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NASA NTRSDate not supplied

Revisiting the Origin of Macromolecular Carbon (MMC) in Lunar Basalts 15556 & 10044

Volatile elements influence the geo-chemical evolution of planetary bodies and they are in magmas at every stage, from melting within planetary interiors to eruption at the surface. Analyses of lunar mare basalts supported the hypothesis that lunar mag-mas were depleted in volatiles (H-C-F-Cl-S), relative to their terrestrial analogs [1]. Nevertheless, several early studies of samples returned during the Apollo program proposed that the mare basalt eruptions, including the “fire fountain” eruptions, were propelled by the oxidation of magmatic graphite to CO (and/or CO2) gas [2, 3]. Seminal studies during the 1970’s measured the bulk concentration and isotopic compositions of C from Apollo 11 samples, and identified several carbonaceous compounds, including: (a) gaseous (CO, CO2, and traces of CH4), (b) metallic carbide, and (c) potentially elemental carbon [4-6]. These studies reported a relatively broad range of C contents (~100-400 μg/g) and isotopic values (δC13 = -30 to +20), and suggested that these heterogeneities can be explained by contribution from multiple factors, including: (a) indigenous carbon, (b) solar wind implantation, (c) bombardment and/or meteorite impact, and (d) terrestrial contamination [5,6]. However, unequivocal observations of magmatic graphite in lunar basalts have never been made. Macromolecular carbon (MMC)—graphitic carbon varying from nearly amorphous to highly crystalline varieties—was identified as inclusions hosted by igneous pyroxenes from Martian meteorites and were attributed to being indigenous to Mars [8]. The authors carefully considered the textural and mineralogical relationship of the MMC phases, and concluded that the subset of MMC located within and/or adjacent to cracks, or at a disrupted surface (e.g., cut) were most consistent with terrestrial contamination. The near absence of con-firmed instances of lunar magmatic MMC within the literature [9], combined with the wide range of isotopic values and bulk carbon contents measured in lunar bas-alts begs the question as to whether previously measured carbon is of an indigenous origin, or the result of terrestrial contamination. Using Raman spectroscopy, we have observed MMC in lunar basalts subjected to different forms of anthropogenic modification related to sample preparation including polished sections, sawn surfaces, and fractured surfaces adjacent to sawn sur-faces. We have observed MMC of unknown origin in all of these settings. Here we report the preliminary textural and spectroscopic characteristics of MMC hosted within the groundmass of Apollo 15 (15556) and Apollo 11 basalts (10044) as part of our ongoing investigation of the origin of these carbonaceous materials.

lunar↗
NASA NTRS2001

Performance of Li-Ion Cells Under Battery Voltage Charge Control

A study consisting of electrochemical characterization and Low-Earth-Orbit (LEO) cycling of Li-Ion cells from three vendors was initiated in 1999 to determine the cycling performance and to infuse the new technology in the future NASA missions. The 8-cell batteries included in this evaluation are prismatic cells manufactured by Mine Safety Appliances Company (MSA), cylindrical cells manufactured by SAFT and prismatic cells manufactured by Yardney Technical Products, Inc. (YTP). The three batteries were cycle tested in the LEO regime at 40% depth of discharge, and under a charge control technique that consists of battery voltage clamp with a current taper. The initial testing was conducted at 20 C; however, the batteries were cycled also intermittently at low temperatures. YTP 20 Ah cells consisted of mixed-oxide (Co and Ni) positive, graphitic carbon negative, LIPF6 salt mixed with organic carbonate solvents. The battery voltage clamp was 32 V. The low temperature cycling tests started after 4575 cycles at 20 C. The cells were not capable of cycling. at low temperature since the charge acceptance at battery level was poor. There was a cell in the battery that showed too high an end-of-charge (EOC) voltage thereby limiting the ability to charge the rest of the cells in the battery. The battery has completed 6714 cycles. SAFT 12 Ah cells consisted of mixed-oxide (Co and NO positive, graphitic carbon negative, LiPF6 salt mixed with organic carbonate solvents. The battery voltage clamp was for 30.8 V. The low temperature cycling tests started after 4594 cycles at 20 C. A cell that showed low end of discharge (EOD) and EOC voltages and three other cells that showed higher EOC voltages limited the charge acceptance at the selected voltage limit during charge. The cells were capable of cycling at 10 C and 0 C but the charge voltage limit had to be increased to 34.3 V (4.3 V per cell). The low temperature cycling may have induced poor chargeability since the voltage had to be increased to achieve the required charge input. The battery has completed 6226 cycles. MSA 10 Ah cells consisted of Co oxide positive, graphitic carbon negative, LiPF6 salt mixed with organic carbonate solvents. The battery voltage clamp was 30.8 V. The low temperature cycling tests were started after 2182 cycles at 20 C. The cells were capable of cycling at 10 C and 0 C. Like SAFT, the voltage limit on charge had to be increased to 36 V (4.5 V per cell). There was a cell (cell S/N 13) in the battery that showed poor performance features such as low EOD voltage and high EOC voltage. The battery has completed 3441 cycles. A reconditioning procedure that consisted of C15 charge to a taper current of C/100 and C/20 discharge improved the voltage behavior of SAFT and MSA cells with no significant effect on YTP cells. We have demonstrated that the charge operation with VT clamp at battery rather than at cell level is feasible for onboard Li-Ion battery operation.

Rao, Gopalakrishna M.↗
NASA NTRS1988

Thermo-oxidative stability studies of Celion 6000/PMR-15 unidirectional composites, PMR-15, and Celion 6000 fiber

Experimental results on the influence of the thermooxidative resistance characteristics of the fiber and matrix resin on the thermal stability of isothermally aged Celion 6000/PMR-15 matrix resin composites are presented. SEM studies reveal that extreme oxidative erosion of the graphite fiber occurs at elevated temperatures in the presence of the polyimide matrix. The activation energy of oxidation of the composite was shown to be greater than those of the fiber and the matrix resin.

Bowles, Kenneth J.↗
NASA NTRS2002

Carbon Nanostructure Examined by Lattice Fringe Analysis of High Resolution Transmission Electron Microscopy Images

The dimensions of graphitic layer planes directly affect the reactivity of soot towards oxidation and growth. Quantification of graphitic structure could be used to develop and test correlations between the soot nanostructure and its reactivity. Based upon transmission electron microscopy images, this paper provides a demonstration of the robustness of a fringe image analysis code for determining the level of graphitic structure within nanoscale carbon, i.e. soot. Results, in the form of histograms of graphitic layer plane lengths, are compared to their determination through Raman analysis.

VanderWal, Randy L.↗
NASA NTRS2003

Carbon Nanostructure Examined by Lattice Fringe Analysis of High Resolution Transmission Electron Microscopy Images

The dimensions of graphitic layer planes directly affect the reactivity of soot towards oxidation and growth. Quantification of graphitic structure could be used to develop and test correlations between the soot nanostructure and its reactivity. Based upon transmission electron microscopy images, this paper provides a demonstration of the robustness of a fringe image analysis code for determining the level of graphitic structure within nanoscale carbon, i.e., soot. Results, in the form of histograms of graphitic layer plane lengths, are compared to their determination through Raman analysis.

VanderWal, Randy L.↗
NASA NTRS1981

Research on graphite reinforced glass matrix composites

A broad group of fibers and matrices were combined to create a wide range of composite properties. Primary material fabrication procedures were developed which readily permit the fabrication of flat plate and shaped composites. Composite mechanical properties were measured under a wide range of test conditions. Tensile, flexure mechanical fatigue, thermal fatigue, fracture toughness, and fatigue crack growth resistance were evaluated. Selected fiber-matrix combinations were shown to maintain their strength at up to 1300 K when tested in an inert atmosphere. Composite high temperature mechanical properties were shown to be limited primarily by the oxidation resistance of the graphite fibers. Composite thermal dimensional stability was measured and found to be excellent.

Prewo, K. M.↗
NASA NTRS2003

Analysis of the Effect of Surface Modification on Polyimide Composites Coated with Erosion Resistant Materials

The aim of this research is to enhance performance of composite coatings through modification of graphite-reinforced polyimide composite surfaces prior to metal bond coat/ hard topcoat application for use in the erosive and/or oxidative environments of advanced engines. Graphite reinforced polyimide composites, PMR-15 and PMR-II-50, formed by sheet molding and pre-pregging will be surface treated, overlaid with a bond coat and then coated with WC-Co. The surface treatment will include cleaning, RF plasma or ultraviolet light- ozone etching, and deposition of SiO(x) groups. These surface treatments will be studied in order to investigate and improve adhesion and oxidation resistance. The following panels were provided by NASA-Glenn Research Center(NASA-GRC): Eight compression molded PMR-II-50; 6 x 6 x 0.125 in. Two vacuum-bagged PMR-II-50; 12 x 12 x 0.125 in. Eight compression molded PMR-15; 6 x 6 x 0.125 in. One vacuum-bagged PMR-15; 12 x 12 x 0.125 in. All panels were made using a 12 x 12 in. T650-35 8HS (3K-tow) graphite fabric. A diamond-wafering blade, with deionized water as a cutting fluid, was used to cut PMR-II-50 and PMR-15 panels into 1 x 1 in. pieces for surface tests. The panel edges exhibiting delamination were used for the preliminary surface preparation tests as these would be unsuitable for strength and erosion testing. PMR-15 neat resin samples were also provided by NASA GRC. Surface profiles of the as-received samples were determined using a Dektak III Surface profile measuring system. Two samples of compression molded PMR-II-50 and PMR-15, vacuum-bagged PMR-II-50 and PMR-15 were randomly chosen for surface profile measurement according to ANSI/ASME B46.1. Prior to each measurement, the samples were blasted with compressed air to remove any artifacts. Five 10 mm-long scans were made on each sample. The short and long wavelength cutoff filter values were set at 100 and 1000 m, diamond stylus radius was 12.5 microns. Table 1 is a summary of the arithmetic average roughness (Ra) and waviness (Wa) for the composite surfaces.

Ndalama, Tchinga↗
NASA NTRS1985

Metallic Foams

The formation of metallic foams by use of a blowing agent in the melt was investigated. It was attempted to produce a metallic foam by melting a mixture of Cu powder and graphite in a SPAR rocket. The graphite combines with the oxide on the copper to form Co and acts as a blowing agent. No foam was formed, and it could not be determined whether the foam fails to form, forms but was lost to surface tension instabilities, or is destroyed by incomplete solidification before reentry.

Pond, R. B.↗
NASA NTRS1985

Solid lubricant materials for high temperatures: A review

Solid lubricants that can be used above 300 C in air are discussed, including coatings and self-lubricating composite bearing materials. The lubricants considered are representative dichalcogenides, graphite, graphite fluoride, polyimides, soft oxides, oxidatively stable fluorides, and hard coating materials. A few general design considerations revelant to solid lubrication are interspersed.

Sliney, Harold E.↗
NASA NTRS1997

Characteristics of Interstellar and Circumstellar Dust

This paper will review our current knowledge of circumstellar and interstellar dust from an astronomical point of view. About half of the interstellar dust volume consists of amorphous silicates. The remainder has to be made up of an carbonaceous component such as graphite, amorphous carbon (i.e., soot), Polycyclic Aromatic Hydrocarbon molecules (PAHs), and/or organic grain mantles (i.e., mixed polymers). The observational evidence for these components will be reviewed and their relative importance assessed. The emphasis will be on recent observations using the Infrared Space Observatory. Most of these dust components are formed in the outflows from stars in the late stages of their evolution (i.e., red giants, planetary nebulae, novae, supergiants, Wolf Rayet stars, and supernovae). Indeed, observation of such objects indicate an even richer spectrum of stardust components, including also SiC, MgS, and aluminates and crystalline silicates. These observations will be briefly discussed. The stardust budget of the galaxy will be reviewed and the relative importance of the various birth sites assessed. Finally, in recent years, isotopic composition studies have shown that some circumstellar and interstellar dust grains have been incorporated into solar system bodies such as planetary dust particles and meteorites without totally losing their identity. Among the components identified are SiC, graphite, diamonds, PAHs, aluminum oxides, as well as various trace element carbides. Studies of this kind have opened up a new window on the composition and structure of interstellar dust. These different sources of information on interstellar and circumstellar dust will be briefly contrasted.

Tielens, A. G. G. M.↗
NASA NTRS1980

Research on graphite reinforced glass matrix composites

High levels of mechanical performance in tension, flexure, fatigue, and creep loading situations of graphite fiber reinforced glass matrix composites are discussed. At test temperatures of up to 813 K it was found that the major limiting factor was the oxidative instability of the reinforcing graphite fibers. Particular points to note include the following: (1) a wide variety of graphite fibers were found to be comparable with the glass matrix composite fabrication process; (2) choice of fiber, to a large extent, controlled resultant composite performance; (3) composite fatigue performance was found to be excellent at both 300 K and 703 K; (4) composite creep and stress rupture at temperatures of up to 813 K was limited by the oxidative stability of the fiber; (5) exceptionally low values of composite thermal expansion coefficient were attributable to the dimensional stability of both matrix and fiber; and (6) component fabricability was demonstrated through the hot pressing of hot sections and brazing using glass and metal joining phases.

Prewo, K. M.↗
NASA NTRS1973

Development of seal ring carbon-graphite materials (tasks 8, 9, and 10)

A screening study was conducted to develop improved carbon-graphite materials for use in self-acting seals at air temperatures to 1300 F (704 C). Property measurements on materials prepared during this study have shown that: (1) The mechanical properties of a carbon-graphite material were significantly improved by using a fine milled artificial graphite filler material and including intensive mixing, warm molding, and pitch impregnation in the processing; and (2) the oxidation resistance of a carbon-graphite material was improved by including fine milled boron carbide as an oxidation-inhibiting additive. These techniques were employed to develop a material that has 10 times more oxidation resistance than that of a widely used commercial grade and mechanical properties that approach those of the commercial grade.

Fechter, N. J.↗
NASA NTRS1999

Intercalation of Lithium in Pitch-Based Graphitized Carbon Fibers Chemically Modified by Fluorine: Soft Carbon With or Without an Oxide Surface

The effects of carbon structure and surface oxygen on the carbon's performance as the anode in lithium-ion battery were studied. Two carbon materials were used for the electrochemical tests: soft carbon made from defluorination of graphite fluoride, and the carbon precursor from which the graphite fluoride was made. In this research the precursor was graphitized carbon fiber P-100. It was first fluorinated to form CF(0.68), then defluorinated slowly at 350 to 450 C in bromoform, and finally heated in 1000 C nitrogen before exposed to room temperature air, producing disordered soft carbon having basic surface oxides. This process caused very little carbon loss. The electrochemical test involved cycles of lithium intercalation and deintercalation using C/saturated LiI-50/50 (vol %) EC and DMC/Li half cell. The cycling test had four major results. (1) The presence of a basic oxide surface may prevent solvent from entering the carbon structure and therefore prolong the carbon's cycle life for lithium intercalation-deintercalation. (2) The disordered soft carbon can store lithium through two different mechanisms. One of them is lithium intercalation. which gives the disordered carbon an electrochemical behavior similar to its more ordered graphitic precursor. The other is unknown in its chemistry, but is responsible for the high-N,oltage portion (less than 0.3V) of the charge-discharge curve. (3) Under certain conditions, the disordered carbon can store more lithium than its precursor. (4) These sample and its precursor can intercalate at 200 mA/g. and deintercalate at a rate of 2000 mA/g without significant capacity loss.

Hung, Ching-Chen↗
NASA NTRS1980

Coatings for Graphite Fibers

Several approaches for applying high resistance coatings continuously to graphite yarn were investigated. Two of the most promising approaches involved (1) chemically vapor depositing (CVD) SiC coatings on the surface of the fiber followed by oxidation, and (2) drawing the graphite yarn through an organo-silicone solution followed by heat treatments. In both methods, coated fibers were obtained which exhibited increased electrical resistances over untreated fibers and which were not degraded. This work was conducted in a previous program. In this program, the continuous CVD SiC coating process used on HTS fiber was extended to the coating of HMS, Celion 6000, Celion 12000 and T-300 graphite fiber. Electrical resistances three order of magnitude greater than the uncoated fiber were measured with no significant degradation of the fiber strength. Graphite fibers coated with CVD Si3N4 and BN had resistances greater than 10(exp 6) ohm/cm. Lower pyrolysis temperatures were used in preparing the silica-like coatings also resulting in resistances as high as three orders of magnitude higher than the uncoated fiber. The epoxy matrix composites prepared using these coated fibers had low shear strengths indicating that the coatings were weak.

Galasso, F. S.↗
NASA NTRS1991

A comparison of fiber effects on polymer matrix composite oxidation

A number of thermo-oxidative stability studies addressing the effects of fiber reinforcement on composite thermal stability and influence of geometry on the results of aging studies were performed at NASA-Lewis. The information presented herein, a compilation of some results from these studies, shows the influence of the reinforcement fibers on the oxidative degradation of various PMR-15 composites. Reinforcement of graphite and ceramics were studied and three composite oxidation mechanisms were observed. One was a dominant attack of the reinforcement fiber, the second was the aggressive oxidation of the matrix material, and the third was interfacial degradation.

Bowles, Kenneth J.↗
NASA NTRS1994

The abundant elements in interstellar dust

We explore the incorporation of the cosmically abundant species O, C, N, Mg, Si, Fe, and S into interstellar dust. Column densities based on Goddard High Resolution Spectrograph 3.5 km/s resolution measurements from the literature for eight individual absorbing regions toward five lines of sight are used. Corrections are applied as needed in order to account for recent improvements in oscillator strengths. In order to acquire the most accurate column densities, and check on the accuracy of the oscillator strengths, we compare column densities based on the very strong Lorentzian damped lines of C II, O I, N I, and Mg II with results for the weak lines of these species, and confirm the previously determined f-values for O I lambda 1335, C II lambda 2325, and N I lambda lambda 1159, 1160. New empirical f-values of 1.25 x 10(exp -3) and 6.25 x 10(exp -4), respectively, are derived for the Mg II weak doublet at 1239 and 1240 A. Assuming a cosmic reference abundance based on solar and B star values, we derive depletions and dust-phase abundances which suggest that more than 70% of the available Mg and Fe is incorporated into dust-grain cores, whereas only 35% of the silicon is. This implies that oxides are important constituents of the grain core population. Mg and Fe atoms are mantled onto grain cores in a ratio of 1.8 to 1, whereas approximately 4.0 Si atoms are in the mantle per Fe atom. Since Si is not expected to accrete onto silicate or graphite grains, other grain cores, perhaps oxides and/or metallic Fe, may provide mantling sites for this species. The abundances of Fe and Mg in mantles would imply that graphite grains must have a substantial coating unless oxides provide significant mantling sites for these species. The abundance of O and N in the dust phase as implied by the solar reference abundance values are difficult to reconcile with the fact that these elements are not expected to participate in mantle formation, and the 3.1 micrometer H2O ice feature is not seen in absorption toward stars similar to those studied. The B star reference abundances for O and N, however, imply that no mantling of these species has occurred. The dust-phase abundance for C implied by solar reference abundances agrees with predictions for the number of graphite grains needed to produce the 2175 A bump. B star reference abundances, however, suggest that the abundance of C in the dust phase is not always sufficient to produce the bump.

Sofia, Ulysses J.↗
NASA NTRS1980

Environmental effects on graphite fiber reinforced PMR-15 polyimide

Studies were conducted to establish the effects of thermo-oxidative and hydrothermal exposure on the mechanical properties of T300 graphite fabric reinforced PMR-15 composites. The effects of hydrothermal exposure on the mechanical properties of HTS-2 continuous graphite fiber composites were also investigated. The thermo-oxidative stability characteristics of T300 fabric and T300 fabric/PMR-15 composites were determined. Flexural strengths of specimens were determined. The useful lifetime of T300 fabric/PMR-15 composites in air at 316 C was found to be about 100 hours. The useful lifetimes in air at 228 and 260 C were determined to be 500 and 1000 hours, respectively. Absorbed moisture was found to reduce the elevated temperature properties of both the T300 fabricate and HTS-2 continuous fiber composites. The moisture effect was found to be reversible.

Serafini, T. T.↗