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2017 Fiscal Year Annual Research Report

Chemical State Visualization of FeOx Catalyst Particles by In Situ Full-Field Imaging XAFS

Research Project

Project/Area Number 16K17863
Research InstitutionInstitute of Physical and Chemical Research

Principal Investigator

石黒 志  国立研究開発法人理化学研究所, 放射光科学総合研究センター, 特別研究員 (20752455)

Project Period (FY) 2016-04-01 – 2018-03-31
Keywords固体触媒 / 結像顕微XAFS法 / タイコグラフィーXAFS法 / 化学状態可視化
Outline of Annual Research Achievements

固体触媒粒子内形状・構造の不均一性が触媒作用に及ぼす要因を明らかにするために、固体触媒粒子の空間分解イメージングXAFS 法による化学状態分布の可視化を行った。平成29年度は、(i)結像顕微XAFS法による樹状型FeOx及びFeCrOx粒子内のFe化学状態の可視化と、(ii)タイコグラフィーXAFS法による酸素貯蔵材料Pt/Ce2Zr2Ox(x=7-8)粒子内の酸素拡散の可視化の実験・解析を実施した。
(i)水熱合成により調製し水素還元処理を行った樹状型FeOxとFeCrOxをそれぞれ423 Kから673 Kの異なる温度で酸化処理を行った。各条件での樹状型FeOx及びFeCrOx粒子のFeK端結像顕微XAFS計測をSPring-8 BL37XUおよびBL32B2ビームラインで行い、得られた空間分解XANESスペクトルからα-Fe2O3/γ-Fe2O3/Fe3O4の相比率の空間分布を検討し各粒子の反応相変化傾向を調べた。
(ii)完全酸化処理を行ったPt/Ce2Zr2O8 (A), 完全還元処理を行ったPt/Ce2Zr2O7 (B), 部分酸化処理行ったPt/Ce2Zr2O7.6 (C)の3種類の粒子分散試料を用意し、SPring-8 BL29LXUにてタイコグラフィーXAFS計測を行った。ピクセル分解能は13 nm, 空間分解能50 nm以下のCe L3端2次元空間分解XAFSスペクトルを得て、その解析からCe密度とCe価数についての化学状態マッピングイメージが得られた。特に(C)ではCeの価数が粒子内で広い分布を持っており、化学状態イメージングデータを 65 nm大のドメインに分割し、ドメイン内の局所的なCe価数とCe密度の相関性を調べると、ドメイン毎に複数のタイプに分けられることがわかり、粒子内で複数の格子酸素拡散パスが存在することを可視化することに成功した。

  • Research Products

    (36 results)

All 2018 2017 Other

All Journal Article (7 results) (of which Int'l Joint Research: 1 results,  Peer Reviewed: 7 results,  Open Access: 1 results) Presentation (28 results) (of which Int'l Joint Research: 13 results,  Invited: 2 results) Remarks (1 results)

  • [Journal Article] Visualization of Heterogeneous Oxygen Storage Behavior in Platinum-Supported Cerium-Zirconium Oxide Three-Way Catalyst Particles by Hard X-ray Spectro-Ptychography2018

    • Author(s)
      Hirose Makoto、Ishiguro Nozomu、Shimomura Kei、Burdet Nicolas、Matsui Hirosuke、Tada Mizuki、Takahashi Yukio
    • Journal Title

      Angewandte Chemie International Edition

      Volume: 57 Pages: 1474~1479

    • DOI

      10.1002/anie.201710798

    • Peer Reviewed
  • [Journal Article] Structural investigations of La0.6Sr0.4FeO3-δ under reducing conditions: kinetic and thermodynamic limitations for phase transformations and iron exsolution phenomena2018

    • Author(s)
      Gotsch Thomas、Schlicker Lukas、Bekheet Maged F.、Doran Andrew、Grunbacher Matthias、Praty Corsin、Tada Mizuki、Matsui Hirosuke、Ishiguro Nozomu、Gurlo Aleksander、Klotzer Bernhard、Penner Simon
    • Journal Title

      RSC Advances

      Volume: 8 Pages: 3120~3131

    • DOI

      10.1039/c7ra12309d

    • Peer Reviewed / Open Access / Int'l Joint Research
  • [Journal Article] Structural Kinetics of Cathode Events on Polymer Electrolyte Fuel Cell Catalysts Studied by Operando Time-Resolved XAFS2018

    • Author(s)
      Ishiguro Nozomu、Tada Mizuki
    • Journal Title

      Catalysis Letters

      Volume: 印刷中 Pages: 印刷中

    • DOI

      10.1007/s10562-018-2383-7

    • Peer Reviewed
  • [Journal Article] Operando 3D Visualization of Migration and Degradation of a Platinum Cathode Catalyst in a Polymer Electrolyte Fuel Cell2017

    • Author(s)
      Matsui Hirosuke、Ishiguro Nozomu、Uruga Tomoya、Sekizawa Oki、Higashi Kotaro、Maejima Naoyuki、Tada Mizuki
    • Journal Title

      Angewandte Chemie International Edition

      Volume: 56 Pages: 9371~9375

    • DOI

      10.1002/anie.201703940

    • Peer Reviewed
  • [Journal Article] In-situ X-ray nano-CT System for Polymer Electrolyte Fuel Cells under Operating Conditions2017

    • Author(s)
      Sekizawa O、Uruga T、Ishiguro N、Matsui H、Higashi K、Sakata T、Iwasawa Y、Tada M
    • Journal Title

      Journal of Physics: Conference Series

      Volume: 849 Pages: 012022~012022

    • DOI

      10.1088/1742-6596/849/1/012022

    • Peer Reviewed
  • [Journal Article] Size Regulation and Stability Enhancement of Pt Nanoparticle Catalyst via Polypyrrole Functionalization of Carbon-Nanotube-Supported Pt Tetranuclear Complex2017

    • Author(s)
      Muratsugu Satoshi、Miyamoto Shota、Sakamoto Kana、Ichihashi Kentaro、Kim Chang Kyu、Ishiguro Nozomu、Tada Mizuki
    • Journal Title

      Langmuir

      Volume: 33 Pages: 10271~10282

    • DOI

      10.1021/acs.langmuir.7b02114

    • Peer Reviewed
  • [Journal Article] 走査型顕微XAFS法を用いた固体粒子のイメージング2017

    • Author(s)
      石黒志、松井公佑、唯美津木
    • Journal Title

      触媒

      Volume: 59(2) Pages: 69~75

    • Peer Reviewed
  • [Presentation] 結像顕微XAFSによる樹状型FeOx粒子の酸化還元サイクルおけるFe化学状態の可視化2018

    • Author(s)
      石黒 志, 松井 公佑, 鈴木 陽也, 関澤 央輝, 新田 清文, 寺田 靖子, 宇留賀 朋哉, 唯 美津木
    • Organizer
      第31回日本放射光学会年会・放射光科学合同シンポジウム
  • [Presentation] タイコグラフィXAFSによるCe2Zr2Ox粒子内の酸素拡散分布の可視化2018

    • Author(s)
      石黒 志, 広瀬 真, 下村 啓, Nicolas BURDET, 松井公佑, 高橋幸生, 唯美津木
    • Organizer
      日本化学会第98春季年会
  • [Presentation] Visualization of Ce Chemical States and Oxygen Diffusion in Ceria-Zirconia Particles by X-ray Spectro-Ptychography2018

    • Author(s)
      Nozomu Ishiguro, Makoto Hirose, Kei Shimomura, Nicolas Burdet, Hirosuke Matsui, Yukio Takahashi, Mizuki Tada
    • Organizer
      18th International Symposium on Relations between Homogeneous and Heterogeneous Catalysts (ISHHC18)
    • Int'l Joint Research
  • [Presentation] XAFS Imaging of Ce2Zr2Ox Exhausting Catalyst Systems2018

    • Author(s)
      Nozomu Ishiguro, Makoto Hirose, Hirosuke Matsui, Mizuki Tada
    • Organizer
      International Symposium on Advancement and Prospect of Catalysis Science & Technology
    • Int'l Joint Research / Invited
  • [Presentation] Nanoscale Chemical Imaging of Three-Way Catalyst Pt/Ce2Zr2Ox Particles by Ptychographic-XAFS2018

    • Author(s)
      Makoto Hirose, Nozomu Ishiguro, Kei Shimomura, Hirosuke Matsui, Mizuki Tada, Yukio Takahashi
    • Organizer
      The 14th International Conference on X-ray Microscopy (XRM2018)
    • Int'l Joint Research
  • [Presentation] オペランドCT-XAFS法による固体高分子形燃料電池の触媒劣化・溶出様式の3次元可視化2018

    • Author(s)
      松井公佑、石黒志、宇留賀朋哉、関澤央輝、唯美津木
    • Organizer
      第31回日本放射光学会年会・放射光科学合同シンポジウム
  • [Presentation] オペランド時間分解XAFS法によるPEFC実発電下におけるPtカソード触媒の酸化反応の速度論解析2018

    • Author(s)
      小澤沙記、松井公佑、石黒志、宇留賀朋哉、関澤央輝、坂田智裕、東晃太朗、唯美津木
    • Organizer
      第31回日本放射光学会年会・放射光科学合同シンポジウム
  • [Presentation] 3D-multiple elemental visualization of PEFC Pt3Co/C cathode catalyst during accelerated degradation test2018

    • Author(s)
      Y. Tan, H. Matsui, N. Ishiguro, T. Uruga, O. Sekizawa, N. Maejima, Mizuki Tada
    • Organizer
      第31回日本放射光学会年会・放射光科学合同シンポジウム
  • [Presentation] EXAFS-CT法による燃料電池触媒のその場局所構造観察2018

    • Author(s)
      前島尚行、松井公佑、石黒志、Tan YuanYuan、小澤沙記、坂田智裕、東晃太朗、関澤央輝、宇留賀朋哉、唯 美津木
    • Organizer
      第31回日本放射光学会年会・放射光科学合同シンポジウム
  • [Presentation] 硬X線スペクトロタイコグラフィによる酸素吸蔵・放出材料の三次元価数識別イメージング2018

    • Author(s)
      広瀬真、石黒志、下村啓、松井公佑、唯美津木、高橋幸生
    • Organizer
      第31回日本放射光学会年会・放射光科学合同シンポジウム
  • [Presentation] Visualization of anisotropic crystalline phase variations inside Cr-supported FeOx dendrite crystals for oxygen storage process2018

    • Author(s)
      H. Matsui, Y. Suzuki, N. Ishiguro, M. Tada
    • Organizer
      日本化学会第98春季年会
  • [Presentation] カソードのガス交換と電位操作によるPEFC Pt/C, Pt3Co/Cカソード触媒の酸化過程の構造速度論解析2018

    • Author(s)
      小澤沙記、松井公佑、田口将寛、石黒志、宇留賀朋哉、関澤央輝、坂田智裕、東晃太朗、唯美津木
    • Organizer
      日本化学会第98春季年会
  • [Presentation] Rh, Crを担持したミクロンサイズのセリア結晶粒子の合成とレドックス特性2018

    • Author(s)
      若松昂平、松井公佑、石黒志、邨次智、唯美津木
    • Organizer
      日本化学会第98春季年会
  • [Presentation] Operando 3D-visualization of local chemical composition in PEFC Pt3Co/C cathode catalyst during accelerated degradation test2018

    • Author(s)
      Y. Tan, H. Matsui, N. Ishiguro, N. Maejima, T. Uruga, O. Sekizawa, M. Tada
    • Organizer
      日本化学会第98春季年会
  • [Presentation] 3D-visualization of distribution and redox property of a PEFC Pt/C cathode catalyst during degradation process by imaging XAFS2018

    • Author(s)
      N. Maejima, H. Matsui, N. Ishiguro, Y. Tan, T. Uruga, T. Sakata, K. Higashi, O. Sekizawa, M. Tada
    • Organizer
      日本化学会第98春季年会
  • [Presentation] Operando Observation of Reaction Distribution in a Composite Positive Electrode for All-Solid-State Lithium-Ion Batteries by Using CT-XAFS2018

    • Author(s)
      Y. Kimura, M. Fakkao, T. Nakamura, T. Okumura, O. Sekizawa, K. Nitta, N. Ishiguro, T. Uruga, M. Tada, Y. Uchimoto, K. Amezawa
    • Organizer
      第16回アジア固体イオニクス会議
    • Int'l Joint Research
  • [Presentation] CT-XAFSを用いたバルク型全固体リチウムイオン電池用合剤電極内の反応分布のオペランド評価2018

    • Author(s)
      木村 勇太,Fakkao Mahunnop,中村 崇司,石黒 志,関澤 央輝,新田 清文,宇留賀 朋哉,奥村 豊旗,唯 美津木,内本 喜晴,雨澤 浩史
    • Organizer
      電気化学会第85回大会
  • [Presentation] Structural Kinetics Study of Redox Processes of Pt/C and Pt3Co/C Cathode Electrocatalysts in a Polymer Electrolyte Fuel Cell during an Accelerated Durability Test by In Situ Time-Resolved XAFS2017

    • Author(s)
      Nozomu Ishiguro, Sutasinee Kityakarn, Oki Sekizawa, Tomoya Uruga, Hirosuke Matsui, Kensaku Nagasawa, Toshihiko Yokoyama, Mizuki Tada
    • Organizer
      253rd ACS National Meeting
    • Int'l Joint Research
  • [Presentation] ADT Processes of Pt/C and Pt3Co/C PEFC Cathode Electrocatalysts Studied by Operando Time-resolved Quick-XAFS2017

    • Author(s)
      Nozomu Ishiguro, Sutasinee Kityakarn, Oki Sekizawa, Tomoya Uruga, Hirosuke Matsui, Kensaku Nagasawa, Toshihiko Yokoyama, Mizuki Tada
    • Organizer
      International Symposium on Novel Energy Nanomaterials, Catalysts and Surfaces for Future Earth
    • Int'l Joint Research
  • [Presentation] In situ Time-resolved XAFS Study for ADT Processes of Pt/C and Pt3Co/C PEFC Cathode Electrocatalysts2017

    • Author(s)
      Nozomu Ishiguro, Sutasinee Kityakarn, Oki Sekizawa, Tomoya Uruga, Hirosuke Matsui, Kensaku Nagasawa, Toshihiko Yokoyama, Mizuki Tada
    • Organizer
      第16回日韓触媒シンポジウム及び第3回北海道大学触媒科学研究所国際シンポジウム
    • Int'l Joint Research
  • [Presentation] Oxidation of Pt and Pt3Co electrocatalysts at PEFC cathode studied by operando time-resolved QXAFS2017

    • Author(s)
      H. Matsui, S. Ozawa, N. Ishiguro, O. Sekizawa, T. Uruga, M. Tada
    • Organizer
      The 8th International Symposium on Surface Science
    • Int'l Joint Research
  • [Presentation] 3D-visualization of PEFC Pt cathode catalyst in MEA during ADT cycles by operando CT-XANES technique2017

    • Author(s)
      H. Matsui, N. Ishiguro, T. Uruga, O. Sekizawa, M. Tada
    • Organizer
      International Symposium on Novel Energy Nanomaterials, Catalysts and Surfaces for Future Earth
    • Int'l Joint Research
  • [Presentation] Visualization of Heterogeneity of Solid Catalysts2017

    • Author(s)
      M. Tada, H. Matsui, N. Ishiguro
    • Organizer
      International Symposium on Novel Energy Nanomaterials, Catalysts and Surfaces for Future Earth
    • Int'l Joint Research / Invited
  • [Presentation] Nanoscale Chemical Imaging of Oxygen Storage and Release Particles by Hard X-ray Spectro-Ptychography2017

    • Author(s)
      M. Hirose, N. Ishiguro, K. Shimomura, N. Burdet, H. Matsui, M. Tada, Y. Takahashi
    • Organizer
      International Symposium on Novel Energy Nanomaterials, Catalysts and Surfaces for Future Earth
    • Int'l Joint Research
  • [Presentation] Kinetics and reaction mechanism of oxidation processes on Pt/C and Pt3Co/C cathode catalysts studied by operando time-resolved QXAFS2017

    • Author(s)
      S. Ozawa, H. Matsui, N. Ishiguro, T. Uruga, O. Sekizawa, T. Sakata, K. Higashi, Mizuki Tada
    • Organizer
      International Symposium on Novel Energy Nanomaterials, Catalysts and Surfaces for Future Earth
    • Int'l Joint Research
  • [Presentation] 3D-Visualization of Pt and Co Segregations in Pt3Co Cathode Catalyst Layer by Operando XAFS-CT Imaging2017

    • Author(s)
      Y. Tan, H. Matsui, N. Ishiguro, N. Maejima, T. Uruga, O. Sekizawa, M. Tada
    • Organizer
      International Symposium on Novel Energy Nanomaterials, Catalysts and Surfaces for Future Earth
    • Int'l Joint Research
  • [Presentation] オペランド 3 次元イメージング XAFS を用いたバルク型全固体リチウムイオン電池用合材電極内の反応分布評価2017

    • Author(s)
      木村勇太、Mahunnop Fakkao、大崎静夏、高野彬、 中村崇司、伊奈稔哲、石黒志、関澤央輝、宇留賀朋哉、 奥村豊旗、唯美津木、内本喜晴
    • Organizer
      第43回固体イオニクス討論会
  • [Presentation] Operando 3-dimensional imaging XAFS of composite electrode for all-solid-state lithium-ion batteries2017

    • Author(s)
      Mahunnop Fakkao, Akira Takano, Yuta Kimura, Takashi Nakamura, Toyoki Okumura, Toshiaki Ina, Nozomu Ishiguro, Tomoya Uraga, Mizuki Tada, Yoshiharu Uchimoto, Koji Amezawa
    • Organizer
      第58回電池討論会
  • [Remarks] タイコグラフィ-X線吸収微細構造法の開発 -酸素吸蔵・放出材料の酸素拡散分布を可視化-

    • URL

      http://www.riken.jp/pr/press/2018/20180112_2/

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Published: 2018-12-17  

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