Hostname: page-component-78c5997874-ndw9j Total loading time: 0 Render date: 2024-11-10T15:35:22.492Z Has data issue: false hasContentIssue false

Site-Specific Specimen Preparation by Focused Ion Beam Milling for Transmission Electron Microscopy of Metal Matrix Composites

Published online by Cambridge University Press:  17 March 2004

Philippe Gasser
Affiliation:
Swiss Federal Institute for Materials Testing and Research (EMPA), Ueberlandstrasse 129, CH-8600 Duebendorf, Switzerland
Ulrich E. Klotz
Affiliation:
Swiss Federal Institute for Materials Testing and Research (EMPA), Ueberlandstrasse 129, CH-8600 Duebendorf, Switzerland
Fazal A. Khalid
Affiliation:
Faculty of Metallurgy and Materials Engineering, Gulam Ishaq Khan Institute of Engineering Sciences and Technology, Topi, North-West Frontier Province, Pakistan
Olivier Beffort
Affiliation:
Swiss Federal Institute for Materials Testing and Research (EMPA), Feuerwerkerstrasse 39, CH-3602 Thun, Switzerland
Get access

Abstract

This work describes the application and usefulness of the focused ion beam (FIB) technique for the preparation of transmission electron microscopy (TEM) samples from metal matrix composite materials. Results on an Al/diamond composite, manufactured by the squeeze casting infiltration process, were chosen for demonstration. It is almost impossible to prepare TEM specimens of this material by any other conventional method owing to the presence of highly inhomogeneous phases and reinforcement diamond particles. The present article gives a detailed account of the salient features of the FIB technique and its operation. One of the big advantages is the possibility to prepare site-specific TEM specimens with high spatial resolution. The artifacts occurring during the specimen preparation, for example, Ga-ion implantation, curtain effects, amorphous layers, bending of the lamella, or different milling behaviors of the materials have been discussed. Furthermore, TEM examination of the specimens prepared revealed an ultrafine amorphous layer of graphite formed at the interface between the Al and diamond particles that may affect the interfacial properties of the composite materials. This may not have been feasible without the successful application of the FIB technique for production of good quality site-specific TEM specimens.

Type
Materials Applications
Copyright
© 2004 Microscopy Society of America

Access options

Get access to the full version of this content by using one of the access options below. (Log in options will check for institutional or personal access. Content may require purchase if you do not have access.)

References

REFERENCES

Anderson, R. (2002). Critical comparison of FIB TEM specimen preparation methods. In Proceedings of the 15th International Congress on Electron Microscopy, Engelbrecht, J., Sewell, T., Witcomb, M., Cross, R. & Richards, P. (Eds.), pp. 253254. Onderstepoort, South Africa: Microscopy Society of South Africa.
Engelmann, H.J., Volkmann, B., Saage, H., Stegmann, H., Ziesche, S., & Zschech, E. (2002). TEM sample preparation using focused ion beam—Capabilities and limits. In Proceedings of the 15th International Congress on Electron Microscopy, Engelbrecht, J., Sewell, T., Witcomb, M., Cross, R. & Richards, P. (Eds.), pp. 257258. Onderstepoort, South Africa: Microscopy Society of South Africa.
Giannuzzi, L.A., Drown, J.L., Brown, S.R., Irwin, R.B., & Stevie, F.A. (1998). Applications of the FIB lift-out technique for TEM specimen preparation. Micros Res Tech 41, 285290.Google Scholar
Giannuzzi, L.A. & Stevie, F.A. (1999). A review of focused ion beam milling techniques for TEM specimen preparation. Micron 30, 197204.Google Scholar
Khalid, F.A., Beffort, O., Klotz, U.E., Keller, B., Gasser, P., & Voucher, S. (2003). Study of microstructure and interfaces in an aluminium-C60 composite material. Acta Mat 51, 45754582.Google Scholar
Kim, S.T. & Dravid, V.P. (2000). Focused ion beam sample preparation of continuous fibre-reinforced ceramic composite specimens for transmission electron microscopy. J Microsc 198, 124133.Google Scholar
Klotz, U.E., Wilcock, I., Henderson, M.B., & Davis, S. (2002). Interdiffusion in HIPped bi-metallic turbine discs. In Proceedings of the 15th International Congress on Electron Microscopy, Engelbrecht, J., Sewell, T., Witcomb, M., Cross, R. & Richards, P. (Eds.), pp. 693694. Onderstepoort, South Africa: Microscopy Society of South Africa.
Lipp, S. (1998). Untersuchungen von Ätz- und Abscheideprozessen im fokusierten Ionenstrahl. In Erlanger Berichte Mikroelektronik, Vol. 98/1, Aachen: Shaker.
Lomness, J.K., Giannuzzi, L.A., & Hampton, M.D. (2001). Site-specific transmission electron microscope characterization of micrometer-sized particles using the focused ion beam lift-out technique. Microsc Microanal 7, 418423.Google Scholar
White, H., Pu, Y., Rafailovich, M., Sokolov, J., King, A.H., Giannuzzi, L.A., Urbanik-Shannon, C., Kempshall, B.W., Eisenberg, A., Schwarz, S.A., & Strzhemechny, Y.M. (2001). Focused ion beam/lift-out transmission electron microscopy cross sections of block copolymer films ordered on silicon substrates. Polymer 42, 16131619.Google Scholar