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Bozzini et al. ChemSusChem , 7

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SYNCHROTRON-BASED IN SITU
CHARACTERIZATION OF PEMFC AND
SOFC COMPONENTS
Matteo Amati
[email protected]
B. Bozzini, P. Bocchetta, A. Gianoncelli, L. Gregoratti, C. Mele and M. Kiskinova
European Fuel Cell 2013
11 – 13 December, Rome, Italy
Matteo Amati | 2
X-ray spectroscopies in electrochemical
system characterization
X-ray spectroscopies
• 
• 
• 
Spatial
resolution
X-ray absorption spectroscopy,
X-ray emission (fluorescence) spectroscopy
X-ray photoelectron spectroscopy
opportunities for monitoring material
changes and mass transport events
occurring at submicron length scales
Matteo Amati | 3
Soft X-ray Imaging and Spectromicroscopy
Elettra
Prof. B. Bozzini
Dipartimento di Ingegneria dell’Innovazione
Universita del Salento, Lecce (Italy)
https://www.elettra.eu/
Matteo Amati | 4
TwinMic – Scanning Transmission X-ray
Microscopy (STXM)
Zone plate that
forms a microprobe
Transmission
Detector System
(energy res < 0.5eV)
OSA
CCD
Photon
energy range
400-2200 eV
Fluorecence Emission
Detector System
(energy res [email protected])
Specimen raster-scanned
across the microprobe
(spatial resolution ~ 50nm )
https://www.elettra.eu/elettra-beamlines/twinmic.html
Matteo Amati | 5
TwinMic – In situ electrochemical STXM
characterizzation
Non vacuum-compatible (aqueous solutions)
Ni / Fe
Au
Nafion in
aqueous
solution
Bozzini et al. ChemSusChem , 7 (2010) 846
Matteo Amati | 6
TwinMic – In situ PEMFC durability
Ni, Fe corrosion and Nafion poisoning
1014 eV
electrolyte
electrode
electrolyte
40 mm
electrode
706/701 eV
Ni electrodes preserve
pristine shape
Fe electrodes
develop corrosion
morphology
Fe: wide
spreading
across interface
Ni: narrow
spreading
across interface
Bozzini et al. ChemSusChem , 7 (2010) 846
Matteo Amati | 7
40 mm
TwinMic – In situ PEFC durability
Ni, Fe corrosion and Nafion poisoning
Bozzini et al. ChemSusChem , 7 (2010) 846
Matteo Amati | 8
ESCAmicroscopy – Scanning PhotoElectron
Microscopy (SPEM)
Hemispherical
electron analyzer
ESCAmicroscopy beamline layout and SPEM setup
Spherical grating
monocromator
Zone Plate
e-
Undulator
N
S
Photon energy range:
350 eV (min) – 1200 eV
(undulator transmission)
D = 200-250 μm
dn: 50-80 nm
OSA
Sample
SPEM actual performances
Spatial resolution
§ Imaging: < 50 nm
§ Microspectroscopy: 120 nm
§  Energy resolution: ~180meV
Overall energy
resolution
§  Standard conditions
§  Room Temperature
Bozzini et al. Scientific Report 3, 2848, 2013 (2013)
Bozzini et al. Electrochem Comm, Vol. 24, pp.104-107 (2012)
Bozzini et al. Journal of Physical Chemistry C 116 (44),
pp. 23188-23193 (2012)
Bozzini et al. ChemSusChem, Vol. 4 - 8, pp. 1099-1103 (2011)
Bozzini et al. Chemistry - A European Journal 18 (33),
pp. 10196-10210 (2012)
Ecc…
§  Photon Energy: 500 eV
https://www.elettra.trieste.it/elettra-beamlines/escamicroscopy.html
Matteo Amati | 9
ESCAmicroscopy – Self Driven Single
Chamber SOFC In operando condition
NiO/MnO2
Single Chamber
MnO2
Cathode
NiO e2-
e2-
Anode
1x10-5 mbar of O2
P=1x10-5 mbar of H2 + O2 (1:1)
200–400 nA
B. Bozzini et al. Scientific Report 3, 2848, 2013
Matteo Amati | 10
100 µm
ESCAmicroscopy – Self Driven Single
Chamber SOFC In operando condition
self-driven activity
of electrochemical
cell starts
Chemical reduction
Ni2++H2→Ni+2H+
B. Bozzini et al. Scientific Report 3, 2848, 2013
Matteo Amati | 11
ESCAmicroscopy – Self Driven Single
Chamber SOFC In operando condition
64x16 µm
Simultaneously
mapping the local
chemical state and
the local
electrochemical
activities
B. Bozzini et al. Scientific Report 3, 2848, 2013
Matteo Amati | 12
Conclusion
1.  in situ and in operando electrochemical experiments
STXM and SPEM experiments can be performed under
operating conditions
2.  Information regarding:
•  compositional, chemical state and overvoltage
localization
•  damaging/material growth mechanisms
•  behaviour of peculiar material couplings
Matteo Amati | 13
Acknowledgments
STAFF:
Matteo Amati
Luca Gregoratti
Alessandra Gianoncelli
Burkhard Kaulich
Maya Kiskinova
Mauro Prasciolu
Ivonne Sgura[
Patrizia Bocchetta
Francesco Bogani
Federica De Riccardis
Deborah Lacitignola
Claudio Mele
Ivonne Sgura
PhD/PostDoc:
Gian Pietro De Gaudenzi
Lucia D’Urzo
Ameriga Fanigliulo
Giuseppe Giovannelli
Hossein Hassannejad
Majid Kazemian Abyaneh
Cristina Lenardi
Ralf Peipmann
Patrizio Raffa
Vincenzo Romanello
Marco Serra
Elisabetta Tondo
Matteo Amati | 14
Thank you!
Matteo Amati | 15
ESCAmicroscopy – Self Driven Single
Chamber SOFC In operando condition
H2
Propagation of
the reduction
front
B. Bozzini et al. Scientific Report 3, 2848, 2013
Matteo Amati | 17
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