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Journal Articles

Inner structure and inclusions in radiocesium-bearing microparticles emitted in the Fukushima Daiichi Nuclear Power Plant accident

Okumura, Taiga*; Yamaguchi, Noriko*; Dohi, Terumi; Iijima, Kazuki; Kogure, Toshihiro*

Microscopy, 68(3), p.234 - 242, 2019/06

 Times Cited Count:8 Percentile:70.45(Microscopy)

Radiocesium-bearing microparticles (CsMPs), consisting substantially of silicate glass, were released to the environment during the Fukushima nuclear accident in March 2011. We investigated a total of nine CsMPs using transmission electron microscopy (TEM) and inferred the atmosphere in the reactors during the accident. From elemental mapping using energy-dispersive X-ray spectrometry, Fe and Zn showing radial inhomogeneities were found in the CsMPs, in addition to the Cs that had been previously reported. Four of the CsMPs included submicron crystals, which were identified as chromite, franklinite, acanthite, molybdenite, and hessite. The chromium-containing spinels, chromite and franklinite, indicated the presence of ferrous iron (Fe$$^{2+}$$), suggesting that the inside of the reactors was reductive to some extent. Electron energy-loss spectroscopy also confirmed that the CsMPs did not contain boron, and therefore the atmosphere in which they were formed might be boron-free.

Journal Articles

Conformation and dynamics of single polymer chain studied by optical microscopy techniques beyond the diffraction limit

Aoki, Hiroyuki

Microscopy, 66(4), p.223 - 233, 2017/08

 Times Cited Count:1 Percentile:2.7(Microscopy)

Journal Articles

Constituent elements and their distribution in the radioactive Cs-bearing silicate glass microparticles released from Fukushima Nuclear Plant

Kogure, Toshihiro*; Yamaguchi, Noriko*; Segawa, Hiroyo*; Mukai, Hiroki*; Motai, Satoko*; Akiyama, Kotone*; Mitome, Masanori*; Hara, Toru*; Yaita, Tsuyoshi

Microscopy, 65(5), p.451 - 459, 2016/10

 Times Cited Count:41 Percentile:97.25(Microscopy)

Journal Articles

Present state of TEM-SXES analysis and its application to SEM aiming chemical analysis of bulk materials

Terauchi, Masami*; Takahashi, Hideyuki*; Handa, Nobuo*; Murano, Takanori*; Koike, Masato; Imazono, Takashi; Koeda, Masaru*; Nagano, Tetsuya*; Sasai, Hiroyuki*; Oue, Yuki*; et al.

Microscopy and Microanalysis, 20(Suppl.3), p.682 - 683, 2014/08

X-rays originate form electronic transitions from valence bands (VB, bonding electron states) to inner-shell electron levels inform us energy states of bonding electrons. We have developed the SXES spectrometers attaching to TEM, EPMA, and SEM. A spectrometer has an energy range of 50-4000 eV by using four varied-line-spacing gratings. Applications of TEM-SXES instrument to C$$_{60}$$ have revealed characteristic energy distribution of bonding electrons. Carbon K-emission spectra of C $$_{60}$$ crystals showed that both the peak structures in $$pi$$- and $$sigma$$-bands and the characteristic dip structure between the $$pi$$- and $$sigma$$-bonding states in monomer-C$$_{60}$$ disappear in the most polymerized-C$$_{60}$$ crystals. Bulk specimens were examined by applying SXES to a SEM. Al L-emission spectra of intermetallic compounds of Al$$_{2}$$Au, AlCo, and aluminum showed different intensity distributions due to different band structures originating from different crystal structures.

Journal Articles

Exciting possibilities of soft X-ray emission spectroscopy as chemical state analysis in EPMA and FESEM

Takahashi, Hideyuki*; Handa, Nobuo*; Murano, Takanori*; Terauchi, Masami*; Koike, Masato; Kawachi, Tetsuya; Imazono, Takashi; Hasegawa, Noboru; Koeda, Masaru*; Nagano, Tetsuya*; et al.

Microscopy and Microanalysis, 20(Suppl.3), p.684 - 685, 2014/08

A novel wavelength dispersive soft X-ray emission spectrometer (SXES) having a X-ray energy range of 50-210 eV has been developed. One feature is that the SXES is parallel detection of the signals so that it can be used like a conventional energy dispersive spectrometer. The other is a high energy resolution, which is about 0.2 eV at Al-L comparable to those revealed by XPS and EELS. These features enable us to obtain meaningful information about chemical bonding in various bulk samples. The SXES can detect Li-K emission spectrum. In the case of an anode electrode of a lithium ion battery (LIB), two types of lithium peaks are observed: one lower energy peak at 50 eV and the other higher energy peak at 54 eV. It was found that the former peak corresponds to the amount of charging, whereas the latter corresponds to the metallic state of lithium.

Journal Articles

Chemical state information of bulk specimens obtained by SEM-based soft-X-ray emission spectrometry

Terauchi, Masami*; Koshiya, Shogo*; Sato, Futami*; Takahashi, Hideyuki*; Handa, Nobuo*; Murano, Takanori*; Koike, Masato; Imazono, Takashi; Koeda, Masaru*; Nagano, Tetsuya*; et al.

Microscopy and Microanalysis, 20(3), p.692 - 697, 2014/06

 Times Cited Count:25 Percentile:88.38(Materials Science, Multidisciplinary)

Electron beam induced soft-X-ray emission spectroscopy (SXES) by using a grating spectrometer has been introduced to a conventional scanning electron microscope (SEM) for characterizing desired specimen areas of bulk materials. The spectrometer was designed as a grazing-incidence flat-field optics by using aberration corrected (varied-line-spacing) gratings and a multi-channel-plate detector combined with a charge-coupled-device camera, which has already applied for a transmission electron microscope. The best resolution was confirmed as 0.13 eV at Mg L-emission (50 eV), which value is comparable to that of recent dedicated electron energy-loss spectroscopy instruments. This SXES-SEM instrument presents density of states of simple metals of bulk Mg and Li. Apparent band structure effects have been observed in Si L-emission of Si-wafer, P L-emission of GaP-wafer, and Al L-emissions of intermetallic compounds of AlCo, AlPd, Al$$_{2}$$Pt, and Al$$_{2}$$Au.

Journal Articles

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

Takahashi, Hideyuki*; Handa, Nobuo*; Murano, Takanori*; Terauchi, Masami*; Koike, Masato; Kawachi, Tetsuya; Imazono, Takashi; Hasegawa, Noboru; Koeda, Masaru*; Nagano, Tetsuya*; et al.

Microscopy and Microanalysis, 19(Suppl.2), p.1258 - 1259, 2013/08

A new wavelength dispersive soft X-ray emission spectrometer (WD-SXES) consisting of newly developed diffraction gratings has been developed for soft X-ray emission spectroscopy. The WD-SXES with two types of diffraction gratings nominally covering an energy range between 50 and 210 eV has been installed to electron probe X-ray microanalyzers, JEOL JXA-8100, for commercial use. The energy resolution of this WD-SXES is nominally 0.3 eV, which is one order of magnitude better than that of conventional WDSs with layered dispersion elements. It is to be noted that the corresponding edge of Al$$_{2}$$B is shifted to higher energy side by about 1 eV. One of the energy range was selected from 72 to 73.5 eV whereas the other was from 73.5 to 75 eV. The contrast in the former map is reversed in the later map as expected even though the energy difference between two maps is only 1.5 eV. The study confirms the high potential for the characterization especially for chemical state mapping.

Journal Articles

Construction of a SXES spectrometer for a conventional SEM

Terauchi, Masami*; Koshiya, Shogo*; Sato, Futami*; Takahashi, Hideyuki*; Handa, Nobuo*; Murano, Takanori*; Koike, Masato; Imazono, Takashi; Koeda, Masaru*; Nagano, Tetsuya*; et al.

Microscopy and Microanalysis, 19(Suppl.2), p.1278 - 1279, 2013/08

We have been developed and tested soft-X-ray emission spectroscopy (SXES) instruments by attaching to TEM and EPMA. The spectrometer has an energy range form 50-4000 eV by using four varied-line-spacing (aberration corrected) gratings. This SXES spectrometer inform us energy states of valence electrons (bonding electrons) form an identified specimen area by electron microscopy, which cannot be obtained by EELS and EDS. This provides not only the probing method for the energy states of valence electrons but also a sensitive tool for elemental and chemical identification. The spectrometer has applied also to a SEM (JEOL JSM-6480LV). As SEM can use a larger probe current and excitation volume of specimen than those of TEM, the detection time is about one order shorter than that of TEM. The energy resolution evaluated at AL-L$$_{3}$$edge is 0.16 eV. The spectrum of LaB$$_{6}$$ shows apparent intensity corresponds to B-K Fermi edge, showing chemical state of boron.

Journal Articles

A New grating X-ray spectrometer for 2-4 keV enabling a separate observation of In-L$$beta$$ and Sn-L$$alpha$$ emissions of indium tin oxide

Terauchi, Masami*; Takahashi, Hideyuki*; Handa, Nobuo*; Murano, Takanori*; Koike, Masato; Kawachi, Tetsuya; Imazono, Takashi; Hasegawa, Noboru; Koeda, Masaru*; Nagano, Tetsuya*; et al.

Microscopy, 62(3), p.391 - 395, 2013/06

 Times Cited Count:11 Percentile:60.43(Microscopy)

A new multilayer-coated varied line-spaced grating, JS4000, was fabricated and tested for extending the upper limit of a grating X-ray spectrometer for electron microscopy. This grating was designed for 2-3.8 keV at a grazing incidence angle of 1.35 deg. It was revealed that this new multilayer structure enables us to take soft-X-ray emission spectra continuously from 1.5 keV to 4 keV at the same optical setting. The full-width at half maximum of Te-L$$alpha$$$$_{1,2}$$ (3.8 keV) emission peak was 27 eV. Sn-L$$alpha$$ (3444 eV) and In-L$$beta$$$$_{1}$$ (3487 eV) peaks, which cannot be resolved by a widely used energy-dispersive X-ray spectrometer.

Journal Articles

Ultrasoft-X-ray emission spectroscopy using a newly designed wevelength-dispersiv spectrometer attached to a transmission electron microscope

Terauchi, Masami*; Takahashi, Hideyuki*; Handa, Nobuo*; Murano, Takanori*; Koike, Masato; Kawachi, Tetsuya; Imazono, Takashi; Koeda, Masaru*; Nagano, Tetsuya*; Sasai, Hiroyuki*; et al.

Journal of Electron Microscopy, 61(1), p.1 - 8, 2012/02

 Times Cited Count:30 Percentile:86.93(Microscopy)

A new grating (JS50XL) for spectroscopy of ultrasoft-X-ray in an energy range of 50-200 eV was designed, manufactured and tested. A spectrometer composed of the grating and a multi-channel plate (MCP) detector was constructed. At the low energy end of this spectrometer, a sharp Fermi-edge of Mg-L emission was observed at 49.5 eV with an energy resolution of 0.15 eV. Li-K emission spectra were obtained from metal-Li, surface-oxidized metal-Li and 5%Li-Al. Relative energy shifts observed in Al-L emission spectra of Al, AlN and MgAl$$_{2}$$O$$_{4}$$ were explained by shifts of core binding energies (chemical shift) and band gap energies of those materials. Si-L emissions from Si, SiC and SiO$$_{2}$$ (quartz), and P-L emissions from GaP and InP were presented. These ultrasoft-X-ray emission spectra show a successful extension to lower energy range by using the new soft-X-ray emission spectroscopy (SXES) instrument in electron microscopy.

Journal Articles

A Newly developed grating and soft X-ray spectrometer for electron probe microanalyser and transmission electron microscope; An Acquisition of the Li K emission spectrum with high-energy resolution and detection of light elements

Takahashi, Hideyuki*; Handa, Nobuo*; Murano, Takanori*; Terauchi, Masami*; Koike, Masato; Kawachi, Tetsuya; Imazono, Takashi; Hasegawa, Noboru; Koeda, Masaru*; Nagano, Tetsuya*; et al.

Proceedings of Microscopy and Microanalysis 2011 (Internet), 2 Pages, 2011/08

Soft X-ray spectroscopy with high-energy resolution gives useful information of the chemical bonding states in compounds. Terauchi et al. recently reported a high-energy resolution of 0.2 eV in the Al-L emission spectrum using the previously developed soft X-ray Emission spectrometer (SXES) with a transmission electron microscope. This spectrometer can design to detect the energy from 60 to 1200 eV. In order to progress this result, we had attempted to enhance the detection energy range. Especially to detect the Li-K emission spectrum, we are developing a spectrometer with newly designed aberration corrected gratings. The newly developed grating JS50XL can cover the X-ray energy range from 50 to 200eV with the high energy resolution. It actually means to detect Li-K (55 eV), Al-L (70 eV), Si-L (100 eV), B-K (180 eV) and high order of C-K (279 eV), N-K (392 eV), O-K (525 eV) and so on. This SXES can be equipped not only with TEM, but also with EPMA. Moreover, we found out that attached EPMA with SXES has another strong feature that the X-ray intensity is in directly proportional to probe current. This feature is very useful for the trace element analysis. In the case of Li-K, Be-K and B-K emissions, the detection limits have been evaluated to be a few tens of ppm. For example trace boron analysis is expected to evaluate the newly developed materials quantitatively. This developed spectrometer is hopeful to observe chemical bonding state and trace element analysis in many kinds of fields. In this presentation we report the results for fundamental and actual samples. This development is conducting as one project of Collaborative Development of Innovative Seeds (Practicability verification stage) by Japan Science and Technology Agency.

Journal Articles

An Extension up to 4 keV by a newly developed multilayer-coated grating for TEM-SXES spectrometer

Terauchi, Masami*; Takahashi, Hideyuki*; Handa, Nobuo*; Murano, Takanori*; Koike, Masato; Kawachi, Tetsuya; Imazono, Takashi; Hasegawa, Noboru; Koeda, Masaru*; Nagano, Tetsuya*; et al.

Microscopy and Microanalysis, 17(Suppl.2), p.604 - 605, 2011/07

We have been developing a soft X-ray emission spectroscopy (SXES) instrument for TEM. SXES combined with microscopy should be a hopeful method to reveal physical properties and chemical bonding states of identified small specimen areas of various compounds. Original SXES instruments for conventional transmission electron microscopes basically designed to detect from 60 eV to 1200 eV (or 2000 eV in extended version). For applying to material science, a much wider energy range is necessary. Thus, a new SXES development for electron microscope has started to obtain an energy range from 50 eV to 3800 eV. An extension in lower energy region was achieved by a new aberration corrected (varied-line-spaced: VLS) grating. Conventional gratings in soft-X-ray energy region have gold surface. Au has M-absorption edge at 2.2 keV and shows only a small reflectance higher than the energy. Thus, a new multilayer-coated (MLC) VLS grating has designed and manufactured for obtaining SXES spectra up to 4 keV at a grazing incident angle of 1.35 deg. This development is conducting as one project of Collaborative Development of Innovative Seeds (Practicability verification stage) by Japan Science and Technology Agency.

Journal Articles

Heavy ion irradiation induces autophagy in irradiated C2C12 myoblasts and their bystander cells

Hino, Mizuki*; Hamada, Nobuyuki*; Tajika, Yuki*; Funayama, Tomoo; Morimura, Yoshihiro*; Sakashita, Tetsuya; Yokota, Yuichiro; Fukamoto, Kana*; Muto, Yasuko; Kobayashi, Yasuhiko; et al.

Journal of Electron Microscopy, 59(6), p.495 - 501, 2010/12

 Times Cited Count:13 Percentile:59.79(Microscopy)

Journal Articles

Developments of wavelength-dispersive soft X-ray emission spectrometers for transmission electron microscopes; An Introduction of valence electron spectroscopy for transmission electron microscopy

Terauchi, Masami*; Koike, Masato; Fukushima, Kurio*; Kimura, Atsushi*

Journal of Electron Microscopy, 59(4), p.251 - 261, 2010/08

 Times Cited Count:30 Percentile:85.05(Microscopy)

Two types of wavelength-dispersive soft-X-ray spectrometers, a high-dispersion type and a conventional one, for transmission electron microscopes were constructed. Both spectrometers were extended energy regions $$>$$ 2000 eV. The best energy resolution of 0.08 eV was obtained for an Al L-emission by using the high-dispersion type. W-M and Si-K emissions were clearly resolved by using the conventional type. Soft-X-ray emission spectroscopy based on transmission electron microscopy has an advantage for obtaining spectra from a single crystalline specimen with a defined crystal setting. From C K-emission spectra of single crystalline graphite with different crystal settings, density of states of $$pi$$- and $$sigma$$-bondings were separately derived. Those results demonstrated a method to analyze the electronic states of valence electrons of materials in the nanometer scale based of transmission electron microscopy.

Journal Articles

Influence of laser irradiation condition on a femtosecond laser-assisted tomographic atom probe

Nishimura, Akihiko; Nogiwa, Kimihiro; Otobe, Tomohito; Okubo, Tadakatsu*; Hono, Kazuhiro*; Kondo, Keietsu; Yokoyama, Atsushi

Ultramicroscopy, 109(5), p.467 - 471, 2009/04

 Times Cited Count:7 Percentile:30.99(Microscopy)

Influence of femtosecond laser pulse condition on the performance of an energy compensated tomographic atom probe (ECOTAP) was investigated. Chirping ratio for laser pulses was controlled by a compressor stage. We have succeeded to get tomographic images of oxide dispersion strengthen steel, which will be used as fast breeder reactors. The ECOTAP successfully observed that the instability of the femtosecond laser pulses make the mass peaks slightly sifted or broadened to higher mass number. To investigate insulator materials, numerical simulation of conductivity increase on diamond has been successfully demonstrated.

Journal Articles

Qualitative detection of Mg content in a leaf of hedera helix by using X-ray radiation from a laser plasma source

Reale, L.*; Lai, A.*; Sighicelli, M.*; Faenov, A. Y.; Pikuz, T.*; Flora, F.*; Zuppella, P.*; Limongi, T.*; Palladino, L.*; Poma, A.*; et al.

Microscopy Research and Technique, 71(6), p.459 - 468, 2008/06

 Times Cited Count:2 Percentile:11.01(Anatomy & Morphology)

Journal Articles

Mapping the intake of different elements in vegetal tissues by dual-energy X-ray imaging at Da$$Phi$$ne synchrotron light source

Reale, L.*; Kaiser, J.*; Reale, A.*; Lai, A.*; Flora, F.*; Balerna, A.*; Cinque, G.-F.*; Fanelli, M.*; Ruggieri, F.*; Faenov, A. Y.; et al.

Microscopy Research and Technique, 71(3), p.179 - 185, 2008/03

 Times Cited Count:2 Percentile:11.01(Anatomy & Morphology)

Journal Articles

High-resolution water window X-ray imaging of in vivo cells and their products using LiF crystal detectors

Bonfigli, F.*; Faenov, A. Y.; Flora, F.*; Francucci, M.*; Gaudio, P.*; Lai, A.*; Martellucci, S.*; Montereali, R. M.*; Pikuz, T.*; Reale, L.*; et al.

Microscopy Research and Technique, 71(1), p.35 - 41, 2008/01

 Times Cited Count:23 Percentile:71.75(Anatomy & Morphology)

Journal Articles

Conformational analysis of the structure of ribosome fit into electron microscopy density maps with normal mode analyses and molecular dynamics simulations

Ishida, Hisashi; Matsumoto, Atsushi; Tsutsumi, Yu*; Yura, Kei

Proceedings of 16th International Microscopy Congress (IMC 2006), P. 242, 2006/09

Supra-biomolecules, which contain numerous proteins and nucleic acids, function when the constituent molecules are assembled. Therefore, it is important to determine not only the 3D structures of the constituent molecules but also the 3D structure of the supra-biomolecule. Although X-ray crystallography can determine the atomic coordinates of biomolecules, it has difficulty in handling supra-biomolecules, because crystals of huge molecules cannot be made with ease. Single particle analysis using an electron microscope (EM) has been used to observe the structure of supra-biomolecules, but the resolution of the EM image has only achieve to the atomic level in a limited situation. Therefore, several attempts have been carried out to determine the 3D structure of supra-biomolecules in atomic resolution by fitting the constituent molecules, determined by X-ray crystallography, into an EM density map. In those attempts, each constituent molecule is usually fit into the EM density map manually, and the constituent molecules may have atomic collisions at their interfaces.

Journal Articles

Development of wavelength-dispersive X-ray spectrometer for a conventional analytical transmission electron microscope

Terauchi, Masami*; Koike, Masato; Fukushima, Kurio*; Kimura, Jun*

Microscopy and Microanalysis, 12(Suppl.2), p.866 - 867, 2006/08

no abstracts in English

47 (Records 1-20 displayed on this page)