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NASA NTRS2006

In-Situ Crystallization of a Lithium Disilicate Glass--Effect of Pressure on Crystal Growth Rate

Crystallization of a Li2O.2SiO2 (LS2) glass subjected to a uniform hydrostatic pressure of 4.5 GPa and 6 GPa was investigated up to a temperature of 750 C. The density of the compressed glass is about 2% greater at 4.5 GPa than at 1 atm and, depending upon the processing temperature, up to 10% greater at 6 GPa. Crystal growth rates investigated as a function of temperature and pressure show that lithium disilicate crystal growth is an order of magnitude slower at 4.5 GPa than 1 atm resulting in a shift of +45 C (plus or minus 10 C) in the growth rate curve at high pressure compared to 1 atm condition. At 6 GPa lithium disilicate crystallization is suppressed entirely, while a new high pressure lithium metasilicate crystallizes at temperatures 95 C (plus or minus 10 C) higher than those reported for lithium disilicate crystallization at 1 atm. The decrease in crystal growth rate with increasing pressure for lithium disilicate glass up to 750 C is related to an increase in viscosity with pressure associated with fundamental changes in glass structure accommodating densification.

Fuss, T.↗

NASA NTRS1991

High resolution synchrotron X-radiation diffraction imaging of crystals grown in microgravity and closely related terrestrial crystals

Irregularities in three crystals grown in space and in four terrestrial crystals grown under otherwise comparable conditions have been observed in high resolution diffraction imaging. The images provide important new clues to the nature and origins of irregularities in each crystal. For two of the materials, mercuric iodide and lead tin telluride, more than one phase (an array of non-diffracting inclusions) was observed in terrestrial samples; but the formation of these multiple phases appears to have been suppressed in directly comparable crystals grown in microgravity. The terrestrial seed crystal of triglycine sulfate displayed an unexpected layered structure, which propagated during directly comparable space growth. Terrestrial Bridgman regrowth of gallium arsenide revealed a mesoscopic structure substantially different from that of the original Czochralski material. A directly comparable crystal is to be grown shortly in space.

Steiner, Bruce↗

NASA NTRS2000

Effect of Crystal Orientation on Fatigue Failure of Single Crystal Nickel Base Turbine Blade Superalloys

High Cycle Fatigue (HCF) induced failures in aircraft gas-turbine engines is a pervasive problem affecting a wide range of components and materials. HCF is currently the primary cause of component failures in gas turbine aircraft engines. Turbine blades in high performance aircraft and rocket engines are increasingly being made of single crystal nickel superalloys. Single-crystal Nickel-base superalloys were developed to provide superior creep, stress rupture, melt resistance and thermomechanical fatigue capabilities over polycrystalline alloys previously used in the production of turbine blades and vanes. Currently the most widely used single crystal turbine blade superalloys are PWA 1480/1493 and PWA 1484. These alloys play an important role in commercial, military and space propulsion systems. PWA1493, identical to PWA1480, but with tighter chemical constituent control, is used in the NASA SSME (Space Shuttle Main Engine) alternate turbopump, a liquid hydrogen fueled rocket engine. Objectives for this paper are motivated by the need for developing failure criteria and fatigue life evaluation procedures for high temperature single crystal components, using available fatigue data and finite element modeling of turbine blades. Using the FE (finite element) stress analysis results and the fatigue life relations developed, the effect of variation of primary and secondary crystal orientations on life is determined, at critical blade locations. The most advantageous crystal orientation for a given blade design is determined. Results presented demonstrates that control of secondary and primary crystallographic orientation has the potential to optimize blade design by increasing its resistance to fatigue crack growth without adding additional weight or cost.

Arakere, Nagaraj K.↗

NASA NTRS1979

Low dimensional magnetic solids and single crystal elpasolites: Need for improved crystal growing techniques

The need for extensive crystal growing experiments to develop techniques for preparing crystals suitable for magnetic anisotropy measurements and detailed X-ray and neutron diffraction studies is rationalized on the basis of the unique magnetic properties of the materials and their hydrogen bonded structures which have many features in common with metalloenzyme and metalloprotein active sites. Single crystals of the single and mixed lanthanide species are prepared by the Bridgeman technique of gradient solidification of molten samples. The effects of crystal imperfections on the optical properties of these materials are an important part of the projected research. A series of a-amido acid complexes of first row transition metals were prepared which crystallize as infinite linear chains and exhibit low dimensional magnetic ordering (one or two) at temperature below 40 K.

Good, M. L.↗

NASA NTRS1990

Crystal-melt interface shape of Czochralski-grown large diameter germanium crystals

Crystal-melt interface shapes of 100 to 200 mm diameter 111-line Ge grown by the Czochralski technique have been examined using the method of fast withdrawal from the melt. Initially, the interface shape is convex, then transforms gradually into a sigmoidal shape, becomes nearly planar at about one third of the final crystal length, and finally assumes a concave profile with progressively increasing curvature. The nearly planar interface has a double-facet structure, with an annular facet at the edge of the crystal in addition to the central (111) facet. Formation of the annular facet is accompanied by a giant oscillation of the pull rate when the maximum average pull rate is exceeded. Such oscillation is detrimental to crystal quality, since it introduces a region of high dislocation density. An average pull rate maximum of 2 cm/h has been found to allow for a smooth growth of 200 mm diameter crystals. The origin of the pull rate perturbation is discussed in terms of an instantaneous change in the equilibrium shape of the meniscus.

Roth, M.↗

NASA NTRS1992

Vapor crystal growth studies of single crystals of mercuric iodide (3-IML-1)

A single crystal of mercuric iodide (HgI2) will be grown during the International Microgravity Lab. (IML-1) mission. The crystal growth process takes place by sublimation of HgI2 from an aggregate of purified material, transport of the molecules in the vapor from the source to the crystal, and condensation on the crystal surface. The objectives of the experiment are as follow: to grow a high quality crystal of HgI2 of sufficient size so that its properties can be extensively analyzed; and to study the vapor transport process, specifically the rate of diffusion transport at greatly reduced gravity where convection is minimized.

Vandenberg, Lodewijk↗

NASA NTRS1992

A comparison between protein crystals grown with vapor diffusion methods in microgravity and protein crystals using a gel liquid-liquid diffusion ground-based method

Crystals of human serum albumin have been successfully grown in a variety of gels using crystallization conditions otherwise equivalent to those utilized in the popular hanging-drop vapor-equilibrium method. Preliminary comparisons of gel grown crystals with crystals grown by the vapor diffusion method via both ground-based and microgravity methods indicate that crystals superior in size and quality may be grown by limiting solutal convection. Preliminary X-ray diffraction statistics are presented.

Miller, Teresa Y.↗

NASA NTRS1999

Searching for the Best Protein Crystals: Synchrotron Based Measurements of Protein Crystal Quality

We are developing X-ray diffraction methods to quantitatively evaluate the quality of protein crystals. The ultimate use for these crystal quality will be to optimize crystal growth and freezing conditions to obtain the best diffraction data. We have combined super fine-phi slicing with highly monochromatic, low divergence synchrotron radiation and the ADSC Quantum 4 CCD detector at the Stanford Synchrotron Radiation laboratory beamline 1.5 to accurately measure crystal mosaicity. Comparisons of microgravity versus earth-grown insulin crystals using these methods will be presented.

Borgstahl, Gloria↗

NASA NTRS2015

Lunar Magma Ocean Crystallization: Constraints from Fractional Crystallization Experiments

The currently accepted paradigm of lunar formation is that of accretion from the ejecta of a giant impact, followed by crystallization of a global scale magma ocean. This model accounts for the formation of the anorthosite highlands crust, which is globally distributed and old, and the formation of the younger mare basalts which are derived from a source region that has experienced plagioclase extraction. Several attempts at modelling the crystallization of such a lunar magma ocean (LMO) have been made, but our ever-increasing knowledge of the lunar samples and surface have raised as many questions as these models have answered. Geodynamic models of lunar accretion suggest that shortly following accretion the bulk of the lunar mass was hot, likely at least above the solidus]. Models of LMO crystallization that assume a deep magma ocean are therefore geodynamically favorable, but they have been difficult to reconcile with a thick plagioclase-rich crust. A refractory element enriched bulk composition, a shallow magma ocean, or a combination of the two have been suggested as a way to produce enough plagioclase to account for the assumed thickness of the crust. Recently however, geophysical data from the GRAIL mission have indicated that the lunar anorthositic crust is not as thick as was initially estimated, which allows for both a deeper magma ocean and a bulk composition more similar to the terrestrial upper mantle. We report on experimental simulations of the fractional crystallization of a deep (approximately 100km) LMO with a terrestrial upper mantle-like (LPUM) bulk composition. Our experimental results will help to define the composition of the lunar crust and mantle cumulates, and allow us to consider important questions such as source regions of the mare basalts and Mg-suite, the role of mantle overturn after magma ocean crystallization and the nature of KREEP

Rapp, J. F.↗

NASA NTRS1979

Growth of silicon carbide crystals on a seed while pulling silicon crystals from a melt

A saturated solution of silicon and an element such as carbon having a segregation coefficient less than unity is formed by placing a solid piece of carbon in a body of molten silicon having a temperature differential decreasing toward the surface. A silicon carbide seed crystal is disposed on a holder beneath the surface of the molten silicon. As a rod or ribbon of silicon is slowly pulled from the melt, a supersaturated solution of carbon in silicon is formed in the vicinity of the seed crystal. Excess carbon is emitted from the solution in the form of silicon carbide which crystallizes on the seed crystal held in the cool region of the melt.

Ciszek, T. F.↗

NASA NTRS1987

In situ observation of mono-molecular growth steps on aqueous solution grown crystals and the transport of molecules to the crystals

Direct in situ observation of mono-molecular growth steps on a crystal growing in an aqueous solution became possible. The combination of this method with high resolution Schlieren methods or interferometry, permits the growth mechanism of crystals to be investigated directly. Since the observation of growth steps on crystals is the most direct and sensitive way for investigating a crystal growth mechanism, it would contribute to revealing fundamental differences between the growth in space and on Earth. The method was recently extended to in situ observation of the growth processes at high temperatures (1800K).

Tsukamoto, Katsuo↗

NASA NTRS1991

High resolution diffraction imaging of crystals grown in microgravity and closely related terrestrial crystals

Irregularities found in three crystals grown in space, in four crystals grown entirely on the ground were examined and compared. Irregularities were observed in mercuric iodide, lead tin telluride, triglycine sulfate, and gallium arsenide by high resolution synchrotron x radiation diffraction imaging. Radiation detectors made from mercuric iodide crystals grown in microgravity were reported to perform far better than conventional detectors grown from the same material under full gravity. Effort is now underway to reproduce these 'space' crystals, optimize their properties, and extend comparable superiority to other types of materials.

Steiner, B.↗

NASA NTRS1994

Direct observation of crystal growth from solution using optical investigation of a growing crystal face

The first technical report for the period 1 Jan. 1993 till 31 Dec. 1993 for the research entitled, 'Direct observation of crystal growth from solution using Optical Investigation of a growing crystal Face' is presented. The work on the project did not start till 1 June 1993 due to the non-availability of the required personnel. The progress of the work during the period 1 June 1993 till the end of 1993 is described. Significant progress was made for testing various optical diagnostic techniques for monitoring crystal solution. Some of the techniques that are being tested are: heterodyne detection technique, in which changes in phase are measured as a interferometric function of time/crystal growth; a conventional technique, in which a fringe brightness is measured as a function of crystal growth/time; and a Mach-Zehnder interferometric technique in which a fringe brightness is measured as a function of time to obtain information on concentration changes. During the second year it will be decided to incorporate the best interferometric technique along with the ellipsometric technique, to obtain real time in-situ growth rate measurements. A laboratory mock-up of the first two techniques were made and tested.

Lal, Ravindra↗

NASA NTRSDate not supplied

Evaluation of a Thermodynamic Ice Crystal Accretion Model using Experimental Data from NASA’s 2nd Fundamental Ice Crystal Icing Test

A thermodynamic model describing ice crystal icing is evaluated using experimental data collected at NASA Propulsion Systems Laboratory. The model makes the distinction between ice accretions that are "freeze-dominated" and "melt-dominated". Freeze-dominated icing occurs when partially melted ice crystals impact a surface and freeze. This type of icing is characterized by strong adhesion. This contrasts with melt-dominated icing, where un-melted ice crystals adhere to a surface. This type of icing is characterized by weak adhesion. In this paper, the thermodynamic model is used to analyze the ice growth rates and facility conditions to explain possible phenomena such as mass loss as well as the melting and freezing fractions. Previous analyses assumed a collection efficiency of unity at the leading edge of the experimental model. LEWICE is used to determine a better estimate of the collection efficiency at the model leading edge as ice accretion grows in time. The result shows that the sticking efficiency could change in a greater percent with time than previously reported.

Ice Crystal Icing↗

NASA NTRS1967

Surface-spike growth on NiBr sub 2 crystals - A VLS mode of crystal growth.

Droplets associated with surface-spike growth of crystals of NiBr 2 by sublimation have been analyzed and found to contain Cu, Co, Mn, and Fe in addition to Ni and Br. These elements exist in the bulk of the original charge material in concentrations that are several orders of magnitude lower than that in the droplets. During crystal growth by sublimation the impurities collect on the surface of growing crystals, until sufficient concentrations are reached to cause the nucleation of a metastable liquid phase droplet. Once the liquid phase droplets have been nucleated, they may then become attached to growth steps and produce accelerated growth from these sites. Such processes occur in NiBr 2 , during growth by sublimation, at approximately 500 °C below the melting point of NiBr 2 .

Edward N Sickafus↗

NASA NTRS1971

Polymer crystallization in a temperature gradient field with controlled crystal growth rate

A method is described for studying the influence of a temperature gradient on the crystallization of quiescent polymer melts. The apparatus used consists of two brass plates with embedded electrical resistance heaters and cooling coils. The crystallizations experiments were conducted by placing polymer specimens between the paltes, and manually adjusting heaters and cooling fluids for temperature control. Linear polyethylene, isotactic polyprophylene, and a high density polyethylene were used. It is concluded that the role of a temperature gradient in producing oriented crystallization is in producing conditions which lead the spherulitic growth pattern to proceed primarily in one direction. Steep gradients diminish the penetration of supercooling and favors oriented growth.

Hansen, D.↗

NASA NTRS1974

Measurements of the short-term stability of quartz crystal resonators: A window on future developments in crystal oscillators

Recent measurements of the inherent short-term stability of quartz crystal resonators are presented. These measurements show that quartz resonators are much more stable for times less than 1s than the best available commercial quartz oscillators. A simple model appears to explain the noise mechanism in crystal controlled oscillators and points the way to design changes which should permit more than 2 orders of magnitude improvement in their short-term stability. Calculations show that a reference signal at 1 THz, derived from frequency multiplying a 5 MHz source with the above measured crystal stability, should have an instantaneous or fast linewidth of order 1 Hz. These calculations explicitly include the noise contribution of our present multiplier chains and are briefly outlined.

Walls, F. L.↗

NASA NTRS1980

Means for growing ribbon crystals without subjecting the crystals to thermal shock-induced strains

A susceptor particularly suited for use in growing a ribbon crystal employing edge defined film fed growth techniques is described. The susceptor includes a die through which a melt is drawn for forming a crystal ribbon. This is combined with a coolant delivery system characterized by a pair of jets for directing a stream of fluid coolant along a path extended to impinge on the susceptor in close proximity with the die in nonincident relation with the crystal being grown.

Berkman, S.↗