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At least 73 records · Page 4
All sourcesNASA NTRSDOE OSTI
NASA NTRS1985

Graphite fiber intercalation: Dynamics of the bromine intercalation process

The resistance of pitch-based graphite fibers was monitored, in situ, during a series of bromine intercalation experiments. The threshold pressure for the bromine intercalation of pitch-based fibers was estimated to be 102 torr. When the bromine atmosphere was removed from the reaction chamber, the resistivity of the intercalated graphite fibers increased consistently. This increase was attributed to loss of bromine from the perimeter of the fiber. The loss was confirmed by mapping the bromine concentration across the diameter of single intercalated fibers with either energy dispersive spectroscopy or scanning Auger microscopy. A statistical study comparing fibers intercalated in bromine vapor with fibers intercalated in bromine liquid showed that similar products were obtained with both methods of intercalation.

Jaworske, D. A.↗
NASA NTRS1986

Graphite fiber intercalation: Basic properties of copper chloride intercalated fibers

In situ resistance measurements were used to follow the intercalation of copper chloride in pitch-based fibers. Subsequent single fiber resistivity measurements reveal a large range of resistivities, from 13 to 160 micro-ohms cm. Additional density measurements reveal a bimodal distribution of mass densities. The dense fibers have lower resistivities and correspond to the stage III compound identified by X-ray diffraction. Neither resistivity nor density correlate with diameter. Both energy dispersive spectroscopy and mass density data suggest that excess chlorine resides in the intercalated fiber, resulting in a stoichiometry of C4.9n CuCl2.5 (where n is the stage number) for the denser fibers. Finally, thermogravimetric analysis shows a 33 percent loss in mass upon heating to 700C. This loss in mass is attributed to loss of both chlorine and carbon.

Jaworske, D. A.↗
NASA NTRS1990

Hydrogen induced fracture characteristics of single crystal nickel-based superalloys

A stereoscopic method for use with x ray energy dispersive spectroscopy of rough surfaces was adapted and applied to the fracture surfaces single crystals of PWA 1480E to permit rapid orientation determinations of small cleavage planes. The method uses a mathematical treatment of stereo pair photomicrographs to measure the angle between the electron beam and the surface normal. One reference crystal orientation corresponding to the electron beam direction (crystal growth direction) is required to perform this trace analysis. The microstructure of PWA 1480E was characterized before fracture analysis was performed. The fracture behavior of single crystals of the PWA 1480E nickel-based superalloy was studied. The hydrogen-induced fracture behavior of single crystals of the PWA 1480E nickel-based superalloy was also studied. In order to understand the temperature dependence of hydrogen-induced embrittlement, notched single crystals with three different crystal growth orientations near zone axes (100), (110), and (111) were tensile tested at 871 C (1600 F) in both helium and hydrogen atmospheres at 34 MPa. Results and conclusions are given.

Chen, Po-Shou↗
NASA NTRS1989

Properties of Pb(1-x)Bi(x)/Ba2YCu3O(x) composites - Reaction of Ba2YCu3O(x) with Pb and Bi

This paper describes experiments conducted with a purpose of fabricating superconducting composites from Pb, Bi, and Ba2YCu3O(x), together the results of SEM examinations and energy dispersive spectroscopy performed on products. Results showed a limited utility of Pb and Pb(1-x)Bi(x) as matrices for ceramic superconductors. It was found that cold pressing followed by sintering at 200 C resulted in a composite which excluded flux below 90 K but did not show zero electrical resistance until the metal superconducting transition. Processing at 400 or 950 C resulted in oxygen depleted perovskite and/or metal oxides; these materials displayed greatly degraded superconducting properties. Finally, processing at 800 C resulted in high Tc only for composites containing more than 90 wt pct ceramic.

Hepp, A. F.↗
NASA NTRS1991

Mechanisms of ilmenite reduction and their impact on the design of effective reactor systems

One of the first activities at a lunar base could be oxygen recovery from ilmenite (FeTiO3). Oxygen produced from lunar soils could be used to fuel transportation vehicles operating in near-earth space. The first step in developing a suitable reactor system for lunar operation is to determine the mechanisms and rates of oxygen removal from ilmenite. In-situ gravimetric measurements and microscopic examinations were used to determine the hydrogen reduction mechanisms of synthetic ilmenite discs between 823 to 1353 K. A shrinking core reaction model, modified to account for the growth of an iron film on the surface of discs, was capable of predicting experimentally observed conversion-time relationships. The observed reduction mechanism, kinetic rates, and associated activation energy established a base line from which comparisons could be made to improve oxygen yield and removal rates. One proposed technique to improve the rate and extent of oxygen removal was to preoxidize ilmenite. Preoxidation is commonly used during the reduction of ilmenite ores in the iron industry and has been employed for many years to lower operating temperatures and increase reduction rates. This technology could prove beneficial for oxygen production facilities on the Moon as less massive reactor vessels and/or less energy could be associated with a process including preoxidation. X ray diffraction and energy dispersive spectroscopy were utilized to follow the progression of ilmenite oxidation at 1123 and 1140 K and the reduction of pseudobrookite (Fe2TiO5) at 873 and 973 K. Structures formed during the progress of oxidation were related to the system's phase diagrams. Results indicated that after initially producing ilmenite-hematite solutions and rutile (TiO2), pseudobrookite was the end product of oxidation at all temperatures examined (1049 to 1273 K). Initial results from the reduction of pseudobrookite indicate a series of phases are produced including ferropseudobrookite (FeTi2O5), ulvospinel (Fe2TiO4), and ilmenite. Rates of pseudobrookite reduction were typically 50 to 200 times that of ilmenite.

Briggs, R. A.↗
NASA NTRS1991

Development of graphite/copper composites utilizing engineered interfaces

In situ measurements of graphite/copper alloy contact angles were made using the sessile drop method. The interfacial energy values obtained from these measurements were then applied to a model for the fiber matrix interfacial debonding phenomenon found in graphite/copper composites. The formation obtained from the sessile drop tests led to the development of a copper alloy that suitably wets graphite. Characterization of graphite/copper alloy interfaces subjected to elevated temperatures was conducted using Scanning Electron Microscopy, Energy Dispersive Spectroscopy, Auger Electron Spectroscopy, and X Ray Diffraction analyses. These analyses indicated that during sessile drop tests conducted at 1130 C for 1 hour, copper alloys containing greater than 0.98 at pct chromium form continuous reaction layers of approx. 10 microns in thickness. The reaction layers are adherent to the graphite surface. The copper wets the reaction layer to form a contact angle of 60 deg or less. X ray diffraction results indicate that the reaction layer is Cr3C2.

Devincent, Sandra M.↗
NASA NTRS1991

Preliminary studies on NiAl/Nb2Be17 reaction and effectiveness of BeO as an interfacial reaction barrier

The interfacial reaction between NiAl and Nb2Be17 (used as a reinforcement for the alloy) was studied by measuring diffusion bonding of NiAl and Nb2Be17 plates in a hot press under a vacuum of 10 exp -5 atm. It was found that, after 2 hrs of hot pressing at 1373 K, the reaction between NiAl and Nb2Be17 was extensive. A 40 to 50-micron-thick reaction zone consisted of three distinct layers at the NiAl/Nb2Be17 interface: layer A next to Nb2Be17, layer B in the middle, and layer C next to NiAl. Results of analysis of the reaction layers using energy dispersive spectroscopy (EDS) were inconclusive because of the inabiliaty of EDS to detect Be.

Misra, Ajay K.↗
NASA NTRS1992

Long-term corrosion evaluation of stainless steels in Space Shuttle iodinated resin and water

The effects of stainless steel exposure to iodinated water is a concern in developing the Integrated Water System (IWS) for Space Station Freedom. The IWS has a life requirement of 30 years, but the effects of general and localized corrosion over such a long period have not been determined for the candidate materials. In 1978, Umpqua Research Center immersed stainless steel 316L, 321, and 347 specimens in a solution of deionized water and the Space Shuttle microbial check valve resin. In April 1990, the solution was chemically analyzed to determine the level of corrosion formed, and the surface of each specimen was examined with scanning electron microscopy and metallography to determine the extent of general and pitting corrosion. This examination showed that the attack on the stainless steels was negligible and never penetrated past the first grain boundary layer. Of the three alloys, 316L performed the best; however, all three materials proved to be compatible with an aqueous iodine environment. In addition to the specimens exposed to aqueous iodine, a stainless steel specimen (unspecified alloy) was exposed to moist microbial check valve resin and air for a comparable period. This environment allowed contact of the metal to the resin as well as to the iodine vapor. Since the particular stainless steel alloy was not known, energy dispersive spectroscopy was used to determine that this alloy was stainless steel 301. The intergranular corrosion found on the specimen was limited to the first grain boundary layer.

Krohn, Douglas D.↗
NASA NTRS1992

Reaction layer formation at the graphite/copper-chromium alloy interface

Sessile drop tests were used to obtain information about copper chromium alloys that suitably wet graphite. Characterization of graphite/copper-chromium alloy interfaces subjected to elevated temperatures were conducted using scanning electron micrography, energy dispersive spectroscopy, auger electron spectroscopy, and x ray diffraction analyses. These analyses indicate that during sessile drop tests conducted at 1130 C for one hour, copper alloys containing greater than 0.98 percent chromium form continuous reaction layers of approximately 10 micron thickness. The reaction layers adhere to the graphite surface. The copper wets the reaction layer to form a contact angle of 60 degrees or less. X ray diffraction results indicate that the reaction layer is chromium carbide. The kinetics of reaction layer formation were modelled in terms of bulk diffusion mechanisms. Reaction layer thickness is controlled initially by the diffusion of Cr out of Cu alloy and later by the diffusion of C through chromium carbide.

Devincent, Sandra M.↗
NASA NTRS1993

Further analysis of LDEF FRECOPA micrometeoroid remnants

In the Al collectors of experiment A0138-1 of the French Cooperative Payload (FRECOPA) payload, we identified a population of small craters (3-9 microns in diameter) induced by the impacts of micron-sized grains, mainly of extraterrestrial origin. Chemical analyses of the Interplanetary Dust Particle (IDP) remnants were made in the bottoms and on the rims of the craters, in addition to immediate off-rim areas. So far, the compositional investigation of the craters by Energy Dispersive Spectroscopy (EDS) has shown evidence of an extraterrestrial origin for the impacting grains. The systematic presence of C and O in the residues has been reported and may be compared with the existence of particles showing high proportions of biogenic light elements and detected in the close environment of P-Halley comet nucleus (called CHON particles). An analytical protocol has been established in order to extract molecular and possible isotopic information on these grains, a fraction of which could be of cometary origin. Although these very small craters may show crater features that are typical of the larger Long Duration Exposure Facility (LDEF) population (greater than 50 microns), some show unique morphologies that we have not previously observed. Our initial Laser Induced Mass Spectrometry (LIMS) analytical results show strong signals for nitrogen-bearing ions in craters characterized by high C and O contents; they also suggest that carbon contents in some craters could exceed that known for carbonaceous chondrites.

Borg, Janet↗
NASA NTRS1993

Reaction layer formation at the graphite/copper-chromium alloy interface

Sessile drop tests were used to obtain information about copper chromium alloys that suitably wet graphite. Characterization of graphite/copper-chromium alloy interfaces subjected to elevated temperatures were conducted using scanning electron micrography, energy dispersive spectroscopy, Auger electron spectroscopy, and X-ray diffraction analyses. These analyses indicate that during sessile drop tests conducted at 1130 C for one hour, copper alloys containing greater than 0.98 percent chromium form continuous reaction layers of approximately 10 micron thickness. The reaction layers adhere to the graphite surface. The copper wets the reaction layer to form a contact angle of 60 degrees or less. X-ray diffraction results indicate that the reaction layer is chromium carbide. The kinetics of reaction layer formation were modelled in terms of bulk diffusion mechanisms. Reaction layer thickness is controlled initially by the diffusion of Cr out of Cu alloy and later by the diffusion of C through chromium carbide.

Devincent, Sandra M.↗
NASA NTRS1993

Mineralogy of chondritic interplanetary dust particle impact residues from LDEF

A detailed structural and compositional analysis of several impactor residues was performed utilizing transmission electron microscopy, energy dispersive spectroscopy, and electron diffraction. Residues from the interior of several craters in gold surfaces were removed with a tungsten needle, mounted in EMBED-812 epoxy, and ultramicrotomed. The presence in these residues of equilibrated ferromagnesian minerals, recrystallization textures, glass, and melted metal and sulfide bodies decorating grain boundaries is indicative of varying degrees of shock metamorphism in all impact residues we have characterized.

Barrett, R. A.↗
NASA NTRS1993

Carbon analyses of IDP's sectioned in sulfur and supported on beryllium films

Carbon is the only major element in interplanetary dust whose abundance, distribution and chemical state are not well understood. Information about carbon could clarify the relationship between the various classes of IDP's, conventional meteorites, and sources (e.g., comets vs. asteroids). To date, the most reliable estimates of C abundance in Interplanetary Dust Particles (IDP's) have been obtained by analyzing particles on thick-flat Be substrates using thin-window energy-dispersive spectroscopy in the SEM. These estimates of C abundance are valid only if C is homogeneously distributed, because detected C x-rays originate from the outer 0.1 micrometers of the particle. An alternative and potentially more accurate method of measuring C abundances is to analyze multiple thin sections (each less than 0.1 less than 0.1 micrometers thick) of IDP's. These efforts however, have been stymied because of a lack of a suitable non-carbonaceous embedding medium and the availability of C-free conductive substrates. We have embedded and thin-sectioned IDP's in glassy sulfur, and transferred the thin sections to Be support films approximately 25 nm thick. The sections were then analyzed in a 200 KeV analytical TEM. S sublimes rapidly under vacuum in the TEM, leaving non-embedded sections supported on Be. Apart from quantitative C (and O) analyses, S sectioning dramatically expands the range of analytical measurements that can be performed on a single IDP.

Bradley, J. P.↗
NASA NTRS1993

The rate of chemical weathering of pyrite on the surface of Venus

This abstract reports results of an experimental study of the chemical weathering of pyrite (FeS2) under Venus-like conditions. This work, which extends the earlier study by Fegley and Treiman, is part of a long range research program to experimentally measure the rates of thermochemical gas-solid reactions important in the atmospheric-lithospheric sulfur cycle on Venus. The objectives of this research are (1) to measure the kinetics of thermochemical gas-solid reactions responsible for both the production (e.g., anhydrite formation) and destruction (e.g., pyrrhotite oxidation) of sulfur-bearing minerals on the surface of Venus and (2) to incorporate these and other constraints into holistic models of the chemical interactions between the atmosphere and surface of Venus. Experiments were done with single crystal cubes of natural pyrite (Navajun, Logrono, Spain) that were cut and polished into slices of known weight and surface area. The slices were isothermally heated at atmospheric pressure in 99.99 percent CO2 (Coleman Instrument Grade) at either 412 C (685 K) or 465 C (738 K) for time periods up to 10 days. These two isotherms correspond to temperatures at about 6 km and 0 km altitude, respectively, on Venus. The reaction rate was determined by measuring the weight loss of the reacted slices after removal from the furnace. The reaction products were characterized by X-ray diffraction, scanning electron microscopy, and energy dispersive spectroscopy on the SEM.

Fegley, B., Jr.↗
NASA NTRS1994

Penetration of multiple thin films in micrometeorite capture cells

As part of a continuing effort to develop cosmic dust detectors/collectors for use in space, we performed a series of hypervelocity impact experiments on combined sensor/capture-cell assemblies using 10-200-micron-diameter glass projectiles and olivine crystals at velocities of 0.9-14.4 km/s. The design objective of the space-flight instrument is to measure the trajectories of individual particles with sufficient accuracy to permit identification of their parent bodies and to capture enough impactor material to allow chemical and isotopic analyses of samples returned to Earth. Three different multiple-film small-particle capture cell designs (0.1-100-micron-thick Al foils with approx. 10, 100, and 1800 micron spacing) were evaluated for their ability to capture impactor fragments and residue. Their performances were compared to two other types of capture cells, foil covered Ge crystals, and 0.50 and 0.120 g/cu cm aerogels. All capture cells were tested behind multifilm (1.4-6.0-micron-thick) polyvinylidene fluoride (PVDF) velocity/trajectory sensor devices. Several tests were also done without the PVDF sensors for comparison. The results of this study were reported by Simon in a comprehensive report in which the morphology of impacts and impactor residues in various types of capture cells after passage through two PVDF sensor films is discussed. Impactor fragments in selected capture cells from impacts at velocities up to 6.4 km/s were identified using scanning electron microscopy with energy dispersive spectroscopy (SEM/EDS).

Simon, Charles G.↗
NASA NTRS1995

Image and compositional characteristics of the LDEF Big Guy impact crater

A 5.2 mm crater in Al-metal represents the largest found on LDEF. We have examined this crater by field emission scanning electron microscopy (FESEM), energy dispersive spectroscopy (EDS) and time-of-flight/secondary ion mass spectroscopy (TOF-SIMS) in order to determine if there is any evidence of impactor residue. Droplet and dome-shaped columns, along with flow features, are evidence of melting. EDS from the crater cavity and rim show Mg, C, O and variable amounts of Si, in addition to Al. No evidence for a chondritic impactor was found, and it hypothesized that the crater may be the result of impact with space debris.

Bunch, T. E.↗
NASA NTRS1993

Characterization of precipitates in CdTe and Cd(1-x)Zn(x)Te grown by vertical Bridgman-Stockbarger technique

Different polishing solutions were tested for exposing precipitates in CdTe and Cd(0.96)Zn(0.04) single crystals grown by vertical Bridgman-Stockbarger technique. A solution of 5-7% Br2 in methanol and E-solution were both effective. High resolution scanning electron microscopy with energy dispersive spectroscopy (SEM/EDS) was employed to characterize those exposed precipitates. Most of the polyhedral-shaped Te precipitates with a size range from 3 to 20 microns had voids inside. Partially dissolved Te precipitates were observed in CdTe samples that had been annealed in Cd vapor at 700 C for 10 min. Isolated areas mis-oriented from the matrix were observed in CdTe and Cd(0.96)Zn(0.04)Te that had been annealed in Cd vapor at 700 C for 20 and 50 h, respectively. Te precipitate images were recorded with EDS. By SEM/EDS, Cd-rich precipitates were observed in some Cd-annealed CdTe. C and Na impurities were detected in some Te precipitates.

Shen, J.↗
NASA NTRS1997

Electrodeposited CuInSe2 Thin Film Junctions

We have investigated thin films and junctions based on copper indium diselenide (CIS) which have been grown by electrochemical deposition. CIS is a leading candidate for use in polycrystalline thin film photovoltaic solar cells. Electrodeposition is a cost-effective method for producing thin-film CIS. We have produced both p and n type CIS thin films from the same aqueous solution by simply varying the deposition potential. A CIS pn junction was deposited using a step-function potential. Stoichiometry of the single layer films was determined by energy dispersive spectroscopy. Carrier densities of these films increased with deviation from stoichiometry, as determined by the capacitance versus voltage dependence of Schottky contacts. Optical bandgaps for the single layer films as determined by transmission spectroscopy were also found to increase with deviation from stoichiometry. Rectifying current versus voltage characteristics were demonstrated for the Schottky barriers and for the pn junction.

Raffaelle, R. P.↗