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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

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.


Local structure study of the iron-based systems of BaFe$$_2$$As$$_2$$ and LiFeAs by X-ray PDF and XAFS analyses

Li, S.*; 豊田 真幸*; 小林 義明*; 伊藤 正行*; 池内 和彦*; 米田 安宏; 大谷 彬*; 松村 大樹; 浅野 駿*; 水木 純一郎*; et al.

Physica C, 555, p.45 - 53, 2018/12

 パーセンタイル:100(Physics, Applied)



Effect of $$B$$-site randomness on the antiferroelectric/relaxor nature of the ground state; Diffuse and inelastic X-ray scattering study of Pb(In$$_{1/2}$$Nb$$_{1/2}$$)O$$_3$$

大和田 謙二*; 塚田 慎也*; 福田 竜生; 筒井 智嗣*; Baron, A. Q. R.*; 水木 純一郎*; 大和 英弘*; 安田 直彦*; 寺内 暉*

Physical Review B, 98(5), p.054106_1 - 054106_10, 2018/08

 パーセンタイル:100(Materials Science, Multidisciplinary)

The effect of $$B$$-site randomness on the antiferroelectric/relaxor nature of the ground state was investigated by studying diffuse and inelastic X-ray scattering from ordered and disordered Pb(In$$_{1/2}$$Nb$$_{1/2}$$)O$$_3$$ (O- and D-PIN) single crystals. The diffuse scattering measurement of O-PIN (antiferroelectric at $$T<T_N$$) shows the existence of ferroelectrically interactive local polarization above $$T_N$$. Inelastic X-ray scattering shows that the transverse-acoustic (TA) and transverse-optic (TO) modes are dominant at $$Tsim$$800 K, while the central peak (CP) and TA modes are coupled and majorly contribute to the critical behavior of the diffuse scattering at $$T_N$$. Upon these results, the $$B$$-site randomness is discussed in terms of suppressing the antiferroelectric instability and enhancing the polarization fluctuation.


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:7 パーセンタイル:25.41(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.


Study of catalytic reaction at electrode-electrolyte interfaces by a CV-XAFS method

草野 翔吾*; 松村 大樹; 朝澤 浩一郎*; 岸 浩史*; 坂本 友和*; 山口 進*; 田中 裕久*; 水木 純一郎*

Journal of Electronic Materials, 46(6), p.3634 - 3638, 2017/06

 被引用回数:1 パーセンタイル:75.57(Engineering, Electrical & Electronic)

A method combining cyclic voltammetry (CV) with X-ray absorption fine structure (XAFS) spectroscopy, viz. CV-XAFS, has been developed to enable in situ real-time investigation of atomic and electronic structures related to electrochemical reactions. We use this method to study the reaction of a Pt/C cathode catalyst in the oxygen reduction reaction (ORR) in an alkaline electrolyte. It was found that the current induced by the ORR was first observed at approximately 0.08 V versus Hg/HgO, although the Pt valence remained almost unchanged. The electronic structure of the catalytic surface in the ORR was observed to be different in the negative and positive scan directions of CV measurements. Hydrogen adsorption is also discussed on the basis of the observation of this spectral change. We have demonstrated that CV-XAFS provides dynamical structural and electronic information related to electrochemical reactions and can be used for in situ real-time measurements of a catalyst.


Study on the deterioration mechanism of layered rock-salt electrodes using epitaxial thin films; Li(Ni, Co, Mn)O$$_{2}$$ and their Zr-O surface modified electrodes

阿部 真知子*; 射場 英紀*; 鈴木 耕太*; 南嶋 宏映*; 平山 雅章*; 田村 和久; 水木 純一郎*; 齋藤 智浩*; 幾原 雄一*; 菅野 了次*

Journal of Power Sources, 345, p.108 - 119, 2017/03

 パーセンタイル:100(Chemistry, Physical)

Ni, Co, Mn三元系リチウムイオン電池正極材料について、その劣化機構について、電気化学測定、X線・中性子線測定により調べた。実験の結果、Ni, Co, Mn三元系正極は、層状岩塩型構造とスピネル構造で構成されており、充放電を繰り返すと、充放電に関与しないスピネル構造が表面を覆っていくことが分かった。一方で、Zr-Oで表面をコートした材料は劣化しないことが知られており、その原因を調べた結果、層状岩塩型構造が安定に存在し続けていることが分かった。さらに、電極/溶液界面のLi濃度を上昇していることも分かった。


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

 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.


Negative correlation between electrical response and domain size in a Ti-composition-gradient Pb[(Mg$$_{1/3}$$Nb$$_{2/3}$$)$$_{1-x}$$Ti$$_{x}$$]O$$_{3}$$ crystal near the morphotropic phase boundary

清水 大輔*; 塚田 慎也*; 松浦 直人*; 坂本 潤哉*; 小島 誠治*; 並河 一道*; 水木 純一郎; 大和田 謙二

Physical Review B, 92(17), p.174121_1 - 174121_5, 2015/11

 被引用回数:4 パーセンタイル:66.91(Materials Science, Multidisciplinary)



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:11 パーセンタイル:36.72(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.


Interfacial analysis of surface-coated LiMn$$_{2}$$O$$_{4}$$ epitaxial thin film electrode for lithium batteries

鈴木 耕太*; 平山 雅章*; Kim, K.-S.*; 田港 聡*; 田村 和久; Son, J.-Y.*; 水木 純一郎; 菅野 了次*

Journal of the Electrochemical Society, 162(13), p.A7083 - A7090, 2015/08

 被引用回数:6 パーセンタイル:60.09(Electrochemistry)



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:8 パーセンタイル:61.22(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.


Mechanistic studies on lithium intercalation in a lithium-rich layered material using Li$$_{2}$$RuO$$_{3}$$ epitaxial film electrodes and ${{it in situ}}$ surface X-ray analysis

田港 聡*; 平山 雅章*; 鈴木 耕太*; Kim, K.-S.*; Zheng, Y.*; 田村 和久; 水木 純一郎; 菅野 了次*

Journal of Materials Chemistry A, 2(34), p.17875 - 17882, 2014/11

 被引用回数:15 パーセンタイル:36.26(Chemistry, Physical)



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:20 パーセンタイル:16.37(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.


Heterophase fluctuations near $$T_{rm c}$$ in the relaxor ferroelectrics (1-x)Pb(Zn$$_{1/3}$$Nb$$_{2/3}$$)O$$_{3}$$-xPbTiO$$_{3}$$ ($$x$$ = 0.09) studied by X-ray diffuse scattering and coherent X-ray scattering

大和田 謙二; 水木 純一郎*; 松下 三芳*; 並河 一道*

Physical Review B, 90(10), p.104109_1 - 104109_12, 2014/09

 被引用回数:4 パーセンタイル:70.33(Materials Science, Multidisciplinary)



High-energy spin and charge excitations in electron-doped copper oxide superconductors

石井 賢司; 藤田 全基*; 佐々木 隆了*; Minola, M.*; Dellea, G.*; Mazzoli, C.*; Kummer, K.*; Ghiringhelli, G.*; Braicovich, L.*; 遠山 貴己*; et al.

Nature Communications (Internet), 5, p.3714_1 - 3714_8, 2014/04

 被引用回数:54 パーセンタイル:4.57(Multidisciplinary Sciences)

We combine X-ray and neutron inelastic scattering measurements to track the doping dependence of both spin and charge excitations in electron-doped materials. Copper $$L_3$$ resonant inelastic X-ray scattering spectra show that magnetic excitations shift to higher energy upon doping. Their dispersion becomes steeper near the magnetic zone center and they deeply mix with charge excitations, indicating that electrons acquire a highly itinerant character in the doped metallic state. Moreover, above the magnetic excitations, an additional dispersing feature is observed near the $$Gamma$$-point, and we ascribe it to particle-hole charge excitations. These properties are in stark contrast with the more localized spin-excitations (paramagnons) recently observed in hole-doped compounds even at high doping-levels.


Bipartite magnetic parent phases in the iron oxypnictide superconductor

平石 雅俊*; 飯村 壮史*; 小嶋 健児*; 山浦 淳一*; 平賀 晴弘*; 池田 一貴*; Miao, P.*; 石川 喜久*; 鳥居 周輝*; 宮崎 正範*; et al.

Nature Physics, 10(4), p.300 - 303, 2014/04

 被引用回数:62 パーセンタイル:3.79(Physics, Multidisciplinary)

High-temperature (high-$$T_{rm c}$$) superconductivity appears as a consequence of the carrier-doping of an undoped parent compound exhibiting antiferromagnetic order; thereby, ground-state properties of the parent compound are closely relevant to the superconducting state. On the basis of the concept, a spin-fluctuation has been addressed as an origin of pairing of the superconducting electrons in cuprates. Whereas, there is growing interest in the pairing mechanism such as an unconventional spin-fluctuation or an advanced orbital-fluctuation due to the characteristic multi-orbital system in iron-pnictides. Here, we report the discovery of an antiferromagnetic order as well as a unique structural transition in electron-overdoped LaFeAsO$$_{1-x}$$H$$_x$$ ($$x sim 0.5$$), whereby another parent phase was uncovered, albeit heavily doped. The unprecedented two-dome superconducting phases observed in this material can be interpreted as a consequence of the carrier-doping starting from the original at $$x sim 0$$ and advanced at $$x sim 0.5$$ parent phases toward the intermediate region. The bipartite parent phases with distinct physical properties in the second magnetic phase provide us with an interesting example to illustrate the intimate interplay among the magnetic interaction, structural change and orbital degree of freedom in iron-pnictides.


Momentum-resolved resonant inelastic X-ray scattering on a single crystal under high pressure

吉田 雅洋*; 石井 賢司; Jarrige, I.*; 綿貫 徹; 工藤 一貴*; 小池 洋二*; 熊谷 健一*; 平岡 望*; 石井 啓文*; Tsuei, K.-D.*; et al.

Journal of Synchrotron Radiation, 21(1), p.131 - 135, 2014/01

 被引用回数:2 パーセンタイル:79.6(Instruments & Instrumentation)

A single-crystal momentum-resolved resonant inelastic X-ray scattering (RIXS) experiment under high pressure using an originally designed diamond anvil cell (DAC) is reported. The diamond-in/diamond-out geometry was adopted with both the incident and scattered beams passing through a 1 mm-thick diamond. This enabled us to cover wide momentum space keeping the scattering angle condition near 90$$^{circ}$$. Elastic and inelastic scattering from the diamond was drastically reduced using a pinhole placed after the DAC. Measurement of the momentum-resolved RIXS spectra of Sr$$_{2.5}$$Ca$$_{11.5}$$Cu$$_{24}$$O$$_{41}$$ at the Cu $$K$$-edge was thus successful. Though the inelastic intensity becomes weaker by two orders than the ambient pressure, RIXS spectra both at the center and the edge of the Brillouin zone were obtained at 3 GPa and low-energy electronic excitations of the cuprate were found to change with pressure.


Instrumental upgrades of the RIXS spectrometer at BL11XU at SPring-8

石井 賢司; Jarrige, I.*; 吉田 雅洋*; 池内 和彦*; 稲見 俊哉; 村上 洋一*; 水木 純一郎

Journal of Electron Spectroscopy and Related Phenomena, 188, p.127 - 132, 2013/06

 被引用回数:8 パーセンタイル:41.65(Spectroscopy)

Two recent instrumental upgrades of the inelastic X-ray scattering spectrometer installed at BL11XU at SPring-8 are reported. The first one is a multianalyzer system, where we can simultaneously use three crystal analyzers aligned perpendicularly to the scattering plane. In a test measurement of polycrystalline $$alpha$$-PtO$$_2$$, the inelastic spectra obtained with each respective analyzer showed a completely identical lineshape, and a slight difference ($$le$$ 10%) in intensity. The system enhances the experimental efficiency, and allows for simultaneous scan at three momenta for a single-crystal sample. The second development is a polarization analyzer for the scattered photons. A pyrolytic graphite (PG) crystal is placed in front of the detector and serves as a polarization-analyzer crystal, using the (006) reflection for the Cu $$K$$-edge. We succeeded to observe clear polarization dependence in the $$d$$-$$d$$ excitations of KCuF$$_3$$.


200 Hz observation of hydrogenation reaction of Pd nanoparticles by using dispersive XAFS optics

松村 大樹; 岡島 由佳*; 西畑 保雄; 水木 純一郎

Journal of Physics; Conference Series, 430, p.012024_1 - 012024_6, 2013/04

 被引用回数:3 パーセンタイル:21.36

Palladium is well known to show high performance for the hydrogen storage materials. We have observed the X-ray absorption fine structure (XAFS) spectra with dispersive optics in order to understand the size effect of the Pd particles concerning the hydrogen storage process. XAFS spectra were observed at BL14B1 of SPring-8 by dispersive mode. Pd-Pd interatomic distance was expanded by about 0.1 ${AA}$ due to the hydrogen absorption reaction at room temperature. We also observed increase of Debye-Waller factor while hydrogen absorption reaction proceeds.


Resonant inelastic X-ray scattering study of intraband charge excitations in hole-doped high-$$T_c$$ cuprates

脇本 秀一; 石井 賢司; 木村 宏之*; 池内 和彦*; 吉田 雅洋*; 足立 匡*; Casa, D.*; 藤田 全基*; 福永 靖*; Gog, T.*; et al.

Physical Review B, 87(10), p.104511_1 - 104511_7, 2013/03

 被引用回数:6 パーセンタイル:59.45(Materials Science, Multidisciplinary)

We have performed resonant inelastic X-ray scattering (RIXS) near the Cu-$$K$$ edge on various cuprate superconductors, covering underdoped to heavily overdoped regimes and focusing on charge excitations inside the charge-transfer gap. RIXS measurements with $$E_i$$= 9.003 keV on metallic La$$_{1.7}$$Sr$$_{0.3}$$CuO$$_{4}$$ and Bi$$_{1.76}$$Pb$$_{0.35}$$Sr$$_{1.89}$$CuO$$_{6+delta}$$ exhibit a dispersive intraband excitation below 4 eV, similar to that observed in the electron-doped Nd$$_{1.85}$$Ce$$_{0.15}$$CuO$$_{4}$$. This is the first observation of a dispersive intraband excitation in a hole-doped system, evidencing that both electron- and hole-doped systems have a similar dynamical charge correlation function.

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