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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.

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At least 37 records · Page 2
All sourcesNASA NTRSDOE OSTI
NASA NTRS1992

Definition of the Spatial Resolution of X-Ray Microanalysis in Thin Foils

The spatial resolution of X-ray microanalysis in thin foils is defined in terms of the incident electron beam diameter and the average beam broadening. The beam diameter is defined as the full width tenth maximum of a Gaussian intensity distribution. The spatial resolution is calculated by a convolution of the beam diameter and the average beam broadening. This definition of the spatial resolution can be related simply to experimental measurements of composition profiles across interphase interfaces. Monte Carlo calculations using a high-speed parallel supercomputer show good agreement with this definition of the spatial resolution and calculations based on this definition. The agreement is good over a range of specimen thicknesses and atomic number, but is poor when excessive beam tailing distorts the assumed Gaussian electron intensity distributions. Beam tailing occurs in low-Z materials because of fast secondary electrons and in high-Z materials because of plural scattering.

Williams, D. B.↗
NASA NTRS2000

Laboratory Astrophysics and Microanalysis with NTD-Germanium-Based X-Ray Microcalorimeter

With the ability to create cosmic plasma conditions in the laboratory it is possible to investigate the dependencies of key diagnostic X-ray lines on density, temperature, and excitation conditions that exist in astrophysical sources with X-ray optics and a high resolution x-ray microcalorimeter. The same instrumentation can be coupled to scanning electron microscopes or x-ray fluorescence probes to analyze the elemental and chemical composition of electronic, biological, geological and particulate materials. We describe how our microcalorimeter and x-ray optics provide significantly improved capabilities for laboratory astrophysics and microanalysis.

Silver, E.↗
NASA NTRS2004

Improvements in Electron-Probe Microanalysis: Applications to Terrestrial, Extraterrestrial, and Space-Grown Materials

Improvement in the accuracy of electron-probe microanalysis (EPMA) has been accomplished by critical assessment of standards, correction algorithms, and mass absorption coefficient data sets. Experimental measurement of relative x-ray intensities at multiple accelerating potential highlights errors in the absorption coefficient. The factor method has been applied to the evaluation of systematic errors in the analysis of semiconductor and silicate minds. Accurate EPMA of Martian soil stimulant is necessary in studies that build on Martian rover data in anticipation of missions to Mars.

Carpenter, Paul↗
NASA NTRS2005

Quantitative Electron Probe Microanalysis: State of the Art

Quantitative electron-probe microanalysis (EPMA) has improved due to better instrument design and X-ray correction methods. Design improvement of the electron column and X-ray spectrometer has resulted in measurement precision that exceeds analytical accuracy. Wavelength-dispersive spectrometer (WDS) have layered-dispersive diffraction crystals with improved light-element sensitivity. Newer energy-dispersive spectrometers (EDS) have Si-drift detector elements, thin window designs, and digital processing electronics with X-ray throughput approaching that of WDS Systems. Using these systems, digital X-ray mapping coupled with spectrum imaging is a powerful compositional mapping tool. Improvements in analytical accuracy are due to better X-ray correction algorithms, mass absorption coefficient data sets,and analysis method for complex geometries. ZAF algorithms have ban superceded by Phi(pz) algorithms that better model the depth distribution of primary X-ray production. Complex thin film and particle geometries are treated using Phi(pz) algorithms, end results agree well with Monte Carlo simulations. For geological materials, X-ray absorption dominates the corretions end depends on the accuracy of mass absorption coefficient (MAC) data sets. However, few MACs have been experimentally measured, and the use of fitted coefficients continues due to general success of the analytical technique. A polynomial formulation of the Bence-Albec alpha-factor technique, calibrated using Phi(pz) algorithms, is used to critically evaluate accuracy issues and can be also be used for high 2% relative and is limited by measurement precision for ideal cases, but for many elements the analytical accuracy is unproven. The EPMA technique has improved to the point where it is frequently used instead of the petrogaphic microscope for reconnaissance work. Examples of stagnant research areas are: WDS detector design characterization of calibration standards, and the need for more complete treatment of the continuum X-ray fluorescence correction.

Carpernter, P. K.↗
NASA NTRS2006

Calibration Issues and Operating System Requirements for Electron-Probe Microanalysis

Instrument purchase requirements and dialogue with manufacturers have established hardware parameters for alignment, stability, and reproducibility, which have helped improve the precision and accuracy of electron microprobe analysis (EPMA). The development of correction algorithms and the accurate solution to quantitative analysis problems requires the minimization of systematic errors and relies on internally consistent data sets. Improved hardware and computer systems have resulted in better automation of vacuum systems, stage and wavelength-dispersive spectrometer (WDS) mechanisms, and x-ray detector systems which have improved instrument stability and precision. Improved software now allows extended automated runs involving diverse setups and better integrates digital imaging and quantitative analysis. However, instrumental performance is not regularly maintained, as WDS are aligned and calibrated during installation but few laboratories appear to check and maintain this calibration. In particular, detector deadtime (DT) data is typically assumed rather than measured, due primarily to the difficulty and inconvenience of the measurement process. This is a source of fundamental systematic error in many microprobe laboratories and is unknown to the analyst, as the magnitude of DT correction is not listed in output by microprobe operating systems. The analyst must remain vigilant to deviations in instrumental alignment and calibration, and microprobe system software must conveniently verify the necessary parameters. Microanalysis of mission critical materials requires an ongoing demonstration of instrumental calibration. Possible approaches to improvements in instrument calibration, quality control, and accuracy will be discussed. Development of a set of core requirements based on discussions with users, researchers, and manufacturers can yield documents that improve and unify the methods by which instruments can be calibrated. These results can be used to continue improvements of EPMA.

Carpenter, P.↗
NASA NTRS2011

Correlated Microanalysis of Cometary Organic Grains Returned by Stardust

Preliminary examination (PE) of samples returned from Comet 81P/Wild 2 by the NASA Stardust mission revealed a wide variety of carbonaceous samples [e.g. 1]. Carbonaceous matter is present as inclusions, rinds, and films in polyminerallic terminal particles [2-4], as carbon-rich particles along track walls [2, 5, 6], and as organic matter in aerogel around tracks [7, 8]. The organic chemistry of these samples ranges from purely aliphatic hydrocarbons to highly-aromatic material, often modified by various organic functional groups [2, 4, 5, 9-11]. Difficulty arises when interpreting the genesis of these carbonaceous samples, since contaminants could be introduced from the spacecraft [12], aerogel [1, 8], or during sample preparation. In addition, hypervelocity capture into aerogel may have heated cometary material in excess of 1000 C, which could have significantly altered the structure and chemistry of carbonaceous matter. Fortunately, much of this contamination or alteration can be identified through correlated microanalysis with transmission electron microscopy (TEM), scanning-transmission X-ray microscopy (STXM), and nanoscale secondary ion mass spectroscopy (SIMS).

DeGregorio, B. T.↗
NASA NTRS2014

Impacts on the Hubble Space Telescope Wide Field and Planetary Camera 2: Microanalysis and Recognition of Micrometeoroid Compositions

Postflight surveys of the Wide Field and Planetary Camera 2 (WFPC2) on the Hubble Space Telescope have located hundreds of features on the 2.2 by 0.8 m curved plate, evidence of hypervelocity impact by small particles during 16 years of exposure to space in low Earth orbit (LEO). The radiator has a 100 - 200 micron surface layer of white paint, overlying 4 mm thick Al alloy, which was not fully penetrated by any impact. Over 460 WFPC2 samples were extracted by coring at JSC. About half were sent to NHM in a collaborative program with NASA, ESA and IBC. The structural and compositional heterogeneity at micrometer scale required microanalysis by electron and ion beam microscopes to determine the nature of the impactors (artificial orbital debris, or natural micrometeoroids, MM). Examples of MM impacts are described elsewhere. Here we describe the development of novel electron beam analysis protocols, required to recognize the subtle traces of MM residues.

Kearsley, A. T.↗
DOE OSTI2024

Final Technical Report - Rapid Surface Microanalysis using a Low Temperature Plasma

This project focused on improving our current understanding and scientific knowledge in the area of plasma-surface interactions and plasma assisted material synthesis related to advanced microelectronics and nanotechnology. Current challenges include: controlling the interaction of Low Temperature Plasma (LTP) with a single layer of atoms to manufacture integrated circuits, continued miniaturization of integrated circuits, LTP processing of material surfaces and thin films to enable industrial scale fabrication of advanced microelectronics, synthesis of new materials, nanomaterials, nanotubes, and complex materials, Technology developed in this subtopic is of value to either (i) enable scans of surfaces (~1 sq. cm area) using various microscopies (electron, optical, other) at high resolution (micron or sub-micron resolution) rapidly (hours or days rather than years to complete a high-resolution scan of such a large surface area), or (ii) enable scans of surfaces (~1 sq. cm area) using various microscopies (electron, optical, other) at relatively low resolution rapidly, then apply algorithms to select spots for micron-scale imaging. Sputtering occurs when particles of a solid material are ejected from its surface by energetic particles from a plasma. While the degradation of the solid material and the subsequent deposition of the ejected material onto vulnerable surfaces are the usual subjects of sputtering studies, plasma science has yet to be combined with sputtering to create new diagnostics devices and systems. Small changes in the design of the plasma discharge device make it possible to create broad plasma beams for rapid scanning or small plasma beams to obtain the distribution of ejected elements with micron resolution. In the high-resolution use, the ion flux is extracted from the gas-discharge plasma and focused by a spherical emission surface to micron sizes onto the target specimen, providing very local sputtering and local elemental analysis. We call this “self-focusing”. The radiation from the excited and ionized sputtered atoms is recorded by a spectrometer through a window and fiberglass cable and analyzed with standard software packages used for optical glow discharge spectroscopy. Computer simulations of beam formation were used to verify and optimize the designs to be tested. A prototype was designed, constructed, and used to start experiments of beam formation.

70 PLASMA PHYSICS AND FUSION TECHNOLOGY↗
DOE OSTI2024

Precise Compositional Characterization of Plutonium Alloys by Electron Probe Microanalysis

Key Takeaway Points: • Unlike most other materials, the precise compositional analysis of plutonium, including compounds and alloys, is riddled by numerous difficulties that are unique to the element, including the high atomic number and radioactive nature. There’s work to be done! • Radioactive materials require special handling to ensure precise compositions can be measured by EPMA. • Mean Atomic Number background corrections are limited due to high average atomic number. • Mass Absorption Coefficients are unknown for most light elements. Quantification relies upon calibration curves. • Principal Component Analysis could be a useful tool to improve interpretation of complicated, multiple element X-ray maps.

Maner, IV, James L.↗
NASA NTRS1974

X-ray spectral microanalysis of composition of individual lunar regolith particles

Determinations were made of the chemical compositions of selected olivine crystals, spherical particles ranging in size from 170 to 350 micrometer, spinels, and magnetic particles. The olivines contain 30 to 50 mole percent fayalite. The spherical particles of various colors are aluminosilicate glasses, significantly enriched in CaO compared with the mean composition of the regolith. The degree of coloration depends on the FeO content and also the admixtures TiO2, MnO, and Cr2O3. Compositionally, the spinel was interpreted to be chromopicotites. Magnetic particles were shown to be complex intergrowths of nickelous iron and aluminosilicates. The composition of the metallic phase of one particle (in percent) was: Fe - 86, Ni - 13.6, and Co - 0.16 in combination with plagioclase and microinclusions of ilmenite in silicate. Kamacite was determined in another intergrowth of Fe, Ni, and Co.

Ilin, N. P.↗
NASA NTRS1975

Exploratory study on microanalysis of thin films by backscattering techniques

Solid phase epitaxial growth of Si layers was studied by backscattering spectrometry for controllable electrical characteristics. Samples were fabricated by vacuum deposition on a thin layer of Sb before deposition of the amorphous Si layer. Analysis of the resulting SPEG layer showed that Sb was present in the SPEG layer of Si. The characteristic of the SPEG layer against the Si substrate was rectifying. A scanning microprobe picture of a cleaved sample established the presence of a depletion region more than 1 micron below the surface. Hall effect data indicated that the SPEG layer was n-type, with average free carrier concentration of about 10 to the 19th power cm/3 and average electron mobility of about 40 sq cm/Vs. SPEG with Pd silicide or Ni silicide transport layers showed fast initial transient growth regimes with slower growth in the steady state regimes.

Mayer, J. W.↗
NASA NTRS1978

Ar-40-Ar-39 microanalysis of single 74220 glass balls and 72435 breccia clasts

Ar-40-Ar-39 age measurements on single orange glass balls from the Apollo 17 soil 74220 and individual clasts from the Apollo 17 highland breccia 72435 are reported. The measurements required the use of newly established microanalytical techniques to obtain high quality analyses on about 0.5 mg particles with only a few hundred ppm K. An age of 3.60 plus or minus 0.04 b.y. is determined for the orange glass. No corrections for a trapped Ar-40 component were required. The glass forming event occurred at the very end of or after the extrusion of the mare basalts at the Apollo 17 site. An extremely well defined age plateau at 3.86 plus or minus 0.04 b.y. was determined for a 72435 plagioclase clast with attached matrix. A second large plagioclase crystal yielded significantly older ages over the last 60% of Ar release at high temperatures and is a relict clast incompletely degassed at the time of breccia formation. 72435 also contains plagioclase clasts with primitive Sr and a 4.55 AE old dunite clast. The Ar results provide additional evidence for the association of chemically unequilibrated, relict clasts with both primitive Sr and older K/Ar ages.

Huneke, J. C.↗