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Journal Articles

Nanometer-thick crystalline ice plates in rapidly-frozen glucose solution observed by spin-contrast-variation small-angle neutron scattering

Kumada, Takayuki; Nakagawa, Hiroshi; Miura, Daisuke; Sekine, Yurina; Motokawa, Ryuhei; Hiroi, Kosuke; Inamura, Yasuhiro; Oku, Takayuki; Oishi, Kazuki*; Morikawa, Toshiaki*; et al.

Hamon, 34(2), p.50 - 53, 2024/05

Spin-contrast-variation (SCV) small-angle neutron scattering (SANS) enabled us to determine structure of nano-ice crystals that were generated in rapidly frozen sugar solution. In the frozen glucose solution, we found that the nano-ice crystals formed a planar structure with a radius larger than several tens of nanometers and a thickness of 2-3 nm, which was close to the critical nucleation size of ice crystals in supercooled water. This result suggests that the glucose molecules were preferentially bound to a specific face of nano-ice crystals, and then blocked the crystal growth perpendicular to that face.

Journal Articles

Nanocellulose hydrogels formed via crystalline transformation from cellulose I to II and subsequent freeze cross-linking reaction

Sekine, Yurina; Nankawa, Takuya; Hiroi, Kosuke; Oba, Yojiro*; Nagakawa, Yoshiyasu*; Sugita, Tsuyoshi; Shibayama, Yuki; Ikeda-Fukazawa, Tomoko*

Carbohydrate Polymers, 327, p.121538_1 - 121538_11, 2024/03

 Times Cited Count:2 Percentile:49.33(Chemistry, Applied)

We describe non-toxic, tough nanocellulose (NC) hydrogels formed from chemically unmodified NC by cellulose crystalline transformation and subsequent freeze cross-linking reaction. Using low-concentration NaOH and freezing together induced the crystalline transformation of NC from cellulose I to II via freeze concentration. After the crystalline transformation, cross-linking between the NC and CA in the freeze concentration layer (FCL) provided a strong NC network structure, forming NC hydrogels with high mechanical strength. The freeze-cross-linked NC hydrogel easily retained powder adsorbents in its inner space by mixing the NC-NaOH sol and the powder, and the hydrogel showed high removal efficiency for heavy metals. The results highlight the versatility of chemically unmodified celluloses in developing functional materials, suggest possible practical applications.

Journal Articles

Contrast dependence of scattering profiles for poly(ethylene glycol) in water; Investigation by small-angle neutron scattering with $$^{3}$$He spin filter and small-angle X-ray scattering

Ryoki, Akiyuki*; Watanabe, Fumi*; Okudaira, Takuya*; Takahashi, Shingo*; Oku, Takayuki; Hiroi, Kosuke; Motokawa, Ryuhei; Nakamura, Yo*

Journal of Chemical Physics, 160(11), p.114907_1 - 114907_9, 2024/03

 Times Cited Count:0 Percentile:0.00(Chemistry, Physical)

Journal Articles

Effects of Fe ions, ultraviolet irradiation, and heating on microscopic structures of black lacquer films

Nankawa, Takuya; Sekine, Yurina; Matsumura, Daiju; Hiroi, Kosuke; Takata, Shinichi; Kamiya, Yoshimi*; Honda, Takayuki*

Langmuir, 40(11), p.5725 - 5730, 2024/03

 Times Cited Count:0 Percentile:0.00(Chemistry, Multidisciplinary)

The chemical reaction between Fe and lacquer has been used to create the black color lacquer since ancient times. Here, the chemical state of Fe ions in black lacquer was investigated by using X-ray absorption near edge structure (XANES), extended X-ray absorption fine structure (EXAFS), and Fourier transform-infrared (FT-IR) spectroscopy. Fe(II) or Fe(III) was added to the lacquer paste to prepare black lacquer films by air drying, heating, or UV irradiation. The XANES spectral features of all the film samples were similar, meaning that the Fe ions in the samples existed in the trivalent state regardless of the oxidation state of the initially added Fe. The corresponding Fourier transforms of the EXAFS spectra around the Fe K-edge were used to investigate Fe sites in the lacquer films. The spectra of all the film samples were similar shapes, but the peak intensities decreased in the order air dried $$>$$ heated $$>$$ UV irradiated films. This result indicates that heating and UV irradiation made the coordination structure of Fe in the lacquer non-uniform, and that heating caused the greatest non-uniformity. The complementary use of XANES, XAFS, and FT-IR spectroscopy is highly effective for non-destructive analysis of black lacquer in precious cultural artifacts.

Journal Articles

Development of a D$$_2$$O/H$$_2$$O vapor generator for contrast-variation neutron scattering

Arima-Osonoi, Hiroshi*; Takata, Shinichi; Kasai, Satoshi*; Ouchi, Keiichi*; Morikawa, Toshiaki*; Miyata, Noboru*; Miyazaki, Tsukasa*; Aoki, Hiroyuki; Iwase, Hiroki*; Hiroi, Kosuke; et al.

Journal of Applied Crystallography, 56(6), p.1802 - 1812, 2023/12

 Times Cited Count:2 Percentile:60.51(Chemistry, Multidisciplinary)

Journal Articles

Upgrade of the small-angle neutron scattering diffractometer SANS-J at JRR-3

Kumada, Takayuki; Motokawa, Ryuhei; Oba, Yojiro; Nakagawa, Hiroshi; Sekine, Yurina; Micheau, C.; Ueda, Yuki; Sugita, Tsuyoshi; Birumachi, Atsushi; Sasaki, Miki; et al.

Journal of Applied Crystallography, 56(6), p.1776 - 1783, 2023/12

 Times Cited Count:10 Percentile:97.31(Chemistry, Multidisciplinary)

The combination of the existing position-sensitive photomultiplier and the $$^{3}$$He main detector with focusing devices, and the newly installed front detectors in SANS-J at JRR-3 covers small-angle neutron scattering signals in the range of the magnitude of the scattering vector Q from 0.002 to 6 nm-1 gaplessly with three standard device layouts. The installation of the front detector and a graphical user interface system largely improved the usability of SANS-J.

Journal Articles

Polarized neutrons observed nanometer-thick crystalline ice plates in frozen glucose solution

Kumada, Takayuki; Nakagawa, Hiroshi; Miura, Daisuke; Sekine, Yurina; Motokawa, Ryuhei; Hiroi, Kosuke; Inamura, Yasuhiro; Oku, Takayuki; Oishi, Kazuki*; Morikawa, Toshiaki*; et al.

Journal of Physical Chemistry Letters (Internet), 14(34), p.7638 - 7643, 2023/08

 Times Cited Count:0 Percentile:0.00(Chemistry, Physical)

The structure of nano-ice crystals in rapidly frozen glucose solution was elucidated by using spin-contrast-variation small-angle neutron scattering, which distinguishes the nano-ice crystal signal from the frozen amorphous solution signal by the polarization-dependent neutron scattering. The analysis revealed that the nano-ice crystals form a planar structure with a diameter exceeding tens of nanometers and a thickness of 1 nm, which is close to the critical nucleation size. This result suggests that the glucose molecules are preferentially bound to a specific face of nano-ice crystals, and then block the crystal growth perpendicular to that face.

Journal Articles

Dynamic exchange of amphiphilic random copolymers between micelles in water; Kinetics and mechanism analyzed by TR-SANS

Hibino, Masayuki*; Takata, Shinichi; Hiroi, Kosuke; Aoki, Hiroyuki; Terashima, Takaya*

Macromolecules, 56(8), p.2955 - 2964, 2023/04

 Times Cited Count:3 Percentile:18.26(Polymer Science)

Journal Articles

Polarized neutron scattering study of hollow Fe$$_{3}$$O$$_{4}$$ submicron spherical particles

Kobayashi, Satoru*; Nomura, Eiji*; Chiba, Momoko*; Kawamura, Yukihiko*; Oishi, Kazuki*; Hiroi, Kosuke; Suzuki, Junichi*

Journal of Magnetism and Magnetic Materials, 569, p.170410_1 - 170410_9, 2023/03

 Times Cited Count:3 Percentile:51.61(Materials Science, Multidisciplinary)

Journal Articles

Sodium diffusion in hard carbon studied by small- and wide-angle neutron scattering and muon spin relaxation

Oishi, Kazuki*; Igarashi, Daisuke*; Tatara, Ryoichi*; Kawamura, Yukihiko*; Hiroi, Kosuke; Suzuki, Junichi*; Umegaki, Izumi*; Nishimura, Shoichiro*; Koda, Akihiro*; Komaba, Shinichi*; et al.

Journal of Physics; Conference Series, 2462, p.012048_1 - 012048_5, 2023/03

 Times Cited Count:0 Percentile:0.00(Physics, Applied)

Journal Articles

Magnetic structural analysis of nanocrystalline soft magnets by small-angle neutron scattering

Mamiya, Hiroaki*; Oba, Yojiro; Hiroi, Kosuke; Miyatake, Takayuki*; Gautam, R.*; Sepehri-Amin, H.*; Okubo, Tadakatsu*

IEEE Magnetics Letters, 14, p.7100105_1 - 7100105_5, 2023/02

 Times Cited Count:2 Percentile:49.60(Engineering, Electrical & Electronic)

Journal Articles

Microscopic structural changes during the freeze cross-linking reaction in carboxymethyl cellulose nanofiber hydrogels

Miura, Daisuke*; Sekine, Yurina; Nankawa, Takuya; Sugita, Tsuyoshi; Oba, Yojiro; Hiroi, Kosuke; Ozawa, Tatsuhiko

Carbohydrate Polymer Technologies and Applications (Internet), 4, p.100251_1 - 100251_9, 2022/12

The reaction mechanism of carboxymethyl cellulose nanofiber (CMCF) hydrogel formed by freeze-crosslinking was investigated. We succeeded in observing the hierarchical structural changes during the freeze-crosslinking reaction. Freeze-crosslinked CMCF hydrogels exhibited a characteristic hierarchical alignment structure from the angstrom to micrometer scale that differed from normal cross-linked CMCF hydrogels produced by a conventional method without freezing. It was shown that the characteristic hierarchical structure contributes the excellent mechanical properties of freeze-crosslinked CMCF hydrogels.

Journal Articles

Magnetization process of cubic Fe$$_3$$O$$_4$$ submicron particles studied by polarized small-angle neutron scattering

Nomura, Eiji*; Chiba, Momoko*; Matsuo, Sakoto*; Noda, Chiaki*; Kobayashi, Satoru*; Manjanna, J.*; Kawamura, Yukihiko*; Oishi, Kazuki*; Hiroi, Kosuke; Suzuki, Junichi*

AIP Advances (Internet), 12(3), p.035034_1 - 035034_5, 2022/03

 Times Cited Count:5 Percentile:52.19(Nanoscience & Nanotechnology)

Journal Articles

Development of spin-contrast-variation neutron powder diffractometry for extracting the structure factor of hydrogen atoms

Miura, Daisuke*; Kumada, Takayuki; Sekine, Yurina; Oku, Takayuki; Takata, Shinichi; Hiroi, Kosuke; Iwata, Takahiro*

J-PARC 22-02; J-PARC MLF Annual Report 2021, p.6 - 7, 2022/03

We carried out spin contrast variation neutron powder diffractometry of glutamic acid crystal. The diffraction peak intensities varied as a function of proton polarization. We extracted the structure factor of hydrogen atoms from the variation of peak intensities.

Journal Articles

Strain distribution visualization of punched electrical steel sheets using neutron Bragg-edge transmission imaging

Sasada, Seiji*; Takahashi, Yoshihito*; Takeuchi, Keisuke*; Hiroi, Kosuke; Su, Y. H.; Shinohara, Takenao; Watanabe, Kenichi*; Uritani, Akira*

Japanese Journal of Applied Physics, 61(4), p.046004_1 - 046004_8, 2022/03

 Times Cited Count:0 Percentile:0.00(Physics, Applied)

Journal Articles

Spontaneous formations of nanoconfined water in ionic liquids by small-angle neutron scattering

Abe, Hiroshi*; Nemoto, Fumiya*; Hiroi, Kosuke; Oishi, Kazuki*; Takata, Shinichi

Journal of Molecular Liquids, 346, p.117035_1 - 117035_6, 2022/01

 Times Cited Count:6 Percentile:61.81(Chemistry, Physical)

Journal Articles

High-spatial-resolution measurement of magnetization distribution using polarized neutron imaging

Sasada, Seiji*; Hiroi, Kosuke; Osanai, Kenta*; Shinohara, Takenao; Watanabe, K.*; Uritani, Akira*

Japanese Journal of Applied Physics, 60(12), p.126003_1 - 126003_6, 2021/12

 Times Cited Count:4 Percentile:29.17(Physics, Applied)

Journal Articles

Development of spin-contrast-variation neutron powder diffractometry for extracting the structure factor of hydrogen atoms

Miura, Daisuke*; Kumada, Takayuki; Sekine, Yurina; Motokawa, Ryuhei; Nakagawa, Hiroshi; Oba, Yojiro; Ohara, Takashi; Takata, Shinichi; Hiroi, Kosuke; Morikawa, Toshiaki*; et al.

Journal of Applied Crystallography, 54(2), p.454 - 460, 2021/04

AA2020-0724.pdf:2.05MB

 Times Cited Count:1 Percentile:14.61(Chemistry, Multidisciplinary)

We developed a spin-contrast-variation neutron powder diffractometry technique that extracts the structure factor of hydrogen atoms, namely, the contribution of hydrogen atoms to a crystal structure factor. Crystals of L-glutamic acid were dispersed in a dpolystyrene matrix containing 4-methacryloyloxy-2,2,6,6,-tetramethyl-1-piperidinyloxy (TEMPO methacrylate) to polarize their proton spins dynamically. The intensities of the diffraction peaks of the sample changed according to the proton polarization, and the structure factor of the hydrogen atoms was extracted from the proton-polarization dependent intensities. This technique is expected to enable analyses of the structures of hydrogen-containing materials that are difficult to determine with conventional powder diffractometry.

Journal Articles

Polarization analysis for small-angle neutron scattering with a $$^{3}$$He spin filter at a pulsed neutron source

Okudaira, Takuya; Ueda, Yuki; Hiroi, Kosuke; Motokawa, Ryuhei; Inamura, Yasuhiro; Takata, Shinichi; Oku, Takayuki; Suzuki, Junichi*; Takahashi, Shingo*; Endo, Hitoshi*; et al.

Journal of Applied Crystallography, 54(2), p.548 - 556, 2021/04

 Times Cited Count:4 Percentile:48.63(Chemistry, Multidisciplinary)

Neutron polarization analysis (NPA) for small-angle neutron scattering (SANS) experiments using a pulsed neutron source was successfully achieved by applying a $$^{3}$$He spin filter as a spin analyzer for the scattered neutrons. The $$^{3}$$He spin filter covers a sufficient solid angle for performing SANS experiments, and the relaxation time of the $$^{3}$$He polarization is sufficient for continuous use over a few days, thus reaching the typical duration required for a complete set of SANS experiments. Although accurate evaluation of the incoherent neutron scattering, which is predominantly attributable to hydrogen atoms in samples, is practically difficult using calculations based on the sample elemental composition, the developed NPA approach with consideration of the influence of multiple neutron scattering enabled reliable decomposition of the SANS intensity distribution into the coherent and incoherent scattering components. To date, NPA has not been well established as a standard technique for SANS experiments at pulsed neutron sources. This work is anticipated to greatly contribute to the accurate determination of the coherent neutron scattering component for scatterers in various types of organic sample systems in SANS experiments at J-PARC.

Journal Articles

Study of neutron-nuclear spin correlation term with a polarized Xe target

Sakai, Kenji; Oku, Takayuki; Okudaira, Takuya; Kai, Tetsuya; Harada, Masahide; Hiroi, Kosuke; Hayashida, Hirotoshi*; Kakurai, Kazuhisa*; Shimizu, Hirohiko*; Hirota, Katsuya*; et al.

JPS Conference Proceedings (Internet), 33, p.011116_1 - 011116_6, 2021/03

In neutron fundamental physics, study of correlation term $${bf s}cdot{bf I}$$ of a neutron spin $${bf s}$$ and a target nuclear spin $${bf I}$$ is important because $${bf s}cdot{bf I}$$ term interferes to parity non-conserving (PNC) and time reversal non-conserving terms. For this study, a xenon (Xe) is an interesting nucleus because it has been observed an enhancement of PNC effect around neutron resonance peaks, and polarizes up to $$ sim 10^{-1}$$ by using a spin exchange optical pumping (SEOP) method. We would plan to develop a polarized Xe gas target with a compact in-situ SEOP system, and to study $${bf s}cdot{bf I}$$ term by utilizing epithermal neutron beams supplied from a high intense pulsed spallation neutron source. As the first step, we attempted to measure neutron polarizing ability caused by $${bf s}cdot{bf I}$$ term at a 9.6 eV s-wave resonance peak of $$^{129}$$Xe at BL10 in MLF, by detecting change $$Delta R$$ of ratio between neutron transmissions with the polarized and unpolarized Xe target. After demonstrating that our apparatus could detect small change ($$Delta R_{rm DB} , {approx},10^{-2}$$) of neutron transmissions caused by Doppler broadening effect, a signified value of $$Delta R$$ has been obtained as preliminary results. For analyzing the obtained $$Delta R$$ in detail, we are improving our nuclear magnetic resonance and electron paramagnetic resonance systems for evaluating Xe polarization independently of neutron beams.

130 (Records 1-20 displayed on this page)