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NASA NTRS2003

New Method Developed To Purify Single Wall Carbon Nanotubes for Aerospace Applications

Single wall carbon nanotubes have attracted considerable attention because of their remarkable mechanical properties and electrical and thermal conductivities. Use of these materials as primary or secondary reinforcements in polymers or ceramics could lead to new materials with significantly enhanced mechanical strength and electrical and thermal conductivity. Use of carbon-nanotube-reinforced materials in aerospace components will enable substantial reductions in component weight and improvements in durability and safety. Potential applications for single wall carbon nanotubes include lightweight components for vehicle structures and propulsion systems, fuel cell components (bipolar plates and electrodes) and battery electrodes, and ultra-lightweight materials for use in solar sails. A major barrier to the successful use of carbon nanotubes in these components is the need for methods to economically produce pure carbon nanotubes in large enough quantities to not only evaluate their suitability for certain applications but also produce actual components. Most carbon nanotube synthesis methods, including the HiPCO (high pressure carbon monoxide) method developed by Smalley and others, employ metal catalysts that remain trapped in the final product. These catalyst impurities can affect nanotube properties and accelerate their decomposition. The development of techniques to remove most, if not all, of these impurities is essential to their successful use in practical applications. A new method has been developed at the NASA Glenn Research Center to purify gram-scale quantities of single wall carbon nanotubes. This method, a modification of a gas phase purification technique previously reported by Smalley and others, uses a combination of high-temperature oxidations and repeated extractions with nitric and hydrochloric acid. This improved procedure significantly reduces the amount of impurities (catalyst and nonnanotube forms of carbon) within the nanotubes, increasing their stability significantly. The onset of decomposition of the purified nanotubes (determined by thermal gravimetric analysis in air) is more than 300 C higher than that of the crude nanotubes. Transmission electron microscopy analysis of nanotubes purified by this method reveals near complete removal of iron catalyst particles. Analysis of the nanotubes using inductively coupled plasma spectroscopy revealed that the iron content of the nanotubes was reduced from 22.7 wt% in the crude nanotubes to less than 0.02 wt%. X-ray photoelectron spectroscopy revealed a decrease in iron content after purification as well as an increase in oxygen content due to the formation of carboxylic acid groups on the surface of the nanotubes. Nanotubes purified by this improved method can be readily dispersed in common organic solvents, in particular N,N-dimethylformamide, using prolonged ultrasonic treatment. These dispersions can then be used to incorporate single wall carbon nanotubes into polymer films.

Lebron, Marisabel↗

NASA NTRS1995

Evaluation of Pd-Cr Wires for Strain Gage Application

A newly developed alloy, palladium-13 weight percent chromium (Pd13Cr), was identified by United Technologies Research Center under a NASA contract to be the best material for high temperature strain gage applications. An electrical resistance strain gage that can provide accurate static strain measurement to a temperature higher than that of a commercially available gage is urgently needed in aerospace and aeronautics research. A strain gage made of a 25.4 micron (1 mil) diameter Pd13Cr wire has been recently demonstrated to be usable for static strain measurements to 800 C. This compares to the 400 C temperature limit of the commercially available strain gages. The performance of the Pd-Cr gage, however, strongly depends on the quality of the Pd13Cr wire. Four batches of Pd-Cr wires purchased from three different manufacturers were therefore evaluated to determine the best source of the wire for strain gage applications. The three suppliers were Precious Metal Institute in China, Sigmund Cohn Co., and G & S Titanium, Inc. in the United States. Two batches of wires obtained from Previous Metal Institute in 1987 and 1992, respectively are referred to herein as China87 and China92 wires. The mechanical, chemical and electrical properties of these wires, both as-received and after high temperature exposures at 800 C for 50 hours were analyzed. The elastic modulus and the failure strength of the wires were evaluated using a tensile test machine equipped with a laser speckle strain measurement system. The chemical and microstructural properties of the wires were inspected using a plasma atomic emission spectrometer and a scanning electron microscope (SEM) equipped with an energy dispersive X-ray spectroscope (EDS). The electrical stability and repeatability of the wires were determined by measuring the electrical resistance of the wires during three thermal cycles to 1000 C and a ten-hour soak at 1000 C. As a result of this study, the wire which has the highest strength, the least impurities content, the best oxidation resistance and the best electrical stability will be selected for upcoming strain gage applications.

Lei, Jih-Fen↗

NASA NTRS1990

Nature and origin of interstellar diamond from the Allende CV3 meteorite

Data and experimental evidence which support the contention that the C delta diamonds may result from grain-grain collisions in supernova shocks in the interstellar medium are presented. Fragments of the Allende CV3 chondrite were acid-treated. A whitish powder was obtained. For the Analytical Electron Microscopy (AEM) a small drop of ethanol suspension was transferred onto holey carbon support films on 3 mm EM grids. The AEM was performed on transmission-thin fragments of the material which overlay holes in the film, to eliminate interference from the substrate. Electron Spectroscopy for Chemical Analysis (ESCA) was performed on a large aliquot of C. Diamond was identified by selected area electron diffraction. Scanning Transmission Electron Microscope / Energy Dispersive X-ray (STEM-EDS) microanalyses of the C delta diamond, using a light-element detector, show that oxygen and possibly nitrogen are the only impurities consistently present. ESCA spectra from bulk C delta material confirm the presence of N at a level of 0.35 percent or less. Under UV irradiation a yellow-red fluorescence is observed, consistent with that of natural diamonds containing substitutional N. Electron Energy Loss Spectra (EELS) were recorded at 2 eV resolution from the C delta diamond, high pressure synthetic diamond, a diamond film produced in a low pressure plasma by chemical vapor deposition (CVD) on a heated silicon substrate (Roy, 1987), graphite, and amorphous arc sputtered carbon. Comparison of the carbon K edge shape and fine structure shows the Allende C delta phase to be largely diamond, but with a significant pre-edge absorption feature indicative of transitions of C 1s electrons into pi asterisk orbitals which are absent in the purely sp(3)-bonded diamond but present in graphite and amorphous carbon.

Blake, David↗

NASA NTRS1992

Dependence of the cathodoluminescence of diamond films on deposition temperature

The deposition temperature dependence of the cathodoluminescence (CL) of diamond thin films grown by microwave-plasma-assisted chemical vapor deposition has been investigated. Depositions were made in the temperature range of 400 to 750 C at a pressure of 10 Torr, with a gas mixture of 5 percent CH4 and 5 percent O2 in hydrogen. The intensity of the luminescent peak at 430 nm was used as a measure of diamond quality for the film. This peak was found to be a maximum above 600 C. Examination of the intensities of CL emissions associated with nitrogen and silicon impurities at 530, 560, and 740 nm indicate incorporation of these impurities is more efficient at temperatures above 600 C. Film quality was thus found to be an optimization of competing mechanisms, i.e., improvement of diamond quality as evidenced by the intensity of the 430 nm peak, with the apparent activation of impurities and vacancy defects at elevated temperatures.

Shing, Y. H.↗

NASA NTRS1979

Physical processes in directed ion beam sputtering

The general operation of a discharge chamber for the production of ions is described. A model is presented for the magnetic containment of both primary and secondary or Maxwellian electrons in the discharge plasma. Cross sections were calculated for energy and momentum transfer in binary collisions between like pairs of Ar, Kr, and Xe atoms in the energy range from about 1 eV to 1000 eV. These calculations were made from available pair interaction potentials using a classical model. Experimental data from the literature were fit to a theoretical expression for the Ar resonance charge exchange cross section over the same energy range. A model was developed that describes the processes of conical texturing of a surface due to simultaneous directed ion beam etching and sputter deposition of an impurity material. This model accurately predicts both a minimum temperature for texturing to take place and the variation of cone density with temperature. It also provides the correct order of magnitude of cone separation. It was predicted from the model, and subsequently verified experimentally, that a high sputter yield material could serve as a seed for coning of a lower sputter yield substrate. Seeding geometries and seed deposition rates were studied to obtain an important input to the theoretical texturing model.

Robinson, R. S.↗

NASA NTRS2004

Improved Method of Purifying Carbon Nanotubes

An improved method of removing the residues of fabrication from carbon nanotubes has been invented. These residues comprise amorphous carbon and metal particles that are produced during the growth process. Prior methods of removing the residues include a variety of processes that involved the use of halogens, oxygen, or air in both thermal and plasma processes. Each of the prior methods entails one or more disadvantages, including non-selectivity (removal or damage of nanotubes in addition to removal of the residues), the need to dispose of toxic wastes, and/or processing times as long as 24 hours or more. In contrast, the process described here does not include the use of toxic chemicals, the generation of toxic wastes, causes little or no damage to the carbon nanotubes, and involves processing times of less than 1 hour. In the improved method, purification is accomplished by flowing water vapor through the reaction chamber at elevated temperatures and ambient pressures. The impurities are converted to gaseous waste products by the selective hydrogenation and hydroxylation by the water in a reaction chamber. This process could be performed either immediately after growth or in a post-growth purification process. The water used needs to be substantially free of oxygen and can be obtained by a repeated freeze-pump-thaw process. The presence of oxygen will non-selectively attach the carbon nanotubes in addition to the amorphous carbon.

Delzeit, Lance D.↗

NASA NTRS1984

Coaxial carbon plasma gun deposition of amorphous carbon films

A unique plasma gun employing coaxial carbon electrodes was used in an attempt to deposit thin films of amorphous diamond-like carbon. A number of different structural, compositional, and electrical characterization techniques were used to characterize these films. These included scanning electron microscopy, scanning transmission electron microscopy, X ray diffraction and absorption, spectrographic analysis, energy dispersive spectroscopy, and selected area electron diffraction. Optical absorption and electrical resistivity measurements were also performed. The films were determined to be primarily amorphous, with poor adhesion to fused silica substrates. Many inclusions of particulates were found to be present as well. Analysis of these particulates revealed the presence of trace impurities, such as Fe and Cu, which were also found in the graphite electrode material. The electrodes were the source of these impurities. No evidence of diamond-like crystallite structure was found in any of the film samples. Details of the apparatus, experimental procedure, and film characteristics are presented.

Sater, D. M.↗

NASA NTRS1998

Toward Optimum Scale and TBC Adhesion on Single Crystal Superalloys

Single crystal superalloys exhibit excellent cyclic oxidation resistance if their sulfur content is reduced from typical impurity levels of approximately 5 ppmw to below 0.5 ppmw. Excellent alumina scale adhesion was documented for PWA 1480 and PWA 1484 without yttrium additions. Hydrogen annealing produced effective desulfurization of PWA 1480 to less than 0.2 ppmw and was also used to achieve controlled intermediate levels. The direct relationship between cyclic oxidation behavior and sulfur content was shown. An adhesion criterion was proposed based on the total amount of sulfur available for interfacial segregation, e.g., less than or equal to 0.2 ppmw S will maximize adhesion for a 1 mm thick sample. PWA 1484, melt desulfurized to 0.3 ppmw S, also exhibited excellent cyclic oxidation resistance and encouraging TBC lives (10 mils of 8YSZ, plasma sprayed without a bond coat) in 1100 C cyclic oxidation tests.

Smialek, James L.↗

NASA NTRS2000

Key Durability Issues with Mullite-Based Environmental Barrier Coatings for Si-Based Ceramics

Plasma-sprayed mullite (3Al2O3.2SiO2) and mullite/yttria-stabilized-zirconia (YSZ) dual layer coatings have been developed to protect silicon -based ceramics from environmental attack. Mullite-based coating systems show excellent durability in air. However, in combustion environments, corrosive species such as molten salt or water vapor penetrate through cracks in the coating and attack the Si-based ceramics along the interface. Thus the modification of the coating system for enhanced crack-resistance is necessary for long-term durability in combustion environments. Other key durability issues include interfacial contamination and coating/substrate bonding. Interfacial contamination leads to enhanced oxidation and interfacial pore formation, while a weak coating/substrate bonding leads to rapid attack of the interface by corrosive species, both of which can cause a premature failure of the coating. Interfacial contamination can be minimized by limiting impurities in coating and substrate materials. The interface may be modified to improve the coating/substrate bond.

Lee, Kang N.↗

NASA NTRS1999

Key Durability Issues with Mullite-Based Environmental Barrier Coatings for Si-Based Ceramics

Plasma-sprayed mullite (3Al2O3 central dot 2SiO2) and mullite/yttria-stabilized-zirconia (YSZ) dual layer coatings have been developed to protect silicon-based ceramics from environmental attack. Mullite-based coating systems show excellent durability in air. However, in combustion environments, corrosive species such as molten salt or water vapor penetrate through cracks in the coating and attack the Si-based ceramics along the interface, Thus modification of the coating system for enhanced crack-resistance is necessary for long-term durability in combustion environments. Other key durability issues include interfacial contamination and coating/substrate bonding. Interfacial contamination leads to enhanced oxidation and interfacial pore formation, while weak coating/substrate bonding leads to rapid attack of the interface by corrosive species, both of which can cause premature failure of the coating. Interfacial contamination can be minimized by limiting impurities in coating and substrate materials. The interface may be modified to improve the coating/substrate bond.

Lee, Kang N.↗

NASA NTRS2007

Sulfur and Moisture Effects on Alumina Scale and TBC Spallation

It has been well established that a few ppmw sulfur impurity may segregate to the interface of thermally grown alumina scales and the underlying substrate, resulting in bond degradation and premature spallation. This has been shown for NiAl and NiCrAl-based alloys, bare single crystal superalloys, or coated superalloys. The role of reactive elements (especially Y) has been to getter the sulfur in the bulk and preclude interfacial segregation. Pt additions are also very beneficial, however a similar thermodynamic explanation does not apply. The purpose of the present discussion is to highlight some observations of these effects on Rene'142, Rene'N5, PWA1480, and PWA1484. For PWA1480, we have mapped cyclic oxidation and spallation in terms of potential sulfur interfacial layers and found that a cumulative amount of about one monolayer is sufficient to degrade long term adhesion. Depending on substrate thickness, optimum performance occurs if sulfur is reduced below about 0.2-0.5 ppmw. This is accomplished in the laboratory by hydrogen annealing or commercially by melt-fluxing. Excellent 1150 C cyclic oxidation is thus demonstrated for desulfurized Rene'142, Rene'N5, and PWA1484. Alternatively, a series of N5 alloys provided by GE-AE have shown that as little as 15 ppmw of Y dopant was effective in providing remarkable scale adhesion. In support of a Y-S gettering mechanism, hydrogen annealing was unable to desulfurize these alloys from their initial level of 5 ppmw S. This impurity and critical doping level corresponds closely to YS or Y2S3 stoichiometry. In many cases, Y-doped alloys or alloys with marginal sulfur levels exhibit an oxidative sensitivity to the ambient humidity called Moisture-Induced Delayed Spallation (MIDS). After substantial scale growth, coupled with damage from repeated cycling, cold samples may spall after a period of time, breathing on them, or immersing them in water. While stress corrosion arguments may apply, we propose that the underlying cause is related to a hydrogen embrittlement reaction: Al alloy + 3 H2O = Al(OH)3 + 3H(+) + 3e(-). This mechanism is derived from an analogous moisture-induced hydrogen embrittlement mechanism originally shown for Ni3Al and FeAl intermetallics. Consequently, a cathodic hydrogen charging technique was used to demonstrate that electrolytic de-scaling occurs for these otherwise adherent alumina scales formed on Y-doped Rene'N5, in support of hydrogen effects. Finally, some TBC observations are discussed in light of all of the above. Plasma sprayed 8YSZ coatings, produced on PWA1484 without a bond coat, were found to survive more than 1000 1-hr cycles at 1100 C when desulfurized to below 0.1 ppmw. At higher sulfur (1.2 ppmw) levels, moisture sensitivity and delayed TBC failure, referred to as Desk Top Spallation, occurred at just 200 hr. Despite a large degree of scatter, a factor of 5 in life improvement is indicated for desulfurized samples in cyclic furnace tests, confirming the beneficial effect of low sulfur alloys on model TBC systems. (DTS and moisture effects are also observed on commercially applied PVD 7YSZ coatings on Rene'N5+Y with Pt-aluminide bond coats). These types of catastrophic failure were subverted on the model system by segmenting the substrate into a network of 0.010 high ribs, spaced in. apart, prior to plasma spraying. No failures occurred after 1000 cycles at 1150 C or after 2000 cycles at 1100 C, even after water immersion. The benefit is described in terms of elasticity models and a critical buckling stress.

Smialek, James L.↗

NASA NTRS1993

Analytical and experimental investigation of the feasibility of accelerated lifetime testing of materials exposed to an atomic oxygen beam

The interaction of atomic particles with surfaces is of both scientific and technological interest. Past work emphasizes the measurement of high-energy sputtering yields. Very little work utilized low-energy beams for which chemical and electronic effects can be important. Even less work has been carried out using well-defined low-energy projectiles. The use of low-energy, reactive projectiles permits one to investigate surface processes that have not been well characterized. As the energy of the projectile decreases, the collisional cascades and spikes, that are common for high-energy projectiles, become less important, and chemical and electronic effects can play a significant role. Aspects of particle-surface interactions are of concern in several areas of technology. For example, the erosion, desorption, and glow of surfaces of spacecraft in orbit are important in the arena of space technology. The materials studied under this contract are of possible use on the exterior portions of the power generation system of Space Station Freedom. Under the original designs, Space Station Freedom's power generation system would generate potential differences on the surface as high as 200 volts. Ions in the plasma that often surround orbiting vehicles would be accelerated by these potentials leading to bombardment and erosion of the exposed surfaces. The major constituent of the atmosphere, approximately 90 percent, in the low earth orbit region is atomic oxygen. Since atomic oxygen is extremely reactive with most materials, chemical effects can arise in addition to the physical sputtering caused by the acceleration of the oxygen ions. Furthermore, the incident oxygen ions can remain embedded in the exposed surfaces, altering the chemical composition of the surfaces. Since the effective binding energy of a chemically altered surface can be quite different from that of the pure substrate, the sputtering yield of a chemically altered surface is usually different also. The low-energy O+ sputtering yield measurements, reported here, will help quantify the erosion rates for materials exposed to the low-earth orbit environment. These measurements are of technological importance in another respect. In most surface analysis techniques, a surface is bombarded with ions, electrons or photons. Information concerning the structure of the surface and near-surface bulk, abundance of impurities and defects, as well as other surface properties are obtained either from the desorbed species or from the scattered projectiles. Because of their low penetration depth, low-energy ions provide an advantage over other techniques because they provide information that is more indicative of conditions on the surface rather than integrated effects arising from deeper in the bulk. A better understanding of the microscopic processes involved in these interactions is not only of basic scientific interest, but will also aid the scientific community by increasing the accuracy and usefulness of these surface analysis techniques.

Albridge, Royal↗