Regarding the EDS-mapping and the SEM-BS micrograph, how do you interpret those big grains? Do you think those dark areas in mapping are caused by the geometry of the big grains so that the x-ray beams did not reach the detector, or it is simply a second-phase?
If it is a second-phase, shouldn't those grains be at least enriched in one of the existent elements?
(These grains probably were formed during thermal-etching treatment.)
This is compositional/ elemental contrast. The element you map for, is absent where the image is dark. Nothing to do with feature size. So it's second-phase in your terms.
Surely it will be enriched in the element present in there, so you need to map for that element. By doing so, reverse area will be dark, and these features will glow.
Never use maps for identifying elements. Use spectra. Your current results say nothing. Most probable - non of mapped elements is present in either particles or substrate. Do analysis again, acquire spectra.
Let me repeat: NEVER USE MAPS for identifying elements.
Dear Vladimir Dusevich, thank you for your kind reply. My sample was a single-phase BaZr0.1Ce0.7Y0.2O3-x compound with 0.5 wt.% NiO additive as a sintering aid, and I had examined the specimen phase purity by the XRD method. So I was completely sure about the elements, and regarding the XRD sensitivity limit, I was almost sure about the phase. By taking the map, I just wanted to qualitatively check if any minor segregation or second phase (below the XRD sensitivity) was formed during sintering.
I completely agree with you that I also had to acquire spectra. But if we suppose that those grains had a different composition than other parts, isn't it a little bit weird that those places were not rich in any of the used elements? I mean, if those big grains became deficient in some of the used elements during the sintering process, shouldn't they become rich in other used elements so that we could observe high intensities in those regions and for that elements?
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