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At least 739 records · Page 41

Process-Induced Morphological Defects in Epitaxial CVD Silicon Carbide

Silicon carbide (SiC) semiconductor technology has been advancing rapidly, but there are numerous crystal growth problems that need to be solved before SiC can reach its full potential. Among these problems is a need for an improvement in the surface morphology of epitaxial films that are grown to produce device structures. Various processes before and during epilayer growth lead to the formation of morphological defects observed in SiC epilayers grown on SiC substrates. In studies of both 6H and 4H-SiC epilayers, atomic force microscopy (AFM) and other techniques have been used to characterize SiC epilayer surface morphology. In addition to the well-known micropipe defect, SiC epilayers contain growth pits, triangular features (primarily) in 4H-SiC, and macro step due to step bunching. In work at NASA Lewis, it has been found that factors contributing to the formation of some morphological defects include: defects in the substrate bulk, defects in the substrate surface caused by cutting and polishing the wafer, the tilt angle of the wafer surface relative to the basal plane, and growth conditions. Some of these findings confirm results of other research groups. This paper presents a review of published and unpublished investigations into processes that are relevant to epitaxial film morphology.

Powell, J. A.↗

Fluorescence Studies of Protein Crystal Nucleation

We have postulated that, in the case of tetragonal chicken egg white lysozyme, crystal growth occurs by the addition of pre-critical nuclei sized n-mers that form in the bulk solution, and that the n-mer growth units were multiples of the tetrameric 4(sub 3) helical structure. These have the strongest intermolecular bonds in the crystal and are therefore likely to be the first species formed. High resolution AFM studies provide strong supporting evidence for this model, but the data also suggest that the actual species in solution may not be identical in structure to that found in the crystal. We are using fluorescence resonance energy transfer (FRET) to study the initial solution phase self-assembly process, using covalent fluorescent derivatives which crystallize in the characteristic P4(sub 3)2(sub 1)2(sub 1) space group. FRET studies are being carried out between the cascade blue (CB-lys, donor, Ex(sub max) 366 nm, Em 420 nm) and lucifer yellow (LY-lys, acceptor, Ex(sub max) 430 nm, Em 528 nm) asp101 derivatives. The estimated R(sub 0) for this probe pair, the distance where 50% of the donor energy is transferred to the acceptor, is approx. 1.2 nm, compared to 2.2 nm between the side chain carboxyls of adjacent asp101's in the crystalline 4(sub 3) helix. The short donor lifetime of 2.80 ns (chi(sup 2) = 0.644), coupled with the large average distances between the molecules (greater than or equal to 50 nm) in solution, ensure that any energy transfer observed is not due to random diffusive interactions. Lifetime data show that CB-lys has a single lifetime when it is the only species in solution. Similarly, LY-lys also exhibits a single lifetime of 4.63 ns (chi(sup 2) = 0.42) when alone in solution. Addition of LY-lys to CB-lys results in the appearance of a third lifetime component of 0.348ns for the CB-lys. The fractional intensities of the different species present can be used to estimate the distribution of monomer and n-mers in solution. The self-association process is a function of the protein concentration relative to the saturation concentration, and observing it in dilute solution (conc. less than or equal to 10(exp -5)M) requires that the experiments be performed under low solubility conditions, i.e., low temperatures and high salt concentrations. Data from preliminary steady state FRET studies with N-terminal bound pyrene acetic acid (PAA-lys, donor, Ex 340 nm, Em 376 nm) and asp101 LY-lys as an acceptor showed a consistent trend of decreasing donor fluorescence intensity with increasing total protein concentration. The FRET data have been obtained at pH 4.6, 0.1M NaAc buffer, at 5 and 7% NaCl, 4 C. The corresponding C(sub sat) values are 0.471 and 0.362 mg/ml (approx. 3.3 and approx. 2.5 x 10(exp -5)M respectively). The donor fluorescence decrease is more pronounced at7% NaCl, consistent with the expected increased intermolecular interactions at higher salt concentrations as reflected in the lower solubility. Results from these and other ongoing studies will be discussed in conjunction with an emerging model for how tetragonal lysozyme crystals nucleate and the relevance of that model to other proteins.

Pusey, Marc↗

Protein Crystal Growth Dynamics and Impurity Incorporation

The general concepts and theories of crystal growth are proven to work for biomolecular crystallization. This allowed us to extract basic parameters controlling growth kinetics - free surface energy, alpha, and kinetic coefficient, beta, for steps. Surface energy per molecular site in thermal units, alpha(omega)(sup 2/3)/kT approx. = 1, is close to the one for inorganic crystals in solution (omega is the specific molecular volume, T is the temperature). Entropic restrictions on incorporation of biomolecules into the lattice reduce the incorporation rate, beta, by a factor of 10(exp 2) - 10(exp 3) relative to inorganic crystals. A dehydration barrier of approx. 18kcal/mol may explain approx. 10(exp -6) times difference between frequencies of adding a molecule to the lattice and Brownian attempts to do so. The latter was obtained from AFM measurements of step and kink growth rates on orthorhombic lysozyme. Protein and many inorganic crystals typically do not belong to the Kossel type, thus requiring a theory to account for inequivalent molecular positions within its unit cell. Orthorhombic lysozyme will serve as an example of how to develop such a theory. Factors deteriorating crystal quality - stress and strain, mosaicity, molecular disorder - will be reviewed with emphasis on impurities. Dimers in ferritin and lysozyme and acetylated lysozyme, are microheterogeneous i.e. nearly isomorphic impurities that are shown to be preferentially trapped by tetragonal lysozyme and ferritin crystals, respectively. The distribution coefficient, K defined as a ratio of the (impurity/protein) ratios in crystal and in solution is a measure of trapping. For acetylated lysoyzme, K = 2.15 or, 3.42 for differently acetylated forms, is independent of both the impurity and the crystallizing protein concentration. The reason is that impurity flux to the surface is constant while the growth rate rises with supersaturation. About 3 times lower dimer concentration in space grown ferritin and lysozyme crystals might be examples explaining higher quality of the space grown protein crystal. Depletion of solution with respect to isomorphic impurities around a growing crystal may be K times deeper than with respect to the crystallizing protein.

Chernov, Alex A.↗

The MSP 2001 Mars Environmental Compatibility Assessment (MECA)

A chemical analysis of soil-water mixtures and the first microscopic images of martian soil will be among the results to be returned by the Mars Environmental Compatibility Assessment (MECA) payload on the Mars Surveyor Program 2001 Lander. Sponsored by the Human Exploration and Development of Space (HEDS) enterprise, MECA's primary goal is to evaluate potential geochemical and environmental hazards that may confront future martian explorers, and to guide HEDS scientists in the development of high fidelity Mars soil simulants. As a survey of soil properties, the MECA data set will also be rich in information relevant to basic geology, paleoclimate, and exobiology. The integrated MECA payload contains a wet-chemistry laboratory, a microscopy station, an electrometer to characterize the electrostatics of the soil and its environment, and arrays of material patches to study the abrasive and adhesive properties of soil grains. MECA is allocated a mass of 10 kg and a peak power usage of 15 W within an enclosure of 35 x 25 x 15 cm. The Wet Chemistry Laboratory (WCL) consists of four identical cells that will accept samples from surface and subsurface regions accessible to the Lander's robotic arm, mix them with water, and perform extensive analysis of the solution. Ion-selective electrodes and related sensors will evaluate total dissolved solids, redox potential, pH, and the concentration of many soluble ions and gases. Cyclic voltammetry will address oxidants, and anodic stripping voltammetry will probe potentially hazardous trace metals. MECA's microscopy station combines optical and atomic-force microscopy (AFM) in a controlled illumination environment to image dust and soil particles from millimeters to nanometers in size. Careful selection of substrates and an abrasion tool allows experimental study of size distribution, adhesion, abrasion, hardness, color, shape, aggregation, magnetic and other properties. Mounted on the end of the robot arm, MECA's electrometer consists of four types of sensors: an electric field meter, several triboelectricity monitors, an ion gauge, and a thermometer. Tempered only by ultra-violet- light-induced ions and a low-voltage break-down threshold, the dry, cold, dusty martian environment presents an imposing electrostatic hazard to both robots and humans. In addition, the electrostatic environment is key to transport of dust and, consequently, martian meteorology. MECA will also observe natural dust accumulation on engineering materials. Viewed with the robot arm camera, the abrasion and adhesion plates are strategically placed to allow direct observation of the inter-action between materials and soils on a macroscopic scale. Materials of graded hardness are placed directly under the robot arm scoop to sense wear and soil hardness. A second array, placed on the lander deck, is deployed after the dust plume of landing has settled. It can be manipulated in a primitive fashion by the arm, first having dirt deposited on it from the scoop and subsequently shaken clean. Dust accumulation as a function of conductivity, magnetic field strength, and other parameters will be explored. The MECA instruments described above will assess potential hazards that the Martian soil might present to human explorers and their equipment. In addition, MECA will provide information on the composition of ancient surface water environments, observing microscopic evidence of geological (and biological?) processes, inferring soil and dust transport, comminution and weathering mechanisms, and characterizing soil horizons that might be encountered during excavation. Additional information is contained in the original extended abstract.

Hecht, M. H.↗

The Mars Environmental Compatibility Assessment (MECA) Abrasion Tool

The Mars Environmental Compatibility Assessment (MECA) experiment, an instrument suite to be flown on Mars Surveyor 2001, will include a tool for doing simple mineralogical scratch and streak tests on particles from the Martian regolith. The Abrasion Tool will be applied to particles that adhere themselves to highly polished substrates of various hardnesses. Granular soil components will be subjected to a compressive force of about 3 N using a leaf spring. The spring will be applied with a paraffin actuator capable of a 0.76 mm throw to achieve a maximum displacement of about 7.5 mm at the tip of the tool. The pressure per grain will be dependent on the grain size, the number of grains that adhere to the substrate and the number of grains in compression. The pressure per particle is expected to be on the order of 100 MPa - 1 GPa. The MECA sample wheel containing the substrates will be rotated after the particles are placed in compression to produce scratches or pits. A primary goal of the Abrasion Tool is to identify quartz (Mohs' hardness = 7) using substrates of varying hardnesses. Quartz is considered hazardous to future human explorers of Mars because it can cause silicosis of the lungs if it is of respirable size. It is also hazardous to machinery, structures, and space suits because of its ability to abrade and scratch surfaces. Since large quantities of minerals harder than quartz are not expected, any scratches produced on polished quartz substrates might be reasonably attributed to quartz particles, although there may be minerals such as impact metamorphic diamond in the soils. Careful calibration of the tool will be necessary to ensure that grains are not overloaded; for example, a steel ball pressed into glass will produce a Hertzian fracture, even though it is softer than glass. Other minerals, such as magnetite (Mohs' hardness = 6.5) have been shown to scratch glass ceramics such as Zerodur (Mohs' hardness = 6.5). Thus, minerals can be differentiated: note that regardless of the mineral species, if any particle is harder than 6.5 it will certainly be an interesting discovery for both planetary geology and human exploration concerns. The scratches will be identified using the 6X optical microscope and profiled with the atomic force microscope included in the MECA instrument suite. Analysis of the scratch morphology will yield evidence concerning the shape of the particle responsible for producing each scratch. For example, angular grains should leave vertical cracks with microconchoidal lateral chipping, while rounded grains might leave chatter marks, or nested partial Hertzian cracks. Particle shape can thus be inferred from these indentation modes, as well as material hardness. In addition, particle size information may also be available if pits caused by rolling particles can be identified. Converse to scratching, the minerals may be crushed at their contact points, and be smeared onto the target substrates to leave what geologists refer to as "streaks". These are cold-welded trails of mineral material that have structure and color indicative of mineral composition. The AFM will determine the morphology of these streaks, while the microscope will ascertain the color. On the harder substrates, we might expect streaking to dominate; on the softer substrates, scratching may dominate. Progressions of material interactions across the substrate selection will be a valuable source of data for mineral discrimination. It should also be noted that many minerals have coatings (such as iron oxides), and these will have to be differentiated from the host mineral grains; laboratory tests will establish the effects of such coatings on the scratch results. Finally, we note that the microscope will provide corroborative data regarding likely mineral species by grain shapes, fracture patterns, surface textures, color, and UV fluorescence reactions. Additional information is contained in the original extended abstract.

Kuhlman, K. R.↗

Optical and Atomic Force Microscopy Characterization of PbI2 Quantum Dots

Lead iodide (PbI2) clusters were synthesized from the chemical reaction of NaI (or KI) with Pb(NO3)2 in H2O, D2O, CH3OH, and C3H7OH media. The observation of the absorption features above 350 nm with the help of integrating sphere accessory strongly suggests the quantum dot formation of PbI2 in solution. Spectral comparison between the synthesized PbI2 clusters in solution and PbI2 nanophase by impregnation of PbI2 in four different pore-sized porous silica indicates that the PbI2 cluster size in solution is less than 2.5 nm in lateral dimension. Atomic force microscopy (AFM) measurements show that the PbL clusters deposited onto three different molecularly flat surfaces are single-layered. The measured height is 1.0 - 0.1 nm. The swollen layer thickness can be attributed to the intralayer contraction from the strong lateral interaction among PbI2 molecules, which is supported by ab initio calculation. Raman scattering measurement of LO and TO modes of PbI2 in bulk and in the confined state were also conducted in 50-150 cu cm region. The observed three bands at 74, %, 106 1/cm are assigned to TO2, LO2, and LO, mode, respectively. The relatively small red-shift in LO modes may be caused by the surface phonon polaritons of PbI2 nanophase in the porous silica.

Mu, R.↗

Au Colloids Formed by Ion Implantation in Muscovite Mica Studied by Vibrational and Electronic Spectroscopes and Atomic Force Microscopy

Au was implanted into the (001) surface of Muscovite mica at an energy of 1.1 MeV and at doses of 1, 3, 6, and 10 x 10(exp 16) ions/cu cm. Optical spectra of the as-implanted samples revealed a peak at 2.28 eV (545 nm) which is attributed to the surface plasmon absorption of Au colloids. The infrared reflectance measurements show a decreasing reflectivity with increasing ion dose in the Si-O stretching region (900-1200 /cm). A new peak observed at 967 /cm increases with the ion dose and is assigned to an Si-O dangling bond. Atomic force microscopy images of freshly cleaved samples implanted with 6 and 10 x 10(exp 16) ions/sq cm indicated metal colloids with diameters between 0.9- 1.5 nm. AFM images of the annealed samples showed irregularly shaped structures with a topology that results from the fusion of smaller colloids.

Tung, Y. S.↗

Saskatchewan Forest Fire Control Centre Surface Meteorological Data

The Saskatchewan Forest Fire Control Centre (SFFCC) provided surface meteorological data to BOREAS from its archive. This data set contains hourly surface meteorological data from 18 of the Meteorological stations located across Saskatchewan. Included in these data are parameters of date, time, temperature, relative humidity, wind direction, wind speed, and precipitation. Temporally, the data cover the period of May through September of 1994 and 1995. The data are provided in comma-delimited ASCII files, and are classified as AFM-Staff data. The data files are available on a CD-ROM (see document number 20010000884), or from the Oak Ridge National Laboratory (ORNL) Distributed Active Archive Center (DAAC).

Hall, Forrest G.↗

BOREAS AES Five-Day Averaged Surface Meteorological and Upper Air Data

The Canadian Atmospheric Environment Service (AES) provided BOREAS with hourly and daily surface meteorological data from 23 of the AES meteorological stations located across Canada and upper air data from 1 station at The Pas, Manitoba. Due to copyright restrictions on the full resolution surface meteorological data, this data set contains 5-day average values for the surface parameters. The upper air data are provided in their full resolution form. The 5-day averaging was performed in order to create a data set that could be publicly distributed at no cost. Temporally, the surface meteorological data cover the period of January 1975 to December 1996 and the upper air data cover the period of January 1961 to November 1996. The data are provided in tabular ASCII files, and are classified as AFM-staff data. The data files are available on a CD-ROM (see document number 20010000884), or from the Oak Ridge National Laboratory (ORNL) Distributed Active Archive Center (DAAC).

Hall, Forrest G.↗

Atomic Force Microscope for Imaging and Spectroscopy

We have developed, built, and tested an atomic force microscope (AFM) for extraterrestrial applications incorporating a micromachined tip array to allow for probe replacement. It is part of a microscopy station originally intended for NASA's 2001 Mars lander to identify the size, distribution, and shape of Martian dust and soil particles. As well as imaging topographically down to nanometer resolution, this instrument can be used to reveal chemical information and perform infrared and Raman spectroscopy at unprecedented resolution.

Pike, W. T.↗

BOREAS Derived Surface Meteorological Data

In 1995, the BOREAS science teams identified the need for a continuous surface meteorological and radiation data set to support flux and surface process modeling efforts. This data set contains actual, substituted, and interpolated 15-minute meteorological and radiation data compiled from several surface measurements sites over the BOREAS SSA and NSA. Temporally, the data cover 01-Jan-1994 to 31-Dec-1996. The data are stored in tabular ASCII files, and are classified as AFM-Staff data.

Hall, Forrest G.↗

BOREAS AES MARSII Surface Meteorological Data

Canadian AES personnel collected several data sets related to surface and atmospheric meteorological conditions over the BOREAS region. This data set contains 15-minute meteorological data from six MARSII meteorology stations in the BOREAS region in Canada. Parameters include site, time, temperature, dewpoint, visibility, wind speed, wind gust, wind direction, two cloud groups, precipitation, and station pressure. Temporally, the data cover the period of May to September 1994. Geo-graphically, the stations are spread across the provinces of Saskatchewan and Manitoba. The data are provided in tabular ASCII files, and are classified as AFM-Staff data.

Atkinson, G. Barrie↗

BOREAS AES READAC Surface Meteorological Data

Canadian AES personnel collected and processed data related to surface atmospheric meteorological conditions over the BOREAS region. This data set contains 15-minute meteorological data from one READAC meteorology station in Hudson Bay, Saskatchewan. Parameters include day, time, type of report, sky condition, visibility, mean sea level pressure, temperature, dewpoint, wind, altimeter, opacity, minimum and maximum visibility, station pressure, minimum and maximum air temperature, a wind group, precipitation, and precipitation in the last hour. The data were collected non-continuously from 24-May-1994 to 20-Sep-1994. The data are provided in tabular ASCII files, and are classified as AFM-Staff data.

Atkinson, G. Barrie↗

BOREAS AES Campbell Scientific Surface Meteorological Data

Canadian AES personnel collected data related to surface and atmospheric meteorological conditions over the BOREAS region. This data set contains 15-minute meteorological data from 14 automated meteorology stations located across the BOREAS region. Included in this data are parameters of date, time, mean sea level pressure, station pressure, temperature, dew point, wind speed, resultant wind speed, resultant wind direction, peak wind, precipitation, maximum temperature in the last hour, minimum temperature in the last hour, pressure tendency, liquid precipitation in the last hour, relative humidity, precipitation from a weighing gauge, and snow depth. Temporally, the data cover the period of August 1993 to December 1996. The data are provided in tabular ASCII files, and are classified as AFM-Staff data.

Atkinson, G. Barrie↗

Inexpensive Method for Growing Unidirectional Oriented Materials Using Friction-Transferred Poly(tetrafluoroethylene) Substrates

In recent years, there has been an increasing interest in properties of unidirectional materials grown on highly oriented polymer surfaces such as the poly(tetrafluoroethylene) (PTFE) films coated onto smooth glass surfaces. In this technique, a thin PTFE film is deposited by sliding or rubbing a Teflon bar over a heated glass surface at a specific temperature. Depending on the pressure, temperature and sliding rate the thickness of deposited layers can be varied from 30 A to 150 A. The PTFE-coated substrate is simple yet surprising versatile for oriented growth of many organic, inorganic and polymer. The significant aspect of PTFE films is their unusual ability to molecularly align a wide variety of materials grown onto them from solution, melt or vapor phase deposition, at temperature below the melting point of PTFE (approx. 340 C). The PTFE structure may be derived, in part, from the multitude of ridges forming in the film and these ridges can presumably provide effective nucleation sites to induce the unidirectional growth of variety of materials. Electron diffraction studies of these films revealed that the PTFE macromolecules are oriented parallel to each other along the sliding direction. Direct observation of the film thickness, molecular structure and individual fluorine atoms from these highly oriented films were achieved using atomic force microscopy (AFM). In this paper, we also report the first direct observation of individual fluorine atoms, and the measurement of the fluorine-helix and carbon-helix radii to be 1.70 A and 0.54 A, respectively.

Lee, Jonathan A.↗

Australian Red Dune Sand: A Potential Martian Regolith Analog

To demonstrate the potential scientific and technical merits of in situ microscopy on Mars, we analyzed a possible Martian regolith analog - an acolian red dune sand from the central Australian desert (near Mt. Olga). This sand was chosen for its ubiquitous red coating and the desert environment in which is it found. Grains of this sand were analyzed using a variety of microanalytical techniques. A database of detailed studies of such terrestrial analogs would assist the study of geological and astrobiological specimens in future missions to Mars. Potential instrument concepts for in situ deployment on Mars include local electrode atom probe nanoanalysis (LEAP), vertical scanning white light interferometry (VSWLI), scanning electron microscopies, energy dispersive x-ray microanalysis (EDX), atomic force microscopy (AFM) and X-ray diffraction (XRD). While in situ deployment of these techniques is many years away, ground-based studies using these analytical techniques extend our understanding of the data obtained from instruments to be flown in the near future.

Kuhlman, K. R.↗

A Model for Macromolecular Crystallization

Macromolecular crystallization is a complex process. involving a system which typically has 5 or more components (macromolecule, water, buffer + counter ion, and precipitant). Whereas small molecules have only several well defined 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 often be readily broken and reformed between other sites. Formation of a consistent, ordered, 3D structure may be 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. Experimental evidence, based upon face growth rate, AFM, and fluorescence energy transfer data, for a postulated model of the nucleation of tetragonal lysozyme crystals and how it transitions into crystal growth will be presented.

Pusey, Marc L.↗

Vacuum Ultraviolet Radiation and Atomic Oxygen Durability Evaluation of HST Bi-Stem Thermal Shield Materials

Bellows-type thermal shields were used on the bi-stems of replacement solar arrays installed on the Hubble Space Telescope (HST) during the first HST servicing mission (SMI) in December 1993. These thermal shields helped reduce the problem of thermal gradient- induced jitter observed with the original HST solar arrays during orbital thermal cycling and have been in use on HST for eight years. This paper describes ground testing of the candidate solar array bi-stem thermal shield materials including backside aluminized Teflon(R)FEP (fluorinated ethylene propylene) with and without atomic oxygen (AO) and ultraviolet radiation protective surface coatings for durability to AO and combined AO and vacuum ultraviolet (VOV) radiation. NASA Glenn Research Center (GRC) conducted VUV and AO exposures of samples of candidate thermal shield materials at HST operational temperatures and pre- and post-exposure analyses as part of an overall program coordinated by NASA Goddard Space Flight Center (GSFC) to determine the on-orbit durability of these materials. Coating adhesion problems were observed for samples having the AO- and combined AO/UV-protective coatings. Coating lamination occurred with rapid thermal cycling testing which simulated orbital thermal cycling. This lack of adhesion caused production of coating flakes from the material that would have posed a serious risk to HST optics if the coated materials were used for the bi-stem thermal shields. No serious degradation was observed for the uncoated aluminized Teflon(R) as evaluated by optical microscopy, although atomic force microscopy (AFM) microhardness testing revealed that an embrittled surface layer formed on the uncoated Teflon(R) surface due to vacuum ultraviolet radiation exposure. This embrittled layer was not completely removed by AO erosion, No cracks or particle flakes were produced for the embrittled uncoated material upon exposure to VUV and AO at operational temperatures to an equivalent exposure of approximately five years in the HST environment. Uncoated aluminized FEP Teflon(R) was determined to be the most appropriate thermal shield material and was used on the bi-stems of replacement solar arrays installed on HST during SMI in December 1993. The SMI -installed solar arrays air scheduled to be replaced during MST's fourth servicing mission (SM3B) in early 2002.

Dever, Joyce↗