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NASA NTRS1976

Adsorption of oxygen on W/100/ - Adsorption kinetics and structure

The adsorption of oxygen on W(100) single-crystal surfaces is studied by Auger electron spectroscopy (AES), flash desorption, low-energy electron diffraction (LEED), and retarding-field work-function measurements. The AES results reveal stepwise changes in the sticking coefficients in the coverage range 0 to 1 and activated adsorption at higher coverages. Upon room-temperature adsorption, a series of complex LEED patterns is observed. In layers adsorbed at 1050 K and cooled to room temperature, the p(2 x 1) structure is the first ordered structure observed. This structure shows a reversible order-disorder transition between 700 and 1000 K and is characterized by a work function which is lower than that of the clean surface. Heating room-temperature adsorbates changes their structure irreversibly. At temperatures below 750 K, some new structures are observed.

Bauer, E.↗

NASA NTRSDate not supplied

Hydrogen Plasma Reduction of Silicates for Lunar Oxygen Liberation

As crewed missions to the moon become closer, the focus on in-situ resource utilization efforts has increased. Since lunar soil has abundant oxygen on the surface of the moon, work has been done to process this resource in an efficient manner. Hydrogen reduction of lunar regolith has emerged as a method of liberating oxygen that can be used for fuel and water production. Traditional reduction techniques require high temperatures and increased complexity when dealing with high amounts of silicates. Plasma can reduce silicates efficiently and thus has become of high interest for use in the lunar highlands where silicates exist in high quantities. NASA’s Kennedy Space Center is exploring the use of low temperature plasmas for the reduction of silicates. This work shows that exposing silicates to a hydrogen plasma produces water. Residual gas analysis and optical emission spectroscopy were used to measure the relative quantities of water vapor production and OH (A-X) emission for hydrogen plasma interactions with lunar highland simulant and silica. X-ray photo-electron spectroscopy and scanning electron microscopy/energy-dispersive X-ray spectroscopy were also used to observe surface modifications to the silicates that reflect the key chemical reactions that occurred. From this data, plasma has emerged as a promising solution to produce oxygen on the lunar surface. *Work supported by NASA's Science Technology Mission Directorate Center Innovation Fund.

R. P. Gott↗

NASA NTRSDate not supplied

Plasma Reduction of Regolith for Oxygen Liberation

Ryan Gott↗

NASA NTRS2001

The X-Ray Spectrometer for Mercury MESSENGER

Mercury is the closest planet to the Sun and because it is so close, it is difficult to study from Earth-based observatories. Its proximity to the Sun has also limited the number of spacecraft to visit this tiny planet to just one, Mariner 10, which flew by Mercury twice in 1974 and once in 1975. Mariner 10 provided a wealth of new information about Mercury, yet much still remains unknown about Mercury's geologic history and the processes that led to its formation. The origin of Mercury's metal-rich composition is just one area of investigation awaiting more and improved data to sort between competing hypotheses. Mercury plays an important role in comparative planetology, and many of the processes that were important during its formation are relevant to the Earth's early history. MESSENGER (Mercury Surface, Space Environment, Geochemistry, and Ranging) is a Discovery mission that has been designed to fly by and orbit Mercury. It will launch in March 2004, flyby Mercury in 2007 and 2008 and enter an elliptical orbit in April 2009. During the one-year orbital phase, a suite of instruments on board the MESSENGER spacecraft will study the exosphere, magnetosphere, surface, and interior of Mercury. One of these instruments will be an X-Ray Spectrometer (XRS) that will measure surface elemental abundances. Remote X-ray spectroscopy has been accomplished before on the Apollo 15 and 16 missions, and more recently on NEAR Shoemaker. The MESSENGER XRS will measure characteristic X-ray emissions induced in the surface of Mercury by the incident solar flux. The Ka lines for the elements Mg, Al, Si, S, Ca, Ti, and Fe will be detected with spatial resolution on the order of 40 km when counting statistics are not a limiting factor. These measurements can be used to obtain quantitative information on elemental composition.

Starr, R. D.↗

NASA NTRS1991

Uranus satellites - Surface properties

The post-Voyager knowledge of the photometric, colorimetric, spectral, and thermal properties of the Uranian satellites is reviewed, focusing on such fundamental physical properties as albedo, color, and surface texture. While albedo variations of at least a factor of 2 exist, color differences are almost absent (Miranda) or subdued (Oberon). In the case of Titania, the strong opposition effect reported by ground-based observers was confirmed by Voyager. Voyager did not observe the opposition parts of the phase curves of the other satellites. Voyager thermal observations of Ariel and Miranda suggest that both have highly porous regoliths, thermophysically similar to those of Jupiter's icy satellites. At the time of the flyby (south pole facing the sun), maximum surface temperatures reached or exceeded 85 K, but nighttime polar temperatures are predicted to drop to 20 to 30 K because each pole spends about 40 yr in darkness. Ground-based spectroscopy identified water ice as an important surface constituent.

Veverka, J.↗

NASA NTRS1985

Aluminum work function: Effect of oxidation, mechanical scraping and ion bombardment

Surface studies have been performed on aluminum polycrystalline surfaces which have been mechanically scraped. Such studies were initiated in order to understand surface effects occurring in tribological processes which involve rubbing surfaces and the effects of adsorption of oxygen. To characterize the surfaces, the following three different experimental approaches have been used: (1) X.P.S. (X-ray photoelectron spectroscopy), in order to check the cleanliness of the surfaces and follow the adsorption and oxidation kinetics; (2) Analysis of the work function changes by following the energy spectra of secondary electrons emitted under low energy electron bombardment; and (3) Analysis of photoemission intensities under U.V. excitation. The reference state being chosen to be the surface cleaned by ion bombardment and exposures to oxygen atmospheres have been shown to lower the work function of clean polycrystalline aluminum by 1.2 eV. The oxygen pressure is found to affect only the kinetics of these experiments. Mechanical scraping has been shown to induce a decrease ( 0.3 eV) in the work function, which could sharply modify the kinetics of adsorption on the surface.

Vinet, P.↗

NASA NTRS1985

Characterization of carbon fibers and fiber-matrix adhesion in composites

The effect of fiber/matrix interactions on the mechanical properties of thermoplastic carbon fiber composites was determined. The experimental approach was a multi-faceted one involving the following areas: characterization of the surface of carbon fibers using X-ray photoelectron spectroscopy (XPS), secondary ion mass spectroscopy (SIMS) and scanning transmission electron microcopy (STEM); determination of the functional groups on carbon fiber surfaces using an elemental tagging scheme - derivatization; determination of the polar and dispersion contribution to the surface energy of carbon fibers by measuring wetting forces in a series of liquids having known polar and dispersion components; and study of the interaction of thermoplastic polymers with carbon surfaces by solution adsorption, STEM and fiber critical length.

Wightman, J. P.↗

NASA NTRS1990

Characterization of hydrogen interactions with the surface of alpha-2 titanium aluminide alloys

The interaction of hydrogen at the surface of alpha-2 titanium aluminide alloys with Nb additions has been investigated with Auger electron spectroscopy (AES) and reflected electron energy loss (REELS) spectroscopy. The hydrogen was either adsorbed onto the alloy surface from the gas phase or it was pre-charged into the alloy forming an alpha-2 hydride. No effect of either adsorbed or absorbed hydrogen was observed in the Auger spectra. A shift in the bulk plasmon loss energy (observed with REELS) was measured for both conditions. The potential significance of these results in relation to hydrogen interactions in this alloy is discussed.

Shanabarger, Mickey R.↗

NASA NTRS1995

The surface properties of fluorinated polyimides exposed to VUV and atomic oxygen

The effect of atomic oxygen flux and VUV radiation alone and in combination on the surface of fluorinated polyimide films was studied using XPS spectroscopy. Exposure of fluorinated polyimides to VUV radiation alone caused no observable damage to the polymer surface, while an atomic oxygen flux resulted in substantial oxidation of the surface. On the other hand, exposure to VUV radiation and atomic oxygen in combination caused extensive oxidation of the polymer surface after only 2 minutes of exposure. The amount of oxidized carbon on the polymer surface indicated that there is aromatic ring opening oxidation. The changes in the O1s/C1s, N1s/C1s, and F1s/C1s ratios suggested that an ablative degradation process is highly favorable. A synergistic effect of VUV radiation in the presence of atomic oxygen is clearly evidenced from the XPS study. The atomic oxygen could be considered as the main factor in the degradation process of fluorinated polyimide films exposed to a low earth orbit environment.

Forsythe, John S.↗

NASA NTRS2008

Development and Optical Testing of the Camera, Hand Lens, and Microscope Probe with Scannable Laser Spectroscopy (CHAMP-SLS)

Conducting high resolution field microscopy with coupled laser spectroscopy that can be used to selectively analyze the surface chemistry of individual pixels in a scene is an enabling capability for next generation robotic and manned spaceflight missions, civil, and military applications. In the laboratory, we use a range of imaging and surface preparation tools that provide us with in-focus images, context imaging for identifying features that we want to investigate at high magnification, and surface-optical coupling that allows us to apply optical spectroscopic analysis techniques for analyzing surface chemistry particularly at high magnifications. The camera, hand lens, and microscope probe with scannable laser spectroscopy (CHAMP-SLS) is an imaging/spectroscopy instrument capable of imaging continuously from infinity down to high resolution microscopy (resolution of approx. 1 micron/pixel in a final camera format), the closer CHAMP-SLS is placed to a feature, the higher the resultant magnification. At hand lens to microscopic magnifications, the imaged scene can be selectively interrogated with point spectroscopic techniques such as Raman spectroscopy, microscopic Laser Induced Breakdown Spectroscopy (micro-LIBS), laser ablation mass-spectrometry, Fluorescence spectroscopy, and/or Reflectance spectroscopy. This paper summarizes the optical design, development, and testing of the CHAMP-SLS optics.

Fluorescence↗

NASA NTRS1979

Improved adherence of sputtered titanium carbide coatings on nickel- and titanium-base alloys

Rene 41 and Ti-6Al-4V alloys were radio frequency sputter coated with titanium carbide by several techniques in order to determine the most effective. Coatings were evaluated in pin-on-disk tests. Surface analysis by X-ray photoelectron spectroscopy was used to relate adherence to interfacial chemistry. For Rene 41, good coating adherence was obtained when a small amount of acetylene was added to the sputtering plasma. The acetylene carburized the alloy surface and resulted in better bonding to the TiC coating. For Ti-6Al-4V, the best adherence and wear protection was obtained when a pure titanium interlayer was used between the coating and the alloy. The interlayer is thought to prevent the formation of a brittle, fracture-prone, aluminum oxide layer.

Wheeler, D. R.↗

NASA NTRS1979

Metal-dielectric interactions

There is a wide variety of situations wherein metals are in solid state contact with dielectric materials. The paper reviews some of the factors that influence solid state interactions for metals in contact with dielectric surfaces. Since surfaces play an important part in these reactions, the use of analytical tools in characterizing surfaces is discussed. Adhesion, friction, and wear are utilized as indicators of the nature of interfacial bonding between metals and dielectrics can be effectively determined with adhesion and friction force measurements. Films present on the surface, such as oxygen or water vapor, markedly alter adhesive bond strength which in turn affects friction force and interfacial fracture when attempts are made to separate the contact regions. Analytical surface tools such as the field ion microscope, Auger emission spectroscopy, and X-ray photoelectron spectroscopy are very effective in providing insight into the effect of contact on the surfaces of metals and dielectrics.

Buckley, D. H.↗

NASA NTRS1983

Surface characteristics of metallic glass spheres of Au(55)Pb(22.5)Sb(22.5)

It is pointed out that the production of metallic glasses of high atomic number is currently of considerable importance for inertial confinement fusion (ICF) target applications. In connection with the present investigation, spherules of the alloy Au(55)Pb(22.5)Sb(22.5) were produced. Metallic glass was formed on solidification. With the aid of X-ray diffraction studies, it was established that the spheres were completely amorphous. A near-surface phase separation on spheres of the metallic glass could be observed. Energy dispersive spectroscopy (EDS) measurements showed that the average composition of the surface differed from that of the bulk.

Lee, M. C.↗

NASA NTRS1976

Effect of adsorbed films on friction of Al2O3-metal systems

The kinetic friction of polycrystalline Al2O3 sliding on Cu, Ni, and Fe in ultrahigh vacuum was studied as a function of the surface chemistry of the metal. Clean metal surfaces were exposed to O2, Cl2, C2H4, and C2H3Cl, and the change in friction due to the adsorbed species was observed. Auger electron spectroscopy assessed the elemental composition of the metal surface. It was found that the systems exposed to Cl2 exhibited low friction, interpreted as the van der Waals force between the Al2O3 and metal chloride. The generation of metal oxide by oxygen exposures resulted in an increase in friction, interpreted as due to strong interfacial bonds established by reaction of metal oxide with Al2O3 to form the complex oxide (spinel). The only effect of C2H4 was to increase the friction of the Fe system, but C2H3Cl exposures decreases friction in both Ni and Fe systems, indicating the dominance of the chlorine over the ethylene complex on the surface

Pepper, S. V.↗

NASA NTRS1975

Wear and interfacial transport of material

Bonding across the interface for two solids in contact and the subsequent transfer of material from one surface to another is a direct result of the interfacial bonds being stronger than the cohesive bonds in either of the two solids. Surface tools such as LEED, Auger emission spectroscopy, field ion microscopy, and the atom probe are used to examine adhesive contacts and to determine the direction, nature, quantity of material transfer and properties of the solids which effect transfer and wear. The electronic nature, cohesive binding energies, surface structure, lattice disregistry and distribution of species in surface layers are all found to effect adhesion and transfer or transport for clean surfaces in solid state contact. The influence of adsorbed and reacted surface films from fractions of a monolayer to multilayer reactive films are considered. It is shown that even fractions of a monolayer of surface active species such as oxygen and sulfur can markedly inhibit adhesion and transport.

Buckley, D. H.↗

NASA NTRS1978

X-ray photoelectron spectroscopic study of surface chemistry of dibenzyl disulfide on steel under mild and severe wear conditions

X-ray photoelectron spectroscopy was used to characterize the chemical composition of 304 stainless steel surfaces run in oil containing dibenzyl disulfide under both mild and severe wear conditions. In severe wear a sulfide was formed at the expense of the normal oxide. This was due to either chemical attack on the oxide or reaction with clean metal exposed by the wear process. In the mild wear scars there was no evidence of either sulfide or mercaptide. The oxide, however, was approximately twice as thick as the normal oxide on an unworn surface. The change in surface chemistry was primarily a function of wear rate rather than load.

Wheeler, D. R.↗

NASA NTRS1986

Hydrazine reduction of transition metal oxides - In situ characterization using X-ray photoelectron spectroscopy

The transition metal oxides (TMOs) V2O5, FeO3, Co3O4, NiO, CuO, and ZnO were exposed to hydrazine at various pressures. The metallic surfaces were surveyed by in situ X-ray photoelectron spectroscopy to determine the irrelative rate of reduction by hydrazine. The most easily reducible oxide, CuO, could be reduced to the metallic state at room temperature and 10 to the -6th torr. The reaction is first order with respect to CuO, with an activation energy of about 35 kJ/mol. Two types of adsorption were seen to occur at 295 K: (1) a reversible component in which the measured N:Cu ratio increased to 0.60 at hydrazine pressures up to 0.5 torr, and (2) an irreversible component, with a N:Cu ratio of 0.28, which could not be removed by extended vacuum pumping. The results of this study are useful for the identification of TMO's that can be used as solid neatallizers of hydrazine spills, and for the preparation of metal surfaces for electroplating and evaporative thin-film coating.

Littrell, D. M.↗

NASA NTRS1978

Planetary gamma-ray spectroscopy

The measured intensities of certain gamma rays of specific energies escaping from a planetary surface can be used to determine the abundances of a number of elements. The fluxes of the more intense gamma-ray lines emitted from 32 elements were calculated using current nuclear data and existing models for the source processes. The source strengths for neutron-capture reactions were modified from those previously used. The fluxes emitted form a surface of average lunar composition are reported for 292 gamma-ray lines. These theoretical fluxes were used elsewhere to convert the data from the Apollo gamma-ray spectrometers to elemental abundances and can be used with measurements from future missions to map the concentrations of a number of elements over a planet's surface. Detection sensitivities for these elements are examined and applications of gamma-ray spectroscopy for future orbiters to Mars and other solar-system objects are discussed.

Reedy, R. C.↗