I have prepared Manganese oxides insitu grown during the synthesis of silica nano spheres with fibrous morphology by one step hydrothermal process. MnOxides concentration shown by XPS is 0.24% while by ICP-AES is 1.1%. EDS also gives the peak. so i believe that Mnoxides may be well dispersed or embedded or without any aggregation to be visible by TEM or detected by XRD. Please anyone can comment that TEM and XRD results are mutually consistent or not? In which case the TEM and XRD can not identify supported metal or metal oxides? -
How large do you think your nano spheres are? XPS has a particular depth penetration, but more importantly, electrons can only escape from a few nm below the surface and it is quite possible that the MnOs are more embedded in the center and thus not showing up as readily. Here is a pdf that explains some of those variables nicely: http://chemistry.st-and.ac.uk/staff/gh/teaching/CH5711/CH5711%20Lecture%203.pdf
Thanks Dr Joseph for your nice comments. nanospheres diameter is in the range of 200-370 nm. yes offcourse you are correct XPS has penetration depth of approx 10 nm.
The size of ur particle still quite big for XRD, it will give u a distinct Bragg peaks.
With Pair Distribution Function, XRD cud detect down to amorphous or short range order (a few angstrom).
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