Exciting Possibilities of Soft X-ray Emission Spectroscopy as Chemical State Analysis in EPMA and FESEM

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

doi:10.1017/s1431927614005145

Microsc Microanal

2014

DOI: 10.1017/s1431927614005145

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Exciting Possibilities of Soft X-ray Emission Spectroscopy as Chemical State Analysis in EPMA and FESEM

Hiroki Takahashi

Nobuo Handa

T. Murano

et al.

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Cited by 12 publications

(6 citation statements)

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“…In this study, we demonstrate the chemical state mapping of B in a modeled B 4 C control rod after a high-temperature steam oxidation test using the newly developed EPMA-soft X-ray emission spectrometer (SXES) with ultra-high energy resolutions 8 9 . EPMA-SXES is a type of WDS that performs a parallel collection of soft X-ray spectra by a combination of an aberration-corrected grating system and a high-sensitivity X-ray charge-coupled device (CCD).…”

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confidence: 99%

Chemical State Mapping of Degraded B4C Control Rod Investigated with Soft X-ray Emission Spectrometer in Electron Probe Micro-analysis

Kasada

Higuchi³

et al. 2016

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B4C is widely used as control rods in light water reactors, such as the Fukushima Daiichi nuclear power plant, because it shows excellent neutron absorption and has a high melting point. However, B4C can melt at lower temperatures owing to eutectic interactions with stainless steel and can even evaporate by reacting with high-temperature steam under severe accident conditions. To reduce the risk of recriticality, a precise understanding of the location and chemical state of B in the melt core is necessary. Here we show that a novel soft X-ray emission spectrometer in electron probe microanalysis can help to obtain a chemical state map of B in a modeled control rod after a high-temperature steam oxidation test.

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Chemical State Mapping of Degraded B4C Control Rod Investigated with Soft X-ray Emission Spectrometer in Electron Probe Micro-analysis

Kasada

Higuchi³

et al. 2016

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“…Thus, soft X-ray emission spectroscopy (SXES) based on electron microscopy (EM) can be a sensitive tool for elemental and chemical identifications of specified specimen areas. For that purpose, a grating spectrometer for SXES-EM has been realized as a commercial instrument with an energy resolution of 0.2-0.3 eV at Al-L emission (73 eV) [1,2].A test SXES-SEM instrument with a micro-channel plate (MCP) detector combined with a CMOS camera has been applied for state analyses of bulk specimens [3]. It performed an energy resolution of 0.13 eV at Al-L emission.…”

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confidence: 99%

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confidence: 99%

Chemical States Analysis of Trace-boron by using an Improved SEM-SXES

et al. 2016

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X-rays originate form electronic transitions from valence bands (bonding electron states) to inner-shell electron levels inform us elementally specific chemical states in materials. The energies of those X-rays range from about 0.1 to a few keV, soft X-ray region. Thus, soft X-ray emission spectroscopy (SXES) based on electron microscopy (EM) can be a sensitive tool for elemental and chemical identifications of specified specimen areas. For that purpose, a grating spectrometer for SXES-EM has been realized as a commercial instrument with an energy resolution of 0.2-0.3 eV at Al-L emission (73 eV) [1,2].A test SXES-SEM instrument with a micro-channel plate (MCP) detector combined with a CMOS camera has been applied for state analyses of bulk specimens [3]. It performed an energy resolution of 0.13 eV at Al-L emission. To improve the energy resolution of the system, the MCP with a channel pitch of 15 m has changed to a new one with that of 7.5 m. Optical component between the MCP and the CMOS camera was readjusted in its magnification. Figure 1 shows Al L-emission spectra of a bulk specimen obtained by the improved system in photon counting mode. A small step of L 2 -edge (E F to L 2 -shell) and a large L 3 -edge (E F to L 2 -shell) is clearly resolved. The energy resolution evaluated from the L 3 -edge by taking into account the thermal broadening of Fermi distribution function is 0.08 eV, which is better than that of the previous one. Although the energy resolution has improved, it takes a longer acquisition time to have a good signal to noise ratio in photon counting mode compared to that of analog integration mode. Thus, analog integration mode has adopted for the present trace-boron analysis, unfortunately the energy resolution is a few times lower than that of photon counting mode. Figure 2 shows an SEM image of a carbon steel specimen. Average contents of B, P, and C are 45, 53, and 41 ppm (wt.%), respectively. The image shows several precipitates with different sizes and shapes are distributed in the matrix. The SXES spectra obtained from the numbered areas in figure 2 are shown in figure 3. Accelerating voltage, probe current and acquisition time were 5 kV, 170 nA and 5 min, respectively. The spectrum of area 3 (matrix area without any precipitates) shows mainly C-K and O-K signals, which may originate from contamination and oxidation of the specimen surface, respectively. It should be noted that there is no apparent B-K intensity in the spectrum. On the other hand, spectra obtained from precipitate areas show characteristic peaks and show different features each other. Area 1 shows mainly C-K and a little B-K. Area 2 shows a dominant B-K and smaller N-K and S-L. Area 4 shows B-K and S-L. Area 5 shows a dominant B-K and small N-K and Si-L. It can be noticed that spectra with dominant B-K intensity, 2 and 5, also show apparent N-K and O-K intensity. O-K intensity of those spectra is larger than that of area 3, matrix without any precipitate. Those results suggest a presence of boron nitride and boron oxi...

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“…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.…”

mentioning

confidence: 99%

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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Exciting Possibilities of Soft X-ray Emission Spectroscopy as Chemical State Analysis in EPMA and FESEM

Cited by 12 publications

References 1 publication

Chemical State Mapping of Degraded B4C Control Rod Investigated with Soft X-ray Emission Spectrometer in Electron Probe Micro-analysis

Chemical State Mapping of Degraded B4C Control Rod Investigated with Soft X-ray Emission Spectrometer in Electron Probe Micro-analysis

Chemical States Analysis of Trace-boron by using an Improved SEM-SXES

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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