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Quantitative analysis of functional elements segregated in general ceramics grain boundaries using nano-electron probe spectroscopy

Research Project

Project/Area Number 17K19101
Research Category

Grant-in-Aid for Challenging Research (Exploratory)

Allocation TypeMulti-year Fund
Research Field Physical chemistry, Functional solid state chemistry, and related fields
Research InstitutionNagoya University

Principal Investigator

MUTO SHUNSUKE  名古屋大学, 未来材料・システム研究所, 教授 (20209985)

Co-Investigator(Kenkyū-buntansha) 大塚 真弘  名古屋大学, 工学研究科, 助教 (60646529)
Research Collaborator IGAMI yohei  
Project Period (FY) 2017-06-30 – 2019-03-31
Project Status Completed (Fiscal Year 2018)
Budget Amount *help
¥6,370,000 (Direct Cost: ¥4,900,000、Indirect Cost: ¥1,470,000)
Fiscal Year 2018: ¥1,950,000 (Direct Cost: ¥1,500,000、Indirect Cost: ¥450,000)
Fiscal Year 2017: ¥4,420,000 (Direct Cost: ¥3,400,000、Indirect Cost: ¥1,020,000)
Keywordsナノ材料物性 / 透過電子顕微鏡 / 蛍光X線分析 / 解析・評価 / セラミックス / 結晶粒界 / ナノ材料 / 粒界偏析 / 電子顕微鏡 / 格子欠陥 / 磁性材料
Outline of Final Research Achievements

This study aims to develop a robust scheme to identify the crystallographic sites where functional dopants segregated in general randomly-oriented grain boundaries occupy and their associated chemical states there by combining the dopant analysis using electron beam rocking and advanced spectral imaging techniques.
we developed a beam controlling software to correct the aberrations of electromagnetic lens of TEM, which enables the incident electron beam to illuminate a sample with parallelly foucued on a area smaller than 100 nm in diameter.
The present method applied to a Y-doped SrTiO3 grain boundary, and we successfully obtained the X-ray channeling signal from Y, suggesting that Y occupies particular atomic columns and also associated oxygen vacancies are introduced to compensate for the charge imbalance at the position next to the doped Y. The present results are summarized as a review report in the annual bulletin of Japan Institute of Metals.

Academic Significance and Societal Importance of the Research Achievements

機能材料において、構成元素の正確なサイト占有率や微量ドーパントの占有サイトを定量的に正確に知ることは、材料設計上きわめて重要である。多くの場合、X線回折データにリートベルト解析を適用することが標準的であるが、ナノ構造を持っている場合、原子番号の近接した元素を含む場合など、この手法が適用できない場合も多い。本研究で開発した手法はこのような制限を一切必要とせず、さらに組成変化に伴う原子位置の変位や、電気的中性条件のために導入される陰イオン空孔の解析へと拡張可能である。実際現在最も民間からの分析依頼が多い手法となっている。

Report

(3 results)
  • 2018 Annual Research Report   Final Research Report ( PDF )
  • 2017 Research-status Report
  • Research Products

    (19 results)

All 2019 2018 2017 Other

All Int'l Joint Research (1 results) Journal Article (3 results) (of which Int'l Joint Research: 1 results,  Peer Reviewed: 3 results,  Open Access: 2 results) Presentation (15 results) (of which Int'l Joint Research: 5 results,  Invited: 2 results)

  • [Int'l Joint Research] ウプサラ大学(スウェーデン)

    • Related Report
      2017 Research-status Report
  • [Journal Article] 電子チャネリング効果を利用した結晶材料定量分析法の現状2019

    • Author(s)
      大塚真弘,武藤俊介
    • Journal Title

      日本金属学会会報「まてりあ」

      Volume: 58 Pages: 73-76

    • NAID

      130007587788

    • Related Report
      2018 Annual Research Report
    • Peer Reviewed / Open Access
  • [Journal Article] Cation mixing in LiNi0.8Co0.15Al0.05O2 positive electrode material studied using high angular resolution electron channeling X-ray spectroscopy2018

    • Author(s)
      Y. Yamamoto, M. Ohtsuka, Y. Azuma, T. Takahashi, S. Muto
    • Journal Title

      Journal of Power Sources

      Volume: 401 Pages: 263-270

    • DOI

      10.1016/j.jpowsour.2018.08.100

    • Related Report
      2018 Annual Research Report
    • Peer Reviewed / Open Access
  • [Journal Article] Unmixing hyperspectral data by using signal subspace sampling2017

    • Author(s)
      Spiegelberg Jakob、Muto Shunsuke、Ohtsuka Masahiro、Pelckmans Kristiaan、Rusz Jan
    • Journal Title

      Ultramicroscopy

      Volume: 182 Pages: 205-211

    • DOI

      10.1016/j.ultramic.2017.07.009

    • Related Report
      2017 Research-status Report
    • Peer Reviewed / Int'l Joint Research
  • [Presentation] 電子チャネリング効果を利用したW型フェライトSrFe18-xZnxO27のサイト選択的電子状態分析2019

    • Author(s)
      大塚真弘, 柳原颯太, 武藤俊介, 阿南義弘
    • Organizer
      日本金属学会2019年春期(第164回)講演大会
    • Related Report
      2018 Annual Research Report
  • [Presentation] 汎用分析電子顕微鏡による電子チャネリング効果を活用した結晶材料定量分析の進展2019

    • Author(s)
      大塚真弘
    • Organizer
      環境調和材料研究会
    • Related Report
      2018 Annual Research Report
    • Invited
  • [Presentation] Multiway hyperspectral data analysis of trace element/valence-state in W-type ferrite magnet by concurrent high-angular resolution electron channeling X-ray/electron spectroscopy2018

    • Author(s)
      M. Ohtsuka, S. Yanagihara, J. Spiegelberg, J. Rusz, S. Muto
    • Organizer
      19th International Microscopy Congress (IMC19)
    • Related Report
      2018 Annual Research Report
    • Int'l Joint Research
  • [Presentation] Trace dopant/oxygen vacancy site determination in Al-doped Y2T2O7 by 2D electron channeling EDX analysis2018

    • Author(s)
      K. Oda, M. Ohtsuka, M. Tanaka, S. Kitaoka, S. Muto
    • Organizer
      19th International Microscopy Congress (IMC19)
    • Related Report
      2018 Annual Research Report
    • Int'l Joint Research
  • [Presentation] Determination of site occupancy from micrometric regions in minerals by high angular resolution electron channeling X-ray spectroscopy2018

    • Author(s)
      Y. Igami, M. Ohtsuka, A. Miyake, T. Kuribayashi, S. Toh, S. Muto
    • Organizer
      19th International Microscopy Congress (IMC19)
    • Related Report
      2018 Annual Research Report
    • Int'l Joint Research
  • [Presentation] 耐環境セラミックス保護膜中の添加元素及び酸素欠損サイトのHARECXS法による評価2018

    • Author(s)
      織田健嗣, 大塚真弘, 武藤俊介, 田中誠, 北岡諭
    • Organizer
      日本顕微鏡学会第74回学術講演会
    • Related Report
      2018 Annual Research Report
  • [Presentation] ビーム制御プラグインQEDを利用した高角度分解能電子チャネリングX線/電子分光分析2018

    • Author(s)
      大塚真弘, 石塚顕在, 武藤 俊介
    • Organizer
      日本顕微鏡学会第74回学術講演会
    • Related Report
      2018 Annual Research Report
  • [Presentation] 拡張統計アルケミ法によるThMn12型磁石材料中の添加元素置換サイト計測2018

    • Author(s)
      阿南義弘, 鈴木啓幸, 大塚真弘, 武藤俊介
    • Organizer
      日本顕微鏡学会第74回学術講演会
    • Related Report
      2018 Annual Research Report
  • [Presentation] Quantitative atomic-site-analysis of functional dopants by electron-channeling-enhanced microanalysis2017

    • Author(s)
      K. Oda, M. Ohtsuka, S. Muto, M. Tanaka, S. Kitaoka
    • Organizer
      International Conference on Materials and Systems for Sustainability (ICMaSS2017)
    • Related Report
      2017 Research-status Report
    • Int'l Joint Research
  • [Presentation] Quantitative analysis of dopant site occupancies in Zn-doped W-type ferrite magnets using extended statistical ALCHEMI method2017

    • Author(s)
      Y. Anan, Y. Kobayashi, M. Ohtsuka, S. Muto
    • Organizer
      11th International Symposium on Atomic Level Characterizations for New Materials and Devices ’17 (ALC’17)
    • Related Report
      2017 Research-status Report
    • Int'l Joint Research
  • [Presentation] 統計学を利用した元素/サイト選択的分光分析とその格子欠陥への応用2017

    • Author(s)
      大塚真弘
    • Organizer
      日本物理学会第73回年次大会
    • Related Report
      2017 Research-status Report
    • Invited
  • [Presentation] ビームロッキングTEM-EDX分析を用いた耐環境保護膜中の微量添加物占有サイト及び酸素欠損サイトの同定2017

    • Author(s)
      織田健嗣, 大塚真弘, 武藤俊介, 田中誠、北岡諭
    • Organizer
      日本顕微鏡学会第73回学術講演会
    • Related Report
      2017 Research-status Report
  • [Presentation] 統計的ALCHEMI法を用いたK1-xNaxNbO3系無鉛圧電材料の添加元素置換サイト解析2017

    • Author(s)
      大塚真弘, 山田嗣人, 大林和重, 武藤俊介
    • Organizer
      日本顕微鏡学会第73回学術講演会
    • Related Report
      2017 Research-status Report
  • [Presentation] 拡張統計アルケミ法によるW型フェライト磁石中の添加Zn置換サイト計測2017

    • Author(s)
      阿南義弘, 小林義徳, 大塚真弘, 武藤俊介
    • Organizer
      日本顕微鏡学会第73回学術講演会
    • Related Report
      2017 Research-status Report
  • [Presentation] ビームロッキング複合電子顕微分光ハイパースペクトルデータのマルチウェイ解析2017

    • Author(s)
      大塚真弘, 武藤俊介
    • Organizer
      日本金属学会2017年秋期(第161回)講演大会
    • Related Report
      2017 Research-status Report

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Published: 2017-07-21   Modified: 2020-03-30  

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