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Focused Ion Beam Sample Preparation of Non-Semiconductor Materials

Published online by Cambridge University Press:  10 February 2011

M. W. Phaneuf
Affiliation:
Fibics Incorporated, 568 Booth Street, Ottawa, ON, CANADA
N. Rowlands
Affiliation:
Micrion Corporation, One Corporation Way, Peabody, MA 01960
G. J. C. Carpenter
Affiliation:
CANMET, Materials Technology Laboratory, 568 Booth Street, Ottawa, ON CANADA K1A 0G1.
G. Sundaram
Affiliation:
Micrion Corporation, One Corporation Way, Peabody, MA 01960
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Abstract

Focused Ion Beam (FIB) systems have been steadily gaining acceptance as specimen preparation tools in the semiconductor industry. This is largely due to the fact that such instruments are relatively commonplace as failure analysis tools in semiconductor houses, and are commonly used in the preparation of cross-sections for imaging under the ion beam or using an electron beam in an SEM. Additionally, the ease with which cross-sectional TEM specimens of semiconductor devices can be prepared using FIB systems has been well demonstrated. However, this technology is largely unknown outside the semiconductor industry. Relatively few references exist in the literature on the preparation of cross-sectional TEM specimens of non-semiconductor materials by FIB. This paper discusses a specific use of FIB technology in the preparation of cross-sectional TEM specimens of non-semiconductor samples that are difficult to prepare by conventional means. One example of such materials is commercial galvannealed steel sheet that is used to form corrosion resistant auto-bodies for the automobile industry. Cross-sectional TEM specimens of this material have proved difficult and time-intensive to prepare by standard polishing and ion milling techniques due to galvanneal's inherent flaking and powdering difficulties, as well as the different sputtering rates of the various Fe-Zn intermetallic phases present in the galvannealed coatings. TEM results from cross-sectional samples of commercial galvannealed steel coatings prepared by conventional ion milling and FIB techniques are compared to assess image quality, the size of the electron-transparent thin regions that can be readily prepared and the quality of samples produced by both techniques. Specimen preparation times for both techniques are reported.

Type
Research Article
Copyright
Copyright © Materials Research Society 1997

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References

1. Morris, S., Tatti, S., Black, E., Dickson, N., Mendez, H., Schwiesow, B., and Pyle, R., “A Technique for preparing TEM Cross Sections to a Specific Area Using the FIB”, ISTFA 91, pp. 417427.Google Scholar
2. Overwijk, M. H. F., van den Heuvel, F. C., and Bull-Lieuwma, C. W. T., “Novel Scheme for the Preparation of Transmission Electron Microscopy Specimens with a Focused Ion Beam”, J. Vac. Sci. Technol. B. Vol.11, No. 6, Nov/Dec 1993, pp. 22012204.Google Scholar
3. Jagannathan, V., “Emerging Technologies in the Hot-Dip Coating of Automotive Sheet Steel”, Journal of Materials, August, (1993), pp. 4851.Google Scholar
4. Bastin, G.F., van Loo, F.J.J. and Rieck, G.D., “On the δ-Phase in the Fe-Zn System”, Z. Metallkde., 67, (1976), pp. 694.Google Scholar
5. Von Bablik, H., Gotzl, F. and , F.H. in Wien, “Uber das System Eisen-Zink”;, Z. Metallkde, 30, (1938), pp. 249252.Google Scholar
6. Foct, J., “Relaxation of Stresses by Cracks in Intermetallic Coatings: Application to Galvanizing”, Scripta Metallurgica et Materialia, 28, (1993), pp. 127132.Google Scholar
7. L'Esperance, G., L'Ecuyer, J.D., Simard, A., Barreto, M.P. and Botton, G., “Analytical Transmission Electron Microscopy of Galvanneal Coatings”, 2nd International Conference on Zinc and Zinc Alloy Coated Steel Sheet (GALVATECH ‘92), Verlag Stahleisen mbH, Dusseldorf, (1992), pp. 442448.Google Scholar
8. L'Ecuyer, J.D., Gange, M., Cheng, C.C. and L'Esperance, G., “Electron Microscopy of Hot-Gip Galvannealed Coatings“, Electron Microscopy 1990, Proceedings of the XIIth International Congress for Electron Microscopy, eds. Peachy, L.D. and Williams, D.B., San Francisco Press, 4, (1990), pp. 10361041.Google Scholar
9. Giannuzzi, L.A., Howell, P.R., Pickering, H.W. and Bitler, W.R., “The Characterization of Intermediate Phases of Electrogalvanized – Iron Couples by Cross-Section Transmission Electron Microscopy – A Brief Overview”, 2nd International Conference on Zinc and Zinc Alloy Coated Steel Sheet (GALVATECH ‘92), Verlag Stahleisen mbH, Dusseldorf, (1992), pp 461467.Google Scholar
10. Giannuzzi, L.A., Ramani, A.S., Howell, P.R., Pickering, H.W. and Bitler, W.R., “High Resolution Electron Microscopy of the Iron-Zinc Delta Intermetallic Phase”, Plating and Surface Finishing, Feb. (1993), pp. 5456.Google Scholar
11. Lin, Y., Chiou, W.A. and Meshii, M., “High Resolution Electron Microscopy Study on the Interface of Electrogalvanized Coatings on Sheet Steel After Heating”, Proceedings of the 49th Annual Meeting of the Electron Microscopy Society of America, (1992), San Francisco Press, San Francisco, pp. 568569.Google Scholar
12. Lin, Y., Chiou, W.A. and Meshii, M., “Atomic Structures of Interfaces in Annealed Electrogalvanized Steel Sheets”, 2nd International Conference on Zinc and Zinc Alloy Coated Steel Sheet (GALVATECH ‘92), Verlag Stahleisen mbH, Dusseldorf, (1992), pp. 429432.Google Scholar
13. Lin, C.S., Chiou, W.A. and Meshii, M., “Direct Observation of Fe-Al-Zn Ternary Intermetallic Compound and Its Transformation During the Early Stages of Hot-Dip Galvanizing”, Proceedings of the 51st Annual Meeting of the Electron Microscopy Society of America (1993), San Francisco Press, San Francisco, pp. 11161117.Google Scholar
14. Phaneuf, M.W., Carpenter, G.J.C. and Saimoto, S., “Direct Observation of Nanocrystalline and Amorphous Phases in Commercial Galvannealed Steel Sheet”, Scripta Metallurgica et Materialia, 31, 1 (1994) pp. 14.Google Scholar