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EELS of Niobium and Stoichiometric Niobium-Oxide Phases—Part I: Plasmon and Near-Edges Fine Structure

Published online by Cambridge University Press:  27 October 2009

David Bach ,
Reinhard Schneider ,
Dagmar Gerthsen ,
Jo Verbeeck  and
Wilfried Sigle
David Bach*
Affiliation:
Laboratorium für Elektronenmikroskopie, Universität Karlsruhe (TH), D-76128 Karlsruhe, Germany
Reinhard Schneider
Affiliation:
Laboratorium für Elektronenmikroskopie, Universität Karlsruhe (TH), D-76128 Karlsruhe, Germany
Dagmar Gerthsen
Affiliation:
Laboratorium für Elektronenmikroskopie, Universität Karlsruhe (TH), D-76128 Karlsruhe, Germany
Jo Verbeeck
Affiliation:
Electron Microscopy for Materials Research (EMAT), University of Antwerp, Groenenborgerlaan 171, 2020 Antwerp, Belgium
Wilfried Sigle
Affiliation:
Max-Planck-Institut für Metallforschung Heisenbergstraße 3, 70569 Stuttgart, Germany
*
Corresponding author. E-mail: bach@lem.uni-karlsruhe.de
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Abstract

A comprehensive electron energy-loss spectroscopy study of niobium (Nb) and stable Nb-oxide phases (NbO, NbO2, Nb2O5) was carried out. In this work (Part I), the plasmons and energy-loss near-edge structures (ELNES) of all relevant Nb edges (Nb-N2,3, Nb-M4,5, Nb-M2,3, Nb-M1, and Nb-L2,3) up to energy losses of about 2600 eV and the O-K edge are analyzed with respect to achieving characteristic fingerprints of Nb in different formal oxidation states (0 for metallic Nb, +2 for NbO, +4 for NbO2, and +5 for Nb2O5). Chemical shifts of the Nb-N2,3, Nb-M4,5, Nb-M2,3, and Nb-L2,3 edges are extracted from the spectra that amount to about 4 eV as the oxidation state increases from 0 for Nb to +5 for Nb2O5. Four different microscopes, including a 200 keV ZEISS Libra with monochromator, were used. The corresponding wide range of experimental parameters with respect to the primary electron energy, convergence, and collection semi-angles as well as energy resolution allows an assessment of the influence of the experimental setup on the ELNES of the different edges. Finally, the intensity of the Nb-L2,3 white-line edges is correlated with niobium 4d-state occupancy in the different reference materials.

Keywords

niobiumniobium oxideNbONbO2Nb2O5EELSELNESoxidation state
Type
Materials Science Applications
Information
Microscopy and Microanalysis , Volume 15 , Issue 6 , December 2009 , pp. 505 - 523
Copyright
Copyright © Microscopy Society of America 2009

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References

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