Accurate Interpretation of Electron Diffraction Data Acquired by Imaging Plates

Imaging Plate에 기록된 전자회절자료의 해석

  • Kim, Young-Min (Division of Nano-Material & Environmental Science, Korea Basic Science Institute) ;
  • Kim, Youn-Joong (Division of Nano-Material & Environmental Science, Korea Basic Science Institute)
  • 김영민 (한국기초과학지원연구원 나노환경연구부) ;
  • 김윤중 (한국기초과학지원연구원 나노환경연구부)
  • Published : 2003.09.01

Abstract

The Experimental calibration method has been investigated to correct d-spacing estimation and to identify phases in the electron diffraction data acquired by imaging plates. When the diffraction data from the imaging plate was corrected by the d-spacing calibration method with the radial intensity distribution plotting in this experiment, The accuracy of d-spacing estimation was significantly increased in errors of about 0.5%. The experimental calibration equation followed up the first order exponential decay function was derived from the trace of d-spacing deviation between the measured and the calculated values. It was applied to the analysis of d-spacing and the phase identification of the transitional phases formed from [001] gibbsite specimen by electron beam irradiation effect. In this case more accurate phase identification and d-spacing evaluation is possible for the transitional phases whose diffraction patterns are complicatedly superimposed. It is concluded that ${\chi}$-alumina, ${\gamma}$-alumina and ${\sigma}$-alumina are clearly identified as the major transitional phases formed from gibbsite by electron beam irradiation for 120 min.

Imaging plate에 기록된 전자회절 자료의 면간 거리 분석과 상동정시 나타나는 오차 요인들을 고찰하고 실험적인 보정방법을 도출하였다. 각각의 회절방향에 대한 radial intensity distribution plot과 실험적으로 도출된 면간 거리 보정식에 의해 전자회절 자료의 디지털 이미지에서 면간 거리 측정오차는 약 0.5%로 낮아짐을 알 수 있었다. Al 표준시료를 이용하여 imaging plate에 기록된 전자회절 자료의 면간 거리 편차 경향을 분석한 후 [001] gibbsite 시편에 동일한 실험적 보정을 수행하여 120분간의 전자빔 조사로부터 형성된 여러 전이 상들에 대한 면간 거리 측정 및 상 동정을 보다 정밀히 수행할 수 있었다. 그 결과, gibbsite로부터 형성된 주요 전이상들은 ${\chi}$-알루미나, ${\gamma}$-알루미나, ${\sigma}$-알루미나로 구성됨을 명확하게 동정할 수 있었다.

Keywords

References

  1. Akira T, Shindo D, Oikawa T: Sensitivity and fading characteristics of the 25 $\mu$m pixel size imaging plate for transmission electron microscopes, J Electron Microsc 45 : 232 235,1996 https://doi.org/10.1093/oxfordjournals.jmicro.a023437
  2. Lee YB, Kim YJ: An investigation of lattice parameter measurement of inorganic crystals by electron diffraction patterns, Korean J Electron Microscopy 29(1) : 75 81, 1999
  3. Mori N, Oikawa T, Harada Y, Miyahara J: Development of the imaging plate for the transmission electron microscope and its characteristics, J Electron Microsc 39 : 433 436, 1990
  4. Mori N, Oikawa T: The imaging plate and its application, Advances in Imaging and Electron Physic 99 : 241 288, 1998
  5. Oikawa T, Shindo D, Hiraga K: Fading characteristic of imaging plate for a transmission electron microscope, J Electron Microsc 43: 402 405,1994
  6. Ohno T, Sengoku M, Arii T: Measurements of electron beam damage for organic crystals in a high voltage electron microscope with image plates, Micron 33(4) :403 406, 2002 https://doi.org/10.1016/S0968-4328(01)00023-3
  7. Shindo D, Hiraga K, Oku T, Oilcawa T: Quantification in high resolution electron microscopy with the imaging plate, Ultramicroscopy 39(1/4): 50 57, 1991 https://doi.org/10.1016/0304-3991(91)90181-5
  8. Shibahara H, Numaguchi K, Kawasaki M, Talcizawa H: Quantification of oxygen vacancies in perovskite using a 300 kV HREM with an imaging plate, J Electron Microsc 44(4) : 174,1995
  9. Shibata T, Ikematsu Y, Shindo D: Elemental mapping using omega type energy filter and imaging plate, J Electron Microsc 50(1):29 31, 2001 https://doi.org/10.1093/jmicro/50.1.29
  10. Wyckoff WG: Crystal structure 2medit, 2: 78, 1964
  11. Zou X, Sukharev Y, Hovmoller S: Quantitative electron diffraction new features in the program system ELD, Ultramicroscopy 52 :436 444, 1993 https://doi.org/10.1016/0304-3991(93)90058-6