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NASA NTRS1982

An unusual layered mineral in chondrules and aggregates of the Allende carbonaceous chondrite

Transmission electron microscopy (TEM), scanning electron microscopy (SEM), and energy dispersive X ray (EDS) and electron energy loss (EELS) spectroscopy examinations of the microstructures and phase relationships of minerals in opaque spherules in the Allende chondrules and aggregates are reported. The studies were carried out on petrographic thin sections which were ion-thinned. A significant metasomatic effect was observed in a highly oxidizing condition of a later cooled stage. An unusually layered Fe-, Ni-, and O-rich mineral related to serpentine was found to occur in the opaque specimen, and was judged to occur by alteration of olivine. It is noted that low temperature and a hydrous condition would have been required for the formation of the serpentine in the spherules, the first observed in Allende. It is suggested that the aqueous conditions occurred before the final stage of the meteorite formation, and proceeded in a nonterrestrial manner.

Tomeoka, K.↗

NASA NTRS1983

Surface analysis of graphite fiber reinforced polyimide composites

Several techniques have been used to establish the effect of different surface pretreatments on graphite-polyimide composites. Composites were prepared from Celion 6000 graphite fibers and the polyimide LARC-160. Pretreatments included mechanical abrasion, chemical etching and light irradiation. Scanning electron microscopy (SEM) and X-ray photoelectron spectroscopy (XPS) were used in the analysis. Contact angle of five different liquids of varying surface tensions were measured on the composites. SEM results showed polymer-rich peaks and polymer-poor valleys conforming to the pattern of the release cloth used durng fabrication. Mechanically treated and light irradiated samples showed varying degrees of polymer peak removal, with some degradation down to the graphite fibers. Minimal changes in surface topography were observed on concentrations of surface fluorine even after pretreatment. The light irradiation pretreatment was most effective at reducing surface fluorine concentrations whereas chemical pretreatment was the least effective. Critical surface tensions correlated directly with the surface fluorine to carbon ratios as calculated from XPS.

Messick, D. L.↗

NASA NTRS1984

Melting, ablation, and vapor phase condensation during atmospheric passage of the Bjurbole meteorite

A detailed study of the Bjurbole fusion crust using scanning electron microscopy (SEM) and energy dispersive analysis (EDS) shows that filamentary crystals and ablation spheres may form on the meteoroid surface. Filamentary crystals, hollow spheres, and porous regions of the surface point to a period of intense vapor phase activity during atmospheric passage. Filamentary crystals can be divided into three categories on the basis of bulk composition and morphology. Two types of filamentary crystals are vapor phase condensation products formed during atmospheric entry of the meteoroid. The other type forms by the interaction of seawater with the fusion surface. The density and composition of ablation spheres varies with the flight orientation of the meteorite. The size range and composition of iron-nickel spheres on the surface of Bjurbole are similar to spheres collected in the stratosphere. A comparison of stratospheric dust collections with meteorite surfaces may provide further insight into the mechanisms of meteoroid entry into planetary atmospheres.

Rietmeijer, F. J. M.↗

NASA NTRS1984

Nitriding of titanium and its alloys by N2, NH3 or mixtures of N2 + H2 in a dc arc plasma at low pressures ( or = to torr)

The dc glow discharges in different gas mixtures of Ar + N2, Ar + NH3 or Ar + N2 + H2 result in the surface nitriding of Ti metal and its alloy (Ti6Al4V). Various gas mixtures were used in order to establish the main active species governing the nitriding process, i.e., N, N2, NH, or NH2 as excited or ionized particles. The dc discharge was sampled and analyzed by quadruple mass spectrometry (QPMS) and optical emission spectroscopy (OES), and the nitrided samples were analyzed by scanning electron microscopy (SEM) with an EDAX attachment, microhardness, and Fourier transform infrared reflectance spectrometry (FTIR). It was found that the excited and ionized nitrogen and hydrogen atoms are the main species responsible for the nitriding process in a dc glow discharge.

Avni, R.↗

NASA NTRS1984

Effect of Interfacial characteristics of metal clad polymeric substrates on electrical high frequency interconnection performance

Etched metallic conductor lines on metal clad polymeric substrates are used for electronic component interconnections. Significant signal losses are observed for microstrip conductor lines used for interconnecting high frequency devices. At these frequencies, the electronic signal travels closer to the metal-polymer interface due to the skin effect. Copper-teflon interfaces were characterized by scanning electron microscopy (SEM) and Auger electron spectroscopy (AES) to determine the interfacial properties. Data relating roughness of the copper film to signal losses was compared to theory. Films used to enhance adhesion are found, to contribute to these losses.

Bhasin, K. B.↗

NASA NTRS1985

Survey of probable micrometer-sized Earth-orbital debris fragments in the NASA-JSC cosmic dust sample collection

A program to collect extraterrestrial dust samples from the stratosphere using impactors mounted on NASA U-2 and WB-57F aircraft is discussed. Sample collection, preparation, and analysis techniques are described and the particle types found are reviewed. Preliminary examination of the particles indicates that they represent not only extraterrestrial material, but some fraction of terrestrial contamination from both natural and manmade sources. This examination involves a combination of optical microscopy, scanning electron microscopy (SEM) and qualitative bulk elemental analysis using an energy-dispersive X-ray spectrometer (EDS) to characterize each particle. The cosmic dust collection contains samples of at least three classes of material that may present some hazard to extended spacecraft operations in near-Earth orbit: (1) micrometeorites/cosmic dust, (2) aluminum oxide spheres, and (3) alloy spherules and fragments.

Clanton, U. S.↗

NASA NTRS1985

Fracture surface analysis in composite and titanium bonding: Part 1: Titanium bonding

Fractured lap shear Ti 6-4 adherends bonded with polyphenyquinoxaline (PPQ) and polysulfone were analyzed. The effects of adherend pretreatment, stress level, thermal aging, anodizing voltage, and modified adhesive of Ti 6-4 adherend bonded with PPQ on lap shear strength were studied. The effect of adherend pretreatment on lap shear strength was investigated for PS samples. Results of scanning electron microscopy (SEM) and X-ray photoelectron spectroscopy (XPS) used to study the surface topography and surface composition are also discussed.

Sanderson, K. A.↗

NASA NTRS1983

Fungi and bacteria involved in desert varnish formation

Desert varnish is a coating of ferromanganese oxides and clays that develops on rock surfaces in arid to semi-arid regions. Active respiration but not photosynthesis was detected on varnished rock surfaces from the Sonoran Desert. Light microscopy, scanning electron microscopy (SEM) and transmission electron microscopy (TEM) observations, and cultivation experiments indicate that both fungi, primarily dematiaceous hyphomycetes, and bacteria are found on and within desert varnish coatings from the arid regions studied. Some fungi grow as microcolonial fungi (MCF) on rocks, and microscopic observations suggest MCF become incorporated in the varnish coating. SEM-EDAX (energy dispersive X-ray systems) analyses indicate the MCF contain 3 of the characteristic elements of varnish: iron, aluminum, and silicon. In some locations, MCF are also enriched in manganese relative to the rock substratum. Furthermore, some of the dematiaceous hyphomycetes that have been cultivated are able to oxidize manganese under laboratory conditions. It is possible that manganese-oxidizing bacteria, which are found in varnish, also play an important role in varnish formation.

Taylor-George, S.↗

NASA NTRS1986

Meteoritic ablation and fusion spherules in Antarctic ice

In the course of two Antarctic expeditions in 1980/1981 and 1982/1983 approximately 4 metric tons of documented ice samples were collected from the Atka Bay Ice Shelf, Antarctica, and subsequently shipped for cosmic dust studies. After filtration of the melt water, approximately 700 Antarctic spherules (AAS) in the size range of 5 to 500 microns were handpicked from the filter residue under optical microscopes. For the chemical investigation of single dust grains the following techniques were applied: scanning electron microscopy (SEM), X-ray analysis (EDAX), instrumental neutron activation analysis (INAA), laser microprobe mass analysis (LAMMA), and accelerator mass spectroscopy (AMS). For more than 95% of the total mass the bulk and trace elements were determined in single grain analyses using EDAX, INAA, and LAMMA. The element pattern of the dust particles was compared with that of typical terrestrial material and meteoritic matter. The majority of the spherules exhibited elemental compositions compatible with meteoritic element patterns.

Thiel, K.↗

NASA NTRS1984

Effects of surface chemistry on hot corrosion life

Hot corrosion life prediction methodology based on a combination of laboratory test data and field service turbine components, which show evidence of hot corrosion, were examined. Components were evaluated by optical metallography, scanning electron microscopy (SEM), and electron micropulse (EMP) examination.

Fryxell, R. E.↗

NASA NTRS1988

In situ fatigue loading stage inside scanning electron microscope

A fatigue loading stage inside a scanning electron microscopy (SEM) was developed. The stage allows dynamic and static high-magnification and high-resolution viewing of the fatigue crack initiation and crack propagation processes. The loading stage is controlled by a closed-loop servohydraulic system. Maximum load is 1000 lb (4450 N) with test frequencies ranging up to 30 Hz. The stage accommodates specimens up to 2 inches (50 mm) in length and tolerates substantial specimen translation to view the propagating crack. At room temperature, acceptable working resolution is obtainable for magnifications ranging up to 10,000X. The system is equipped with a high-temperature setup designed for temperatures up to 2000 F (1100 C). The signal can be videotaped for further analysis of the pertinent fatigue damage mechanisms. The design allows for quick and easy interchange and conversion of the SEM from a loading stage configuration to its normal operational configuration and vice versa. Tests are performed entirely in the in-situ mode. In contrast to other designs, the NASA design has greatly extended the life of the loading stage by not exposing the bellows to cyclic loading. The loading stage was used to investigate the fatigue crack growth mechanisms in the (100)-oriented PWA 1480 single-crystal, nickel-based supperalloy. The high-magnification observations revealed the details of the crack growth processes.

Telesman, Jack↗

NASA NTRS1987

A comparative review of optical surface contamination assessment techniques

This paper will review the relative sensitivities and practicalities of the common surface analytical methods that are used to detect and identify unwelcome adsorbants on optical surfaces. The compared methods include visual inspection, simple reflectometry and transmissiometry, ellipsometry, infrared absorption and attenuated total reflectance spectroscopy (ATR), Auger electron spectroscopy (AES), scanning electron microscopy (SEM), secondary ion mass spectrometry (SIMS), and mass accretion determined by quartz crystal microbalance (QCM). The discussion is biased toward those methods that apply optical thin film analytical techniques to spacecraft optical contamination problems. Examples are cited from both ground based and in-orbit experiments.

Heaney, James B.↗

NASA NTRS1988

Crystallization kinetics of BaO-Al2O3-SiO2 glasses

Barium aluminosilicate glasses are being investigated as matrix materials in high-temperature ceramic composites for structural applications. Kinetics of crystallization of two refractory glass compositions in the barium aluminosilicate system were studied by differential thermal analysis (DTA), X-ray diffraction (XRD), and scanning electron microscopy (SEM). From variable heating rate DTA, the crystallization activation energies for glass compositions (wt percent) 10BaO-38Al2O3-51SiO2-1MoO3 (glass A) and 39BaO-25Al2O3-35SiO2-1MoO3 (glass B) were determined to be 553 and 558 kJ/mol, respectively. On thermal treatment, the crystalline phases in glasses A and B were identified as mullite (3Al2O3-2SiO2) and hexacelsian (BaO-Al2O3-2SiO2), respectively. Hexacelsian is a high-temperature polymorph which is metastable below 1590 C. It undergoes structural transformation into the orthorhombic form at approximately 300 C accompanied by a large volume change which is undesirable for structural applications. A process needs to be developed where stable monoclinic celsian, rather than hexacelsian, precipitates out as the crystal phase in glass B.

Bansal, Narottam P.↗

NASA NTRS1989

Chemical profiling of silicon nitride structures

X ray photoelectron spectroscopy (XPS), spectroscopic ellipsometry (SE), and scanning electron microscopy (SEM) were used to study structural and chemical inhomogeneities in several electronic materials and device structures of relevance to radiation hard electronics. The systems studied include metal nitride oxide semiconductor (MNOS) structures, silicon oxynitride (SiO(x)N(y)) formed by the thermal nitridation of SiO2, and semiconductor on insulator (SOI) structures. Studies of MNOS structures suggest that the effect of H2 annealing is to make the Si3N4/SiO2 interface less abrupt by causing interdiffusion of silanol and silamine groups with subsequent oxynitride formation. Another effect of the annealing appears to be to relieve the strain at the SiO2/Si interface.

Vasquez, R. P.↗

NASA NTRS1989

Liquid oxygen LOX compatibility evaluations of aluminum lithium (Al-Li) alloys: Investigation of the Alcoa 2090 and MMC weldalite 049 alloys

The behavior of liquid oxygen (LOX) compatibility of aluminum lithium (Al-Li) alloys is investigated. Alloy systems of Alcoa 2090, vintages 1 to 3, and of Martin Marietta Corporation (MMC) Weldalite 049 were evaluated for their behavior related to the LOX compatibility employing liquid oxygen impact test conditions under ambient pressures and up to 1000 psi. The developments of these aluminum lithium alloys are of critical and significant interest because of their lower densities and higher specific strengths and improved mechanical properties at cryogenic temperatures. Of the different LOX impact tests carried out at the Marshall Space Flight Center (MSFC), it is seen that in certain test conditions at higher pressures, not all Al-Li alloys are LOX compatible. In case of any reactivity, it appears that lithium makes the material more sensitive at grain boundaries due to microstructural inhomogeneities and associated precipitate free zones (PFZ). The objectives were to identify and rationalize the microstructural mechanisms that could be relaxed to LOX compatibility behavior of the alloy system in consideration. The LOX compatibility behavior of Al-Li 2090 and Weldalite 049 is analyzed in detail using microstructural characterization techniques with light optical metallography, scanning electron microscopy (SEM), electron microprobe analysis, and surface studies using secondary ion mass spectrometry (SIMS), electron spectroscopy in chemical analysis (ESCA) and Auger electron spectroscopy (AES). Differences in the behavior of these aluminum lithium alloys are assessed and related to their chemistry, heat treatment conditions, and microstructural effects.

Diwan, Ravinder M.↗

NASA NTRS1989

Crystallization kinetics of BaO-Al2O3-SiO2 glasses

Bansal, Narottam P.↗

NASA NTRS1990

Reaction zone microstructure in a Ti3Al + Nb/SiC composite

A composite of Ti-25Al-13Nb (atomic percent) matrix with a continuous SiC fiber (SCS-6) reinforcement was fabricated by hot pressing powder cloths and mats of fiber. The fiber/matrix reaction zone was studied using scanning electron microscopy (SEM) and transmission electron microscopy/analytical electron microscopy (TEM/AEM) techniques. The extent of reaction was determined, phases were identified, and solute partitioning among the phases was determined. It was found that the matrix had reacted only with a portion of the carbon-rich outer layer of the SCS-6 fiber. The reaction zone contained two concentric zones which are distinguished by the presence of different carbide phases. Both zones contained a hexagonal Si-bearing phase, and one of the zones also contained some fine scattered porosity. The results are discussed with reference to available phase equilibria data.

Baumann, S. F.↗

NASA NTRS1990

Study of diamond film growth and properties

The objective was to study diamond film growth and its properties in order to enhance the laser damage threshold of substrate materials. Calculations were performed to evaluate laser induced thermal stress parameter, R(sub T) of diamond. It is found that diamond has several orders of magnitude higher in value for R(sub T) compared to other materials. Thus, the laser induced damage threshold (LIDT) of diamond is much higher. Diamond films were grown using a microwave plasma enhanced chemical vapor deposition (MPECVD) system at various conditions of gas composition, pressure, temperature, and substrate materials. A 0.5 percent CH4 in H2 at 20 torr were ideal conditions for growing of high quality diamond films on substrates maintained at 900 C. The diamond films were polycrystalline which were characterized by scanning electron microscopy (SEM) and Raman scattering spectroscopy. The top surface of the growing film is always rough due to the facets of polycrystalline film while the back surface of the film replicates the substrate surface. An analytical model based on two dimensional periodic heat flow was developed to calculate the effective in-plane (face parallel) diffusivity of a two layer system. The effective diffusivity of diamond/silicon samples was measured using a laser pulse technique. The thermal conductivity of the films was measured to be 13.5 W/cm K, which is better than that of a type Ia natural diamond. Laser induced damage experiments were performed on bare Si substrates, diamond film coated Si, and diamond film windows. Significant improvements in the LIDT were obtained for diamond film coated Si compared to the bare Si.

Albin, Sacharial↗