Imaging with Diffraction

Contrast
Duncan Alexander
EPFL-CIME

Duncan Alexander: Imaging with Diffraction Contrast 1

Introduction

When you study crystalline samples TEM image contrast is dominated by diffraction contrast.

An objective aperture to select either the direct beam for a bright-field image,
or diffracted beam(s) for a dark-field image.

The TEM image effectively maps spatially the intensity in this beam.

Changes in intensity are given by:

- general crystal orientation relative to the electron beam, and crystal phase
- local changes in crystal orientation from crystal defects and bending
- sample thickness changes.

These effects combine to give the diffraction contrast that are your TEM data.

Inherent connection to diffraction pattern of your specimen.

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 Diffraction contrast?
• Possible interactions of beam with specimen

• Only some lead to contrast in TEM image

secondary electrons

Incident beam
Backscattered electrons
BSE SE Characteristic
X-rays

visible light
Auger electrons

“absorbed” electrons electron-hole pairs

1-100 nm Specimen

direct beam

elastically scattered Bremsstrahlung

electrons X-rays
inelastically
scattered electrons

Duncan Alexander: Imaging with Diffraction Contrast

Diffraction contrast?
• Biological specimen with heavy metal stain: majority of contrast from
“absorption of electrons.
• Sample of interest biologically, but physics of scattering are boring.
Incident beam

Backscattered electrons
BSE

“absorbed” electrons
1-100 nm Specimen
direct beam

elastically scattered
electrons

inelastically
scattered electrons

Duncan Alexander: Imaging with Diffraction Contrast

 Diffraction contrast?
• Materials science specimen: CVD-grown ZnO thin film. Elastic scattering of
the electrons (i.e. diffraction) by crystal is major contribution to contrast.
• Changes in crystal orientation from grain to grain or within grains at defects
change the diffraction condition and hence the contrast.

Incident beam
Backscattered electrons
BSE

“absorbed” electrons
1-100 nm Specimen
direct beam

elastically scattered
electrons

inelastically
scattered electrons

Duncan Alexander: Imaging with Diffraction Contrast

TEM imaging/diffraction modes recap

Diffraction Image
mode mode

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 Bright-field image vs dark-field image
Bright-field image Dark-field image
= =
select direct beam select diffracted beam
with objective aperture with objective aperture

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Nanocrystalline sample image/diffraction

Bright field image setup - select direct beam with objective aperture
Diffraction mode Image mode

Contrast from different crystals according to

diffraction condition

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Nanocrystalline sample image/diffraction
Dark field image setup - select some transmitted beams with objective aperture
Diffraction mode Image mode

Only crystals diffracting strongly into objective

aperture give bright contrast in image

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Nanocrystalline sample image/diffraction

Dark field image setup - select some transmitted beams with objective aperture
Diffraction mode Image mode

Only crystals diffracting strongly into objective

aperture give bright contrast in image

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 Nanocrystalline sample image/diffraction
DF A

BF

DF B

DF images allow us to pick out

individual grains

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Diffraction contrast on/off zone axis

In bright-field imaging, zone axis condition => more scattering to diffracted beams
Therefore intensity in direct beam goes down and bright-field image has strong contrast

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 Diffraction contrast on/off zone axis
In bright-field imaging, zone axis condition => more scattering to diffracted beams
Therefore intensity in direct beam goes down and bright-field image has strong contrast
Example: GaN nanowire

CBED SADP BF

Off zone
axis

CBED SADP BF

On zone
axis

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Diffraction contrast on/off zone axis

In bright-field imaging, zone axis condition => more scattering to diffracted beams
Therefore intensity in direct beam goes down and bright-field image has strong contrast
Example: GaN nanowire
BF off zone axis BF on zone axis

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 Image delocalization

TEM image with no objective aperture. Image formed from direct beam and diffracted
beams. Dark-field images from diffracted beams delocalize from bright-field image of
direct beam. Gives shadow images that move with objective focus (mostly result from Cs).

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Image delocalization

Image of same nanowires but with objective aperture to make bright-field image. No
diffracted beams => no shadow images.
This is how you should take your TEM data!

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 Image delocalization
TEM (multi-beam) image Bright-field image

Direction of delocalization depends on direction of diffracted beam in diffraction pattern

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Dark-field imaging:
displaced aperture vs beam tilt

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 Bend contours

From Williams & Carter Transmission Electron Microscopy

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Bend contours
Example: electropolished Ni3Al superalloy

Sample at lower magnification.

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 Bend contours
Example: electropolished Ni3Al superalloy

Bright-field images. Same region at different sample tilts.

See bend contours interacting with dislocations.

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Bend contours
Example: mechanically polished and ion beam milled silicon

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 Thickness fringes
Dynamical scattering in the dark-field image –

=> Intensity zero for thicknesses t = nξg (integer n)

See effect as dark “thickness fringes” on wedge-shaped sample:

Composition changes in quantum wells

=> extinction at different thickness compared to substrate

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Phase contrast
Example: electropolished Ni3Al superalloy
Simple cubic γ’ precipitates in FCC γ matrix
SADP simple cubic γ’ SADP FCC γ

000
000
100 200
200

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 Phase contrast
Example: electropolished Ni3Al superalloy
Simple cubic γ’ precipitates in FCC γ matrix
SADP simple cubic γ’ Bright-field image

000
100
200

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Phase contrast
Example: electropolished Ni3Al superalloy
Simple cubic γ’ precipitates in FCC γ matrix
SADP simple cubic γ’ Dark-field image g = 1 0 0

000
100
200

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 Phase contrast
Example: electropolished Ni3Al superalloy
Simple cubic γ’ precipitates in FCC γ matrix
SADP simple cubic γ’ Dark-field image g = 2 0 0

000
100
200

Duncan Alexander: Imaging with Diffraction Contrast 27

Crystal defects: dislocations

Burgers vector for edge (top right) and screw (bottom right) dislocations

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 Crystal defects: dislocations
Local bending of crystal planes around the dislocation change their diffraction condition
This produces a contrast in the image => g.b analysis for Burgers vector

From Williams & Carter

Transmission Electron Microscopy

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Crystal defects: dislocations - g.b analysis

Invisibility criterion!

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 Crystal defects: dislocations - g.b analysis
Example: threading dislocations in GaN

From visibility in for images a)

to c) and near invisibility in d),
dislocation B found to have:
b = ±1/3[2 -1 -1 3]
or b = ±1/3[1 -2 -1 3]

Sakai et al. APL 71 (1997) 2259

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Planar defects – stacking faults

Similarly to Burgers vector analysis, stacking faults with displacement vector R
are invisible for g.R = 0

Example: analysis of basal plane stacking faults in ZnO

SADP on [1 1 00] zone axis Bright-field g = 1 -1 0 0 Dark-field g = 1 -1 0 0

g g

g parallel to R: stacking faults visible

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 Planar defects – stacking faults
Similarly to Burgers vector analysis, stacking faults with displacement vector R
are invisible for g.R = 0

Example: analysis of basal plane stacking faults in ZnO

SADP on [1 1 00] zone axis Bright-field g = 0 0 0 2 Dark-field g = 0 0 0 2

g g

g perpendicular to R: stacking faults invisible

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Amorphous? Or low diffraction contrast?

Bright-field image of Al-Cr-N-O thin film

• Some regions show clear

diffraction contrast, so
obviously crystalline.
• Other regions did not.
Combined with contrast
from probable amorphous
surface layer, looked
amorphous.
• However CBED proved
crystalline, just in low
diffraction contrast
condition.

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 Phase contrast, grain boundaries, bend
contours, dislocations in one image

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Summary
When imaging crystalline samples in the TEM, any change in the crystal will change the elastic
scattering diffraction condition and hence intensity and contrast in the resulting image. This can be
from:
- crystal orientation relative to the electron beam and deviations from bending
- defects in the crystal
- changes in phase (e.g. precipitates)
- changes in thickness (dynamical scattering).

Using an objective aperture to select the direct beam (bright-field image) or diffracted beam (dark-
field image) combined with carefully selected diffraction conditions gives many possibilities for
analysing and understanding your specimen.

Even without pursuing this you still have to learn to live with diffraction contrast and how it can
unhelpfully affect your TEM data (e.g. bend contours). In this way TEM is not like other types of
microscopy!

No objective aperture => ill-defined diffraction condition and image delocalization!

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