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Metallurgical and Materials Transactions A

, Volume 29, Issue 9, pp 2399–2406 | Cite as

Transmission electron microscope specimen preparation of Zn powders using the focused ion beam lift-out technique

  • B. I. Prenitzer
  • L. A. Giannuzzi
  • K. Newman
  • S. R. Brown
  • R. B. Irwin
  • F. A. Stevie
  • T. L. Shofner
Article

Abstract

Particles of Zn powder have been studied to show that high-quality scanning electron microscope (SEM) and transmission electron microscope (TEM) specimens can be rapidly produced from a site-specific region on a chosen particle by the focused ion beam (FIB) lift-out technique. A TEM specimen approximately 20-µm long by 5-µm wide was milled to electron transparency, extracted from the bulk particle, and micromanipulated onto a carbon coated copper mesh TEM grid. Using the FIB lift-out method, we were able to prepare a site-specific TEM specimen from a difficult material in under 3 hours. The TEM analysis of the lift-out specimen revealed a large amount of thin area free from characteristic signs of damage that may be observed as a result of conventional argon ion milling. The overall microstructure of the specimen prepared by the FIB lift-out method was consistent with samples prepared by conventional metallographic methods. A grain size of ∼10 to 20 µm was observed in all specimens by both TEM and SEM analysis. Light optical microscopy revealed the presence of internal voids in ∼10 to 20 pct of all particles. The SEM analysis showed the voids to extend over ∼70 pct of the particle volume in some cases.

Keywords

Material Transaction Transmission Electron Micro Specimen Metal Powder Industry Federation Scanning Electron Microscopy Specimen Transmission Electron Micro Specimen Preparation 
These keywords were added by machine and not by the authors. This process is experimental and the keywords may be updated as the learning algorithm improves.

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References

  1. 1.
    Randall M. German: Powder Metallurgy Science, 2nd ed., Metal Powder Industries Federation, Princeton, NJ, 1994, pp. 16–25.Google Scholar
  2. 2.
    Donald G. White: Des. News, 1996, vol. 51, p. 102.Google Scholar
  3. 3.
    Donald G. White: Mach. Des., 1994, vol. 66.Google Scholar
  4. 4.
    Thomas B. Gurganus: Adv. Mater. Processes, 1995, vol. 148, pp. 57–59.Google Scholar
  5. 5.
    David T. Gethen, Viet D. Tran, and Roland W. Lewis: Int. J. Powder Metall., 1994, vol. 30, pp. 385–98.Google Scholar
  6. 6.
    Animesh Bose: Int. J. Powder Metall., 1995, vol. 47, pp. 26–30.Google Scholar
  7. 7.
    Reginald L. Eadie and Xiolin Chen: Int. J. Powder Metall., 1996, No. 3, pp. 265–75.Google Scholar
  8. 8.
    David B. Williams and Barry Carter: Transmission Electron Microscopy, Plenum Press, New York, NY, 1996, pp. 163–64.Google Scholar
  9. 9.
    Manfred Von Heimendahl: Electron Microscopy of Materials, An Introduction, Academic Press, Inc., San Diego, CA, 1980, pp. 89–91.Google Scholar
  10. 10.
    J.A. Yater and M.O. Thompson: J. Vac. Sci. Technol. B, 1992, vol. 10 (1), pp. 183–86.CrossRefGoogle Scholar
  11. 11.
    C.E. Sanborn and S.A. Myers: Materials Research Society Symp. on Specimen Preparation for Transmission Electron Microscopy of Materials—III, American Institute of Physics, College Park, MD, 1992, vol. 254, pp. 239–48.Google Scholar
  12. 12.
    M.H.F. Overwijk, F.C. van den Heuvel, and C.W.T. Bule-Lieuwma: J. Vac. Sci. Technol. B, 1993, vol. 11(6), pp. 2021–24.CrossRefGoogle Scholar
  13. 13.
    M. Tartuani, Y. Takai, R. Shimizu, K. Uda, and H. Takahashi: Tech. Rep. Osaka Univ., 1993, vol. 43 (2143), pp. 167–73.Google Scholar
  14. 14.
    M.L. Thayer: ISTFA ’93, Proc. 19th Int. Symp. on Testing Failure Analysis, ASM International, Materials Park, OH, 1993, pp. 425–29.Google Scholar
  15. 15.
    T. Ishitani, H. Tsuboi, T. Yaguchi, and H. Koike: J. Electron Microsc., 1994, vol. 43, pp. 322–26.Google Scholar
  16. 16.
    F.A. Stevie, T.C. Shane, P.M. Kahora, R. Hull, D. Bahnck, V.C. Kanna, and E. David: Surf. Interface Anal., 1995, vol. 23, pp. 61–68.CrossRefGoogle Scholar
  17. 17.
    Y. Kitano, Y. Fujikawa, T. Kamino, T. Yaguchi, and H. Saka: J. Electron Microsc., 1995, vol. 44, pp. 410–13.Google Scholar
  18. 18.
    L.A. Giannuzzi, J.L. Drown, S.R. Brown, R.B. Irwin, and F.A. Stevie: Microsc. Res. Technol, Wiley-Liss, Inc., vol. 41, 1998, pp. 285–90.CrossRefGoogle Scholar
  19. 19.
    L.A. Giannuzzi, J.L. Drown, S.R. Brown, and R.B. Irwin, and F.A. Stevie: Workshop on Specimen preparation for TEM of Materials IV, Materials Research Society Symposia Proceedings, Materials Research Society, Pittsburgh, PA, 1997, pp. 19–27.Google Scholar
  20. 20.
    R. Noone: Euro ASIC ’92, Proc. Euro ASIC 92, 1992, IEEE Service Center, Piscataway, NJ, pp. 414–15.CrossRefGoogle Scholar
  21. 21.
    H. Mendez, S. Morris, S. Tatti, N. Dickson, and R.E. Pyle: SPIE Proc. Microelectronics Manufacturing and Reliability, 1992, vol. 1802, pp. 126–33.Google Scholar
  22. 22.
    F.C. van den Heuvel, M.H.F. Overwijk, E.M. Fleuren, H. Laisina, and K.J. Sauer: Microelectron. Eng., 1993, vol. 21, pp. 209–12.CrossRefGoogle Scholar
  23. 23.
    A.B. Soto and S.L. Riley: ISTFA ’93, Proc. 19th Int. Symp. on Testing Failure Analysis, ASM International, Materials Park, OH, 1993, pp. 419–24.Google Scholar
  24. 24.
    K. Van Doorselaer, M. Van den Reeck, L. Van den Bempt, R. Young, and J. Whitney: ISTFA ’93, Proc. 19th Int. Symp. on Testing Failure Analysis, ASM International, Materials Park, OH, 1993, pp. 405–15.Google Scholar
  25. 25.
    K. Van Doorselaer and L. Van den Bempt: ISTFA ’94, Proc. 20th Int. Symp. on Testing Failure Analysis, ASM International, Materials Park, OH, 1994, pp. 397–405.Google Scholar
  26. 26.
    S.X. Li, D. Lee, and S. Leung: ISTFA ’94, Proc. 20th Int. Symp. on Testing Failure Analysis, ASM International, Materials Park, OH, 1994, pp. 415–19.Google Scholar
  27. 27.
    J.M. Chabala, R. Levi-Setti, and Y.L. Wang: J. Vasc. Sci Technol. B, 1988 vol. 6 (3), pp. 910–14.CrossRefGoogle Scholar
  28. 28.
    D.E. Newbury: Microbeam Analysis, San Francisco Press, Inc., San Francisco, CA, 1988, pp. 93–101.Google Scholar
  29. 29.
    C.H. Chu, Y.F. Hseih, L.R. Harriot, and H.H. Wade: J. Vac. Sci Technol. B, 1991; vol. 9 (6), pp. 3451–55.CrossRefGoogle Scholar
  30. 30.
    M-Bond 600 Adhesive Manufacturer’s Literature, M-Line Accessories, Measurements Group, Inc., Raleigh, NC.Google Scholar
  31. 31.
    Randall M. German: Powder Metallurgy Science, 2nd ed., Metal Powder Industries Federation, Princeton, NJ, 1994, pp. 100–06.Google Scholar
  32. 32.
    T. Ishitani, K. Umemura, Y. Kawanami, and T. Ohnishi: J. Electrochem. Soc., 1989, vol. 136 (11), pp. 3502–05.CrossRefGoogle Scholar
  33. 33.
    M.H.F. Overwijk and F.C. van den Heuvel: Nucl. Instrum. Methods Phys. Res., 1993, sect. B, vol. 80, pp. 1324–27.CrossRefGoogle Scholar
  34. 34.
    H. Yamaguchi, A. Shimase, S. Haraaichi, and T. Miyauchi: J. Vac. Sci. Technol. B, 1985, vol. 3, pp. 71–74.CrossRefGoogle Scholar
  35. 35.
    FEI Focused Ion Beam Application Note, High Aspect Ratio Hole Drilling Using FIB Enhanced Etch Process, 1993.Google Scholar
  36. 36.
    J.F. Walker: Unpublished research.Google Scholar
  37. 37.
    L.A. Giannuzzi: Ph.D. Thesis, The Pennsylvania State University, University Park, PA, 1992.Google Scholar

Copyright information

© ASM International & TMS-The Minerals, Metals and Materials Society 1998

Authors and Affiliations

  • B. I. Prenitzer
    • 1
  • L. A. Giannuzzi
    • 1
  • K. Newman
    • 2
  • S. R. Brown
    • 3
  • R. B. Irwin
    • 3
  • F. A. Stevie
    • 3
  • T. L. Shofner
    • 4
  1. 1.the Department of Mechanical, Materials, and Aerospace EngineeringUniversity of Central FloridaOrlando
  2. 2.Process DevelopmentKeystone Powdered Metal CompanySt. Marys
  3. 3.Cirent SemiconductorOrlando
  4. 4.The Bartech GroupOrlando

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