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Universiteit Antwerpen
Complementarity of TEM to
bulk diffraction techniques for
structures at nanoscale
Joke Hadermann
Lecture downloadable from
Slideshare.net/johader
Universiteit Antwerpen
Collaboration with Rosseinsky Group, U. Liverpool
Nature Chemistry 8 (2016) 347
Universiteit Antwerpen
Nature Chemistry 8 (2016) 347
Universiteit Antwerpen
[110]F
[001]P
I
III
2
4
6
Fluorite
Perovskite
I
III
2
4
6
Nature Chemistry 8 (2016) 347
Universiteit Antwerpen
EDX EELS
Nature Chemistry 8 (2016) 347
Fluorite Perov.
Universiteit Antwerpen
I
III
2
4
6
Universiteit Antwerpen
Pb0.650Bi0.309Fe1.042O2.675
Overview in
Acta Cryst. B 71 (2015) 127
Fe
Pb/Bi
Universiteit Antwerpen
Pb0.650Bi0.309Fe1.042O2.675
Overview in
Acta Cryst. B 71 (2015) 127
Fe
O
Universiteit Antwerpen
Pb0.650Bi0.309Fe1.042O2.675
Overview in
Acta Cryst. B 71 (2015) 127
Universiteit Antwerpen
Overview in
Acta Cryst. B 71 (2015) 127
Universiteit Antwerpen
K6.4(Nb,Ta)36.3O94
“K2Nb8O21”
a = 37.468(9) Å,
b = 12.493(3) Å,
c = 3.95333(15) Å
Collaboration with
Taras Shevchenko National
University of Kyiv
Universidad de Oviedo
Dalton Transactions
45 (2016) 973
Universiteit Antwerpen
J. Sol. St. Chem. 242 (2016) 86
Collaboration with Peter Battle group, Oxford University
I4/m
P-3c
Universiteit Antwerpen
J. Sol. St. Chem. 242 (2016) 86
Collaboration with Peter Battle group, Oxford University
Universiteit Antwerpen
Quantitative electron diffraction
example: cycled Li-batteries
Bulk
- low sensitivity to Li
- poor quality of powder
diffraction pattern
Bulk
+ sensitive to Li
- necessary amount of
sample>1g
Single crystal
+ sensitive to Li
+ necessary amount of
sample <1 mg
- 1D projection of
3D reciprocal space
+ 3D reconstructions of
3D reciprocal space
Ab-initio structure
determination
Powder
X-ray
diffraction
Powder
neutron
diffraction
Electron
diffraction
tomography
Universiteit Antwerpen
3D reconstruction of reciprocal space
Electron diff. tom.:U. Kolb et al., Ultramicroscopy 107 (2007) 507-513
PETS: L. Palatinus, PETS-Program for analysis of electron diffraction data,
2011
Universiteit Antwerpen
Li1-xFe0.5Mn0.5PO4
Mn0.5Fe0.5PO4
+3 +3
LiMn0.5Fe0.5PO4
+2 +2
Fe0.5Mn0.5PO4
Li
LiFe0.5Mn0.5PO4
Electrochimica acta, 191(2016) 149
Universiteit Antwerpen
Li2FePO4F
LiFePO4
Li/Fe
Submitted to Chem. Mater.
Universiteit Antwerpen
LiRhO2 Li0.55RhO2 LixRhO2
charge
-0.45 Li+
charge
-~0.45 Li+
4.1 V3.85 V
In-situ synchrotron powder diffraction in electrochemical test cells
NEW
PHASE
Collaboration with D. Mikhailova, Max Planck Inst.Chem.Phys. of Solids Dresden
Inorg. Chem., 55 (14), 7079–7089, (2016)
Universiteit Antwerpen
ramsdellite
2x1 channel rutile
1x1 channel
Inorg. Chem., 55 (14), 7079–7089, (2016)
LixRhO2
Universiteit Antwerpen
LixRhO2
Inorg. Chem., 55 (14), 7079–7089, (2016)
Universiteit Antwerpen
Summary
Advanced TEM can add crucial pieces of the puzzle by
information on e.g.
composition at atomic resolution (EELS, EDX, HAADF-
STEM)
positions of light atoms (ABF-STEM, EDT)
valence and coordination at atomic resolution (EELS)
structure of multiphased samples, samples with weak
extra reflections, low quality bulk diffraction data, ...
(EDT)
Lecture downloadable from
Slideshare.net/johader
Universiteit Antwerpen
Acknowledgements
Students and postdocs at EMAT:
Dmitry&Maria Batuk, Olesia Karakulina, Robert Paria Sena
Collaborators:
Artem M. Abakumov, Skoltech
V. Sumanov, O. Drozhzhin, E. Antipov
Moscow State University
D. Mikhailova, Max Planck Inst.Chem.Phys. of Solids Dresden
M. O'Sullivan, M.S. Dyer, J. Alaria, T.D. Manning, J.B. Claridge, M.J.
Rosseinsky, University of Liverpool
A.A. Babaryk, N.S. Slobodyanik, Taras Shevchenko Natl Univ Kyiv
S. Garcia-Granda, U. Oviedo
FWO grant
G040116N

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Complementarity of advanced TEM to bulk diffraction techniques