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At least 127 records · Page 7
All sourcesNASA NTRSDOE OSTI
NASA NTRS2017

Chemical and Microstructural Changes in Metallic and Ceramic Materials Exposed to Venusian Surface Conditions

The chemical and microstructural behavior of steels (304, 310, 316, and 1018), nickel-based alloys (beta-NiAl, G30, and 625), gold, coatings (4YSZ, SilcoNert(TradeMark) 1040 (SilcoTek Co.), Dursan(TradeMark) (SilcoTek Co.), and porcelain), and bulk ceramics (alpha-Al2O3, fused quartz, beta-SiC, and alpha-Si3N4) were probed after exposure to supercritical fluid with temperature, pressure, and composition mimicking the Venus lower atmosphere. Exposures were carried out in the Glenn Extreme Environments Rig (GEER) chamber with the Venusian gas mixture (96.5% CO2, 3.5% N2, 30 ppm H2O, 150 ppm SO2, 28 ppm CO, 15 ppm OCS, 3 ppm H2S, 0.5 ppm HCl, and 5 ppb HF) at 92 bar (1330 psi) and 467 C (873 F) for durations of 10 and 42 days. An additional 21-day exposure was done to stainless steel uncoated and coated with SilcoNert(TradeMark) and Dursan(TradeMark). Samples were characterized before and after the experiment by gravimetric analysis, X-ray diffraction, X-ray photoelectron and Auger electron spectroscopies, and cross section electron microscopy analysis. All steels exposed for 10 and 42 days formed double-layered scales consisting mainly of metal (Cr, Fe, Ni) oxides and sulfides showing different chemistry, microstructure, and crystalline phases. The alloys G30 and 625 formed double-layered scales consisting mainly of nickel sulfides. After 10 days, the beta-NiAl exhibited no detectable scale, suggesting only a very thin film was formed. The 304 and 316 stainless steels coated with 4YSZ that were exposed for 10 and 42 days exhibited no significant oxidation. Steel 1018 coated with 4YSZ exhibited a corrosion scale of iron and/or chromium oxide formed at the base of the alloy. The 304 steel coated with porcelain did not exhibit corrosion, although the coating exhibited recession. SilcoNert(TradeMark) exposed for 10 and 42 days exhibited recession, although no oxidation was found to occur at the base of the alloy. Stainless steel 316 coated with Dursan(TradeMark)  exhibited corrosion at the base of the alloy. All ceramics tested showed no clear evidence of reaction. The weight-gain-per-area performance of the materials exposed in the GEER for 10 and 42 days are reported from the lowest to the highest weight gain per area as follows: gold did not exhibit any weight change; nickel-based alloys: beta- NiAl < G30 < 625; steels: 304 < 310 < 316 < 1018; ceramics: considering the experimental uncertainties, no weight change was observed for all ceramics of this work (alpha-Al2O3, Si3N4, SiC, and amorphous SiO2).

Costa, Gustavo C. C.↗
NASA NTRS1977

The adsorption and early stages of condensation of Ag and Au on W single-crystal surfaces

Silver and gold were evaporated up to several monolayers in thickness onto W single-crystal surfaces of the 110 and 100 plane types in the temperature range between 300 and 1300 K. The mode of growth and the structure of the layers were studied by Auger electron spectroscopy and low-energy electron diffraction. The results are compared with thermal desorption spectroscopy data and work-function change measurements. They show certain similarities but also some striking differences between the two systems Ag/W and Au/W as well as a strong crystallographic anisotropy of adsorption and condensation.

Bauer, E.↗
NASA NTRS1978

The co-adsorption of copper and oxygen on a tungsten 100 plane-type surface

The coadsorption of Cu on O2 and a W 100 plane-type surface is studied by Auger electron spectroscopy, thermal desorption, low energy electron diffraction and by work function change measurements. It is shown that the presence of Cu on the surface initially decreases the sticking coefficient of O2. For longer oxygen exposures and for higher adsorption temperatures, the coverage of preadsorbed oxygen reaches values larger than those on the clean surface for the same O2 exposure. Except at the highest values and temperatures of the coverage of preadsorbed oxygen, the sticking coefficient for copper is unity and is independent of the oxygen coverage in the range studied. Coadsorption at room temperatures does not produce any long range order while coadsorption at elevated temperature leads to ordered structures. The saturation coverage of the two dimensional coadsorbate at 800 K is given by a relation. The work function is a complicated function of the coverage of preadsorbed oxygen and the coverage of preadsorbed Cu and is determined predominantly by the temperature at which oxygen is adsorbed. At high temperatures the sequence of adsorption has no influence, in contrast to the room temperature behavior.

Bauer, E.↗
NASA NTRS1983

Drastic reduction of adsorption of CO and H2 on (111)-type Pd layers

Clean surfaces of (111)-type Pd layers, grown from the vapor phase on Mo(110) at room temperature, were used to study the adsorption of CO and H2 by temperature-programmed desorption, Auger electron spectroscopy, and low-energy electron diffraction. Mild annealing of the as-grown layers during a single desorption cycle (to about 600 K) drastically reduces the adsorption for both adsorbates. Low-dose argon-ion bombardment introduces surface imperfections which restore a high adsorption probability. The results are interpreted in terms of particular (111)-type surface structures that persist tp layer thicknesses of about four monolayers; the results raise questions with respect to the surface structure of supported thin epitaxial islands and particles of Pd and possibly also with respect to conventional methods of preparing bulk surfaces of Pd for adsorption studies.

Poppa, H.↗
NASA NTRS1994

Thermal desorption of CO and H2 from degassed 304 and 347 stainless steel

Thermal desorption spectroscopy (TDS), along with Auger electron spectroscopy, was used to study the desorption of H2 and CO from baked 304 and 347 stainless-steel samples exposed only to residual gases. Both 347 and 304 samples gave identical TDS spectra. The spectra for CO contained a sharp leading peak centered in the temperature range 410-440C and an exponentially increasing part for temperatures higher than 500C, with a small peak around 600C appearing as a shoulder. The leading peak followed a second-order desorption behavior with an activation energy of 28+/-2 kcal/mol, suggesting that the rate-limiting step for this peak is most likely a surface reaction that produces the CO molecules in the surface layer. The amount of desorbed CO corresponding to this peak was approximately 0.5X10(exp 14) molecules/cm(exp 2) . The exponentially rising part of the CO spectrum appeared to originate from a bulk diffusion process. The TDS spectrum for H2 consisted of a main peak centered also in the temperature range 410-440C, with two small peaks appearing as shoulders at approximately 500 and 650C. The main peak in this case also displayed a second-order behavior with an activation energy of 14+/-2 kcal/mol. The amount of desorbed H2, approximately 1.9X 10(exp 15) molecules/cm(exp 2) , appeared to be independent of the concentration of hydrogen in the bulk, indicating that the majority of the desorbed H2 originated from the surface layer.

Rezaie-Serej, S.↗
NASA NTRS2000

Segregation Behavior of Sulfur and Other Impurities Onto the Free Surfaces of ED-Ni Deposits

Most researchers attribute grain boundary embrittlement in electro-deposited Nickel (ED-Ni) to the presence of small quantities of Sulfur as an impurity. It occurs in a highly mobile form that segregates to the grain boundaries. Evaluation of Sulfur segregation requires that a sample be fractured through the grain boundaries. However, this action may not always be possible. ED-Ni is inherently tough at ambient temperature, especially if a low level of Sulfur was intentionally maintained. A new method was developed to study Sulfur and other migrant species to the grain boundaries, which also migrate to free surfaces. A test specimen is heated by a quartz lamp within the sample preparation chamber, allowing the mobile species to migrate to polished free surfaces. There the mobile species are analyzed using X-ray photoelectron spectroscopy (XPS) also known as Electron Spectroscopy for Chemical Analysis (ESCA).

Panda, Binayak↗
NASA NTRS2001

Segregation Behavior of Sulfur and Other Impurities onto the Free Surfaces of ED-NI Deposits

Most researchers attribute grain boundary embrittlement in electro-deposited nickel (ED-Ni) to the presence of small quantities of sulfur as an impurity. It occurs in a highly mobile form that segregates to the grain boundaries. Evaluation of sulfur segregation requires that a sample be fractured through the grain boundaries. However, this action may not always be possible. ED-Ni is inherently tough at ambient temperature, especially if a low level of sulfur was intentionally maintained. A new method was developed to study sulfur and other migrant species to the grain boundaries, which also migrate to free surfaces. A test specimen is heated by a quartz lamp within the sample preparation chamber, allowing the mobile species to migrate to polished free surfaces. There the mobile species are analyzed using X-ray photoelectron spectroscopy (XPS) also known as Electron Spectroscopy for Chemical Analysis (ESCA).

Panda, B.↗
NASA NTRS2012

Temperature Induced Voltage Offset Drifts in Silicon Carbide Pressure Sensors

We report the reduction of transient drifts in the zero pressure offset voltage in silicon carbide (SiC) pressure sensors when operating at 600 C. The previously observed maximum drift of +/- 10 mV of the reference offset voltage at 600 C was reduced to within +/- 5 mV. The offset voltage drifts and bridge resistance changes over time at test temperature are explained in terms of the microstructure and phase changes occurring within the contact metallization, as analyzed by Auger electron spectroscopy and field emission scanning electron microscopy. The results have helped to identify the upper temperature reliable operational limit of this particular metallization scheme to be 605 C.

Okojie, Robert S.↗
NASA NTRS1991

Imaging analysis of LDEF craters

Two small craters in Al from the Long Duration Exposure Facility (LDEF) experiment tray A11E00F (no. 74, 119 micron diameter and no. 31, 158 micron diameter) were analyzed using Auger electron spectroscopy (AES), time-of-flight secondary ion mass spectroscopy (TOF-SIMS), low voltage scanning electron microscopy (LVSEM), and SEM energy dispersive spectroscopy (EDS). High resolution images and sensitive elemental and molecular analysis were obtained with this combined approach. The result of these analyses are presented.

Radicatidibrozolo, F.↗
NASA NTRS1988

Auger and ESCA analysis

X-ray photoelectron spectroscopy (XPS or ESCA) and Auger electron spectroscopy (AES) techniques are discussed. The XPS instrument is a Perkin-Elmer 5400 system which provides both elemental and chemical state information without restriction on the type of material that can be analyzed. The AES instrument is a Kratos Analytical XSAM 800 system. AES uses a beam of high energy electrons as a surface probe. Following electronic rearrangements within excited atoms by this probe, Auger electrons characteristic of each element present are emitted from the sample. Specific examples of analytic techniques and results are presented.

Gregory, John C.↗
NASA NTRS1976

Formation, structure, and orientation of gold silicide on gold surfaces

The formation of gold silicide on Au films evaporated onto Si(111) surfaces is studied by Auger electron spectroscopy (AES) and low-energy electron diffraction (LEED). Surface condition, film thickness, deposition temperature, annealing temperature, and heating rate during annealing are varied. Several oriented crystalline silicide layers are observed.

Green, A. K.↗
NASA NTRS1981

Chemical and morphological characteristics of lithium electrode surfaces

Lithium electrode surfaces were analyzed for chemical and morphological characteristics, using electron spectroscopy chemical analysis (ESCA) and scanning electron microscopy (SEM). Samples included lithium metal and lithium electrodes which were cycled in a 1.5 M lithium arsenic hexafluoride/two-methyl tetrahydrofuran electrolyte. Results show that the surface of the as-received lithium metal was already covered by a film composed of LiO2 and an Li2O/CO2 adduct with a thickness of approximately 100-200 A. No evidence of Ni3 was found. Upon exposure of the lithium electrode to a 1.5 M LiAsF6/2-Me-THF electrochemical environment, a second film was observed to form on the surface, consisting primarily of As, Si, and F, possibly in the form of lithium arsenic oxyfluorides or lithium fluorosilicates. It is suggested that the film formation may be attributed to salt degradation.

Yen, S. P. S.↗
NASA NTRS1988

Effect of substrate preparation on the structure and chemisorption properties of Pd/MgO model catalyst

Pd/MgO model catalysts are prepared by vapor deposition of Pd particles on MgO thin films which are deposited, at different temperatures, on UHV cleaved mica. MgO films and Pd particles are characterized in situ by Auger electron spectroscopy and energy-loss spectroscopy and ex situ by transmission electron microscopy. Succesive temperature programmed desorption (TPD) of CO shows a different evolution of the morphology of the Pd particles deposited on MgO films prepared at low and high temperature. In addition, on MgO prepared at low temperature, the smallest particles show a continuous decay of CO adsorption during TPD due to contamination by support species.

Henry, C. R.↗
NASA NTRS2011

Improved Reliability of SiC Pressure Sensors for Long Term High Temperature Applications

We report advancement in the reliability of silicon carbide pressure sensors operating at 600 C for extended periods. The large temporal drifts in zero pressure offset voltage at 600 C observed previously were significantly suppressed to allow improved reliable operation. This improvement was the result of further enhancement of the electrical and mechanical integrity of the bondpad/contact metallization, and the introduction of studded bump bonding on the pad. The stud bump contact promoted strong adhesion between the Au bond pad and the Au die-attach. The changes in the zero offset voltage and bridge resistance over time at temperature were explained by the microstructure and phase changes within the contact metallization, that were analyzed with Auger electron spectroscopy (AES) and field emission scanning electron microscopy (FE-SEM).

Okojie, R. S.↗
NASA NTRS1974

Auger spectroscopy of fracture surfaces of ceramics

Results of Auger electron spectroscopy (AES) studies of fracture surfaces in a series of ceramic materials, including Al2O3, MgO, and Si3N4, which were formed using different processing techniques. AES on the fractured surface of a lunar sample is also discussed. Scanning electron micrograph fractography is used to relate the surface chemistry to the failure mode. Combined argon ion sputtering and AES studies demonstrate the local variations in chemistry near the fracture surface. The problems associated with doing AES in insulators are also discussed, and the experimental techniques directed toward solving them are described.

Marcus, H. L.↗
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

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.

Ryan Gott↗