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Nanoscale evaluation of all-solid-state battery reactions by operando transmission electron microscopy

Research Project

Project/Area Number 17H02792
Research Category

Grant-in-Aid for Scientific Research (B)

Allocation TypeSingle-year Grants
Section一般
Research Field Thin film/Surface and interfacial physical properties
Research InstitutionJapan Fine Ceramics Center

Principal Investigator

Yamamoto Kazuo  一般財団法人ファインセラミックスセンター, その他部局等, 主任研究員 (80466292)

Project Period (FY) 2017-04-01 – 2020-03-31
Project Status Completed (Fiscal Year 2019)
Budget Amount *help
¥17,680,000 (Direct Cost: ¥13,600,000、Indirect Cost: ¥4,080,000)
Fiscal Year 2019: ¥2,080,000 (Direct Cost: ¥1,600,000、Indirect Cost: ¥480,000)
Fiscal Year 2018: ¥2,210,000 (Direct Cost: ¥1,700,000、Indirect Cost: ¥510,000)
Fiscal Year 2017: ¥13,390,000 (Direct Cost: ¥10,300,000、Indirect Cost: ¥3,090,000)
Keywordsリチウムイオン電池 / 全固体電池 / オペランド計測 / 電子線ホログラフィー / 電子エネルギー損失分光法 / 電子顕微鏡 / 固体イオニクス / 界面 / 空間電荷層
Outline of Final Research Achievements

In this study, we developed operando scanning/transmission electron microscopy (S/TEM) techniques to visualize the electrochemical reactions in all-solid-state Li-ion batteries. We succeeded in observing ionic space charge layer at Cu-metal-electrode/solid-electrolyte interface using electron holography and electron energy-loss spectroscopy (EELS). Moreover, we visualized dynamical behavior of Li-ions in LiCoO2 electrode during charge-discharge reactions by operando STEM-EELS. In order to improve a time-resolution of the Li-map observations, we applied one of the information science techniques, sparse coding. As a result, we succeeded in visualizing 10-times more rapid behavior of Li-ions in the electrodes, in which the Li-ions move not only to the direction toward the electrolyte but also in the in-plane direction of the electrode film.

Academic Significance and Societal Importance of the Research Achievements

全固体電池内部の電極/固体電解質界面近傍におけるイオン移動の様子は不明な点が多く残されているが,本研究で開発したオペランド電子顕微鏡技術により,イオン移動の様子や界面抵抗の要因を明らかにすることができた.この成果は,固体界面イオニクスの学理構築に大きく貢献すると考えられる.また,高性能な全固体電池は,将来,電気自動車やハイブリッド自動車に搭載される可能性が高く,本研究の成果は地球温暖化対策の一助として社会的にも意義が高い.

Report

(4 results)
  • 2019 Annual Research Report   Final Research Report ( PDF )
  • 2018 Annual Research Report
  • 2017 Annual Research Report
  • Research Products

    (39 results)

All 2020 2019 2018 2017 Other

All Journal Article (8 results) (of which Peer Reviewed: 6 results,  Open Access: 3 results) Presentation (27 results) (of which Int'l Joint Research: 11 results,  Invited: 13 results) Book (1 results) Remarks (3 results)

  • [Journal Article] Dynamic imaging of lithium in solid-state batteries by operando electron energy-loss spectroscopy with sparse coding2020

    • Author(s)
      Yuki Nomura, Kazuo Yamamoto, Mikiya Fujii, Tsukasa Hirayama, Emiko Igaki, Koh Saitoh
    • Journal Title

      Nature Communications

      Volume: 印刷中

    • Related Report
      2019 Annual Research Report
    • Peer Reviewed / Open Access
  • [Journal Article] Visualization of different carrier concentrations in n-type-GaN semiconductors by phase-shifting electron holography with multiple electron biprisms2019

    • Author(s)
      Yamamoto Kazuo、Nakano Kiyotaka、Tanaka Atsushi、Honda Yoshio、Ando Yuto、Ogura Masaya、Matsumoto Miko、Anada Satoshi、Ishikawa Yukari、Amano Hiroshi、Hirayama Tsukasa
    • Journal Title

      Microscopy

      Volume: 69 Issue: 1 Pages: 1-10

    • DOI

      10.1093/jmicro/dfz037

    • Related Report
      2019 Annual Research Report
    • Peer Reviewed / Open Access
  • [Journal Article] 最先端電子顕微鏡技術を用いた全固体電池のオペランド観察2019

    • Author(s)
      山本和生,野村優貴
    • Journal Title

      MATERIAL STAGE

      Volume: 19 Pages: 32-36

    • Related Report
      2019 Annual Research Report
  • [Journal Article] 最先端電子顕微鏡技術を用いた機能性デバイスのオペランド観察2019

    • Author(s)
      山本和生,穴田智史,野村優貴
    • Journal Title

      クリーンテクノロジー

      Volume: 9 Pages: 31-35

    • Related Report
      2019 Annual Research Report
  • [Journal Article] 高精度位相シフト電子線ホログラフィーによる Ⅲ - Ⅴ族化合物半導体の精密解析と高速観察への可能性2019

    • Author(s)
      山本 和生,穴田智史,仲野靖孝,野村優貴,松本実子,平山司
    • Journal Title

      顕微鏡

      Volume: 54 Pages: 31-38

    • NAID

      130007655726

    • Related Report
      2019 Annual Research Report
    • Peer Reviewed
  • [Journal Article] Direct Observation of a Li-ionic Space-Charge Layer Formed at an Electrode/Solid-Electrolyte Interface2019

    • Author(s)
      Y. Nomura, K.Yamamoto, T. Hirayama, S. Ouchi, E. Igaki, and K. Saitoh
    • Journal Title

      Angewandte Chemie

      Volume: 58 Issue: 16 Pages: 5292-5296

    • DOI

      10.1002/anie.201814669

    • Related Report
      2018 Annual Research Report
    • Peer Reviewed
  • [Journal Article] Quantitative operando visualization of electrochemical reactions and Li ions in All-Solid-State batteries by STEM-EELS with hyperspectral image analyses2018

    • Author(s)
      Y. Nomura, K. Yamamoto, T. Hirayama, M. Ohkawa, E. Igaki, N. Hojo, and K. Saitoh
    • Journal Title

      Nano Lett.

      Volume: 18 Issue: 9 Pages: 5892-5898

    • DOI

      10.1021/acs.nanolett.8b02587

    • Related Report
      2018 Annual Research Report
    • Peer Reviewed
  • [Journal Article] Electric shielding films for biased TEM samples and their application to in situ electron holography2018

    • Author(s)
      Yuki Nomura, Kazuo Yamamoto, Tsukasa Hirayama, Koh Saitoh
    • Journal Title

      Microscopy

      Volume: 印刷中 Issue: 3 Pages: 178-186

    • DOI

      10.1093/jmicro/dfy018

    • Related Report
      2017 Annual Research Report
    • Peer Reviewed / Open Access
  • [Presentation] 透過型電子顕微鏡を用いた全固体電池の充放電中in situ / operando計測2020

    • Author(s)
      山本和生
    • Organizer
      技術情報協会 セミナー
    • Related Report
      2019 Annual Research Report
    • Invited
  • [Presentation] In situ / Operando電子顕微鏡法による機能性デバイスの計測と将来展望2020

    • Author(s)
      山本和生
    • Organizer
      九州大学 ナノテクセミナー
    • Related Report
      2019 Annual Research Report
    • Invited
  • [Presentation] Direct Evaluation of Functional Devices by Operando Transmission Electron Microscopy2019

    • Author(s)
      Kazuo Yamamoto, Yuki Nomura, Satoshi Anada, Tsukasa Hirayama
    • Organizer
      The 6th International Symposium on Advanced Microscopy and Theoretical Calculations
    • Related Report
      2019 Annual Research Report
    • Int'l Joint Research / Invited
  • [Presentation] Visualization of a Li-ionic space-charge layer in a solid-electrolyte by transmission electron microscopy2019

    • Author(s)
      Yuki Nomura, Kazuo Yamamoto, Tsukasa Hirayama, Emiko Igaki, Koh Saitoh
    • Organizer
      The 6th International Symposium on Advanced Microscopy and Theoretical Calculations
    • Related Report
      2019 Annual Research Report
    • Int'l Joint Research
  • [Presentation] Operando位相シフト電子線ホログラフィーによる全固体電池の電位分布観察2019

    • Author(s)
      山本和生,野村優貴,穴田智史,平山司
    • Organizer
      日本顕微鏡学会 学術講演会
    • Related Report
      2019 Annual Research Report
  • [Presentation] 電子線ホログラフィーとEELSによる固体電解質内の空間電荷層の可視化2019

    • Author(s)
      野村優貴,山本和生,平山司,大内暁,井垣恵美子,齋藤晃
    • Organizer
      日本顕微鏡学会 学術講演会
    • Related Report
      2019 Annual Research Report
  • [Presentation] Precise measurement of carrier concentrations in n-type GaN by phase-shifting electron holography2019

    • Author(s)
      Kazuo Yamamoto, Kiyotaka Nakano, Atsushi Tanaka, Yoshio Honda, Yuto Ando, Masaya Ogura, Miko Matsumoto, Satoshi Anada, Yukari Ishikawa, Hiroshi Amano, Tsukasa Hirayama
    • Organizer
      Microscopy and Microanalysis 2019
    • Related Report
      2019 Annual Research Report
    • Int'l Joint Research
  • [Presentation] In situ observation of electrochemical reactions in a solid--state Li-ion battery2019

    • Author(s)
      Y. Nomura, K. Yamamoto, T. Hirayama, E. Igaki, K. Saitoh
    • Organizer
      Microscopy and Microanalysis 2019
    • Related Report
      2019 Annual Research Report
    • Int'l Joint Research
  • [Presentation] 機能性デバイスのオペランド観察に必要となる電圧印加用TEM試料作製技術とその応用2019

    • Author(s)
      山本和生,穴田智史,野村優貴
    • Organizer
      第35回 分析電子顕微鏡討論会
    • Related Report
      2019 Annual Research Report
    • Invited
  • [Presentation] 金属/Liイオン伝導性固体電解質界面における空間電荷層の可視化2019

    • Author(s)
      山本和生,野村優貴
    • Organizer
      応用物理学会 秋季学術講演会
    • Related Report
      2019 Annual Research Report
  • [Presentation] Dynamical visualization of Nano-Scale Electrochemical Reactions in Solid-State Batteries by Advanced Transmission Electron Microscopy2019

    • Author(s)
      K. Yamamoto, Y. Nomura
    • Organizer
      2nd World Conference on Solid Electrolyte for Advanced Applications: Garnets and Competitors
    • Related Report
      2019 Annual Research Report
    • Int'l Joint Research / Invited
  • [Presentation] Nano-scale evaluation of functional devices by in situ transmission electron microscopy2019

    • Author(s)
      K. Yamamoto, Y. Nomura, S. Anada, T. Hirayama
    • Organizer
      International Conference on Materials and Systems for Sustainability
    • Related Report
      2019 Annual Research Report
    • Int'l Joint Research / Invited
  • [Presentation] 最先端電子顕微鏡法による機能性デバイス/材料のin situ / operando観察と将来展望2019

    • Author(s)
      山本和生,野村優貴,穴田智史
    • Organizer
      学振158委員会「真空エレクトロニクス」研究会
    • Related Report
      2019 Annual Research Report
    • Invited
  • [Presentation] 最先端電子顕微鏡技術を用いた機能性デバイスのオペランド観察2019

    • Author(s)
      山本和生
    • Organizer
      nanotech 2019 (東京ビッグサイト)
    • Related Report
      2018 Annual Research Report
    • Invited
  • [Presentation] 最先端電子顕微鏡法を用いた全固体Liイオン電池のオペランド観察2019

    • Author(s)
      山本和生
    • Organizer
      新型電池オープンラボ第25回講演会(神奈川大学)
    • Related Report
      2018 Annual Research Report
    • Invited
  • [Presentation] 電子線ホログラフィー II(応用編)2018

    • Author(s)
      山本和生
    • Organizer
      大阪大学社会人教育プログラム (大阪)
    • Related Report
      2018 Annual Research Report
    • Invited
  • [Presentation] 全固体リチウムイオン電池のオペランドSTEM-EELS観察2018

    • Author(s)
      野村優貴,山本和生,平山司,齋藤晃
    • Organizer
      日本顕微鏡学会 第74回学術講演会 (久留米)
    • Related Report
      2018 Annual Research Report
  • [Presentation] 最先端電子顕微鏡法による全固体Liイオン電池のオペランド評価2018

    • Author(s)
      山本和生
    • Organizer
      荷電粒子ビームの工業への応用 学振132委員会主催 研究会 (東京)
    • Related Report
      2018 Annual Research Report
    • Invited
  • [Presentation] 透過型電子顕微鏡を用いた機能性デバイスのオペランド計測技術2018

    • Author(s)
      山本和生,穴田智史
    • Organizer
      JFCC研究発表会(東京(7/6)、名古屋(7/13)、大阪(7/20))
    • Related Report
      2018 Annual Research Report
  • [Presentation] Direct observation of electrochemical reactions in all-solid-state Li-ion batteries by electron holography and spatially-resolved TEM EELS2018

    • Author(s)
      Kazuo Yamamoto
    • Organizer
      Open Seminar at Brookhaven National Laboratory, USA
    • Related Report
      2018 Annual Research Report
    • Invited
  • [Presentation] Sample preparation technique with electric nano-shield films for in situ electron holography of battery materials2018

    • Author(s)
      Kazuo Yamamoto, Yuki Nomura, Tsukasa Hirayama, Koh Saitoh
    • Organizer
      International Microscopy Cngress 19 at Sydney in Australia
    • Related Report
      2018 Annual Research Report
    • Int'l Joint Research
  • [Presentation] In situ STEM-EELS observation in an all-solid-state lithium-ion battery2018

    • Author(s)
      Yuki Nomura, K. Yamamoto, T. Hirayama, K. Saitoh
    • Organizer
      International Microscopy Cngress 19 at Sydney in Australia
    • Related Report
      2018 Annual Research Report
    • Int'l Joint Research
  • [Presentation] in situ 電子線ホログラフィー観察のための漏れ電場遮断TEM試料作製技術の開発2017

    • Author(s)
      野村優貴,山本和生,斉藤晃,平山司
    • Organizer
      日本顕微鏡学会
    • Related Report
      2017 Annual Research Report
  • [Presentation] In situ and ex situ observations of solid-state electrochemical reactions in Li-ion batteries by advanced electron microscopy2017

    • Author(s)
      Kazuo Yamamoto, Tsukasa Hirayama
    • Organizer
      21st International Conference on Solid State Ionics
    • Related Report
      2017 Annual Research Report
    • Int'l Joint Research
  • [Presentation] In situ TEM observation of the charge/discharge reactions at LiCoO2/solid-electrolyte interfaces2017

    • Author(s)
      Yuki Nomura, Kazuo Yamamoto, Tsukasa Hirayama, Koh Saito
    • Organizer
      International Conference on Materials and Systems for Sustainability
    • Related Report
      2017 Annual Research Report
    • Int'l Joint Research
  • [Presentation] Direct visualization of solid-state electrochemical reactions in Li-ion batteries by spatially-resolved TEM-EELS2017

    • Author(s)
      Kazuo Yamamoto
    • Organizer
      3rd East-Asia Microscopy Conference
    • Related Report
      2017 Annual Research Report
    • Int'l Joint Research / Invited
  • [Presentation] 全固体Liイオン電池におけるLiイオン分布のnm分解能その場観察2017

    • Author(s)
      野村優貴,山本和生,斉藤晃,平山司
    • Organizer
      電池討論会
    • Related Report
      2017 Annual Research Report
  • [Book] 全固体電池の界面抵抗低減と作製プロセス,評価技術2020

    • Author(s)
      山本和生,野村優貴
    • Total Pages
      490
    • Publisher
      技術情報協会
    • ISBN
      9784861047800
    • Related Report
      2019 Annual Research Report
  • [Remarks] JFCC ナノ構造研究所 電子線ホログラフィーグループ

    • URL

      https://www.jfcc.or.jp/develop/nano-gr1.html

    • Related Report
      2019 Annual Research Report
  • [Remarks] 【プレスリリース】 次世代電池内部のリチウムイオンの動きを充放電中に可視化する技術を開発

    • URL

      http://www.jfcc.or.jp/25_press/r18_6.html

    • Related Report
      2018 Annual Research Report
  • [Remarks] 【プレスリリース】 世界初!次世代電池内部の リチウムイオンの動きを充放電中に可視化

    • URL

      http://www.imass.nagoya-u.ac.jp/

    • Related Report
      2018 Annual Research Report

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Published: 2017-04-28   Modified: 2021-02-19  

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