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NASA NTRS1999

Analyses of Contaminated Solar Array Handrail Samples Retrieved from Mir

In January 1998 during, the STS-89 mission, an eight section Russian solar array panel was retrieved after more than ten years exposure to the orbital space environment on the Russian space station Mir. Two darkened handrail samples from the Russian solar array have been evaluated for contamination: a section of a white paint covered rigid handrail and a section of woven fabric over-wrapped around a flexible handhold. The handrail samples were evaluated using optical microscopy (OM), field emission scanning electron microscopy (FESEM) and energy dispersive spectroscopy (EDS). Optical properties were also obtained. Microscopy has shown the discolored areas to have thick layers of contaminant that has crazed and spalled off in regions. Energy dispersive spectroscopy revealed that the brown contaminant is composed of oxidized silicon. No silicon was present on the unexposed fabric over-wrap, and very small amounts were present in the white paint. Therefore, the contaminant layer on both samples is attributed to silicone contamination from other spacecraft materials that have been oxidized by atomic oxygen while in orbit. A significant source of the silicone contamination appears to be from the solar array itself.

deGroh, Kim K.↗
NASA NTRS1999

Characterization of In-Situ BN Interface Formed by Nitridation of Nextel 312

Treatment of Nextel (TM) 312 in a reactive environment has been used as a low cost approach to the formation of BN on the fiber surface. Although the BN enriched surface region is extremely thin (less than 40 run), it is effective in providing debonding and composite behavior. Variation in mechanical behavior of Nextel (TM) 312/BN/Blackglas (TM) composites has been noted among panels fabricated with AF-10 cloth treated in different nitridation runs, Understanding this variation became the rationale for undertaking a detailed characterization of the nitrided fiber using field emission scanning electron microscopy, low voltage energy dispersive x-ray and Auger electron spectroscopy. Chemical composition and surface morphology are discussed in relation to observed mechanical behavior of NeXtel (TM) 312/Blackglas (TM) composites tested in bending.

Hurwitz, Fances I.↗
NASA NTRS1992

Black Carbon (Soot) Aerosol in the Lower Stratosphere and Upper Troposphere

We have used two approaches to measure BCA in the stratosphere. The first method consists of collecting aerosols by impaction on quartz rods, upon which are mounted strips of polystyrene filter material. Each 25 mm by 0.5 mm filter strip is alternately masked and exposed in 5 mm long sections. After sampling, the optical density of the exposed sections is measured and compared with the optical density of the masked (unexposed) sections. The filter strip is a Lambertian collector, the scattering property of which is not affected by the deposition of liquid sulfuric acid droplets which dominate the stratospheric aerosol. Hence, all attenuation greater in the exposed than in the non-exposed sections is due to absorption by BCA or rare opaque materials such as meteoritic iron. In a second approach we expose carbon-coated gold or palladium wires to air outside the aircraft boundary layer [Farlow et al., 1979; Pueschel et al., 1989]. With a field emission scanning electron microscope we are able to characterize BCA particles in addition to the dominant sulfuric acid droplets. Typically, soot is comprised of 20 nm diameter spheres linked together as branching chains or loosely packed aggregates (Figure 1a). The microscope has a lateral image resolution of 1.5 nm and can clearly resolve individual spheres making up BCA aggregates. Their morphology is uniquely different from that of the liquid sulfuric acid-water aerosol (Figure 1b). We approximate the size of each BCA particle by that of a sphere of equivalent volume and fit a lognormal size distribution to both the BCA and H2SO4/H2O aerosols. Both sampler types have been mounted on NASA's ER-2 high-altitude research aircraft (altitude ceiling of 70,000 feet), and on NASA's DC-8 (40,000 feet ceiling) aircraft to sample aerosols from a significant portion of the atmosphere.

Pueschel, R. F.↗
NASA NTRS2000

New Data on Microfossils from Shungites

Shungites are pre-cambrian (2Gya) carbon-rich, silicate rocks known from deposits in the north-western part of lake Onega, near the city of Petrozavodsk in Karelia (North from St. Petersburg, Russia). Shungites are extremely rich in carbon, with carbon accounting for 98% in vein shungites. Shungites have been found to exhibit interesting optical, ultrasonic, thermal, mechanical, electrical properties and have recently been found to contain small amounts of C60 fullerene. Shungite rocks from Karelia have a characteristic globular structure and are chemically inert and metastable. As part of our ongoing search for biomarkers in ancient terrestrial rocks that are of potential significance to Astrobiology, we have conducted Environmental and Field Emission Scanning Electron Micrographs of freshly fractured interior surfaces of Shungites. We find them to contain indigenous miocrofossils, similar to cyanobacteria known from the phosphorites of Khubsugul, Mongolia. We describe this investigation and provide ESEM and FESEM images of biomorphic microstructures that we interpret as indigenous microfossils in Shungites.

Hoover, Robert B.↗
NASA NTRS2001

Progress on BN and Doped-BN Coatings on Woven Fabrics

A novel, multistep process for applying interface coatings to woven structures using a pulsed CVD process is being evaluated. Borazine (B3N3H6), a neat liquid, and several Si precursors are used in the process to produce BN and SiBN coatings on Hi- Nicalon fabrics and preforms. A three variable, two level, full factorial matrix is proposed to define the influence of processing parameters. Coating morphology, uniformity and chemistry are characterized by field emission scanning electron microscopy (FESEM), energy dispersive (EDS) and Auger spectroscopies.

Hurwitz, Frances I.↗
NASA NTRS2001

Abiotic Versus Biotic Weathering Of Olivine As Possible Biosignatures

We are investigating the weathering of silicate minerals by both purely inorganic, and biologically mediated processes using field-emission scanning electron microscopy (FESEM) and energy dispersive x-ray spectroscopy (EDS). By resolving surface textures and chemical compositions of weathered surfaces at the sub-micron scale we hope to be able to distinguish abiotic from biotic weathering processes and so establish a new biosignature applicable to the study of astromaterials including but not limited to the Martian meteorites. Sterilized olivine grains (San Carlos, Arizona) no more than 1-2 mm in their longest dimension were optically assayed to be uniform in color and free of inclusions were selected as weathering subjects. Prior to all experiments surface morphologies and Fe/Mg ratios were determined for each grain using FE-SEM and EDS. Experiments were divided into two categories abiotic and biotic and were compared with "naturally" weathered samples. For the preliminary experiments, two trials (open and closed to the ambient laboratory environment) were performed under abiotic conditions, and three trials under biotic conditions (control, day 1 and day 2). The open system abiotic trials used sterile grains heated at 98 C and 200 C for both 24 and 48 hours in 1L double distilled de-ionized water. The closed system abiotic trials were conducted under the same conditions but in a sealed two layer steel/Teflon "bomb" apparatus. The biotic trials used sterile grains mounted in a flow-through device attached to a wellhead on the Columbia River aquifer. Several discolored, altered, grains were selected to document "natural" weathering surface textures for comparison with the experimental samples. Preliminary results indicate there are qualitative differences in weathered surface textures among all the designed experiments. The olivine grains in abiotic trials displayed etching, pitting, denticulate margins, dissolution and clay formation. The scale of the features ranged from tens to a few microns with textures that remained relatively sharp and were crystallographically controlled. These results were comparable to that observed in the "naturally" weathered comparison/reference grains. Chemical analysis by EDS indicates these textures correlated with the relative loss of Mg and Fe cations by diffusional processes. In contrast the biotic results indicated changes in the etching patterns on the scale of hundreds of nm, which are neither sharp nor crystallographically controlled (nanoetching). Organisms, organic debris and/or extracellular polymeric substances (biofilm) were often in close proximity or direct contact with the nanoetching. While there are many poorly constrained variables in natural weathering experiments to contend with, such as the time scale, the chemistry of the fluids and degree of biologic participation, some preliminary observations can be made: (1) certain distinct surface textures appear correlated with the specific processes giving rise to these textures; (2) the process of diffusing cations can produce many similar styles of surface textural changes; and (3) the main difference between abiotic and biotically produced weathering is the scale (microns versus nanometers) and the style (crystallographically versus noncrystallographically controlled) of the textural features. Further investigation into nanosize scale surface textures should attempt to quantify both textures and chemical changes of the role of microorganisms in the weathering of silicates. Additional experiments addressing nanoscale textures of shock features for comparison with the current data set.

Longazo, Teresa G.↗
NASA NTRS2002

C-Coupon Studies of SiC/SiC Composites: Microstructual Characterization - Part 2

A 'C-coupon' was used to measure the interlaminar tensile behavior of five different composite materials: Sylramic/MI (melt infiltration SiC matrix), ZMl/MI, Sylramic/S300, and ZMI and Hi-Nicalon with an S200 matrix at room temperature, 816 C, and 1204 C. Fracture behavior was characterized by field emission scanning electron microscopy, and observed cracking compared with events measured by modal acoustic emission. Both radial and matrix hoop cracking along the inner radius arising from hoop stresses were observed for all material types. In those composites in which the radial cracks were sufficiently wide to view the composite interior, fracture was observed to occur at the fiber BN or BN matrix interface.

Hurwitz, Frances I.↗
NASA NTRS1995

Soot Aerosol In The Atmosphere: Pole-to-Pole Distribution And Contributions by Aircraft

Interest in the distribution of black carbon (soot) aerosol (BCA) in the atmosphere is warranted for the following reasons: (1) BCA has the highest absorption cross section of any compound known, thus it can absorb solar radiation to cause atmospheric warming; (2) BCA is a strong adsorber of gases, thus it can catalyze heterogeneous chemical reactions to modify the chemical composition of the atmosphere; (3) If aircraft emission is the major source of atmospheric BCA, it can serve as an atmospheric tracer of aircraft exhaust. We collect BCA particles greater than or equal to 0.02 micrometer diameter by wires mounted on both the DC-8 and ER-2 aircraft. After return to the laboratory, the wires are examined with a field emission scanning electron microscope to identify BCA particles by their characteristic morphology. Typically, BCA exists in the atmosphere as small particles of complex morphology. The particle sizes at the source are measured in tens of Angstrom units; after a short residence time in the atmosphere, individual particles coalesce to loosely packed agglomerates of typical dimensions 0.01 to 0.1 micrometer. We approximate the size of each BCA aggregate by that of a sphere of equivalent volume. This is done by computing the volume of a sphere whose diameter is the mean between averaged minimum and maximum dimensions of the BCA particle. While this procedure probably underestimates the actual surface area, it permits us to compare BCA size distributions among themselves and with other types of aerosols. When statistically justified, we fit lognormal distributions to the data points to determine number concentrations, geometric mean radii, standard deviations, BCA surface areas and volumes. Results to date permit the following conclusions: (1) BCA concentration in the northern stratosphere averages 0.6 ng per cubic meters. This amount is one part in 10(exp 4) after a volcanic eruption (e.g., Pinatubo) increasing to about one percent during volcanic quiescence. In the northern troposphere, BCA concentration averages 3.2 ng per cubic meters, or 0.3 percent of the background aerosol. (2) Applying an BCA emission index EI(BCA)=5 x 10(exp -5), measured in the exhaust wake of a Concorde supersonic jet aircraft, to realistic estimates of fuel burnt by the current and projected fleets permits us to conclude that: (i) Most BCA in the northern stratosphere results from aircraft emissions; (ii) Most BCA in the northern troposphere results from other sources than aircraft; (iii) A projected supersonic fleet will increase the northern stratospheric BCA concentration by one order of magnitude, unless the emission index is substantially reduced. (3) A strong gradient between the northern and southern hemispheres indicates that mixing across the equator is greatly inhibited in relation to atmospheric residence times of BCA. (4) The single scatter albedo of BCA/"background" aerosol mixtures suggests a cooling effect for most of the globe; an exemption is the Arctic because of the high surface albedo of the snow/ice covered earth's surface.

Pueschel, R. F.↗
NASA NTRS1995

Soot Aerosols in the Atmosphere: Contributions by Aircraft

Interest in the distribution of black carbon (soot) aerosol (BCA) in the atmosphere is based on the following: (1) Because BCA has the highest absorption cross section of any compound know, it can absorb solar radiation to cause atmospheric warming; (2) Because BCA is a strong adsorber of gases, it can catalyze heterogeneous chemical reactions to modify the chemical composition of the atmosphere; (3) If aircraft emission is the major source of BCA, it can serve as an atmospheric tracer of aircraft exhaust. We collect BCA particles as small as 0.02 micrometers by wires mounted on both the DC-8 and ER-2 aircraft. After return to the laboratory, the wires are examined with a field emission scanning electron microscope to identify BCA particles by their characteristics morphology, Typically, BCA exists in the atmosphere as small particles of complex morphology. The particle sizes at the source are measured in tens of Angstrom units; after a short residence time in the atmosphere, individual particles coalesce to loosely packed agglomerates of typical dimensions 0.01 to 0.1 micrometer. We approximate the size of each BCA aggregate by that of a sphere of equivalent volume. This is done by computing the volume of a sphere whose diameter is the mean between averaged minimum and maximum dimensions of the BCA particle. While this procedure probably underestimates the actual surface area, it permits us to compare BCA size distributions among themselves and with other types of aerosols.

Pueschel, R. F.↗
NASA NTRS2002

Bn and Si-Doped Bn Coatings on Woven Fabrics

A computer controlled, pulsed chemical vapor infiltration (CVI) system has been developed to deposit BN from a liquid borazine (B3N3H6) source, as well as silicon doped BN coatings using borazine and a silicon source, into 2-D woven ceramic fabric preforms. The coating process was evaluated as a function of deposition temperature, pressure, and precursor flow rate. Coatings were characterized by field emission scanning electron microscopy, electron dispersive spectroscopy and Auger spectroscopy. By controlling the reactant feed ratios, Si incorporation could be controlled over the range of 6-24 atomic percent.

Hurwitz, Frances I.↗
NASA NTRS2003

Pristine Presolar Silicon Carbide

In this talk we discuss a simple physical disaggregation technique coupled with an X-ray mapping procedure used to locate 81 micrometer-sized presolar SiC grains from the Murchison carbonaceous chondrite, that preserves them in their pristine state. We then describe pristine SiC surface characteristics and overall morphologies determined by high resolution field emission scanning electron microscopy (FESEM), and compare these features to those of presolar SiC grains that have been prepared using chemical dissolution techniques.

Bernatowicz, T. J.↗
NASA NTRS1961

An Experimental Study of Continuous Plasma Flows Driven by a Confined Arc in a Transverse Magnetic Field

A crossed-field, continuous-flow plasma accelerator has been built and operated. The highest measured velocity of the flow, which was driven by the interaction of the electric and magnetic fields, was about 500 meters per second. Some of the problems discussed are ion slip, stability and uniformity of the discharge, effect of the magnetic field on electron emission, use of preionization, and electrode contamination.

Barger, R. L.↗
NASA NTRS1999

A Mossbauer investigation of iron-rich terrestrial hydrothermal vent systems: lessons for Mars exploration

Hydrothermal spring systems may well have been present on early Mars and could have served as a habitat for primitive life. The integrated instrument suite of the Athena Rover has, as a component on the robotic arm, a Mossbauer spectrometer. In the context of future Mars exploration we present results of Mossbauer analysis of a suite of samples from an iron-rich thermal spring in the Chocolate Pots area of Yellowstone National Park (YNP) and from Obsidian Pool (YNP) and Manitou Springs, Colorado. We have found that Mossbauer spectroscopy can discriminate among the iron-bearing minerals in our samples. Those near the vent and on the surface are identified as ferrihydrite, an amorphous ferric mineraloid. Subsurface samples, collected from cores, which are likely to have undergone inorganic and/or biologically mediated alteration (diagenesis), exhibit spectral signatures that include nontronite (a smectite clay), hematite (alpha-Fe2O3), small-particle/nanophase goethite (alpha-FeOOH), and siderite (FeCO3). We find for iron minerals that Mossbauer spectroscopy is at least as efficient in identification as X-ray diffraction. This observation is important from an exploration standpoint. As a planetary surface instrument, Mossbauer spectroscopy can yield high-quality spectral data without sample preparation (backscatter mode). We have also used field emission scanning electron microscopy (FESEM), in conjunction with energy-dispersive X ray (EDX) fluorescence spectroscopy, to characterize the microbiological component of surface sinters and the relation between the microbiological and the mineralogical framework. Evidence is presented that the minerals found in these deposits can have multi-billion-year residence times and thus may have survived their possible production in a putative early Martian hot spring up to the present day. Examples include the nanophase property and the Mossbauer signature for siderite, which has been identified in a 2.09-billion-year old hematite-rich chert stromatolite. Our research demonstrates that in situ Mossbauer spectroscopy can help determine whether hydrothermal mineral deposits exist on Mars, which is significant for exobiology because of the issue of whether that world ever had conditions conductive to the origin of life. As a useful tool for selection of samples suitable for transport to Earth, Mossbauer spectroscopy will not only serve geological interests but will also have potential for exopaleontology.

NASA Discipline Exobiology↗
NASA NTRS2003

Oxidation of ZrB2-and HfB2-Based Ultra-High Temperature Ceramics: Effects of Ta Additions

Several compositions of ZrB2- and HfB2-based Ultra-High Temperature Ceramics (UHTC) were oxidized in stagnant air at 1627 C in ten minute cycles for times up to 100 minutes. These compositions include: ZrB2 - 20v% SiC, HfB2 - 20v% SiC, ZrB2 - 20v% SiC - 20v% TaSi2, ZrB2 - 33v% SiC, HfB2 - 20v% SiC - 20v% TaSi2, and ZrB2 - 20v% SiC - 20v% TaC. The weight change due to oxidation was recorded. The ZrB2 - 20v% SiC - 20v% TaSi2 composition was also oxidized in stagnant air at 1927 C and in an arc jet atmosphere. Samples were analyzed after oxidation by x-ray diffraction, field emission scanning electron microscopy, and energy dispersive spectroscopy to determine the reaction products and to observe the microstructure. The ZrB2 - 20v% SiC - 20v% TaSi2 showed the lowest oxidation rate at 1627 C, but performed poorly under the more extreme tests due to liquid phase formation. Effects of Ta-additions on the oxidation of the diboride-based UHTC are discussed.

Opila, Elizabeth↗
NASA NTRS2004

Oxidation of High-temperature Alloy Wires in Dry Oxygen and Water Vapor

Small diameter wires (150 to 250 microns) of the high temperature alloys Haynes 188, Haynes 230, Haynes 230, Haynes 214, Kanthal Al and PM2000 were oxidized at 1204 C in dry oxygen or 50% H2O /50% O2 for 70 Hours. The oxidation kinetics were monitored using a thermogravimetric technique. Oxide phase composition and morphology of the oxidized wires were determined by X-ray diffraction,field emission scanning electron microscopy, and energy dispersive spectroscopy. The alumina-forming alloys, Kanthal Al and PM2000, out-performed the chromia-forming alloys under this conditions. PM2000 was recommended as the most promising candidate for advanced hybrid seal applications for space reentry control surface seals or hypersonic propulsion system seals. This study also demonstrated that thermogravimetric analysis of small diameter wires is a powerful technique for the study of oxide volatility, oxide adherence, and breakaway oxidation.

Opila, Elizabeth J.↗
NASA NTRS2005

NSTAR Extended Life Test Discharge Chamber Flake Analysis

The Extended Life Test (ELT) of the NASA Solar Electric Propulsion Technology Readiness (NSTAR) ion thruster was concluded after 30,352 hours of operation. The ELT was conducted using the Deep Space 1 (DS1) back-up flight engine, a 30 cm diameter xenon ion thruster. Post-test inspection of the ELT engine revealed numerous contaminant flakes distributed over the bottom of the cylindrical section of the anode within the discharge chamber (DC). Extensive analyses were conducted to determine the source of the particles, which is critical to the understanding of degradation mechanisms of long life ion thruster operation. Analyses included: optical microscopy (OM) and particle length histograms, field emission scanning electron microscopy (FESEM) combined with energy dispersive spectroscopy (EDS), and atomic oxygen plasma exposure tests. Analyses of the particles indicate that the majority of the DC flakes consist of a layered structure, typically with either two or three layers. The flakes comprising two layers were typically found to have a molybdenum-rich (Mo-rich) layer on one side and a carbon-rich (C-rich) layer on the other side. The flakes comprising three layers were found to be sandwich-like structures with Mo-rich exterior layers and a C-rich interior layer. The presence of the C-rich layers indicates that these particles were produced by sputter deposition build-up on a surface external to the discharge chamber from ion sputter erosion of the graphite target in the test chamber. This contaminant layer became thick enough that particles spalled off, and then were electro-statically attracted into the ion thruster interior, where they were coated with Mo from internal sputter erosion of the screen grid and cathode components. Atomic oxygen tests provided evidence that the DC chamber flakes are composed of a significant fraction of carbon. Particle size histograms further indicated that the source of the particles was spalling of carbon flakes from downstream surfaces. Analyses of flakes taken from the downstream surface of the accelerator grid provided additional supportive information. The production of the downstream carbon flakes, and hence the potential problems associated with the flake particles in the ELT ion thruster engine is a facility induced effect and would not occur in the space environment.

deGroh, Kim K.↗
NASA NTRS2000

Very Long Term Oxidation of Titanium Aluminides Investigated

Titanium aluminides (TiAl) are of great interest for intermediate-temperature (600 to 850 C) aerospace and power-generation applications because they offer significant weight savings over today's nickel alloys. TiAl alloys are being investigated for low-pressure turbine blade applications, exhaust nozzle components, and compressor cases in advanced subsonic and supersonic engines. Significant progress has been made in understanding the fundamental aspects of the oxidation behavior of binary TiAl alloys. However, most of this work has concentrated on short term (<1000 hr), high-temperature (900 to 1000 C) exposures. Also, there is not much data available in the literature regarding the oxidation behavior of the quaternary and higher order engineering alloys. This is especially true for the very long term, low-temperature conditions likely to be experienced during aerospace applications. An investigation at the NASA Glenn Research Center at Lewis Field was undertaken to characterize the long-term oxidation behavior of various model and advanced titanium aluminides for periods up to 7000 hr at 704 C in air using a high-resolution field emission scanning electron microscope. Also, a unique surface treatment technique developed to improve the oxidation resistance of TiAl was evaluated. The alloys included in this investigation are listed in the table. The table also shows typical alloy compositions and the specific weight changes and scale thickness measured for each alloy after exposure to 700 C for 7000 hr in air.

Locci, Ivan E.↗
NASA NTRS2000

Contaminated Solar Array Handrail Samples Retrieved From Mir Analyzed

In January 1998 during the shuttle STS 89 mission, an eight-section Russian solar array panel was retrieved after more than 10 years of exposure to the orbital space environment on Mir. The array was deployed June 16, 1987, and removed on November 3, 1997. It had been actively used as a source of electrical power for 8 years. This operational array had been located on the Mir core module, located directly above the Kvant-2 module. Its retrieval provided a unique opportunity to study the effects of the low-Earth-orbit environment on a functional solar array. The intact solar array underwent scientific inspections and preliminary tests by a joint team of U.S. and Russian investigators to evaluate the effects of long-term space exposure. Upon initial examination, significant contamination was observed over most components of the array. One panel, panel 8, was provided to the U.S. scientists for further evaluation. As part of the U.S. investigations, two solar array handrail samples from panel 8 were evaluated for contamination at the NASA Glenn Research Center at Lewis Field. One is a section of a rigid handrail, and the other is a section of woven fabric tape that was overwrapped around a flexible handhold. Both the flexible handhold woven fabric and the rigid handrail were significantly darkened after 10 years of space exposure. They were evaluated with optical microscopy, field emission scanning electron microscopy (FESEM), and energy-dispersive spectroscopy. Solar absorptance and room-temperature emittance values also were obtained. The returned contaminated solar array segment is very similar in design to the solar arrays being supplied by the Russians for the International Space Station. Therefore, it was desirable to determine what the contaminants on various surfaces are and what the sources of the contamination were.

deGroh, Kim K.↗