Direct space structure solution from precession electron diffraction data: Resolving heavy and light scatterers in Pb13Mn9O25 - Short summary of the paper

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The presentation shows the main points from the publication "Direct space structure solution from precession electron diffraction data: Resolving heavy and light scatterers in Pb13Mn9O25" about how thee structure of Pb13Mn9O25 was solved using transmission electron microscopy.

Technologie

Pb13Mn9O25, a complex oxide
solved from transmission
electron microscopy data

Problem to solve
New unknown
compound in multiple
phased sample
All phases
perovskite based
Peaks overlap in X-
ray data, so no
solution from that

So we turn to the
transmission electron
microscope...

$Electron diffraction gives us the cell parameters and space group.$

$We collect the intensities of the reflections from precession electron diffraction data.$

We feed the
intensities and all
collected data to
direct methods
(SIR2008)

Pb
Mn
Perovskite subcell
Out comes a
solution for the
cation
positions.
Mn-vacancy

Pb
Mn
Perovskite subcell
There are
ordered
manganese
vacancies.
Mn-vacancy

HAADF-STEM
confirms that Mn is
missing, but gives
no info on oxygen

We find the oxygen with
a global optimization in
direct space (FOX) using
the output from direct
methods as input.

Structure is solved with ...
two solutions !?

E = -7.42 eV E = -11.1 eV
Structure optimisation
favors one model

The calculated images
for this model agree well
with the experimental
HREM images

$Joke Hadermann, Artem M. Abakumov, Alexander A. Tsirlin, Mauro Gemmi, Hans D’Hondt, Vladimir P.Filonenko, Julie Gonnissen, Haiyan Tan, Johan Verbeeck, HelgeRosner, EvgenyV.Antipov All precise details and data can be found in the publication Ultramicroscopy 110 (2010) 881–890 by the authors Direct space structure solution from precession electron diffraction data: Resolving heavy and light scatterers in Pb13Mn9O25$

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Direct space structure solution from precession electron diffraction data: Resolving heavy and light scatterers in Pb13Mn9O25 - Short summary of the paper

1. Pb13Mn9O25, a complex oxide solved from transmission electron microscopy data

2. Ultramicroscopy 110 (2010) 881–890

3. Problem to solve New unknown compound in multiple phased sample All phases perovskite based Peaks overlap in X- ray data, so no solution from that

4. So we turn to the transmission electron microscope...

5. Electron diffraction gives us the cell parameters and space group.

6. a=b=14.2 Å=ap√13 c=3.9 Å=ap P4/m

7. EELS and EDX give us the composition.

8. Pb13Mn9O5

9. We collect the intensities of the reflections from precession electron diffraction data.

10. We feed the intensities and all collected data to direct methods (SIR2008)

11. Pb Mn Perovskite subcell Out comes a solution for the cation positions. Mn-vacancy

12. Pb Mn Perovskite subcell There are ordered manganese vacancies. Mn-vacancy

13. But where is the oxygen?

14. HAADF-STEM confirms that Mn is missing, but gives no info on oxygen

15. We find the oxygen with a global optimization in direct space (FOX) using the output from direct methods as input.

16. Structure is solved with ... two solutions !?

17. E = -7.42 eV E = -11.1 eV Structure optimisation favors one model

18. The calculated images for this model agree well with the experimental HREM images

19. Joke Hadermann, Artem M. Abakumov, Alexander A. Tsirlin, Mauro Gemmi, Hans D’Hondt, Vladimir P.Filonenko, Julie Gonnissen, Haiyan Tan, Johan Verbeeck, HelgeRosner, EvgenyV.Antipov All precise details and data can be found in the publication Ultramicroscopy 110 (2010) 881–890 by the authors Direct space structure solution from precession electron diffraction data: Resolving heavy and light scatterers in Pb13Mn9O25

Direct space structure solution from precession electron diffraction data: Resolving heavy and light scatterers in Pb13Mn9O25 - Short summary of the paper

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