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Accurate crystal structure analysis by quantitative high-resolution electron microscopy

Research Project

Project/Area Number 05402048
Research Category

Grant-in-Aid for General Scientific Research (A)

Allocation TypeSingle-year Grants
Research Field Physical properties of metals
Research InstitutionTohoku University

Principal Investigator

HIRAGA Kenji  Institute for Materials Research, Professor, 金属材料研究所, 教授 (30005912)

Co-Investigator(Kenkyū-buntansha) OHNISHI Naoyuki  Institute for Materials Research, Assistant Researcher, 金属材料研究所, 助手 (60201977)
SHINDO Daisuke  Institute for Advanced Materials Processing, Professor, 素材工学研究所, 教授 (20154396)
Project Period (FY) 1993 – 1995
Project Status Completed (Fiscal Year 1995)
Budget Amount *help
¥29,000,000 (Direct Cost: ¥29,000,000)
Fiscal Year 1995: ¥1,300,000 (Direct Cost: ¥1,300,000)
Fiscal Year 1994: ¥3,700,000 (Direct Cost: ¥3,700,000)
Fiscal Year 1993: ¥24,000,000 (Direct Cost: ¥24,000,000)
Keywordshigh-resolution elect electron microscopy / crystal structure analysis / quantitative image analysis / CCD camera / image processing / zeorite / 精密結晶構造解析 / 残差因子 / 精密構造解析
Research Abstract

We have tried to establish the process of crystal structure analysis with high-resolution electron microscopy and electron diffraction. High-resolution electron micrographs and electron diffraction patterns are measured as quantitative data by a slow-scan CCD (charge-coupled device) camera and IP (imaging-plate) attached to a 400 kV transmission electron microscope (JEM-4000EX) having a resolution of 0.17nm. The main purpose of this work has been to develop a procedure of crystal structure analysis with computer work of the quantitative data of high-resolution micrographs and electron diffraction patterns. Our results are summarized as the follows.
1. In order to try accurate crystal structure analysis of a Tl_2Ba_2CuO_y superconducting oxide, a residual index between observed quantitative images and simulated images was introduced. From minimizing the residual index with some parameters of thickness and defocus values, partial occupancy of metal atoms can be quantitatively evaluated and deficient oxygen atom positions can be detected.
2. By using high-sensitive properties of the CCD camera, we observed high-resolution electron microscopic images of zeorites introduced with Ni, which are extremely weak for electron beam. From image processing and image analysis of the high-resolution electron micrographs, accurate structure analysis of Ni atoms can be evaluated.
3. We demonstrate herein the application of a slow-scan CCD camera for improvement in the experimental resolution of contrast details in the synthetic zeorite structure ZSM-5 (MFI). The improvement in the amount and quality of structural detail through the use of the CCD camera is also shown by a comparison of a Fourier synthesis, made by using the observed electron diffraction intensities. R-factors based on the normalized diffraction intensities have been employed to evaluate the result of the structure analysis.

Report

(4 results)
  • 1995 Annual Research Report   Final Research Report Summary
  • 1994 Annual Research Report
  • 1993 Annual Research Report
  • Research Products

    (8 results)

All Other

All Publications (8 results)

  • [Publications] N. Ohnishi and K. Hiraga: "Slow-scan CCD casmera analysis of electron diffraction and high-resolution micrographs of feorite TPA/ZSM-5" Journal of Electron Microscopy. 45. 85-92 (1996)

    • Description
      「研究成果報告書概要(和文)」より
    • Related Report
      1995 Final Research Report Summary
  • [Publications] N. Ohnishi and K. Hiraga: "Transmission electron microscopy of zeorite TPA/ZSM-5 using a slow-scan CCD camera" Materials Science and Engineering. (印刷中).

    • Description
      「研究成果報告書概要(和文)」より
    • Related Report
      1995 Final Research Report Summary
  • [Publications] N.Ohnishi and K.Hiraga: "Slow-scan CCD camera analysis of electron diffraction and high-resolution micrographs of zeorite TPA/ZSM-5" Journal of Electron Microscopy. 45. 85-92 (1996)

    • Description
      「研究成果報告書概要(欧文)」より
    • Related Report
      1995 Final Research Report Summary
  • [Publications] N.Ohnishi and K.Hiraga: "Transmission electron study of zeorite TPA/ZSM-5 using a slow-scan CCD camera" Materials Science and Engineering. (in press).

    • Description
      「研究成果報告書概要(欧文)」より
    • Related Report
      1995 Final Research Report Summary
  • [Publications] N.Ohnishi and K.Hiraga: "Slow-scan CCD camera analysis of electron deffraction and high-resolution micrographs of georite TPA/ZSM-5" Jounal of Electron Microscopy. 45. 85-92 (1996)

    • Related Report
      1995 Annual Research Report
  • [Publications] N.Ohnishi and K.Hiraga: "Transmission electron microscopy study of georite TPA/ZSM-5 using a slow-scan CCD camera" Materials Science and Engineering. (印刷中).

    • Related Report
      1995 Annual Research Report
  • [Publications] D.Shindo: "Quantitative High-Resolution Electron Microscopy with a Residual Index" Proc.ICEM 13-PARIS. 359-360 (1994)

    • Related Report
      1994 Annual Research Report
  • [Publications] T.Oikawa: "Fading Characteristic of Imaging Plate for a Trans mission Electron Microscope" J.Electron Microsc.43. 402-405 (1994)

    • Related Report
      1994 Annual Research Report

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Published: 1993-04-01   Modified: 2016-04-21  

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