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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：0.01(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.
Kumada, Takayuki; Miura, Daisuke*; Akutsu, Kazuhiro*; Oku, Takayuki; Torikai, Naoya*; Niizeki, Tomotake*
Hamon, 32(4), p.165 - 168, 2022/11
We demonstrated the advantage of spin-contrast-variation neutron reflectometry on the structure analysis of buried interface between resin and porous silica layers. The interface structure was not reproduced by the normal Gaussian model, but by the asymmetric interface model where crosslinked polymer chains neither permeate the pore nor follow the surface roughness of the silica layer.
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.
Miura, Daisuke*; Kumada, Takayuki; Iwata, Takahiro*
Nihon Kessho Gakkai-Shi, 63(4), p.287 - 293, 2021/12
We have developed the spin-contrast-variation neutron powder diffractometry to observe hydrogen atoms in a crystalline sample by polarized neutron and polarized proton in the crystal. L-glutamic acid crystals were dispersed in a deuterated polystyrene matrix containing a polarizing agent. The intensities of the diffraction peaks of the sample changed according to the proton polarization. The spin-contrast-variation neutron powder diffractometry can extract diffraction from hydrogen atoms because of the variation of peak intensities as a function of the proton polarization. This technique is expected to enable analyses of the structures of hydrogen-containing materials that are difficult to determine with conventional powder diffractometry.
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
Times Cited Count：1 Percentile：16.63(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.
Kumada, Takayuki; Miura, Daisuke*; Akutsu, Kazuhiro*; Suzuki, Junichi*; Torikai, Naoya*
Hamon, 30(4), p.207 - 211, 2020/11
We developed a technique of spin-contrast-variation neutron reflectivity (SCV-NR) for structural analyses of multilayer films. The SCV-NR curves of the polystyrene monolayer film were precisely reproduced using a common set of structural parameters and neutron scattering length density at each proton polarization. This result ensures that SCV-NR curves are not deformed by inhomogeneous PH due to the spin-diffusion mechanism. The number of structural parameters of the lamellar microphase-separated poly(styrene-block-isoprene) thin film is too large to determine with a single unpolarized reflectivity curve only. However, these parameters converged through the global analysis of the SCV-NR curves. In this manner, SCV-NR determines the structure of multilayer films while excluding the incorrect structural model that accidentally accounts for a single unpolarized reflectivity curve only.
Kumada, Takayuki; Akutsu, Kazuhiro*; Oishi, Kazuki*; Morikawa, Toshiaki*; Kawamura, Yukihiko*; Sahara, Masae*; Suzuki, Junichi*; Torikai, Naoya*
Journal of Applied Crystallography, 52(5), p.1054 - 1060, 2019/10
Times Cited Count：3 Percentile：31.93(Chemistry, Multidisciplinary)We developed a technique of spin-contrast-variation neutron reflectometry (SCV-NR). Polarized-neutron reflectivity curves of film samples vary as a function of their proton-polarization P. The P-dependent reflectivity curves of a polystyrene film was precisely reproduced using a common set of structure parameters and the P-dependent neutron scattering length. The reflectivity curve of poly (styrene-block-isoprene) (PSPI) presented a shoulder attributed to holes with the depth corresponding to one period of periodic lamellae on the free surface only at a specific P. In this way, structural information about specific surfaces or interfaces can be obtained by controlling the P.
Kumada, Takayuki; 7 of others*
JPS Conference Proceedings (Internet), 22, p.011015_1 - 011015_5, 2018/11
Kumada, Takayuki
Denshi Supin Saiensu, 15(Autumn), p.86 - 91, 2017/10
no abstracts in English
Osa, Akihiko; Koizumi, Mitsuo; Sekine, Toshiaki; Yamamoto, Hiroshi*; *; *; *
"Fuanteikaku No Rikogaku Oyobi Kaku Keisokuho(II)" Ni Kansuru Semmon Kenkyukai Hokokusho, 0, p.28 - 30, 1997/00
no abstracts in English
Kumada, Takayuki
no journal, ,
no abstracts in English
Kumada, Takayuki; Akutsu, Kazuhiro*; Oishi, Kazuki*; Morikawa, Toshiaki*; Kawamura, Yukihiko*; Suzuki, Junichi*; Torikai, Naoya*
no journal, ,
no abstracts in English
Kumada, Takayuki
no journal, ,
no abstracts in English
Kumada, Takayuki
no journal, ,
Kumada, Takayuki; Akutsu, Kazuhiro*; Oishi, Kazuki*; Morikawa, Toshiaki*; Kawamura, Yukihiko*; Sahara, Masae*; Suzuki, Junichi*; Torikai, Naoya*
no journal, ,
Scattering power of neutron against proton remarkably depends on relative direction of these spins. Spin contrast variation (SCV) is a technique to determine structure of composite materials from their polarized neutron scattering profiles that vary as a function of proton polarization. Very recently, we succeeded in the first SCV neutron reflectometry measurement. We determined roughness of two surfaces of a thin-film polymer from the SCV neutron reflection curves. We will use this technique to study structures of multilayered films such as coupling agents (glues) between organic and inorganic materials.
Kumada, Takayuki; Akutsu, Kazuhiro*; Oishi, Kazuki*; Morikawa, Toshiaki*; Kawamura, Yukihiko*; Sahara, Masae*; Suzuki, Junichi*; Torikai, Naoya*
no journal, ,
Scattering power of neutron against proton remarkably depends on relative direction of these spins. Spin contrast variation (SCV) is a technique to determine structure of composite materials from their polarized neutron scattering profiles that vary as a function of proton polarization. Very recently, we succeeded in the first SCV neutron reflectometry measurement. We determined roughness of two surfaces of a thin-film polymer from the SCV neutron reflection curves. We will use this technique to study structures of multilayered films such as coupling agents (glues) between organic and inorganic materials.
Kumada, Takayuki
no journal, ,
Kumada, Takayuki; Akutsu, Kazuhiro*; Oishi, Kazuki*; Morikawa, Toshiaki*; Kawamura, Yukihiko*; Sahara, Masae*; Suzuki, Junichi*; Torikai, Naoya*
no journal, ,
We have developed a technique of spin contrast variation neutron reflectometry (SCV-NR). The reflectivity curve of the polarized neutrons nonsimilarly varies as a function of proton polarization PH of a polymer thin film on silicon substrate. The PH-dependent reflectivity curve determines the roughnesses of the surface and interface of the polymer thin film, whereas single reflection curve of non-polarized neutrons cannot determine uniquely. We consider that the SCV-NR would be a promising technique to determine surface and interface structure of thin films of soft materials.
Kumada, Takayuki
no journal, ,
Scattering length of thermal and cold neutrons for protons remarkably depends on relative direction of their spins. Thus, scattering pattern of polarized neutrons varies as a function of proton-polarization of target samples. Spin-contrast-variation (SCV) is a technique to determine detailed structural information of composite materials from the polarization-dependent multiple scattering curves. We started the SCV-SANS measurements in 2009 in Japan Research Reactor (JRR-3) and Japan Proton Accelerator Research Complex (J-PARC), and carried out a lot of measurements. Recently, we succeed in determining multiple surface and interface structure parameters of multi-layered systems using SCV neutron reflectometry. We are also developing SCV neutron powder diffractometry, which determines crystalline structure by distinguishing overlapped multiple peaks from the polarization-dependent peak patterns.
Kumada, Takayuki
no journal, ,
Spin contrast variation (SCV) is a technique to determine structure of complex materials from their polarized neutron scattering profiles that vary as a function of proton polarization of the sample. Now, we are planning to apply the SCV neutron scattering techniques to the high-specification hydrogen materials.
