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At least 19 records

Energy Dispersive Spectrometry and Quantitative Analysis Short Course. Introduction to X-ray Energy Dispersive Spectrometry and Quantitative Analysis

This course will cover practical applications of the energy-dispersive spectrometer (EDS) to x-ray microanalysis. Topics covered will include detector technology, advances in pulse processing, resolution and performance monitoring, detector modeling, peak deconvolution and fitting, qualitative and quantitative analysis, compositional mapping, and standards. An emphasis will be placed on use of the EDS for quantitative analysis, with discussion of typical problems encountered in the analysis of a wide range of materials and sample geometries.

Carpenter, Paul↗

hpMCA: A Python-based Graphical Program for Energy Dispersive X-Ray Diffraction Data Collection and Analysis

Energy-dispersive X-ray diffraction (EDXD) at synchrotron beamlines is commonly used for the study of material properties under high pressure and/or high temperature. Experimenters typically rely on the availability of robust data collection and analysis at a beamline, but this has become increasingly difficult, especially with the introduction of multi-element detectors that generate complex, multi-dimensional data sets. These data sets have energy resolution, and they can also be resolved in relation to sample position, diffraction angle, or different external stimuli. We report a new Python-based graphical program, hpMCA, for EDXD data collection and analysis that streamlines the experimental process for the beamline users. The program features a user-friendly interface, capability for online viewing and analyzing data from multi-element energy-dispersive detectors, and includes features useful for working with samples under high pressure and/or high temperature, such as crystal phase identification, real-time unit cell lattice refinement, and pressure determination based on an equation of state.

data analysis software↗

Inverse Energy Dispersion of Energetic Ions Observed in the Magnetosheath

We present a case study of energetic ions observed by the Energetic Particle Detector (EPD) on the Magnetospheric Multiscale spacecraft in the magnetosheath just outside the subsolar magnetopause that occurred at 1000 UT on 8 December 2015. As the magnetopause receded inward, the EPD observed a burst of energetic (approximately 50-1000 keV) proton, helium, and oxygen ions that exhibited an inverse dispersion, with the lowest energy ions appearing first. The prolonged interval of fast antisunward flow observed in the magnetosheath and transient increases in the H components of global ground magnetograms demonstrate that the burst appeared at a time when the magnetosphere was rapidly compressed. We attribute the inverse energy dispersion to the leakage along reconnected magnetic field lines of betatron-accelerated energetic ions in the magnetosheath, and a burst of reconnection has an extent of about 1.5 R(sub E) using combined Super Dual Auroral Radar Network radar and EPD observations.

Lee, S. H.↗

Ion and electron energy dispersion features detected by ISEE 1

An energy dispersion feature observed by the ISEE 1 medium energy particle instrument is reported. This feature is characterized by enhancements in both electron and ion fluxes which occur in the 20-200 keV energy range and at radial distances from 5 to 13.5 earth radii. There is a strong energy dependence in the onset times of the enhancements. The time period between the first appearance of an enhancement at high energy to its eventual disappearance in the 20 keV channel can be as much as an hour. The duration of the enhancement in a given energy channel decreases with increasing energy. The species and pitch angle of particles in which the feature is most marked depend on local time. It is shown that the feature is a new manifestation of an old phenomenon, the drift dispersion that frequently produces signatures in particle data from geosynchronous satellites.

Greenspan, M. E.↗

Low energy X-ray spectra measured with a mercuric iodide energy dispersive spectrometer in a scanning electron microscope

A mercuric iodide energy dispersive X-ray spectrometer, with Peltier cooling provided for the detector and input field effect transistor, has been developed and tested in a scanning electron microscope. X-ray spectra were obtained with the 15 keV electron beam. An energy resolution of 225 eV (FWHM) for Mn-K(alpha) at 5.9 keV and 195 eV (FWHM) for the Mg-K line at 1.25 keV has been measured. Overall system noise level was 175 eV (FWHM). The detector system characterization with a carbon target demonstrated good energy sensitivity at low energies and lack of significant spectral artifacts at higher energies.

Iwanczyk, J. S.↗

The structure of high-Mg alkali-bearing aluminosilicate glasses investigated in situ at ambient and high pressure by multi-angle energy dispersive X-ray diffraction and infrared microspectroscopy

The structural properties of synthetic high-Mg alkali-bearing aluminosilicate glasses analogues of natural picritic-to-komatiitic magmas were investigated in situ by multiangle energy dispersive X-ray diffraction at 2.1 GPa and ambient pressure and by Fourier Transform infrared spectroscopy up to 5.4 GPa in a cycle of compression and decompression experiments. Our results show that the intermediate range ordering of the glass structure at 2.1 GPa is 3.14 Å, increasing to 3.19 Å when decompressed. The local structure shows T-O lengths of 1.66 Å (2.1 GPa) and 1.65 Å (ambient pressure), T-T distances of 3.19 Å at high pressure, which lengthen to 3.21 Å at ambient pressure, causing the T-O-T angle of 147° determined at 2.1 GPa to widen to 154° upon decompression. The deconvoluted infrared spectra result in the presence of Q 1 , Q 2 , Q 3 populations in the aluminosilicate spectral region, whose proportions remain relatively unchanged up to 5.4 GPa. The structural response of the investigated glasses to cold-compression does not involve changes in polymerization, but rather a shrinking and compaction of the structure as evidenced by the Qn species shifting to higher wavenumbers as a function of pressure. The structural properties determined from X-ray diffraction for this glass composition are discussed together with those of glasses emerging from previous studies to highlight a compositional dependence mainly dictated by the amount of SiO 2 and Al 2 O 3 .

glass structure↗

Energy dispersive X-ray diffraction in the diamond anvil, high-pressure apparatus - Comparison of synchrotron and conventional X-ray sources

The use of both conventional fixed-anode X-ray sources and synchrotron radiation to carry out energy-dispersive X-ray diffraction experiments at high pressure in a diamond anvil cell, is discussed. The photon flux at the sample and at the detector for the two cases are compared and the results are presented in graphs. It is shown that synchrotron radiation experiments can be performed with nearly two orders of magnitude increase in data rate if superior detectors and detector electronics are available.

Spain, I. L.↗

MMS Observation of Inverse Energy Dispersion in Shock Drift Accelerated Ions

The four Magnetospheric Multiscale (MMS) spacecraft observed a ∼1 min burst of energetic ions (50–1000 keV) in the region upstream from the subsolar quasi-perpendicular bow shock on 6 December 2015. The composition, flux levels, and spectral indices of these energetic protons, helium, and oxygen ions greatly resemble those seen in the outer magnetosphere earlier while MMS crossed the magnetopause and differ significantly from those simultaneously observed far upstream by Advanced Composition Explorer (ACE). However, the event cannot be explained solely in terms of leakage from the magnetosphere. The strongly southward orientation of the interplanetary magnetic field (IMF) lines at the time of the event precludes any connection to the magnetosphere. This point is confirmed by the presence of energetic electrons, known to occur on magnetic field lines that graze the bow shock rather than connect to the magnetosphere. We suggest that the ions gradient drifted out of the nearby quasi-parallel foreshock and into the quasi-perpendicular bow shock. Each of the ion species exhibited an inverse energy dispersion. As predicted by models for shock drift acceleration, the energies of the ions increased as 𝜃(sub Bn), the angle between the IMF and the shock normal, increased. Finally, we note that a similar event was observed a few minutes later in the subsolar magnetosheath, indicating that such events can be swept downstream of the bow shock.

Lee, S. H.↗

Structural Tolerance of Zirconium Diboride under Electron Irradiation through in-situ Convergent Beam Electron Diffraction and Energy-dispersive X-ray Spectroscopy

Zirconium diboride (ZrB 2 ) is a ultra-high temperature ceramic with high melting temperature (>3000 K), super strength and hardness, good thermal conductivity, and excellent resistance to plasma erosion and chemical erosion, being widely applied in hypersonic flight, arc-electrodes, refractory materials, and plasma-facing materials in fusion reactors. Therefore, the structural stability of the material is essential for the applications. Up to now, the material was investigated under neutron irradiation and high-energy ion irradiations. It was reported that the neutron irradiation caused swelling and catastrophic cracking. High-energy ions (30 keV He + ) changed the surface morphology and caused the bright blue and brown colors on ZrB 2 surfaces between 920 K and 1120 K. The electron irradiation tolerance of the material has not been reported yet. Here we used convergent beam electron diffraction (CBED) and energy-dispersive X-ray spectroscopy (EDS) to investigate structural tolerances of ZrB 2 crystals under high-energy electrons at room temperature under vacuum. Finally, the investigation would benefit the understanding of its structural tolerance at microscales.

42 ENGINEERING↗

NASA Li/CF(x) cell problem analysis: Scanning electron microscopy with energy dispersive x ray spectrometry

An analysis was made of Lithium/carbon fluoride cell parts for possible chloride contamination induced by exposure to thionyl chloride (SOCl2); various samples were submitted for analysis. Only a portion of the analysis which has been conducted is covered, herein, namely analysis by scanning electron microscopy with energy dispersive x ray spectrometry (SEM/EDS). A strip of nickel was exposed to SOCl2 vapors to observe variations in surface concentrations of sulfur and chlorine with time. By detecting chlorine one can not infer contamination by SOCl2 only that contamination is present. Six samples of stainless steel foil were analyzed for chlorine using EDS. Chlorine was not detected on background samples but was detected on the samples which had been handled including those which had been cleaned. Cell covers suspected of being contaminated while in storage and covers which were not exposed to the same storage conditions were analyzed for chlorine. Although no chlorine was found on the covers from cells, it was found on all stored covers. Results are presented with techniques shown for analysis and identification. Relevant photomicrographs are presented.

Baker, John↗

ENERGY DISPERSIVE DIFFRACTION TOMOGRAPHY OF SHARK VERTEBRAL CENTRA

Shark vertebrae and their centra (vertebral bodies) are high-performance structures able to survive millions of cycles of high amplitude strain despite lacking a repair mechanism for accumulating damage. Shark centra consist of mineralized cartilage, a biocomposite of bioapatite (bAp), and collagen, and the nanocrystalline bAp's contribution to functionality remains largely uninvestigated. Using the multiple detector energy-dispersive diffraction (EDD) system at 6-BM-B, the Advanced Photon Source, and 3D tomographic sampling, the 3D functionality of entire centra were probed. Immersion in ethanol vs phosphate-buffered saline produces only small changes in bAp d-spacing within a great hammerhead centrum. EDD mapping under in situ loading was performed an entire blue shark centrum, and 3D maps of bAp strain showed the two structural zones of the centrum, the corpus calcareum and intermedialia, contained opposite-signed strains approaching 0.5%, and application of similar to 8% nominal strain did not alter these strain magnitudes and their spatial distribution.

Park, Jun-Sang↗

Automated Energy-Dispersive X-ray Spectroscopy Analysis for Multi-Modal Few-Shot Learning

Scanning transmission electron microscopy (STEM) is a powerful tool that allows for the atomic-scale analysis of a materials’ structure, chemistry, and defect domains (Akers et al. 2021). The current generation of microscopes generate vast amounts of data, surpassing the limits of effective manual analysis traditionally performed by domain experts (Spurgeon et al. 2021). While recent strides in machine learning have significantly enhanced the processing of large and intricate datasets acquired through electron microscopy, the prevalent use of proprietary software packages for initial data collection poses a challenge. In many cases, these software packages act as a ‘black box’, constraining user functionality and hindering the output of data in a format that is conducive to seamless integration into machine learning models. This work addresses these challenges by adapting HyperSpy, an open-source Python library, for the analysis and quantification of raw energy dispersive spectroscopy (EDS) data acquired through STEM. The modified HyperSpy code successfully facilitates user-defined segmentation of the data, enabling the integration of atomic %, weight %, and raw EDS spectra for each segmented region into an existing few-shot machine learning model. While initial results reveal discrepancies in quantified atomic and weight percentages when compared to proprietary software, ongoing efforts aim to rectify this issue by refining the fit of the HyperSpy model to the EDS spectra. Overall, this research underscores the potential of open-source tools like HyperSpy to enhance the accessibility of analytical tools, fostering a transparent and user-friendly environment for seamlessly incorporating electron microscopy data into machine learning models.

36 MATERIALS SCIENCE↗

The geomagnetic mass spectrometer - Mass and energy dispersions of ionospheric ion flows into the magnetosphere

Observations of ion flows in the polar magnetosphere, made by the retarding ion mass spectrometer on NASA's Dynamics Explorer (DE) 1, are compared with those made simultaneously in the topside ionosphere by the ion drift meter on the lower-altitude DE 2 spacecraft. The results show the dayside auroral ionosphere to be a significant and highly persistent source of plasma for the magnetosphere. The upwelling ionospheric ions are spatially dispersed, according to both their energy and mass, by the combined actions of the geomagnetic field and the dawn-to-dusk convection electric field, in an effect analogous to the operation of an ion mass spectrometer.

Lockwood, M.↗

Estimation of dipole-quadrupole dispersion energies.

The calculation of the dipole-quadrupole dispersion coefficient is discussed through a perturbation and a variation method. Accurate combination rules are obtained from both methods, one new and one already known. Further approximations permit computations in terms of accessible parameters. Values are calculated for the interactions of atomic pairs formed from hydrogen, alkali, and rare-gas atoms. A new relation giving the dipole-quadrupole coefficient in terms of the dipole-dipole coefficient and the dipole and quadrupole polarizabilities seems accurate, but needs further testing.

Alvarez-Rizzatti, M.↗

Residual strain gradient determination in metal matrix composites by synchrotron X-ray energy dispersive diffraction

An X-ray technique for the measurement of internal residual strain gradients near the continuous reinforcements of metal matrix composites has been investigated. The technique utilizes high intensity white X-ray radiation from a synchrotron radiation source to obtain energy spectra from small (0.001 cu mm) volumes deep within composite samples. The viability of the technique was tested using a model system with 800 micron Al203 fibers and a commercial purity titanium matrix. Good agreement was observed between the measured residual radial and hoop strain gradients and those estimated from a simple elastic concentric cylinders model. The technique was then used to assess the strains near (SCS-6) silicon carbide fibers in a Ti-14Al-21Nb matrix after consolidation processing. Reasonable agreement between measured and calculated strains was seen provided the probe volume was located 50 microns or more from the fiber/matrix interface.

Kuntz, Todd A.↗

Relationship of dusk sector radial electric field to energy dispersion at the inner edge of the electron plasma sheet

It is shown that, by assuming that the magnetospheric particle boundaries are the result of steady state convection, the electron boundaries in the dusk sector are essentially sensitive to the local, not the global, electric field configuration. A simple, direct relationship is obtained between the dusk sector radial electric field and the inner edge of electron boundaries at various energies.

Horwitz, J. L.↗