An Extension of detectable energy-range of SXES spectrometer for electron microscopes

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

JAEA-Conf 2013-001, p.77 - 80, 2013/09

https://doi.org/10.11484/jaea-conf-2013-001

We have been developing a soft X-ray emission spectroscopy (SXES) instrument for electron microscopes (TEM, EPMA/SEM) with an extension of detectable energy range to 50-4000 eV. An introduction of valence electron spectroscopy with microscopy will supply fruitful information on bonding electrons, which cannot be obtained by EELS and EDS. For extend the lowest (or highest) detection energy upto 50 eV (or 4000 eV), a new laminar-type varied-line-spacing (VLS) grating, JS50XL, (or JS4000) has designed and manufactured. JS50XL and JS4000 having 1200 and 2400 lines/mm as well as coated by Au and a new multilayer-structure of W/BC for a wide-band energy region of 2000-3800 eV, respectively. Those gratings were installed and tested in a SXES spectrometer attached to a TEM. The extension in lowest detection energy was confirmed by Mg-L emission (JS50XL). The energy resolution was 0.2 eV at Fermi edge of 49.5 eV. It can be also seen a sharp Fermi edge for Li-K emission spectrum of metal-Li. The high energy resolution was confirmed by Te-La emission at 3.8 keV (JS4000). The full width at half maximum of the peak was 27 eV. The detection energy range was successfully extended by using the two new VLS-gratings.

Development of an objective flat-field spectrograph for electron microscopic soft X-ray emission spectrometry in 50-4000 eV

Imazono, Takashi; Koike, Masato; Kawachi, Tetsuya; Hasegawa, Noboru; Koeda, Masaru*; Nagano, Tetsuya*; Sasai, Hiroyuki*; Oue, Yuki*; Yonezawa, Zeno*; Kuramoto, Satoshi*; et al.

Proceedings of SPIE, Vol.8848, p.884812_1 - 884812_14, 2013/09

https://doi.org/10.1117/12.2024652

We have developed an objective soft X-ray flat-field spectrograph to be able to attach to electron microscopes. This spectrograph has two attractive features. One is that it is designed to cover a wide energy range of 50-4000 eV by using four varied-line-spacing holographic gratings optimized for 50-200 eV, 155-350 eV, 300-2200 eV, and 2000-4000 eV. They can be accommodated in the single spectrograph. The other is a newly invented W/BC multilayer coating covering the 2000-4000 eV range. It can enhance the diffraction efficiency above a practical level of % at a constant incidence angle in the whole energy range.

In-plane orientation control of 2,7-diphenyl[1]benzothieno[3,2-][1]benzothiophene monolayer on bismuth-terminated Si(111) vicinal surfaces with wettability optimization

Otomo, Manabu; Tsuchida, Yuya*; Muraya, Naoki*; Yanase, Takashi*; Sakai, Seiji; Yonezawa, Tetsu*; Nagahama, Taro*; Hasegawa, Tetsuya*; Shimada, Toshihiro*

Journal of Physical Chemistry C, 117(22), p.11555 - 11561, 2013/06

https://doi.org/10.1021/jp3117837

We report in-plane orientation control of newly developed high-mobility organic semiconductor: 2,7-diphenyl[1]benzothieno[3,2-][1]benzothiophene (DPh-BTBT). As previously reported on monolayer pentacene, it was revealed that bunched steps on vicinal Si(111) with bismuth termination break the surface symmetry and reduce three-fold symmetry of DPh-BTBT grains into quasi-single orientation. Interestingly, the critical step height necessary for the orientation control was different from that of pentacene. We examined several mechanisms of orientation control and concluded that the facet nano structure fabricated by step bunching is working as an anisotropic template. We will also show the wettability control of bismuth terminated silicon surface and show that the growth mode of DPh-BTBT is dependent on the surface nanostructure of Bi-Si.

Development of a flat-field spectrograph with a wide-band multilayer grating and prefocusing mirror covering 2-4 keV

Imazono, Takashi; Koike, Masato; Hasegawa, Noboru; Koeda, Masaru*; Nagano, Tetsuya*; Sasai, Hiroyuki*; Oue, Yuki*; Yonezawa, Zeno*; Kuramoto, Satoshi*; Terauchi, Masami*; et al.

Journal of Physics; Conference Series, 425(15), p.152008_1 - 152008_4, 2013/03

https://doi.org/10.1088/1742-6596/425/15/152008

We have developed a flat-field spectrograph equipped with a wide-band multilayer grating and prefocusing mirror for the 2-4 keV range. To realize a spectrograph without any mechanical movement, the multilayer has a newly invented layer structure to uniformly enhance the diffraction efficiency (or reflectivity) of the grating (or prefocusing mirror) at a fixed angle of incidence in the whole energy region. The multilayer structure consisting of W and BC layers has been deposited by ion beam sputtering method on a varied-line-spacing laminar-type holographic grating. Also the same multilayer has been done on a spherical substrate. The average diffraction efficiency (or reflectivity) of the multilayer grating (or spherical mirror) is in excess of 3% at 88.65 (or 4% at 88.00) in the 2.1-3.8 keV range. The throughput of the spectrograph with multilayer optics can be evaluated to be 2-5000 times higher than that with conventional optics coated by a gold layer.

Laminar and blazed type holographic gratings for a versatile soft X-ray spectrograph attached to an electron microscope and their evaluation in the 50-200 eV range

Imazono, Takashi; Koike, Masato; Kawachi, Tetsuya; Hasegawa, Noboru; Koeda, Masaru*; Nagano, Tetsuya*; Sasai, Hiroyuki*; Oue, Yuki*; Yonezawa, Zeno*; Kuramoto, Satoshi*; et al.

Applied Optics, 51(13), p.2351 - 2360, 2012/05

https://doi.org/10.1364/AO.51.002351

Laminar and blazed types holographic varied-line-spacing spherical gratings for use in a versatile soft X-ray flat-field spectrograph attached to an electron microscope are designed, fabricated, and evaluated. The absolute diffraction efficiencies of laminar (or blazed) master and replica gratings at 86.00 incidence evaluated by synchrotron radiation show over 5% (or 8%) in the 50-200 eV range with the maxima of 22% (or 26-27%). Also the resolving power evaluated by a laser produced plasma source is in excess of 700 at the energy near the emission spectrum of lithium (55 eV) for all gratings. Moreover, the emission spectrum of metallic Li with high spectral resolution is successfully observed with the spectrograph attached to a transmission electron microscope.

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

http://www.microscopy.org/MandM/2011/abstracts/LB-1.pdf

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.

Performance testing of vapor-liquid equilibrium type of gas permeation source with vacuum balance

Hatano, Toshihisa; Hiratsuka, Hajime; Hasegawa, Koichi; Kaifuku, Yuichiro*; Abe, Tetsuya

Journal of the Vacuum Society of Japan, 54(5), p.313 - 316, 2011/05

https://doi.org/10.3131/jvsj2.54.313

In the quantitative measure of air pollution gas and impurity gas in the aluminum recycle material etc, it is requested to show the amount of the gas directly by the weight value from the viewpoint of global standard. Therefore, standard gas sources expressed in units of weight are needed. The vapor-liquid equilibrium type of gas permeation sources (hereafter "P-tube") is used well in the atmosphere as calibration gas of the measuring equipment and a standard gas source for low concentration of gas. The study aims to estimate performance of P-tubes in the vacuum. Specifically, weight change of P-tubes were measured with the vacuum balance and at the same time concentration of gas constituents were also measured by Electron Ionization-Quadrupole Mass Spectrometer (hereafter, EI-QMS). The relation of both was examined. The prospect was obtained that the P-tube was able to be used as a standard gas source in the vacuum though the warming was needed.

Investigation and design of the dismantling process of irradiation capsules containing tritium, 2; Detailed design and trial fabrication of capsule dismantling apparatus and investigation of glove box facility

Hayashi, Kimio; Nakagawa, Tetsuya; Onose, Shoji; Ishida, Takuya; Nakamichi, Masaru; Katsuyama, Kozo; Iwamatsu, Shigemi; Hasegawa, Teiji; Kodaka, Hideo; Takatsu, Hideyuki; et al.

JAEA-Technology 2009-007, 168 Pages, 2009/03

JAEA-Technology-2009-007.pdf:31.88MB

In-pile functional tests of breeding blankets have been planned by Japan Atomic Energy Agency (JAEA), using a test blanket module (TBM) which will be loaded in the International Thermonuclear Experimental Reactor (ITER). In preparation for the in-pile functional tests, JAEA has been being performed irradiation experiments of lithium titanate (LiTiO), which is the first candidate of solid breeder materials for the blanket of the demonstration reactor (DEMO) under designing in Japan. The present report describes (1) results of a detailed design and trial fabrication tests of a dismantling apparatus for irradiation capsules which were used in irradiation experiments by the Japan Materials Testing Reactor (JMTR) of JAEA, and (2) results of a preliminary investigation of a glove box facility for post-irradiation examinations (PIEs). In the detailed design of the dismantling apparatus, datailed specifications and the installation methods were examined, based on results of a conceptual design and basic design. In the trial fabrication, cutting tests were curried out by making a mockup of a cutting component. Furthermore, a preliminary investigation of a glove box facility was carried out in order to secure a facility for PIE work after the capsule dismantling, which revealed a technical feasibility.

Design and application of NOBORU; NeutrOn Beam line for Observation and Research Use at J-PARC

Oikawa, Kenichi; Maekawa, Fujio; Harada, Masahide; Kai, Tetsuya; Meigo, Shinichiro; Kasugai, Yoshimi; Oi, Motoki; Sakai, Kenji; Teshigawara, Makoto; Hasegawa, Shoichi; et al.

Nuclear Instruments and Methods in Physics Research A, 589(2), p.310 - 317, 2008/05

https://doi.org/10.1016/j.nima.2008.02.019

NOBORU, NeutrOn Beam-line for Observation and Research Use, has been constructed in the Materials and Life Science Facility (MLF) of J-PARC. NOBORU is designed to "Observe" a 1 MW Japan Spallation Neutron Source (JSNS), i.e., to study the neutronic performance of JSNS. NOBORU also will be used for "Research" activities, i.e., as a test port for R&D activities and trial users who have new ideas. In this paper, the design and application of NOBORU are described, and its expected performance is investigated by Monte Carlo simulations.

Measurement of expiratory alcohol by QMS gas analyzer

Arai, Takashi; Hiratsuka, Hajime; Hasegawa, Koichi; Hatano, Toshihisa; Nemoto, Masahiro; Abe, Tetsuya

Heisei-18-Nendo Nagoya Daigaku Sogo Gijutsu Kenkyukai Sochi Gijutsu Kenkyukai Hokokushu, p.76 - 79, 2007/03

Recently, the accident because of drunken driving is taken up in the topic of news, and the concern is had at the amount of the drinking and the drinking time etc. of the inside of the body. It is said that there is a correlation in the alcoholic density included in an alcoholic amount and the expiration in blood so far, and is reported on the equipment that measures an alcoholic density of the expiration based on this. We also are executing the breath analysis as an example of applying QMS (four pile polar mass spectrometer) gas analyzer "Gravimas". This time, an alcoholic density in the expiration was measured, the performance of this device to alcoholic detection was examined, and the change at the time of an alcoholic density in the expiration high sensitivity was measured. These results suggest the utility of the breath analysis that uses QMS.