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NASA NTRS1998

Gaseous Etching for Characterization of Structural Defects in Silicon Carbide Single Crystals

Single crystal SiC substrates were subjected to high-temperature H2/C3H8 gaseous etches. The etches resulted in a variety of surface features on 4H-SiC substrates that included elongated hillocks from 10 to more than 100 microns in length by a few microns in width. In some 4H- and 6H-SiC substrates, the etches resulted in a continuous coverage of macrosteps. We conclude that the morphology observed after the etching process is influenced by the local Si-C bilayer stacking sequence on the surface of off-(0001)oriented substrates. A model is presented for the formation of the hillocks, based on localized transformations of the 4H substrates during the high temperature etch process.

Powell, J. A.↗

NASA NTRS2000

Design and Performance of McRas in SCMs and GEOS I/II GCMs

The design of a prognostic cloud scheme named McRAS (Microphysics of clouds with Relaxed Arakawa-Schubert Scheme) for general circulation models (GCMs) will be discussed. McRAS distinguishes three types of clouds: (1) convective, (2) stratiform, and (3) boundary-layer types. The convective clouds transform and merge into stratiform clouds on an hourly time-scale, while the boundary-layer clouds merge into the stratiform clouds instantly. The cloud condensate converts into precipitation following the auto-conversion equations of Sundqvist that contain a parametric adaptation for the Bergeron-Findeisen process of ice crystal growth and collection of cloud condensate by precipitation. All clouds convect, advect, as well as diffuse both horizontally and vertically with a fully interactive cloud-microphysics throughout the life-cycle of the cloud, while the optical properties of clouds are derived from the statistical distribution of hydrometeors and idealized cloud geometry. An evaluation of McRAS in a single column model (SCM) with the GATE Phase III and 5-ARN CART datasets has shown that together with the rest of the model physics, McRAS can simulate the observed temperature, humidity, and precipitation without many systematic errors. The time history and time mean incloud water and ice distribution, fractional cloudiness, cloud optical thickness, origin of precipitation in the convective anvil and towers, and the convective updraft and downdraft velocities and mass fluxes all show a realistic behavior. Performance of McRAS in GEOS 11 GCM shows several satisfactory features but some of the remaining deficiencies suggest need for additional research involving convective triggers and inhibitors, provision for continuously detraining updraft, a realistic scheme for cumulus gravity wave drag, and refinements to physical conditions for ascertaining cloud detrainment level.

Sud, Yogesh C.↗

NASA NTRSDate not supplied

Energy landscape in Ni-Co-Cr and related alloys

Among multi-principal element alloys, the NiCoCr middle-entropy alloy has an outstanding combination of strength and ductility at both low and elevated temperatures. Equiatomic NiCoCr is a single-phase alloy with the face centered cubic (fcc) crystal structure. A low stacking fault energy in the fcc matrix is a cause of a relatively low creep in this alloy. The hexagonal close-packed (hcp) structure differs from the fcc by a stacking of atomic layers. The energy difference between the hcp and fcc structures is known to correlate with the stacking fault energy in the fcc phase. We compute formation and relative structural energies versus composition in the Ni-Co-Cr ternary and related quaternary systems, discuss possibilities of compositional adjustments, and compare theoretical predictions with experiment. We acknowledge funding by NASA’s Aeronautics Research Mission Directorate (ARMD) via Transformational Tools and Technologies (TTT) Project.

NiCoCr↗

NASA NTRSDate not supplied

Energy landscape in Ni-Co-Cr and related alloys

Multiscale↗

NASA NTRS2012

CIRS and CIRS-Lite as Designed for the Outer Planets: TSSM, EJSM, JUICE

Brasunas, J.↗

NASA NTRS2020

Shock Deformation in Zircon, a Comparison of Results from Shock-Reverberation and Single-Shock Experiments

The utility of the mineral zircon, ZrSiO4, as a shock-metamorphic geobarometer and geochronometer, has been steadily growing within the planetary science community. Zircon is an accessory phase found in many terrestrial rock types, lunar samples, lunar meteorites, martian meteorites and various other achondrites. Because zircon is refractory and has a high closure temperature for Pb diffusion, it has been used to determine the ages of some of the oldest material on Earth and elsewhere in the Solar System. Furthermore, major (O) and trace-element (REE, Ti, Hf) abundances and isotope compositions of zircon help characterize the petrogenetic environments and sources from which they crystallized. The response of zircon to impact-induced shock deformation is predominantly crystallographic, including dislocation creep and the formation of planar and sub-planar, low-angle grain boundaries; the formation of mechanical {112} twins; transformation to the high pressure polymorph reidite; the development of polycrystalline microtextures; and dissociation to the oxide constituents SiO2 and ZrO2. Shock microstructures can also variably affect the U- Pb isotope systematics of zircon and, in some instances, be used to constrain the impact age. While numerous studies have characterized shock deformation in zircon recovered from a variety of terrestrial impact craters and ejecta deposits and Apollo samples, experimental studies of shock deformation in zircon are limited to a handful of examples in the literature. In addition, the formation conditions (e.g., P, T) of various shock microstructures, such as planar-deformation bands, twins, and reidite lamellae, remain poorly con-strained. Furthermore, previous shocked-zircon experimental charges have not been analyzed using modern analytical equipment. This study will therefore under-take an new set of zircon shock experiments, which will then be microstructurally characterized using state-of-the-art instrumentation within the Astromaterials Research and Exploration Science Division (ARES), NASA Johnson Space Center.

Erickon, T. M.↗

NASA NTRS1998

Interaction between Convection and Heat Transfer in Crystal Growth

Crystals are integral components in some of our most sophisticated and rapidly developing industries. Single crystals are solids with the most uniform structures that can be obtained on an atomic scale. Because of their structural uniformity, crystals can transmit acoustic and electromagnetic waves and charged particles with essentially no scattering or interferences. This transparency, which can be selectively modified by controlled additions of impurities known as dopants, is the foundation of modern electronic industry. It has brought about widespread application of crystals in transistors, lasers, microwave devices, infrared detectors, magnetic memory devices, and many other magnets and electro-optic components. The performance of a crystal depends strongly on its compositional homogeneity. For instance, in modern microcircuitry, compositional variations of a few percent (down to a submicron length scale) can seriously jeopardize predicted yields. Since crystals are grown by carefully controlled phase transformations, the compositional adjustment in the solid is often made during growth from the nutrient. Hence, a detailed understanding of mass transfer in the nutrient is essential. Moreover, since mass transfer is often the slowest process during growth, it is usually the rate limiting mechanism. Crystal growth processes are usually classified according to the nature of the parent phase. Nevertheless, whether the growth occurs by solidification from a melt (melt growth), nucleation from a solution (solution growth), condensation from a vapor (physical vapor transport) or chemical reaction of gases (chemical vapor deposition), the parent phase is a fluid. As is with most non-equilibrium processes involving fluids, liquid or vapor, fluid motion plays an important role, affecting both the concentration and temperature gradients at the soli-liquid interface.

Source record↗

NASA NTRS1984

Containerless drop tube solidification and grain refinement of NiAl3

The possibility of undercooling Ni-Al alloys below the liquidus in order to produce a single phase peritectic structure by containerless drop tube solidification was studied. Containerless process is a technique for both high purity contamination free studies as well as for investigating the undercooling and rapid solidification of alloys by suppression of heterogeneous nucleation on container walls. In order to achieve large undercoolings one must avoid heterogeneous nucleation of crystallization. It was shown that the Marshall Space Flight Center drop tubes ae unique facilities for containerless solidification experiments and large undercoolings are possible with some alloys. The original goal of undercooling the liquid metal well below the liquidus to the peritectic temperature during containerless free to form primarily NiAl3 was achieved. The microstructures were interesting from another point of view. The microstructure from small diameter samples is greatly refined. Small dendrite arm spacings such as these could greatly facilitate the annealing and solid state transformation of the alloy to nearly 10% NiAl3 by reducing the distance over which diffusion needs to occur. This could minimize annealing time and might make it economically feasible to produce NiAl3 alloy.

Ethridge, E. C.↗

NASA NTRS2005

Thermophysical and Optical Properties of Semiconducting Ga2Te3 Melt

The majority of bulk semiconductor single crystals are presently grown from their melts. The thermophysical and optical properties of the melts provide a fundamental understanding of the melt structure and can be used to optimize the growth conditions to obtain higher quality crystals. In this paper, we report several thermophysical and optical properties for Ga2Te3 melts, such as electrical conductivity, viscosity, and optical transmission for temperatures ranging from the melting point up to approximately 990 C. The conductivity and viscosity of the melts are determined using the transient torque technique. The optical transmission of the melts is measured between the wavelengths of 300 and 2000 nm by an dual beam reversed-optics spectrophotometer. The measured properties are in good agreement with the published data. The conductivities indicate that the Ga2Te3 melt is semiconductor-like. The anomalous behavior in the measured properties are used as an indication of a structural transformation in the Ga2Te3 melt and discussed in terms of Eyring's and Bachinskii's predicted behaviors for homogeneous melts.

Li, Chao↗

NASA NTRS2003

Diaplectic Glass Content in Experimentally Shock-loaded Quartz Determined by X-Ray Powder Diffraction

Quartz is the most common mineral of terrestrial crustal rocks and thus a widespread indicator for impact cratering and associated shock metamorphism. Planar deformation features (PDFs) are among the most prominent and diagnostic shock features in quartz and they represent thin lamellae of glass that formed via solid-state transformations. This socalled 'diaplectic' glass becomes pervasive at higher pressures and results in optically isotropic and X-ray-amorphous phases that resemble texturally the original quartz grains (without evidence of melt flow). In the past, it has been shown that the amount of this amorphous material in experimentally shock-loaded quartz correlates with peak shock pressure. Both reports derive the glass content from density measurements of individual crystals employing the equation X(%) = (rho(sub x) - rho(sub 0))/(rho(sub x) - rho(sub gl)), where x and 0 stands for X-ray and average (optical) density, respectively. The density of glass, rho(sub gl), was adopted as 2.2 g/cu cm. Though the same procedures had been applied, the resulting glass content differs significantly among the above studies. In the present study, we are using a new approach based solely on the integral intensity of a single, carefully selected reflection in the XRD pattern, and we will compare our data to those reported in the literature.

Skala, R.↗

NASA NTRSDate not supplied

TPSAS-NF1676L-17800-DND

Currently, there are two national challenge problems that guide much of the research in durability and damage tolerance at NASA Langley. The first, Airframe Digital Twin, is a concept that combines as-built vehicle components, as-experienced loads and environments, and other vehicle-specific characteristics to enable ultrahigh fidelity modeling of aircraft and spacecraft throughout their service lives. The second, Materials Genome Initiative, is an analog to the Human Genome Project, and is intended to improve the rate at which materials scientists can discover, understand fundamental physics, and improve material systems. This presentation will highlight several research projects ongoing at NASA Langley that are in support of the above challenge problems. Two of those topics will be the subject of detailed discussion. First, investigations of microstructurally-small fatigue cracking (MSFC) in Al-2Cu and Al-4Cu, fabricated in-house, will be presented. Single- and oligo-crystals of Al-Cu specimens were loaded in uniaxial fatigue, while high-resolution in-situ measurements of deformation were made using image correlation (IC) in a scanning-electron microscope (SEM). The Al-Cu specimens were then replicated as crystal plasticity finite element models (CPFEM), where evolution of slip localization near grain boundaries was computed. Comparison among experiment and CPFEM is made. In addition, XRay diffraction measurements of the as-fabricated specimens were carried out, where direct measurements of the embedded copper precipitates were made, and their influence on growing MSFCs were directly observed. The second main topic will illustrate ongoing work in the area of so-called damage-sensing particles. In this work, shape-memory alloys are embedded in an aluminum alloy matrix. Upon the propagation of a fatigue crack, these particles undergo a strain-induced phase transformation which is detected using an acoustic sensor, providing real-time information on propagating cracks. Experiments and simulations regarding the development of this system will also be detailed.

Jacob Hochhalter↗

NASA NTRS1998

Ground Based Program for the Physical Analysis of Macromolecular Crystal Growth

During the past year we have focused on application of in situ Atomic Force Microscopy (AFM) for studies of the growth mechanisms and kinetics of crystallization for different macromolecular systems. Mechanisms of macrostep formation and their decay, which are important in understanding of defect formation, were studied on the surfaces of thaumatin, catalase, canavalin and lysozyme crystals. Experiments revealed that step bunching on crystalline surfaces occurred either due to two- or three-dimensional nucleation on the terraces of vicinal slopes or as a result of uneven step generation by complex dislocation sources. No step bunching arising from interaction of individual steps in the course of the experiment was observed. The molecular structure of the growth steps for thaumatin and lipase crystals were deduced. It was further shown that growth step advance occurs by incorporation of single protein molecules. In singular directions growth steps move by one-dimensional nucleation on step edges followed by lateral growth. One-dimensional nuclei have different sizes, less then a single unit cell, varying for different directions of step movement. There is no roughness due to thermal fluctuations, and each protein molecule which incorporated into the step remained. Growth kinetics for catalase crystals was investigated over wide supersaturation ranges. Strong directional kinetic anisotropy in the tangential step growth rates in different directions was seen. The influence of impurities on growth kinetics and cessation of macromolecular crystals was studied. Thus, for catalase, in addition to pronounced impurity effects on the kinetics of crystallization, we were also able to directly observe adsorption of some impurities. At low supersaturation we repeatedly observed filaments which formed from impurity molecules sedimenting on the surfaces. Similar filaments were observed on the surfaces of thaumatin, canavalin and STMV crystals as well, but the frequency was low compared with catalase crystallization. Cessation of growth of xylanase and lysozyme crystals was also observed and appeared to be a consequence of the formation of dense impurity adsorption layers. Attachment: "An in situ AFM investigation of catalase crystallization", "Atomic force microscopy studies of living cells: visualization of motility, division, aggregation, transformation, and apoptosis", AFM studies on mechanisms of nucleation and growth of macromolecular crystals", and "In situ atomic force microscopy studies of surface morphology, growth kinetics, defect structure and dissolution in macromolecular crystallization".

Malkin, Alexander J.↗

NASA NTRS2003

Creep Resistance of ZrO2 Ceramic Improved by the Addition of a Small Amount of Er2O3

Zirconia (ZrO2) has great technological importance in structural, electrical, and chemical applications. It is the crucial component for state-of-the art thermal barrier coatings and an enabling component as a solid electrolyte for solid-oxide fuel cell systems. Pure ZrO2 is of limited use for industrial applications because of the phase transformations that occur. Upon the addition of stabilizers, cubic (c-ZrO2) and tetragonal (t-ZrO2) forms can be preserved. It is the stabilized and partially stabilized forms of zirconia that function as thermal barrier coatings, solid electrolytes, and oxygen sensors and that have numerous applications in the electrochemical industry. The cubic form of ZrO2 is typically stabilized through Y2O3 additions. However, Y2O3-stabilized zirconia is susceptible to deformation at high temperatures (greater than 900 C) because of the large number of slip systems and the high oxygen diffusion rates, which result in high creep rates at high temperatures. Successful use of ZrO2 at high temperatures requires that new dopant additives be found that will retain or enhance the desirable properties of cubic ZrO2 and yet produce a material with lower creep rates. At the NASA Glenn Research Center, erbium oxide (Er2O3) was identified as a promising dopant for improving the creep resistance of. ZrO2. The selection of Er2O3 was based on the strong interactions of point defects and dislocations. Single crystals of 5 mol% Er2O3- doped ZrO2 rods (4 mm in diameter) and monofilaments (200 to 300 mm in diameter and 30 cm long) were grown using the laser-heated float zone technique, and their creep behavior was measured as a function of temperature. The addition of 5 mol% Er2O3 to single-crystal ZrO2 improved its creep resistance at high temperatures by 2 to 3 orders of magnitude over state-of-the-art Y2O3-doped crystals. Detailed microstructural characterization of ZrO2-Er2O3 single crystals has identified new mechanisms for improving the creep resistance of this class of materials. Adding Er2O3 to ZrO2 results in microstructure of stable and metastable tetragonal precipitates that with thermal treatment evolve to a tweed structure of nanosize tetragonal lamellae. The superior high-temperature creep resistance of Er2O3-doped ZrO2 is attributed to nanoscale precipitation hardening. Doping with Er2O3 will significantly increase the upper-use temperature limit of ZrO2. Potential applications include using Er2O3-doped ZrO2 as a high-temperature fiber for structural applications and adding Er2O3 to reduce the sintering rates of ZrO2 thermal barrier coatings. This work was conducted at Dpto. de F sica de la Materia Condensada, Universidad de Sevilla, Spain, and at NASA Glenn.

Martinez-Fernandez, Julian↗

NASA NTRS2000

Over-Expression, Purification and Crystallization of Human Dihydrolipoamide Dehydrogenase

Dehydrolipoamide dehydrogenase (E3; dihydrolipoan-tide:NAD+ oxidoreductase, EC 1.8.1.4) is a common catalytic component found in pyruvate dehydrogenase complex, alpha-ketoglutarate dehydrogenase complex, and branched-chain cc-keto acid dehydrogenase complex. E3 is also a component (referred to as L protein) of the glycine cleavage system in bacterial metabolism (2). Active E3 forms a homodimer with four distinctive subdomain structures (FAD binding, NAD+ binding, central and interface domains) with non-covalently but tightly bound FAD in the holoenzyme. Deduced amino acids from cloned full-length human E3 gene showed a total of 509 amino acids with a leader sequence (N-terminal 35 amino acids) that is excised (mature form) during transportation of expressed E3 into mitochondria membrane. So far, three-dimensional structure of human E3 has not been reported. Our effort to achieve the elucidation of the X-ray crystal structure of human E3 will be presented. Recombinant pPROEX-1 expression vector (from GIBCO BRL Life Technologies) having the human E3 gene without leader sequence was constructed by Polymerase Chain Reaction (PCR) and subsequent ligation, and cloned in E.coli XL1-Blue by transformation. Since pPROEX-1 vector has an internal His-tag (six histidine peptide) located at the upstream region of a multicloning site, one-step affinity purification of E3 using nickelnitriloacetic acid (Ni-NTA) agarose resin, which has a strong affinity to His-tag, was feasible. Also a seven-amino-acid spacer peptide and a recombinant tobacco etch virus protease recognition site (seven amino acids peptide) found between His-tag and first amino acid of expressed E3 facilitated the cleavage of His-tag from E3 after the affinity purification. By IPTG induction, ca. 15 mg of human E3 (mature form) was obtained from 1L LB culture with overnight incubation at 25C. Over 98% of purity of E3 from one-step Ni-NTA agarose affinity purification was confirmed by SDS-PAGE analysis. For crystallization, E3 samples were prepared with and without His-tag. To minimize the aggregation of E3, apo- and holo- forms of E3s were tested, as well as a mutated E3. Dynamic light scattering measurements revealed that the E3 preparations without His-tag and substrate are highly monodispersive with regard to homodimers. Consequent crystallization trials of this E3 preparation led to single crystals of E3 grown by the vapor diffusion method. Crystals were obtained within a few days from solution containing poly (ethylene glycol) monomethyl ether 5000 as a precipitant. Autoindexing and integration of the X-ray diffraction data showed that E3 crystals belong to an orthorhombic system with unit cell parameters a-- 123. 1, b= 165.3 and c=214.3A. Further optimization of protein preparation and crystallization experiments for the structural determination will be discussed.

Hong, Y. S.↗

NASA NTRS2011

CIRS-lite, a Fourier Transform Spectrometer for Low-Cost Planetary Missions

Passive spectroscopic remote sensing of planetary atmospheres and surfaces in the thermal infrared is a powerful tool for obtaining information about surface and atmospheric temperatures, composition, and dynamics (via the thermal wind equation). Due to its broad spectral coverage, the Fourier transform spectrometer (FTS) is particularly suited to the exploration and discovery of molecular species. NASA's Goddard Space Flight Center (GSFC) developed the CIRS (Composite Infrared Spectrometer) FTS for the NASA/ESA Cassini mission to the Saturnian system. CIRS observes Saturn, Titan, icy moons such as Enceladus, and the rings in thermal self-emission over the spectral range of 7 to 1000 ell11. CIRS has given us important new insights into stratospheric composition and jets on Jupiter and Saturn, the cryo-geyser and thermal stripes on Enceladus, and the winter polar vortex on Titan. CIRS has a mass of 43 kg, contrasted with the earlier GSFC FTS, pre-Voyager IRIS (14 kg). Future low-cost planetary missions will have very tight constraints on science payload mass, thus we must endeavor to return to IRIS-level mass while maintaining CIRS-level science capabilities ("do more with less"). CIRS-lite achieves this by pursuing: a) more sensitive infrared detectors (high Tc superconductor) to enable smaller optics. b) changed long wavelength limit from 1000 to 300 microns to reduce diffraction by smaller optics. c) CVD (chemical vapor deposition) diamond beam-splitter for broad spectral coverage. d) single FTS architecture instead of a dual FTS architecture. e) novel materials, such as single crystal silicon for the input telescope primary.

Brasunas, J.↗

NASA NTRS2010

315mJ, 2-micrometers Double-Pulsed Coherent Differential Absorption Lidar Transmitter for Atmospheric CO2 Sensing

The design of a double pulsed, injection seeded, 2-micrometer compact coherent Differential absorption Lidar (DIAL) transmitter for CO2 sensing is presented. This system is hardened for ground and airborne applications. The design architecture includes three continuous wave lasers which provide controlled on and off line seeding, injection seeded power oscillator and a single amplifier operating in double pass configuration. As the derivative a coherent Doppler wind lidar, this instrument has the added benefit of providing wind information. The active laser material used for this application is a Ho: Tm:YLF crystal operates at the eye-safe wavelength. The 3-meter long folded ring resonator produces energy of 130-mJ (90/40) with a temporal pulse length around 220 nanoseconds and 530 nanosecond pulses for on and off lines respectively. The separation between the two pulses is on the order of 200 microseconds. The line width is in the order of 2.5MHz and the beam quality has an M(sup 2) of 1.1 times diffraction limited beam. A final output energy for a pair of both on and off pulses as high as 315 mJ (190/125) at a repetition rate of 10 Hz is achieved. The operating temperature is set around 20 C for the pump diode lasers and 10 C for the rod. Since the laser design has to meet high-energy as well as high beam quality requirements, close attention is paid to the laser head design to avoid thermal distortion in the rod. A side-pumped configuration is used and heat is removed uniformly by passing coolant through a tube slightly larger than the rod to reduce thermal gradient. This paper also discusses the advantage of using a long upper laser level life time laser crystal for DIAL application. In addition issues related to injection seeding with two different frequencies to achieve a transform limited line width will be presented.

Yu, Jirong↗