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A Method for Directly Correlating Site-Specific Cross-Sectional and Plan-View Transmission Electron Microscopy of Individual Nanostructures

Published online by Cambridge University Press:  12 November 2012

Daniel K. Schreiber ,
Praneet Adusumilli ,
Eric R. Hemesath ,
David N. Seidman ,
Amanda K. Petford-Long  and
Lincoln J. Lauhon
Daniel K. Schreiber*
Affiliation:
Department of Materials Science and Engineering, Northwestern University, Evanston, IL 60208-3108, USA Materials Science Division, Argonne National Laboratory, Argonne, IL 60439, USA
Praneet Adusumilli
Affiliation:
Department of Materials Science and Engineering, Northwestern University, Evanston, IL 60208-3108, USA
Eric R. Hemesath
Affiliation:
Department of Materials Science and Engineering, Northwestern University, Evanston, IL 60208-3108, USA
David N. Seidman
Affiliation:
Department of Materials Science and Engineering, Northwestern University, Evanston, IL 60208-3108, USA Northwestern University Center for Atom-Probe Tomography, 2220 Campus Drive, Evanston, IL 60208-3108, USA
Amanda K. Petford-Long
Affiliation:
Department of Materials Science and Engineering, Northwestern University, Evanston, IL 60208-3108, USA Materials Science Division, Argonne National Laboratory, Argonne, IL 60439, USA Center for Nanoscale Materials, Argonne National Laboratory, Argonne, IL 60439, USA
Lincoln J. Lauhon
Affiliation:
Department of Materials Science and Engineering, Northwestern University, Evanston, IL 60208-3108, USA
*
*Corresponding author. E-mail: [email protected]
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Abstract

A sample preparation method is described for enabling direct correlation of site-specific plan-view and cross-sectional transmission electron microscopy (TEM) analysis of individual nanostructures by employing a dual-beam focused-ion beam (FIB) microscope. This technique is demonstrated using Si nanowires dispersed on a TEM sample support (lacey carbon or Si-nitride). Individual nanowires are first imaged in the plan-view orientation to identify a region of interest; in this case, impurity atoms distributed at crystalline defects that require further investigation in the cross-sectional orientation. Subsequently, the region of interest is capped with a series of ex situ and in situ deposited layers to protect the nanowire and facilitate site-specific lift-out and cross-sectioning using a dual-beam FIB microscope. The lift-out specimen is thinned to electron transparency with site-specific positioning to within ∼200 nm of a target position along the length of the nanowire. Using the described technique, it is possible to produce correlated plan-view and cross-sectional view lattice-resolved TEM images that enable a quasi-3D analysis of crystalline defect structures in a specific nanowire. While the current study is focused on nanowires, the procedure described herein is general for any electron-transparent sample and is broadly applicable for many nanostructures, such as nanowires, nanoparticles, patterned thin films, and devices.

Keywords

transmission electron microscopyfocused ion beamsample preparationnanowires
Type
Materials Applications
Information
Microscopy and Microanalysis , Volume 18 , Issue 6 , December 2012 , pp. 1410 - 1418
Copyright
Copyright © Microscopy Society of America 2012

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Footnotes

†

Current address: Pacific Northwest National Laboratory, Richland, WA 99352, USA

References

Allen, J.E., Hemesath, E.R., Perea, D.E., Lensch-Falk, J.L., Li, Z.Y., Yin, F., Gass, M.H., Wang, P., Bleloch, A.L., Palmer, R.E. & Lauhon, L.J. (2008). High-resolution detection of Au catalyst atoms in Si nanowires. Nat Nanotechnol 3, 168–173.Google Scholar
Bullis, W.M. (1966). Properties of gold in silicon. Solid State Electron 9, 143–168.Google Scholar
Davison, E. & Colquhoun, W. (1985). Ultrathin formvar support films for transmission electron-microscopy. J Electron Microsc Techniq 2, 35–43.CrossRefGoogle Scholar
De Veirman, A.E.M. (2003). ‘3-Dimensional’ TEM silicon-device analysis by combining plan-view and FIB sample preparation. Mat Sci Eng B-Solid 102, 63–69.CrossRefGoogle Scholar
Ercius, P., Gignac, L.M., Hu, C.K. & Muller, D.A. (2009). Three-dimensional measurement of line edge roughness in copper wires using electron tomography. Microsc Microanal 15, 244–250.Google Scholar
Fissel, A., Bugiel, E., Wang, C.R. & Osten, H.J. (2006). Formation of Si twinning-superlattice: First step towards Si polytype growth. Mat Sci Eng B-Solid 134, 138–141.Google Scholar
Giannuzzi, L.A. & Stevie, F.A. (1999). A review of focused ion beam milling techniques for TEM specimen preparation. Micron 30, 197–204.CrossRefGoogle Scholar
Gignac, L.M., Mittal, S., Bangsaruntip, S., Cohen, G.M. & Sleight, J.W. (2009). Precision, double XTEM sample preparation of site specific Si nanowires. Microsc Microanal 15(S2), 330–331CD.CrossRefGoogle Scholar
Gignac, L.M., Mittal, S., Bangsaruntip, S., Cohen, G.M. & Sleight, J.W. (2010). Multiple double XTEM sample preparation of sub-10 nm diameter Si nanowires. Microsc Microanal 16(S2), 168–169CD.CrossRefGoogle Scholar
Gignac, L.M., Mittal, S., Bangsaruntip, S., Cohen, G.M. & Sleight, J.W. (2011). Multiple double cross-section transmission electron microscope sample preparation of specific sub-10 nm diameter Si nanowire devices. Microsc Microanal 17, 889–895.Google Scholar
Hemesath, E.R., Schreiber, D.K., Gulsoy, E.B., Kisielowski, C.F., Petford-Long, A.K., Voorhees, P.W. & Lauhon, L.J. (2011). Catalyst incorporation at defects during nanowire growth. Nano Lett 12, 167–171.Google Scholar
Hemesath, E.R., Schreiber, D.K., Kisielowski, C.F., Petford-Long, A.K. & Lauhon, L.J. (2012). Atomic structural analysis of nanowire defects and polytypes enabled through cross-sectional lattice imaging. Small 201102404. CrossRefGoogle ScholarPubMed
Hertog, M.I.D., Cayron, C., Gentile, P., Dhalluin, F., Oehler, F., Baron, T. & Rouviere, J.L. (2012). Hidden defects in silicon nanowires. Nanotechnology 23, 025701. Google Scholar
Hillmann, L., Prang, R., Muhle, U. & Osterreicher, I. (2009). TEM preparation in three spatial directions for a defect analysis. Prakt Metallogr-Pr M 46, 292–302.Google Scholar
Ke, X.X., Bals, S., Cott, D., Hantschel, T., Bender, H. & Van Tendeloo, G. (2010). Three-dimensional analysis of carbon nanotube networks in interconnects by electron tomography without missing wedge artifacts. Microsc Microanal 16, 210–217.Google Scholar
Langford, R.M. (2006). Focused ion beams techniques for nanomaterials characterization. Microsc Res Techniq 69, 538–549.Google Scholar
Langford, R.M., Ozkaya, D., Huey, B. & Petford-Long, A.K. (2001a). Broad ion beam milling of focused ion beam prepared transmission electron microscopy cross-section specimens for high resolution electron microscopy using silicon support membranes. Microsc Semicond Mater 2001, 511–514.Google Scholar
Langford, R.M., Ozkaya, D., Kaufman, C., Gledhill, S., Dobson, P.J. & Petford-Long, A.K. (2001b). Assessment of different focused ion beam milling conditions for the preparation of TEM cross-sections for high-resolution electron microscopy. Electron Microsc Anal 2001, 437–440.Google Scholar
Lawrence, D., Alvis, R. & Olson, D. (2008). Specimen preparation for cross-section atom probe analysis. Microsc Microanal 14(S2), 1004–1005CD.CrossRefGoogle Scholar
Lopez, F.J., Hemesath, E.R. & Lauhon, L.J. (2009). Ordered stacking fault arrays in silicon nanowires. Nano Lett 9, 2774–2779.Google Scholar
Mayer, J., Giannuzzi, L.A., Kamino, T. & Michael, J. (2007). TEM sample preparation and FIB-induced damage. MRS Bull 32, 400–407.Google Scholar
Midgley, P.A. & Weyland, M. (2003). 3D electron microscopy in the physical sciences: The development of Z-contrast and EFTEM tomography. Ultramicroscopy 96, 413–431.CrossRefGoogle ScholarPubMed
Phatak, C., Petford-Long, A.K. & De Graef, M. (2010). Three-dimensional study of the vector potential of magnetic structures. Phys Rev Lett 104, 253901. Google Scholar
Rittner, J.D. & Seidman, D.N. (1997). Solute-atom segregation to ⟨110⟩ symmetric tilt grain boundaries. Acta Mater 45, 3191–3202.Google Scholar
Schmidt, V., Wittemann, J.V., Senz, S. & Gosele, U. (2009). Silicon nanowires: A review on aspects of their growth and their electrical properties. Adv Mater 21, 2681–2702.Google Scholar
Schwalbach, E.J. & Voorhees, P.W. (2008). Phase equilibrium and nucleation in VLS-grown nanowires. Nano Lett 8, 3739–3745.Google Scholar
Sprokel, G.J. & Fairfiel, J.M. (1965). Diffusion of gold into silicon crystals. J Electrochem Soc 112, 200–203.Google Scholar
Sugiyama, M. & Sigesato, G. (2004). A review of focused ion beam technology and its applications in transmission electron microscopy. J Electron Microsc 53, 527–536.Google Scholar
Thompson, K., Lawrence, D., Larson, D.J., Olson, J.D., Kelly, T.F. & Gorman, B. (2007). In situ site-specific specimen preparation for atom probe tomography. Ultramicroscopy 107, 131–139.Google Scholar
Wagner, R.S. & Ellis, W.C. (1964). Vapor-liquid-solid mechanism of single crystal growth (new method growth catalysis from impurity whisker epitaxial + large crystals Si E). Appl Phys Lett 4, 89–90.Google Scholar
Ziegler, J.F., Biersack, J.P. & Littmark, U. (1985). The Stopping and Range of Ions in Solids. New York: Pergamon.Google Scholar