Matteo Amati |
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
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European Fuel Cell 2013 11 – 13 December, Rome, Italy
Matteo Amati |
X-ray spectroscopies in electrochemical system characterization
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Spatial resolution
X-ray spectroscopies
• 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 | 4
Soft X-ray Imaging and Spectromicroscopy
Elettra
https://www.elettra.eu/
Prof. B. Bozzini Dipartimento di Ingegneria dell’Innovazione Universita del Salento, Lecce (Italy)
Matteo Amati |
TwinMic – Scanning Transmission X-ray Microscopy (STXM)
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Zone plate that forms a microprobe
Transmission Detector System
(energy res < 0.5eV)
Specimen raster-scanned across the microprobe
(spatial resolution ~ 50nm )
Fluorecence Emission Detector System
(energy res 70eV@Na)
OSA
https://www.elettra.eu/elettra-beamlines/twinmic.html
Photon energy range 400-2200 eV
CCD
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TwinMic – In situ electrochemical STXM characterizzation
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Non vacuum-compatible (aqueous solutions)
Ni / Fe Au
Nafion in aqueous solution
Bozzini et al. ChemSusChem , 7 (2010) 846
Matteo Amati |
TwinMic – In situ PEMFC durability Ni, Fe corrosion and Nafion poisoning
7 Bozzini et al. ChemSusChem , 7 (2010) 846
706/701 eV 1014 eV
40 m
m
electrode electrode electrolyte electrolyte Ni electrodes preserve pristine shape
Fe electrodes develop corrosion
morphology
Ni: narrow spreading
across interface
Fe: wide spreading
across interface
Matteo Amati |
TwinMic – In situ PEFC durability Ni, Fe corrosion and Nafion poisoning
8 Bozzini et al. ChemSusChem , 7 (2010) 846
40 m
m
Matteo Amati |
ESCAmicroscopy – Scanning PhotoElectron Microscopy (SPEM)
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SPEM actual performances § Imaging: < 50 nm
§ Microspectroscopy: 120 nm
§ Energy resolution: ~180meV
§ Standard conditions
§ Room Temperature
§ Photon Energy: 500 eV
Spatial resolution
Overall energy resolution
https://www.elettra.trieste.it/elettra-beamlines/escamicroscopy.html
N
S
Photon energy range: 350 eV (min) – 1200 eV
(undulator transmission)
Undulator
Sample
Zone Plate
OSA D = 200-250 μm dn: 50-80 nm
Spherical grating monocromator
ESCAmicroscopy beamline layout and SPEM setup
Hemispherical electron analyzer
e-
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…
Matteo Amati |
ESCAmicroscopy – Self Driven Single Chamber SOFC In operando condition
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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
NiO/MnO2 Single Chamber
e2- e2- NiO
Anode
MnO2 Cathode
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ESCAmicroscopy – Self Driven Single Chamber SOFC In operando condition
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100 µm
self-driven activity of electrochemical
cell starts
Chemical reduction Ni2++H2→Ni+2H+
B. Bozzini et al. Scientific Report 3, 2848, 2013
Matteo Amati |
ESCAmicroscopy – Self Driven Single Chamber SOFC In operando condition
12 B. Bozzini et al. Scientific Report 3, 2848, 2013
Simultaneously mapping the local chemical state and
the local electrochemical
activities
64x16 µm
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Conclusion
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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 |
Acknowledgments
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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