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At least 19 records

Electron energy-loss spectroscopy of carbon in interplanetary dust particles

The nature of the carbon-bearing phases in IDP's provides information regarding the chemical and physical processes involved in the formation and evolution of the early solar system. Several carbon-bearing materials have been observed in IDP's, but details of their nature, abundance, and distribution are still poorly known. A knowledge of the abundance and nature of carbon in IDP's is useful in constraining the sources of IDP's and for comparisons with other chondritic materials. Estimates of carbon abundance in anhydrous and hydrated IDP's indicate that most of these particles have significantly higher carbon than the carbonaceous chondrites. Mineralogical analyses show that carbonates are only a minor component of most hydrated IDP's, and so the high carbon abundances in this group of IDP's indicates that other carbon-bearing phases are present in significant concentrations. Using the technique of electron energy-loss spectroscopy (EELS), we have identified two forms of carbon in a hydrated IDP, oxidized carbon (carbonates), and amorphous elemental carbon.

Keller, Lindsay P.↗

Electron Energy-Loss Spectroscopy (EELS) of Fe-bearing Sheet Silicates in CM Chondrites

The primitive character and hydrated mineralogy of the CM chondrites offers insight into some of the earliest reactions between solids and water. Such reactions profoundly affected the matrices and fine-grained rims (FGRs) [1-4], two of the most significant components of these meteorites [5]. We are using EELS combined with a transmission electron microscope (TEM) to investigate the compositions of Fe-bearing minerals, with emphasis on determining oxidation states and quantification of oxidation-state ratios. Iron is among the most abundant elements in the solar system and it can occur naturally in three oxidation states: Fe0, Fe2+, and Fe3+. Determination of oxidation- state ratios is useful because they can be used to infer the redox conditions under which the minerals formed or were last equilibrated [6, 7]. We are particularly interested in understanding how the oxidation state of Fe was affected by the aqueous reactions of the CM chondrites.

Zega, Thomas J.↗

Integrated material-surface analyzer

These 10 surface-analysis tests can be run without breaking vacuum: secondary-ion mass spectroscopy, ion-scattering spectroscopy, electron-stimulated desorption, residual-gas analysis, auger electron spectroscopy, x-ray photoelectron spectroscopy, ultraviolet photoelectron spectroscopy, characteristic-electron energy-loss spectroscopy, scanning electron microscope, scanning low-energy electron probe. Quadruple mass spectrometer, used in first 4 tests, serves as electron transfer lens in last 6 tests.

Grunthaner, F. J.↗

The nature of carbon-bearing phases in hydrated interplanetary dust particles

We have been quantitatively measuring C abundances in hydrated interplanetary dust particles for the past few years, but in general, we have had to infer the distribution and nature of the C-bearing materials within these particles because of the complex microtextures of hydrated IDPs. Aside from rare carbonate grains, other C-bearing phases are difficult to distinguish from the fine-grained, poorly crystalline phyllosilicates that comprise the bulk of these particles. We know that carbonates alone cannot account for the high C abundances observed in most hydrated IDPs and that additional C-bearing phases must be present. We have recently applied the technique of electron energy-loss spectroscopy (EELS) in the transmission electron microscope (TEM) to identify and form the distribution of C-bearing phases in hydrated IDPs. These preliminary data show that several C-rich hydrated IDPs contain a mixture of two major forms of C, Mg-Fe carbonate and amorphous C. The near-edge structure in the C k-edges from these IDPs shows no evidence for the development of graphite or even poorly graphitized C. We conclude that the 'elemental' C in these IDPs is either very poorly ordered or is exceedingly fine-grained (we refer to this C as 'amorphous C'). The amorphous C is intimately intergrown with the fine-grained phyllosilicates and is evenly distributed within three of the four IDPs analyzed (only G1 contains discrete 'hot spots' of amorphous C). Not all hydrated IDPs contain carbonates.

Keller, L. P.↗

Defect Clustering and Nano-phase Structure Characterization of Multicomponent Rare Earth-Oxide-Doped Zirconia-Yttria Thermal Barrier Coatings

Advanced thermal barrier coatings (TBCs) have been developed by incorporating multicomponent rare earth oxide dopants into zirconia-based thermal barrier coatings to promote the creation of the thermodynamically stable, immobile oxide defect clusters and/or nanophases within the coating systems. In this paper, the defect clusters, induced by Nd, Gd, and Yb rare earth dopants in the zirconia-yttria thermal barrier coatings, were characterized by high-resolution transmission electron microscopy (TEM). The TEM lattice imaging, selected area diffraction (SAD), and electron energy-loss spectroscopy (EELS) analyses demonstrated that the extensive nanoscale rare earth dopant segregation exists in the plasma-sprayed and electron-physical-vapor-deposited (EB PVD) thermal barrier coatings. The nanoscale concentration heterogeneity and the resulting large lattice distortion promoted the formation of parallel and rotational defective lattice clusters in the coating systems. The presence of the 5-to 100-nm-sized defect clusters and nanophases is believed to be responsible for the significant reduction of thermal conductivity, improved sintering resistance, and long-term high temperature stability of the advanced thermal barrier coating systems.

Zhu, Dongming↗

Electron energy loss spectra of polycyclic aromatic hydrocarbons

A survey of the electron energy-loss spectroscopy is reported of gas-phase polycyclic aromatic hydrocarbon (PAH) molecules consisting of up to seven rings where the study is limited to the more thermodynamically stable pericondensed systems. The aim of this work is to obtain absorption profiles (proportional to the oscillator strengths) from the visible to the soft X-ray region near 30 eV.

Keller, John W.↗

Chemically anomalous, pre-accretionally irradiated grains in interplanetary dust -- interstellar grains?

Ultrafine-grained matrix is a unique and fundamental building block of chondritic porous (CP) interplanetary dust particles. Most IDPs so far determined to be of cometary origin belong to the CP class. The matrix in CP IDPs is not homogeneous but rather a loose mixture of discrete single crystals (e.g., olivine, pyroxene, Fe sulfides) and polyphase grains. The petrographic diversity observed among the polyphase grains suggest that they were formed under variable physiochemical conditions. One particular class of polyphase grains are a dominant component in cometary IDPs. Although their occurrence is well documented, the terminology used to describe them is confused. They have been called many names. Here they are simply called GEMS (Glass with Embedded Metal and Sulfides). The bulk compositions of GEMS are within a factor of 3 chondritic (solar) for all major elements except C. Quantitative thin-film X-ray (EDS) analyses have shown that GEMS are systematically depleted in Mg and Si, enriched in S, Fe, and Ni, and stoichiometrically enriched in O. Electron energy-loss spectroscopy (EELS) suggests that the excess O is present as hydroxyl (-OH) groups. These same chemical 'anomalies' were observed in solar-wind-irradiated amorphous rims on the surfaces of IDPs, suggesting that the compositions of GEMS reflect prior exposure to ionizing radiation. In order to test this hypothesis, a sample of Allende (CV3) matrix was exposed to proton flux. Radiation-damaged amorphous rims on olivine and pyroxene crystals in the Allende sample were found to be depleted in Mg and Ca, enriched in S, Fe, and Ni, and stoichiometrically enriched in O. Thus, the compositions of GEMS are indeed consistent with exposure to ionizing radiation. This study suggests that chemical as well as isotopic anomalies may be used to identify presolar interstellar grains in primitive meteoritic materials.

Bradley, J. P.↗

Defect Clustering and Nano-Phase Structure Characterization of Multi-Component Rare Earth Oxide Doped Zirconia-Yttria Thermal Barrier Coatings

Advanced oxide thermal barrier coatings have been developed by incorporating multi-component rare earth oxide dopants into zirconia-yttria to effectively promote the creation of the thermodynamically stable, immobile oxide defect clusters and/or nano-scale phases within the coating systems. The presence of these nano-sized defect clusters has found to significantly reduce the coating intrinsic thermal conductivity, improve sintering resistance, and maintain long-term high temperature stability. In this paper, the defect clusters and nano-structured phases, which were created by the addition of multi-component rare earth dopants to the plasma-sprayed and electron-beam physical vapor deposited thermal barrier coatings, were characterized by high-resolution transmission electron microscopy (TEM). The defect cluster size, distribution, crystallographic and compositional information were investigated using high-resolution TEM lattice imaging, selected area diffraction (SAD), electron energy-loss spectroscopy (EELS) and energy dispersive spectroscopy (EDS) analysis techniques. The results showed that substantial defect clusters were formed in the advanced multi-component rare earth oxide doped zirconia- yttria systems. The size of the oxide defect clusters and the cluster dopant segregation was typically ranging from 5 to 50 nm. These multi-component dopant induced defect clusters are an important factor for the coating long-term high temperature stability and excellent performance.

Zhu, Dongming↗

Electron-Impact Excitation of the B ^1SIGMA^+, C^1SIGMA^+ and E^1PI States of

Electron impact excitation of CO plays an important role in planetary atmospheres andinterstellar clouds. At the present time, serious discrepancies exist among excitation cross sectionsreported in the literature for this molecule. We measured electron impact excitation cross sections forB^1SIGMA^+right arrowX^1SIGMA^+, C^1SIGMA^+right arrowX^1SIGMA^+ and E^1PIrightarrowX^1SIGMA^+ states of CO at 100eV impact energy using electron energy-loss spectroscopy.

Kanik, I.↗

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.↗

Electron-impact excitation of UF6 at an electron energy of 20 eV in the energy-loss range of 0-10 eV

A technique combining electron impact excitation and optical absorption spectroscopy was applied to UF6. The crucial features of the experiment were that: (1) the electron optics was differentially pumped relative to the scattering chamber and (2) the target UF6 beam was condensed on a liquid nitrogen cold trap placed immediately above the scattering center. Energy loss spectra are presented at an incident electron energy of 20 eV and at scattering angles between 20 and 135 degrees. It is shown that no transitions are found below the first-detected feature at 3.0 eV and an optically forbidden excitation is found at 4.2 eV. A fairly strong optical absorption at 4.8 eV is observed to 'fill-in' at a scattering angle of 20 degrees but is practically absent at higher angles.

Chutjian, A.↗

Electron energy-loss spectra in molecular fluorine

Electron energy-loss spectra in molecular fluorine, for energy losses from 0 to 17.0 eV, have been taken at incident electron energies of 30, 50, and 90 eV and scattering angles from 5 to 140 deg. Features in the spectra above 11.5 eV energy loss agree well with the assignments recently made from optical spectroscopy. Excitations of many of the eleven repulsive valence excited electronic states are observed and their location correlates reasonably well with recent theoretical results. Several of these excitations have been observed for the first time and four features, for which there are no identifications, appear in the spectra.

Nishimura, H.↗

Direct spectroscopy of electron and hole scattering

A new spectroscopy has been developed for the first direct probe of carrier-carrier scattering in materials. This spectroscopy provides spatial and energy resolution of the scattering process and has been used to investigate transport, scattering phenomena, and hot-carrier creation in two important metal-semiconductor systems. A theoretical treatment of this scattering spectroscopy yields excellent agreement with experimental spectra and provides direct evidence that carrier-carrier scattering is a dominant energy-loss mechanism in hot-carrier transport.

Bell, L. D.↗

Electron impact excitation of coronene

A preliminary study of the electron-impact excitation of thermally evaporated coronene at 550 C was carried out using electron-energy-loss spectroscopy. Measurements of the energy-loss spectra of coronene at high (100 eV) and low (5-20 eV) impact energies are presented. One of the high-energy spectra was converted to an apparent generalized oscillator strength spectrum and compared to the photoabsorption spectrum of coronene. Observations concerning vibrational excitation of coronene by electron impact are also presented and discussed.

Khakoo, M. A.↗

X-Ray Microanalysis and Electron Energy Loss Spectrometry in the Analytical Electron Microscope: Review and Future Directions

This paper reviews and discusses future directions in analytical electron microscopy for microchemical analysis using X-ray and Electron Energy Loss Spectroscopy (EELS). The technique of X-ray microanalysis, using the ratio method and k(sub AB) factors, is outlined. The X-ray absorption correction is the major barrier to the objective of obtaining I% accuracy and precision in analysis. Spatial resolution and Minimum Detectability Limits (MDL) are considered with present limitations of spatial resolution in the 2 to 3 microns range and of MDL in the 0.1 to 0.2 wt. % range when a Field Emission Gun (FEG) system is used. Future directions of X-ray analysis include improvement in X-ray spatial resolution to the I to 2 microns range and MDL as low as 0.01 wt. %. With these improvements the detection of single atoms in the analysis volume will be possible. Other future improvements include the use of clean room techniques for thin specimen preparation, quantification available at the I% accuracy and precision level with light element analysis quantification available at better than the 10% accuracy and precision level, the incorporation of a compact wavelength dispersive spectrometer to improve X-ray spectral resolution, light element analysis and MDL, and instrument improvements including source stability, on-line probe current measurements, stage stability, and computerized stage control. The paper reviews the EELS technique, recognizing that it has been slow to develop and still remains firmly in research laboratories rather than in applications laboratories. Consideration of microanalysis with core-loss edges is given along with a discussion of the limitations such as specimen thickness. Spatial resolution and MDL are considered, recognizing that single atom detection is already possible. Plasmon loss analysis is discussed as well as fine structure analysis. New techniques for energy-loss imaging are also summarized. Future directions in the EELS technique will be the development of new spectrometers and improvements in thin specimen preparation. The microanalysis technique needs to be simplified and software developed so that the EELS technique approaches the relative simplicity of the X-ray technique. Finally, one can expect major improvements in EELS imaging as data storage and processing improvements occur.

Goldstein, J. I.↗

Measurement of Absolute Excitation Cross Sections in Highly-Charged Ions Using Electron Energy Loss and Merged Beams

There is increasing emphasis during this decade on understanding energy balance and phenomena observed in high electron temperature plasmas. The UV spectral return from FUSE, the X-ray spectral return from the HETG on Chandra and the LETGS 011 XMM-Newton are just beginning. Line emissions are almost entirely from highly-charged ions (HCIs) of C, N, 0, Ne, Mg, S, Si, Ca, and Fe. The Constellation-X mission will provide X-ray spectroscopy up to photon energies of 0.12 nm (10 keV) where primary line emitters will be HCIs. A variety of atomic parameters are required to model the stellar and solar plasma. These include cross sections for excitation, ionization, charge-exchange, X-ray emission, direct and indirect recombination, lifetimes and branching ratios, and dependences on l, m mixing by external E and B fields. In almost all cases the atomic quantities are calculated, and few comparisons to experiment have been carried out. Collision strengths and Einstein A-values are required to convert the observed spectral intensities to electron temperatures and densities in the stellar plasma. The JPL electron energy-loss and merged beam approach has been used to measure absolute collision strengths in a number of ions, with critical comparison made to the best available theories.

Chutjian, A.↗