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Automated diffraction tomography combined with electron precession: a new tool for ab initio nanostructure analysis

Published online by Cambridge University Press:  31 January 2011

Ute Kolb ,
Tatiana Gorelik  and
Enrico Mugnaioli
Ute Kolb
Affiliation:
kolb@uni-mainz.de, Johannes Gutenberg-University, Instiut for Physical Chemistry, Mainz, Germany
Tatiana Gorelik
Affiliation:
gorelik@uni-mainz.de, Johannes Gutenberg-University, Instiut for Physical Chemistry, Mainz, Germany
Enrico Mugnaioli
Affiliation:
mugnaiol@uni-mainz.de, Johannes Gutenberg-University, Instiut for Physical Chemistry, Mainz, Germany
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Abstract

Three-dimensional electron diffraction data was collected with our recently developed module for automated diffraction tomography and used to solve inorganic as well as organic crystal structures ab initio. The diffraction data, which covers nearly the full relevant reciprocal space, was collected in the standard nano electron diffraction mode as well as in combination with the precession technique and was subsequently processed with a newly developed automated diffraction analysis and processing software package. Non-precessed data turned out to be sufficient for ab initio structure solution by direct methods for simple crystal structures only, while precessed data allowed structure solution and refinement in all of the studied cases.

Keywords

scanning transmission electron microscopy (STEM)nanostructurecrystallographic structure
Type
Research Article
Information
MRS Online Proceedings Library (OPL) , Volume 1184: Symposium GG – Electron Crystallography for Materials Research and Quantitive Characterization of Nanostructured Materials , 2009 , 1184-GG01-05
Copyright
Copyright © Materials Research Society 2009

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References

1. O'Keefe, M. A., Microscopy and Microanalysis 10 (Suppl 2), 972 (2004).Google Scholar
2. Zou, X., Hovmöller, A. and Hovmöller, S., Ultramicroscopy, 98, 187 (2004); J. Jansen, D. Tang, H. W. Zandbergen and H. Schenk, Acta Cryst. A54, 91 (1998); R. Kilaas, L. D. Marks and C. S. Own Ultramicroscopy 102, 233 (2005).Google Scholar
3. Kolb, U., Gorelik, T., in: Weirich, Th. et al. (Eds.), Electron Crystallography, vol. 211, Kluwer Academic Publishers, Netherlands, NATO ASI Series E: Applied Sciences, 2005, p. 421.Google Scholar
4. Vainshtein, B. K., Structure Analysis by Electron Diffraction, Plenum, 1964.Google Scholar
5. Vincent, R., Midgley, P. A., Ultramicroscopy 53, 271 (1994).; C.S.Own, System design and verification of the precession electron diffraction technique, Ph. D. Dissertation, Northwestern University Evanston Illinois, 2005 /http://www.numis.northwestern.edu/Research/Current/precessions; A. Avilov, K. Kuligin, S. Nicolopoulos, M. Nickolskiy, K. Boulahya, J. Portillo, G. Lepeshov, B. Sobolev, J. P. Collette, N. Martin, A. C. Robins, P. Fischione, Ultramicroscopy 107, 431 (2007); M. Gemmi, S. Nicolopoulos, Ultramicroscopy 107, 483 (2007).Google Scholar
6. Weirich, T. E., Rameau, R., Simon, A., Hovmöller, S., Zou, X. D., Nature 382, 144–146, (1996); I. G. Voigt-Martin, Z. X. Zhang, U. Kolb, C. Gilmore, Ultramicroscopy 68, 43-59 (1997); D. L. Dorset, Structural Electron Crystallography, Plenum Press, New York, 1995.Google Scholar
7. Kolb, U., Gaelic, T., Keble, C., Otten, M. T. and Hubert, D., Ultramicroscopy 107, 507 (2007)Google Scholar
8. Kolb, U., Gaelic, T., Otten, M. T., Ultramicroscopy 108, 763 (2008).Google Scholar
9. Dιéz, D. Castano, Seybert, A., Frangakis, A. S., J. Struct. Biol. 154, 195 (2006).Google Scholar
10. Maslen, E. N., Streltsov, V. A., Streltsova, N. R. and Ishizawa, N., Acta Cryst. B51, 929 (1995).Google Scholar
11. Jacobsen, S. D., Smyth, J. R., Swope, J., Can Miner. 36, 1053 (1998).Google Scholar
12. Mozharivsky, Y., Pecharsky, A. O., Bud’ko, S., and Miller, G. J.: Chem. Mater. 16, 1580 (2004).Google Scholar
13. Rozhdestvenskaya, I. V., Kogure, T., and Drits, V. A., Abstracts of Meeting “Crystal chemistry and X-ray diffraction of Minerals”, Miass 2007, p. 48–49.Google Scholar
14. Schmidt, M. U., Brühne, S., Wolf, A. K., Rech, A., Brüning, J., Alig, E., Fink, L., Buchsbaum, Ch., Glinnemann, J., Streek, J. van de, Gozzo, F., Brunelli, M., Stowasser, F., Gorelik, T., Mugnaioli, E. and Kolb, U. Acta Cryst. B65, 189 (2009).Google Scholar
15. Kolb, U. and Matveeva, G. N., Zeitschrift für Kristallographie 218(4), 259 (2003), Special issue: Electron Crystallography.Google Scholar
16. Gorelik, T., Kolb, U., Matveeva, G., Schleuß, T., Kilbinger, A. F. M., Streek, J. van de, in preparation.Google Scholar
17.Basolite A100 purchased from Sigma Aldrich 688738.Google Scholar
18. Tahir, M. N. and Tremel, W., unpublished results.Google Scholar
19.Hielscher USA, Inc., 19, Forest Rd., NJ 07456, Ringwood, USA.Google Scholar
20.MRC: basic file format of the Medical Research Council, extended with additional headers for up to 1024 images.Google Scholar
21.UCSF Chimera package from the Resource for Biocomputing, Visualization, and Informatics at the University of California, San Francisco (supported by NIH P41 RR-01081).Google Scholar
22. Pettersen, E. F., Goddard, T. D., Huang, C. C., Couch, G. S., Greenblatt, D. M., Meng, E. C., and Ferrin, T. E., J. Comput. Chem. 25, 1605 (2004).Google Scholar
23. Burla, M. C., Caliandro, R., Camalli, M., Carrozzini, B., Cascarano, G. L., L. De Caro, Giacovazzo, C., Polidori, G., Diliqi, S., Spagna, R.: J. Appl. Cryst. 40, 609 (2007).Google Scholar
24. Sheldrick, G. M., Acta Crystallogr. A64, 112–122 (2008).Google Scholar
25. Jacobsen, S. D., Smyth, J. R. and Swope, J., Can. Miner. 36 (1998) 1053 Google Scholar
26. Mugnaioli, E., Gorelik, T., Kolb, U., Ultramicroscopy, 109, 758 (2009).Google Scholar
27. Mugnaioli, E., Gorelik, T., Panthoefer, M., Schade, Ch., Tremel, W. and Kolb, U., A combination of electron diffraction tomography and precession applied to Zn1+xSb nanophases, to be publishedGoogle Scholar
28. Putz, H., Schoen, J. C., Jansen, M., J. Appl. Cryst,. 32, 864 (1999).Google Scholar
29. Schmidt, M. U., Hofmann, D. W. M., Buchsbaum, Ch., and Metz, H. J., Angew. Chem. Int. Ed,. 45, 1313 (2006).Google Scholar
30. Georgieva, D. and Abrahams, J.-P., Leiden University, unpublished results.Google Scholar
31. Burla, M. C., Carrozzini, B., Cascarano, G. L., Giacovazzo, C. & Polidori, G. Z. Kristallogr. 217, 629 (2002).Google Scholar
32. Wilson, A. J. C. Acta Cryst.. 3, 397 (1950).Google Scholar