Title
EELS of niobium and stoichiometric niobium-oxide phases: part 1: plasmon and Near-edges fine structure EELS of niobium and stoichiometric niobium-oxide phases: part 1: plasmon and Near-edges fine structure
Author
Faculty/Department
Faculty of Sciences. Physics
Publication type
article
Publication
Cambridge, Mass. ,
Subject
Physics
Source (journal)
Microscopy and microanalysis. - Cambridge, Mass.
Volume/pages
15(2009) :6 , p. 505-523
ISSN
1431-9276
ISI
000272433200005
Carrier
E
Target language
English (eng)
Full text (Publishers DOI)
Affiliation
University of Antwerp
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.
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