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Fysica – Chemie 2012
THE TRANSMISSION
ELECTRON MICROSCOPE:
ITS EARLY DEVELOPMENT
AND RECENT ACHIEVEMENTS
Stan Konings
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First electron microscope
1926 Magnetic lens theory: Hans Busch
1928-1931 First electron microscope (with Max Knoll)
1933 Better than optical spatial resolution!
1939 First commercial electron microscope (Siemens)
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Ernst Ruska and Max Knoll (1928-1931) First commercial electron microscope
(Siemens 1939)
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13 x Platina grid
4.8 x Bronze grid
17 x Platina grid
4.8 x Bronze grid
Platina grid
Bronze grid
1-stage “microscope” 2-stage microscope
1929 1931
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1933: Das ϋbermikroskop
Magnification: up to 12000x
Wing of a house fly
M=2200x
Driest and Müller: Z. Wiss. Mikroskopie 52, 53-57 (1935)
Bacteria culture
M=2000x
Krause: Naturwissenschaften 25,
817-825 (1937)
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Scanning TEM
1938: The scanning transmission electron
microscope invented by Manfred von Ardenne
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Early adopter in the Netherlands:
Willy Burgers
• First to build a “low magnification” electron microscope in the
Netherlands : 1935 (Philips Research lab)
• Alpha-gamma transition in iron at high temperature
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Jan le Poole: founding father of electron optics in the Netherlands
X-ray projection microscope
SEM with quadrupole lenses
Microprobe x-ray analyzer
Compact 1 MV microscope
Stigmators
Intermediate lens
Twin lens configuration
TEM / STEM switch
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1941: build his first electron microscope
1957: prof. of electron optics group (Delft)
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The quest for better resolution
Accelerating voltage
Why use electrons?
R = 0.612 λ / n sin α
At 3000 kV and an opening angle of 20 mrad: R = 20 pm
At 75 kV and an opening angle of 20 mrad: R = 264 pm
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3 MV transmission electron microscope Osaka
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Lens aberations limit spatial resolution
Spherical aberation Cs Chromatic aberation Cc
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Picture from:
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Hexapole lenses for spherical aberation correction
Aberation correction for TEM and STEM
Dodecapole lens for chromatic aberation correction
60-300 kV
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STEM
Pic:
TEM
Aberation-corrected TEM and STEM show the
atomic arrangement at high quality
GaSb
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Grab all signals!
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Energy-dispersive X-ray spectroscopy (EDX)
Most important components for
mapping at atomic level
• Silicon Drift Detector
• High brightness gun (X-FEG)
• Probe corrector
(Cs corrector for STEM imaging) Super-X setup
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EDX of several perovskite materials
Counts
Raw data (top)
averaged map (lower left)
and simulation (lower right)
Sr
Ti O
A.J. D’Alfonso et al. PRB 81 (2010)
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0.01
0.1
1
10
100
1000
10000
1950 1960 1970 1980 1990 2000 2010
spati
al re
solu
tion (
nm
)
year
Trend in X-ray microanalysis and STEM resolution over the last 60 years
EDX resolution
STEM resolution
1/2 every 5 yrs
1/2 every 15 yrs
Castaing’s Microprobe
FEG
100kV
Cs
correctors
Crewe’s
FEG 30kV
0.1sr
0.3sr
300kV ~1sr
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In-situ TEM
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Environmental TEM: gas + heat
Creemer et al, J MEMS, 2010
Differential pumping system
Gas flow through microscope
Nanoreactor with thin electron tranparent windows
Gas flow integrated on holder
20 mbar
10-9 mbar
Sample
heating holder
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Catalysts are often in the form of nanoparticles (1-10 nm) Structure of metal species is non uniform
Metal - support interaction
Deactivation due to coalescence
Where are the active sites? the role of defects (vacancies, dislocations), steps and edges
Typical gases: H2, O2, H2O, CO, CO2, C2H2, CH4 ……
Typical temperatures: 500-800 ˚C
Nikkel catalysts with CH4/H2 @ 2.1 mbar and heated to 536 ˚C
Time scale 2 frames/sec
5 nm
Reconstructed gold Adhesion of a single layer of CO
!
Simulation
Nanoparticles change shape under the influence of gas
CO oxidation by gold nanoparticles on CeO2
Growth of carbon nanotubes
Environmental TEM: tool for catalysis
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Helveg et al. Nature, 427, 426 (2004)
Yoshida et al.Science, 335, 317 (2012)
Uchiyama et al. Angew. Chem. (2011)
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Thank you !
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