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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:22 Percentile:86.04(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 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

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

Journal Articles

A New high energy-resolution soft-X-ray spectrometer for a transmission electron microscope

Terauchi, Masami*; Koike, Masato

Microscopy and Microanalysis, 9(S02), p.894 - 895, 2003/08

We have been developing a high energy-resolution soft-X-ray spectrometer for a transmission electron microscope to obtain the information of the density of states (DOS) of the valence band (occupied states) from identified small specimen areas. We have designed and produced a new grating. The new varied-line-spacing laminar-type holographic grating was designed to have a focal distance of about 50 cm. An energy resolution of about 0.7 eV is expected for X-ray energy of about 1000 eV.

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