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Tools for ultrahigh resolution imaging and analysis
KULeuven - RES METALLICA 2018 - 9th May 2018Advanced Electron Microscopy and Spectroscopy for Deep Insight of Materials
Stefan KuypersJEOL (Europe) BV
Outlook
• JEM-ARM200F CF @ KUL
• JEOL
History
Today
instrument line-up
• ARM series TEM/STEM
• TEM/STEM key developments illustrated
2
JEM-ARM200F CF @ KUL
JEM-ARM200F CF @ KUL
*JEM = JEOL Electron Microscope
*ARM = Atomic Resolution Microscope
*200 = up to 200kV beam energy
*F= field emission electron source
*CF = cold field emission electron source
Detectors:
*CCD camera
*ABF
*HAADF
*SE/BSE*100mm² SD for EDS
*GIF for EELS
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JEM-ARM200F CF @ KUL Demo @ JEOL
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JEM-ARM200F CF @ KUL Demo @ JEOL
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JEM-ARM200F CF @ KUL Demo @ JEOL
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JEM-ARM200F CF @ KUL Delivery @ KUL
C-ARM
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JEOL
JEM-1
JEOL co-founder and 1st PresidentMr. Kenji Kazato
Japan Electron Optics Laboratory
日本電子 Nihon Denshi
• 1947 prototype transmission electron microscope DA-1
• 1949 established in Akishima (Tokyo), Japan
• 1949 first commercial transmission electron microscope JEM-1
• 1956 first TEM JEM-5G installed in Europe (CEA, Saclay, France)
• 1962 first commercial x-ray microanalyzer (EPMA) JXA-3
• 1966 first commercial scanning electron microscope JSM-1
• 1973 established in the Benelux as JEOL (Europe) BV
JEOL
10
Max Knoll (1897-1969) Ernst Ruska (1906-1988)
1933 Siemens EM-1
Nobel Prize in Physics 1986
First commercial transmission electron microscope 1933
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• over 3000 employees worldwide
• development, production, support and service of electron microscopes, analytical tools and semiconductor tools
Electron Microscopy & Surface Analysis
• (S)TEM - SEM - SEM/FIB - EPMA - Auger - XPS - EDS
Sample Preparation for EM
• FIB - Cross Section Polisher - Ion Slicer – Coaters
Analytical
• XRF - NMR - ESR - Mass Spectrometry
Semiconductor
• E-beam Lithography
• JEOL (Europe) BV or « JEOL Benelux » since 1973
45 years of experience for sales, service and support
offices in Zaventem and Nieuw-Vennep
20 employees
JEOL
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JEM-ARM1300JEM-ARM200F CF JEM-Z300FSC
CryoARM
JEM-F200 JEM-1400Flash
JSM-7900FJSM-IT500
JSM-6000Plus
NeoScopeJSX-1000S
EagleEyeIB-19530CP
JXA-8530FPlus
JAMP-9510F
JPS-9030
JMS-MT3010 HRGA
InfiToF
JNM-ECZ400SJBX-8100FS
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JEM-ARM1300JEM-ARM200F CF JEM-Z300FSC
CryoARM
JEM-F200 JEM-1400Flash
JSM-7900FJSM-IT500
JSM-6000Plus
NeoScopeJSX-1000S
EagleEyeIB-19530CP
JXA-8530FPlus
JAMP-9510F
JPS-9030
JMS-MT3010 HRGA
InfiToF
JNM-ECZ400SJBX-8100FS
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ARM series TEM/STEM
ARM series (1/2)
・C-FEG・ASCOR・dual-SDD・low kV tuning (30kV)
JEM-ARM200F JEM-ARM200F MONO
・Monochromator・ARM200F base・≤ 20meV e-res
・C-FEG・wide gap PP・dual-SDD withlargest solid angle
JEM-ARM300F
Grand-ARM
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ARM series (2/2)
JEM-Z300FSC
CryoARM300
JEM-Z200FSC
CryoARM200
・cryo TEM・300/200kV C-FEG・in-column-filter・cryo auto loader (12 grid)
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TEM/STEM key developments illustrated
TEM/STEM key developments
• aberration (Cs) correctors for lens system (CL and OL)
• cold field emission gun (C-FEG)
• monochromator
• large solid angle SD EDS detectors (Dual-SDD)
• 3D EDS (EDS tomogrpahy)
• cryo auto loader for cryoTEM
• in-column energy filter (-filter)
• cameras/detectors cfr. Peter
• imaging strategies cfr. Peter
• « environmental » specimen holders cfr. Damien
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without Cs corrector with Cs corrector
Breakthrough for STEM!
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Schottky Cold FEG
Comparison of HAADF STEM image at high current probe condition
220(192 pm) 004
(136 pm)
Condition = Acc vol:200kV, Probe Current:500pA
Intensity profile
Histogram
FFT
444(78pm)
624(72pm)
804(60pm)713(70pm)
Intensity profile from FFT spot
78 pm(real image)60pm(FFT spot)
GaN[211] 63pm dumbbells at 200kV/63pm(real image)/53pm(FFT spot)
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GaN[211] 63pm dumbbells at 200kVand 50pm information
1Kx1K atomic resolution EDS map
Low kV(40kV) imaging for 2D material and single atoms
EELS atomic resolution map and chemical state analysis
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Nature Materials 10, 278–281 (2011) doi:10.1038/nmat2957Received 18 October 2010 Accepted 07 January 2011 Published online 13 February 2011
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Large solid angle SD EDS detectors (Dual-SDD)
SiLi detector with Liquid Nitrogen
Current model
30 mm2
Silicon drift detector and Dual detector
Evolution in EDS detectors
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JEOL G-ARM (Dual SDD)
SDD1
SD
D2
SDD2 : much better for EDS tomography
Detector Polepiece SDD1(sr) SDD2(sr) Total(sr)
100mm2
UHR 0.65 0.59 1.24
HR 0.97 0.78 1.75
FHP
WGP 0.55 1.08 1.63
158mm2 WGP 1.106 1.108 2.214
New holder for Dual SDD
JEOL Dual SDD set-up
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EDS elemental map images of SrTiO3[001]
Acc. voltage 80 kV
Scan 128 x 128 pix
Probe current 150 pA
Acquisition time 13.5 min
Dwell time 20 μs/pix
Radia
l
diffe
rence filt
er
Raw
data
Sr Ti O Sr+Ti Sr+O
1 nm
TiO2column
O
column
Sr
column29
Sr+
O
80 kV
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Porous structure of Pt-Pd-Au (formed core shell structure)
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Edge structure of Pt-Pd-Au
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128x128pix : 13min24pA at 300kV
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128x128pix : 10min24pA at 300kV
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CryoARMTM
CryoARM
JEM-Z300FSC
CryoARM300
JEM-Z200FSC
CryoARM200
・cryo TEM・300/200kV C-FEG・omega-filter・cryo auto loader (12 grid)
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Comparison of TEM images
SchottkyCFEG
Acc. Voltage: 200 kVSample: Platinum on amorphous iridium
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Omega filterHigh contrast Zero loss imaging as standard
Aperture
Zero-loss electrons Energy-loss electrons
Energy-loss spectrumEnergy selecting slit
Energy dispersion plane
Zero-loss image
Electron beam
Specimen
Ω-typeenergy filter
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Omega filter: applications dataZero-loss imageConventional image
Accelerating voltage: 200kVEnergy slit width: 20eV
Total dose: 20 e-/Å2
Defocus: -3 μm
CryoARM for SPA
CryoARM
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Temperature: 100 KSample: β-galactosidaseDefocus: -1.5µmDetector: Gatan K2 Summit
β-galactosidase Particle picking
CryoARM application data
b-galactosidase at 2.6 Å
resolution
Sample: b-galactosidase with PETG
Microscope: CRYO ARM (Schottky 200 kV) / K2 summit
Number of Images: 2,500 over 3 days by JADAS
Image pixel size: 0.8 Å/pixel
Number of particle images: 350,000 (initial pick up), 88,564 (for final 3D
reconstruction)
Software: Motioncor2, Gctf, Gautomatch, Relion2.0
Total dose: 70 e-/Å2 (70 frames (0.2 sec/frames x 14 sec)
Data: courtesy by Dr. T. Kato and Dr. K. Namba, Osaka University, August, 2017
Ligand
Mg
Y929
P928
V930
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« environmental » specimen holders
Gas cell holder
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(136 pm)-1
(116 pm)-1
HAADF-STEM
(88 pm)-1 (104 pm)-1
FFT
High resolution performance @ N2 103 Pa & 1 atm
with JEM-ARM300F & Atmosphere holder
FFT
N2 103 Pa
Distance
Inte
nsity
134 pm
N2 1 atm (105Pa)
Specimen: TiO2 (Anatase)[111]
Temperature: 300℃Gas Pressure: N2 10
3 or 105 Pa
Acc. Voltage: 300 kV
103 Pa
High resolution performance with gas cell holder
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EDS and EELS with gas cell holder
Temperature: 300℃Gas Pressure: N2 1 kPa
STEM-BF STEM-DF
Initial condition of Cu Powder for Redox reaction
ADF-STEM
O K Cu K
RG Overlay
N2 1 kPa, 300 ℃
45
EDS and EELS with gas cell holder
H2 10 kPa, 300 ℃
0
10
20
30
40
50
60
70
80
90
100
19:12 19:40 20:09 20:38 21:07 21:36 22:04 22:33 23:02 23:31 0:00
N2 pressure H2 pressure O2 pressure
ADF-STEM
O K Cu K
RG Overlay
H2 10 kPa, 300 ℃
ADF-STEM
O K Cu K
RG Overlay
N2 1 kPa, 300 ℃
ADF-STEM
O K Cu K
RG Overlay
O2 10 kPa, 300 ℃
N2 1 kPa, 300 ℃
O2 10 kPa, 300 ℃
gas pressure vs. time for redox
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EDS and EELS with gas cell holder
Cu oxide
Cu metal
Cu oxide
Cu metal
H2 10 kPa, 300 ℃
N2 1 kPa, 300 ℃
O2 10 kPa, 300 ℃
ADF-STEM O K Cu K RG Overlay
ADF-STEM O K Cu K RG Overlay
ADF-STEM O K Cu K RG Overlay
Ref data
Cu L (Cu2+ : CuO)
Cu L (Cu+ : Cu2O)
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JEM-ARM200F CF @ KUL Delivery KUL
• Thank you and congratulations
• Good luck with your research
• Looking forward to a strong collaboration KUL/JEOL48