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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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All sourcesNASA NTRSDOE OSTI
DOE OSTI2019

Microscopy & Microanalysis 2019 in Portland, Oregon

The Microscopy Society of America (MSA), the Microanalysis Society (MAS), and the International Field Emission Society (IFES) cordially invite you to Microscopy & Microanalysis 2019 in Portland, Oregon. We are excited and honored to feature two Nobel Prize laureates as our plenary lecturers. Our first plenary speaker will be Dr. Joachim Frank, Professor of Biochemistry and Molecular Biophysics and of Biological Sciences at Columbia University, New York. He shared with Jacques Dubochet and Richard Henderson the 2017 Nobel Prize in Chemistry for “Developing cryo-electron microscopy for the high resolution structure determination of biomolecules in solution.” Our second plenary speaker will be Dr. Richard Henderson of the Medical Research Council Laboratory of Molecular Biology (MRC LMB), Cambridge, UK. He will present a talk titled “Single particle cryoEM: potential for further improvement.” As usual, M&M 2019 will present a great variety of symposia topics in analytical, life, and physical sciences. This year, we have a special symposium: “Cryo-EM – from Physics to Cell Biology: Honoring the Remarkable Legacy of Ken Downing.” It will showcase the late Dr. Downing’s work in single-particle cryo-EM, cryo-electron tomography, and the microscopy methods he used for his seminal discoveries. Preceding the M&M 2019 technical program, we will have two pre-meeting congresses. Education and training are important components of the M&M technical program each year, and 2019 is no exception. Six Sunday short courses on material science, biology, and data analysis will be presented. Additional opportunities are available in tutorials in biology and physical sciences during the meeting week. Finally, our popular microscopy outreach workshop “Project MICRO” will be in the MegaBooth all week. For a complete description of the technical program and educational opportunities, please go to http://www.microscopy.org/MandM/2019. The Call for Papers and other aspects of the program and the meeting are provided under “Scientific Program.” The Executive Program Committee welcomes you to Portland for an excellent and compelling Microscopy & Microanalysis 2019. Catch up with old friends and make new ones! Look for opportunities to attend society business meetings and socials during the week. On behalf of MSA, MAS, IFES, in cooperation with over a hundred symposia organizers and countless volunteers, we look forward to seeing you in Portland this August!

Microscopy, microanalysis↗
NASA NTRS1992

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.↗
DOE OSTI2025

Mixed Element Microparticle Characterization by Electron Probe Microanalysis

Abstract Microparticle compositional characterization for nuclear forensics has traditionally been achieved by “gold-standard” destructive analytical techniques such as large geometry-secondary ion mass spectrometry and fission track-thermal ionization mass spectrometry, but long processing times and total sample consumption eliminate the option of subsequent analysis by other methods. Electron probe microanalysis has long been widely employed for rapid, nondestructive, micrometer-scale compositional measurements and imaging in fields such as material science and geology and may therefore need to be reevaluated as an alternative tool for microparticle analysis for the nuclear forensics community. This study presents the use of electron probe microanalysis for imaging and quantitative characterization of homogeneous microparticles utilizing a calibration curve based on high-precision quadrupole-inductively coupled plasma-mass spectrometry analyses. Samples of opportunity synthesized at Savannah River National Laboratory, nickel-doped cerium oxide microparticles, were selected as analogs for plutonium-doped uranium oxide microparticles. Positive detection and accurate quantification of variable amounts of nickel dopant down to trace levels (10s of parts per million) suggest applicability of this technique to other mixed element systems (e.g., actinides). Quantitative single-particle characterization via electron probe microanalyzer may thus provide a high fidelity, nondestructive complement to techniques currently in use.

Riche, Alexis T. (ORCID:0009000121978126)↗
NASA NTRS1990

Spatial Resolution and Detectability Limits in Thin-Film X-Ray Microanalysis

The major advantages of performing x-ray microanalysis in the analytical electron microscope (AEM) are the high compositional spatial resolution and the elemental analysis sensitivity. Unfortunately, there is usually a trade-off between these two advantages. This paper discusses the factors involved in the optimization of both spatial resolution and sensitivity during x-ray microanalysis and shows the results of such optimization experiments for several AEM instruments.

Goldstein, J. I.↗
NASA NTRS2003

Electron Probe MicroAnalysis (EPMA) Standards. Issues Related to Measurement and Accuracy Evaluation in EPMA

Electron-probe microanalysis standards and issues related to measurement and accuracy of microanalysis will be discussed. Critical evaluation of standards based on homogeneity and comparison with wet-chemical analysis will be made. Measurement problems such as spectrometer dead-time will be discussed. Analytical accuracy issues will be evaluated for systems by alpha-factor analysis and comparison with experimental k-ratio databases.

Carpenter, Paul↗
NASA NTRS2005

Analysis of Iron Meteorites Using Computed Tomography and Electron-probe Microanalysis

Computed tomography (CT) imaging and electron-probe microanalysis (EPMA) have been used to study samples of the Mundrabilla and Colomera iron meteorites in order to perform structural, textural, and mineralogical analysis. Both gamma-ray (Co-60 source, essentially monochromatic 1.25MeV avg.) and x-ray (420 KeV, continuous) sources have been used, with effective resolution of approximately 1 mm and 0.25 mm, respectively. The gamma-ray source provides approx. 15 cm penetration through steel and is used for larger samples, whereas the x-ray source provides superior resolution at reduced penetration but exhibits beam hardening artifacts. Here we present a combined approach where CT and EPMA imaging and microanalysis aid in the identification of structural and compositional features in iron meteorites.

Carpenter, P. K.↗
NASA NTRS2012

Microanalysis of Hypervelocity Impact Residues of Possible Interstellar Origin

The NASA Stardust spacecraft deployed two collector trays, one dedicated to the collection of dust from Comet Wild 2, and the other for the capture of interstellar dust (ISD). The samples were returned successfully to Earth in 2006, and now provide an unprecedented opportunity for laboratory-based microanalysis of materials from the outer solar system and beyond. Results from the cometary sample studies have demonstrated that Wild 2 contains much more refractory condensate material and much less pristine extra-solar material than expected, which further indicates that there was significant transport of inner solar system materials to the Kuiper Belt in the early solar system [1]. The analysis of the interstellar samples is still in the preliminary examination (PE) phase, due to the level of difficulty in the definitive identification of the ISD features, the overall low abundance, and its irreplaceable nature, which necessitates minimally invasive measurements [2]. We present here coordinated microanalysis of the impact features on the Al foils, which have led to the identification of four impacts that are possibly attributable to interstellar dust. Results from the study of four ISD candidates captured in aerogel are presented elsewhere [2].

Stroud, Rhonda M.↗
DOE OSTI2019

Measurement of PuO 2 film thickness by electron probe microanalysis (EPMA) calibration curve method

Plutonium (Pu) surfaces are highly reactive toward oxygen containing species and, therefore, invariably covered with oxides (e.g. PuO 2 ) during transport and handling. The actual thickness of the surface oxide may dictate if a plutonium part is suitable for a certain application. As a result, a cost-effective, quick, non-destructive, yet reliable means to measure the oxide layer thickness formed on Pu samples is desirable. In this study, the cross-sections of a series of room temperature grown oxides on Pu samples were trenched by focus ion beam (FIB) then observed by scanning electron microscopy (SEM) to measure the surface oxide thicknesses, which were then combined with the corresponding oxygen k-ratios provided by electron probe microanalysis (EPMA) to form calibration curves. Oxide thickness measurements for the calibration curves were made on samples within the typical SEM observable range for PuO 2 (35–400 nm). The portion of the calibration curve in the thinner oxide region (<35 nm) were approximated via Pouchou and Pichoir’s Φ(ρz) theory. Two specimens with micrometer-thick PuO 2 standards (one formed at room temperature and the other at higher temperature with a higher level of crystallinity) were made for the k-ratios in this study, allowing EPMA users to choose the standard that best suits their needs. If the surface corrosion is known to be PuO 2 (from the environment in which the Pu sample is stored) or if the stoichiometry of the surface oxide is confirmed by a preliminary/compliment technique, these calibration curves allow EPMA users to quickly and efficiently determine PuO 2 thicknesses from the measured oxygen k-ratios of their samples. The methodology presented in this study can also be used as a template for creating calibration curves for oxides grown on other actinides.

36 MATERIALS SCIENCE↗
DOE OSTI2024

Exploring constituent redistribution in irradiated U-19Pu-14Zr fuel via electron probe microanalysis

Here, the phenomena of constituent redistribution, wherein a previously homogeneous metallic fuel forms discrete, radially concentric compositional zones upon irradiation was investigated by examining an irradiated U-19Pu-14Zr fuel (where numbers represent wt. %) with a burnup of 11.5 at.% with electron probe microanalysis (EPMA) and quadruple inductively coupled plasma mass spectroscopy (Q-ICP-MS). EPMA-generated U, Pu, and Zr compositional data obtained from a diameter traverse of the sample was converted to mass and was used to: 1) compare the overall fuel element analysis results between the two methods, 2) determine the number of compositionally distinct zones forming as a result of constituent redistribution; and 3) quantify the post-irradiation loss or gain of U, Pu, and Zr atoms in each distinct compositional zone. Weight percent concentrations of U, Pu, and Zr for the overall cross section compare favorably between the two analytical methods, suggesting that the spatially resolved EPMA analysis complements bulk chemical analysis. Among the four identified compositional zones, post-irradiation quantification of U, Pu, and Zr elemental atom content changes shows that the quantity of U atoms lost from the innermost zone is slightly less than the quantity of U atoms gained by the middle two zones, and the quantity of Zr atoms lost from the high-U third zone is slightly less than is gained by the two innermost zones. Pu is lost from all four zones, although the innermost zone and the high-U third zone lose a significantly higher percentage (> 22 %) of their initial Pu atoms than the other two zones. For all three elements, EPMA cannot distinguish between atoms lost due to transport to a different zone from atoms lost due to nuclear processes; however, the insight gained from using this process can be used to experiment with new modeling techniques to predict constituent redistribution in U-Pu-Zr fuels.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗
DOE OSTI2020

Investigation of N in Ammonium-bearing Silicates with Electron Probe Microanalysis (EPMA)

Nitrogen is a primary constituent of Earth’s atmosphere and an essential component of many biological processes. Recent developments in understanding N incorporation into silicate minerals suggest that the solid earth and lithosphere could provide a substantial reservoir for the planetary N budget. Furthermore, determining the concentration and distribution of low abundances of N in silicates presents a significant challenge in microanalysis. We tested capabilities for high spatial resolution quantification of low levels of N using EPMA with the goal of developing standards to be used in coupled N and noble gas analyses of silicate minerals. We investigated the concentration and distribution of N in a suite of ammonium-bearing silicate minerals that reflect the dominant N-bearing phases of the lithosphere: tobelite, buddingtonite, ammonioleucite, tsaregorodtsevite, and hyalophane. These minerals form during NH4-rich alteration of K-bearing silicate minerals, and the bonding environment of N in each mineral is likely to differ based on crystal structure. Using an optimized analytical routine for N quantification enables sensitivity approaching 0.02 weight% N and high-resolution quantitative mapping of sub-micron variations in N contents.

58 GEOSCIENCES↗
NASA NTRS1966

Standards for electron probe microanalysis of silicates prepared by convenient method

Standard compositions suitable for electron probe microanalysis of various silicates are prepared by coprecipitation of specified salts with colloidal silica to form a gel which is decomposed into a powdered oxide mixture and compressed into thin pellets. These pellets of predetermined standard are compared with a silicate sample to determine its composition.

Walter, L. S.↗
NASA NTRS1966

Apparatus enables automatic microanalysis of body fluids

Apparatus will automatically and quantitatively determine body fluid constituents which are amenable to analysis by fluorometry or colorimetry. The results of the tests are displayed as percentages of full scale deflection on a strip-chart recorder. The apparatus can also be adapted for microanalysis of various other fluids.

Soffen, G. A.↗
NASA NTRS1989

Calibration approach to electron probe microanalysis: A study with PWA-1480, a nickel base superalloy

The utility of an indirect calibration approach in electron probe microanalysis is explored. The methodology developed is based on establishing a functional relationship between the uncorrected k-ratios and the corresponding concentrations obtained using one of the ZAF correction schemes, for all the desired elements in the concentration range of interest. In cases where a very large number of analyses are desired, such a technique significantly reduces the total time required for the microprobe analysis without any significant loss of precision in the data. A typical application of the method in the concentration mapping of the transverse cross-section of a dendrite in directionally solidified PWA-1480, a nickel-based superalloy, is described.

Terepka, F. M.↗