Chemical State Mapping via Soft X-rays using a Wavelength Dispersive Soft X-ray Emission Spectrometer with High Energy Resolution

Takahashi, Hiroki; Handa, Nobuo; Murano, T.; Terauchi, Masami; Koike, Masato; Imazono, Takashi; Hasegawa, Noboru; Koeda, M.; Nagano, T.; Sasai, Hiroyuki; Oue, Y.; Yonezawa, Z.; Kuramoto, Satoshi

doi:10.1017/s1431927613008283

Cited by 7 publications

(6 citation statements)

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“…Among those X-rays, X-rays due to transitions from valence bands (bonding state) to inner-shell levels, usually lower than 1 keV, have information about the chemical bonding states of elements. Recent soft X-ray emission spectrometry using gratings, which was first developed for TEM [22][23][24] and then transferred to SEM and EPMA [5][6][7], has an energy resolution better than 1 eV, which is about two orders better than that of EDS and allowed us to obtain chemical bonding information by using X-ray emission. Another spectrometer system for soft X-rays is under examination [25].…”

Section: Chemical State Information By Sxesmentioning

confidence: 99%

“…The peak energy positions (vertical arrows) and the shoulder structures (vertical lines) of the B K of these materials are different from each other, reflecting different chemical bonding states owing to different crystal structures. By using a high energy resolution, elemental and chemical state analyses and those mappings are possible [5][6][7][26][27][28][29][30]. The emission due to the process d is also affected by the chemical state of the materials [31,32].…”

Section: Chemical State Information By Sxesmentioning

confidence: 99%

“…For a nondestructive inspection process with a high spatial resolution, evaluations based on scanning electron microscopy are useful. A soft X-ray emission spectroscopy (SXES) instrument, combined with a scanning electron microscope (SEM) and/or an electron probe microanalyzer (EPMA) can realize a nondestructive inspection process of the chemical state of materials, with a spatial resolution of about 1 µm or better [5][6][7]. If this occurs, SXES microscopy can make a quick feedback loop of the evaluated results of new products for materials processing.…”

Section: Introductionmentioning

confidence: 99%

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Chemical State Mapping of p/n-Controlled SrB6 Bulk Specimens by Soft X-ray Emission Electron Microscope

2021

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Elemental and chemical state maps of p/n-controlled SrB6 bulk specimens are presented by using a soft X-ray emission spectroscopy electron microscope. Those bulk specimens were obtained by sintering powder specimens, prepared by the molten-salt method with different compositions of initial materials. A Sr-map, a chemical shift map of B K-emission, and the spectra of characteristic regions of those materials were compared. It was observed that a local Sr deficiency caused a local hole-doped region, confirmed by a chemical shift in the B K-emission spectrum. n-type SrB6 was rather homogeneous. On the other hand, the p-type SrB6 bulk specimen was a mixture of two different p-type regions. This mixed nature originated, presumably, from an uneven Sr content of SrB6 particles prepared by the molten-salt method using a Sr-deficient starting material. A separation process of the two types of materials will realize a high-quality homogeneous p-type SrB6 bulk specimens.

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Section: Chemical State Information By Sxesmentioning

confidence: 99%

Section: Chemical State Information By Sxesmentioning

confidence: 99%

Section: Introductionmentioning

confidence: 99%

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Chemical State Mapping of p/n-Controlled SrB6 Bulk Specimens by Soft X-ray Emission Electron Microscope

2021

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“…Moreover, it provides a chemical state mapping that enables the visualization of two-dimensional distributions of crystallographic phases in a specimen. 25,26 DFT calculations are performed to simulate the density of state (DOS) in Be 12 M and to directly compare the experimental SXES spectra.…”

Section: Introductionmentioning

confidence: 99%

Valence Electron and Chemical State Analysis of Be₁₂M (M = Ti, V) Beryllides by Soft X-ray Emission Spectroscopy

Mukai

Kasada

Yabuuchi

et al. 2019

ACS Appl. Energy Mater.

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Be-rich intermetallics (beryllides) have gathered wide attentions to be adopted for high temperature environments, such as an advanced neutron multiplier in fusion reactors. This study reveals the valence electron structure of Be 12 M (M = Ti,V) by using soft X-ray emission spectroscopy with ultra-high resolution (~0.22 eV). The Be-K spectra from the Be 12 M phases show significantly lower densities of the occupied states near the Be-K edge than thaose of metallic beryllium. Theoretical calculations indicate that changes in the valence electron structure are derived from the large downward shift of the Fermi level in Be 12 M, by at least 0.8 eV. Based on the knowledge of the valence electron structures and the chemical shift, chemical state mappings of BeO and Be 12 V in the oxidized beryllide specimen were successfully obtained. The approach is applicable for visualization and identification of metallic/oxidized phase in light-element compounds by electron microscope.

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“…This enables us the ability to obtain important information about chemical bonding in bulk samples from observed spectra as a result of the very high-energy resolution. We have already reported a few examples obtained with the WD-SXES [3]. One important feature of the WD-SXES is that it can detect the Li-K emission spectrum.…”

mentioning

confidence: 99%

Trace Element Analysis under 100 ppm and Chemical State Analysis in Small Area using Wavelength Dispersive Soft X-ray Emission Spectrometer in FE-SEM

Takahashi¹,

Asahina

Terauchi

et al. 2015

Microsc Microanal

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A novel wavelength dispersive soft X-ray emission spectrometer (WD-SXES) has been developed. It covers nominally the X-ray energy range between 50 and 210 eV [1, 2] using two kinds of gratings. One of the characteristic features of the WD-SXES is its parallel detection of the signal. This allows it to be used like a conventional energy dispersive spectrometer. A second feature is its high energy resolution, which is about 0.2 eV for Al-L emission. This resolution is comparable to that of X-ray photoelectron spectroscopy or electron energy-loss spectroscopy. This enables us the ability to obtain important information about chemical bonding in bulk samples from observed spectra as a result of the very high-energy resolution. We have already reported a few examples obtained with the WD-SXES [3]. One important feature of the WD-SXES is that it can detect the Li-K emission spectrum. In the case of an anode electrode from a lithium ion battery (LIB), two types of lithium peaks are observed; one lower energy peak at 50eV, from the valence band, and the other higher energy peak at 54 eV, from the core loss. In addition, we have documented the ability to measure various kinds of X-ray spectra of K, L, M and N emission from Lithium to Uranium [4].In the modern FE-SEM, a wide variety of attachments are used, including multi-SDD, EBSD, WDS, many kinds of electron signal detectors, sputtering tools, low vacuum devices, cathodeluminescence detectors, etc. These are very important for characterizing a wide range of materials. Now, due to its good peak to background ratio and high sensitive CCD camera, the WD-SXES would be an ideal attachment for trace element analysis. Combining the WD-SXES with a FE-SEM, the higher spatial resolution and high sensitivity can provide new insights in material science. For example, the SEM is very useful for observing the distribution of microstructures for metals and ceramics. We have also demonstrated that trace carbon contents

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Chemical State Mapping via Soft X-rays using a Wavelength Dispersive Soft X-ray Emission Spectrometer with High Energy Resolution

Abstract: Extended abstract of a paper presented at Microscopy and Microanalysis 2013 in Indianapolis, Indiana, USA, August 4 – August 8, 2013.

Cited by 7 publications

References 0 publications

Chemical State Mapping of p/n-Controlled SrB6 Bulk Specimens by Soft X-ray Emission Electron Microscope

Chemical State Mapping of p/n-Controlled SrB6 Bulk Specimens by Soft X-ray Emission Electron Microscope

Valence Electron and Chemical State Analysis of Be₁₂M (M = Ti, V) Beryllides by Soft X-ray Emission Spectroscopy

Trace Element Analysis under 100 ppm and Chemical State Analysis in Small Area using Wavelength Dispersive Soft X-ray Emission Spectrometer in FE-SEM

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Chemical State Mapping via Soft X-rays using a Wavelength Dispersive Soft X-ray Emission Spectrometer with High Energy Resolution

Abstract: Extended abstract of a paper presented at Microscopy and Microanalysis 2013 in Indianapolis, Indiana, USA, August 4 – August 8, 2013.

Cited by 7 publications

References 0 publications

Chemical State Mapping of p/n-Controlled SrB6 Bulk Specimens by Soft X-ray Emission Electron Microscope

Chemical State Mapping of p/n-Controlled SrB6 Bulk Specimens by Soft X-ray Emission Electron Microscope

Valence Electron and Chemical State Analysis of Be12M (M = Ti, V) Beryllides by Soft X-ray Emission Spectroscopy

Trace Element Analysis under 100 ppm and Chemical State Analysis in Small Area using Wavelength Dispersive Soft X-ray Emission Spectrometer in FE-SEM

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Product

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Valence Electron and Chemical State Analysis of Be₁₂M (M = Ti, V) Beryllides by Soft X-ray Emission Spectroscopy