Details of the Researcher

PHOTO

Masashi Watanabe
Section
Institute for Materials Research
Job title
Professor
Degree

  • 博士（工学）（九州大学）

  • 修士（工学）（九州大学）

e-Rad No.
10304734

Research History 1

  • 2023/05 - Present
    Tohoku University　Institute for Materials Research Analytical Science　Professor

Education 3

  • Kyushu University　Faculty of Engineering　Department of Metallurgy

    1993/04 - 1996/03

  • Kyushu University　Faculty of Engineering　Department of Metallurgy

    1991/04 - 1993/03

  • Kyushu University　Faculty of Engineering　Department of Metallurgy

    1987/04 - 1991/03

Committee Memberships 3

  • Microscopy Society of America　Award Committee member for the Microscopy Society of America

    2021/01 - Present

  • Frontiers of Electron Microscopy for Materials Science (FEMMS)　Board member

    2019/01 - Present

  • Microscopy and Microanalysis (Journal)　Editor

    2016/05 - Present

Professional Memberships 3

  • Microanalysis Society

    - Present

  • Microscopy Society of America

    - Present

  • The Japanese Society of Microscopy

    - Present

Research Interests 1

  • Electron microscopy, Scanning transmission electron microscopy, Transmission electron microscopy, Scanning electron microscopy, Nanostructure analysis, Microanalysis, Materials Science, Metallurgy, Quantitative analysis, X-ray energy dispersive spectrometry, Electron energy-loss spectrimetry

Research Areas 1

  • Nanotechnology/Materials / Metallic materials /

Awards 1

  1. The Microanalysis Society Presidential Science Award

    2023/08　Microanalysis Society

Papers 12

  1. Grain boundary energy control in zinc aluminate nanoceramics

    Luis Sotelo Martin, Alexander Campos‐Quiros, Masashi Watanabe, Jeremy K. Mason, Paul C. M. Fossati, Blas P. Uberuaga, Ricardo H. R. Castro

    Journal of the American Ceramic Society　108　(5)　2025/01/22

    Publisher: Wiley

    DOI： 10.1111/jace.20383 　

    ISSN： 0002-7820

    eISSN： 1551-2916

    More details Close

    Abstract This study investigates the grain boundary energy dependence on segregated dopants in nanocrystalline zinc aluminate ceramics. Atomistic simulations of Σ3 and Σ9 grain boundaries showed that trivalent ions of varying ionic radii [Sc3+ (74.5 pm), In3+ (80.0 pm), Y3+ (90.0 pm), and Nd3+ (98.3 pm)] have a tendency to segregate to both interfaces, with Y3+ presenting the highest segregation potentials. The connection between segregation and the reduction of interfacial energies was explored by measuring the grain boundary energy on nanoceramics fabricated via high‐pressure spark plasma sintering (HP‐SPS) using differential scanning calorimetry (DSC). The results revealed that Y3+ doping at 0.5 mol% reduces the grain boundary energy in zinc aluminate nanoceramics from 1.1–1.3 J/m2 to 0.6–0.8 J/m2; the range correlates with the observed size dependence of the excess energy, with higher values observed for the smaller grain sizes (∼17 nm). The noted decrease in interfacial energies for doped samples suggests it is indeed possible to alter the stability of zinc aluminate grain boundaries via dopant segregation.

  2. Correlation between grain-boundary segregation behaviors of calcium and yttrium and enhanced fracture toughness in magnesium aluminate spinel

    Alexander Campos-Quiros, Metri Zughbi, Animesh Kundu, Masashi Watanabe

    Journal of Materials Science　60　(4)　1826-1852　2025/01/03

    Publisher: Springer Science and Business Media LLC

    DOI： 10.1007/s10853-024-10569-9 　

    ISSN： 0022-2461

    eISSN： 1573-4803

  3. Quantitative analysis of grain boundary segregation and fracture behavior in Ca-doped magnesium aluminate spinel

    Alexander Campos-Quiros, Metri Zughbi, Animesh Kundu, Masashi Watanabe

    Journal of Materials Science　59　(36)　16862-16883　2024/09/13

    Publisher: Springer Science and Business Media LLC

    DOI： 10.1007/s10853-024-10171-z 　

    ISSN： 0022-2461

    eISSN： 1573-4803

  4. Instrument Optimization of a High-Energy Electron Energy-loss Spectrometry System in an Aberration-Corrected Scanning Transmission Electron Microscope

    Masashi Watanabe, Alexander Campos-Quiros, Giulio Guzzinati, Pirmin Kükelhan, Volker Gerheim, Martin Linck, Heiko Müller, Max Haider, Thomas F Hoffman, Kotaro Sakaguchi, Masaki Mukai, Thomas Isabell, Naoki Shimura, Hidetaka Sawada

    Microscopy and Microanalysis　30　(Supplement_1)　2024/07/24

    Publisher: Oxford University Press (OUP)

    DOI： 10.1093/mam/ozae044.685 　

    ISSN： 1431-9276

    eISSN： 1435-8115

  5. EELS Quantification of Ca and Y Segregation Behaviors in Magnesium Aluminate Spinel

    Alexander Campos-Quiros, Animesh Kundu, Masashi Watanabe

    Microscopy and Microanalysis　30　(Supplement_1)　2024/07/24

    Publisher: Oxford University Press (OUP)

    DOI： 10.1093/mam/ozae044.684 　

    ISSN： 1431-9276

    eISSN： 1435-8115

  6. From Silver Nanoparticle to Thin Films Produced by Pulsed Laser Deposition: Effects of Ar Gas Pressure and Substrate Surface Free Energy

    C S C Nogueira, A C Agra, D F Franceschini, M Watanabe, Y T Xing

    Microscopy and Microanalysis　30　(Supplement_1)　2024/07/24

    Publisher: Oxford University Press (OUP)

    DOI： 10.1093/mam/ozae044.636 　

    ISSN： 1431-9276

    eISSN： 1435-8115

  7. Application of ζ-factor Microanalysis to Quantify Grain Boundary Enrichment in Eu-doped B6O

    C J Marvel, K D Behler, J C LaSalvia, R A Haber, M Watanabe, M P Harmer

    Microscopy and Microanalysis　30　(Supplement_1)　2024/07/24

    Publisher: Oxford University Press (OUP)

    DOI： 10.1093/mam/ozae044.092 　

    ISSN： 1431-9276

    eISSN： 1435-8115

  8. High-resolution electron microscopy study of particle dispersion and precipitation in a nanostructured Al–2%Fe alloy

    Jorge M. Cubero-Sesin, Masashi Watanabe, Zenji Horita

    Journal of Materials Science　59　(14)　5787-5804　2024/04/01

    Publisher: Springer Science and Business Media LLC

    DOI： 10.1007/s10853-024-09570-z 　

    ISSN： 0022-2461

    eISSN： 1573-4803

  9. Physical and Numerical Modeling of Micro-extrusion Behavior of AA3xxx Aluminum Alloy in Cold Roll Bonding

    Mahsa Navidirad, John E. Plumeri, Natasha Vermaak, Masashi Watanabe, Wojciech Z. Misiolek

    Lecture Notes in Mechanical Engineering　291-298　2023/08/23

    Publisher: Springer Nature Switzerland

    DOI： 10.1007/978-3-031-41023-9_30 　

    ISSN： 2195-4356

    eISSN： 2195-4364

  10. Installation of New Systems for High-Energy Electron Energy-loss Spectrometry in an Aberration-Corrected Scanning Transmission Electron Microscope

    Masashi Watanabe, Giulio Guzzinati, Pirmin Kükelhan, Volker Gerheim, Martin Linck, Heiko Müller, Max Haider, Thomas F Hoffman, Thomas Isabell, Naoki Shimura, Hidetaka Sawada

    Microscopy and Microanalysis　29　(Supplement_1)　416-417　2023/07/22

    Publisher: Oxford University Press (OUP)

    DOI： 10.1093/micmic/ozad067.196 　

    ISSN： 1431-9276

    eISSN： 1435-8115

  11. EELS Spectrum Imaging of Ca Segregation at Grain Boundaries in Magnesium Aluminate Spinel

    Alexander Campos-Quiros, Animesh Kundu, Masashi Watanabe

    Microscopy and Microanalysis　29　(Supplement_1)　407-408　2023/07/22

    Publisher: Oxford University Press (OUP)

    DOI： 10.1093/micmic/ozad067.191 　

    ISSN： 1431-9276

    eISSN： 1435-8115

  12. Development of an Automated Reciprocal-Space Navigator in a JEOL FEMTUS Platform

    Surui Huang, Brian Chen, Aparna Bharati, Martin P Harmer, Masashi Watanabe

    Microscopy and Microanalysis　29　(Supplement_1)　728-729　2023/07/22

    Publisher: Oxford University Press (OUP)

    DOI： 10.1093/micmic/ozad067.359 　

    ISSN： 1431-9276

    eISSN： 1435-8115

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Misc. 3

  1. Quantification of Oxide Materials Using a Newly Installed CEOS Energy Filtering and Imaging Device in an Aberration-corrected Scanning Transmission Electron Microscope JEM-ARM200CF Peer-reviewed

    M. Watanabe, G. Guzzinati, P. Kükelhan, V. Gerheim, M. Linck, H. Müller, M. Haider, T.F Hoffman, T. Isabell, N. Shimura, H. Sawada

    Proc. International Microscopy Congress 20　2023/09

  2. EELS Characterization of Y- and Ca-Doped Magnesium Aluminate Spinel Invited

    A. Campos-Quiros, A. Kundu, M. Watanabe

    Proc. International Materials Research Congress 2023　2023/08

  3. A High-Energy Electron Energy-loss Spectrometry System for Advanced Analytical Electron Microscopes Invited Peer-reviewed

    M. Watanabe, G. Guzzinati, P. Kükelhan, V. Gerheim, M. Linck, H. Müller, M. Haider, T.F Hoffman, T. Isabell, N. Shimura, H. Sawada

    Proc. International Workshop on Advanced and In-situ Microscopies of Functional Nanomaterials and Devices (IAMNano) 2023　61-61　2023/06

Books and Other Publications 1

  1. Transmission electron microscopy : diffraction, imaging, and spectrometry

    Carter, C. Barry, Williams, David B, (Eds). Chapter author, Masashi Watanabe

    Springer　2016/09/05

    ISBN: 3319266497

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    2nd edition will be published in 2024

Presentations 23

  1. 走査透過電子顕微鏡STEMによる材料の 定量評価の基礎と応用

    渡辺万三志

    金属材料研究所2024年度テクニカルセンター 職員研修会　2024/12/10

  2. 高エネルギー電子線損失分光システムの開発と期待される応用研究

    渡辺万三志

    日本顕微鏡学会分析電顕討論会　2024/12/05

  3. 透過電子顕微鏡によるX線分析の基礎と応用

    渡辺万三志

    日本顕微鏡学会電顕大学　2024/11/21

  4. Quantitative Analysis of Ca and Y Segregation Behaviors in Magnesium Aluminate Spinel

    A. Campos-Quiros, A. Kundu, M. Watanabe

    MS&T 2024　2024/10/07

  5. Development and Applications of a High-Energy Electron Energy-loss Spectrometry System in an Aberration-Corrected Scanning Transmission Electron Microscope

    M. Watanabe, A. Campos-Quiros, G. Guzzinati, P. Kükelhan, V. Gerheim, M. Linck, H. Müller, M. Haider, T.F. Hoffman, K. Sakaguchi, M. Mukai, T. Isabell, N. Shimura, H. Sawada

    Frontiers of Electron Microscopy and Materials Science (FEMMS) 2024　2024/09/30

  6. From Silver Nanoparticle to Thin Films Produced by Pulsed Laser Deposition: Effects of Ar Gas Pressure and Substrate Surface Free Energy

    C.S.C. Nogueira, A.C. Agra, D.F. Franceschini, M. Watanabe, Y.T. Xing

    Annual meeting of Microscopy & Microanalysis 2024　2024/08/01

  7. Instrument Optimization of a High-Energy Electron Energy-loss Spectrometry System in an Aberration-Corrected Scanning Transmission Electron Microscope

    M. Watanabe, A. Campos-Quiros, G. Guzzinati, P. Kükelhan, V. Gerheim, M. Linck, H. Müller, M. Haider, T.F. Hoffman, K. Sakaguchi, M. Mukai, T. Isabell, N. Shimura, H. Sawada

    Annual meeting of Microscopy & Microanalysis 2024　2024/07/30

  8. EELS Quantification of Ca and Y Segregation Behaviors in Magnesium Aluminate Spinel

    A. Campos-Quiros, A. Kundu, M. Watanabe

    Annual meeting of Microscopy & Microanalysis 2024　2024/07/30

  9. Application of ζ-factor Microanalysis to Quantify Grain Boundary Enrichment in Eu-doped B6O

    C.J. Marvel, K.D. Behler, J.C. LaSalvia, R.A. Haber, M. Watanabe, M.P. Harmer

    Microscopy and Microanalysis 2024　2024/07/29

  10. Installation of New Systems for High-Energy Electron Energy-loss Spectrometry in an Aberration-Corrected Scanning Transmission Electron Microscope

    Masashi Watanabe

    Annual meeting of Microscopy & Microanalysis 2024　2024/07/24

  11. Energy Dispersive X-ray Spectroscopy and Nanoanalysis

    Masashi Watanabe

    Arizona State University Winter School for Electron Microscopy　2024/01/09

  12. Fundamentals of X-ray Energy Dispersive Spectrometry

    Masashi Watanabe

    Arizona State University Winter School for Electron Microscopy　2024/01/08

  13. Microscopy Hacks for Materials Characterization Invited

    Masashi Watanabe

    145th IMR Workshop　2023/12/06

  14. Analytical Electron Microscopy: 2. Electron Energy-Loss Spectrometry (EELS) Invited

    Masashi Watanabe

    5th High-Resolution Electron Microscopy and Nanofabrication School at Universidade Federal Fluminense　2023/10/20

  15. Analytical Electron Microscopy: 1. X-ray Energy Dispersive Spectrometry (XEDS) Invited

    Masashi Watanabe

    5th High-Resolution Electron Microscopy and Nanofabrication School at Universidade Federal Fluminense　2023/10/16

  16. Quantification of Oxide Materials Using a Newly Installed CEOS Energy Filtering and Imaging Device in an Aberration-corrected Scanning Transmission Electron Microscope JEM-ARM200CF Invited

    Masashi Watanabe

    International Microscopy Congress 20　2023/09/14

  17. Installation of New Systems for High-Energy Electron Energy-loss Spectrometry in an Aberration-Corrected Scanning Transmission Electron Microscope Invited

    Masashi Watanabe

    Microscopy & Microanalysis 2023　2023/07/24

  18. A High-Energy Electron Energy-loss Spectrometry System for Advanced Analytical Electron Microscopes Invited

    Masashi Watanabe

    International Workshop on Advanced and In-situ Microscopies of Functional Nanomaterials and Devices (IAMNano) 2023　2023/06/30

  19. Current Status of Electron Microscopy Studies in the United States of America Invited

    Masashi Watanabe

    Annual Meeting of Japanese Microscopy Society　2023/06/26

  20. Crystalline Structure and Composition Analysis at Atomic Levels by Atomic-Resolution Scanning Transmission Electron Microscopy

    Masashi Watanabe

    Workshop on the Latest Crystal Characterization Approaches, Japanese Association for Crystal Growth　2023/06/23

  21. Exploration of Single-Atom Characterization and Quantification in Analytical Electron Microscopy Invited

    Masashi Watanabe

    A Chesapeake Microscopy & Microanalysis Society Event "Dale-abration: Celebrating Dale Newbury’s 50 years at NIST"　2023/02/15

  22. Energy Dispersive X-ray Spectroscopy and Nanoanalysis Invited

    Masashi Watanabe

    Arizona State University Winter School for Electron Microscopy　2023/01/10

  23. Fundamentals of X-ray Energy Dispersive Spectrometry Invited

    Masashi Watanabe

    Arizona State University Winter School for Electron Microscopy　2023/01/09

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Research Projects 9

  1. MRI: Acquisition of a Plasma Focused Ion Beam System for Dynamic In-situ Micro-Mechanical Testing Over Cryogenic and Elevated Temperatures

    Masashi Watanabe

    Offer Organization: National Science Foundation

    System: MRI

    2022/08 - 2025/07

  2. A Systematic Dopant-selection Strategy for Advanced Manufacturing of High Strength Transparent Magnesium Aluminate Spinel

    Masashi Watanabe

    Offer Organization: National Science Foundation

    System: CMMI

    2020/08 - 2025/07

  3. MRI: Development of a high energy-loss electron spectrometry system with improved detection sensitivity for an advanced electron microscope

    Masashi Watanabe

    Offer Organization: National Science Foundation

    System: MRI

    2020/08 - 2024/07

  4. High Angular Resolution Electron Channeling X-ray Spectroscopy for Radiation-Induced Local Disordering in Magnesium Aluminate Spinel Compounds

    MATSUMURA Syo, YASUDA Kazuhiro, KANEKO Kenji

    Offer Organization: Japan Society for the Promotion of Science

    System: Grants-in-Aid for Scientific Research

    Category: Grant-in-Aid for Scientific Research (B)

    Institution: Kyushu University

    2000 - 2002

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    This project aimed to promote basic understanding of radiation-induced structural change in magnesium aluminate spinel compounds (MgO-nAl_2O_3), which are drawing much attention as candidates for radiation resistant materials in future nuclear programs. To this end, we developed a new experimental technique of transmission electron microscopy to analyze quantitatively local atomic configuration. Then the technique, which is called as high angular resolution electron channeling x-ray spectroscopy (HARECXS), was applied to MgO-nlAl_2O_3 irradiated with 1 MeV Ne^+ or 500 keV He^+ ions to disclose ion displacements involved in structural disordering. The project started in FY 2000 with examination of HARECXS as a practical tool to locate lattice ions in spinel compounds. In the procedure of HARECXS, characteristic x-ray emission from an electron-illuminated local specimen area is measured as a function of the electron beam direction with high angular resolution. The theoretical arguments based on the dynamical electron diffraction and inelastic scattering clearly showed that the HARECXS profiles of x-ray intensity variations thus obtained sensitively depends on not only ion-configuration but also specimen thickness and Debye-Waller factors. From the profiles, one can determine accurately the occupation probabilities of constituent ions on specific sites in the crystal lattice. In the next two years, the research work was mostly focused on partially ordered states in as-grown crystals and evolution of structural disordering under ion irradiation. In MgO-nAl_2O_3 with n=1.0 and 2.4, most Al^<3+> lattice-ions occupy the octahedral (VI) sites with 6-fold coordination, while Mg^<2+> lattice-ions reside on both the tetrahedral (IV) and the octahedral (VI) sites. The structural vacancies are enriched in the IV-sites. Irradiation with 1 MeV Ne^+ ions causes disordering of cation configuration in the pre-peak damaged range without any defect cluster formations, while it displaces not only cations but also anions from their crystallographic sites and forms small defect clusters in the peak-damaged area. It is suggested that the structural vacancies due to nonstoichiometry for n=2.4 take part in recombinations with displaced ions. Irradiation with 500 keV He^+ causes less disordering than 1 MeV Ne^+ irradiation does. A higher ionizing rate under the former condition is ascribed to the less disordering tendency, since recovery or reordering is more promoted with ionization-enhanced migration of displaced ions.

  5. 分析電子顕微鏡による薄膜試料定量分析の一般化およびオンライン化に関する研究

    渡辺 万三志

    Offer Organization: 日本学術振興会

    System: 科学研究費助成事業

    Category: 奨励研究(A)

    Institution: 九州大学

    2001 - 2001

  6. Quantitative Analysis of Local Structure in High Tc Superconductors by Energy Filtering Convergent-Beam Electron Diffraction

    TOMOKIYO Yoshitsugu, KANEKO Kenji, MATSUMURA Syo

    Offer Organization: Japan Society for the Promotion of Science

    System: Grants-in-Aid for Scientific Research

    Category: Grant-in-Aid for Scientific Research (B)

    Institution: Kyushu University

    1999 - 2001

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    Improvement of the critical current density, Jc is one of the important subjects for practical application of high Tc superconductor YBa_2Cu_3O_<7-x> (YBCO). The crystal structure and superconducting properties sensitively depend on oxygen concentration that easily changes depending on atmosphere. Convergent beam electron diffraction has been used to extract information on oxygen concentration and/or charge distribution and/or oxygen. The observed diffraction intensities are analyzed with the dynamical theory of electron diffraction. Large angle CBED patterns were observed with a FE-TEM : JEM-2010FEF equipped with an energy filter of omega-type. The accuracy of the measured oxygen concentration depends on the reliability of temperature factors (B-factors) used in the analysis. An actual temperature of a specimen under electron beam irradiation is estimated with anisotropic temperature factors. The local oxygen concentration determined vary from point to point. This result shows that oxygen concentration is not uniform in YBCO and oxygen deficiency fluctuates locally. No super lattice spots were observed in [001] diffraction patterns indicating that oxygen deficiency occurs with random depopulation of oxygen along a Cu-O chain. Fluctuation of oxygen deficiency is the most probable reason for the peak-effect in YBCO. Information on charge distribution on CuO_2 and CuO planes are extracted by more precise analysis of CBED patterns.

  7. 電子分光電子顕微鏡法によるSi中の酸素析出物の微細構造評価

    友清 芳二, 奥山 哲也, 渡辺 万三志

    Offer Organization: 日本学術振興会

    System: 科学研究費助成事業

    Category: 特定領域研究(A)

    Institution: 九州大学

    1999 - 1999

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    目的:半導体デバイスプロセスの不純物ゲッタリング効果改善のための手がかりをつかむために、(1)不純物ゲッタリングシンクとしてSiウエハー中に導入された板状酸素析出物(SiO2)周辺の格子歪み分布を詳細に調べる。(2)Siウエハー裏面にCVD法でPoly-Siを被着させた場合の界面近傍のSi格子の歪み分布と比較検討を行う。 方法:新型のナノプローブ電子分光型電子顕微鏡(電界放射電子銃、Ω型エネルギーフィルター装備)を使用して、収束電子回折(CBED : Convergent Beam Electron Diffraction)の高次ラウエゾーン(HOLZ : Higher Order Laue Zone)の回折線(HOLZ線)を観察する。 結果:(1)酸素析出物の板面に垂直な方向(母相Siの[010]方向)には圧縮歪みが、板面と平行な方向(母相の[100]方向)には引っ張り歪みが存在することがわかった。(2)HOLZ線の分裂間隔および回折ディスクに現れる消衰縞の形状変化から、析出物とSi母相界面近傍でのSi格子の湾曲を定量的に評価することができた(板面から0.5μm離れた地点で20〜30mrad)。(3)ウエハー裏面に被着させたポリSiとの界面近傍の格子歪みと比べると、析出物周辺の方が歪み量は約1桁大きい。これにより、ウエハー裏面に被着させたポリSiとの界面よりも酸素析出物界面の方が不純物ゲッタリング効果が高いことを説明できた。これは半導体デバイスプロセスにおける不純物ゲッタリング効果改善のための重要な手がかりを与えてくれる。(4)新型のナノプローブ電子分光型電子顕微鏡を使用すると、従来の分析電顕に比べて回折の空間分解能(プローブ径:1〜2nm)は1桁改善され、試料は1.5倍厚いもの(Siでは約450nm)が使用できることを証明した。

  8. ELECTRON SPECTROSCOPIC MICROSCOPY IN MATERIALS SCIENCE

    TOMOKIYO Yoshitsugu, YASUDA Kazuhiro, WATANABE Masashi, MATSUMURA Syo

    Offer Organization: Japan Society for the Promotion of Science

    System: Grants-in-Aid for Scientific Research

    Category: Grant-in-Aid for Scientific Research (B).

    Institution: KYUSHU UNIVERSITY

    1998 - 1999

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    We investigated performance and applicability of the new energy filtering transmission electron microscope which was recently installed in Kyushu University (KU), and compared with those of microscopes in Max-Planck Institute and Arizona State University. The new microscope in KU has a field emission gun of Shottcky type and an imaging filter of omega-type. The imaging energy spectrometer enables us to use the information included in the inelastically scattered electrons and to improve the contrasts of magnified images as well as diffraction patterns. (1) Electron spectroscopic imaging : By changing a position and a width of energy selecting slit, we can select the energy of electrons to be used for imaging. The contrasts of filtered zero-loss images are improved in the multi-beam resolution images as well as bright-field or dark-field images, although the size and position of an objective apertureare are different in these imaging modes. Images of coherent precipitates, stacking faults and dislocations in metals and alloys are sharp in filtered zero-loss images. The effect of energy filtering is pronounced in thicker spsecimen and lower accelerating voltage. A filtered core-loss (inner-shell ionization) image includes information on composition of a particular element in material (element mapping). Thin oxide layer in Si water is visualized in a two-dimensional scale in the filtered K-loss oxygen image. (2) Electron spectroscopic diffraction : Energy filtered diffraction patterns are obtained by changing the energy slit in the diffraction mode. Inelastically scattered electrons are responsible for the background in diffraction patterns. The background is well eliminated and contrast is much improved in the zero-loss filtered diffraction patterns. We can observe weak diffraction spots or diffuse maxima in the selected-area diffraction patters, and weak diffraction lines of a higher order Laue zone in convergent electron diffraction patters.

  9. 電子分光電子顕微鏡法によるSi中の酸素析出物の微細構造評価

    友清 芳二, 奥山 哲也, 渡辺 万三志

    Offer Organization: 日本学術振興会

    System: 科学研究費助成事業

    Category: 特定領域研究(A)

    Institution: 九州大学

    1998 - 1998

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    昨年度はsiウエハー中に1000℃で形成される板状酸素析出物SiO_2が非晶質ではなく、α-クリストバライト型結晶であることを明らかにした。この析出物はSiデバイスプロセス中の不純物ゲッタリングシンクとして導入されたものである。ゲッタリング機構を解明するために、今年度はその板状酸素析出物周辺の格子歪みを最新鋭の電子分光型電子顕微鏡を使って調べた。局所的歪みを定量的に評価するために、収束電子回折(CBED)の高次ラウエゾーン(HOLZ)線を利用した。新しい電子顕微鏡は電界放射電子銃を備えているので輝度が高く、照射プロープを従来より一桁細く絞ってもHOLZ線を観察できる。さらに、Ω型エネルギー分光装置を内蔵しているので電子の非弾性散乱成分を除去できる。そうするとバックグランド強度が低下し、従来に比べて厚い試料からでも明瞭なHOLZ線が得られる。また、記録装置としてイメージングプレートやスロースキャンCCDを使うと微弱な回折強度も記録できる。以上の結果、厚さ450nmのSiに直径1〜2nmのプローブを照射しても格子定数を測定できるような明瞭なHOLZ線を観察することができた。Si母相の(001)面に平行な板状酸素析出物の周辺で[510]晶帯軸入射CBEDパターンを観察した結果、板面に垂直方向にはSi格子が圧縮応力を受け正方晶に歪んでいること、板面から垂直方向に0.2μm離れた所ではC軸長が約0.5%収縮していること、0.1μm離れた所では歪み0.01%以下であることがわかった。回折線の分裂から見積もった最大格子湾曲は約5度であった。

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Teaching Experience 6

  1. MAT427 Advanced Scanning Electron Microscopy　Lehigh Univeristy

  2. MAT203 Structure at Nanoscale　Lehigh University

  3. MAT405 Advanced kinetics　Lehigh University

  4. MAT334 Electron Microscopy and Microanalysis　Lehigh University

  5. MAT423 Advanced Transmission Electron Microscopy　Lehigh University

  6. MAT203 Structure at Nanoscale　Lehigh University

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