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

kuypers@jeolbenelux.com

Outlook

• JEM-ARM200F CF @ KUL

• JEOL

History

Today

instrument line-up

• ARM series TEM/STEM

• TEM/STEM key developments illustrated

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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

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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 ℃

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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