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Results for “X-ray adsorption spectroscopy”

Search indexed NASA NTRS and DOE OSTI research on propulsion, heat transfer, battery materials and energy systems. Follow report and document links to the original sources.

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At least 19 records
All sourcesNASA NTRSDOE OSTI
NASA NTRS1983

Ion bombardment and adsorption studies on ilmenite (FeTiO3) by X-ray photoelectron spectroscopy

The effects of 5 KeV argon and oxygen ion bombardment on FeTiO3 (ilmenite) at low temperatures have been studied using X-ray photoelectron spectroscopy (XPS). Also, using this same technique, the adsorption of O2, NO, N2O, and CO at 300 K and the adsorption of O2 and D2O at 150K have been studied. Argon and oxygen ion bombardment of ilmenite have confirmed earlier studies on metal oxides that argon ions generally reduce the anion species while oxygen ions generally oxidize the anion species. The two iron states involved were Fe sup +2 and Fe sup O. The reduction of Ti sup +4 was not verified although a significant shift in the Ti(2p1,3) binding energies toward the metallic state was observed after oxygen ion bombardment at low temperatures. At temperatures above 150K, O2 adsorbs dissociatively on ilmenite while D2O adsorbs molecularly below 170K. Above 300 K No, N2O, and CO do not appear to adsorb dissociatively. Low temperature adsorption of D2O was found to be inhibited by predosing the ilmenite with O2.

Schulze, P. D.↗
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

XPS studies of water and oxygen on iron-sputtered natural ilmenite

The adsorption of D2O and O2 on polycrystalline FeTiO3 (natural ilmenite) has been studied by X-ray photoelectron spectroscopy. Oxygen was found to absorb reactively with Fe(0) on Ar(+)-sputtered surfaces at and above 150 K while D2O was found to adsorb molecularly or in ice layers below 170 K on both Ar(+) and O2(+) ion-bombarded ilmenite. The D2O desorbs at 170 K with either the formation of an OD complex or a strongly bound molecular layer of water.

Schulze, P. D.↗
NASA NTRS1983

Interaction of hydrogen chloride and water with oxide surfaces. III - Titanium dioxide

The adsorption of hydrogen chloride and water vapors on five TiO2 powders in both the anatase and rutile crystalline forms was studied as a function of temperature, pressure, and outgas conditions. The adsorbents were characterized utilizing X-ray powder diffraction, scanning electron microscopy, surface area analysis, indicator method, microelectrophoresis, XPS, and infrared spectroscopy. It was found that both outgas temperature and adsorption temperature influenced the adsorption of water vapor on TiO2, while water vapor adsorption on TiO2 was completely reversible. It is argued that the number of hydroxyl groups present on the surface determines the adsorption capacity of water on the different titanium dioxides. It was found that heats of immersion in water were affected significantly by outgas temperature. Hydrogen chloride adsorption isotherms at 30 C measured on TiO2 after outgassing at 100-400 C showed that a part of the total HCl adsorbed was irreversibly adsorbed. The highest HCl adsorption capacity per unit area was exhibited by anatase, while pure rutile exhibited the lowest adsorption capacity.

Siriwardane, R. V.↗
NASA NTRS1987

Use of hydrophilic polymer coatings for control of electroosmosis and protein adsorption

The purpose of this project was to examine the utility of polyethylene glycol (PEG) and dextran coatings for control of electroosmosis and protein adsorption; electroosmosis is an important, deleterious process affecting electrophoretic separations, and protein adsorption is a factor which needs to be controlled during protein crystal growth to avoid multiple nucleation sites. Performance of the project required use of X-ray photoelectron spectroscopy to refine previously developed synthetic methods. The results of this spectroscopic examination are reported. Measurements of electroosmotic mobility of charged particles in appropriately coated capillaries reveals that a new, one-step route to coating capillaries gives a surface in which electroosmosis is dramatically reduced. Similarly, both PEG and dextran coatings were shown by protein adsorption measurements to be highly effective at reducing protein adsorption on solid surfaces. These results should have impact on future low-g electrophoretic and protein crystal growth experiments.

Harris, J. Milton↗
NASA NTRS1978

Interaction of hydrogen chloride with alumina

The influence of temperature, pressure, and outgas conditions on the absorption of hydrogen chloride and water vapor on both alpha and gamma alumina was studied. Characterization of the adsorbents was performed using X-ray powder diffraction, scanning electron microscopy (SEM), low temperature nitrogen adsorption desorption measurements, BET nitrogen surface area measurements and electron spectroscopy for chemical analysis (ESCA). Water vapor adsorption isotherms at 30, 40, and 50 C were measured on alpha and gamma alumina after outgassing at 80, 200, and 400 C. Both outgas temperature and adsorption temperature influenced the adsorption of water vapor on the aluminas. The water vapor adsorption was completely reversible. Alpha alumina absorbed more water per unit area than gamma alumina. Differences in the adsorption capacity for water vapor of the two aluminas were explained on the basis of ideal surface models of alpha and gamma alumina. Isosteric heats of adsorption for water vapor on the aluminas were determined over a limited range of surface coverage.

Bailey, R. R.↗
NASA NTRS1983

The adsorption and thermal decomposition of tricresylphosphate (TCP) on iron and gold

Because tricresyl-phosphate (TCP) is a common antiwear additive in lubricants, there is great interest in its interactions with metal substrates. The TCP was allowed to adsorb on polycrystalline iron and gold at room temperature. X-ray photoelectron spectroscopy (XPS) was used to analyze the adsorbed species. The substrate was then heated in steps to 330 C, and the changes in the adsorbate were analyzed after each step. On both substrates saturation adsorption occurred at about one monolayer, but the sticking coefficient was less on gold than on iron. Comparison of the XPS spectra of TCP on each substrate with the spectrum from condensed TCP indicated nondissociative adsorption on gold, possibly by dipole-induced dipole interaction. On iron, there was apparently additional interaction between the substrate and the tolyl groups on the TCP molecule. TCP began to desorb molecularly from gold as soon as the gold was heated above room temperature. The desorption was complete by 200 C. However, when the iron substrate was heated, TCP did not desorb but decomposed between 150 and 250 C.

Wheeler, D. R.↗
NASA NTRS1992

Studies of the kinetics and mechanisms of perfluoroether reactions on iron and oxidized iron surfaces

Polymeric perfluoroalkylethers are being considered for use as lubricants in high temperature applications, but have been observed to catalytically decompose in the presence of metals. X-ray photoelectron spectroscopy (XPS) and temperature programmed desorption (TPD) were used to explore the decomposition of three model fluorinated ethers on clean polycrystalline iron surfaces and iron surfaces chemically modified with oxygen. Low temperature adsorption of the model fluorinated ethers on the clean, oxygen modified and oxidized iron surfaces was molecular. Thermally activated defluorination of the three model compounds was observed on the clean iron surface at remarkably low temperatures, 155 K and below, with formation of iron fluoride. Preferential C-F bond scission occurred at the terminal fluoromethoxy, CF3O, of perfluoro-1-methoxy-2-ethoxy ethane and perfluoro-1-methoxy-2-ethoxy propane and at CF3/CF2O of perfluoro-1,3-diethoxy propane. The reactivity of the clean iron toward perfluoroalkylether decomposition when compared to other metals is due to the strength of the iron fluoride bond and the strong electron donating ability of the metallic iron. Chemisorption of an oxygen overlayer lowered the reactivity of the iron surface to the adsorption and decomposition of the three model fluorinated ethers by blocking active sites on the metal surface. Incomplete coverage of the iron surface with chemisorbed oxygen results in a reaction which resembles the defluorination reaction observed on the clean iron surface. Perfluoro-1-methoxy-2-ethoxy ethane reacts on the oxidized iron surface at 138 K, through a Lewis acid assisted cleavage of the carbon oxygen bond, with preferential attack at the terminal fluoromethoxy, CF3O. The oxidized iron surface did not passivate, but became more reactive with time. Perfluoro-1-methoxy-2-ethoxy propane and perfluoro-1,3-diethoxy propane desorbed prior to the observation of decomposition on the oxidized iron surface.

Napier, Mary E.↗
NASA NTRS2001

The Effect of O2, H2O, and N2 on the Fatigue Crack Growth Behavior of an Alpha + Beta Titanium Alloy at 24 C and 177 C

To study the effects of atmospheric species on the fatigue crack growth behavior of an a+B titanium alloy (Ti 6-2-2-2-2) at room temperature and 177 C, fatigue tests were performed in laboratory air, ultrahigh vacuum, and high purity water vapor, oxygen, nitrogen and helium at various partial pressures. Accelerated fatigue crack growth rates in laboratory air compared to ultrahigh vacuum are linked to the damaging effects of both water vapor and oxygen. Observations of the fatigue crack growth behavior in ultrahigh purity environments, along with surface film analysis using X-ray photoelectron spectroscopy (XPS), suggest that multiple crack-tip processes govern the damaging effects of air. Three possible mechanisms are proposed: 1) at low pressure (less than 10(exp -1) Pa), accelerated da/dN is likely due to monolayer adsorption on crack-tip surfaces presumably resulting in decreased bond strengths at the fatigue crack tip, 2) for pressures greater than 10(exp -1) Pa, accelerated da/dN in oxygen may result from oxidation at the crack tip limiting reversible slip, and 3) in water vapor, absorption of atomic hydrogen at the reactive crack tip resulting in process zone embrittlement.

Smith, Stephen W.↗
NASA NTRS1985

Size and shape dependence of CO adsorption sites on sapphire supported Fe microcrystals

The surface structure and stoichiometry of alumina substrates, as well as the size, growth characteristics, and shape of Fe deposits on sapphire substrates have been investigated by low energy electron diffraction (LEED), Auger electron spectroscopy, electron energy loss spectroscopy, and X-ray photoemission spectroscopy (XPS), as well as work function measurements, in conjunction with transition electron microscopy observations. The substrates used in this work were the following: (1) new, clean Al2O3; (2) same surface amorphized by Ar ion bombardment; (3) same surface regenerated by 650 C annealing; (4) amorphous alumina films on Ta slab; and (5) polycrystal alumina films, obtained by heating amorphous films to 600 C. Substrate cleaning was found to be most effective in producing a reproducible surface upon oxygen RF plasma treatment. The Fe nucleation and growth process was found to depend strongly on the type of substrate surface and deposition conditions. Ar ion bombardment under beam flooding, and subsequent annealing at 650 C was found an effective means to restore the original Al2O3 (1102) surface for renewed Fe deposition.

Papageorgopoulos, C.↗
NASA NTRS1979

Characterization of the adsorption of water vapor and chlorine on microcrystalline silica

The characterization of water adsorption on silica is necessary to an understanding of how hydrogen chloride interacts with silica. The adsorption as a function of outgas temperatures of silica and as a function of the isotherm temperature was studied. Characterization of the silica structure by infrared analysis, X-ray diffraction and differential scanning calorimetry, surface area determinations, characterization of the sample surface by electron spectroscopy for chemical analysis (ESCA), and determinations of the heat of immersion in water of silica were investigated. The silica with a scanning electron microscope was examined.

Skiles, J. A.↗
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 NTRS1990

The effect of Sr and Bi on the Si(100) surface oxidation - Auger electron spectroscopy, low energy electron diffraction, and X-ray photoelectron spectroscopy study

The effect of Sr and Bi on the oxidation of the Si(100) surface has been studied by Auger electron spectroscopy, low electron diffraction, and X-ray photoelectron spectroscopy. A dramatic enhancement, by a factor of 10, of the Si oxidation has been observed for Si(100) with a Sr overlayer. The SR-enhanced Si oxidation has been studied as a function of O2 exposure and Sr coverage. In contrast to the oxidation promotion of Sr on Si, it has been also observed that a Bi overlayer on Si(100) reduced Si oxidation significantly. Sr adsorption on the Si(100) with a Bi overlayer enhances Si oxidation only at Sr coverage of greater than 0.3 ML.

Fan, W. C.↗
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 NTRS1993

Ordered organic thin films self-assembled from the vapor phase

Organic films self-assembled from a liquid phase, as in Langmuir-Blodgett or adsorption from solution, have received much attention in the past decade as techniques to achieve highly oriented-ordered polymeric thin films. Many organic compounds including some of the same fatty acids have been vapor deposited as well. However, organic pigments and dyes comprise a major class of important materials which have very low solubilities yet excellent thermal stabilities, making them ideally suited for film deposition from the vapor phase. Surprisingly, such molecular systems exhibit a significant propensity to self order, a high sensitivity to deposition parameters, and a range of microstructural forms that cannot be duplicated by the less energetic mechanisms associated with solution adsorption processes. Molecular solids such as heterocyclic polynuclear aromatics are excellent candidates for film formation by vacuum deposition means. Over the past decade, our work and that of others investigating a wide variety of perylene and phthalocyanine derivatives identified five deposition parameters that can significantly affect film morphology, physical microstructure, and type and extent of ordering developed in vacuum and vapor transport grown films. These parameters are substrate temperature, deposition rate, substrate chemistry and epitaxy, ambient gas convective flows, and post deposition annealing. Examples of how each of these conditions manifest themselves in the film structure and ordering, most frequently revealed by scanning electron microscopy, reflection absorption infrared spectroscopy (RAIR), and grazing incidence x-ray diffraction (GIX), are presented.

Debe, M. K.↗
NASA NTRS1983

X-ray photoelectron spectroscopy and friction studies of nickel-zinc and manganese-zinc ferrites in contact with metals

X-ray photoelectron spectroscopy analysis and sliding friction experiments were conducted with hot-pressed, polycrystalline Ni-Zn and Mn-Zn ferrites in sliding contact with various transition metals at room temperature in a vacuum of 30 nPa. The results indicate that the coefficients of friction for Ni-Zn and Mn-Zn ferrites in contact with metals are related to the relative chemical activity in these metals: the more active the metal, the higher is the coefficient of friction. The coefficients of friction for the ferrites correlate with the free energy of formation of the lowest metal oxide. The interfacial bond can be regarded as a chemical bond between the metal atoms and the oxygen anions in the ferrite surfaces. The adsorption of oxygen on clean metal and ferrite surfaces increases the coefficients of friction for the Ni-Zn and Mn-Zn ferrite-metal interfaces.

Miyoshi, K.↗
NASA NTRS1979

Smectite clays in Mars soil - Evidence for their presence and role in Viking biology experimental results

Evidence for the presence of smectite clays in Martian soils is reviewed and results of experiments with certain active clays simulating the Viking biology experiments are reported. Analyses of Martian soil composition by means of X-ray fluorescence spectrometry and dust storm spectroscopy and Martian geological history strongly suggest the presence of a mixture of weathered ferro-silicate minerals, mainly nontronite and montmorillonite, accompanied by soluble sulphate salts, as major constituents. Samples of montmorillonite and nontronite incubated with (C-14)-formate or the radioactive nutrient medium solution used in the Viking Labeled Release experiment, were found to produce patterns of release of radioactive gas very similar to those observed in the Viking experiments, indicating the iron-catalyzed decomposition of formate as the reaction responsible for the Viking results. The experimental results of Hubbard (1979) simulating the results of the Viking Pyrolytic Release experiment using iron montmorillonites are pointed out, and it is concluded that many of the results of the Viking biology experiments can be explained in terms of the surface activity of smectite clays in catalysis and adsorption.

Banin, A.↗
NASA NTRS1982

Surface chemistry, friction and wear of Ni-Zn and Mn-Zn ferrites in contact with metals

X-ray photoelectron and Auger electron spectroscopy analysis were used in sliding friction experiments. These experiments were conducted with hot-pressed polycrystalline Ni-Zn and Mn-Zn ferrites, and single-crystal Mn-Zn ferrite in contact with various transition metals at room temperature in both vacuum and argon. The results indicate that Ni2O3 and Fe3O4 were present on the Ni-Zn ferrite surface in addition to the nominal bulk constituents, while MnO2 and Fe3O4 were present on the Mn-Zn ferrite surface in addition to the nominal bulk constituents. The coefficients of friction for the ferrites in contact with metals were related to the relative chemical activity of these metals. The more active the metal, the higher is the coefficient of friction. The coefficients of friction for the ferrites were correlated with the free energy of formation of the lowest metal oxide. The interfacial bond can be regarded as a chemical bond between the metal atoms and the oxygen anions in the ferrite surfaces. The adsorption of oxygen on clean metal and ferrite does strengthen the metal-ferrite contact and increase the friction. The ferrites exhibit local cracking and fracture with sliding under adhesive conditions. All the metals transferred to he surfaces of the ferrites in sliding.

Miyoshi, K.↗