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Research

Keywords

Electron Microscopy, Electron Energy-Loss Spectroscopy, Material Characterization

- Material evaluation using transmission electron microscopy (TEM), scanning transmission electron microscopy (STEM), and electron energy-loss spectroscopy (EELS).
- Automated measurement and analysis of STEM/TEM/EELS using scripting with DigitalMicrograph (Gatan Inc.).
- Unsupervised machine learning techniques for advanced electron microscopy (e.g., 4D-STEM).

PublicationsNIMS affiliated publications since 2004.

Books
    Proceedings
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          Society memberships

          日本顕微鏡学会

          Awards

          • 日本電子顕微鏡学会 論文賞 (1991),応用物理学会賞B(奨励賞) (1997),日本電子顕微鏡学会 奨励賞 (2001),日本電子顕微鏡学会 瀬藤賞/学会賞 (2008),文部科学大臣表彰 科学技術賞(研究部門)(2009) ()
          Center for Basic Research on Materials
          Title

          Development and Application of Transmission Electron Microscopy for Materials Characterization

          Keywords

          Transmission Electron Microscopy (TEM), Scanning Transmission Electron Microscopy (STEM), Electron Energy-Loss Spectroscopy (EELS), 4D-STEM, Monochromator, Scripting

          Overview

          Advanced transmission electron microscopy (TEM) allows for various microstructural analyses, such as atomic imaging, crystallographic diffractometry, and elemental analysis. The development of spherical aberration correctors, monochromators, and high-sensitivity detectors has made it possible to evaluate and analyze samples at the atomic level. We have developed TEM techniques for high-precision and high-sensitivity measurements, as well as data analysis methods. Using STEM-EELS, we have successfully observed atomic arrangements for individual elements, single-atom dopants, and atomic displacements on the picometer scale. We are pioneering analyses that incorporate knowledge of electron diffraction by combining 4D-STEM with unsupervised machine learning. By combining these various TEM techniques to evaluate microstructures with unique physical properties and superior performance, we aim to strengthen innovation in materials science.

          Novelty and originality

          ● High-precision, high-sensitivity, and quantitative structural analysis using advanced STEM imaging with custom software. In particular, this technique enables the detection of dopants, the observation of atomic defects, and the analysis of atomic positions with picometer precision. Additionally, it supports low-acceleration, high-resolution TEM and high-energy-resolution, high-spatial-resolution STEM using a monochromator.
          ● Combination of 4D-STEM and unsupervised machine learning custom software (e.g., non-negative matrix factorization). Development of automated measurement using DigitalMicorgraph (Gatan Inc.) scripts.

          Details

          image

          High-Resolution, High-Sensitivity Crystal Structure Observation Using STEM:
          We used STEM to observe the crystal sites occupied by single-atom dopants in Eu-doped SiAlON phosphors synthesized by Hirosaki et al. at NIMS. Although these atoms cannot be detected in conventional TEM images, Eu atoms are visible in high signal-to-noise ratio (SNR) images obtained through multiple measurements using annular dark-field (ADF) imaging. Through simulation-based analysis, we also identified the TEM sample thickness and imaging conditions, thereby determining the positions of the single-atom Eu dopants.
          Quantitative measurement of ADF images provides information regarding atomic number Z. We found that as Z increases and the acceleration voltage decreases, the relationship deviates from the so-called power law for Z. By performing quantitative comparisons with simulations, it is also possible to identify atoms in ADF images.

          image

          Microstructural Analysis Using 4D-STEM and Machine Learning:
          The technique of acquiring a large number of diffraction patterns while scanning the STEM probe is called 4D-STEM. We first observed atomic resolution in 2011. In 2021, we were the first to combine non-negative matrix factorization (NMF), a machine learning technique, with 4D-STEM. Furthermore, we independently developed a clustering method based on the similarity of diffraction patterns and used it to analyze the nanosized crystalline structures precipitated in metallic glasses through heat treatment (2024). Using these methods, we have also succeeded in polarity mapping of single-layer MoS₂ (2025). Some of our scripts for DigitalMicrograph (Gatan Inc.) are available on our group’s website and on GitHub.

          Summary

          We can analyze atomic structures with high precision and sensitivity using STEM, TEM, and EELS techniques with custom software, including machine learning.
          We can analyze dopants, defects, and variations in atomic positions at the picometer level with atomic resolution.
          Combining various TEM measurement techniques allows us to solve materials development problems and gain new insights.

          この機能は所内限定です。
          この機能は所内限定です。

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