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At least 37 records · Page 2

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

Wear tests were performed on 304 stainless steel lubricated with pure mineral oil with and without dibenzyl-disulfide. Both mild and severe wear were observed. The type of wear was distinguished by a marked change in wear rate, friction coefficient, and wear scar appearance. The chemical composition of the wear scar surface was examined with X-ray photoelectron spectroscopy in conjunction with argon ion sputter etching. In severe wear scars, a sulfide was formed at the expense of the normal oxide layer. In mild wear scars, there were only superficial sulfur compounds, but there was a substantial increase in the oxide thickness.

Wheeler, D. R.↗

Friction and wear properties of three hard refractory coatings applied by radiofrequency sputtering

The adherence, friction, and wear properties of thin hard refractory compound coatings applied to 440C bearing steel by radiofrequency sputtering were investigated. Friction and wear tests were done with nonconforming pin on disk specimens. The compounds examined were chromium carbide, molybdenum silicide, and titanium carbide. The adherence, friction, and wear were markedly improved by the application of a bias voltage to the bearing steel substrate during coating deposition. Analysis by X-ray photoelectron spectroscopy indicated that the improvement may be due to a reduction in impurities in bias deposited coatings. A fivefold reduction in oxygen concentration in MoSi2 coating by biasing was noted. Chromium carbide was not effective as an antiwear coating. Molybdenum silicide provided some reduction in both friction and wear. Titanium carbide exhibited excellent friction and antiwear properties at light loads. Plastic flow and transfer of the coating material onto the pin specimen appears to be important in achieving low friction and wear.

Brainard, W. A.↗

Migratory gold resistive shorts - Chemical aspects of a failure mechanism

Integrated-circuit devices using the Ti/W/Au metal system are subject to failure mechanisms based on electrolytic corrosion. The migratory gold resistive short (MGRS) failure mode is one example of this mechanism and results in the formation of filamentary or dendritic deposits of gold between adjacent stripes on the IC chip. This reaction requires the presence of a sufficient amount of water, a bias voltage between adjacent stripes, and the activation of the cathodic (-) stripe. Gold ions are transported from anode to cathode through a film of moisture adsorbed on the surface of the chip; halide ions are probably involved in the transfer. Their presence is verified experimentally by X-ray photoelectron spectroscopy. Some of the chemical and electrostatic factors involved in the MGRS mechanism are discussed in this paper, including the questions of a threshold level of moisture and contamination.

Grunthaner, F. J.↗

Technology of GaAs metal-oxide-semiconductor solar cells

The growth of an oxide interfacial layer was recently found to increase the open-circuit voltage (OCV) and efficiency by up to 60 per cent in GaAs metal-semiconductor solar cells. Details of oxidation techniques to provide the necessary oxide thickness and chemical structure and using ozone, water-vapor-saturated oxygen, or oxygen gas discharges are described, as well as apparent crystallographic orientation effects. Preliminary results of the oxide chemistry obtained from X-ray, photoelectron spectroscopy are given. Ratios of arsenic oxide to gallium oxide of unity or less seem to be preferable. Samples with the highest OVC predominantly have As(+3) in the arsenic oxide rather than As(+5). A major difficulty at this time is a reduction in OCV by 100-200 mV when the antireflection coating is vacuum deposited.

Stirn, R. J.↗

Application of ESCA to the determination of stoichiometry in sputtered coatings and interface regions

X-ray photoelectron spectroscopy was used to characterize radiofrequency sputter deposited films of several refractory compounds. Both the bulk film properties such as purity and stoichiometry and the character of the interfacial region between the film and substrate were examined. The materials were CrB2, MoS2, Mo2C, and Mo2B5 deposited on 440C steel. It was found that oxygen from the sputtering target was the primary impurity in all cases. Biasing improves the film purity. The effect of biasing on film stoichiometry is different for each compound. Comparison of the interfacial composition with friction data suggests that adhesion of these films is improved if a region of mixed film and iron oxides can be formed.

Wheeler, D. R.↗

Single crystal and polycrystalline GaAs solar cells using AMOS technology

A description is given of current technology for fabricating single AMOS (antireflection-coated metal oxide semiconductor) solar cells, with attention given to thermal, plasma, and anodic oxidation, native oxide stripping, and X-ray photoelectron spectroscopy results. Some preliminary results are presented on the chemistry and electrical characterization of such cells, and the characteristics of cells fabricated on sliced polycrystalline GaAs wafers are examined. Consideration is also given to the recrystallization of evaporated Ge films for use as low-cost substrates for polycrystalline GaAs solar cells.

Stirn, R. J.↗

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.↗

Adherence of sputtered titanium carbides

Sputtered coatings of the refractory metal carbides are of great interest for applications where hard wear-resistant materials are desired. The usefulness of sputtered refractory carbides is often limited, in practice, by spalling or interfacial separation. In this work improvements in the adherence of refractory carbides on iron, nickel and titanium based alloys were obtained by using oxidation, reactive sputtering or sputtered interlayers to alter the coating-substrate interfacial region. X-ray photoelectron spectroscopy and argon ion etching were used to characterize the interfacial regions, and an attempt was made to correlate adherence as measured in wear tests with the chemical nature of the interface.

Brainard, W. A.↗

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.↗

Surface chemistry of iron sliding in air and nitrogen lubricated with hexadecane and hexadecane containing dibenzyl-dilsulfide

Wear experiments were conducted on iron sliding in hexadecane and hexadecane plus one weight percent dibenzyl dilsulfide (DBDS) in atmospheres of air and nitrogen at room temperature. The wear scars and the wear debris were analyzed by X-ray photoelectron spectroscopy. The presence of air reduced wear but increased friction, while DBDS reduced friction but had little effect on wear except that the wear increased somewhat when DBDS was used in air. Wear scar analysis indicated that oxygen and sulfur competed chemically for the surface, with the oxide predominating. Low wear was associated with a thick oxide layer and low friction with a thin predominantly sulfide layer. Analysis of the wear debris indicated the presence of a sulfate in the high wear case (hexadecane plus DBDS in air), and showed the presence of an organic sulfide in the low wear case (Hexadecane plus DBDS in nitrogen).

Wheeler, D. R.↗

Application of ESCA to the determination of stoichiometry in sputtered coatings and interface regions

X-ray Photoelectron Spectroscopy (XPS) was used to characterize radiofrequency sputter deposited films of several refractory compounds. Both the bulk film properties such as purity and stoichiometry and the character of the interfacial region between the film and substrate were examined. The materials were CrB2, MoS2, Mo2C, and Mo2B5 deposited on 440C steel. It was found that oxygen from the sputtering target was the primary impurity in all cases. Biasing improves the film purity. The effect of biasing on film stoichiometry is different for each compound. Comparison of the interfacial composition with friction data suggests that adhesion of these films is improved if a region of mixed film and iron oxides can be formed.

Wheeler, D. R.↗

An XPS study of the adherence of refractory carbide, silicide, and boride RF-sputtered wear-resistant coatings

Radio frequency sputtering was used to deposit refractory carbide, silicide, and boride coatings on 440-C steel substrates. Both sputter etched and pre-oxidized substrates were used and the films were deposited with and without a substrate bias. The composition of the coatings was determined as a function of depth by X-ray photoelectron spectroscopy combined with argon ion etching. Friction and wear tests were conducted to evaluate coating adherence. In the interfacial region there was evidence that bias may produce a graded interface for some compounds. Biasing, while generally improving bulk film stoichiometry, can adversely affect adherence by removing interfacial oxide layers. Oxides of all film constituents except carbon and iron were present in all cases but the iron oxide coverage was only complete on the preoxidized substrates. The film and iron oxides were mixed in the MoSi2 and Mo2C films but layered in the Mo2B5 films. In the case of mixed oxides, preoxidation enhanced film adherence. In the layered case it did not.

Brainard, W. A.↗

Adherence of sputtered titanium carbides

The study searches for interface treatment that would increase the adhesion of TiC coating to nickel- and titanium-base alloys. Rene 41 (19 wt percent Cr, 11 wt percent Mo, 3 wt percent Ti, balance Ni) and Ti-6Al-4V (6 wt percent Al, 4 wt percent V, balance Ti) are considered. Adhesion of the coatings is evaluated in pin-and disk friction tests. The coatings and interface regions are examined by X-ray photoelectron spectroscopy. Results suggest that sputtered refractory compound coatings adhere best when a mixed compound of coating and substrate metals is formed in the interfacial region. The most effective type of refractory compound interface appears to depend on both substrate and coating material. A combination of metallic interlayer deposition and mixed compound interface formation may be more effective for some substrate coating combinations than either alone.

Brainard, W. A.↗

Chemical processes involved in the initiation of hot corrosion of B-1900 and NASA-TRW VIA

Sodium sulfate induced hot corrosion of B-1900 and NASA-TRW VIA at 900 C was studied with special emphasis on the chemical reactions occurring during and immediately after the induction period. Thermogravimetric tests were run for set periods of time after which the samples were washed with water and water soluable metal salts and/or residual sulfates were analyzed chemically. Element distributions within the oxide layer were obtained from electron microprobe X-ray micrographs. A third set of samples were subjected to surface analysis by X-ray photoelectron spectroscopy. Evolution of SO2 was monitored throughout many of the hot corrosion tests. Results are interpreted in terms of acid-base fluxing mechanisms.

Fryburg, G. C.↗

Local atomic and electronic structure of oxide/GaAs and SiO2/Si interfaces using high-resolution XPS

The chemical structures of thin SiO2 films, thin native oxides of GaAs (20-30 A), and the respective oxide-semiconductor interfaces, have been investigated using high-resolution X-ray photoelectron spectroscopy. Depth profiles of these structures have been obtained using argon ion bombardment and wet chemical etching techniques. The chemical destruction induced by the ion profiling method is shown by direct comparison of these methods for identical samples. Fourier transform data-reduction methods based on linear prediction with maximum entropy constraints are used to analyze the discrete structure in oxides and substrates. This discrete structure is interpreted by means of a structure-induced charge-transfer model.

Grunthaner, F. J.↗

Improved adhesion of sputtered refractory carbides to metal substrates

Sputtered coatings of the refractory metal carbides are of great interest for applications where hard wear-resistant materials are desired. The usefulness of sputtered refractory carbides is often limited in practice by spalling or interfacial separation. In this work improvements in the adherence of refractory carbides on iron, nickel and titanium base alloys were obtained by using oxidation, reactive sputtering or sputtered interlayers to alter the coating-substrate interfacial region. X-ray photoelectron spectroscopy and argon ion etching were used to characterize the interfacial regions, and an attempt was made to correlate adherence as measured in wear tests with the chemical nature of the interface.

Wheeler, D. R.↗

XPS study of the chemical structure of the nickel/silicon interface

The chemical nature of the Ni/Si, Ni/Ni2Si, and Si/Ni2Si interfaces is studied using X-ray photoelectron spectroscopy. Two approaches are employed: (1) the Ni/silicide and Si/silicide interfaces are examined by dynamically monitoring the advancing reaction front during in situ growth and (2) as-deposited Ni/Si interfacial properties are analyzed by sequential evaporating monolayer Ni films on Si. These experiments show that the Ni/Ni2Si interface consists of a Ni-rich silicide phase, while the Si/Ni2Si interface has a transitional region that is correspondingly Si-rich silicide.

Grunthaner, P. J.↗

Chemical depth profiles of the GaAs/native oxide interface

The final-state oxidation products and their distribution in thin native oxides (30-40 A) on GaAs have been studied using X-ray photoelectron spectroscopy in conjunction with chemical depth profiling. Extended room-temperature-oxidation conditions have been chosen to allow the native oxide to attain its equilibrium composition and structure. The work emphasizes the use of chemical depth-profiling methods which make it possible to examine the variation in chemical reactivity of the oxide structure. A minimum of two distinct regions of Ga2O3 with differing chemical reactivity is observed. Chemical shift data indicate the presence of As2O3 in the oxide together with an elemental As overlayer at the interface. A change in relative charge transfer between oxygen and both arsenic and gallium-oxide species is observed in the region of the interface.

Grunthaner, P. J.↗