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NASA NTRS1972

Structure of lunar glasses by Raman and soft X-ray spectroscopy.

X-ray spectra and Raman spectra have been measured from individual particles of lunar glasses. Each particle was analyzed separately by electron microprobe. Silicon emission shifts vary between parent rock types and can be interpreted as a range of Si-O distances from 1.612 to 1.637 A. Aluminum emission shifts relate to the amount of 4- and 6-coordinated Al in the glass. Raman spectra show broadened bands. Certain bands recur in many specimens and relate to the main normative minerals for the glass bulk composition, olivine, pyroxene, and anorthite.

Fabel, G. W.↗

NASA NTRS1984

Coordination of Fe, Ga and Ge in high pressure glasses by Moessbauer, Raman and X-ray absorption spectroscopy, and geological implications

For some time, it has been recognized that the structure of silicate liquids has a great bearing on such magma properties as viscosity, diffusivity, and thermal expansion and on the extrapolation of thermodynamic quantities outside of the experimentally measurable range. In this connection it is vital to know if pressure imposes changes in melt structure similar to the pressure-induced reconstructive transformations in crystals. In the present study on 1 bar and high pressure glasses, an investigation is conducted regarding the coordination of Fe(3+) in Fe silicate glasses by Moessbauer spectroscopy. Raman spectroscopy is employed to explore the coordinations of Ge(4+) in GeO2 glasses and of Ga(3+) in NaGa silicate glasses, while the coordination of Ga(3+) in NaGaSiO4 glasses is studied with the aid of methods of X-ray absorption spectroscopy.

Fleet, M. E.↗

NASA NTRS1992

Synthesis and characterization of fine grain diamond films

A fine grain diamond film has been developed by microwave plasma assisted chemical vapor deposition. Various analytical techniques, including Rutherford backscattering, proton recoil analysis, Raman spectroscopy, and X-ray diffraction, were utilized to characterize the diamond films. The grain size of the film was determined from bright and dark field electron micrographs, and found to be 200-1000 A. The films exhibited good optical transmission between 2.5 and 10 microns, with a calculated absorption coefficient of 490/cm. The friction coefficients of this film were found to be 0.035 and 0.030 at dry nitrogen and humid air environments, respectively, and the films had low wear rates.

Wu, Richard L. C.↗

NASA NTRS1972

Quantitative micro-luminescence and related studies of fine and/or glassy lunar surface materials

Papers on Raman and soft X-ray spectroscopy of lunar glasses and electron microscopy of lunar fines are presented. Individual particles of glasses from Apollo 11, 12, 14, and 15 samples were analyzed separately. Silicon emission shifts vary between parent rock types and can be interpreted as a range of Si-O distances from 1.612 to 1.637 A. Aluminum emission shifts relate to the amount of 4- and 6-coordinated Al in the glass. Raman spectra show broadened bands. Certain bands recur in many specimens and relate to the main normative minerals for the glass bulk composition, olivine, pyroxene, and anorthite. Quantitative size and shape analyses were carried out on six Apollo 14 and 15 samples of fines by computer evaluation of scanning electron microspace images. For the size range of 0.50 to 30 micron diameter, the distributions are log-normal on a number count basis. Aspect ratios range from 0.1 to 1.0 with an average value of about 0.6. The aspect ratios and a shape complexity factor vary only slightly among the samples.

Roy, R.↗

NASA NTRS1994

Structure and stability of hydrous minerals at high pressure

The presence of even small amounts of hydrogen in the Earth's deep interior may have profound effects on mantle melting, rheology, and electrical conductivity. The recent discovery of a large class of high-pressure H-bearing silicates further underscores the potentially important role for hydrous minerals in the Earth's mantle. Hydrogen may also be a significant component of the Earth's core, as has been recently documented by studies of iron hydride at high pressure. In this study, we explore the role of H in crystal structures at high pressure through detailed Raman spectroscopic and x ray diffraction studies of hydrous minerals compressed in diamond anvil cells. Brucite, Mg(OH)2, has a simple structure and serves as an analogue for the more complex hydrous silicates. Over the past five years, this material has been studied at high pressure using shock-compression, powder x ray diffraction, infrared spectroscopy, Raman spectroscopy, and neutron diffraction. In addition, we have recently carried out single-crystal synchrotron x-ray diffraction on Mg(OH)2 and Raman spectroscopy on Mg(OD)2 at elevated pressure. From all these studies, an interesting picture of the crystal chemical behavior of this material at high pressure is beginning to emerge. Some of the primary conclusions are as follows: First, hydrogen bonding is enhanced by the application of pressure. Second, layered minerals which are elastically anisotropic at low pressure may not be so at high pressure. Furthermore, the brucite data place constraints on the effect of hydrogen on seismic velocities and density at very high pressure. Third, the stability of hydrous minerals may be enhanced at high P by subtle structural rearrangements that are difficult to detect using traditional probes and require detailed spectroscopic analyses. Finally, brucite appears to be unique in that it undergoes pressure-induced disordering that is confined solely to the H-containing layers of the structure.

Duffy, T. S.↗

NASA NTRS1995

Low temperature Zn diffusion for GaSb solar cell structures fabrication

Low temperature Zn diffusion in GaSb, where the minimum temperature was 450 C, was studied. The pseudo-closed box (PCB) method was used for Zn diffusion into GaAs, AlGaAs, InP, InGaAs and InGaAsP. The PCB method avoids the inconvenience of sealed ampoules and proved to be simple and reproducible. The special design of the boat for Zn diffusion ensured the uniformality of Zn vapor pressure across the wafer surface, and thus the uniformity of the p-GaSb layer depth. The p-GaSb layers were studied using Raman scattering spectroscopy and the x-ray rocking curve method. As for the postdiffusion processing, an anodic oxidation was used for a precise thinning of the diffused GaSb layers. The results show the applicability of the PCB method for the large-scale production of the GaSb structures for solar cells.

Sulima, Oleg V.↗

NASA NTRS1999

Surface Diagnostics in Tribology Technology and Advanced Coatings Development

This paper discusses the methodologies used for surface property measurement of thin films and coatings, lubricants, and materials in the field of tribology. Surface diagnostic techniques include scanning electron microscopy, transmission electron microscopy, atomic force microscopy, stylus profilometry, x-ray diffraction, electron diffraction, Raman spectroscopy, Rutherford backscattering, elastic recoil spectroscopy, and tribology examination. Each diagnostic technique provides specific measurement results in its own unique way. In due course it should be possible to coordinate the different pieces of information provided by these diagnostic techniques into a coherent self-consistent description of the surface properties. Examples are given on the nature and character of thin diamond films.

Miyoshi, Kazuhisa↗

NASA NTRS1999

Measurements and Diagnostics of Diamond Films and Coatings

The commercial potential of chemical-vapor-deposited (CVD) diamond films has been established and a number of applications have been identified through university, industry, and government research studies. This paper discusses the methodologies used for property measurement and diagnostic of CVD diamond films and coatings. Measurement and diagnostic techniques studied include scanning electron microscopy, transmission electron microscopy, atomic force microscopy, stylus profilometry, x-ray diffraction, electron diffraction, Raman spectroscopy, Rutherford backscattering, elastic recoil spectroscopy, and friction examination. Each measurement and diagnostic technique provides unique information. A combination of techniques can provide the technical information required to understand the quality and properties of CVD diamond films, which are important to their application in specific component systems and environments. In this study the combination of measurement and diagnostic techniques was successfully applied to correlate deposition parameters and resultant diamond film composition, crystallinity, grain size, surface roughness, and coefficient of friction.

Miyoshi, Kazuhisa↗

NASA NTRS1998

Tribometer for Lubrication Studies in Vacuum

The NASA Lewis Research Center has developed a new way to evaluate the liquid lubricants used in ball bearings in space mechanisms. For this evaluation, a liquid lubricant is exercised in the rolling contact vacuum tribometer shown in the photo. This tribometer, which is essentially a thrust bearing with three balls and flat races, has contact stresses similar to those in a typical preloaded, angular contact ball bearing. The rotating top plate drives the balls in an outward-winding spiral orbit instead of a circular path. Upon contact with the "guide plate," the balls are forced back to their initial smaller orbit radius; they then repeat this spiral orbit thousands of times. The orbit rate of the balls is low enough, 2 to 5 rpm, to allow the system to operate in the boundary lubrication regime that is most stressful to the liquid lubricant. This system can determine the friction coefficient, lubricant lifetime, and species evolved from the liquid lubricant by tribodegradation. The lifetime of the lubricant charge is only few micrograms, which is "used up" by degradation during rolling. The friction increases when the lubricant is exhausted. The species evolved by the degrading lubricant are determined by a quadrupole residual gas analyzer that directly views the rotating elements. The flat races (plates) and 0.5-in.-diameter balls are of a configuration and size that permit easy post-test examination by optical and electron microscopy and the full suite of modern surface and thin-film chemical analytical techniques, including infrared and Raman microspectroscopy and x-ray photoelectron spectroscopy. In addition, the simple sphere-on-a-flat-plate geometry allows an easy analysis of the contact stresses at all parts of the ball orbit and an understanding of the frictional energy losses to the lubricant. The analysis showed that when the ball contacts the guide plate, gross sliding occurs between the ball and rotating upper plate as the ball forced back to a smaller orbit radius. The friction force due to gross sliding is sensed by the piezoelectric force transducer behind the guide plate and furnishes the coefficient of friction for the system. This tribometer has been used to determine the relative lifetimes of Fomblin Z-25, a lubricant often used in space mechanisms, as a function of the material of the plates against which it was run. The balls were 440C steel in all cases; the plate materials were aluminum, chromium (Cr), 440C steel (17 wt % Cr), and 4150 steel (1 wt % Cr). As shown in the bar graph, the lifetime is greatest for the plate material with least chromium, thus implicating chromium as a tribochemically active element attacking Fomblin Z-25.

Pepper, Stephen V.↗

NASA NTRS1984

Characterization and measurement of polymer wear

Analytical tools which characterize the polymer wear process are discussed. The devices discussed include: visual observation of polymer wear with SEM, the quantification with surface profilometry and ellipsometry, to study the chemistry with AES, XPS and SIMS, to establish interfacial polymer orientation and accordingly bonding with QUARTIR, polymer state with Raman spectroscopy and stresses that develop in polymer films using a X-ray double crystal camera technique.

Buckley, D. H.↗

NASA NTRS1985

Characterization and measurement of polymer wear

Buckley, D. H.↗

NASA NTRS1994

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↗

NASA NTRS1996

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↗

NASA NTRS1992

The growth and characterization of Al(x)Ga(1-x)As/Ge heterostructures

The effects of the growth temperature and the Al(x)Ga(1-x)As layer thickness on the structural, optical, and electrical properties of Al(x)Ga(1-x)As/Ge heterostructures grown for photovoltaic applications were investigated using different-thickness (between 1 micron and 5 microns) Al(x)Ga(1-x)As layers grown by MOCVD in the temperature range between 660 and 780 C. Results obtained from double-crystal X-ray rocking curve measurements, electron beam induced current, cross-sectional TEM, Raman spectroscopy, SIMS, and steady-state and time-resolved photoluminescence measurements are presented. It was found that the highest minority carrier lifetime, 2.41 ns, was obtained for T(G) = 780 C, but the lowest interfacial recombination velocity, 1.6 x 10 exp 4, was obtained at 660 C.

Choi, S. W.↗

NASA NTRS1994

Raman structural studies of the nickel electrode

The objectives of this investigation have been to define the structures of charged active mass, discharged active mass, and related precursor materials (alpha-phases), with the purpose of better understanding the chemical and electrochemical reactions, including failure mechanisms and cobalt incorporation, so that the nickel electrode may be improved. Although our primary tool has been Raman spectroscopy, the structural conclusions drawn from the Raman data have been supported and augmented by three other analysis methods: infrared spectroscopy, powder X-ray Diffraction (XRD), and x-ray absorption spectroscopy (in particular EXAFS, Extended X-ray Absorption Fine Structure spectroscopy).

Cornilsen, Bahne C.↗

NASA NTRS1999

A Mossbauer investigation of iron-rich terrestrial hydrothermal vent systems: lessons for Mars exploration

Hydrothermal spring systems may well have been present on early Mars and could have served as a habitat for primitive life. The integrated instrument suite of the Athena Rover has, as a component on the robotic arm, a Mossbauer spectrometer. In the context of future Mars exploration we present results of Mossbauer analysis of a suite of samples from an iron-rich thermal spring in the Chocolate Pots area of Yellowstone National Park (YNP) and from Obsidian Pool (YNP) and Manitou Springs, Colorado. We have found that Mossbauer spectroscopy can discriminate among the iron-bearing minerals in our samples. Those near the vent and on the surface are identified as ferrihydrite, an amorphous ferric mineraloid. Subsurface samples, collected from cores, which are likely to have undergone inorganic and/or biologically mediated alteration (diagenesis), exhibit spectral signatures that include nontronite (a smectite clay), hematite (alpha-Fe2O3), small-particle/nanophase goethite (alpha-FeOOH), and siderite (FeCO3). We find for iron minerals that Mossbauer spectroscopy is at least as efficient in identification as X-ray diffraction. This observation is important from an exploration standpoint. As a planetary surface instrument, Mossbauer spectroscopy can yield high-quality spectral data without sample preparation (backscatter mode). We have also used field emission scanning electron microscopy (FESEM), in conjunction with energy-dispersive X ray (EDX) fluorescence spectroscopy, to characterize the microbiological component of surface sinters and the relation between the microbiological and the mineralogical framework. Evidence is presented that the minerals found in these deposits can have multi-billion-year residence times and thus may have survived their possible production in a putative early Martian hot spring up to the present day. Examples include the nanophase property and the Mossbauer signature for siderite, which has been identified in a 2.09-billion-year old hematite-rich chert stromatolite. Our research demonstrates that in situ Mossbauer spectroscopy can help determine whether hydrothermal mineral deposits exist on Mars, which is significant for exobiology because of the issue of whether that world ever had conditions conductive to the origin of life. As a useful tool for selection of samples suitable for transport to Earth, Mossbauer spectroscopy will not only serve geological interests but will also have potential for exopaleontology.

NASA Discipline Exobiology↗

NASA NTRS1985

Raman structural studies of the nickel electrode

Raman spectroscopy is sensitive to empirically controlled nickel electrode structural variations, and has unique potential for structural characterization of these materials. How the structure relates to electrochemical properties is examined so that the latter can be more completely understood, controlled, and optimized. Electrodes were impregnated and cycled, and cyclic voltammetry is being used for electrochemical characterization. Structural variation was observed which has escaped detection using other methods. Structural changes are induced by: (1) cobalt doping, (2) the state of change or discharge, (3) the preparation conditions and type of buffer used, and (4) the formation process. Charged active mass has an NiOOH-type structure, agreeing with X-ray diffraction results. Discharged active mass, however, is not isostructural with beta-Ni(OH)2. Chemically prepared alpha phases are not isostructural either. A disordered structural model, containing point defects, is proposed for the cycled materials. This model explains K(+) incorporation. Band assignments were made and spectra interpreted for beta-Ni(OH)2, electrochemical NiOOH and chemically precipitated NiOOH.

Cornilsen, B. C.↗

NASA NTRS1996

Synthesis, Structure, and Characterization of Cu4S10(4-methylpyridine)4

The title compound, Cu4S10(4-methylpyridine)(sub 4) (dot) 4-methylpyridine was prepared by three different reactions: the oxidation of copper powder by sulfur and the reaction of copper (I) sulfide (or CuBr (dot) SMe2) with excess sulfur, both in the coordinating solvent, 4-methylpyridine. Red crystals of the compound obtained by layering with hexanes were subjected to single crystal X-ray diffraction. The structure was refined to R = 0.026 and R(sub w) = 0.036 in a space group P1bar (No. 2), with Z = 2, a = 13.983 (2) A, b = 15.384 (2) A, c = 9.660 (1) A, alpha = 93.87 (1)deg., beta = 93.38 (1)deg., gamma = 99.78 (1)deg., V = 2037.9 (9) A(exp 3). The compound has approximate S(sub 4) symmetry and consists of two pentasulfide chains linking four Cu(I) ions, each with a corrdinating 2-methylpyridine. The infrared spectrum was dominated by absorption due to coordinated 4-methylpyridine with several low-energy peaks attributable to S-S stretches, which were also observed by Raman spectroscopy. A featureless electronic absorption spectrum yielded a single peak in the near ultraviolet upon computer enhancement (lambda = 334 nm, epsilon = 10,000), most likely an intraligand transition. Cyclic voltammetry indicates that the polysulfide complex undergoes irrversible oxidation and reduction at +0.04 and -0.34 V vs. SCE, respectively, at 298 K in 4-methylpyridine when swept at 20 mV/sec. The electrochemical behavior was unvaried even at sweep rates as high as 100 V/sec.

Hepp, Aloysius F.↗