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Alternative FIB TEM Sample Preparation Method for Cross-Sections of Thin Metal Films Deposited on Polymer Substrates

  • Felipe Rivera (a1), Robert Davis (a1) and Richard Vanfleet (a1)
Abstract

Transmission electron microscopy (TEM) and focused ion beam (FIB) are proven tools to produce site-specific samples in which to study devices from initial processing to causes for failure, as well as investigating the quality, defects, interface layers, etc. However, the use of polymer substrates presents new challenges, in the preparation of suitable site-specific TEM samples, which include sample warping, heating, charging, and melting. In addition to current options that address some of these problems such as cryo FIB, we add an alternative method and FIB sample geometry that address these challenges and produce viable samples suitable for TEM elemental analysis. The key feature to this approach is a larger than usual lift-out block into which small viewing windows are thinned. Significant largely unthinned regions of the block are left between and at the base of the thinned windows. These large unthinned regions supply structural support and thermal reservoirs during the thinning process. As proof-of-concept of this sample preparation method, we also present TEM elemental analysis of various thin metallic films deposited on patterned polycarbonate, lacquer, and poly-di-methyl-siloxane substrates where the pattern (from low- to high-aspect ratio) is preserved.

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Corresponding author
* Corresponding author. E-mail: rrv3@physics.byu.edu
References
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Aubry, C. (2002). Polymer gratings achieved by focused ion beam. Synth Met 127, 307311.
Bals, S., Tirry, W., Geurts, R., Yang, Z. & Schryvers, D. (2007). High-quality sample preparation by low kV FIB thinning for analytical TEM measurements. Microsc Microanal 13, 8086.
Biance, A., Gierak, J., Bourhis, E., Madouri, A., Lafosse, X., Patriarche, G., Oukhaled, G., Ulysse, C., Galas, J. & Chen, Y. (2006). Focused ion beam sculpted membranes for nanoscience tooling. Microelectron Eng 83, 14741477.
Brostow, W., Gorman, B. & Olea-Meija, O. (2007). Focused ion beam milling and scanning electron microscopy characterization of polymer+metal hybrids. Mater Lett 61, 13331336.
Da Silva, M.M., Vaz, A.R., Moshkalev, S.A. & Swart, J.W. (2007). Electrical characterization of platinum thin films deposited by focused ion beam. ECS Trans 9, 235241.
de Winter, D.A.M. & Mulders, J.J.L. (2007). Redeposition characteristics of focused ion beam milling for nanofabrication. J Vacuum Sci Tech B 25, 22152218.
de Winter, D., Schneijdenberg, C., Lebbink, M., Hekking, L., Post, J., Lich, B., Verkleij, A., Drury, M. & Humbel, B. (2009). Tomography of biological materials using focused ion beam sectioning and backscattered electron imaging. Microsc Microanal 15 (Suppl 2), 576577.
Floresca, H.C., Jeon, J., Wang, J.G. & Kim, M.J. (2009). The focused ion beam fold-out: sample preparation method for transmission electron microscopy. Microsc Microanal 15, 558563.
Fujii, T., Iwasaki, K., Munekane, M., Takeuchi, T., Hasuda, M., Asahata, T., Kiyohara, M., Kogure, T., Kijima, Y. & Kaito, T. (2005). A nanofactory by focused ion beam. J Micromech Microeng 15, S286S291.
Giannuzzi, L.A. (1999). A review of focused ion beam milling techniques for TEM specimen preparation. Micron 30, 197204.
Hamley, I.W. & Castelletto, V. (2007). Biological soft materials. Angew Chem Int Ed Engl 46, 44424455.
Hata, S., Sosiati, H., Kuwano, N., Itakura, M., Nakano, T. & Umakoshi, Y. (2006). Removing focused ion-beam damages on transmission electron microscopy specimens by using a plasma cleaner. J Electron Microsc (Tokyo) 55, 2326.
Jiang, G., Rivera, F., Kanyal, S.S., Davis, R.C., Vanfleet, R., Lunt, B.M. & Linford, M.R. (2010). Analysis of the plastic substrates, the reflective layers, and the adhesives of today's archival-grade DVDs. Proc. SPIE 7730, Optical Data Storage 2010, 77301N
Jiang, G., Rivera, F., Kanyal, S.S., Davis, R.C., Vanfleet, R., Lunt, B.M., Shutthanandan, V. & Linford, M.R. (2011). Characterization of the plastic substrates, the reflective layers, the adhesives, and the grooves of today's archival-grade recordable DVDs. Opt Eng 50, 015201.
Kim, S., Jeong Park, M., Balsara, N.P., Liu, G. & Minor, A.M. (2011). Minimization of focused ion beam damage in nanostructured polymer thin films. Ultramicroscopy 111, 191199.
Kirk, E.C.G., Cleaver, J.R.A. & Ahmed, H. (1987). In situ microsectioning and imaging of semiconductor devices using a scanning ion microscope. In Microscopy of Semiconducting Materials, 1987, Cullis, A.G. & Augustus, P.D. (Eds.), pp. 691696. London: Institute of Physics.
Ko, D.-S., Park, Y.M., Kim, S.D. & Kim, Y.W. (2007). Effective removal of Ga residue from focused ion beam using a plasma cleaner. Ultramicroscopy 107, 368373.
Kooi, S. (2008). Focused ion beam processing of polymeric materials for analytical sample preparation. Microsc Microanal 14, 688689.
Langford, R.M. (2006). Focused ion beam nanofabrication: a comparison with conventional processing techniques. J Nanosci Nanotechno 6, 661668.
Latif, A. (2005). Nanofabrication Using Focused Ion Beam. Cambridge, UK: University of Cambridge.
Li, J., Malis, T. & Dionne, S. (2006). Recent advances in FIB TEM specimen preparation techniques. Mater Characterization 57, 6470.
Longo, D. (1999). Experimental method for determining Cliff–Lorimer factors in transmission electron microscopy (TEM) utilizing stepped wedge-shaped specimens prepared by focused ion beam (FIB) thinning. Ultramicroscopy 80, 8597.
Magni, S., Milani, M., Riccardi, C. & Tatti, F. (2007). FIB/SEM characterization of carbon-based fibers. Scanning 29, 185195.
Mahoney, C., Fahey, A., Gillen, G., Xu, C. & Batteas, J. (2006). Temperature-controlled depth profiling in polymeric materials using cluster secondary ion mass spectrometry (SIMS). Appl Surf Sci 252, 65026505.
Matsui, S. & Ochiai, Y. (1996). Focused ion beam applications to solid state devices. Nanotech 7, 247258.
Melngailis, J. (1993). Focused ion beam lithography. Nucl Instrum Methods Phys Res Sect B 8081, 12711280.
Minor, A. (2009). FIB sample preparation of thin films and soft materials. Microsc Microanal 15(Suppl 2), 15441545.
Moon, M.-W., Han, J.H., Vaziri, A., Her, E.K., Oh, K.H., Lee, K.-R. & Hutchinson, J.W. (2009). Nanoscale ripples on polymers created by a focused ion beam. Nanotech 20, 115301.
Moon, M.-W., Lee, S.H., Sun, J.-Y., Oh, K.H., Vaziri, A. & Hutchinson, J.W. (2007). Wrinkled hard skins on polymers created by focused ion beam. Proc Natl Acad Sci USA 104, 11301133.
Munroe, P.R. (2009). The application of focused ion beam microscopy in the material sciences. Mater Characterization 60, 213.
Nagamachi, S., Yamakage, Y., Ueda, M., Maruno, H. & Ishikawa, J. (1996). Focused ion-beam direct deposition of metal thin film. Rev Sci Instrum 67, 23512359.
Nassar, R. (1998). Mathematical modeling of focused ion beam microfabrication. J Vacuum Sci & Tech B 16, 109115.
Nellen, P.M., Callegari, V. & Sennhauser, U. (2006). Preparative methods for nanoanalysis of materials with focused ion beam instruments. CHIMIA Int J Chem 60, 735741.
Pei, L., Balls, A., Tippets, C., Abbott, J., Linford, M., Hu, J., Madan, A., Allred, D., Vanfleet, R. & Davis, R. (2011). Polymer molded templates for nanostructured amorphous silicon photovoltaics. J Vacuum Sci & Tech A 29(2), 021017.
Peterson, B.L. (2008). TEM sample preparation tips. FEI company application notes. Available at http://www.fei.com/uplaodedfiles/documentsprivate/content/tem_sample_prep.pdf.
Repetto, L., Buzio, R., Denurchis, C., Firpo, G., Piano, E. & Valbusa, U. (2009). Fast three-dimensional nanoscale metrology in dual-beam FIB-SEM instrumentation. Ultramicroscopy 109, 13381342.
Russell, P.E. (1998). Chemically and geometrically enhanced focused ion beam micromachining. J Vacuum Sci & Tech B 16, 24942498.
Russell, P.E. & Stevie, F.A. (2002). Focused ion beam (FIB) microscopy and technology. Microsc Microanal 8, 558559.
Schaffer, B., Mitterbauer, C., Schertel, A., Pogantsch, A., Rentenberger, S., Zojer, E. & Hofer, F. (2004). Cross-section analysis of organic light-emitting diodes. Ultramicroscopy 101, 123128.
Schmidt, F., Kühbacher, M., Gross, U., Kyriakopoulos, A., Schubert, H. & Zehbe, R. (2011). From 2D slices to 3D volumes: Image based reconstruction and morphological characterization of hippocampal cells on charged and uncharged surfaces using FIB/SEM serial sectioning. Ultramicroscopy 111, 259266.
Spoenak, R., Sauter, L. & Eberl, C. (2005). Reversible orientation-biased grain growth in thin metal films induced by a focused ion beam. Scripta Mater 53, 12911296.
Stokes, D.J.J., Morrissey, F. & Lich, B.H. (2006). A new approach to studying biological and soft materials using focused ion beam scanning electron microscopy (FIB SEM). J Phys: Conf Ser 26, 5053.
Stokes, D.J., Wilhelmi, O., Reyntjens, S., Jiao, C. & Roussel, L. (2009). New methods for the study and fabrication of nano-structured materials using FIB SEM. J Nanosci Nanotechnol 9, 12681271.
Thangaduraii, P., Lumelsky, Y., Silverstein, M. & Kaplan, W. (2008). TEM specimen preparation of semiconductor—PMMA—metal interfaces. Mater Character 59, 16231629.
Thompson, L.E., Rice, P.M., Delenia, E., Lee, V.Y., Brock, P.J., Magbitang, T.P., Dubois, G., Volksen, W., Miller, R.D. & Kim, H.-C. (2006). Imaging thin films of nanoporous low-k dielectrics: comparison between ultramicrotomy and focused ion beam preparations for transmission electron microscopy. Microsc Microanal 12, 156159.
Tjerkstra, R.W., Segerink, F.B., Kelly, J.J. & Vos, W.L. (2008). Fabrication of three-dimensional nanostructures by focused ion beam milling. J Vacuum Sci Tech B 26, 973977.
Volkert, C.A. & Minor, A.M. (2007). Focused ion beam microscopy and micromachining. MRS Bull 32, 389399.
Yao, N. (2007). Focused Ion Beam Systems. Cambridge, UK: Cambridge University Press.
Yogev, S., Levin, J., Molotskii, M., Schwarzman, A., Avayu, O. & Rosenwaks, Y. (2008). Charging of dielectrics under focused ion beam irradiation. J Appl Phys 103, 064107.
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