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NASA NTRS1984

XPS study of the Al/SiO2 interface viewed from the SiO2 side

The first nondestructive measurement of the chemical and physical characteristics of the interface between bulk SiO2 and thick aluminum films is presented. Both X-ray photoelectron spectroscopy (XPS) and electrical measurements of unannealed resistively evaporated Al films on thermal SiO2 indicate an atomically abrupt interface. Postmetallization annealing (PMA) at 450 C induces reduction of the SiO2 by the aluminum, resulting in the layer ordering SiO2/Al2O3/Si/Al. The XPS measurement is performed from the SiO2 side after removal of the Si substrate after etching with XeF2 gas and thinning of the SiO2 layer with HF:ETOH. This represents a powerful new approach to the study of metal-insulator and other interfaces.

Hecht, M. H.↗

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 NTRS1985

Study of the kinetics and mechanism of the thermal nitridation of SiO2

X-ray photoelectron spectroscopy (XPS) has been used to study the nitridation time and temperature dependence of the nitrogen distribution in thermally nitrided SiO2 films. The XPS data show that the maximum nitrogen concentration near the (SiO(x)N(y)/Si interface is initially at the interface, but moves 20-25 A away from the interface with increasing nitridation time. Computer modeling of the kinetic processes involved is carried out and reveals a mechanism in which diffusing species, initially consisting primarily of nitrogen, react with the substrate, followed by formation of the oxygen-rich oxynitride due to reaction of the diffusing oxygen displaced by the slower nitridation of the SiO2. The data are consistent with this mechanism provided the influence of the interfacial strain on the nitridation and oxidation kinetics is explicitly accounted for.

Vasquez, R. P.↗

NASA NTRS1985

Role of GaAs surface clearing in plasma deposition of silicon nitride films for encapsulated annealing

The role of GaAs surface cleaning and plasma reactor cleaning prior to deposition of silicon nitride films for encapsulated annealing has been investigated. X-ray photoelectron spectroscopy was employed to determine the surface characteristics of GaAs treated with HCl, HF, and NH4OH solutions preceded by a degreasing procedure. The HCl clean left the least amount of oxygen on the surface. Fluorine contamination resulting from the CF4 plasma used to clean the reactor was found to be located at the film-substrate interface by Auger electron spectroscopy with argon-ion sputtering. A modified deposition procedure was developed to eliminate the fluorine contamination. Plasma deposition of silicon nitride encapsulating films was found to modify the I-V characteristics of Schottky diodes subsequently formed on GaAs surface. The reverse current of the diodes was slightly reduced. Substrates implanted with Si at 100 keV and a dose of 5 x 10 to the 12th/sq cm showed a peak electron concentration of 1.7 x 10 to the 17th/cu cm at a depth of 0.1-micron with 60 percent activation after encapsulation and annealing at 800 C for 7 min.

Valco, G. J.↗

NASA NTRS1985

SEM/XPS analysis of fractured adhesively bonded graphite fibre-reinforced polyimide composites

The surfaces of the graphite fiber-reinforced polyimide composites presently pretreated prior to bonding with polyimide adhesive contained variable amounts of a fluoropolymer, as determined by X-ray photoelectron spectroscopy. Lap shear strengths were determined for unaged samples and for those aged over 500- and 1000-hour periods at 177 and 232 C. Unaged sample lap strengths, which were the highest obtained, exhibited no variation with surface pretreatment, but a significant decrease is noted with increasing aging temperature. These thermally aged samples, however, had increased surface fluorine concentration, while a minimal concentration was found in unaged samples. SEM demonstrated a progressive shift from cohesive to adhesive failure for elevated temperature-aged composites.

Devilbiss, T. A.↗

NASA NTRS1985

A fundamental study of the sticking of insect residues to aircraft wings

The aircraft industry has long been concerned with the increase of drag on airplanes due to fouling of the wings by insects. The present research studied the effects of surface energy and surface roughness on the phenomenon of insect sticking. Aluminum plates of different roughnesses were coated with thin films of polymers with varying surface energies. The coated plates were attached to a custom jig and mounted on top of an automobile for insect collection. Contact angle measurements, X-ray photoelectron spectroscopy and specular reflectance infrared spectroscopy were used to characterize the surface before and after the insect impact experiments. Scanning electron microscopy showed the topography of insect residues on the exposed plates. Moments were calculated in order to find a correlation between the parameters studied and the amount of bugs collected on the plates. An effect of surface energy on the sticking of insect residues was demonstrated.

Eiss, N. S., Jr.↗

NASA NTRS1985

The effects of surface pretreatment and nitrogen tetroxide purification on the corrosion rate of Type 304L stainless steel

Corrosion rates of 304L stainless steel coupons in MON-1 oxidizer have been measured as a function of cleaning procedures employed, surface layer positions, propellant impurity levels, and short-term exposure durations (14 to 90 days). Of special interest was propellant contamination by buildup of soluble iron, which may cause flow decay. Surface treatments employed were combinations of cleaning, pickling, and passivation procedures. Propellants used were MIL-SPEC MON-1 and several types of purified NTO (i.e., low water, low chloride) which may, at a later time, be specified as spacecraft grade. Pretest coupon surface analysis by X-ray photoelectron spectroscopy (XPS-ESCA) has revealed important differences, for the different cleaning procedures, in the make-up of the surface layer, both in composition and state of chemical combination of the elements involved. Comparisons will be made of XPS/ESCA data, for different cleaning procedures, for specimens before and after propellant exposure.

Blue, G. D.↗

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 NTRS1986

Fracture surface analysis in composite and titanium bonding

Carbon fibers were obtained from several manufacturers. Surface treatments were performed on these fibers by anodization. The surfaces of these fibers were analyzed by X-ray photoelectron spectroscopy and wetting force measurement. The breaking strength of these fibers was measured at 2.5 cm length. It was seen that the surface treatments reduces the strength of the fibers. It was also seen that the Hercules fibers had a higher breaking strength than the Union Carbide fibers. Fiber critical length measurements showed no difference in critical lengths between AS-4 and AU-4 fibers embedded in polysulfone. However, the fiber lengths were much shorter for the surface treated fibers. This effect could be related to increased adhesion between fiber and matrix, or it could be due to the lower breaking strength of the surface treated fiber.

Devilbiss, T. A.↗

NASA NTRS1985

Thermal and sputtered aluminum oxide coatings for high temperature electrical insulation

Aluminum oxide coatings have been investigated as electrically insulating layers for mounting thin film Pt-Pt/Rh thermocouples on gas turbine blade and vane alloys (MAR M200 + Hf and MAR M509). Thermal oxides were grown directly onto NiCoCrAlY and FeCrAlY coatings on these alloys at temperature between 1300 and 1400 K in oxygen partial pressures 10 to the -7th to 2 x 10 to the 4th Pa. Although these thermal oxides exhibited good adherence, analytical characterizations using electron and optical microscopy, as well as X-ray photoelectron spectroscopy showed that they had defects and impurities which limited their insulating ability. The insulating quality of the coating was greatly improved however by reactively sputtering an aluminum oxide film over the thermal oxide. Results are presented on the electrical performance of the 2-5 micron thick composite layers for temperatures up to 1300 K.

Kreider, K. G.↗

NASA NTRS1986

Presence, segregation and reactivity of H, C and N dissolved in some refractory oxides

The sources of impurities, particularly carbon, in high melting oxides and silicates are discussed, along with detection and quantification methods. The impurities are important for their effects on bulk material properties through the media of, e.g., surface or grain boundary characteristics. The impurities are usually encountered by the contact of the oxide (refractory) material with volatiles such as H2O and CO2, which become incorporated in the material and form anion complexes with oxygen acting as a covalent bonded ligand. The specific processes undergone by MgO in assimilating C impurities are delineated, using data obtained with X-ray photoelectron spectroscopy, Auger electron spectroscopy, secondary ion mass spectrometry and nuclear reaction profiling. Finally, maintenance of a supersaturated solid solution with C impurities by space charge control is described as a means of offset impurity effects.

Freund, F.↗

NASA NTRS1986

Tribological characteristics of gold films deposited on metals by ion plating and vapor deposition

The graded interface between an ion-plated film and a substrate is discussed as well as the friction and wear properties of ion-plated gold. X-ray photoelectron spectroscopy (XPS) depth profiling and microhardness depth profiling were used to investigate the interface. The friction and wear properties of ion-plated and vapor-deposited gold films were studied both in an ultra high vacuum system to maximize adhesion and in oil to minimize adhesion. The results indicate that the solubility of gold on the substrate material controls the depth of the graded interface. Thermal diffusion and chemical diffusion mechanisms are thought to be involved in the formation of the gold-nickel interface. In iron-gold graded interfaces the gold was primarily dispersed in the iron and thus formed a physically bonded interface. The hardness of the gold film was influenced by its depth and was also related to the composition gradient between the gold and the substrate. The graded nickel-gold interface exhibited the highest hardness because of an alloy hardening effect. The effects of film thickness on adhesion and friction were established.

Miyoshi, K.↗

NASA NTRS1982

XPS, AES and friction studies of single-crystal silicon carbide

The surface chemistry and friction behavior of a single crystal silicon carbide surface parallel to the 0001 plane in sliding contact with iron at various temperatures to 1500 C in a vacuum of 3 x 10 nPa are investigated using X-ray photoelectron and Auger electron spectroscopy. Results show that graphite and carbide-type carbon are seen primarily on the silicon carbide surface in addition to silicon at temperatures to 800 C by both types of spectroscopy. The coefficients of friction for iron sliding against a silicon carbide surface parallel to the 0001 plane surface are found to be high at temperatures up to 800 C, with the silicon and carbide-type carbon at maximum intensity in the X-ray photoelectron spectroscopy at 800 C. The concentration of the graphite increases rapidly on the surface as the temperature is increased above 800 C, while the concentrations of the carbide-type carbon and silicon decrease rapidly and this presence of graphite is accompanied by a significant decrease in friction. Preheating the surfaces to 1500 C also gives dramatically lower coefficients of friction when reheating in the sliding temperature range of from room temperature to 1200 C, with this reduction in friction due to the graphite layer on the silicon carbide surface.

Miyoshi, K.↗

NASA NTRS1981

Surface chemistry and friction behavior of the silicon carbide (0001) surface at temperatures to 1500 deg C

X-ray photoelectron and Auger electron spectroscopy analyses and friction studies were conducted with a silicon carbide (0001) surface in contact with iron at various temperatures to 1200 or 1500 C in a vacuum of 10 to the minus 8th power Pa. The results indicate that there is a significant temperature influence on both the surface chemistry and friction properties of silicon carbide. The principal contaminant of adsorbed amorphous carbon on the silicon carbide surface in the as received state is removed by simply heating to 400 C. Above 400 C, graphite and carbide type carbine are the primary species on the silicon carbide surface, in addition to silicon. The coefficients of friction of polycrystalline iron sliding against a single crystal silicon carbide (0001) surface were high at temperatures to 800 C. Similar coefficients of friction were obtained at room temperature after the silicon carbide was preheated at various temperatures up 800 C. When the friction experiments were conducted above 800 C or when the specimens were preheated to above 800 C, the coefficients of friction were dramatically lower. At 800 C the silicon and carbide type carbon are at a maximum intensity in the XPS spectra. With increasing temperature above 800 C, the concentration of the graphite increases rapidly on the surface, whereas those of the carbide type carbon and silicon decrease rapidly.

Miyoshi, K.↗

NASA NTRS1982

Surface chemistry and wear behavior of single-crystal silicon carbide sliding against iron at temperatures to 1500 C in vacuum

X-ray photoelectron and Auger electron spectroscopy analyses and morphological studies of wear and metal transfer were conducted with a single-crystal silicon carbide 0001 surface in contact with iron at various temperatures to 1500 C in a vacuum of 10 to the minus 8th power pascal. The results indicate that below 800 C, carbide-carbon and silicon are primarily seen on the silicon carbide surface. Above 800 C the graphite increases rapidly with increase in temperature. The outermost surficial layer, which consists mostly of graphite and little silicon at temperatures above 1200 C is about 2 nm thick. A thicker layer, which consists of a mixture of graphite, carbide, and silicon is approximately 100 nm thick. The closer the surface sliding temperature is to 800 C, the more the metal transfer produced. Above 800 C, there was a transfer of rough, discontinuous, and thin iron debris instead of smooth, continuous and thin iron film which was observed to transfer below 800 C. Two kinds of fracture pits were observed on the silicon carbide surface: (1) a pit with a spherical asperity; and (2) multiangular shaped pits.

Miyoshi, K.↗

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.↗

NASA NTRS1983

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

Miyoshi, K.↗

NASA NTRS1967

Molecular orbitals and inner-electron-shell chemical shifts for sulfur and chlorine oxy- anions.

Chemical effects in X-ray spectra and inner shell photoelectron spectra of sulfur- and chlorine- oxygen anions and molecular orbital method

MOLECULAR ORBIT↗