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Measuring Electrostatic Potential Profiles across Amorphous Intergranular Films by Electron Diffraction

Published online by Cambridge University Press:  09 December 2005

Christoph T. Koch ,
Somnath Bhattacharyya ,
Manfred Rühle ,
Raphaëlle L. Satet  and
Michael J. Hoffmann
Christoph T. Koch
Affiliation:
Max Planck Institut für Metallforschung, Heisenbergstr. 3, D-70569 Stuttgart, Germany
Somnath Bhattacharyya
Affiliation:
Max Planck Institut für Metallforschung, Heisenbergstr. 3, D-70569 Stuttgart, Germany
Manfred Rühle
Affiliation:
Max Planck Institut für Metallforschung, Heisenbergstr. 3, D-70569 Stuttgart, Germany
Raphaëlle L. Satet
Affiliation:
Universität Karlsruhe, Institut für Keramic im Maschinenbau-Zentrallaboratorium, D-73131 Karlsruhe, Germany
Michael J. Hoffmann
Affiliation:
Universität Karlsruhe, Institut für Keramic im Maschinenbau-Zentrallaboratorium, D-73131 Karlsruhe, Germany
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Abstract

Amorphous 1–2-nm-wide intergranular films in ceramics dictate many of their properties. The detailed investigation of structure and chemistry of these films pushes the limits of today's transmission electron microscopy. We report on the reconstruction of the one-dimensional potential profile across the film from an experimentally acquired tilt series of energy-filtered electron diffraction patterns. Along with the potential profile, the specimen thickness, film orientation with respect to the grain lattice and specimen surface, and the absolute specimen orientation with respect to the laboratory frame of reference are retrieved.

Keywords

energy-filtered electron diffractionintergranular amorphous filmsceramicsphase problemthermal diffuse scatteringelectrostatic potentialone-dimensional potential profile
Type
MICROSCOPY TECHNIQUES
Information
Microscopy and Microanalysis , Volume 12 , Issue 2 , April 2006 , pp. 160 - 169
Copyright
© 2006 Microscopy Society of America

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References

REFERENCES

Balluffi, R.W. & Bristowe, P.D. (1984). On the detection of expansion at large-angle grain-boundaries using electron diffraction. Scripta Metall 18, 617.Google Scholar
Bishop, C.M. (2003). Continuum models for intergranular films in silicon nitride and comparison to atomistic simulations. Ph.D. thesis. Cambridge, MA: MIT.
Bishop, C.M. & Carter, C.W. (2002). Relating atomistic grain boundary simulation results to the phase-field model. Comp Mat Sci 25, 378–386.Google Scholar
Cahn, J.W. & Hilliard, J.E. (1958). Free energy of a non-uniform system. 1. Interfacial free energy. J Chem Phys 28, 258–267.Google Scholar
Cinibulk, M.K., Kleebe, H.J., & Rühle, M. (1993). Quantitative comparison of TEM techniques for determining amorphous intergranular film thickness. J Am Cer Soc 76, 426–432.Google Scholar
Clarke, D.R. (1987). On the equilibrium thickness of intergranular glassy phases in ceramic. J Am Cer Soc 70, 15–22.Google Scholar
Clarke, D.R., Shaw, T.M., Philipse, A.P., & Horn, R.G. (1993). Possible electrical double-layer contribution to the equilibrium thickness of intergranular glass phases in polycrystalline ceramics. J Am Cer Soc 76, 1201–1204.Google Scholar
Doyle, P.A. & Turner, P.S. (1968). Relativistic Hartree-Fock X-ray and electron scattering factors. Acta Cryst A 24, 390–397.Google Scholar
Dunin-Borkowski, R.E. (2000). The development of Fresnel contrast analysis, and the interpretation of mean inner potential profiles at interfaces. Ultramicroscopy 83, 193–216.Google Scholar
Dunin-Borkowski, R.E. & Stobbs, W. (1993). The defocus contrast of a θ′ precipitate in Al-4 wt% Cu: Fresnel fringe analysis applied to an atomically abrupt interface. Ultramicroscopy 52, 404–414.Google Scholar
Fienup, J.R. (1982). Phase retrieval algorithms—A comparison. Appl Optics 21, 2758.Google Scholar
Gajdardziska-Josifovska, M., Weiss, J.K., & Cowley, J.M. (1995). Studies of Mo/Si multilayers with coherent electron beams. Ultramicroscopy 58, 65–78.Google Scholar
Gu, H. (2004). Electron energy-loss spectroscopy characterization of ≈1nm-thick amorphous film at grain boundary in Si-based ceramics. Mat Trans 45, 2091–2098.Google Scholar
Gu, H., Pan, X., Cannon, R.M., & Rühle, M. (1998). Dopand distribution in grain-boundary films in calcia-doped silicon nitride ceramics. J Am Cer Soc 81, 3125–3135.Google Scholar
Howie, A. (2004). Hunting the Stobbs factor. Ultramicroscopy 98, 73–79.Google Scholar
Koch, C.T. & Spence, J.C.H. (2003). A useful disentanglement of the exponential of the sum of two non-commuting matrices, one of which is diagonal. J Phys A: Math Gen 36, 803–816.Google Scholar
Lamarre, P. & Sass, S.L. (1983). Detection of the expansion at a large-angle [001] twist boundary using electron-diffraction. Scripta Metall 17, 1141.Google Scholar
Marchesini, S., He, H., Chapman, H., Hau-Riege, S., Noy, A., Howells, M., Weierstall, U., & Spence, J. (2003). X-ray image reconstruction from a diffraction pattern alone. Phys Rev B 68, 140101.Google Scholar
McGuire, G.E. (1988). Semiconductor Materials and Process Technology Handbook. Park Ridge, NJ: William Andrew Publishing, Noyes.
Oszlanyi, G. & Suto, A. (2004). Ab initio structure solution by charge flipping. Acta Cryst A 60, 134.Google Scholar
Satet, R.L. & Hoffmann, M.J. (2004). Impact of the intergranular film properties on microstructure and mechanical behavior of silicon nitride. Key Eng Mater 264–268, 775–780.Google Scholar
Shibata, N., Pennycook, S.J., Gosnell, T.R., Painter, G.S., Shelton, W.A., & Becher, P.F. (2004). Observation of rare-earth segregation in silicon nitride ceramics at subnanometre dimensions. Nature 428, 730–733.Google Scholar
Vitek, J.M. (1986). Influence of segregation on the diffraction effects from homophase interfaces. Ultramicroscopy 22, 197–206.Google Scholar
Vitek, J.M., Vaudin, M.D., Rühle, M., & Sass, S.L. (1989). Diffraction effects along the normal to a grain-boundary. Scripta Metall 23, 349–354.Google Scholar
Walther, T. (2003). Electron energy-loss spectroscopic profiling of thin film structures: 0.39 nm line resolution and 0.04 eV precision measurement of near-edge structure shifts at interfaces. Ultramicroscopy 96, 401.Google Scholar
Wang, Y.G. & Dravid, V.P. (2002). Determination of electrostatic characteristics at a 24°, [001] tilt grain boundary in a SrTiO3 bicrystal by electron holography. Phil Mag Lett 82, 425.Google Scholar
Winkelmann, G. (2004). Arrangement of rare-earth elements at prismatic grain boundaries in silicon nitride. Phil Mag Lett 84, 755–762.Google Scholar
Wu, J.S., Weierstall, U., Spence, J.C.H., & Koch, C.T. (2004). Iterative phase retrieval without support. Optics Lett 29, 2737–2739.Google Scholar
Ziegler, A., Idrobo, J.C., Cinibulk, M.K., Kisielowski, C., Browning, N.D., & Ritchie, R.O. (2004). Interface structure and atomic bonding characteristics in silicon nitride ceramics. Science 306, 1768–1770.Google Scholar
Zuo, J.M., Vartanyants, I., Gao, M., Zhang, R., & Nagahara, L.A. (2003). Atomic resolution imaging of a carbon nanotube from diffraction intensities. Science 300, 1419.Google Scholar