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NASA NTRS2007

Arrays of Bundles of Carbon Nanotubes as Field Emitters

Experiments have shown that with suitable choices of critical dimensions, planar arrays of bundles of carbon nanotubes (see figure) can serve as high-current-density field emitter (cold-cathode) electron sources. Whereas some hot-cathode electron sources must be operated at supply potentials of thousands of volts, these cold-cathode sources generate comparable current densities when operated at tens of volts. Consequently, arrays of bundles of carbon nanotubes might prove useful as cold-cathode sources in miniature, lightweight electron-beam devices (e.g., nanoklystrons) soon to be developed. Prior to the experiments, all reported efforts to develop carbon-nanotube-based field-emission sources had yielded low current densities from a few hundred microamperes to a few hundred milliamperes per square centimeter. An electrostatic screening effect, in which taller nanotubes screen the shorter ones from participating in field emission, was conjectured to be what restricts the emission of electrons to such low levels. It was further conjectured that the screening effect could be reduced and thus emission levels increased by increasing the spacing between nanotubes to at least by a factor of one to two times the height of the nanotubes. While this change might increase the emission from individual nanotubes, it would decrease the number of nanotubes per unit area and thereby reduce the total possible emission current. Therefore, to maximize the area-averaged current density, it would be necessary to find an optimum combination of nanotube spacing and nanotube height. The present concept of using an array of bundles of nanotubes arises partly from the concept of optimizing the spacing and height of field emitters. It also arises partly from the idea that single nanotubes may have short lifetimes as field emitters, whereas bundles of nanotubes could afford redundancy so that the loss of a single nanotube would not significantly reduce the overall field emission.

Manohara, Harish↗

NASA NTRS2007

Creep Forming of Carbon-Reinforced Ceramic-Matrix Composites

A set of lecture slides describes an investigation of creep forming as a means of imparting desired curvatures to initially flat stock plates of carbon-reinforced ceramic-matrix composite (C-CMC) materials. The investigation is apparently part of a continuing effort to develop improved means of applying small CCMC repair patches to reinforced carbon-carbon leading edges of aerospace vehicles (e.g., space shuttles) prior to re-entry into the atmosphere of the Earth. According to one of the slides, creep forming would be an intermediate step in a process that would yield a fully densified, finished C-CMC part having a desired size and shape (the other steps would include preliminary machining, finish machining, densification by chemical vapor infiltration, and final coating). The investigation included experiments in which C-CMC disks were creep-formed by heating them to unspecified high temperatures for time intervals of the order of 1 hour while they were clamped into single- and double-curvature graphite molds. The creep-formed disks were coated with an oxidation- protection material, then subjected to arc-jet tests, in which the disks exhibited no deterioration after exposure to high-temperature test conditions lasting 490 seconds.

Vaughn, Wallace L.↗

NASA NTRS2010

Thermogravimetric Analysis of Single-Wall Carbon Nanotubes

An improved protocol for thermogravimetric analysis (TGA) of samples of single-wall carbon nanotube (SWCNT) material has been developed to increase the degree of consistency among results so that meaningful comparisons can be made among different samples. This improved TGA protocol is suitable for incorporation into the protocol for characterization of carbon nanotube material. In most cases, TGA of carbon nanotube materials is performed in gas mixtures that contain oxygen at various concentrations. The improved protocol is summarized.

Arepalli, Sivram↗

NASA NTRS2010

Dispersions of Carbon nanotubes in Polymer Matrices

Dispersions of carbon nanotubes exhibiting long term stability are based on a polymer matrix having moieties therein which are capable of a donor-acceptor complexation with carbon nanotubes. The carbon nanotubes are introduced into the polymer matrix and separated therein by standard means. Nanocomposites produced from these dispersions are useful in the fabrication of structures, e.g., lightweight aerospace structures.

Wise, Kristopher Eric↗

NASA NTRS2010

Understanding High Recession Rates of Carbon Ablators Seen in Shear Tests in an Arc Jet

High rates of recession in arc jet shear tests of Phenolic Impregnated Carbon Ablator (PICA) inspired a series of tests and analysis on FiberForm (a carbon preform used in the fabrication of PICA). Arc jet tests were performed on FiberForm in both air and pure nitrogen for stagnation and shear configurations. The nitrogen tests showed little or no recession, while the air tests of FiberForm showed recession rates similar to that of PICA (when adjusted for the difference in density). While mechanical erosion can not be ruled out, this is the first step in doing so. Analysis using a carbon oxidation boundary condition within DPLR was used to predict the recession rate of FiberForm. The analysis indicates that much of the anomalous recession behavior seen in shear tests may simply be an artifact of the non-flight like test configuration (copper upstream of the test article) a result of dissimilar enthalpy and oxygen concentration profiles on the copper. Shape change effects were also investigated and shown to be relatively small.

Driver, David M.↗

NASA NTRS2010

Progress in Measurement of Carbon Dioxide Using a Broadband Lidar

In order to better understand the budget of carbon dioxide in the Earth's atmosphere it is necessary to develop a global high precision understanding of the carbon dioxide column. In order to uncover the 'missing sink" that is responsible for the large discrepancies in the budget as we presently understand it calculation has indicated that measurement accuracy on the order of 1 ppm is necessary. Because typical column average CO2 has now reached 380 ppm this represents a precision on the order of .25% for these column measurements. No species has ever been measured from space at such a precision. In recognition of the importance of understanding the CO2 budget in order to evaluate its impact on global warming the National Research Council in its decadal survey report to NASA recommended planning for a laser based total CO2 mapping mission in the near future. The extreme measurement accuracy requirements on this mission places very strong requirements on the laser system used for the measurement. This work presents an overview of the characteristics necessary in a laser system used to make this measurement. Consideration is given to the temperature dependence, pressure broadening, and pressure shift of the CO2 lines themselves and how these impact the laser system characteristics We have been examining the possibility of making precise measurements of atmospheric carbon dioxide using broad band source of radiation. This means that many of the difficulties in wavelength control can be treated in the detector portion of the system rather than the laser source. It also greatly reduces the number of individual lasers required to make a measurement. Simplifications such as these are extremely desirable for systems designed to operate from space.

Heaps, William S.↗

NASA NTRS2010

Laser ablation for the synthesis of carbon nanotubes

Single walled carbon nanotubes are produced in a novel apparatus by the laser-induced ablation of moving carbon target. The laser used is of high average power and ultra-fast pulsing. According to various preferred embodiments, the laser produces an output above about 50 watts/cm.sup.2 at a repetition rate above about 15 MHz and exhibits a pulse duration below about 10 picoseconds. The carbon, carbon/catalyst target and the laser beam are moved relative to one another and a focused flow of side pumped, preheated inert gas is introduced near the point of ablation to minimize or eliminate interference by the ablated plume by removal of the plume and introduction of new target area for incidence with the laser beam. When the target is moved relative to the laser beam, rotational or translational movement may be imparted thereto, but rotation of the target is preferred.

Holloway, Brian C.↗

NASA NTRS2010

Using Leaf Chlorophyll to Parameterize Light-Use-Efficiency Within a Thermal-Based Carbon, Water and Energy Exchange Model

Chlorophylls absorb photosynthetically active radiation and thus function as vital pigments for photosynthesis, which makes leaf chlorophyll content (C(sub ab) useful for monitoring vegetation productivity and an important indicator of the overall plant physiological condition. This study investigates the utility of integrating remotely sensed estimates of C(sub ab) into a thermal-based Two-Source Energy Balance (TSEB) model that estimates land-surface CO2 and energy fluxes using an analytical, light-use-efficiency (LUE) based model of canopy resistance. The LUE model component computes canopy-scale carbon assimilation and transpiration fluxes and incorporates LUE modifications from a nominal (species-dependent) value (LUE(sub n)) in response to short term variations in environmental conditions, However LUE(sub n) may need adjustment on a daily timescale to accommodate changes in plant phenology, physiological condition and nutrient status. Day to day variations in LUE(sub n) were assessed for a heterogeneous corn crop field in Maryland, U,S.A. through model calibration with eddy covariance CO2 flux tower observations. The optimized daily LUE(sub n) values were then compared to estimates of C(sub ab) integrated from gridded maps of chlorophyll content weighted over the tower flux source area. The time continuous maps of daily C(sub ab) over the study field were generated by focusing in-situ measurements with retrievals generated with an integrated radiative transfer modeling tool (accurate to within +/-10%) using at-sensor radiances in green, red and near-infrared wavelengths acquired with an aircraft imaging system. The resultant daily changes in C(sub ab) within the tower flux source area generally correlated well with corresponding changes in daily calibrated LUE(sub n) derived from the tower flux data, and hourly water, energy and carbon flux estimation accuracies from TSEB were significantly improved when using C(sub ab) for delineating spatio-temporal variations in LUE(sub n). The results demonstrate the synergy between thermal infrared and shortwave reflective wavebands in producing valuable remote sensing data for operational monitoring of carbon and water fluxes.

Houlborg, Rasmus↗

NASA NTRS2010

Comparative Spectra of Oxygen-Rich Versus Carbon-Rich Circumstellar Shells: VY Canis Majoris and IRC(plus)10216 at 215-285 GHz

A sensitive (1sigma rms at 1 MHz resolution approx.3 mK) 1 mm spectral line survey (214.5-285.5 GHz) of VY Canis Majoris (VY CMa) and IRC +10216 has been conducted to compare the chemistries of oxygen- and carbon-rich circumstellar envelopes. This study was carried out using the Submillimeter Telescope of the Arizona Radio Observatory with a new Atacama Large Millimeter Array type receiver. This survey is the first to chemically characterize an O-rich circumstellar shell at millimeter wavelengths. In VY CMa, 128 emission features were detected arising from 18 different molecules; and in IRC +10216, 720 lines were observed, assigned to 32 different species. The 1 mm spectrum of VY CMa is dominated by SO, and SiS; in IRC +10216, C4H and SiC2 are the most recurrent species. Ten molecules were common to both sources: CO, SiS, SiO, CS, CN, HCN, HNC, NaCl, PN, and HCO(+). Sulfur plays an important role in VY CMa, but saturated/ unsaturated carbon dominates the molecular content of IRC +102.16, producing CH2NH, for example. Although the molecular complexity of IRC +10216 is greater, VY CMa supports a unique "inorganic" chemistry leading to the oxides PO, AlO, and AlOH. Only diatomic and triatomic compounds were observed in VY CMa, while species with four or more atoms are common in IRC +10216, reflecting carbon's ability to form multiple strong bonds, unlike oxygen. In VY CMa, a new water maser (v2 = 2) has been found, as well as vibrationally excited NaCl. Toward IRC +10216, vibrationally excited CCH was detected for the first time.

Tenebaum, E. D.↗

NASA NTRS2001

Iron Catalyst Chemistry in High Pressure Carbon Monoxide Nanotube Reactor

The high-pressure carbon monoxide (HiPco) technique for producing single wall carbon nanotubes (SWNT) is analyzed using a chemical reaction model coupled with properties calculated along streamlines. Streamline properties for mixing jets are calculated by the FLUENT code using the k-e turbulent model for pure carbon monixide. The HiPco process introduces cold iron pentacarbonyl diluted in CO, or alternatively nitrogen, at high pressure, ca. 30 atmospheres into a conical mixing zone. Hot CO is also introduced via three jets at angles with respect to the axis of the reactor. Hot CO decomposes the Fe(CO)5 to release atomic Fe. Cluster reaction rates are from Krestinin, et aI., based on shock tube measurements. Another model is from classical cluster theory given by Girshick's team. The calculations are performed on streamlines that assume that a cold mixture of Fe(CO)5 in CO is introduced along the reactor axis. Then iron forms clusters that catalyze the formation of SWNTs from the Boudouard reaction on Fe-containing clusters by reaction with CO. To simulate the chemical process along streamlines that were calculated by the fluid dynamics code FLUENT, a time history of temperature and dilution are determined along streamlines. Alternative catalyst injection schemes are also evaluated.

Scott, Carl D.↗

NASA NTRS2010

Functionalization of Single-Wall Carbon Nanotubes by Photo-Oxidation

new technique for carbon nanotube oxidation was developed based upon the photo-oxidation of organic compounds. The resulting method is more benign than conventional oxidation approaches and produces single-wall carbon nanotubes (SWCNTs) with higher levels of oxidation. In this procedure, an oxygen saturated suspension of SWNTs in a suitable solvent containing a singlet oxygen sensitizer, such as Rose Bengal, is irradiated with ultraviolet light. The resulting oxidized tubes are recovered by filtering the suspension, followed by washing to remove any adsorbed solvent and sensitizer, and drying in a vacuum oven. Chemical analysis by FT-infrared and x-ray photoelectron spectroscopy revealed that the oxygen content of the photo-oxidized SWCNT was 11.3 atomic % compared to 6.7 atomic % for SWCNT that had been oxidized by standard treatment in refluxing acid. The photo-oxidized SWCNT produced by this method can be used directly in various polymer matrixes, or can be further modified by chemical reactions at the oxygen functional groups and then used as additives. This method may also be suitable for use in oxidation of multiwall carbon nanotubes and graphenes.

Lebron-Colon, Marisabel↗

NASA NTRS2010

Carbon Isotope Characterization of Organic Intermediaries in Hydrothermal Hydrocarbon Synthesis by Pyrolysis-GC-MS-C-IRMS

We report results of experiments designed to characterize the carbon isotope composition of intermediate organic compounds produced as a result of mineral surface catalyzed reactions. The impetus for this work stems from recently reported detection of methane in the Martian atmosphere coupled with evidence showing extensive water-rock interaction during Martian history. Abiotic formation by Fischer-Tropsch-type (FTT) synthesis during serpentinization reactions may be one possible process responsible for methane generation on Mars, and measurement of carbon and hydrogen isotopes of intermediary organic compounds can help constrain the origin of this methane. Of particular interest within the context of this work is the isotopic composition of organic intermediaries produced on the surfaces of mineral catalysts (i.e. magnetite) during hydrothermal experiments, and the ability to make meaningful and reproducible isotope measurements. Our isotope measurements utilize a unique analytical technique combining Pyrolysis-Gas Chromatograph-Mass Spectrometry-Combustion-Isotope Ratio Mass Specrometry (Py-GC-MS-C-IRMS). Others have conducted similar pyrolysis-IRMS experiments on low molecular weight organic acids (Dias, et al, Organic Geochemistry, 33 [2002]). Our technique differs in that it carries a split of the pyrolyzed GC-separated product to a Thermo DSQ-II quadrupole mass spectrometer as a means of making qualitative and semi-quantitative compositional measurements of the organic compounds. A sample of carboxylic acid (mixture of C1 through C6) was pyrolyzed at 100 XC and passed through the GC-MS-C-IRMS (combusted at 940 XC). In order to test the reliability of our technique we compared the _13C composition of different molecular weight organic acids (from C1 through C6) extracted individually by the traditional sealed-tube cupric oxide combustion (940 XC) method with the _13C produced by our pyrolysis technique. Our data indicate that an average 4.3. +/-0.5. (V-PDB) apparent isotopic fractionation accompanies the pyrolysis extractions. We postulate that this isotope offset could be the result of incomplete thermal desorption during pyrolysis. We are continuing to investigate the reliability of this pyrolysis technique for correcting carbon isotope measurements of mineral surface catalyzed organic compounds.

Socki, Richard A.↗

NASA NTRS2010

Evaluation of Commercial Off-the-Shelf Sorbents and Catalysts for Control of Ammonia and Carbon Monoxide

Designers of future space vehicles envision simplifying the Atmosphere Revitalization (AR) system by combining the functions of trace contaminant (TC) control and carbon dioxide removal into one swing-bed system. Flow rates and bed sizes of the TC and CO2 systems have historically been very different. There is uncertainty about the ability of trace contaminant sorbents to adsorb adequately in high-flow or short bed length configurations, and to desorb adequately during short vacuum exposures. There is also concern about ambient ammonia levels in the absence of a condensing heat exchanger. In addition, new materials and formulations have become commercially available, formulations never evaluated by NASA for purposes of trace contaminant control. The optimal air revitalization system for future missions may incorporate a swing-bed system for carbon dioxide (CO2) and partial trace contaminant control, with a reduced-size, low-power, targeted trace contaminant system supplying the remaining contaminant removal capability. This paper describes the results of a comparative experimental investigation into materials for trace contaminant control that might be part of such a system. Ammonia sorbents and low temperature carbon monoxide (CO) oxidation catalysts are the foci. The data will be useful to designers of AR systems for future flexible path missions. This is a continuation of work presented in a prior year, with extended test results.

Luna, Bernadette↗

NASA NTRS2011

Carbon Dioxide Reduction Technology Trade Study

For long-term human missions, a closed-loop atmosphere revitalization system (ARS) is essential to minimize consumables. A carbon dioxide (CO2) reduction technology is used to reclaim oxygen (O2) from metabolic CO2 and is vital to reduce the delivery mass of metabolic O2. A key step in closing the loop for ARS will include a proper CO2 reduction subsystem that is reliable and with low equivalent system mass (ESM). Sabatier and Bosch CO2 reduction are two traditional CO2 reduction subsystems (CRS). Although a Sabatier CRS has been delivered to International Space Station (ISS) and is an important step toward closing the ISS ARS loop, it recovers only 50% of the available O2 in CO2. A Bosch CRS is able to reclaim all O2 in CO2. However, due to continuous carbon deposition on the catalyst surface, the penalties of replacing spent catalysts and reactors and crew time in a Bosch CRS are significant. Recently, technologies have been developed for recovering hydrogen (H2) from Sabatier-product methane (CH4). These include methane pyrolysis using a microwave plasma, catalytic thermal pyrolysis of CH4 and thermal pyrolysis of CH4. Further, development in Sabatier reactor designs based on microchannel and microlith technology could open up opportunities in reducing system mass and enhancing system control. Improvements in Bosch CRS conversion have also been reported. In addition, co-electrolysis of steam and CO2 is a new technology that integrates oxygen generation and CO2 reduction functions in a single system. A co-electrolysis unit followed by either a Sabatier or a carbon formation reactor based on Bosch chemistry could improve the overall competitiveness of an integrated O2 generation and CO2 reduction subsystem. This study evaluates all these CO2 reduction technologies, conducts water mass balances for required external supply of water for 1-, 5- and 10-yr missions, evaluates mass, volume, power, cooling and resupply requirements of various technologies. A system analysis and comparison among the technologies was made based on ESM, technology readiness level and reliability. Those technologies with potential were recommended for development.

Jeng, Frank F.↗

NASA NTRS2011

Crew Health and Performance Improvements with Reduced Carbon Dioxide Levels and the Resource Impact to Accomplish Those Reductions

Carbon dioxide (CO2) removal is one of the primary functions of the International Space Station (ISS) atmosphere revitalization systems. Primary CO2 removal is via the ISS s two Carbon Dioxide Removal Assemblies (CDRAs) and the Russian carbon dioxide removal assembly (Vozdukh); both of these systems are regenerable, meaning that their CO2 removal capacity theoretically remains constant as long as the system is operating. Contingency CO2 removal capability is provided by lithium hydroxide (LiOH) canisters, which are consumable, meaning that their CO2 removal capability disappears once the resource is used. With the advent of 6 crew ISS operations, experience showing that CDRA failures are not uncommon, and anecdotal association of crew symptoms with CO2 values just above 4 mmHg, the question arises: How much lower do we keep CO2 levels to minimize the risk to crew health and performance, and what will the operational cost to the CDRAs be to do it? The primary crew health concerns center on the interaction of increased intracranial pressure from fluid shifts and the increased intracranial blood flow induced by CO2. Typical acute symptoms include headache, minor visual disturbances, and subtle behavioral changes. The historical database of CO2 exposures since the beginning of ISS operations has been compared to the incidence of crew symptoms reported in private medical conferences. We have used this database in an attempt to establish an association between the CO2 levels and the risk of crew symptoms. This comparison will answer the question of the level needed to protect the crew from acute effects. As for the second part of the question, operation of the ISS s regenerable CO2 removal capability reduces the limited life of constituent parts. It also consumes limited electrical power and thermal control resources. Operation of consumable CO2 removal capability (LiOH) uses finite consumable materials, which must be replenished in the long term. Therefore, increased CO2 removal means increased resource use, with increased logistical capability to maintain necessary resources on board ISS. We must strike a balance between sufficiently low CO2 levels to maintain crew health and CO2 levels which are operationally feasible for the ISS program

James, John T.↗

NASA NTRS2010

NASA-JSC Protocol for the Characterization of Single Wall Carbon Nanotube Material Quality

It is well known that the raw as well as purified single wall carbon nanotube (SWCNT) material always contain certain amount of impurities of varying composition (mostly metal catalyst and non-tubular carbon). Particular purification method also creates defects and/or functional groups in the SWCNT material and therefore affects the its dispersability in solvents (important to subsequent application development). A number of analytical characterization tools have been used successfully in the past years to assess various properties of nanotube materials, but lack of standards makes it difficult to compare these measurements across the board. In this work we report the protocol developed at NASA-JSC which standardizes measurements using TEM, SEM, TGA, Raman and UV-Vis-NIR absorption techniques. Numerical measures are established for parameters such as metal content, homogeneity, thermal stability and dispersability, to allow easy comparison of SWCNT materials. We will also report on the recent progress in quantitative measurement of non-tubular carbon impurities and a possible purity standard for SWCNT materials.

Arepalli, Sivaram↗

NASA NTRS2000

Single-Wall Carbon Nanotube Production by the Arc Process: A Parametric Study

Single wall carbon nanotubes are produced using the arc discharge process. Graphite anodes are filled with a mixture of nickel and yttrium metallic powders, then vaporized by creating a high current arc. By varying the current, gap distance, and ambient pressure it is shown that the best yield of single wall carbon nanotubes is obtained within a narrow range of conditions. The relative yield and purity of the product are indicated semi-quantitatively from scanning electric microscopy (SEM) and thermogravimetric analysis (TGA). Two types of anodes have been investigated. The first is hollow and filled with a powder mixture of graphite, nickel and yttrium. The second is filled with a paste made of a mixture of metal nitrates, graphite powder and carbon adhesive, then reduced in an argon atmosphere at high temperature. Product purity and yield will be compared for the two types of anodes. The graphite in the anodes may have hydrogen attached in the pores. To remove this impurity anodes have been baked up to 1400 - 1500 C. The effect of baking the anodes on impurities in the product will be given.

Scott, Carl D.↗

NASA NTRS2011

Field Characterization of the Mineralogy and Organic Chemistry of Carbonates from the 2010 Arctic Mars Analog Svalbard Expedition by Evolved Gas Analysis

The 2010 Arctic Mars Analog Svalbard Expedition (AMASE) investigated two geologic settings using methodologies and techniques being developed or considered for future Mars missions, such as the Mars Science Laboratory (MSL), ExoMars, and Mars Sample Return. The Sample Analysis at Mars (SAM) [1] instrument suite, which will be on MSL, consists of a quadrupole mass spectrometer (QMS), a gas chromatograph (GC), and a tunable laser mass spectrometer (TLS); all will be applied to analyze gases created by pyrolysis of samples. During AMASE, a Hiden Evolved Gas Analysis-Mass Spectrometer (EGA-MS) system represented the EGA-MS capability of SAM. Another MSL instrument, CheMin, will use x-ray diffraction (XRD) and x-ray fluorescence (XRF) to perform quantitative mineralogical characterization of samples [e.g., 2]. Field-portable versions of CheMin were used during AMASE. AMASE 2010 focused on two sites that represented biotic and abiotic analogs. The abiotic site was the basaltic Sigurdfjell vent complex, which contains Mars-analog carbonate cements including carbonate globules which are excellent analogs for the globules in the ALH84001 martian meteorite [e.g., 3, 4]. The biotic site was the Knorringfjell fossil methane seep, which featured carbonates precipitated in a methane-supported chemosynthetic community [5]. This contribution focuses on EGA-MS analyses of samples from each site, with mineralogy comparisons to CheMin team results. The results give insight into organic content and organic-mineral associations, as well as some constraints on the minerals present.

McAdam, A. C.↗