very difficult to crystallize. In yttrium silicate bulk glasses, similar in composition to the intergranular glass in Si3N4, a number of polymorphs of Y2Si2O7 were crystallized. The conditions under which these polymorphs formed are compared with crystallization in Si3N4.

Drummond, Charles H., III↗

Crystallization during emplacement of lava flows

Thermal models of lava flows provide a way of estimating emplacement durations and eruption rates of planetary lava flows, which can help constrain magma ascent, rheology and composition. Most of the models that have been developed consider only the effects of cooling by radiation. However, heating due to crystallization can be a large component of the overall heat budget of a flow. Little is known about the amount of crystallization and latent heating during flow advance. Crystal size distribution (CSD) measurements were made to quantify and study the effects of crystallization in the 1984 Mauna Loa flow. For flows on Mars, we must assume that the amount of crystallization is similar to that in terrestrial flows and place minimum and maximum bounds on the latent heat effect. Unfortunately, as examples given here show, there can be anywhere from 0 to 60 percent crystallization during flow advance. To improve constraints for Martian flows, we need to search for correlations in terrestrial flows between flow morphology and the amount of crystallization during emplacement.

Crisp, J.↗

Visualization of boundary-layer development on turbomachine blades with liquid crystals

This report documents a study of the use of liquid crystals to visualize boundary layer development on a turbomachine blade. A turbine blade model in a linear cascade of blades was used for the tests involved. Details of the boundary layer development on the suction surface of the turbine blade model were known from previous research. Temperature sensitive and shear sensitive liquid crystals were tried as visual agents. The temperature sensitive crystals were very effective in their ability to display the location of boundary layer flow separation and reattachment. Visualization of natural transition from laminar to turbulent boundary layer flow with the temperature sensitive crystals was possible but subtle. The visualization of separated flow reattachment with the shear sensitive crystals was easily accomplished when the crystals were allowed to make a transition from the focal-conic to a Grandjean texture. Visualization of flow reattachment based on the selective reflection properties of shear sensitive crystals was achieved only marginally because of the larger surface shear stress and shear stress gradient levels required for more dramatic color differences.

Vanzante, Dale E.↗

A shear sensitive monomer-polymer liquid crystal system for wind tunnel applications

Characteristics of a liquid crystal system, comprised of a shear-sensitive cholesteric-monomer liquid crystal thin-film coated on a liquid-crystal polymer substrate, are described. The system provides stable Grandjean texture, a desirable feature for shear-stress measurements using selective reflection from the monomer liquid-crystal helix structure. Impingement of gas or air flow on the monomer liquid-crystal free surface changes the wavelength of the selective reflection for an incident white light from red toward blue with increase in the rate of gas flow. The contrast of the selectively reflected light improves considerably by providing a thin black coating of about 5 microns at the monomer-polymer interface. The coating thickness is such that the steric interactions are still sufficiently strong to maintain Grandjean texture. For a small angle of incidence of a monochromatic light, the measurement of the reflected light intensity normal to the monomer-polymer liquid-crystal interface enables the determination of the wavelength for selective reflection as a function of the gas-flow differential pressure applied in the plane of the interface. The variation of the wavelength with the pressure is linear with a slope of about 2 nm/mmHg. Furthermore, the shear-stress effects are reversible unlike for monomer liquid crystal-metal systems used for flow visualization on wind-tunnel model surfaces. The present system offers a suitable method for direct on-line measurement of shear stress field from measurements of the wavelength for selective reflection for an incident white light.

Parmar, D. S.↗

Secondary orientation effects in a single crystal superalloy under mechanical and thermal loads

The nickel-base single crystal superalloy PWA 1480 is a candidate blading material for the advanced turbopump development program of the SSME. In order to improve thermal fatigue resistance of the turbine blades, the single crystal superalloy PWA 1480 is grown along the low modulus zone axes (001) crystal orientation by a directional solidification process. Since cubic single crystal materials such as PWA 1480 exhibit anisotropic elastic behavior, the stresses developed within the single crystal superalloy due to mechanical and thermal loads are likely to be affected by the exact orientation of the secondary crystallographic direction with respect to the geometry of the turbine blade. The effects of secondary crystal orientation on the elastic response of single crystal PWA 1480 superalloy were investigated.

Kalluri, Sreeramesh↗

Mapping crystal defects with a digital scanning ultramicroscope

A computer controlled scanning ultramicroscope has been built to assist in the characterization of transparent crystals. The device measures the scattering of a focused He-Ne laser beam by crystalline defects. As an XYZ translation table moves the crystal under the ultramicroscope, the scattered light is measured by a photodetector whose output is digitized and recorded. From this data, contour maps or three dimensional perspective plots of the scattering regions of the crystal can be generated to assist in finding patterns of defects which might be correlated with perturbations in the growth process. The verified resolution of the present instrument is about 1 micrometer, which is limited by the minimum step of the stepper-motor driven translation stages, optical diffraction effects and the sensitivity of the detector at the laser light frequency. The instrument was used to build a database of defects patterns in commercial laboratory grown triglycine sulphate (TGS) crystals, and to map defects in a TGS crystal grown from aqueous solution during the flight of Spacelab 3. This crystal shows indications of a reduction both in the generation of defects at the seed-new growth interface and in their propagation into the new crystal.

Springer, J. M.↗