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Investigation of hydrogen superoxide adsorption during ORR on Pt/C catalyst in acidic solution for PEFC by ${it in-situ}$ high energy resolution XAFS

山本 直生*; 松村 大樹; 萩原 悠人*; 田中 啓偉*; 長谷川 優太*; 石井 賢司*; 田中 裕久*

Journal of Power Sources, 557, p.232508_1 - 232508_10, 2023/02

Oxygen Reduction Reaction (ORR) is one of the key electrochemical reactions, especially in Polymer Electrolyte Fuel Cells (PEFCs). In this work, the reaction pathway and intermediate species such as molecular-type oxygen during ORR were discussed. High energy resolution X-ray absorption fine structure spectra at the Pt L$$_{3}$$-edge were obtained to observe the electronic structure of Pt catalyst. Carbon-supported Pt nanoparticles as powder catalysts were used for measurement as more realistic conditions, and the species adsorbed on the Pt nanoparticles were analyzed while controlling under the potentials in acidic electrolyte solution with N$$_{2}$$ or O$$_{2}$$ gas bubbling. Molecular-type oxygen adsorption species is observed only in the O$$_{2}$$-bubbled electrolyte solution. This intermediate adsorption species is assigned to a hydrogen superoxide.


Distinct variation of electronic states due to annealing in $$T'$$-type La$$_{1.8}$$Eu$$_{0.2}$$CuO$$_{4}$$ and Nd$$_{2}$$CuO$$_{4}$$

浅野 駿*; 石井 賢司*; 松村 大樹; 辻 卓也; 工藤 康太*; 谷口 貴紀*; 齋藤 真*; 春原 稔樹*; 川股 隆行*; 小池 洋二*; et al.

Physical Review B, 104(21), p.214504_1 - 214504_7, 2021/12

 被引用回数:0 パーセンタイル:0(Materials Science, Multidisciplinary)

We performed Cu K-edge X-ray absorption fine-structure measurements on $$T'$$-type La$$_{1.8}$$Eu$$_{0.2}$$CuO$$_{4}$$ (LECO) and Nd$$_{2}$$CuO$$_{4}$$ (NCO) to investigate the variation in the electronic state associated with the emergence of superconductivity due to annealing. The X-ray absorption near-edge structure spectra of as-sintered (AS) LECO are quite similar to those of AS NCO, indicating that the ground state of AS LECO is a Mott insulator. The electron density after annealing $$n_{rm AN}$$ was evaluated for both superconducting LECO and nonsuperconducting NCO and was found to be 0.40 and 0.05 electron per Cu atom, respectively. In LECO but not in NCO, extended X-ray absorption fine-structure analysis revealed a reduction in the strength of the Cu-O bond in the CuO$$_{2}$$ plane due to annealing, which is consistent with the screening effect on phonons in the metallic state. The origin of the difference in doping processes due to annealing is discussed in relation to the size of the charge-transfer gap.


Feasibility study of magnetic-domain observation by means of non-resonant magnetic X-ray diffraction

稲見 俊哉*; 菖蒲 敬久; 石井 賢司*

IEEE Transactions on Magnetics, 57(3, Part2), p.6400105_1 - 6400105_5, 2021/03

 被引用回数:0 パーセンタイル:0(Engineering, Electrical & Electronic)

Although the observation of magnetic domains well below the surface of a sample appears to be relatively easy, in reality, magnetic domains inside metallic samples have not been investigated in detail due to a lack of adequate techniques. Non-resonant magnetic X-ray diffraction (NRMXRD) is a candidate for such 3-D magnetic microscopy. A relatively small focus size of less than 100 nm and a relatively long attenuation length of more than 100 $$mu$$m can be obtained by using high-energy synchrotron X-rays. However, NRMXRD has a disadvantage in that the magnetic contrast is low. It is known that the magnetic contrast in NRMXRD increases with increasing the total polarization of the incident X-rays. In this feasibility study, we carried out NRMXRD experiments on a metallic iron sample to examine whether the magnetic contrast can be sufficiently enhanced even for high-energy X-rays.



松原 章浩*; 藤田 奈津子; 石井 邦和*; 木村 健二*

放射線(インターネット), 45(3), p.134 - 138, 2020/04



幌延深地層研究計画における地下施設での調査研究段階; (第3段階: 必須の課題2015-2019年度)研究成果報告書

中山 雅; 雑賀 敦; 木村 駿; 望月 陽人; 青柳 和平; 大野 宏和; 宮川 和也; 武田 匡樹; 早野 明; 松岡 稔幸; et al.

JAEA-Research 2019-013, 276 Pages, 2020/03




Electrochemical adsorption on Pt nanoparticles in alkaline solution observed using in situ high energy resolution X-ray absorption spectroscopy

草野 翔吾*; 松村 大樹; 石井 賢司*; 田中 裕久*; 水木 純一郎*

Nanomaterials (Internet), 9(4), p.642_1 - 642_14, 2019/04

 被引用回数:4 パーセンタイル:27.5(Chemistry, Multidisciplinary)

The oxygen reduction reaction (ORR) on Pt/C in alkaline solution was studied by in situ high energy resolution X-ray absorption spectroscopy. To discuss the X-ray absorption near-edge structure (XANES), this paper introduced the rate of change of the $$Delta mu$$ (RCD), which is an analysis method that is sensitive to surface adsorption. The surface adsorptions as hydrogen (below 0.34 V), superoxide anion (from 0.34 V to 0.74 V), hydroxyl species (from 0.44 V to 0.74 V), atomic oxygen (above 0.74 V), and $$alpha$$-PtO$$_{2}$$ (above 0.94 V) were distinguished. It is clarified that the catalytic activity in an alkaline solution is enhanced by the stability of atomic oxygen and the low stability of superoxide anion/peroxide adsorption on the platinum surface.


Numerical evaluation on fluctuation absorption characteristics based on nuclear heat supply fluctuation test using HTTR

高田 昌二; 本多 友貴*; 稲葉 良知; 関田 健司; 根本 隆弘; 栃尾 大輔; 石井 俊晃; 佐藤 博之; 中川 繁昭; 沢 和弘*

Proceedings of 9th International Topical Meeting on High Temperature Reactor Technology (HTR 2018) (USB Flash Drive), 7 Pages, 2018/10



Ce substitution and reduction annealing effects on electronic states in Pr$$_{2-x}$$Ce$$_x$$CuO$$_4$$ studied by Cu $$K$$-edge X-ray absorption spectroscopy

浅野 駿*; 石井 賢司*; 松村 大樹; 辻 卓也; 伊奈 稔哲*; 鈴木 謙介*; 藤田 全基*

Journal of the Physical Society of Japan, 87(9), p.094710_1 - 094710_5, 2018/09

 被引用回数:11 パーセンタイル:66.62(Physics, Multidisciplinary)

We investigated the Ce substitution and reduction annealing effects on the electronic states at copper sites by Cu $$K$$-edge X-ray absorption near-edge structure measurements in Pr$$_{2-x}$$Ce$$_x$$CuO$$_{4+alpha-delta}$$ (PCCO) with varying $$x$$ and $$delta$$ (amount of oxygen loss during annealing). Absorption near-edge spectra were modified by Ce substitution and reduction annealing similarly with increasing $$x$$ and $$delta$$. Considering electron doping by Ce substitution, this similarity indicates an increase in electron number at the copper sites due to annealing ($$n_{AN}$$). Furthermore, quantitative analyses of the spectra clarified that the number of Cu$$^+$$ sites, corresponding to the induced electron number by Ce substitution increases linearly with $$x$$ in the as-sintered PCCO, whereas $$n_{AN}$$ is not exactly equal to 2$$delta$$. For each $$x$$-fixed sample, $$n_{AN}$$tends to exceed 2$$delta$$ with increasing $$delta$$, suggesting the emergence of two types of carrier due to annealing.


Pt, PtCo触媒表面の酸素吸着に及ぼす水の影響

Cui, Y.-T.*; 原田 慈久*; 丹羽 秀治*; 尾嶋 正治*; 畑中 達也*; 中村 直樹*; 安藤 雅樹*; 吉田 利彦*; 石井 賢司*; 松村 大樹

NanotechJapan Bulletin (インターネット), 11(4), 6 Pages, 2018/08



Reduction and oxidation annealing effects on Cu $$K$$-edge XAFS for electron-doped cuprate superconductors

浅野 駿*; 鈴木 謙介*; 松村 大樹; 石井 賢司*; 伊奈 稔哲*; 藤田 全基*

Journal of Physics; Conference Series, 969, p.012051_1 - 012051_5, 2018/04

 被引用回数:3 パーセンタイル:85.12

Reduction and oxidation annealing effects on the electronic states around the copper sites for Pr$$_{2-x}$$Ce$$_x$$CuO$$_4$$ and Nd$$_{2-x}$$Ce$$_x$$CuO$$_4$$ with $$x$$ = 0 and $$x$$ = 0.15 were investigated by Cu $$K$$-edge X-ray absorption measurements. Cu $$K$$ near-edge spectra were changed by the reduction annealing in a manner similar to the case of Ce substitution for both $$x$$ = 0 and $$x$$ = 0.15. This means an increase of electron density at the copper sites, indicating the aspect of electron doping in the reduction annealing. This reduction annealing effect on the near-edge spectra are reverted by the additional oxidation annealing. The amount of electron density around the copper sites is varied by the reduction and oxidation annealing, reversibly, corresponding to the reversible variation of the physical property from insulating to superconductivity.


Observation of momentum-dependent charge excitations in hole-doped cuprates using resonant inelastic X-ray scattering at the oxygen $$K$$ edge

石井 賢司*; 遠山 貴巳*; 浅野 駿*; 佐藤 研太朗*; 藤田 全基*; 脇本 秀一; 筒井 健二*; 曽田 繁利*; 宮脇 淳*; 丹羽 秀治*; et al.

Physical Review B, 96(11), p.115148_1 - 115148_8, 2017/09


 被引用回数:25 パーセンタイル:76.53(Materials Science, Multidisciplinary)

We investigate electronic excitations in La$$_{2-x}$$(Br,Sr)$$_x$$CuO$$_4$$ using resonant inelastic X-ray scattering (RIXS) at the oxygen $$K$$ edge. We observed momentum-dependent spectral weight below 1 eV, which is consistent with theoretical calculation of the dynamical charge structure factor on oxygen orbitals in a three-band Hubbard model. Our results confirm that the momentum-dependent charge excitations exist on the order of the transfer energy ($$t$$), and the broad spectral line shape indicates damped and incoherent character of the charge excitations at the energy range in the doped Mott insulators.


Wetting induced oxidation of Pt-based nano catalysts revealed by ${{it in situ}}$ high energy resolution X-ray absorption spectroscopy

Cui, Y.-T.*; 原田 慈久*; 丹羽 秀治*; 畑中 達也*; 中村 直樹*; 安藤 雅樹*; 吉田 稔彦*; 石井 賢司*; 松村 大樹; 陰地 宏*; et al.

Scientific Reports (Internet), 7(1), p.1482_1 - 1482_8, 2017/05

 被引用回数:15 パーセンタイル:45.81(Multidisciplinary Sciences)

In situ high energy resolution fluorescence detection X-ray absorption spectroscopy (HERFD-XAS) was used to systematically evaluate interactions of H$$_{2}$$O and O$$_{2}$$ adsorbed on Pt and Pt$$_{3}$$Co nanoparticle catalysts in different particle sizes. The systematic increase in oxidation due to adsorption of different species (H$$_{2}$$O adsorption $$<$$ O$$_{2}$$ adsorption $$<$$ O$$_{2}$$ + H$$_{2}$$O coadsorption) suggests that cooperative behavior between O$$_{2}$$ and H$$_{2}$$O adsorptions is responsible for the overpotential induced by hydrated species in fuel cells. From the alloying and particle size effects, it is found that both strength of O$$_{2}$$/H$$_{2}$$O adsorption and their cooperative effect upon coadsorption are responsible for the specific activity of Pt catalysts.


Absence of a polar phase in perovskite chromite $$R$$CrO$$_{3}$$ ($$R$$=La and Pr)

吉井 賢資; 池田 直*; 下条 豊; 石井 慶信*

Materials Chemistry and Physics, 190, p.96 - 101, 2017/04

 被引用回数:15 パーセンタイル:53.17(Materials Science, Multidisciplinary)

ペロブスカイト構造を持つクロム酸化物LaCrO$$_{3}$$, PrCrO$$_{3}$$およびLa$$_{0.5}$$Pr$$_{0.5}$$CrO$$_{3}$$の磁性と誘電性について調べた。これら酸化物は、近年、磁性と誘電性が重畳したマルチフェロイックであると報告されている$${it R}$$CrO$$_{3}$$系($${it R}$$:希土類)に属するため、対称系もマルチフェロイックであるとすれば興味深い。磁化測定からは、対象系はネール温度が240-288 Kの反強磁性体であることを観測した。中性子回折測定からは、これらの結晶構造は中心対称性を持つ斜方晶$${it Pnma}$$であり、NdCrO$$_{3}$$で報告された単斜晶構造とは異っており、強誘電体にはならないことを観測した。この結果と誘電率測定から、対象系の10000ほどの大きな誘電率は、電気双極子ではなく電荷の移動によるものと結論した。



佐藤 稔紀; 笹本 広; 石井 英一; 松岡 稔幸; 早野 明; 宮川 和也; 藤田 朝雄*; 棚井 憲治; 中山 雅; 武田 匡樹; et al.

JAEA-Research 2016-025, 313 Pages, 2017/03




Electronic structure of Pt and Pt-Co nanoparticles with O$$_{2}$$ and O$$_{2}$$/H$$_{2}$$O adsorption revealed by in situ XAFS and hard X-ray photoelectron spectroscopy

Cui, Y.*; 原田 慈久*; 畑中 達也*; 中村 直樹*; 安藤 雅樹*; 吉田 稔彦*; 池永 英司*; 石井 賢司*; 松村 大樹; Li, R.*; et al.

ECS Transactions, 72(8), p.131 - 136, 2016/10

 被引用回数:1 パーセンタイル:50.82

The electronic structures of Pt and Pt-Co nanoparticles with O$$_{2}$$ adsorption and O$$_{2}$$/H$$_{2}$$O co-adsorption were investigated by in situ hard X-ray photoelectron spectroscopy (HAXPES) and in situ high resolution fluorescence detection X-ray absorption spectroscopy (HERFD-XAS) to clarify the effects of water adsorption on fuel cell cathode catalysis surface. The experimental results suggest that under the pressure of 1 mbar, the adsorption of H$$_{2}$$O hinders the successive O$$_{2}$$ adsorption on Pt surface, while under the pressure of 1 bar, the adsorption of H$$_{2}$$O enhances the adsorption of O$$_{2}$$ on Pt surface. This water effect is found to be more significant on Pt surface than on Pt-Co surface. These results would be helpful to understand how the water affects the fuel cell performance and why Pt-Co nanoparticles show higher oxygen reduce reaction (ORR) activity than Pt nanoparticles.


Resonant inelastic X-ray scattering study of entangled spin-orbital excitations in superconducting PrFeAsO$$_{0.7}$$

野村 拓司*; 原田 慈久*; 丹羽 秀治*; 石井 賢司*; 石角 元志*; 社本 真一; Jarrige, I.*

Physical Review B, 94(3), p.035134_1 - 035134_9, 2016/07

 被引用回数:10 パーセンタイル:47.31(Materials Science, Multidisciplinary)



Observation of momentum-resolved charge fluctuations proximate to the charge-order phase using resonant inelastic X-ray scattering

吉田 雅洋*; 石井 賢司; 中 惇*; 石原 純夫*; Jarrige, I.*; 池内 和彦*; 村上 洋一*; 工藤 一貴*; 小池 洋二*; 永田 知子*; et al.

Scientific Reports (Internet), 6, p.23611_1 - 23611_8, 2016/03

 被引用回数:1 パーセンタイル:12.34(Multidisciplinary Sciences)

In strongly correlated electron systems, enhanced fluctuations in the proximity of the ordered states of electronic degrees of freedom often induce anomalous electronic properties such as unconventional superconductivity. While spin fluctuations in the energy-momentum space have been studied widely using inelastic neutron scattering, other degrees of freedom, i.e., charge and orbital, have hardly been explored thus far. Here, we use resonant inelastic X-ray scattering to observe charge fluctuations proximate to the charge-order phase in transition metal oxides. In the two-leg ladder of Sr$$_{14-x}$$Ca$$_x$$Cu$$_{24}$$O$$_{41}$$, charge fluctuations are enhanced at the propagation vector of the charge order ($$mathbf{q}_mathrm{CO}$$) when the order is melted by raising the temperature or by doping holes. In contrast, charge fluctuations are observed not only at $$mathbf{q}_mathrm{CO}$$ but also at other momenta in a geometrically frustrated triangular bilayer lattice of LuFe$$_2$$O$$_4$$. The observed charge fluctuations have a high energy ($$sim$$ 1 eV), suggesting that the Coulomb repulsion between electrons plays an important role in the formation of the charge order.



石井 賢司

固体物理, 51(2), p.79 - 92, 2016/02

In the last decade, resonant inelastic X-ray scattering for the study of electronic excitations in strongly correlated electron systems has achieved significant progress utilizing brilliant synchrotron radiation X-rays. Some representative studies on cuprates and iridates are reviewed.


Clay-based modeling approach to diffusion and sorption in the argillaceous rock from the Horonobe URL; Application to Ni(II), Am(III), and Se(IV)

舘 幸男; 陶山 忠宏; 四辻 健治; 石井 康雄; 高橋 宏明*

CMS Workshop Lectures, Vol.21, p.241 - 250, 2016/00

放射性廃棄物地層処分の安全評価において粘土質岩石中の核種の収着・拡散挙動は把握すべき重要なプロセスである。幌延深地層研究所における泥岩試料中のNi(II), Am(III), Se(IV)の拡散・収着挙動を、実験とモデルの両面から調査した。透過拡散試験によって得られた実効拡散係数は、先行研究の結果も含めて、Cs$$^{+}$$, Ni$$^{2+}$$, HTO, I$$^{-}$$, Se(SeO$$_{4}$$$$^{2-}$$), Am(Am(CO$$_{3}$$)$$^{2-}$$)の順に低下する傾向となった。一方で、拡散試験から得られた収着分配係数は、バッチ収着試験によって取得された値との整合的であった。これらの結果は、粘土成分(スメクタイトとイライト)の寄与を仮定した収着モデル、電気二重層理論と単純化された間隙モデルを考慮した拡散モデルとを組み合せた、粘土を主体としたモデル化手法によって解釈された。この粘土を主体としたモデルによって、一連のデータを概ね説明することが可能であり、この手法が多様な核種に対して適用可能と評価された。


Large trigonal-field effect on spin-orbit coupled states in a pyrochlore iridate

植松 大介*; 佐賀山 基*; 有馬 孝尚*; 石川 洵*; 中辻 知*; 高木 英典*; 吉田 雅洋*; 水木 純一郎; 石井 賢司

Physical Review B, 92(9), p.094405_1 - 094405_6, 2015/09

 被引用回数:21 パーセンタイル:68.04(Materials Science, Multidisciplinary)

The half-filled topmost valence band of Ir$$^{4+}$$ in several iridates such as Sr$$_2$$IrO$$_4$$, IrO$$_2$$, and CaIrO$$_3$$ has been proposed to originate mainly from the spin-orbit coupled $$J_{rm eff}=1/2$$ states. In pyrochlore iridates $$R_2$$Ir$$_2$$O$$_7$$ ($$R$$: rare earth), some exotic electronic states are theoretically proposed by assuming $$J_{rm eff}=1/2$$ states. However, the octahedral coordination around Ir is trigonally distorted, which may affect the energy level scheme of Ir $$5d$$ states. Here, we report spectra of resonant elastic and inelastic X-ray scattering in Eu$$_2$$Ir$$_2$$O$$_7$$ at the Ir $$L$$ edges. A large suppression of the magnetic scattering signal at the Ir $$L_{rm II}$$ edge supports the $$J_{rm eff}=1/2$$ picture rather than the $$S=1/2$$ one. The inelastic scattering spectrum indicates that the magnitude of the trigonal field on the Ir$$^{4+}$$ states is evaluated to be comparable to the spin-orbit interaction. The energy diagram of the $$5d$$ state is proposed based on the simple cluster model.

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