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Quantitative Energy-Dispersive X-Ray Analysis of Catalyst Nanoparticles Using a Partial Cross Section Approach

  • Katherine E. MacArthur (a1), Thomas J. A. Slater (a2), Sarah J. Haigh (a2), Dogan Ozkaya (a3), Peter D. Nellist (a1) and Sergio Lozano-Perez (a1)...
Abstract

The new generation of energy-dispersive X-ray (EDX) detectors with higher count rates than ever before, paves the way for a new approach to quantitative elemental analysis in the scanning transmission electron microscope. Here we demonstrate a method of calculating partial cross sections for use in quantifying EDX data, beneficial especially because of the simplicity of its implementation. Applying this approach to acid-leached PtCo catalyst nanoparticles leads to quantitative determination of the Pt surface enrichment.

Copyright
© Microscopy Society of America 2016 
Corresponding author
*Corresponding author.k.macarthur@oxon.org
References
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Allen, L.J., D’Alfonso, A.J., Freitag, B. & Klenov, D.O. (2012). Chemical mapping at atomic resolution using energy-dispersive X-ray spectroscopy. MRS Bull 37, 47–52.
Batson, P.E., Dellby, N. & Krivanek, O.L. (2002). Sub-Ångstrom resolution using aberration corrected electron optics. Nature 418, 617–620.
Cliff, G. & Lorimer, G.W. (1975). The quantitative analysis of thin specimens. J Microsc 103, 203–207.
E., H., MacArthur, K.E., Pennycook, T.J., Okunishi, E., D’Alfonso, A.J., Lugg, N.R., Allen, L.J. & Nellist, P.D. (2013). Probe integrated scattering cross sections in the analysis of atomic resolution HAADF STEM images. Ultramicroscopy 133, 109–119.
Egerton, R.F. (2011). Electron Energy Loss Spectroscopy in the Electron Microscope, 3rd ed. New York: Springer.
Genc, A., Kovarik, L., Gu, M., Cheng, H., Plachinda, P., Pullan, L., Freitag, B. & Wang, C. (2013). XEDS STEM tomography for 3D chemical characterization of nanoscale particles. Ultramicroscopy 131, 24–32.
Goldstein, J.I., Costley, J.L., Lorimer, G.W. & Reed, R.J.B. (1977). Quantitative X-ray analysis in the electron microscope. In Scanning Electron Microscopy, vol. 1, Johari, O (Ed.), pp. 315–324. Chicago: IIT Research Institute.
Goldstein, J., Newbury, D.E., Joy, D.C., Lyman, C.E., Echlin, P., Lifshin, E., Sawyer, L. & Michael, J.R. (2003). Scanning Electron Microscopy and X-Ray Microanalysis, 3rd ed. New York, USA: Springer US.
Hofer, F. (1991). Determination of inner-shell cross sections for EELS-quantification. Microsc Microanal Microstruct 2, 215–230.
Iakoubovskii, K., Mitsuishi, K., Nakayama, Y. & Furuya, K. (2008). Thickness measurements with electron energy loss spectroscopy. Microsc Res Tech 71, 626–631.
Itakura, M., Watanabe, N., Nishida, M., Daio, T. & Matsumura, S. (2013). Atomic-resolution X-ray energy-dispersive spectroscopy chemical mapping of substitutional Dy atoms in a high-coercivity neodymium magnet. Jpn J Appl Phys 52, 050201.
Jones, L., MacArthur, K.E., Fauske, V.T., van Helvoort, A.T.J. & Nellist, P.D. (2014). Rapid estimation of catalyst nanoparticle morphology and atomic-coordination by high-resolution z-contrast electron microscopy. Nano Lett 14, 6336–6341.
Kothleitner, G., Neish, M.J., Lugg, N.R., Findlay, S.D., Grogger, W., Hofer, F. & Allen, L.J. (2014). Quantitative elemental mapping at atomic resolution using X-ray spectroscopy. Phys Rev Lett 112, 085501.
Kotula, P.G., Klenov, D.O. & Von Harrach, H.S. (2012). Challenges to quantitative multivariate statistical analysis of atomic-resolution X-ray spectral. Microsc Microanal 18, 691–698.
Krivanek, O.L., Dellby, N., Spence, A.J., Camps, R.A. & Brown, L.M. (1997). Aberration correction in the STEM. Electron Microsc Anal 153, 35–40.
Lechner, P., Fiorini, C., Hartmann, R., Kemmer, J., Krause, N., Leutenegger, P., Longoni, A., Soltau, H., Stotter, D., Stotter, R., Struder, L. & Weber, U. (2001). Silicon drift detectors for high count rate X-ray spectroscopy at room temperature. Nucl Instrum Methods Phys Res A 458, 281–287.
Liu, Z., Ma, L., Zhang, J.Y., Hongsirikarn, K. & Goodwin, J.G. (2013). Pt alloy electrocatalysts for proton exchange membrane fuel cells: A review. Catal Rev 55, 255–288.
Lugg, N.R., Kothleitner, G., Shibata, N. & Ikuhara, Y. (2014). On the quantitativeness of EDS STEM. Ultramicroscopy 151, 150–159.
MacArthur, K.E., Alfonso, A.J.D., Ozkaya, D., Allen, L.J. & Nellist, P.D. (2015). Optimal ADF STEM imaging parameters for tilt-robust image quantification. Ultramicroscopy 156, 1–8.
Maher, D.M., Joy, D.C., Ellington, M.B., Zaluzec, N.J. & Mochel, P.E. (1981). Relative accuracy of k-factor calculations for thin-film X-ray analysis. In Analytical Electron Microscopy, Geiss, R.H. (Ed.), pp. 33--38. San Francisco: San Francisco Press.
Malis, T., Cheng, S.C. & Egerton, R.F. (1988). EELS log-ratio technique for specimen-thickness measurement in the TEM. J Electron Microsc Tech 8, 193–200.
Meltzman, H., Kauffmann, Y., Thangadurai, P., Drozdov, M., Baram, M., Brandon, D. & Kaplan, W.D. (2009). An experimental method for calibration of the plasmon mean free path. J Microsc 236, 165–173.
Newbury, D.E., Williams, D.B., Goldstein, J.I. & Fiori, C.E. (1984). Observations on the calculation of kAB factors for analytical electron microscopy. Anal Electron Microsc 2, 276–278.
Ni, N., Lozano-Perez, S., Sykes, J. & Grovenor, C. (2011). Quantitative EELS analysis of zirconium alloy metal/oxide interfaces. Ultramicroscopy 111, 123–130.
Phillips, P.J., Paulauskas, T., Rowlands, N., Nicholls, A.W., Low, K.-B., Bhadare, S. & Klie, R.F. (2014). A new silicon drift detector for high spatial resolution STEM-XEDS: Performance and applications. Microsc Microanal 20, 1046–1052.
Retsky, M. (1974). Observed single atom elastic cross sections in a scanning electron microscope. Optik 41, 127–142.
Rosenauer, A., Mehrtens, T., Müller, K., Gries, K., Schowalter, M., Satyam, P.V., Bley, S., Tessarek, C., Hommel, D., Sebald, K., Seyfried, M., Gutowski, J., Avramescu, A., Engl, K. & Lutgen, S. (2011). Composition mapping in InGaN by scanning transmission electron microscopy. Ultramicroscopy 111, 1316–1327.
Skiff, W.M., Carpenter, R.W., Lin, S.H. & Higgs, A. (1988). K, L, M, N, O and P ionziation cross sections for electron energy loss spectroscopy. Ultramicroscopy 25, 47–60.
Slater, T.J.A., Camargo, P.H.C., Burke, M.G., Zaluzec, N.J. & Haigh, S.J. (2014 a). Understanding the limitations of the Super-X energy dispersive X-ray spectrometer as a function of specimen tilt angle for tomographic data acquisition in the S/TEM. J Phys Conf Ser 522, 012025.
Slater, T.J.A., Macedo, A., Schroeder, S.L.M., Burke, M.G., O’Brien, P., Camargo, P.H.C. & Haigh, S.J. (2014 b). Correlating catalytic activity of Ag-Au nanoparticles with 3D compositional variations. Nano Lett 14, 1921–1926.
Strasser, P., Koh, S., Anniyev, T., Greeley, J., More, K., Yu, C., Liu, Z., Kaya, S., Nordlund, D., Ogasawara, H., Toney, M.F. & Nilsson, A. (2010). Lattice-strain control of the activity in dealloyed core-shell fuel cell catalysts. Nat Chem 2, 454–460.
Watanabe, M., Ackland, D.W., Kiely, C.J., Williams, D.B., Kanno, M., Hynes, R. & Sawada, H. (2006). The aberration corrected JEOL JEM-2200FS FEG-STEM/TEM fitted with an Ω electron energy-filter: Performance characterization and selected applications. JEOL News 41, 2–7.
Watanabe, M., Horita, Z. & Nemoto, M. (1996). Absorption correction and thickness determination using the zeta factor in quantitative X-ray microanalysis. Ultramicroscopy 65, 187–198.
Watanabe, M. & Williams, D.B. (2006). The quantitative analysis of thin specimens: A review of progress from the Cliff-Lorimer to the new zeta-factor methods. J Microsc 221, 89–109.
Watanabe, M., Williams, D.B. & Tomokiyo, Y. (2003). Comparison of detectability limits for elemental mapping by EF-TEM and STEM-XEDS. Micron 34, 173–183.
Zaluzec, N.J. (2013). Direct comparison of X-ray detector solid angles in analytical electron microscopes. Microsc Microanal 19, 1262–1263.
Zaluzec, N.J. (2014). Analytical formulae for calculation of X-ray detector solid angles in the scanning and scanning/transmission analytical electron microscope. Microsc Microanal 20, 1318–1326.
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Microscopy and Microanalysis
  • ISSN: 1431-9276
  • EISSN: 1435-8115
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