Contrast in TEM and STEM Amplitude and Phase contrast.

Contrast in TEM and STEM

Amplitude and Phase contrast

TEM STEM

Amplitude contrast andPhase-contrast images

We select imaging conditions so that one of them dominates.

Si

SiO2

Al2O3

Ag

The electron wave can change both its amplitude and phase as it traverses the specimen

Gives rise to contrast

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

BF image

Objectiveaperture

DF image

Amplitude/Diffraction contrast

HREM image

Phase contrast

BF–DF in STEM

Collects Bragg electrons

Collects only electrons scatteredmore than 50 mrad (~3o). Intensity: Z-dependent.

Diameters of the Fischione HAADF detector: 4- 28 mm.

A B

BF-DF in TEM mode

The effect of varying the camera length (L) in STEM mode

The collection angle of the detector depend on L

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

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 effect of varying the camera length (L) in STEM mode

Amplitude Contrast

Amplitude Contrast• Difference in intensity of two adjacent areas:

11

12 )(

I

I

I

IIC

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:

11

12 )(

I

I

I

IIC

Si

ITO

EFTEM (16 eV): Bright = Si

The eyes can not see intensity differences < 5-10%.However, contrast in images can be enhanced digitally.

Amplitude Contrast

Mass-thickness contrast Diffraction contrast

Two principal types

Both types of contrasts are seen in BF and DF images

-Primary contrast source in amorphousmaterials

In TEM and STEM mode

-In crystaline materials

-Assume incoherent electron scattering(atoms scatter independently)

-Coherent electron scattering(atoms does not scatter independently)

-Can use any scattered electrons to form DF images showing mass-thickness contrast

-Two beam to get strong contrast in both BF and DF images.

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 Z2. 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)

Objective aperture size effect on mass-thickness contrast in TEM mode

d=70 μm d=10 μm

Similar effect as reducing the HT of the microscope

Calculate the mass thickness contrast:

Characteristic screening angle (by the electron cloud)

Collection semi-angle(angle of collection of the obj. app.)

kV

Atom. Nr.

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 contrastB) 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 contrastB) Crystalline samples: ADF/HAADF mode

STEM- ADF1. 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 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:-Thick specimen (aberrations)-Beam-sensitive specimens (…)-Specimen has low contrast in TEM-Z-contrast

e- ( BF)

e- ( DF)

DF: TEM - STEM

The TEM image of the two phase polymer is noisier, but has better resolution.

STEM ADF contrast is greater than DF TEM Optimal L

TEM-DF STEM-ADF

HAADF

HAADF has the advantage that the contrast is generally unaffected by small changes in objective lens defocus (Df) and specimen thickness.

TEM

Z-contrast(Bi in Si)

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

Noise reduction of Z-contrast images

Grain boundary in SrTiO3

HAADF images can be processed and refined via a maximum entropy approach to reduce noise.

Direct map of f(θ) variation in the specimen(similar to an X-ray map).

Example of HR Z-contrast with the HAADF detector

HREM-TEM HR Z-contrast STEM

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:

Contrast Cross-section for elastic scattered by matrix A

Fraction of the alloying element that sub. For matrix atoms

Alloying/dopant BAtomic concentration of alloying element

The uneven metal shadowing increases the mass contrast and thus accentuates the topography.

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.

Effect of inversing the contrast of the image.

What is the contrast due to in the image?

Enhancement of contrast -Staining of polymers and biological specimens

Stained two phase polymer (BF-TEM mode)

(BF-STEM mode)

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.

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

The excess hkl Kikuchi line, just outside the hkl spot;

Diff. rotation

1. What is S?2. And how to determine S ?

Two-beam conditionS: small and positive

The excess (bright) hkl Kikuchi line, just outside the hkl spot;

S is..?

zero small + larger +

Variation in the diffraction contrast when s is varied from

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)

2. Erbium-oxide nanoclusters in silicon oxide

SummaryMass-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 reducediffraction contrast.-TEM always shows better contrast than STEM images (noisier and almost never used)

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Phase-Contrast Imaging

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

BF image

Objectiveaperture

DF image

Amplitude/Diffraction contrast

HREM image

Phase contrast

Phase Contrast Imaging

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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 Schrödinger 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:

K is the difference vector : K = KD – KI

KD = K + KI

K = Sg + g

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

The intensity in the image: I = ψ*ψ

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Summary

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

Contrast in TEM and STEM Amplitude and Phase contrast.

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Transcript of Contrast in TEM and STEM Amplitude and Phase contrast.