Hostname: page-component-848d4c4894-2xdlg Total loading time: 0 Render date: 2024-07-07T14:06:10.309Z Has data issue: false hasContentIssue false
  • English
  • Français

Transmission Electron Microscopy Specimen Preparation Method for Multiphase Porous Functional Ceramics

Published online by Cambridge University Press:  13 February 2013

W. Zhang ,
L. Theil Kuhn ,
P.S. Jørgensen ,
K. Thydén ,
J.J. Bentzen ,
E. Abdellahi ,
B.R. Sudireddy ,
M. Chen  and
J.R. Bowen
W. Zhang*
Affiliation:
Department of Energy Conversion and Storage, Technical University of Denmark, Risø campus, Frederiksborgvej 399, 4000 Roskilde, Denmark
L. Theil Kuhn
Affiliation:
Department of Energy Conversion and Storage, Technical University of Denmark, Risø campus, Frederiksborgvej 399, 4000 Roskilde, Denmark
P.S. Jørgensen
Affiliation:
Department of Energy Conversion and Storage, Technical University of Denmark, Risø campus, Frederiksborgvej 399, 4000 Roskilde, Denmark
K. Thydén
Affiliation:
Department of Energy Conversion and Storage, Technical University of Denmark, Risø campus, Frederiksborgvej 399, 4000 Roskilde, Denmark
J.J. Bentzen
Affiliation:
Department of Energy Conversion and Storage, Technical University of Denmark, Risø campus, Frederiksborgvej 399, 4000 Roskilde, Denmark
E. Abdellahi
Affiliation:
Department of Energy Conversion and Storage, Technical University of Denmark, Risø campus, Frederiksborgvej 399, 4000 Roskilde, Denmark
B.R. Sudireddy
Affiliation:
Department of Energy Conversion and Storage, Technical University of Denmark, Risø campus, Frederiksborgvej 399, 4000 Roskilde, Denmark
M. Chen
Affiliation:
Department of Energy Conversion and Storage, Technical University of Denmark, Risø campus, Frederiksborgvej 399, 4000 Roskilde, Denmark
J.R. Bowen
Affiliation:
Department of Energy Conversion and Storage, Technical University of Denmark, Risø campus, Frederiksborgvej 399, 4000 Roskilde, Denmark
*
*Corresponding author. E-mail: [email protected], [email protected]
Get access

Abstract

An optimum method is proposed to prepare thin foil transmission electron microscopy (TEM) lamellae of multiphase porous functional ceramics: prefilling the pore space of these materials with an epoxy resin prior to focused ion beam milling. Several advantages of epoxy impregnation are demonstrated by successful preparation of TEM specimens that maintain the structural integrity of the entire lamella. Feasibility of the TEM alignment procedure is demonstrated, and ideal TEM analyses are illustrated on solid oxide fuel cell and solid oxide electrolysis cell materials. Some potential drawbacks of the TEM specimen preparation method are listed for other samples.

Keywords

porous ceramic compositesepoxyTEMFIB
Type
Software, Techniques, and Equipment Development: Short Communications
Information
Microscopy and Microanalysis , Volume 19 , Issue 2 , April 2013 , pp. 501 - 505
Copyright
Copyright © Microscopy Society of America 2013

Access options

Get access to the full version of this content by using one of the access options below. (Log in options will check for institutional or personal access. Content may require purchase if you do not have access.)

References

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, 80–86.CrossRefGoogle ScholarPubMed
Bassim, N.D. & Twigg, M.E. (2005). Technique for site-specific plan-view transmission electron microscopy of nanostructural electronic devices. J Vac Sci Tech 23(3), 1107–1109.Google Scholar
Cronin, J.S., Wilson, J.R. & Barnett, S.A. (2011). Impact of pore microstructure evolution on polarization resistance of Ni-Yttria-stabilized zirconia fuel cell anodes. J Power Sources 196(5), 2640–2643.Google Scholar
Dieterle, L., Butz, B. & Müller, E. (2011). Optimized Ar(+)-ion milling procedure for TEM cross-section sample preparation. Ultramicroscopy 111, 1636–1644.Google Scholar
Egerton, R.F. (1996). Electron Energy Loss Spectroscopy in the Electron Microscope, 2nd ed. New York: Plenum.Google Scholar
Gostovic, D., Vito, N.J., O'Hara, K.A., Jones, K.S. & Wachsman, E.D. (2011). Microstructure and connectivity quantification of complex composite solid oxide fuel cell electrode three-dimensional networks. J Am Ceram Soc 94(2), 620–627.Google Scholar
Hoeven, S.V.D., Dekker, A.D. & Tejada, A. (2009). Alignment control of STEM: A ronchigram based approach. Microsc Microanal 15(S2), 118–119.Google Scholar
Jensen, S.H., Larsen, P.H. & Mogensen, M. (2007). Hydrogen and synthetic fuel production from renewable energy sources. Int J Hydrogen Energy 32, 3253–3257.Google Scholar
Liu, J. (2005). Scanning transmission electron microscopy and its application to the study of nanoparticles and nanoparticle systems. J Electron Microsc 54(3), 251–278.Google Scholar
Liu, Y. & Jiao, C. (2005). Microstructure degradation of an anode/electrolyte interface in SOFC studied by transmission electron microscopy. Solid State Ionics 176, 435–442.Google Scholar
Luft, J.H. (1961). Improvements in epoxy resin embedding methods. J Biophys Biochem Cytol 9(2), 409–414.Google Scholar
Minh, N.Q. (1993). Ceramic fuel cells. J Am Ceram Soc 76(3), 563–588.Google Scholar
Mohammed Hussain, A., Høgh, J.V.T., Zhang, W. & Bonanos, N. (2012). Efficient ceramic anodes infiltrated with binary and ternary electrocatalysts for SOFCs operating at low temperatures. J Power Sources 216, 308–313.Google Scholar
Phelps, J.M. (2005). Cross-section sample preparation of a free-standing thin-film coupon for transmission electron microscopy analysis. Microsc Microanal 4, 128–132.Google Scholar
Sivel, V.G.M., Van Den Brand, J., Wang, W.R., Mohdadi, H., Tichelaar, F.D., Alkemade, P.F.A. & Zandbergen, H.W. (2004). Application of the dual-beam FIB/SEM to metals research. J Microsc 214(Pt 3), 237–245.Google Scholar
Studart, A.R., Gonzenbach, U.T., Tervoort, E. & Gauckler, L.J. (2006). Processing routes to macroporous ceramics: A review. J Am Ceram Soc 89(6), 1771–1789.Google Scholar
Thydén, K. (2008). Microstructural degradation of Ni-YSZ anodes for solid oxide fuel cells. PhD Thesis. Denmark: Risø-PhD-32 (EN). Google Scholar
Wiedenmann, D., Hauch, A., Grobéty, B., Mogensen, M. & Vogt, U.F. (2010). Complementary techniques for solid oxide electrolysis cell characterisation at the micro- and nano-scale. Int J Hydrogen Energy 35(10), 5053–5060.Google Scholar
Wilson, J.R., Duong, A.T., Gameiro, M., Chen, H.-Y., Thornton, K., Mumm, D.R. & Barnett, S.A. (2009). Quantitative three-dimensional microstructure of a solid oxide fuel cell cathode. Electrochem Comm 11, 1052–1056.Google Scholar
Zhang, W., Liu, Z.-Q. & Furuya, K. (2008). Fabrication and characterization of cellular iron nanocrystalline film. Nanotechnology 19, 135302. Google Scholar