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Contrast

in TEM and STEM


Amplitude and Phase contrast
TEM STEM
TEM STEM
Amplitude contrast and
Phase-contrast images
The electron wave can change both its
amplitude and phase as it traverses the specimen

Gives rise to contrast


Si
We select imaging conditions so
SiO2
that one of them dominates.
Al2O3

Ag
Size of objective aperture
Bright Field (BF), Dark Field (DF) and High Resolution EM (HREM)

Objective
aperture

BF image DF image HREM image

Amplitude/Diffraction contrast Phase contrast


BFDF in STEM BF-DF in TEM mode

A B

Collects only electrons scattered


more than 50 mrad (~3o).
Intensity: Z-dependent.
Diameters of the Fischione
HAADF detector: 4- 28 mm.
Collects Bragg electrons
The effect of varying the
camera length (L) in STEM mode
Varying the camera length (L)
corresponds to varying the size of
an objective aperture in the
TEM mode!

STEM DF images are formed by


collecting most of the scattered
electrons on the ADF detector

The collection angle of the


detector depend on L
The effect of varying the
camera length (L) in STEM mode
Varying the cameralength (L)
correspond to varying the size of
an objective aperture in the
TEM mode!

STEM DF images are formed by


collecting most of the scattered
electrons on the ADF deteector

The collection angle of the


detector depend on L
Amplitude Contrast
Amplitude Contrast
Difference in intensity of two adjacent areas:
( I 2 I1 ) I
C
I1 I1
The eyes can not see intensity differences < 5-10%.
However, contrast in images can be enhanced digitally.

NB! It is correct to talk about strong and weak contrast,


but not bright and dark contrast

(dark and bright refers to density (number/unit area) of electrons hitting


the screen/detector)
Amplitude Contrast
Difference in intensity of two adjacent areas:
( I 2 I1 ) I
C
I1 I1
The eyes can not see intensity differences < 5-10%.
However, contrast in images can be enhanced digitally.

Si

ITO

EFTEM (16 eV): Bright = Si


Amplitude Contrast
Two principal types

Mass-thickness contrast Diffraction contrast


-Primary contrast source in amorphous -In crystaline materials
materials
-Assume incoherent electron scattering -Coherent electron scattering
(atoms scatter independently) (atoms does not scatter independently)

Both types of contrasts are seen in BF and DF images


-Can use any scattered electrons to -Two beam to get strong contrast
form DF images showing mass- in both BF and DF images.
thickness contrast

In TEM and STEM mode


Mass-Thickness
Contrast
Rutherford Scattering
Mass thickness contrast arises from incoherent elastic scattering
(Rutherford scattering)

- Peaked in the forward direction in thin samples

- t and Z-dependent

Differential cross-section for high angle scattering:

1. Cross-section for elastic scattering is a function of Z


2. As t increases, more elastic scattering because the mean elastic free
path is fixed
TEM variables that affect the contrast:
-The objective aperture size (large -- bad).
-The high tension of the TEM (small -- good)
TEM variables that affect the contrast:
-The objective aperture size (large -- bad).
-The high tension of the TEM (small -- good)
Objective aperture size effect on
mass-thickness contrast in TEM mode

d=70 m d=10 m

Similar effect as reducing the HT of the microscope


Calculate the mass thickness contrast: kV

Atom. Nr.

Collection semi-angle Characteristic screening angle


(angle of collection of the obj. app.) (by the electron cloud)

Derived from:

To determine the probability that an e- will be scattered farther


than a given angle.
Imaging electron scattering at:

1. Low angles (<~5o) : - Mass-thickness contrast + Bragg diffraction

2. Higher angles: - Only mass-thickness contrast


(low intensity scattered beams)
- Intensity only depends on Z (and on thickness)

Only mass-thickness contrast How?


A) Amorphous samples: All contrast is mass contrast
B) Crystalline samples: ADF/HAADF mode
Imaging electron scattering at:

1. Low angles (<~5o) : - Mass-thickness contrast + Bragg diffraction

2. Higher angles: - Only mass-thickness contrast


(low intensity scattered beams)
- Intensity only depends on Z (and on thickness)

Only mass-thickness contrast:


A) Amorphous samples: All contrast is mass contrast
B) Crystalline samples: ADF/HAADF mode
STEM- ADF
1. Less noisy than DF-TEM: Gathers all scattered
electrons, not just electrons scattered from one atomic
plane.

2. The lenses are not used to make the ADF image less
chromatic aberration.

3. More contrast than TEM-DF: Adjust L to optimize the e- ( DF)


ratio of the number of scattered e- hitting the detector.

4. Lower resolution than TEM-DF (probe size + intensity)

5. Alignment, alignment, alignment

When use STEM: e- ( BF)


- Thick specimen (aberrations)
- Beam-sensitive specimens ()
- Specimen has low contrast in TEM
- Z-contrast
DF: TEM - STEM
STEM ADF contrast is greater than DF TEM Optimal L

TEM-DF STEM-ADF

The TEM image of the two phase polymer is noisier, but


has better resolution.
HAADF
At high angles (> 5o) Bragg scattering is negligible:
Z-contrast images HAADF images.

TEM

Z-contrast
(Bi in Si)

HAADF has the advantage that the contrast is generally unaffected by


small changes in objective lens defocus (Df) and specimen thickness.
Noise reduction of
Z-contrast images
HAADF images can be processed
and refined via a maximum entropy
approach to reduce noise.

Direct map of f() variation in the specimen


(similar to an X-ray map).

Grain boundary in SrTiO3


Example of HR Z-contrast
with the HAADF detector
Atomic structures are visible in both
HREM and HAADF images.
HAADF image:
noisier but Z-contrast.

Relate the intensity differences to an


absolute measure of the Bi concentration:

Cross-section for elastic scattered by matrix A


Contrast
Fraction of the alloying element that sub.
For matrix atoms

HREM-TEM HR Z-contrast STEM

Atomic concentration of alloying element


Alloying/dopant B
Example of mass-thickness contrast in TEM mode-
Metal shadowing
BF-TEM image of latex particles on an
amorphous C-film.

The contrast is t-dependent.

What is the shape of the particles?

Effect of evaporation of a heavy metal


(Au or Au-Pd) thin coating at an oblique angle.

What is the contrast due to in the image?

Effect of inversing the contrast of the image.

The uneven metal shadowing increases


the mass contrast and thus accentuates
the topography.
Enhancement of contrast -
Staining of polymers and biological specimens
Heavy metal stains: Os, Pd and U

The heavy metals are left in spesific regions of the structures:


Unsaturated C=C bonds in polymers and cell walls in biological tissue.

Stained two phase polymer (BF-STEM mode)


(BF-TEM mode)
Increased contrast, but
lower image quality (unless FEG).
Diffraction Contrast
TEM diffraction contrast

Bragg diffraction contrast: - Coherent elastic scattering


(atoms do not scatter independently)
- Crystal structure
- Orientation of the sample
Two-beam condition
S: small and positive
1. What is S?
The excess hkl Kikuchi line, just outside the
2. And how to
hkl spot;
determine S ?

Diff. rotation
Two-beam condition
S: small and positive
The excess (bright) hkl Kikuchi line, just
outside the hkl spot;

S is..?
Variation in the diffraction contrast when s is varied from

zero small + larger +

TEM always shows better contrast than STEM images


How to make a CDF - TEM
Contrast Examples
Examples

1. Two types of steel (Martensite + Austenite)


Examples

1. Two types of steel (Martensite + Austenite)


Examples

1. Two types of steel (Martensite + Austenite)

2. Erbium-oxide nanoclusters in silicon oxide


Examples

1. Two types of steel (Martensite + Austenite)

2. Erbium-oxide nanoclusters in silicon oxide


Summary
Mass-thickness contrast
-Areas of greater Z and or t scatter more strongly
-TEM images are better quality (lower noise and higher resolution) than
STEM images, but digital STEM images can be processed to show higher
contrast than analog TEM images.
-STEM mass-thickness contrast images are most useful for thick and/or
beam-sensitive specimens.
-Z-contrast (HAADF) images can show atomic-level resolution.

Diffraction contrast
-Arises when the electrons are Bragg scattered.
-In TEM, the objective aperture selects one Bragg scattered beam.
-Often, the STEM detectors gather several Bragg beams which reduce
diffraction contrast.
-TEM always shows better contrast than STEM images (noisier and almost
never used)
Phase-Contrast Imaging

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Size of objective aperture
Bright Field (BF), Dark Field (DF) and High Resolution EM (HREM)

Objective
aperture

BF image DF image HREM image

Amplitude/Diffraction contrast Phase contrast


Phase Contrast Imaging
Exploits differences in the refractive index of different materials to differentiate
between structures under analysis

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Why different phases?
- Transmitted and diffracted waves travel
through different distances in the crystal
- Each diffracted wave will have its own
phase
- Each diffracted wave represents a
different solution to the Schrdinger
equation

When several waves are allowed to interact, the phase differences manifest
themselves in the 2-D interference pattern in the image plane
--- Phase contrast image

Factors that contribute to the phase shift:


Thickness, orientation, scattering factor, focus and astigmatism.

Be careful when interpreting them

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Be careful when interpreting the images

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The origin of the lattice fringes (2-D interference pattern)

Rewrite the wave equation for two beams:

KD = K + KI
K is the difference vector : K = KD KI

K = Sg + g

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The intensity in the image: I = *

Now g0 is effectively perpendicular to the beam so well set it parallel to x and replace d giving

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Summary
- Phase contrast Many beam imaging High resolution imaging
- Interference pattern
- - Be careful when interpret the images Image simulations

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