Three-dimensional Structure Analysis of $SmZn_{0.67}Sb_2$ by Transmission Electron Microscopy

투과전자현미경을 이용한 $SmZn_{0.67}Sb_2$의 3차원적 구조 분석

  • Kim, Jin-Gyu (Division of Nano-Material & Environment Science, Korea Basic Science Institute) ;
  • Kang, Sung-Kwon (Dept. of Chemistry, Chungnam National University) ;
  • Kim, Wan-Cheol (Dept. of Chemistry, Chungnam National University) ;
  • Kim, Youn-Joong (Division of Nano-Material & Environment Science, Korea Basic Science Institute)
  • 김진규 (한국기초과학지원연구원 나노환경연구부 전자현미경팀) ;
  • 강성권 (충남대학교 화학과) ;
  • 김완철 (충남대학교 화학과) ;
  • 김윤중 (한국기초과학지원연구원 나노환경연구부 전자현미경팀)
  • Published : 2004.12.01

Abstract

The three-dimensional (3D) structure of an inorganic crystal, $SmZn_{0.67}Sb_2$ (space group P4/nmm, $a=4.26{\AA}\;and\;c=10.37{\AA}$) was solved by electron crystallography. High resolution electron microscopy (HREM) images from 3 different major zone axes and selected-area electron diffraction patterns from 16 different zone axes were combined to obtain a 3D information. A crystallographic image processing (CIP) of HREM images was used for more accurate determination of the crystal structure. As a result of this electron crystallography, average phase errors (${\Phi}_{res}$) of [001], [100] and [110] HREM images are $17.0^{\circ},\;8.3^{\circ}\;and\;21.9^{\circ}$, respectively. Xray crystallography of $SmZn_{0.67}Sb_2$ has attempted to compare accuracy of the structure determination by electron crystallography, which resulted in the cell parameters of $a=4.2976(6){\AA}\;and\;c=10.287(2){\AA}$, and the R-factor ($R_{sym}$) of 4.16%.

무기결정질인 $SmZn_{0.67}Sb_2$의 3차원적 구조 (공간군 P4/nmm, $a=4.26{\AA},\;c=10.37{\AA}$)를 전자결정학을 이용하여 분석하였다. 3차원적 정보를 얻기 위해서 주요 정대축인 세 방향의 고분해능 이미지의 정보와 16개의 정대축 방향의 회절도형을 조합하였다. 고분해능 이미지의 결정학적 화상처리(CIP)를 결정구조의 보다 정확한 분석을 위하여 사용하였다. 전자결정학을 이용한 분석 결과, [001], [100], [110] 방향에 대한 고분해능 이미지의 ${\Phi}_{res}$는 각각 $17.0^{\circ},\;8.3^{\circ},\;21.9^{\circ}$를 나타내었다. 전자결정학을 이용한 구조 분석 결과에 대한 정확도를 비교하기 위하여 X-ray 회절 분석을 시도하였다. $SmZn_{0.67}Sb_2$의 X-ray 구조 분석 결과, $a=4.276{\AA},\;c=10.287{\AA}$이고 신뢰도($R_{sym}$)는 4.16% 이었다.

Keywords

References

  1. Dorset DL, Hovmoller S, Zou XD (eds): Electron Crystallography. Kluwer Academic Publishers, Dordrecht/Boston/London, pp. 439, 1997
  2. Dorset DL: Structural Electron Crystallography. Plenum Press, New york and London, pp. 135 166, 1995
  3. Hahn T: International Tables for Crystallograhy. Vol. A. Dordrecht Reidel Publishing Company, pp. 854, 1983
  4. Sven Hovmollera: CRISP Crystallographic Image Processing on a Personal Computer. Ultramicroscopy 41 : 121 135, 1992 https://doi.org/10.1016/0304-3991(92)90102-P
  5. Sheldrick GM: SHELXS97. SHELXL97 program, University of Goettingen, Germany, 1997
  6. Zou XD, Hovmoller A, Hovmoller S: TRICE A program for reconstructing 3D reciprocal space and determining unit cell parameters. Ulramicroscopy 98 : 187 193, 2004 https://doi.org/10.1016/j.ultramic.2003.08.025
  7. Zou XD, Sukharev Y, Hovmoller S: ELD A Computer Program System for Extracting Intensities From Electron Diffraction Patterns. Ultramicroscopy 49 : 147 158, 1993 https://doi.org/10.1016/0304-3991(93)90221-I
  8. Zou XD, Sundberg M, Larine M, Hovmoller S: Structure projection retrieval by image processing of HREM images taken under non optimum defocus conditions. Ultramicroscopy 62 : 103 121, 1996 https://doi.org/10.1016/0304-3991(95)00090-9
  9. Zou XD: Electron Crystallography of Inorganic Structures. Stockholm, pp.1 9, 1995