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At least 109 records · Page 6

X-ray Topographic Methods and Application to Analysis of Electronic Materials

Three supplementary X-ray techniques new to semiconductor applications are discussed. These are the Computer Aided Rocking Curve Analyzer, the Divergent Beam Method and a new method based on enhanced X-ray flourescence. The first method is used for quantitative mapping of an elastic or plastic strain field while the other two methods are used only to measure elastic strains. The divergent beam method is used for measuring the full strain tensor while the microfluorescence method is useful for monitoring strain uniformity. These methods are discussed in detail and examples of their application is presented. Among these are determination of the full strain ellipsoid in state-of-the-art liquid phase epitaxy deposited III-V epitaxial films; mapping of the plastic strain concentrations in tensile deformed Si; and quantitative determination of damage in V3Si due to ion implantation.

Mayo, W. E.↗

Surface composition of solid-rocket exhausted aluminum oxide particles

Particulate samples of aluminum oxide were collected on Teflon filters from the exhaust plume of the Space Shuttle (STS-61A, October 30, 1985) over the altitude interval 4.6-7.6 km immediately after launch. These particles were analyzed using SEM, energy-dispersive X-ray analysis, electron spectroscopy for chemical analysis, X-ray fluorescent spectroscopy, and conventional wet-chemical techniques. The samples were 0.6-1.0 percent surface-chlorided (chlorided meaning predominantly aluminum chlorides and oxychlorides, possibly including other adsorbed forms of chloride) by weight. This level of chloriding is about one-third of the amount determined previously from laboratory-prepared alumina and surface site samples of solid-rocket-produced alumina (SRPA) after both had been exposed to moist HCl vapor at temperatures down to ambient. This level is equivalent to previous laboratory results with samples exposed to moist HCl at temperatures above the boiling point of water. It is suggested that the present lower chloriding levels, determined for samples from a 'dry' Shuttle exhaust cloud, underscore the importance of a liquid water/hydrochloric acid phase in governing the extent of surface chloriding of SRPA. The reduced chloriding is not trivial with respect to potential physical/chemical modification of the SRPA particle surfaces and their corresponding interaction with the atmosphere.

Cofer, Wesley R., III↗

A comprehensive analysis of electron conical distributions from multi-satellite databases

This report consists of a copy of a paper that has been submitted to the 'Journal of Geophysical Research', entitled 'DE 1 and Viking Observations Associated With Electron Conical Distributions,' and an abstract of another paper (included as an appendix to the report) that is about to be submitted to the same journal entitled 'Perpendicular Electron Heating by Absorption of Auroral Kilometric Radiation.' A bibliography of other papers that have been published as a result of this project follows. The purpose of this project was to use the DE 1 and Viking particle and wave data to better understand the source mechanism of electron conical distributions. We have shown that electron conics are often associated with upper hybrid waves in the nightside auroral region. We have also shown that electron conics are observed near auroral kilometric radiation (AKR) source regions and may be the result of perpendicular heating due to waves. We have completed a statistical study of electron conics observed by DE-l and Viking. The study shows the occurrence frequency and location of electron conical distributions; there are some differences between the results of DE and Viking perhaps due to different regions sampled.

Menietti, J. Douglas↗

Interfacing LabVIEW With Instrumentation for Electronic Failure Analysis and Beyond

The Laboratory Virtual Instrumentation Engineering Workstation (LabVIEW) software is designed such that equipment and processes related to control systems can be operationally lined and controlled by the use of a computer. Various processes within the failure analysis laboratories of NASA's Kennedy Space Center (KSC) demonstrate the need for modernization and, in some cases, automation, using LabVIEW. An examination of procedures and practices with the Failure Analaysis Laboratory resulted in the conclusion that some device was necessary to elevate the potential users of LabVIEW to an operational level in minimum time. This paper outlines the process involved in creating a tutorial application to enable personnel to apply LabVIEW to their specific projects. Suggestions for furthering the extent to which LabVIEW is used are provided in the areas of data acquisition and process control.

Buchanan, Randy K.↗

Meta-Analysis of Electron Cyclotron Resonance Absorption Features Detected in High-Mass X-Ray Binaries

Using recent compilations of detailed X-ray observations and spectral models of exceptional quality, we record the electron cyclotron resonance absorption (ECRA) features that have been detected in 45 pulsating high-mass X-ray binaries (HMXBs) and ultraluminous X-ray (ULX) sources harboring neutron stars, although seven of these detections are still questionable and another 21 are single and/or not independently confirmed. From the comprehensive catalogs of Jaisawal & Naik and Staubert et al. and from several additional recent observations, we produce two lists of HMXB ECRA sources: a list of 17 sources in which multiple ECRA lines or single very low-energy lines are seen, in which we can reasonably assume that the lowest energy reveals the fundamental cyclotron level for each source; and a "contaminated" list of 38 sources including the 21 detections of single ECRA lines that may (not) be higher-level harmonics. Both lists confirm a previous result that we have obtained independently by modeling the propeller lines of Magellanic HMXB pulsars: the surface dipolar magnetic fields B * of HMXB neutron stars are segregated around five distinct values with B * = 0.28 ± 0.08, 0.55 ± 0.11, 1.3 ± 0.37, 3.0 ± 0.68 and 7.9 ± 3.1, in units of TG. However, an explanation of this phenomenon is currently lacking. We have found no correlation between these B * values and the corresponding observed spin periods, spin period derivatives, orbital periods, maximum X-ray luminosities, neutron star masses or companion star masses.

Christodoulou, Dimitris M.↗

Understanding TRISO Coated Particle Neutron Irradiation Behavior:Evolution of Advanced Micro Analysis and Electron Microscopy Approaches

Objectives and motivation• Provide data for fuel qualification in support of reactor licensing• Establish a domestic commercial TRISO fuel fabrication capability Approach • Focus is on developing and testing UCO TRISO fuel –Develop fuel fabrication and QC measurement methods, first at lab scale and then at industrial scale –Perform irradiation testingover a range of conditions (burnup, temperature, fast neutron fluence) –Perform post-irradiation examination and safety testingto demonstrate and understand performance during irradiation and during accident conditions –Develop fuel performance modelsto better predict fuel behavior –Perform fission product transport experiments to improve understanding and refine models of fission product transport

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

Electron image contrast analysis of mosaicity in rutile nanocrystals using direct electron detection

Direct electron detection provides high detective quantum efficiency, significantly improved point spread function and fast read-out which have revolutionized the field of cryogenic electron microscopy. However, these benefits for high-resolution electron microscopy (HREM) are much less exploited, especially for in situ study where major impacts on crystallographic structural studies could be made. By using direct detection in electron counting mode, rutile nanocrystals have been imaged at high temperature inside an environmental transmission electron microscope. The improvements in image contrast are quantified by comparison with a charge-coupled device (CCD) camera and by image matching with simulations using an automated approach based on template matching. Together, these approaches enable a direct measurement of 3D shape and mosaicity (~1°) of a vacuum-reduced TiO 2 nanocrystal about 50 nm in size. Thus, this work demonstrates the possibility of quantitative HREM image analysis based on direct electron detection.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Controlling superstructural ordering in the clathrate-I Ba 8 M 16 P 30 (M = Cu, Zn) through the formation of metal–metal bonds

Order–disorder–order phase transitions in the clathrate-I Ba 8 Cu 16 P 30 were induced and controlled by aliovalent substitutions of Zn into the framework. Unaltered Ba 8 Cu 16 P 30 crystallizes in an ordered orthorhombic ( Pbcn ) clathrate-I superstructure that maintains complete segregation of metal and phosphorus atoms over 23 different crystallographic positions in the clathrate framework. The driving force for the formation of this Pbcn superstructure is the avoidance of Cu–Cu bonds. This superstructure is preserved upon aliovalent substitution of Zn for Cu in Ba 8 Cu 16– x Zn x P 30 with 0 < x < 1.6 (10% Zn/M total ), but vanishes at greater substitution concentrations. Higher Zn concentrations (up to 35% Zn/M total ) resulted in the additional substitution of Zn for P in Ba 8 M 16+ y P 30– y (M = Cu, Zn) with 0 ≤ y ≤ 1. This causes the formation of Cu–Zn bonds in the framework, leading to a collapse of the orthorhombic superstructure into the more common cubic subcell of clathrate-I ( Pm n ). In the resulting cubic phases, each clathrate framework position is jointly occupied by three different elements: Cu, Zn, and P. Detailed structural characterization of the Ba–Cu–Zn–P clathrates-I via single crystal X-ray diffraction, joint synchrotron X-ray and neutron powder diffractions, pair distribution function analysis, electron diffraction and high-resolution electron microscopy, along with elemental analysis, indicates that local ordering is present in the cubic clathrate framework, suggesting the evolution of Cu–Zn bonds. For the compounds with the highest Zn content, a disorder–order transformation is detected due to the formation of another superstructure with trigonal symmetry and Cu–Zn bonds in the clathrate-I framework. It is shown that small changes in the composition, synthesis, and crystal structure have significant impacts on the structural and transport properties of Zn-substituted Ba 8 Cu 16 P 30 .

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Methods of shield analysis for protection against electrons in space

It is anticipated that many future manned space operations will be radiation limited and that laminated wall structures and the use of new materials will be required to reduce radiation exposure. Methods for electron shield analysis are reviewed in light of anticipated needs in the space program. The most general method is still the Monte Carlo method, which is of limited usefulness for shield analysis due to excessive computer requirements. Methods based on energy deposition coefficients or energy transmission and reflection factors are quite accurate, but are currently limited to aluminum shield material. Analytical methods based on Mar's approximation for the electron transmission factor are relatively general and computer efficient but seriously underestimate shield requirements. A correction to methods using Mar's approximate transmission factor is derived herein and results in a slightly conservative estimate of shield requirements. Techniques for laminated shield design are still lacking.

Wilson, J. W.↗

The Combined Detection of Morphological and Molecular Biomarkers: Implications for Astrobiology

Experience gathered by previous researchers during their hunt for evidence of early Earth life has shown the complexity in interpreting observations of possible microfossils and to establish the evidence to be positive. Similarly, the stillsimmering controversy on the nature of the nano-structures in Martian meteorite ALH84001 described by McKay et al. (1996) emphasizes the difficulties of conclusively identifying those structures as (a) fossilized bacterial cells and (b) establish their indigeneity. A better understanding of biological signatures in rocks is needed in order to identify traces of microbial life, which include morphological, mineralogical and chemical traces. It is thus considered crucial to tackle the problems emerging in the search for evidence of early life on Earth and in exopaleontological research with a multidisciplinary approach. With this is mind we applied surface sensitive Time of Flight-Secondary Ion Mass Spectroscopy (ToF-SIMS) to a previously described 25 m.y. old fossil bacterial biofilm. This technique allows in situ analysis with high mass resolution as well as molecular imaging of micron sized structures. As no extraction or derivatisation of the sample is required for ToF-SIMS analysis, electron microscopical investigation of the same samples subsequent to analysis is possible, thus allowing the combination of molecular and morphological biomarkers. The analysed fossil bacterial biofilms were associated with macrofossils from volcanoclastic lacustrine sediments from the Upper Oligocene Enspel formation (Germany). Preliminary scanning electron microscopy (SEM) studies have shown that a fossil structure interpreted as a coprolite purely consisted of fossilized bacterial biofilm. For ToF-SIMS investigation small particles were taken from the fossil biofilm and mounted onto Au-coated In-foil and analysed in a Phi Evans T-2000 TRIFT system. The ToF-SIMS analysed samples were Au/Pd-sputter coated and imaged using a Philips XL40 Field Emission Gun SEM (FEG-SEM). ToF-SIMS analysis of the organic rich fossil biofilm (TOC 29%) in the 0-100 Dalton (Da) range showed significant amounts of inorganic species, confirming the results obtained previously by EDX analysis, clearly showing the bacterial fossils to be mineralised. ToF-SIMS furthermore revealed the presence of a variety of low- and high-mass organic molecules and fragments thereof. These include peaks indicative of alkenes and alkanes, aromatic organic species and the polycyclic aromatic hydrocarbon naphthalene. More tentatively, peaks indicative of alkyl pyrroles and pyridyl-CH2 were identified. Other peaks of interest include peaks indicative of C(n)H(2n)O2 and C(n)H(2n-2)O2, which according to their general formula would suggest the presence of both saturated and unsaturated fatty acids although further in situ derivatisation experiments and GC-MS (Gas Chromatography MS) need to be applied to verify this beyond doubt. Furthermore, peaks at m/z 370, 384, 398, 412, 426, 440, 454 and 468 were identified, which indicate the potential presence of bacterial hopanes, a class of biomarkers indicative of bacteria. The main diagnostic peak for this group of chemicals is the fragment at m/z 191.18. Our studies conducted on purified hopane standards have shown that in the high-mass resolution mode differentiation of this diagnostic hopane peak and polyethylene at m/z 191.05 is possible. However, the spectra discussed here were collected in the lower resolution mapping mode, therefore this differentiation was not possible. The centroids of the possible hopane peaks obtained on the fossil biofilms are well within the range associated with bacterial hopanes. There is a strong possibility therefore that hopanoids may be associated with the fossil bacterial cells. Due to the non-destructive nature of ToF-SIMS, analysed samples can be studied using SEM, thus allowing the combination of morphological and molecular biomarkers. Subsequent SEM analysis of the ToF-SIMS analysed samples confirmed that the analysed material purely consists of fossil bacterial cells. This is thus the first successful effort to demonstrate the combination of spectral and morphological biomarkers. The advantages of highly sensitive non-destructive in situ analysis techniques for biomarker detection are invaluable, particularly with respect to envisaged Mars sample return missions, as it may allow us to identify remains and traces of former microbial life in both ancient terrestrial and extraterrestrial materials. This technique may prove particularly useful in the quest for extraterrestrial life with respect to precious extraterrestrial materials, as minute quantities are sufficient to conduct analysis.

Toporski, J.↗