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Real-time observation of photocatalytic reaction at solid-liquid interface by using wavelength-dispersive soft X-ray absorption spectroscopy

Research Project

Project/Area Number 20K22475
Research Category

Grant-in-Aid for Research Activity Start-up

Allocation TypeMulti-year Fund
Review Section 0401:Materials engineering, chemical engineering, and related fields
Research InstitutionHigh Energy Accelerator Research Organization

Principal Investigator

Sakata Kaoruho  大学共同利用機関法人高エネルギー加速器研究機構, 物質構造科学研究所, 博士研究員 (80514215)

Project Period (FY) 2020-09-11 – 2022-03-31
Project Status Completed (Fiscal Year 2021)
Budget Amount *help
¥2,860,000 (Direct Cost: ¥2,200,000、Indirect Cost: ¥660,000)
Fiscal Year 2021: ¥1,430,000 (Direct Cost: ¥1,100,000、Indirect Cost: ¥330,000)
Fiscal Year 2020: ¥1,430,000 (Direct Cost: ¥1,100,000、Indirect Cost: ¥330,000)
Keywords軟X線吸収分光 / 電気化学反応 / 光触媒 / リアルタイム測定 / 固液界面 / 軟X線吸収分光法 / 表面化学 / リアルタイム観察
Outline of Research at the Start

水分解用光触媒と溶液の界面近傍における放射光軟X線の吸収スペクトルを、触媒の動作中に秒オーダーの時間分解能で連続測定することで、触媒表面の原子レベルでの形状と触媒活性の相関について明らかにする。そのために、電気化学反応中の触媒反応をX線吸収分光測定できるセルを作製し、反応のリアルタイム追跡を行うことで、電極/電解質溶液界面での触媒表面の電子状態や構造について解析を行う。

Outline of Final Research Achievements

In this study, a liquid cell was prepared aiming for a real-time observation of the photoelectrochemical reactions (oxygen evolution reaction) of semiconductor photocatalyst at solid/liquid interface by using the wavelength-dispersive X-ray absorption spectroscopy (XAS) in soft X-ray region. For the further improvement of the photocatalytic performance, it would be significant to clarify the reaction mechanism of the catalyst at solid/liquid interface.
The liquid part was separated from the measurement chamber in vacuum by using ultrathin Si3N4 window. An electrodes with TiO2 thin film was laminated onto the Si3N4 window attached with Pt thin film conductive layer. The electrode potential was swept to positive direction with/without illuminating UV light (wavelength 365 nm), and we succeeded to observed the XAFS spectra of oxygen K-edge (around 531 eV) of TiO2 during the electrode potential sweep, in real time.

Academic Significance and Societal Importance of the Research Achievements

軟X線吸収分光は化学種の同定や金属酸化物半導体の電子状態の観察ができる強力な手法だが、通常は真空中での測定に限られるため、電位を印加した状態で固液界面の光触媒反応時の電子状態をoperando解析した研究はこれまでにほとんど無く、特色がある。さらに、本研究では、触媒と溶液の界面近傍における軟X線の吸収スペクトルを,触媒の動作中に秒を切る時間分解能で連続測定することで、電気化学測定中の光の照射のon/offや電位の掃引に対する、半導体光触媒電極表面の非定常な反応過程についての知見が得られることが期待される。

Report

(3 results)
  • 2021 Annual Research Report   Final Research Report ( PDF )
  • 2020 Research-status Report
  • Research Products

    (8 results)

All 2022 2021

All Journal Article (2 results) (of which Int'l Joint Research: 2 results,  Peer Reviewed: 2 results) Presentation (6 results) (of which Int'l Joint Research: 4 results)

  • [Journal Article] Development of <i>Operando</i> Observation Technique of Electrochemical Reactions at the Solid-Liquid Interface by Fluorescence-yield Wavelength-dispersive Soft X-ray Absorption Spectroscopy2021

    • Author(s)
      Sakata Kaoruho、Amemiya Kenta
    • Journal Title

      Chemistry Letters

      Volume: 50 Issue: 9 Pages: 1710-1713

    • DOI

      10.1246/cl.210380

    • NAID

      130008088242

    • Related Report
      2021 Annual Research Report
    • Peer Reviewed / Int'l Joint Research
  • [Journal Article] Real-Time Observation of Surface Chemical Reactions Proceeding in the Depth Direction by Wavelength-Dispersive Soft X-ray Absorption Spectroscopy2021

    • Author(s)
      Sakata Kaoruho、Suzuki-Sakamaki Masako、Amemiya Kenta
    • Journal Title

      Nano Letters

      Volume: 21 Issue: 17 Pages: 7152-7158

    • DOI

      10.1021/acs.nanolett.1c01783

    • Related Report
      2021 Annual Research Report
    • Peer Reviewed / Int'l Joint Research
  • [Presentation] Fluorescence-yield wavelength-dispersive soft x-ray absorption spectroscopy with liquid cell aimed for a real-time observation at a solid/liquid interface2022

    • Author(s)
      Kaoruho Sakata、Amemiya Kenta
    • Organizer
      The international Conference on Synchrotron Radiation Instrumentation (SRI) 2021
    • Related Report
      2021 Annual Research Report
    • Int'l Joint Research
  • [Presentation] Real-time observation of surface chemical reaction by fluorescence-yield wavelength-dispersive soft x-ray absorption spectroscopy2022

    • Author(s)
      Amemiya Kenta、Kaoruho Sakata、Suzuki-Sakamaki Masako
    • Organizer
      The international Conference on Synchrotron Radiation Instrumentation (SRI) 2021
    • Related Report
      2021 Annual Research Report
    • Int'l Joint Research
  • [Presentation] 蛍光収量波長分散型軟X線吸収分光法による Cu表面の酸化過程のリアルタイム測定2022

    • Author(s)
      阪田薫穂、雨宮健太
    • Organizer
      第35回日本放射光学会年会・放射光科学合同シンポジウム
    • Related Report
      2021 Annual Research Report
  • [Presentation] Real-time Observation of the Electrochemical Reaction at a Solid-liquid Interface by Fluorescence-yield Wavelength-dispersive Soft X-ray Absorption Spectroscopy2021

    • Author(s)
      Kaoruho Sakata、Amemiya Kenta
    • Organizer
      The 9th International Symposium on Surface Science (ISSS-9)
    • Related Report
      2021 Annual Research Report
    • Int'l Joint Research
  • [Presentation] Development of Fluorescence-yield Wavelength-dispersive Soft X-ray Absorption Spectroscopy for Real-time Observation of Surface Chemical Reaction2021

    • Author(s)
      Amemiya Kenta、Kaoruho Sakata、Suzuki-Sakamaki Masako
    • Organizer
      The 9th International Symposium on Surface Science (ISSS-9)
    • Related Report
      2021 Annual Research Report
    • Int'l Joint Research
  • [Presentation] 蛍光収量波長分散型軟X線吸収分光法を用いた固液界面における電気化学反応のオペランド解析2021

    • Author(s)
      阪田薫穂、雨宮健太
    • Organizer
      第24回XAFS討論会
    • Related Report
      2021 Annual Research Report

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Published: 2020-09-29   Modified: 2023-01-30  

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