On the consistency of QCBED structure factor measurements for TiO₂ (Rutile)

Journal Article · 15 September 2003 · Microscopy and Microanalysis

DOI: https://doi.org/10.1017/S1431927603030381 · OSTI ID:1164063

Jiang, Bin ^[1]; Zuo, Jian -Min ^[2]; Friis, Jesper ^[3]; Spence, John C. H. ^[4]

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1. Arizona State Univ., Tempe, AZ (United States); Arizona State University
2. Univ. of Illinois, Urbana, IL (United States)
3. Arizona State Univ., Tempe, AZ (United States); Norwegian Univ. of Science and Technology, Trondheim (Norway)
4. Arizona State Univ., Tempe, AZ (United States)

The same Bragg reflection in TiO₂ from twelve different CBED patterns (from different crystals, orientations and thicknesses) are analysed quantitatively in order to evaluate the consistency of the QCBED method for bond-charge mapping. The standard deviation in the resulting distribution of derived X-ray structure factors is found to be an order of magnitude smaller than that in conventional X-ray work, and the standard error (0.026% for F_X(110)) is slightly better than obtained by the X-ray Pendellosung method applied to silicon. This is sufficiently accuracy to distinguish between atomic, covalent and ionic models of bonding. We describe the importance of extracting experimental parameters from CCD camera characterization, and of surface oxidation and crystal shape. Thus, the current experiments show that the QCBED method is now a robust and powerful tool for low order structure factor measurement, which does not suffer from the large extinction (multiple scattering) errors which occur in inorganic X-ray crystallography, and may be applied to nanocrystals. Our results will be used to understand the role of d electrons in the chemical bonding of TiO₂.

• Research Organization: Arizona State Univ., Tempe, AZ (United States)
• Sponsoring Organization: USDOE Office of Science (SC), Basic Energy Sciences (BES) (SC-22)
• Grant/Contract Number: FG03-02ER45996
• OSTI ID: 1164063
• Journal Information: Microscopy and Microanalysis, Journal Name: Microscopy and Microanalysis Journal Issue: 05 Vol. 9; ISSN 1431-9276; ISSN applab
• Publisher: Microscopy Society of America (MSA)Copyright Statement
• Country of Publication: United States
• Language: English