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Development of a dynamical operando hard x-ray photoelectron spectroscopic system for liquid reaction field

Research Project

Project/Area Number 21H04677
Research Category

Grant-in-Aid for Scientific Research (A)

Allocation TypeSingle-year Grants
Section一般
Review Section Medium-sized Section 32:Physical chemistry, functional solid state chemistry, and related fields
Research InstitutionInstitute for Molecular Science

Principal Investigator

YOKOYAMA TOSHIHIKO  分子科学研究所, 物質分子科学研究領域, 教授 (20200917)

Co-Investigator(Kenkyū-buntansha) 小板谷 貴典  京都大学, 理学研究科, 准教授 (60791754)
山本 航平  国立研究開発法人量子科学技術研究開発機構, 次世代放射光施設整備開発センター, 研究員 (30844823)
倉橋 直也  分子科学研究所, 物質分子科学研究領域, 特任助教 (20973382)
Project Period (FY) 2021-04-05 – 2024-03-31
Project Status Completed (Fiscal Year 2023)
Budget Amount *help
¥42,120,000 (Direct Cost: ¥32,400,000、Indirect Cost: ¥9,720,000)
Fiscal Year 2023: ¥12,350,000 (Direct Cost: ¥9,500,000、Indirect Cost: ¥2,850,000)
Fiscal Year 2022: ¥11,570,000 (Direct Cost: ¥8,900,000、Indirect Cost: ¥2,670,000)
Fiscal Year 2021: ¥18,200,000 (Direct Cost: ¥14,000,000、Indirect Cost: ¥4,200,000)
Keywords大気圧光電子分光 / オペランド分光 / 界面 / 二酸化炭素 / メタノール合成 / 電気化学的還元反応 / 光電子分光 / 化学反応 / 固液界面 / 気液界面 / シンクロトロン放射光
Outline of Research at the Start

固体‐液体界面および液体‐気体界面における化学反応機構の解明を目的として、オペランド固液・気液界面硬X線雰囲気制御光電子分光システムを新たに開発する。定常状態・平衡状態・遅い化学反応を観測する「静的オペランド固液・気液界面X線光電子分光システム」と液体の流れを利用した時間分解測定のための「動的オペランド固液・気液界面X線光電子分光システム」を新たに開発し、多様なタイムスケールで化学反応のリアルタイム分光観測を実施する。これににより均一系触媒・不均一触媒・電気化学反応の反応機構解明に展開することで新たな化学反応学理の構築ならびに触媒反応の開発・改良に大きく貢献できる。

Outline of Final Research Achievements

X-ray photoelectron spectroscopy (XPS), which is widely used in materials characterization, is usually performed under high vacuum due to requirement of precise measurement of the photoelectron kinetic energy, but recent advances in synchrotron radiation sources and measurement instruments have made it possible to perform XPS measurements under atmospheric pressure. In this study, we have developed a measurement method for operando hard X-ray photoelectron spectroscopy (HAXPES) of catalysts and electrochemical cells in operation, especially for systems containing liquids, and succeeded in identifying surface adsorption products during reactions on CO2-reducing heterogeneous CuZnAl catalysts and electrochemical cells. The practical measurement conditions are up to 300°C sample temperature and 0.5 atm gas pressure, making it one of the highest performance instruments in the world.

Academic Significance and Societal Importance of the Research Achievements

近年の科学技術計測におけるデバイスやシステムの評価・解析では、動作中の状態をありのままオペランド観測することが強く期待されるようになった。光電子分光法は実験室でも物質・材料の化学状態解析等で広く活用されている計測手法であり、本研究で開発した電池等の液体状態を含む系でもオペランド硬X線光電子分光法はSPring-8において共用機器に供されており、我が国の多くの研究者に活用していただける。本システムは、環境・エネルギー分野で必須の緊喫課題であるCO2還元、窒素固定化、蓄電池・燃料電池・電気分解、動作中半導体デバイスなど極めて広い物質・材料開発に極めて有効に機能しうる。

Report

(5 results)
  • 2023 Annual Research Report   Final Research Report ( PDF )
  • 2022 Annual Research Report
  • 2021 Comments on the Screening Results   Annual Research Report
  • Research Products

    (23 results)

All 2024 2023 2022 2021 Other

All Journal Article (8 results) (of which Int'l Joint Research: 3 results,  Peer Reviewed: 8 results,  Open Access: 2 results) Presentation (13 results) (of which Int'l Joint Research: 4 results,  Invited: 10 results) Remarks (2 results)

  • [Journal Article] <i>Operando</i> Observation of Hydrogenation of Carbon Dioxide by Near Ambient Pressure X-ray Photoelectron Spectroscopy2024

    • Author(s)
      KOITAYA Takanori、YAMAMOTO Susumu、MATSUDA Iwao、YOSHINOBU Jun、YOKOYAMA Toshihiko
    • Journal Title

      Vacuum and Surface Science

      Volume: 67 Issue: 3 Pages: 117-122

    • DOI

      10.1380/vss.67.117

    • ISSN
      2433-5835, 2433-5843
    • Year and Date
      2024-03-10
    • Related Report
      2023 Annual Research Report
    • Peer Reviewed
  • [Journal Article] Present Status and Prospects of Operando Measurement by Atmospheric Pressure Hard X-ray Photoelectron Spectroscopy2024

    • Author(s)
      TAKAGI Yasumasa, YOKOYAMA Toshihiko
    • Journal Title

      Vacuum and Surface Science

      Volume: 67 Pages: 123-128

    • Related Report
      2023 Annual Research Report
    • Peer Reviewed
  • [Journal Article] Operando Characterization of Copper?Zinc?Alumina Catalyst for Methanol Synthesis from Carbon Dioxide and Hydrogen by Ambient-Pressure Hard X-ray Photoelectron Spectroscopy2023

    • Author(s)
      Koitaya Takanori、Yamamoto Kohei、Uruga Tomoya、Yokoyama Toshihiko
    • Journal Title

      The Journal of Physical Chemistry C

      Volume: 127 Issue: 27 Pages: 13044-13054

    • DOI

      10.1021/acs.jpcc.3c02785

    • Related Report
      2023 Annual Research Report
    • Peer Reviewed
  • [Journal Article] Metallic bonds and thermal vibration in brass2023

    • Author(s)
      Yokoyama Toshihiko
    • Journal Title

      Physical Chemistry Chemical Physics

      Volume: 25 Issue: 4 Pages: 3413-3419

    • DOI

      10.1039/d2cp05035h

    • Related Report
      2022 Annual Research Report
    • Peer Reviewed
  • [Journal Article] Pt17 nanocluster electrocatalysts: preparation and origin of high oxygen reduction reaction activity2023

    • Author(s)
      Kawawaki Tokuhisa、Mitomi Yusuke、Nishi Naoki、Kurosaki Ryuki、Oiwa Kazutaka、Tanaka Tomoya、Hirase Hinoki、Miyajima Sayuri、Niihori Yoshiki、Osborn D. J.、Koitaya Takanori、Metha Gregory F.、Yokoyama Toshihiko、Iida Kenji、Negishi Yuichi
    • Journal Title

      Nanoscale

      Volume: in press Issue: 16 Pages: 7272-7279

    • DOI

      10.1039/d3nr01152f

    • Related Report
      2022 Annual Research Report
    • Peer Reviewed / Open Access / Int'l Joint Research
  • [Journal Article] Metastable Structure of Photoexcited WO3 Determined by the Pump-probe Extended X-ray Absorption Fine Structure Spectroscopy and Constrained Thorough Search Analysis2022

    • Author(s)
      Kido Daiki、Uemura Yohei、Wakisaka Yuki、Koide Akihiro、Uehara Hiromitsu、Niwa Yasuhiro、Nozawa Shunsuke、Ichiyanagi Kohei、Fukaya Ryo、Adachi Shin-ichi、Sato Tokushi、Jenkins Harry、Yokoyama Toshihiko、Takakusagi Satoru、Hasegawa Jun-ya、Asakura Kiyotaka
    • Journal Title

      Chemistry Letters

      Volume: 51 Issue: 11 Pages: 1083-1086

    • DOI

      10.1246/cl.220381

    • Related Report
      2022 Annual Research Report
    • Peer Reviewed / Open Access / Int'l Joint Research
  • [Journal Article] Layer-resolved magnetic moments in N-surfactant assisted FeNi ordered alloy thin films2022

    • Author(s)
      Kawaguchi K.、Miyamachi T.、Gozlinski T.、Iimori T.、Takahashi Y.、Hattori T.、Yamamoto K.、Koitaya T.、Iwayama H.、Ishiyama O.、Nakamura E.、Kotsugi M.、Wulfhekel W.、Yokoyama T.、Komori F.
    • Journal Title

      Japanese Journal of Applied Physics

      Volume: 61 Issue: SL Pages: SL1001-SL1001

    • DOI

      10.35848/1347-4065/ac66c1

    • Related Report
      2022 Annual Research Report
    • Peer Reviewed / Int'l Joint Research
  • [Journal Article] Sulfur Poisoning Pt and PtCo Anode and Cathode Catalysts in Polymer Electrolyte Fuel Cells Studied by Operando Near Ambient Pressure Hard X-ray Photoelectron Spectroscopy2021

    • Author(s)
      S. Chaveanghong, T. Nakamura, Y. Takagi, B. Cagnon, T. Uruga, M. Tada, Y. Iwasawa and T. Yokoyama
    • Journal Title

      Phys. Chem. Chem. Phys.

      Volume: 23 Issue: 6 Pages: 3866-3873

    • DOI

      10.1039/d0cp06020h

    • Related Report
      2021 Annual Research Report
    • Peer Reviewed
  • [Presentation] 硬X線光電子分光による電気化学反応のオペランド観測2024

    • Author(s)
      小板谷 貴典
    • Organizer
      日本物理学会
    • Related Report
      2023 Annual Research Report
  • [Presentation] 様々な光で解析する高分子電解質膜と水の関係2024

    • Author(s)
      倉橋直也
    • Organizer
      水素・燃料電池材料研究会
    • Related Report
      2023 Annual Research Report
    • Invited
  • [Presentation] 雰囲気制御型硬X線光電子分光によるパラジウム合金への水素吸蔵過程のその場観測2023

    • Author(s)
      小板谷 貴典
    • Organizer
      日本物理学会
    • Related Report
      2023 Annual Research Report
  • [Presentation] 物質科学のための放射光X線分光2023

    • Author(s)
      横山 利彦
    • Organizer
      第26回日本XAFS討論会
    • Related Report
      2023 Annual Research Report
    • Invited
  • [Presentation] Operando ambient pressure hard x-ray photoelectron spectroscopic studies of working fuel cells and CO2 reduction catalyst2023

    • Author(s)
      Toshihiko YOKOYAMA
    • Organizer
      16th Eurasia Conference on Chemical Sciences 2023
    • Related Report
      2023 Annual Research Report
    • Invited
  • [Presentation] 雰囲気制御光電子分光による表面反応過程のその場観測2023

    • Author(s)
      小板谷貴典
    • Organizer
      日本物理学会
    • Related Report
      2022 Annual Research Report
    • Invited
  • [Presentation] 燃料電池のその場X線光電子分光と次世代放射光への期待2022

    • Author(s)
      横山利彦
    • Organizer
      触媒学会次世代放射光WG 公開シンポジウム
    • Related Report
      2022 Annual Research Report
    • Invited
  • [Presentation] 雰囲気制御硬X線光電子分光と燃料電池・触媒反応その場観察への応用2022

    • Author(s)
      横山利彦
    • Organizer
      2022年度立命館大学SRセンター研究成果報告会
    • Related Report
      2022 Annual Research Report
    • Invited
  • [Presentation] Surface chemistry of carbon dioxide studied by ambient-pressure XPS2022

    • Author(s)
      Takanori Koitaya
    • Organizer
      14th International Symposium on Atomic Level Characterizations for New Materials and Devices
    • Related Report
      2022 Annual Research Report
    • Int'l Joint Research / Invited
  • [Presentation] Operando observation of working polymer electrolyte fuel cell studied by ambient pressure hard X-ray photoelectron spectroscopy2021

    • Author(s)
      Toshihiko Yokoyama
    • Organizer
      Pacifichem2021
    • Related Report
      2021 Annual Research Report
    • Int'l Joint Research / Invited
  • [Presentation] Ambient Pressure Hard X-ray Photoelectron Spectroscopy on Polymer Electrolyte Fuel Cells under Working Conditions2021

    • Author(s)
      Toshihiko Yokoyama
    • Organizer
      MRM2021
    • Related Report
      2021 Annual Research Report
    • Int'l Joint Research / Invited
  • [Presentation] Operando observation of heterogeneous catalysts by near ambient pressure X-ray photoelectron spectroscopy2021

    • Author(s)
      Takanori Koitaya
    • Organizer
      2nd IMS-SKKU-UJN Symposium on Chemical Catalysis
    • Related Report
      2021 Annual Research Report
    • Int'l Joint Research / Invited
  • [Presentation] 雰囲気光電子分光法によるパラジウムー金合金の水素吸蔵過程のリアルタイム観測2021

    • Author(s)
      小板谷貴典、山本達、松田巌、吉信淳、横山利彦
    • Organizer
      2021年日本表面真空学会学術講演会
    • Related Report
      2021 Annual Research Report
  • [Remarks] 電解質の電位を測る: 気体存在下の光電子分光

    • URL

      https://www.ims.ac.jp/publications/letters85/85_3.pdf

    • Related Report
      2021 Annual Research Report
  • [Remarks] Exploitation of Novel Spectroscopic Methods ...

    • URL

      https://www.ims.ac.jp/about/publication/ann_rev_2021/2021yokoyama.pdf

    • Related Report
      2021 Annual Research Report

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Published: 2021-04-28   Modified: 2025-01-30  

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