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TEMSpec - 4th International workshop on TEM spectroscopy in Material Science
EELS: introduction and new developments
Cécile Hébert Centre Interdisciplinaire de Microscopie Electronique
Laboratoire de Spectrométrie et Microscopie Electronique Ecole Polytechnique Fédérale de Lausanne
.
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TEMSpec - 4th International workshop on TEM spectroscopy in Material Science
Outline
• Introduction • Core Loss EELS • Low losses • Super low losses • Conclusion
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TEMSpec - 4th International workshop on TEM spectroscopy in Material Science
Outline
• Introduction • Core Loss EELS • Low losses • Super low losses • Conclusion
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TEMSpec - 4th International workshop on TEM spectroscopy in Material Science
Introduction EELS in the TEM Probe = electrons
100-300 kV 80�60�30�20� Velocity: 0.55-0.77 c
Incoming e-
Auger e-
Elastically scattered e-
Inelastically scattered e-
X-rays photons
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TEMSpec - 4th International workshop on TEM spectroscopy in Material Science
Introduction: inelastic? Incoming e-
Auger e-
Elastically scattered e-
Inelastically scattered e-
X-rays photons
?
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TEMSpec - 4th International workshop on TEM spectroscopy in Material Science
Introduction: inelastic? Incoming e-
Auger e-
Elastically scattered e-
Inelastically scattered e-
X-rays photons
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TEMSpec - 4th International workshop on TEM spectroscopy in Material Science
Introduction: inelastic!
Interaction E loss Crystal Atom Electron
Phonon 10 meV inelastic elastic --
At. displacement 10 eV inelastic elastic --
interband ~ eV inelastic inelastic elastic
exciton ~ eV inelastic inelastic --
plasmon ~10 eV inelastic -- --
ionization ~100-1000eV inelastic inelastic elastic
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TEMSpec - 4th International workshop on TEM spectroscopy in Material Science
Introduction: excitation processes
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TEMSpec - 4th International workshop on TEM spectroscopy in Material Science
Introduction
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TEMSpec - 4th International workshop on TEM spectroscopy in Material Science
Introduction ⇒
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loss
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,
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TEMSpec - 4th International workshop on TEM spectroscopy in Material Science
Cross over (chromatic object plane)
Filtered image or DP
Chromatic image plane (spectrum,energy selecting slit)
Achromatic image plane
Image or diff.pattern on the SEA (achromatic object plane)
Sample
Filter
Operated as energy filter
Introduction: energy filter
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TEMSpec - 4th International workshop on TEM spectroscopy in Material Science
Cross over (chromatic object plane)
Spectrum
Chromatic image plane (spectrum,energy selecting slit)
Achromatic image plane
Image or diff.pattern on the SEA (achromatic object plane)
Sample
Filter
Two possibilites: in- or post-column
Operated as spectrometer
Introduction: energy filter
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TEMSpec - 4th International workshop on TEM spectroscopy in Material Science
ΔE
ΔE
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3D Data cubes: EFTEM vs. (STEM)-EELS
An energy filtered image is a slice from the 3D data cube.
Ex
y
e-
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Each recorded spectrum corresponds to a column in the 3D data cube.
Introduction: I want it all
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TEMSpec - 4th International workshop on TEM spectroscopy in Material Science
Outline • Introduction • Core Loss EELS • Low losses • Super low losses • Conclusion
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TEMSpec - 4th International workshop on TEM spectroscopy in Material Science
Core Losses: chemical quantification
R F Egerton, Electron energy-loss spectroscopy in the TEM, Rep. Prog. Phys. 72 (2009) 016502 (25pp); Egerton R F 1996 Electron Energy-Loss Spectroscopy in the Electron Microscope 2nd edn (New York: Plenum/Springer)
% .
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TEMSpec - 4th International workshop on TEM spectroscopy in Material Science
Core Losses: new developments 3D tomography using EELS and EDX
Nanoscale, 2014,6, 14563-14569
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TEMSpec - 4th International workshop on TEM spectroscopy in Material Science
Raw EFTEM datacube. Energy loss range: 350-760 eV 10 eV slit width, 5 eV step Microscope: TEM JEOL 2200 FS 200 keV, FEG, in column Omega filter
Ti L2,3
O K
Cr L2,3
Fe L2,3
Data cleaning: 1- removal of “X-rays”, 2- drift correction, 3- PCA
Sample preparation: C- extraction
EFTEM in core loss: ODS steel
1
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TEMSpec - 4th International workshop on TEM spectroscopy in Material Science
Principal Components Analysis applied to EFTEM data cube Energy loss range: 350-760 eV Microscope: TEM JEOL 2200 FS 200 keV, FEG, in column Omega filter
Ti L2,3
O K
Cr L2,3
Fe L2,3
EFTEM in core loss: ODS steel o.
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TEMSpec - 4th International workshop on TEM spectroscopy in Material Science
EELS fingerprints:
ß Y-O particles: 6 %, 16 nm
ß Ti-Cr-O particles: 4 %, 33 nm
ß Y-Ti-O particles: 90 %, 6 nm P. Unifantowicz, R. Schäublin, C. Hébert, T. Płociński, G. Lucas, N. Baluc, Journal of Nuclear Materials Volume 422, Issue 1-3, March 2012, Pages 131-136
EFTEM chemical maps
EFTEM in core loss: ODS steel
0
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TEMSpec - 4th International workshop on TEM spectroscopy in Material Science
Core Losses: challenge
In multi-modal electron tomography, tilt series of several signals such as X-ray spectra, electron energy-loss spectra, annular dark-field, or bright-field data are acquired at the same time in a transmission electron microscope and subsequently reconstructed in three dimensions. However, the acquired data are often incomplete and suffer from noise, and generally each signal is reconstructed independently of all other signals, not taking advantage of correlation between different datasets. ��In this paper, we show how image quality in multi-modal electron tomography can be greatly improved by employing variational modeling and multi-channel regularization techniques. �This favors similar interface positions for all reconstructions, thereby improving the image quality for all data, in particular, for 3D elemental maps. We demonstrate the joint multi-channel TGV reconstruction on tomographic energy-dispersive X-ray spectroscopy (EDXS) and high-angle annular dark field (HAADF) data, but the reconstruction method is generally applicable to all types of signals used in electron tomography, as well as all other types of projection-based tomographies.
Nanoscale, 2019,11, 5617-5632
IT
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TEMSpec - 4th International workshop on TEM spectroscopy in Material Science
Core Losses fine structures
R F Egerton, Electron energy-loss spectroscopy in the TEM, Rep. Prog. Phys. 72 (2009) 016502 (25pp); Egerton R F 1996 Electron Energy-Loss Spectroscopy in the Electron Microscope 2nd edn (New York: Plenum/Springer)
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TEMSpec - 4th International workshop on TEM spectroscopy in Material Science
Core losses: ELNES
Diamond Graphite
Carbon K edge
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TEMSpec - 4th International workshop on TEM spectroscopy in Material Science
ELNES
ELNES or “Electron Energy Loss Near”
EELS
•
÷
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TEMSpec - 4th International workshop on TEM spectroscopy in Material Science
ELNES of anisotropic materials
k k’
q
Core losses: ELNES
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TEMSpec - 4th International workshop on TEM spectroscopy in Material Science
Applications: Irradiated graphite
Loïc Fave, Teresa Dennenwaldt, Duncan Alexander, Cédric Baumier, Manuel A. Pouchon, Cécile Hébert : in preparation.
- SiC/SiC composites forseen as cladding tubed for nuclear power plants.
- A graphitic carbon inter layer acts as mechanical improvement of the otherwise brittle ceramics
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TEMSpec - 4th International workshop on TEM spectroscopy in Material Science
Application: Iron oxidation state in minerals
Iron content and valence state
PNAS October 4, 2016 113 (40) 11127-11130
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TEMSpec - 4th International workshop on TEM spectroscopy in Material Science
Application: EMCD -
O
a
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TEMSpec - 4th International workshop on TEM spectroscopy in Material Science
Outline • Introduction • Core Loss EELS • Low losses • Super low losses • Conclusion
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TEMSpec - 4th International workshop on TEM spectroscopy in Material Science
Angular resolved low loss
,
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TEMSpec - 4th International workshop on TEM spectroscopy in Material Science
A. Alkauskas et al., Ultramicroscopy 110 (2010) 1081–1086
Evolution of the loss function of bulk Silver in the energy range 0-55 eV as a function of momentum transfer q in the (1 1 1) direction including local field effects.
Angular resolved EELS in Ag, calculation
" I
-
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TEMSpec - 4th International workshop on TEM spectroscopy in Material Science
Data acquisition Standard acquisition method
µ" " " °
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TEMSpec - 4th International workshop on TEM spectroscopy in Material Science
Data Acquisition
•,
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:
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TEMSpec - 4th International workshop on TEM spectroscopy in Material Science
EFTEM acquisition : NBD
①•
20
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TEMSpec - 4th International workshop on TEM spectroscopy in Material Science
A. Alkauskas et al. Ultramicroscopy 110 (2010) 1081–1086
TEM image spectrum, Sputtered Ag
1 2
3
4
5 6
7
2 3
4
5 6 7
1
Experimentl results
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TEMSpec - 4th International workshop on TEM spectroscopy in Material Science
Experimental results
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TEMSpec - 4th International workshop on TEM spectroscopy in Material Science
Experimental results
Yoyo !
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TEMSpec - 4th International workshop on TEM spectroscopy in Material Science
Outline • Introduction • Core Loss EELS • Low losses • Super low losses • Conclusion &
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TEMSpec - 4th International workshop on TEM spectroscopy in Material Science
Ultra-high energy resolution EELS
Ultramicroscopy 203 60–67 (2019)
-
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•
AEK
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TEMSpec - 4th International workshop on TEM spectroscopy in Material Science
Momentum-resolved EELS Senga and Suenaga arXiv: 1812.08294
MORE-TEM project: Mtm-resolved (0.01 Å–1) Spatially-resolved 1 meV !E 4 K temperature “To compete with the synchrotron”
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TEMSpec - 4th International workshop on TEM spectroscopy in Material Science
Conclusion
Amazing recent developments Challenges in data handling and analysis New generation of detectors Software / open versus closed��