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論文

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:1 パーセンタイル:100(Nanoscience & Nanotechnology)

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.

論文

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:4 パーセンタイル:42.19(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.

論文

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

固体高分子形燃料電池の正極には白金ナノ粒子触媒が使用されているが、加湿によって活性化過電圧が発生して性能が低下することが知られている。この原因を解明し、低減する技術を確立することが、燃料電池の性能向上とコスト低減に向けた喫緊の課題となっている。しかしながら、従来の方法で測定した白金ナノ粒子触媒のX線吸収スペクトルでは、白金の内殻正孔の寿命によるスペクトル幅の広がりで微細な構造がぼやけてしまい、吸着に起因する電子状態の変化を捉えることが困難であった。そこで本研究では、非弾性X線散乱装置を利用した高分解能型の蛍光X線吸収分光法による測定を行った。結果、酸素が水と共存することにより、白金の酸化を促進することが明瞭に検出でき、実験的に初めて明らかにすることができた。本来、触媒である白金は反応前後で不変であるべきものであるが、この反応では、白金上で酸素が水と共吸着することにより安定化して反応の進行を遅らせた結果、過電圧がより大きく生じていると解釈できる。また、白金コバルト合金ナノ粒子についても調べたところ、酸素と水の共吸着による酸化促進効果がほとんど起こらないことを見出した。

論文

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:2 パーセンタイル:9.99

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.

論文

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

AA2017-0402.pdf:0.81MB

 被引用回数:15 パーセンタイル:23.77(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.

論文

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:7 パーセンタイル:63.35(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.

論文

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:41.37

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.

論文

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:7 パーセンタイル:52.06(Materials Science, Multidisciplinary)

Fe-$$L_{3}$$吸収端での共鳴非弾性X線散乱(RIXS)を用いて、典型的な鉄系超伝導体PrFeAsO$$_{0.7}$$の単結晶で、低エネルギー電子励起スペクトルを測定した。

論文

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:0 パーセンタイル:100(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.

論文

共鳴非弾性X線散乱を用いた強相関電子系研究の進展

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.

論文

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:15 パーセンタイル:32.98(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.

論文

Engineering a spin-orbital magnetic insulator by tailoring superlattices

松野 丈夫*; 井原 康太*; 山村 周玄*; 和達 大樹*; 石井 賢司; Shankar, V.*; Kee, H.-Y.*; 高木 英典*

Physical Review Letters, 114(24), p.247209_1 - 247209_5, 2015/06

 被引用回数:102 パーセンタイル:1.99(Physics, Multidisciplinary)

In $$5d$$ Ir oxides with interplay of spin-orbit coupling and electron correlations, we have tailored a spin-orbital magnetic insulator out of a semimetal SrIrO$$_3$$ by tuning the structure through superlattices [(SrIrO$$_3$$)$$_m$$, SrTiO$$_3$$] ($$m$$ = 1, 2, 3, 4, and $$infty$$). We observed the systematic decrease of the magnetic ordering temperature and the resistivity as a function of $$m$$. The transition from the semimetal to the insulator is found to be closely linked to the appearance of magnetism at $$m$$ $$simeq$$ 3. Long range magnetic ordering was realized even in the $$m$$ = 1 single layer superlattice, implying that the design and realization of novel electronic phases is feasible at the level of a single atomic layer in complex Ir oxides.

論文

Extending resonant inelastic X-ray scattering to the extreme ultraviolet

Wray, L. A.*; Huang, S.-W.*; Jarrige, I.*; 池内 和彦*; 石井 賢司; Li, J.*; Qiu, Z. Q.*; Hussain, Z.*; Chuang, Y.-D.*

Frontiers in Physics (Internet), 3, p.32_1 - 32_11, 2015/05

 被引用回数:4

In resonant inelastic X-ray scattering (RIXS), core hole resonance modes are used to enhance coupling between photons and low energy electronic degrees of freedom. Resonating with shallow core holes accessed in the extreme ultraviolet (EUV) can provide greatly improved energy resolution at standard resolving power, but has been found to often yield qualitatively different spectra than similar measurements performed with higher energy X-rays. This paper uses experimental data and multiplet-based numerical simulations for the M-edges of Co-, Ni-, and Cu-based Mott insulators to review the properties that distinguish EUV RIXS from more commonly performed higher energy measurements. Key factors such as the origin of the strong EUV elastic line and advantages of EUV spectral functions over soft X-ray RIXS for identifying intrinsic excitation line shapes are discussed.

論文

High-energy magnetic excitations in overdoped La$$_{2-x}$$Sr$$_{x}$$CuO$$_{4}$$ studied by neutron and resonant inelastic X-ray scattering

脇本 秀一; 石井 賢司; 木村 宏之*; 藤田 全基*; Dellea, G.*; Kummer, K.*; Braicovich, L.*; Ghiringhelli, G.*; Debeer-Schmitt, L. M.*; Granroth, G.*

Physical Review B, 91(18), p.184513_1 - 184513_7, 2015/05

 被引用回数:16 パーセンタイル:30.91(Materials Science, Multidisciplinary)

We have performed neutron inelastic scattering and resonant inelastic X-ray scattering (RIXS) at the Cu-$$L_3$$ edge to study high-energy magnetic excitations at energy transfers of more than 100 meV for overdoped La$$_{2-x}$$Sr$$_{x}$$CuO$$_{4}$$ with $$x$$ = 0.25 ($$T_c$$ = 15 K) and $$x$$ = 0.30 (nonsuperconducting) using identical single-crystal samples for the two techniques. Our results indicate consistency between neutron inelastic scattering and RIXS, and elucidate the entire magnetic excitation in the $$(pi, pi)$$ direction by the complementary use of two probes. The paramagnon along $$(pi, 0)$$ agrees well with the LCO spin-wave dispersion, while the paramagnon in the $$(pi, pi)$$ direction probed by RIXS appears to be less dispersive.

論文

Kondo interactions from band reconstruction in YbInCu$$_4$$

Jarrige, I.*; 小谷 章雄*; 山岡 人志*; 辻井 直人*; 石井 賢司; Upton, M.*; Casa, D.*; Kim, J. H.*; Gog, T.*; Hancock, J. N.*

Physical Review Letters, 114(12), p.126401_1 - 126401_5, 2015/03

 被引用回数:7 パーセンタイル:41.67(Physics, Multidisciplinary)

We combine resonant inelastic X-ray scattering and model calculations in the Kondo lattice compound YbInCu$$_4$$, a system characterized by a dramatic increase in Kondo temperature and associated valence fluctuations below a first-order valence transition at T $$simeq$$ 42 K. The bulk-sensitive, element-specific, and valence-projected charge excitation spectra reveal an unusual quasigap in the Yb-derived state density which drives an instability of the electronic structure and renormalizes the low-energy effective Hamiltonian at the transition. Our results provide long-sought experimental evidence for a link between temperature-driven changes in the low-energy Kondo scale and the higher-energy electronic structure of this system.

論文

Towards optimizing the performance of self-regenerating Pt-based perovskite catalysts

Jarrige, I.*; 石井 賢司; 松村 大樹; 西畑 保雄; 吉田 雅洋*; 岸 浩史*; 谷口 昌司*; 上西 真里*; 田中 裕久*; 笠井 秀明*; et al.

ACS Catalysis, 5(2), p.1112 - 1118, 2015/02

 被引用回数:11 パーセンタイル:60.17(Chemistry, Physical)

Self-regenerating automotive catalysts owe their remarkable performance to the repeated motion of the precious metal atoms in and out of the perovskite lattice under fluctuating oxidizing and reducing conditions, preventing coalescence of the metal nanoparticles. Here we use resonant inelastic X-ray scattering to characterize the occupied and unoccupied Pt 5d states in two self-regenerating Pt-perovskite catalysts, CaTi$$_{0.95}$$Pt$$_{0.05}$$O$$_3$$ and CaZr$$_{0.95}$$Pt$$_{0.05}$$O$$_3$$. Upon reduction, the element and symmetry-specific charge excitation spectra reveal a sizeable hybridization between the Pt 5d and the Ti 3d or Zr 4d states at the interface between the nanoparticles and the perovskite, which involves the occupied states and is thus invisible in X-ray absorption spectra. A correlation is found between the strength of this d-band hybridization and the proportion of Pt nanoparticles that remain buried below the surface during reduction, indicating that the motion of the Pt atoms towards the surface is hindered by this hybridization specifically, rather than by the Pt-O bonding. These results provide direct evidence that the strength of the metal-metal d-band hybridization plays a pivotal role in determining the efficiency of self-regeneration in perovskite catalysts.

論文

電子ドープ型銅酸化物超伝導体の高エネルギー磁気励起

藤田 全基*; 石井 賢司

波紋, 25(1), p.18 - 21, 2015/02

We introduce the inelastic neutron and synchrotron X-ray scattering studies on the magnetic excitation in the electron-doped copper oxide. The recent development of state-of-the-art spectrometers at large facilities such as J-PARC enables us to study composite dynamics in the energy-momentum space arising from the interacting degrees of freedom. High-$$T_c$$ copper oxide superconductor is exotic systems, in which the spin and charge degrees of freedom are coupled. We found the elongation of spin excitation by the electron-doping, which is quite different from the negligible doping effect in the hole-doped system. Therefore, there exists the electron-hole asymmetry in the observed spin excitation against the doping.

論文

軟X線・硬X線・中性子非弾性散乱を用いた銅酸化物超伝導体のダイナミクス研究

石井 賢司; 藤田 全基*

日本結晶学会誌, 57(1), p.20 - 26, 2015/02

We combine soft X-ray, hard X-ray, and neutron inelastic scattering measurements to study both spin and charge excitations in electron-doped copper oxide superconductors. Thanks to the recent development of beam sources and related experimental techniques, accessible energy range of the these inelastic scattering measurements overlaps each other and it enables us to investigate spin and charge dynamics in the important but unexplored energy-momentum space of the cuprate superconductors. Our study demonstrates that complementary use of X-ray and neutron has become effective in inelastic scattering for studying electron dynamics of materials.

論文

3種の量子ビームを用いた電子の動きの観測

石井 賢司; 藤田 全基*

Isotope News, (728), p.10 - 13, 2014/12

非弾性散乱の分野では、SPring-8やJ-PARCといった最先端量子ビーム源の発展やそれに伴う実験技術の進歩により、これまでは困難であったより精緻な測定、より広汎な測定が可能となってきている。本稿では、これまで得られなかった全く新しい情報が得られるようになった一例として、三種の量子ビーム、軟X線,中性子,硬X線の非弾性散乱を相補的に利用することで銅酸化物高温超伝導体中の電子の動き(スピンと電荷の励起)を解明した研究について紹介する。

論文

Spin-orbit coupling induced semi-metallic state in the 1/3 hole-doped hyper-kagome Na$$_3$$Ir$$_3$$O$$_8$$

高山 知弘*; Yaresko, A.*; 松本 章代*; Nuss, J.*; 石井 賢司; 吉田 雅洋*; 水木 純一郎; 高木 英典*

Scientific Reports (Internet), 4, p.6818_1 - 6818_6, 2014/10

 被引用回数:26 パーセンタイル:15.94(Multidisciplinary Sciences)

The complex iridium oxide Na$$_3$$Ir$$_3$$O$$_8$$ with a B-site ordered spinel structure was synthesized in single crystalline form, where the chiral hyper-kagome lattice of Irions, as observed in the spin-liquid candidate Na$$_4$$Ir$$_3$$O$$_8$$, was identified. The average valence of Ir is 4.33+ and, therefore, Na$$_3$$Ir$$_3$$O$$_8$$ can be viewed as a doped analogue of the hyper-kagome spin liquid with Ir$$^{4+}$$. The transport measurements, combined with the electronic structure calculations, indicate that the ground state of Na$$_3$$Ir$$_3$$O$$_8$$ is a low carrier density semi-metal. We argue that the semi-metallic state is produced by a competition of the molecular orbital splitting of $$t_{2g}$$ orbitals on Ir$$_3$$ triangles with strong spin-orbit coupling inherent to heavy Ir ions.

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