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Chapter 8

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Chapter 8

Uploaded by

Kevin
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© © All Rights Reserved
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Transmission Electron Microscopy

Chapter 8
Scanning Transmission Electron Microscopy
(STEM)

@ Department of Materials Science and Engineering, NTHU 1


Outline

• Principles of STEM

• Ronchigram

• Cs-Corrector

• Image Modes in STEM

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@ Department of Materials Science and Engineering, NTHU 3
Principles of STEM
• Unlike the parallel beam in TEM, a fine probe is used to form images in
STEM, the beam must scan parallelly to the optic axis at all times.

E. Abe, Chem. Soc. Rev 41, 6787–6798 (2012)


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Principles of STEM

• The STEM operates in a very


similar way to a scanning
electron microscope (SEM).

• In STEM the electron beam is


focused to a fine spot which is
then scanned over the sample
in a raster.

• We don’t use lenses to form


the image, therefore, the
chromatic aberration is absent
in STEM images. We can deal
with the thicker specimen in
STEM.

@ Department of Materials Science and Engineering, NTHU 10


Principles of STEM

• We scan the beam on the


specimen by adjusting
the scan coils; these
same coils are used to
scan the computer
display synchronously.

• The electron detector


acts as the interface
between the electrons
coming from the
specimen and the image
viewed on the display
screen.
• The whole process of creating a STEM image is much slower than
TEM imaging: it’s serial recording instead of parallel recording.

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Detectors in STEM

• Semiconductor Detector: a Si-based p-n junction plate for detecting the


electrons.

1. e-h pairs generated by the energy


transfer from incident electrons.

2. The incident electron signal is


converted to a current in the
external circuit.

3. STEM detector in ring shape (annular


detector).

ADF/HAADF STEM Detector

BF/ABF STEM Detector


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Outline

• Principles of STEM

• Ronchigram

• Cs-Corrector

• Image Modes in STEM

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Ronchigram

• A Ronchigram, discovered by Ronchi in


1948, is a projection (shadow) image
of a specimen formed on the
diffraction plane with a convergent
beam.

• We use the Ronchigram formed with


amorphous specimen.

• Ronchigram is useful in the STEM for


two purposes,
1. Characterize and optimize the
electron probe.

2. Determine the focus condition of


the electron probe.
Overfocus At focus Underfocus

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Shadow Image

The Ring of
Infinite Radial
Magnification

The Ring of
Infinite Angular
Magnification
(Azimuthal circles)

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Focusing with Ronchigram

• The Ronchigram is used to obtain the exact focus of the incident


electron probe onto the specimen in STEM.

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Aberration Correction using Ronchigram

• Twofold Astigmatism • Coma Aberration

Overfocus Underfocus Overfocus Underfocus


• If three sets of
radial lines vary in
• The lines appear Corrected
length, the coma
in the center
exists.
when out of
focus.

Out of focus At focus

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Ronchigram Size

• If the spherical aberration is not corrected, the area with a uniform


electron intensity is confined to a small extent. When the aberration
is corrected, the area is largely extended.

uncorrected Cs-corrected

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Fringes from Crystalline Specimen

• Appearance of the interference fringes means that the probe


diameter is smaller than the lattice spacing.

Amophrous Specimen Crystalline Specimen

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Outline

• Principles of STEM

• Ronchigram

• Cs-Corrector

• Image Modes in STEM

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Cs Corrector
w/o Cs correction

w/o Cs
correction

w/ Cs
correction
w/ Cs correction

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Cs-corrected TEM

• Without Cs corrector
- r is 0.2-3 nm (depending on the
accelerate voltage)

• With Cs corrector
- r is 0.06-0.08 nm

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Nion Corrector CEOS System

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Cs Corrector

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Spherical Aberration (Cs)

Probe Correction Image Correction

Specimen

CM: mini condenser lens

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Main Configuration of Cs TEM

Name: JEM-ARM200FTH
Accelerate Voltage: 80/200 kV
Electron Source: Cold type Field Emission Gun
(CFEG) with EDS detector (Oxford X-Max) and
CEOS aberration corrector(CESCOR)

Resolution
200KV
TEM Lattice resolution: 72 pm
STEM DF image: 78 pm
STEM BF image: 0.136 nm

80KV
TEM Lattice resolution: 0.102 nm
STEM DF image: 0.136 nm
STEM BF image: 0.136 nm

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Cs Corrector

 Image Correction (TEM mode)

W/O Cs corrector W/ Cs corrector

The grain boundary in SrTiO3 imaged without and with Cs corrector.

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Cs Corrector

 Probe Correction (STEM mode)


• Atomic resolution in STEM requires a probe size smaller than the
interatomic spacing.

Cs = 1 mm W/ Cs Corrector (Cs = 2 um)


Probe size: 0.3 nm Probe size: 0.1 nm
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Outline

• Principles of STEM

• Ronchigram

• Cs-Corrector

• Image Modes in STEM

@ Department of Materials Science and Engineering, NTHU 30


@ Department of Materials Science and Engineering, NTHU 31
Imaging Modes in STEM

• Bright-Field (BF) STEM imaging:


forward-scattered electrons are
collected by disk-shaped detector.

• Annular Dark-Field (ADF) STEM


imaging: forward-scattered
electrons with small angles (~3o )
are collected.

• High-Angle Annular Dark-Field


(HAADF) STEM imaging: electrons
scattered out to higher angles are
ADF ADF collected. This is also called Z-
contrast imaging.

@ Department of Materials Science and Engineering, NTHU 32


Bright-Field (BF) Imaging in STEM

• BF detector is a solid disc and collects


the scattered signals within the
collection angle of 10 mrad .

• BF detector gives simultaneous phase- .


contrast image, which is equivalent to 𝛃𝛃 < 𝟏𝟏𝟏𝟏 𝐦𝐦𝐦𝐦𝐦𝐦𝐦𝐦
HR-TEM image.

BF STEM image
Sr
O
Ti

ADF STEM image


BF

(100) SrTiO3

@ Department of Materials Science and Engineering, NTHU 33


Annular Dark-Field (ADF) Imaging

• When scattering angle > screening


parameter (θ0), the electron-nucleus
interaction is dominant.

• ADF detector is a ring-like detector and


collects the scattered signals with a
range between 20 and 50 mrad .

𝟐𝟐𝟎𝟎 𝐦𝐦𝐦𝐦𝐦𝐦𝐦𝐦 < 𝛃𝛃 < 𝟓𝟓𝟎𝟎 𝐦𝐦𝐦𝐦𝐦𝐦𝐦𝐦


• The contrast in ADF images strongly
depend on atomic number (Z) of the
ADF
specimen. (Z- contrast image)
BF
I ∝ 𝑍𝑍1.5

@ Department of Materials Science and Engineering, NTHU 34


High-Angle Annular Dark-Field Imaging
Incident
Beam

• HAADF image collects the


scattered signals ranging
from 50 to 200 mrad .

• HAADF provides better


𝟓𝟓𝟎𝟎 𝐦𝐦𝐦𝐦𝐦𝐦𝐦𝐦 < 𝛃𝛃 < 𝟐𝟐𝟐𝟐𝟎𝟎 𝐦𝐦𝐦𝐦𝐦𝐦𝐦𝐦
contrast to the Z than ADF.
HAADF
I ∝ 𝑍𝑍 2 ADF
BF

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ADF and HAADF Images

HAADF Image ADF Image

NbC precipitates

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HAADF (ADF) Images
ZGa: 35 ZN: 7
A
• The HR STEM images provide the direct B
C-axis
interpretation of the crystal structure. A
B

Crystal 1 GaN Nanowire Ga N


Crystal 2

ADF STEM
Shift
A
B
TEM A
B
A
B
C
Stacking B
C
Fault B

Distortion

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HAADF (ADF) Images

• The contrast in the ADF images is about the mass, thickness and atomic
numbers.

Twinned Si Nanowire

TEM ADF STEM

Delocalization

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HAADF (ADF) Images
Cs-lead halide (CsPbBr3)Cube

z y
c x b

ZBr: 35 ZCs: 55 ZPb: 82


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HAADF (ADF) Images

• The contrasts in HAADF depend on the DF Contrast Profile


atomic numbers of atoms, such that the EDS line scan of In

Intensity (a.u.)
contrasts can be used for quantitative
elemental analysis.

0 2 4 6 8 10 12
Distance (nm)

ADF STEM images of In/ZnO interface

@ Department of Materials Science and Engineering, NTHU 40


HAADF (ADF) Images

• HAADF is not useful for imaging light atoms with heavy atoms, because the
contrast shows strong dependence to atomic number.

InGaN

InGaN

InGaN
GaN
GaN
GaN

ADF STEM images of InGaN@GaN nanorod

ZIn: 49 ZGa: 35 ZN: 7


@ Department of Materials Science and Engineering, NTHU 41
Annular Bright-Field (ABF) Imaging

• ABF imaging, the latest imaging mode of STEM, is introduced for


reaching enough sensitivity to image the light atoms.

• ABF imaging, where the central part


of BF detector is blocked , provides
the information of both light and
heavy atoms.
BFABF
• The collection angle for ABF
imaging is between 10 and 50 mrad .

𝟏𝟏𝟏𝟏 𝐦𝐦𝐦𝐦𝐦𝐦𝐦𝐦 < 𝛃𝛃 < 𝟓𝟓𝟓𝟓 𝐦𝐦𝐦𝐦𝐦𝐦𝐦𝐦

@ Department of Materials Science and Engineering, NTHU 42


Annular Bright-Field (ABF) Imaging
ABF image
ZY: 39
ZH: 1

[010]
BF image ADF image

BF image: Bright Field STEM image


ABF image: Annular Bright Field STEM image
ADF image: Annular Dark Field STEM image
R. Ishikawa, et al. Nature Mater. 10, 278-281 (2011) P. Batson, Nature Mater. 10, 270-271 (2011)

@ Department of Materials Science and Engineering, NTHU 43


Annular Bright-Field (ABF) Imaging

• The contrast is reversed, but there is no difference between ADF and ABF
images for single-element materials.

ADF STEM ABF STEM

[110] Ge

ABF image: Annular Bright Field ADF image: Annular Dark Field
@ Department of Materials Science and Engineering, NTHU 44
Annular Bright-Field (ABF) Imaging

ADF STEM ABF STEM

GaN

The Stacking _
(0001)-N
A • N atoms lie on
B top of the Ga-N
A dumbbells
B indicating the
A Nitrogen polarity
B of GaN nanorod.
(0001)-Ga
Wurtzite Structure

@ Department of Materials Science and Engineering, NTHU 45


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Any Questions?

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