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Quantitative WDXS Microanalysis of Bismuth-Based BaBi4Ti4O15 Perovskites Doped with Nb and Fe
Authors:Zoran Samardžija  Darko Makovec  Miran Čeh
Affiliation:(1) “Jozef Stefan” Institute, Jamova 39, SI-1000 Ljubljana, Slovenia, SI
Abstract:
 Quantitative electron-probe microanalysis was used to determine the chemical composition of an Fe- and Nb-doped bismuth-based BaBi4Ti4O15 perovskite compound. Elemental concentrations of Fe, Nb, Bi, Ba and Ti were accurately measured using wavelength-dispersive X-ray spectroscopy that was optimised for the analysis of a complex oxide matrix containing minor concentrations of dopants. Measurements were performed with a JEOL JXA 840A electron probe microanalyser at 20 and 26 kV, 50 nA beam current, 100 s maximum counting time and 0.3% preset counting deviation (σc) using both PET and LiF crystals. K-ratios were quantified by the ZAF and the φ(ρz) PAP matrix-correction procedures. The results showed that dopants incorporate into the BaBi4Ti4O15 at Ti4 +  sites according to the Ba1−4XBi4 + 4XTi4−4XFe4XO15 and Ba1 + 4XBi4−4XTi4−4XNb4XO15 solid-solution formulae. The majority of the excess charge introduced by the substitution of Ti4 +  with Fe3 +  or Nb5 +  is compensated for the change in the Ba2 + /Bi3 +  ratio.
Keywords::   EPMA   Nb-   Fe-doped BaBi4Ti4O15.
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