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NASA NTRS1972

Adhesion, friction, wear, and lubrication research by modern surface science techniques.

The field of surface science has undergone intense revitalization with the introduction of low-energy electron diffraction, Auger electron spectroscopy, ellipsometry, and other surface analytical techniques which have been sophisticated within the last decade. These developments have permitted submono- and monolayer structure analysis as well as chemical identification and quantitative analysis. The application of a number of these techniques to the solution of problems in the fields of friction, lubrication, and wear are examined in detail for the particular case of iron; and in general to illustrate how the accumulation of pure data will contribute toward the establishment of physiochemical concepts which are required to understand the mechanisms that are operational in friction systems. In the case of iron, LEED, Auger and microcontact studies have established that hydrogen and light-saturated organic vapors do not establish interfaces which prevent iron from welding, whereas oxygen and some oxygen and sulfur compounds do reduce welding as well as the coefficient of friction. Interpretation of these data suggests a mechanism of sulfur interaction in lubricating systems.

Keller, D. V., Jr.↗

NASA NTRS2003

Investigating Surface Mineralogy, Alteration Processes, and Biomarkers on Mars Using Laser Raman Spectroscopy

Despite a wealth of information from past and ongoing missions to Mars, the capability to determine the mineralogy of surface materials and to connect mineralogy with lithologic characteristics that are diagnostic of the environment in which those materials formed remains inadequate. The 2003 Mars Exploration Rovers (MER) will carry a Mini-TES and a Mossbauer spectrometer, which will provide some detailed mineralogy information. For general characterization of minerals and/or biogenic phases (reduced carbon, PAHs, etc) on the surface of Mars, we have been developing a miniaturized laser Raman spectrometer for in situ analyses -- the Mars Microbeam Raman Spectrometer, MMRS. We are also developing strategies to use Raman spectroscopy as a stand-alone technique and to be used synergistically with other in situ analysis methods in future planetary missions. Through studies of Martian meteorites and terrestrial analogs, we are gaining experience of what compositional and structural information can be obtained on key mineral groups using in-situ Raman measurements. We are developing methods for determining mineral proportions in rocks or soils and identifying rock types from sets of closely spaced, rapidly acquired spectra. We are studying how weathering and alteration affect the Raman and luminescence features of minerals and rocks, and we are investigating the Raman characteristics of biogenic organisms and their remains. These studies form the scientific basis for in-situ planetary Raman spectroscopy, and they are being done in parallel with instrument development towards a flight version of the MMRS.

Alian Wang↗

NASA NTRS1974

Structure and properties of solid surfaces

Difficulties in experimental studies of crystalline surfaces are related to the fact that surface atoms have an intrinsic tendency to react with their environment. A second problem is connected with the effective thickness of surfaces, which ranges from one to several atom layers. The phenomenology of surface interactions with gases are considered, taking into account physical adsorption, chemisorption, and the oxidation of surfaces. Studies of the surface structure are discussed, giving attention to field emission microscopy, field-ion microscopy, electron diffraction techniques, Auger spectroscopy, scanning electron microscopy, electron probe microanalysis, ion microprobe methods, and low-energy backscattering spectroscopy. Investigations of semiconductor surfaces are also described.

Gatos, H. C.↗

NASA NTRS1990

Characterization of the surfaces of platinum/tin oxide based catalysts by Fourier Transform Infrared Spectroscopy (FTIR)

A Pt/SnO2 catalyst has been developed at NASA Langley that is effective for the oxidation of CO at room temperature (1). A mechanism has been proposed to explain the effectiveness of this catalyst (2), but most of the species involved in this mechanism have not been observed under actual catalytic conditions. A number of these species are potentially detectable by Fourier Transform Infrared Spectroscopy (FTIR), e.g., HOSnO sub x, HO sub y PtO sub z, Pt-CO, and SnHCO3. Therefore a preliminary investigation was conducted to determine what might be learned about this particular catalyst by transmission FTIR. The main advantage of FTIR for this work is that the catalyst can be examined under conditions similar to the actual catalytic conditions. This can be of critical importance since some surface species may exist only when the reaction gases are present. Another advantage of the infrared approach is that since vibrations are probed, subtle chemical details may be obtained. The main disadvantage of this approach is that FTIR is not nearly as sensitive as the Ultra High Vacuum (UHV) surface analytical techniques such as Auger, Electron Spectroscopy for Chemical Analysis (ESCA), Electron Energy Loss Spectroscopy (EELS), etc. Another problem is that the assignment of the observed infrared bands may be difficult.

Keiser, Joseph T.↗

NASA NTRS1979

Mechanical and chemical effects of ion-texturing biomedical polymers

To determine whether sputter etching may provide substantial polymer surface texturing with insignificant changes in chemical and mechanical properties, an 8 cm beam diameter, electron bombardment, argon ion source was used to sputter etch (ion-texture process) nine biomedical polymers. The materials included silicone rubber, 32% carbon impregnated polyolefin, polyoxymethylene, polytetrafluoroethylene, ultrahigh molecular weight (UHMW) polyethylene, UHMW polyethylene with carbon fibers (10%), and several polyurethanes (bioelectric, segmented, and cross linked). Ion textured microtensile specimens of each material except UHMW polyethylene and UHMW polyethylene with 10% carbon fibers were used to determine the effect of ion texturing on tensile properties. Scanning electron microscopy was used to determine surface morphology changes, and electron spectroscopy for chemical analysis was used to analyze the near surface chemical changes that result from ion texturing. Ion energies of 500 eV with beam current densities ranging from 0.08 to 0.19 mA/sq cm were used to ion texture the various materials. Standard microtensile specimens of seven polymers were exposed to a saline environment for 24 hours prior to and during the tensile testing. The surface chemical changes resulting from sputter etching are minimal in spite of the often significant changes in the surface morphology.

Weigand, A. J.↗

NASA NTRS1995

Au/Cr Sputter Coating for the Protection of Alumina During Sliding at High Temperatures

A sputter deposited bilayer coating of gold and chromium was investigated as a potential solid lubricant to protect alumina substrates in applications involving sliding at high temperature. The proposed lubricant was tested in a pin-on-disk tribometer with coated alumina disks sliding against uncoated alumina pins. Three test parameters; temperature, load, and sliding velocity were varied over a wide range in order to determine the performance envelope on the gold/chromium (Au/Cr) solid lubricant film. The tribo-tests were run in an air atmosphere at temperatures of 25 to 1000 C, under loads of 4.9 to 49.0 N and at sliding velocities from 1 to 15 m/sec. Post test analyses included surface profilometry, wear factor determination and scanning electron microscopy/energy dispersive spectroscopy (SEM/EDS) examination of worn surfaces. Compared to unlubricated Al2O3 sliding, the use of the Au/Cr film reduced friction by 30 to 50 percent and wear by one to two orders of magnitude. Increases in test temperature resulted in lower friction and the Au/Cr film continued to provide low friction, about 0.3, even at 1000 C. Pin wear factors and friction were largely unaffected by increasing loads up to 29.4 N. Sliding velocity had essentially no effect on friction, however, increased velocity reduced coating life (total sliding distance). Based upon these research results, the Au/Cr film is a promising lubricant for moderately loaded, low speed applications operating at temperatures as high as 1000 C.

Benoy, Patricia A.↗

NASA NTRS1966

A nondispersive X-ray spectrometer for lunar and planetary geochemical analysis.

Nondispersive X-ray spectrometer for remote geochemical analysis of lunar or planetary surfaces

GEOCHEMISTRY↗

NASA NTRS2003

Micro-Spectroscopy as a Tool for Detecting Micron-Scale Mineral Variations Across a Rock Surface: An Example Using a Thin Section of Martian Meteorite ALH 84001

Imaging spectroscopy is a powerful tool for mineral detection across broad spatial regions. A prototype micro-imaging spectrometer at NASA Ames is tested in this study on a scale of tens to hundreds of microns across rock surfaces. Initial measurements were performed in the visible spectral region on a thin section of martian meteorite ALH 84001.

Dalton, J. Brad↗

NASA NTRS1995

P-polarized reflectance spectroscopy: A high sensitive real-time monitoring technique to study surface kinetics under steady state epitaxial deposition conditions

This paper describes the results of real-time optical monitoring of epitaxial growth processes by p-polarized reflectance spectroscopy (PRS) using a single wavelength application under pulsed chemical beam epitaxy (PCBE) condition. The high surface sensitivity of PRS allows the monitoring of submonolayer precursors coverage on the surface as shown for GaP homoepitaxy and GaP on Si heteroepitaxy as examples. In the case of heteroepitaxy, the growth rate and optical properties are revealed by PRS using interference oscillations as they occur during growth. Super-imposed on these interference oscillations, the PRS signal exhibits a fine structure caused by the periodic alteration of the surface chemistry by the pulsed supply of chemical precursors. This fine structure is modeled under conditions where the surface chemistry cycles between phosphorus supersaturated and phosphorus depleted surfaces. The mathematical model describes the fine structure using a surface layer that increases during the tertiarybutyl phosphine (TBP) supply and decreases during and after the triethylgallium (TEG) pulse, which increases the growing GaP film thickness. The imaginary part of the dielectric function of the surface layer is revealed from the turning points in the fine structure, where the optical response to the first precursor pulse in the cycle sequence changes sign. The amplitude of the fine structure is determined by the surface layer thickness and the complex dielectric functions for the surface layer with the underlying bulk film. Surface kinetic data can be obtained by analyzing the rise and decay transients of the fine structure.

Dietz, Nikolaus↗

NASA NTRS1982

Diamond /111/ studied by electron energy loss spectroscopy in the characteristic loss region

Unoccupied surface states on diamond (111) annealed at greater than 900 C are studied by electron energy loss spectroscopy with valence band excitation. A feature found at 2.1 eV loss energy is attributed to an excitation from occupied surface states into unoccupied surface states of energy within the bulk band gap. A surface band gap of approximately 1 eV is estimated. This result supports a previous suggestion for unoccupied band gap states based on core level energy loss spectroscopy. Using the valence band excitation energy loss spectrosocpy, it is also suggested that hydrogen is removed from the as-polished diamond surface by a Menzel-Gomer-Redhead mechanism.

Pepper, S. V.↗

NASA NTRS1989

A characterization study of a hydroxylated polycrystalline tin oxide surface

In this study Auger electron spectroscopy, electron spectroscopy for chemical analysis (ESCA) and electron-stimulated desorption (ESD) have been used to examine a polycrystalline tin oxide surface before and after annealing in vacuum at 500 C. Features due to surface hydroxyl groups are present in both the ESCA and ESD spectra, and ESD shows that several chemical states of hydrogen are present. Annealing at 500 C causes a large reduction in the surface hydrogen concentration but not complete removal.

Hoflund, Gar B.↗

NASA NTRS2012

Geochemistry at 4 Vesta: Observations Using Fast Neutrons

Dawn is currently in orbit around the asteroid 4 Vesta, and one of the major objectives of the mission is to probe the relationship of Vesta to the Howardite, Eucrite, and Diogenite (HED) meteorites. As Vesta is an example of a differentiated planetary embryo, Dawn will also provide fundamental information about planetary evolution in the early solar system [1]. To help accomplish this overall goal, the Dawn spacecraft carries the Gamma-Ray and Neutron Detector (GRaND). GRaND uses planetary gamma-ray and neutron spectroscopy to measure the surface elemental composition of Vesta and will provide information that is unique and complementary to that provided by the other Dawn instruments and investigations. Gamma-ray and neutron spectroscopy is a standard technique for measuring planetary compositions [2], having successfully made measurements at near-Earth asteroids, the Moon, Mars, Mercury and now Vesta. GRaND has made the first measurements of the neutron spectrum from any asteroid (previous asteroid measurements were only made with gamma-rays). Dawn has been collecting data at Vesta since July 2011. The prime data collection period for GRaND is the Low-Altitude Mapping Orbit (LAMO), which started on 12 December 2011 and will last through spring 2012. During LAMO, the Dawn spacecraft orbits at an average altitude of ~210 km above the surface of Vesta, which allows good neutron and gamma-ray signals to be detected from Vesta. A description of the overall goals of GRaND and a summary of the initial findings are given elsewhere [3,4]. The subject of this study is to present the information that will be returned from GRaND using fast neutron measurements. Here, we discuss what fast neutrons can reveal about Vesta s surface composition, how such data can address Dawn science goals, and describe fast neutron measurements made in the early portion of the Vesta LAMO phase.

Lawrence, David J.↗

NASA NTRS2020

A Review of LIBS for Real-Time Detection of Trace Silicone Contaminants on CFRP Surfaces

Laser ablation is the removal of material by laser pulses through photochemical, photothermal, or photophysical mechanisms, which is useful to prepare an adherend surface for adhesive bonding. Laser surface treatment is a method that has been under research for the past decade at NASA Langley Research Center (LaRC) to prepare surfaces for adhesive joining of aerospace composite materials and metallic alloys. Laser ablation of composite materials increases surface area and removes the surface contaminants introduced during material handling and fabrication processes. By adjustment of laser parameters, it is possible to obtain repeatable surface conditions, and superficial contaminants can be selectively and efficiently removed without damaging the underlying carbon fibers or the carbon fiber reinforced polymer (CFRP) substrate. Laser induced breakdown spectroscopy (LIBS) is a surface characterization and inspection technique that can be seamlessly integrated into the laser surface treatment process. At NASA LaRC, a single laser system has been used for both laser surface treatment and LIBS, which enables in-situ monitoring of surface contaminants. This work focuses on the advancements at LaRC using LIBS to detect surface silicone contaminants on aerospace CFRP materials and to provide surface quality control in adhesive bonding.

Rodolfo I Ledesma↗

NASA NTRS2020

A Review of LIBS for Real-Time Detection of Trace Silicone Contaminants on CFRP Surfaces

Rodolfo I Ledesma↗

NASA NTRS1977

Auger spectroscopic examination of MgF2-coated Al mirrors before and after UV irradiation

Magnesium fluoride protected Al films were studied since these mirrors are commonly used in astronomical instruments whenever a highly reflecting optical surface is required in the wavelength region from 1100 A to 2000 A. Freshly prepared samples of evaporated Al + 250-A thick MgF2 on glass were analyzed by Auger electron spectroscopy in conjunction with surface erosion by Ar(+) ion bombardment before and after UV irradiation. The analysis showed that a very thin layer of surface contamination and not bulk photolysis in the MgF2 film was reponsible for the irradiation-induced reflectance loss. Postirradiation polishing with a mild calcium carbonate abrasive can restore a mirror's reflectance by removing the photolyzed surface film without disturbing the MgF2 layer.

Heaney, J. B.↗

NASA NTRS2013

Laboratory Instruments Available to Support Space Station Researchers at Marshall Space Flight Center

A number of research instruments are available at NASA's Marshall Space Flight Center (MSFC) to support ISS researchers and their investigations. These modern analytical tools yield valuable and sometimes new informative resulting from sample characterization. Instruments include modern scanning electron microscopes equipped with field emission guns providing analytical capabilities that include angstron-level image resolution of dry, wet and biological samples. These microscopes are also equipped with silicon drift X-ray detectors (SDD) for fast yet precise analytical mapping of phases, as well as electron back-scattered diffraction (EBSD) units to map grain orientations in crystalline alloys. Sample chambers admit large samples, provide variable pressures for wet samples, and quantitative analysis software to determine phase relations. Advances in solid-state electronics have also facilitated improvements for surface chemical analysis that are successfully employed to analyze metallic materials and alloys, ceramics, slags, and organic polymers. Another analytical capability at MSFC is a mganetic sector Secondary Ion Mass Spectroscopy (SIMS) that quantitatively determines and maps light elements such as hydrogen, lithium, and boron along with their isotopes, identifies and quantifies very low level impurities even at parts per billion (ppb) levels. Still other methods available at MSFC include X-ray photo-electron spectroscopy (XPS) that can determine oxidation states of elements as well as identify polymers and measure film thicknesses on coated materials, Scanning Auger electron spectroscopy (SAM) which combines surface sensitivity, spatial lateral resolution (approximately 20 nm), and depth profiling capabilities to describe elemental compositions in near surface regions and even the chemical state of analyzed atoms. Conventional Transmission Electron Microscope (TEM) for observing internal microstructures at very high magnifications and the Electron Probe Micro-analyzer (EPMA) for very precise microanalysis are available as needed by the researcher. Space Station researchers are invited to work with MSFC in analyzing their samples using these techniques.

Panda, Binayak↗

NASA NTRS1998

Multi-Bandwidth Frequency Selective Surfaces for Near Infrared Filtering: Design and Optimization

Frequency selective surfaces are widely used in the microwave and millimeter wave regions of the spectrum for filtering signals. They are used in telecommunication systems for multi-frequency operation or in instrument detectors for spectroscopy. The frequency selective surface operation depends on a periodic array of elements resonating at prescribed wavelengths producing a filter response. The size of the elements is on the order of half the electrical wavelength, and the array period is typically less than a wavelength for efficient operation. When operating in the optical region, diffraction gratings are used for filtering. In this regime the period of the grating may be several wavelengths producing multiple orders of light in reflection or transmission. In regions between these bands (specifically in the infrared band) frequency selective filters consisting of patterned metal layers fabricated using electron beam lithography are beginning to be developed. The operation is completely analogous to surfaces made in the microwave and millimeter wave region except for the choice of materials used and the fabrication process. In addition, the lithography process allows an arbitrary distribution of patterns corresponding to resonances at various wavelengths to be produced. The design of sub-millimeter filters follows the design methods used in the microwave region. Exacting modal matching, integral equation or finite element methods can be used for design. A major difference though is the introduction of material parameters and thicknesses that may not be important in longer wavelength designs. This paper describes the design of multi- bandwidth filters operating in the 1-5 micrometer wavelength range. This work follows on a previous design. In this paper extensions based on further optimization and an examination of the specific shape of the element in the periodic cell will be reported. Results from the design, manufacture and test of linear wedge filters built using microlithographic techniques and used in spectral imaging applications will be presented.

Cwik, Tom↗

NASA NTRS1999

Multi-Bandwidth Frequency Selective Surfaces for Near Infrared Filtering: Design and Optimization

Frequency selective surfaces are widely used in the microwave and millimeter wave regions of the spectrum for filtering signals. They are used in telecommunication systems for multi-frequency operation or in instrument detectors for spectroscopy. The frequency selective surface operation depends on a periodic array of elements resonating at prescribed wavelengths producing a filter response. The size of the elements is on the order of half the electrical wavelength, and the array period is typically less than a wavelength for efficient operation. When operating in the optical region, diffraction gratings are used for filtering. In this regime the period of the grating may be several wavelengths producing multiple orders of light in reflection or transmission. In regions between these bands (specifically in the infrared band) frequency selective filters consisting of patterned metal layers fabricated using electron beam lithography are beginning to be developed. The operation is completely analogous to surfaces made in the microwave and millimeter wave region except for the choice of materials used and the fabrication process. In addition, the lithography process allows an arbitrary distribution of patterns corresponding to resonances at various wavelengths to be produced. The design of sub-millimeter filters follows the design methods used in the microwave region. Exacting modal matching, integral equation or finite element methods can be used for design. A major difference though is the introduction of material parameters and thicknesses tha_ may not be important in longer wavelength designs. This paper describes the design of multi-bandwidth filters operating in the I-5 micrometer wavelength range. This work follows on previous design [1,2]. In this paper extensions based on further optimization and an examination of the specific shape of the element in the periodic cell will be reported. Results from the design, manufacture and test of linear wedge filters built using micro-lithographic techniques and used ir spectral imaging applications will be presented.

Cwik, Tom↗