Engineering Papers⌕ Search

SEARCH · Engineering Papers

Results for “Photoelectron 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.

Quote a phrase for an exact phrase match. Source license links do not imply unrestricted reuse.

At least 109 records · Page 6

Analysis of the Solid Products from the OSCAR and the AOWG Trash Processing Systems

Two trash conversion systems that process space logistical trash for conversion into gases and liquids have minor solid product formation consisting of primarily high carbon ash, inorganic salts, and aluminum metal flakes. These solid products necessarily comprise part of the system output because the thermal degradation processes intentionally operate at temperatures below aluminum vaporization and do not convert all solid inorganics or carbon-based compounds into gaseous compounds (i.e., CO 2 or CH 4 ). The two systems included the Orbital Syngas/Commodity Augmentation Reactor (OSCAR) combustion system funded by the NASA Space Technology Mission Directorate (STMD) located at NASA’s Kennedy Space Center, and the Advanced Organic Waste Gasifier (AOWG) steam reforming system developed by Pioneer Astronautics in Lakewood, Colorado, and funded by the NASA Small Business Innovation Research (SBIR) Exploration Systems Development Mission Directorate (ESDMD). OSCAR residual solids were collected from suborbital flight and ground-based laboratory testing, while all AOWG samples were collected from ground testing. This report discusses the solid product characterization, including elemental analyses performed with scanning electron microscopy (SEM) with energy dispersive X-ray spectroscopy (EDS), and a surface chemistry performed with x-ray photoelectron spectroscopy (XPS). A particle size analysis was performed with sieves, followed by SEM analyses. These analyses were performed to elucidate what high value products can be extracted or utilized from the solid products for follow on infusion into chemical feedstocks, manufacturing additives, or in-situ construction-based material needs.

OSCAR↗

LDEF polymeric materials: A summary of Langley characterization

The NASA Long Duration Exposure Facility (LDEF) enabled the exposure of a wide variety of materials to the low earth orbit (LEO) environment. This paper provides a summary of research conducted at the Langley Research Center into the response of selected LDEF polymers to this environment. Materials examined include graphite fiber reinforced epoxy, polysulfone, and additional polyimide matrix composites, films of FEP Teflon, Kapton, several experimental high performance polyimides, and films of more traditional polymers such as poly(vinyl toluene) and polystyrene. Exposure duration was either 10 months or 5.8 years. Flight and control specimens were characterized by a number of analytical techniques including ultraviolet-visible and infrared spectroscopy, thermal analysis, scanning electron and scanning tunneling microscopy, x-ray photoelectron spectroscopy, and, in some instances, selected solution property measurements. Characterized effects were found to be primarily surface phenomena. These effects included atomic oxygen-induced erosion of unprotected surfaces and ultraviolet-induced discoloration and changes in selected molecular level parameters. No gross changes in molecular structure or glass transition temperature were noted. The intent of this characterization is to increase our fundamental knowledge of space environmental effects as an aid in developing new and improved polymers for space application. A secondary objective is to develop benchmarks to enhance our methodology for the ground-based simulation of environmental effects so that polymer performance in space can be more reliably predicted.

Young, Philip R.↗

Electron spectroscopy analysis

The Surface Science Laboratories at the University of Alabama in Huntsville (UAH) are equipped with x-ray photoelectron spectroscopy (XPS or ESCA) and Auger electron spectroscopy (AES) facilities. These techniques provide information from the uppermost atomic layers of a sample, and are thus truly surface sensitive. XPS provides both elemental and chemical state information without restriction on the type of material that can be analyzed. The sample is placed into an ultra high vacuum (UHV) chamber and irradiated with x-rays which cause the ejection of photoelectrons from the sample surface. Since x-rays do not normally cause charging problems or beam damage, XPS is applicable to a wide range of samples including metals, polymers, catalysts, and fibers. 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. The main advantage of electron induced AES is that the electron beam can be focused down to a small diameter and localized analysis can be carried out. On the rastering of this beam synchronously with a video display using established scanning electron microscopy techniques, physical images and chemical distribution maps of the surface can be produced. Thus very small features, such as electronic circuit elements or corrosion pits in metals, can be investigated. Facilities are available on both XPS and AES instruments for depth-profiling of materials, using a beam of argon ions to sputter away consecutive layers of material to reveal sub-surface (and even semi-bulk) analyses.

Gregory, John C.↗

Study of sulfur-containing molecules in the EUV region. I - Photoabsorption cross section of SO2

Using synchrotron radiation as a continuum background, the absorption cross sections of SO2 have been measured using a double ionization chamber. The cross sections range from 10 to a maximum value of 56 Mb in the 175-760 A region. A possible window resonance series was observed and tentatively assigned to a Ryberg series converging to the (6a sub 1) to the -1st ion state. From the fluorescence excitation function the vibrational progressions of the SO2(+) ion states have been measured and found in good agreement with those observed from photoelectron spectroscopy. The same correspondence between peaks in the fragment fluorescence excitation function and the photoelectron spectrum suggests that these ion states of SO2 are dissociative in nature.

Wu, C. Y. R.↗

Friction and Wear Properties of As-deposited and Carbon Ion-implanted Diamond Films

Recent work on the friction and wear properties of as-deposited and carbon ion-implanted diamond films was reviewed. Diamond films were produced by the microwave plasma chemical vapor deposition (CVD) technique. Diamond films with various grain sizes and surface roughnesses were implanted with carbon ions at 60 ke V ion energy, resulting in a dose of 1.2310(exp 17) carbon ions/cm(exp 2). Various analytical techniques, including Raman spectroscopy, proton recoil analysis, Rutherford backscattering, transmission and scanning electron microscopy, x-ray photoelectron spectroscopy, and x-ray diffraction, were utilized to characterize the diamond films. Sliding friction experiments were conducted with a polished natural diamond pin in contact with diamond films in the three environments: humid air (40 percent relative humidity), dry nitrogen (less than 1 percent relative humidity), and ultrahigh vacuum (10(exp -7) Pa). The CVD diamond films indeed have friction and were properties similar to those of natural diamond in the three environments. The as-deposited, fine-grain diamond films can be effectively used as self-lubricating, wear-resistant coatings that have low coefficients of friction (0.02 to 0.04) and low wear rates (10(exp -7) to 10(exp -8)mm(exp 3)/N-m) in both humid air and dry nitrogen. However, they have high coefficients of friction (1.5 to 1.7) and a high wear rate (10(exp -4)mm(exp 3/N-m) in ultrahigh vacuum. The carbon ion implanation produced a thin surficial layer (less than 0.1 micron thick) of amorphous, nondiamond carbon on the diamond films. In humid air and dry nitrogen, the ion-implanted, fine- and coarse-grain diamond films have a low coefficient of friction (around 0.1) and a low wear rate (10(exp -7)mm(exp 3/N-m). Even in ultrahigh vacuum, the presence of the nondiamond carbon layer reduced the coefficient of friction of fine-grain diamond films to 0.1 or lower and the wear rate to 10(exp -6)mm(exp 3)/N-m. Thus, the carbon ion-implanted, fine-grain diamond films can be effectively used as wear-resistant, self-lubricating coatings not only in air and dry nitrogen, but also in ultrahigh vacuum. The wear mechanism of diamond films is that of small fragments chipping off the surface. The size of wear particles is related to the extent of wear rates.

Miyoshi, Kazuhisa↗

Friction and Wear Properties of As-Deposited and Carbon Ion-Implanted Diamond Films

Recent work on the friction and wear properties of as-deposited and carbon ion-implanted diamond films was reviewed. Diamond films were produced by the microwave plasma chemical vapor deposition (CVD) technique. Diamond films with various grain sizes and surface roughnesses were implanted with carbon ions at 60 keV ion energy, resulting in a dose of 1.2 x 10(exp 17) carbon ions per cm(exp 2). Various analytical techniques, including Raman spectroscopy, proton recoil analysis, Rutherford backscattering, transmission and scanning electron microscopy, X-ray photoelectron spectroscopy, and X-ray diffraction, were utilized to characterize the diamond films. Sliding friction experiments were conducted with a polished natural diamond pin in contact with diamond films in the three environments: humid air (40% relative humidity), dry nitrogen (less than 1 percent relative humidity), and ultrahigh vacuum (10(exp -7) Pa). The CVD diamond films indeed have friction and wear properties similar to those of natural diamond in the three environments. The as-deposited, fine-grain diamond films can be effectively used as self-lubricating, wear-resistant coatings that have low coefficients of friction (0.02 to 0.04) and low wear rates (10(exp -7) to lO(exp -8) mm(exp 3) N(exp -1) m(exp -1)) in both humid air and dry nitrogen. However, they have high coefficients of friction (1.5 to 1.7) and a high wear rate (10(exp -4) mm(exp 7) N(exp -1) m(exp -1)) in ultrahigh vacuum. The carbon ion implantation produced a thin surficial layer (less than 0.1 micron thick) of amorphous, non-diamond carbon on the diamond films. In humid air and dry nitrogen, the ion-implanted, fine and coarse-grain diamond films have a low coefficient of friction (around 0.1) and a low wear rate (10(exp -7) mm(exp 3) N(exp -1) m(exp-1)). Even in ultrahigh vacuum, the presence of the non-diamond carbon layer reduced the coefficient of friction of fine-grain diamond films to 0.1 or lower and the wear rate to 10(exp -6) mm(exp 3) N(exp -1) m(exp -1). Thus, the carbon ion-implanted, fine-grain diamond films can be effectively used as wear-resistant, self-lubricating coatings not only in air and dry nitrogen, but also in ultrahigh vacuum.

Miyoshi, Kazuhisa↗

Determination of Trace Silicone Contamination on Composites by Quantitative XPS and LIBS

Surface treatment and surface characterization techniques are critical to ensure that adherends are chemically activated and free of contaminants prior to adhesive bonding. Silicone contamination from mold-release agents and other sources can interfere with interfacial bonding, decreasing the durability and performance of bonded composite structures. Tools and methods are needed that can be used in a production environment to reliably detect low levels of contaminants in a rapid, simple, and cost-effective manner to improve bond reliability. In this work, surface characterization of carbon fiber reinforced polymer (CFRP) composites was performed using laser induced breakdown spectroscopy (LIBS) and the results were compared with those obtained from X-ray photoelectron spectroscopy (XPS). The objective was to investigate the ability to quantify the surface species measured by LIBS since it offers many advantages over XPS in terms of ease of use, sample preparation, and real-time results. The as-processed CFRP panels had trace surface silicone contamination from the fabrication process, the source of which was not investigated. The composites were laser treated at select average laser power levels, resulting in varying levels of contamination reduction. The Si atomic percentage measurements using XPS were conducted both before and after laser ablation. The XPS results were compared with those obtained from LIBS to assess the reliability of each technique for surface contaminant characterization. The results showed an excellent correlation in Si atomic concentration between the two techniques.

Ledesma, Rodolfo↗

Perovskite oxides: Oxygen electrocatalysis and bulk structure

Perovskite type oxides were considered for use as oxygen reduction and generation electrocatalysts in alkaline electrolytes. Perovskite stability and electrocatalytic activity are studied along with possible relationships of the latter with the bulk solid state properties. A series of compounds of the type LaFe(x)Ni1(-x)O3 was used as a model system to gain information on the possible relationships between surface catalytic activity and bulk structure. Hydrogen peroxide decomposition rate constants were measured for these compounds. Ex situ Mossbauer effect spectroscopy (MES), and magnetic susceptibility measurements were used to study the solid state properties. X ray photoelectron spectroscopy (XPS) was used to examine the surface. MES has indicated the presence of a paramagnetic to magnetically ordered phase transition for values of x between 0.4 and 0.5. A correlation was found between the values of the MES isomer shift and the catalytic activity for peroxide decomposition. Thus, the catalytic activity can be correlated to the d-electron density for the transition metal cations.

Carbonio, R. E.↗

Perovskite-type oxides - Oxygen electrocatalysis and bulk structure

Perovskite type oxides were considered for use as oxygen reduction and generation electrocatalysts in alkaline electrolytes. Perovskite stability and electrocatalytic activity are studied along with possible relationships of the latter with the bulk solid state properties. A series of compounds of the type LaFe(x)Ni1(-x)O3 was used as a model system to gain information on the possible relationships between surface catalytic activity and bulk structure. Hydrogen peroxide decomposition rate constants were measured for these compounds. Ex situ Mossbauer effect spectroscopy (MES), and magnetic susceptibility measurements were used to study the solid state properties. X ray photoelectron spectroscopy (XPS) was used to examine the surface. MES has indicated the presence of a paramagnetic to magnetically ordered phase transition for values of x between 0.4 and 0.5. A correlation was found between the values of the MES isomer shift and the catalytic activity for peroxide decomposition. Thus, the catalytic activity can be correlated to the d-electron density for the transition metal cations.

Carbonio, R. E.↗

Chemical structure of interfaces

The interfacial structure of silicon/dielectric and silicon/metal systems is particularly amenable to analysis using a combination of surface spectroscopies together with a variety of chemical structures of Si/SiO2, Si/SiO2Si3N4, Si/Si2N2O, Si/SiO2/Al, and Si/Native Oxide interfaces using high resolution (0.350 eV FWHM) X ray photoelectron spectroscopy. The general structure of these dielectric interfaces entails a monolayer chemical transition layer at the Si/dielectric boundary. Amorphous Si substrates show a wide variety of hydrogenated Si and Si(OH) sub x states that are not observed in thermal oxidation of single crystal material. Extended SiO2 layers greater than 8 A in thickness are shown to be stoichiometric SiO2, but to exhibit a wide variety of local network structures. In the nitrogen containing systems, an approach to stoichiometric oxynitride compounds with interesting impurity and electron trapping properties are seen. In native oxides, substantial topographical nonuniformity in oxide thickness and composition are found. Analysis of metal/oxide interfacial layers is accomplished by analytical removal of the Si substrate by UHV XeF2 dry etching methods.

Grunthaner, F. J.↗

New Method Developed To Purify Single Wall Carbon Nanotubes for Aerospace Applications

Single wall carbon nanotubes have attracted considerable attention because of their remarkable mechanical properties and electrical and thermal conductivities. Use of these materials as primary or secondary reinforcements in polymers or ceramics could lead to new materials with significantly enhanced mechanical strength and electrical and thermal conductivity. Use of carbon-nanotube-reinforced materials in aerospace components will enable substantial reductions in component weight and improvements in durability and safety. Potential applications for single wall carbon nanotubes include lightweight components for vehicle structures and propulsion systems, fuel cell components (bipolar plates and electrodes) and battery electrodes, and ultra-lightweight materials for use in solar sails. A major barrier to the successful use of carbon nanotubes in these components is the need for methods to economically produce pure carbon nanotubes in large enough quantities to not only evaluate their suitability for certain applications but also produce actual components. Most carbon nanotube synthesis methods, including the HiPCO (high pressure carbon monoxide) method developed by Smalley and others, employ metal catalysts that remain trapped in the final product. These catalyst impurities can affect nanotube properties and accelerate their decomposition. The development of techniques to remove most, if not all, of these impurities is essential to their successful use in practical applications. A new method has been developed at the NASA Glenn Research Center to purify gram-scale quantities of single wall carbon nanotubes. This method, a modification of a gas phase purification technique previously reported by Smalley and others, uses a combination of high-temperature oxidations and repeated extractions with nitric and hydrochloric acid. This improved procedure significantly reduces the amount of impurities (catalyst and nonnanotube forms of carbon) within the nanotubes, increasing their stability significantly. The onset of decomposition of the purified nanotubes (determined by thermal gravimetric analysis in air) is more than 300 C higher than that of the crude nanotubes. Transmission electron microscopy analysis of nanotubes purified by this method reveals near complete removal of iron catalyst particles. Analysis of the nanotubes using inductively coupled plasma spectroscopy revealed that the iron content of the nanotubes was reduced from 22.7 wt% in the crude nanotubes to less than 0.02 wt%. X-ray photoelectron spectroscopy revealed a decrease in iron content after purification as well as an increase in oxygen content due to the formation of carboxylic acid groups on the surface of the nanotubes. Nanotubes purified by this improved method can be readily dispersed in common organic solvents, in particular N,N-dimethylformamide, using prolonged ultrasonic treatment. These dispersions can then be used to incorporate single wall carbon nanotubes into polymer films.

Lebron, Marisabel↗

Continuum ionization transition probabilities of atomic oxygen

The technique of photoelectron spectroscopy was employed in the investigation. Atomic oxygen was produced in a microwave discharge operating at a power of 40 W and at a pressure of approximately 20 mtorr. The photoelectron spectrum of the oxygen with and without the discharge is shown. The atomic states can be clearly seen. In connection with the measurement of the probability for transitions into the various ionic states, the analyzer collection efficiency was determined as a function of electron energy.

Samson, J. A. R.↗

Characterization of Molybdate Conversion Coatings for Aluminum Alloys by Electrochemical Impedance Spectroscopy

Electrochemical impedance spectroscopy (EIS) was used to investigate the corrosion inhibiting properties of newly developed proprietary molybdate conversion coatings on aluminum alloy 2024-T3 under immersion in aerated 5% (w/w) NaCl. Corrosion potential and EIS measurements were gathered for six formulations of the coating at several immersion times for two weeks. Nyquist as well as Bode plots of the data were obtained. The conversion-coated alloy panels showed an increase in the corrosion potential during the first 24 hours of immersion that later subsided and approached a steady value. Corrosion potential measurements indicated that formulations A, D, and F exhibit a protective effect on aluminum 2024-T3. The EIS spectra of the conversion-coated alloy were characterized by an impedance that is higher than the impedance of the bare alloy at all the immersion times. The low frequency impedance, Z(sub lf) (determined from the value at 0.05 Hz) for the conversion-coated alloy was higher at all the immersion times than that of the bare panel. This indicates improvement of corrosion resistance with addition of the molybdate conversion coating. Scanning electron microscopy (SEM) revealed the presence of cracks in the coating and the presence of cubic crystals believed to be calcium carbonate. Energy dispersive spectroscopy (EDS) of the test panels revealed the presence of high levels of aluminum, oxygen, and calcium but did not detect the presence of molybdenum on the test panels. X-ray photoelectron spectroscopy (XPS) indicated the presence of less than 0.01 atomic percent molybdenum on the surface of the coating.

Calle, Luz Marina↗

A microwave plasma cleaning apparatus

In a microwave electron cyclotron resonance plasma source, reactive plasmas of oxygen and its mixtures of argon have been used for evaluating plasma cleaning technologies. Small aluminum samples (0.95 x 1.9 cm) were coated with thin films (less than or equal to 20 micrometers in thickness) of Shell Vitrea oil and cleaned with reactive plasmas. The discharge parameters, such as gas pressure, magnetic field, substrate biasing, and microwave power, were varied to change cleaning conditions. A mass spectroscopy (or residual gas analyzer) was used to monitor the status of plasma cleaning. Mass loss of the samples after plasma cleaning was measured to estimate cleaning rates. Measured cleaning rates of low-pressure (0.5-m torr) argon/oxygen plasmas were as high as 2.7 micrometers/min. X-ray photoelectron spectroscopy was used to determine cleanliness of the sample surfaces. In this paper, significant results of the plasma cleaning are reported and discussed.

Tsai, C. C.↗

Effect of ion sputtering on interface chemistry and electrical properties of Au GaAs(100) Schottky contacts

The effects of sputtering n-type (100)GaAs with 1 to 5 keV argon ions have been studied in ultrahigh vacuum. Auger electron and X-ray photoelectron spectroscopies have been used to characterize the surface before and after sputtering. Gold Schottky contacts were prepared in situ to avoid contamination at the metal/semiconductor interface. The data show that sputtering depletes the surface in As, and the extent of depletion increased as the ion energy was increased. However, angular-resolved photoelectron data showed As was enriched on the outer atom layer by 5 keV but depleted by 1 keV Ar(+) sputtering. Current and capacitance versus voltage data showed that sputtering always lowered the Schottky barrier height and generally increased the ideality factor. However, the barrier height after 3 keV sputtering was higher than after 1 keV sputtering. Those effects are explained based on a combined effective work function model and creation of a donorlike surface damage layer. The donor layer was correlated with As depletion by sputtering. Deep level trap formation and annealing of sputtering effects were studied.

Wang, Y.-X.↗

Teflon FEP Analyzed After Retrieval From the Hubble Space Telescope

During the Hubble Space Telescope (HST) Second Servicing Mission, 6.8 years after the telescope was deployed in low Earth orbit, degradation of unsupported Teflon FEP (DuPont; fluorinated ethylene propylene), used as the outer layer of the multilayer insulation (MLI) blankets, was evident as large cracks on the telescope light shield. A sample of the degraded outer layer (see the photograph) was retrieved during the second servicing mission and returned to Earth for ground testing and evaluation. Also retrieved was a Teflon FEP radiator surface from a cryogen vent cover that was exposed to the space environment on the aft bulkhead of the HST. NASA Goddard Space Flight Center directed the efforts of the Hubble Space Telescope MLI Failure Review Board, whose goals included determining the FEP degradation mechanisms. As part of the investigations into the degradation mechanisms, specimens retrieved from the first and second HST servicing missions, 3.6 and 6.8 years after launch, respectively, were characterized through exhaustive mechanical, optical, and chemical testing. Testing led by Goddard included scanning electron microscopy, optical microscopy, tensile testing, solar absorptance measurements, time-of-flight secondary ion mass spectroscopy (TOF-SIMS), Fourier transform infrared microscopy (m-FTIR), attenuated total reflectance infrared microscopy (ATR/FTIR), and x-ray diffraction (XRD). The NASA Lewis Research Center contributed significantly to the analysis of the retrieved HST materials by leading efforts and providing results of bend testing, surface microhardness measurements, x-ray photoelectron spectroscopy, solid-state nuclear magnetic resonance spectroscopy, and density measurements. Other testing was conducted by Nano Instruments, Inc., and the University of Akron.

Dever, Joyce A.↗

Recent Advances in LIBS for Real-Time Detection of Silicone Contaminants on CFRP Surfaces

Laser induced breakdown spectroscopy (LIBS) is a materials characterization technique that has been advanced and refined to provide in situ, real-time quality control of carbon fiber reinforced polymer (CFRP) surfaces. As part of an effort to improve process control for adhesive bonding, a LIBS system was designed and assembled at NASA Langley Research Center (LaRC) to enable detection of ultralow concentrations of silicone contamination on CFRP adherends. The LIBS instrument provides high sensitivity detection and quasi-nondestructive surface characterization of CFRP adherends prior to adhesive bonding. This review focuses on the advancements at LaRC using LIBS as a quality control tool for the detection of silicone contaminants for improved adhesive bonding reliability of CFRP materials. This work describes how the LIBS technique was advanced by analyzing the laser parameters, studying the laser-matter interactions, and performing time-resolved measurements to determine the optimal plasma conditions for elemental detection. In addition, LIBS results were compared to X-ray photoelectron spectroscopy data to enable quantitative analysis from analytical calibration curves. Examples are shown of how to perform surface mapping of silicone contamination. Finally, a brief discussion is also presented on LIBS instrumentation, recommendations for laser parameters and instrumentation components, and LIBS technique maturity.

Surface characterization, Carbon fiber reinforced ↗

Recent Advances in LIBS for Real-Time Detection of Silicone Contaminants on CFRP Surfaces

Laser induced breakdown spectroscopy (LIBS) is a materials characterization technique that has been advanced and refined to provide in situ, real-time quality control of carbon fiber reinforced polymer (CFRP) surfaces. As part of an effort to improve process control for adhesive bonding, aLIBS system was designed and assembled at the NASA Langley Research Center (LaRC) to enable detection of ultra low concentrations of silicone contamination on CFRP adherends. The LIBS instrument provides high sensitivity detection and quasi-nondestructive surface characterization ofCFRP adherends prior to adhesive bonding. This review focuses on the advancements at LaRC using LIBS as a quality control tool for the detection of silicone contaminants for improved adhesive bonding reliability of CFRP materials. This work describes how the LIBS technique was advanced by analyzing the laser parameters, studying the laser-matter interactions, and performing time-resolved measurements to determine the optimal plasma conditions for elemental detection. In addition, LIBS results were compared to X-ray photoelectron spectroscopy data to enable quantitative analysis from analytical calibration curves. Examples are shown of how to perform surface mapping of silicone contamination. Finally, a brief discussion is presented on LIBS instrumentation, recommendations for laser parameters and instrumentation components, and LIBS technique maturity

Rodolfo I. Ledesma↗