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TEM of Sub-Micrometer Particles using the FIB Lift-Out Technique

Published online by Cambridge University Press:  02 July 2020

Janice K. Lomness ,
Brian W. Kempshall ,
Lucille A. Giannuzzi  and
Mark B. Watson
Janice K. Lomness
Affiliation:
Advanced Materials Processing and Analysis Center, Mechanical Materials & Aerospace Engineering, Orlando, FL, 32816.
Brian W. Kempshall
Affiliation:
Advanced Materials Processing and Analysis Center, Mechanical Materials & Aerospace Engineering, Orlando, FL, 32816.
Lucille A. Giannuzzi
Affiliation:
Advanced Materials Processing and Analysis Center, Mechanical Materials & Aerospace Engineering, Orlando, FL, 32816.
Mark B. Watson
Affiliation:
Millennium Inorganic Chemical, 6752 Baymeadow Dr., Glen Burnie, MD, 21060
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Abstract

The ability to acquire TEM specimens from micrometer sized particles using an innovative FIB LO technique has been previously demonstrated [1-3]. This technique allowed for the preparation of a TEM LO specimen from regions which were smaller than the conventional dimensions of the LO specimen (∼5 μm × 20 μm). This paper shows how the LO technique previously developed for the preparation of micrometer sized particles [3] may be extended and utilized for the preparation of submicrometer sized particles for TEM analysis.

In this study, TiO2 particles on the order of 200 nm in width were investigated. A small portion of the TiO2 particles was dusted onto double stick carbon tape adhered to a sample stud and then sputtered coated with Au-Pd to protect the outer surface from FIB imaging. The sample stud containing the TiO2 particles was placed in an FEI 200TEM FIB workstation. Figure 1 is a FIB image of the Ti02 particles of interest. Gaps around these particles were deposited with Pt using the FIB assisted CVD process as shown in Figure 2. in this procedure, the Pt acts as a “weld” to hold the particles together, and to allow for a larger region to be milled (e.g., >10 μm) for subsequent specimen preparation.

Type
Applications and Developments of Focused Ion Beam (FIB) Instruments (Organized by L. Giannuzzi)
Information
Microscopy and Microanalysis , Volume 7 , Issue S2: Proceedings: Microscopy & Microanalysis 2001, Microscopy Society of America 59th Annual Meeting, Microbeam Analysis Society 35th Annual Meeting, Long Beach, California August 5-9, 2001 , August 2001 , pp. 950 - 951
Copyright
Copyright © Microscopy Society of America 2001

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References

references

1.Giannuzzi, et al., Microscopy Research and Technique,41 (1998) 285.3.0.CO;2-Q>CrossRefGoogle ScholarPubMed
2.Prenitzer, et al., Metall. and Mats. Trans. A., SEP 01 (1998) v29 n 9, p2399.CrossRefGoogle Scholar
3.Lomness, et al., Microsc. Microanal. 6 (suppl 2: Proceedings), MSA 2000, 518.CrossRefGoogle Scholar
4. The support of the Florida Space Grant Consortium and NSF DMR 9703281 is greatly appreciated. A special thanks to Cirent Semiconductor for their instrumentation support.Google Scholar