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Stoichiometry and valence measurements of niobium oxides using electron energy‐loss spectroscopy
Author(s) -
OLSZTA M. J.,
WANG J.,
DICKEY E. C.
Publication year - 2006
Publication title -
journal of microscopy
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.569
H-Index - 111
eISSN - 1365-2818
pISSN - 0022-2720
DOI - 10.1111/j.1365-2818.2006.01709.x
Subject(s) - niobium , electron energy loss spectroscopy , niobium oxide , valence (chemistry) , stoichiometry , oxide , spectroscopy , chemistry , analytical chemistry (journal) , ionization , ionization energy , metal , natural bond orbital , materials science , ion , computational chemistry , density functional theory , physics , transmission electron microscopy , organic chemistry , chromatography , quantum mechanics , nanotechnology
Summary Qualitative and quantitative electron energy‐loss spectroscopy analyses have been performed on niobium and stable niobium oxides (NbO, NbO 2 and Nb 2 O 5 ). At integration windows (Δ) greater than 75 eV, k‐factor analysis can be used to distinguish between the stoichiometry of the three oxides within 5.7% error. As seen in other metal oxides, with increasing oxidation state the metal ionization edges shift to higher energies relative to the O‐K edge. Normalized M 2,3 white‐line intensities show a strong correlation with 4 d occupancy for each compound. The data are in correspondence with that observed in the literature for 4 d transition metals using normalized L 2,3 white lines. Lastly, a distinctive energy‐loss near‐edge, structure of the O‐K edge was observed for each oxide, which could be used as a fingerprint for analysis of unknowns.