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Convenient Preparation of High-Quality Specimens for Annealing Experiments in the Transmission Electron Microscope

  • Martial Duchamp (a1), Qiang Xu (a2) (a3) and Rafal E Dunin-Borkowski (a1)

Abstract

A procedure based on focused ion beam milling and in situ lift-out is introduced for the preparation of high-quality specimens for in situ annealing experiments in the transmission electron microscope. The procedure allows an electron-transparent lamella to be cleaned directly on a heating chip using a low ion energy and back-side milling in order to minimize redeposition and damage. The approach is illustrated through the preparation of an Al–Mn–Fe complex metallic alloy specimen.

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Corresponding author

* Corresponding author. martial.duchamp@gmail.com

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Balanetshyy, S., Meisterernst, G. & Feuerbacher, M. (2011). The Al-rich region of the Al-Mn-Ni alloy sytem. Part I: Ternary phases at the 750-950°C. J Alloys Compd 209, 37873794.
Dunin-Borkowski, R.E., Newcomb, S.B., Kasama, T., McCartney, M.R., Weyland, M. & Midgley, P.A. (2005). Conventional and back-side focused ion beam milling for off-axis electron holography of electrostatic potentials in transistors. Ultramicroscopy 103, 6781.
FEI Company, xT (2003). Nova NanoLab User’s Manual (1st ed.). Eindhoven: FEI Company, xT. pp. 5–57.
Field, R.D. & Papin, P.A. (2004). Location specific in situ TEM straining specimens made using FIB. Ultramicroscopy 102, 2326.
Figuerola, A., van Huis, M., Zanella, M., Genovese, A., Marras, S., Falqui, A., Zandbergen, H.W., Cingolani, R. & Manna, L. (2010). Epitaxial CdSe-Au nanocrystal heterostructures by thermal annealing. Nano Lett 10, 30283036.
Giannuzzi, L.A., Drown, J.L., Brown, S.R., Irwin, R.B. & Stevie, F.A. (1997). Focused ion beam milling and micromanipulation lift-out for site specific cross-section TEM specimen preparation. Mater Res Soc Symp Proc 480, 1927.
Harlow, W., Ghassemi, H. & Taheri, M.L. (2014). In-situ TEM study of the corrosion behavior of Zry-4. Microsc Microanal 20(Suppl 3), 16021603.
Heggen, M., Houben, L. & Feuerbacher, M. (2010). Plastic deformation mechanism in complex solids. Nat Mater 9, 332336.
Heggen, M., Houben, L. & Feuerbacher, M. (2011). Metadislocations in complex metallic alloys T-Al-Mn- (Pd, Fe). Acta Mater 59, 44584466.
Jeangros, Q., Faes, A., Wagner, J.B., Hansen, T.W., Van Herle, J., Hessler-Wyser, A. & Dunin-Borkowski, R.E. (2010). In situ redox cycle of a nickel-YSZ fuel cell anode in an environmental transmission electron microscope. Acta Mater 58, 45784589.
Kempshall, B.W., Schwarzx, B.W. & Giannuzzi, L. (2002). In situ FIB lift-out for site specific TEM specimen preparation of grain boundaries and interfaces. Int Congress Electron Microsc Durban South Africa Proc 1, 249.
Langford, R.M., Huang, Y.Z., Lozano-Perez, S., Titchmarsh, J.M. & Petford-long, A.K. (2001). Preparation of site specific transmission electron microscopy plan-view specimens using a focused ion beam system. J Vacuum Sci Technol B 19, 755758.
Langford, R.M. & Petford-Long, A.K. (2000). Preparation of transmission electron microscopy cross-section specimens using focused ion beam milling. J Vacuum Sci Technol A 19, 21862193.
Legros, M., Dehm, G., Keller-Flaig, R.M., Arzt, E., Hemker, K.J. & Suresh, S. (2001). Dynamic observation of Al thin films plastically strained in a TEM. Mater Sci Eng A 463, 309310.
Longworth, H.P. & Thompson, C.V. (1991). Abnormal grain growth in aluminum alloy thin films. J Appl Phys 69, 39293940.
Orloff, J., Utlaut, M. & Swanson, L. (2003). High Resolution Focused Ion Beams: FIB and its Applications, 1st ed. New York, NY: Kluwer Academic/Plenum Publishers.
Radulescu, F., McCarthy, J.M. & Stach, E. (2000). In situ annealing transmission electron microscopy study of Pd/Ge/Pd/GaAs interfacial reactions. Mater Res Soc Symp Proc 589, 179184.
Ramasse, Q., Anapolsky, A., Lazik, C., Jin, M., Armstrong, K. & Wang, D. (2009). Atomic scale observation and characterization of redox-induced interfacial layers in commercial Si thin film photovoltaics. J Appl Phys 105, 033716.
Rogers, M., Kothleitner, G., Berendes, A., Bock, W. & Kolbesen, B.O. (2005). Focused ion beam preparation and EFTEM/EELS studies of vanadium nitride thin films. Pract Metallography 42, 172187.
Schaffer, M., Schaffer, B. & Ramasse, Q. (2012). Sample preparation for atomic-resolution STEM at low voltages by FIB. Ultramicroscopy 114, 6271.
van Huis, M.A., Kunneman, L.T., Overgaag, K., Xu, Q., Pandraud, G., Zandbergen, H.W. & Vanmaekelbergh, D.L. (2008). Low-temperature nanocrystal unification through rotations and relaxations probed by in situ transmission electron microscopy. Nano Lett 8, 39593963.
van Huis, M.A., Young, N.P., Pandraud, G., Creemer, J.F., Vanmaekelbergh, D., Kirkland, A.I. & Zandbergen, H.W. (2009). Atomic imaging of phase transitions and morphology transformations in nanocrystals Adv Mater 21, 49924995.
Venkatraman, R., Bravman, J.C., Nix, W.D., Davies, P.W., Flinn, P.A. & Fraser, D.B. (1990). Mechanical properties and microstructural characterization of AI-0.5%Cu thin films. J Electron Mater 19, 12311237.
Xu, Q., Wu, M.Y., Schneider, G.F., Houben, L., Malladi, S.K., Dekker, C., Yucelen, E., Dunin-Borkowski, R.E. & Zandbergen, H.W. (2013). Controllable atomic scale patterning of freestanding monolayer graphene at elevated temperature. ACS Nano 7, 15661572.
Zheng, P., Ruault, M.O., Denanot, M.F., Descouts, B. & Krauz, P. (1991). In situ thermal annealing of InP amorphous layer induced by Si+ implantation. J Appl Phys 69, 197202.

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Convenient Preparation of High-Quality Specimens for Annealing Experiments in the Transmission Electron Microscope

  • Martial Duchamp (a1), Qiang Xu (a2) (a3) and Rafal E Dunin-Borkowski (a1)

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