Chapter 16 - High-Resolution TEM PDF

High Resolution Transmission Electron
Microscopy
P. Stadelmann
CIME-EPFL
Bât. MX-C, Station 12
CH-1015 Lausanne
Switzerland
Pierre.Stadelmann@epfl.ch
30 janvier 2009
P. Stadelmann CIME-EPFL Bât. MX-C, Station 12 CH-1015 Lausanne High

Switzerland
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Pierre.Stadelmann@epfl.ch
Transmission Electron Microscopy
What is HRTEM ?
1 TEM imaging technique at atomic resolution.

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What is HRTEM ?

2 Atomic columns.

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What is HRTEM ?

2 Atomic columns.
3 Very thin samples.

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What is HRTEM ?

2 Atomic columns.
3 Very thin samples.
4 High symmetry orientation.

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Example 1 : ZrO2
Questions : where are the atoms ? Do we see the oxygen

atoms ?
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Example 2 : Au particle
Question : do the atoms appear as white or dark spots ?

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Nano crystals

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Indium oxide

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PbTiO3 : CM300
Tm = 205 °C Tm = 300 °C
4 nm 4 nm
Tm = 400 °C Tm = 452 °C
4 nm 4 nm

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Ray optics : principal rays
FFP BFP
o
i
Fi
Fo O z
f f
In the back focal plane of the lens T & D beams converge to

points (secondary spherical sources).
Why is the objective lens so most important lens of the TEM ?
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Perfect optical system

PE PS
PS
PE
ye
O ys
z
-ys
-ye
PE entrance and PS exit pupils.

O (object) and I (image) are conjugate points (what does it
mean ?).
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Spherical aberration
PE PS
P M
Ao
Ai

ri
A'i
Wavefront is deformed −→ inclined incidents rays are not focused

at same point.
Coefficient of spherical aberration Cs is close to the focal length f
of the objective lens.
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Important properties of optical system S
The optical system has two important properties :

1 Linearity.

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1 Linearity.
2 Space invariance.

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1 Linearity.
2 Space invariance.
3 1 + 2 −→ optical system characterized by a transfer
function T̃ (k ).

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1 Linearity.
2 Space invariance.
3 1 + 2 −→ optical system characterized by a transfer
function T̃ (k ).
4 What does it mean ?

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Linearity
S {a1 Ψ1o (x ) + a2 Ψ2o (x )} = a1S {Ψ1o (x )} + a2S {Ψ2o (x )}
S {a1 Ψ1o (x ) + a2 Ψ2o (x )} = a1 Ψ1i (x ) + a2 Ψ2i (x )
Allows to :
decompose the object wavefunction into points sources.
consider only the transfer by the optical system of a point
source (impulse).
∞
Ψo (x ) = Ψo (u )δ(x −u )du
−∞

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Impulse response
Image wavefunction Ψi (x ) is :
∞
Ψi (x ) = S Ψo (u )δ(x −u )du
−∞
By linearity property (Ψo (x ) → coefficients real or complex) :

∞
Ψi (x ) = Ψo (u )S {δ(x −u )}du
−∞
Optical system impulse response t (x ;u ) :
t (x ;u ) = S {δ(x −u )}
By linearity one has to consider only how the optical system

transfer a spherical wave (point source).
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Space invariance : point spread function
t (x ;u ) = t (x −u )

Transfer is a convolution integral of Ψo (u ) and the point spread
function t (x ) :
∞
Ψi (x ) = Ψo (u )t (x −u )du = Ψo (x ) ⊗ t (x )
−∞
In Fourier space (or reciprocal space) :
i (k ) = Ψ
Ψ o (k )T
(k )

2
Cs λ3 k 4 Δf λ k
−2π ı 4 − 2
T̃ (k ) = e
Electrical systems have the property of time invariance.

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Abbe image formation : transfer function
Diffusion Plan
& focal
Interference image
Objet S1
u
z
-u
S-1
f
~ ~
(x) (u) T(u)
π
Remember 2 phase shift of the diffracted beams !
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Understanding HRTEM image formation
Very simple object model : weak phase object approximation

(WPOA).
Crystal potential V (r ) (constant over dz small enough),
wavevector is (e E + V (r )) :

2 m e (E + V (r ))
k=
h2
Imagine a plane wave arriving on a crystal.
How does the wavefront deform ?

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Refraction index n
Refraction index of object n −→ ratio object wavevector and

wacuum wavevector (|V (r )| << E :

km E + V (r ) V (r )
n= = ≈ 1+
kv E 2E
=⇒ phase change dϕ as a function of object thickness dz :
χ
dϕ = (km − kν ) · dr = (n − 1)|kν |dz = V (r )dz
2E
with χ = |kv |.
Question : value of n (compare to glass) ?

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Phase object transmittance

For object of thickness Δz, phase shift Δϕ written as :

χ z +Δz
Δϕ = V (x ; z )dz
2E z
χ
= Vp (x ; z )Δz
2E
Transmittance function of phase object over Δz is :
Ψo (x ) = e 2πıΔϕ
χ
= e 2πı 2E Vp (x ;z )Δz
= e ıσVp (x ;z )Δz
πχ π
with σ = E = λE .
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WPOA : weak phase object
Ψo (x ) = e ı σVp (x ;z ) ≈ 1 + ı σVp (x ; z )Δz
In the back focal plane of the objective lens (Fourier

transform) :
o (k ) = δ(k ) + ı σ V
Ψ p (k; z )Δz

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i (k ) image wavefunction (back focal plane)

Ψ
Abbe image formation model :
i (k ) = Ψ
Ψ o (k )T
(k )
o (k )e −2πıχ(k )
= Ψ
where χ(h ) is (defocus Δf and spherical aberration Cs ) :
Cs λ3 (k · k )2 Δf λ(k · k )
χ (k ) = −
4 2

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Ψi (x )Ψi∗ (x ) image intensity (image plane)
In objective lens back focal plane :

Ψi (k ) = δ(k ) + ı σVp (k; z )Δz ][cos 2πχ(k ) − ı sin 2πχ(k )
Choosing sin 2πχ(k ) = −1 et cos 2πχ(k ) = 0 for diffracted

beams k , Ψ
i (k ) becomes :
i (k ) = δ(k ) − σV
Ψ p (k; z )Δz
Image intensity (Ψi (x )Ψi∗ (x )) given by :
I (x ) = (1 − σVp (x ; z ))(1 + σVp (x ; z )) ≈ 1 − 2σVp (x ; z )Δz
Dark dots at the position of the atomic columns !

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Remarks
π
1 Transfer function compensates the 2 phase shift due to
diffraction.
2 Direct interpretation of HRTEM micrographs possible.
3 Spots are darker when projected potential is important
(heavy atoms).
4 Spots are darker when specimen thickness increases.
5 WPOA approximation only valid for very thin crystals (Au ≤
1 unit cell !).
sin 2πχ(k ) = −1 is selected by changing the specimen defocus
Δz .

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WPOA : contrast inverted micrographs
Choosing sin 2π χ(h ) = 0 et cos 2π χ(h ) = −1, (Ψi (x )Ψi∗ (x ))
is since :
i (h ) = [δ(h ) + ı σ V
Ψ p (h; z )Δz ]
I (x ) = (1 − ı σ Vp (x ; z )Δz )(1 + ı σVp (x ; z )Δz )

= 1 + σ2 Vp2 (x ; z )Δz 2
White dots at the position of the atomic columns !

Contrast no more proportional to projected potential. Very small
Δz change necessary to get contrast inverted micrographs.

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Model : Ti2Nb10O29

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Image simulation : Ti2Nb10O29
Questions : where are the atoms ? Do we see the oxygen

atoms ?
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Aberrations corrected TEM
Transfer function limited by gun and objective lens current

instabilities (and incident beam convergence).

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High Resolution Transmission Electron

P. Stadelmann CIME-EPFL Bât. MX-C, Station 12 CH-1015 Lausanne High

1 TEM imaging technique at atomic resolution.

P. Stadelmann CIME-EPFL Bât. MX-C, Station 12 CH-1015 Lausanne High

1 TEM imaging technique at atomic resolution.

P. Stadelmann CIME-EPFL Bât. MX-C, Station 12 CH-1015 Lausanne High

1 TEM imaging technique at atomic resolution.

P. Stadelmann CIME-EPFL Bât. MX-C, Station 12 CH-1015 Lausanne High

1 TEM imaging technique at atomic resolution.

P. Stadelmann CIME-EPFL Bât. MX-C, Station 12 CH-1015 Lausanne High

Questions : where are the atoms ? Do we see the oxygen

Question : do the atoms appear as white or dark spots ?

P. Stadelmann CIME-EPFL Bât. MX-C, Station 12 CH-1015 Lausanne High

P. Stadelmann CIME-EPFL Bât. MX-C, Station 12 CH-1015 Lausanne High

P. Stadelmann CIME-EPFL Bât. MX-C, Station 12 CH-1015 Lausanne High

In the back focal plane of the lens T & D beams converge to

Perfect optical system

PE entrance and PS exit pupils.

Wavefront is deformed −→ inclined incidents rays are not focused

Important properties of optical system S

The optical system has two important properties :

P. Stadelmann CIME-EPFL Bât. MX-C, Station 12 CH-1015 Lausanne High

The optical system has two important properties :

P. Stadelmann CIME-EPFL Bât. MX-C, Station 12 CH-1015 Lausanne High

Important properties of optical system S

The optical system has two important properties :

P. Stadelmann CIME-EPFL Bât. MX-C, Station 12 CH-1015 Lausanne High

The optical system has two important properties :

P. Stadelmann CIME-EPFL Bât. MX-C, Station 12 CH-1015 Lausanne High

P. Stadelmann CIME-EPFL Bât. MX-C, Station 12 CH-1015 Lausanne High

By linearity property (Ψo (x ) → coeﬃcients real or complex) :

t (x ;u ) = S {δ(x −u )}

By linearity one has to consider only how the optical system

Space invariance : point spread function

t (x ;u ) = t (x −u )

Electrical systems have the property of time invariance.

Understanding HRTEM image formation

Very simple object model : weak phase object approximation

P. Stadelmann CIME-EPFL Bât. MX-C, Station 12 CH-1015 Lausanne High

Refraction index of object n −→ ratio object wavevector and

P. Stadelmann CIME-EPFL Bât. MX-C, Station 12 CH-1015 Lausanne High

Phase object transmittance

Ψo (x ) = e ı σVp (x ;z ) ≈ 1 + ı σVp (x ; z )Δz

In the back focal plane of the objective lens (Fourier

P. Stadelmann CIME-EPFL Bât. MX-C, Station 12 CH-1015 Lausanne High

 i (k ) image wavefunction (back focal plane)

Abbe image formation model :

where χ(h ) is (defocus Δf and spherical aberration Cs ) :

P. Stadelmann CIME-EPFL Bât. MX-C, Station 12 CH-1015 Lausanne High

Choosing sin 2πχ(k ) = −1 et cos 2πχ(k ) = 0 for diﬀracted

Image intensity (Ψi (x )Ψi∗ (x )) given by :

I (x ) = (1 − σVp (x ; z ))(1 + σVp (x ; z )) ≈ 1 − 2σVp (x ; z )Δz

Dark dots at the position of the atomic columns !

P. Stadelmann CIME-EPFL Bât. MX-C, Station 12 CH-1015 Lausanne High

I (x ) = (1 − ı σ Vp (x ; z )Δz )(1 + ı σVp (x ; z )Δz )

White dots at the position of the atomic columns !

P. Stadelmann CIME-EPFL Bât. MX-C, Station 12 CH-1015 Lausanne High

P. Stadelmann CIME-EPFL Bât. MX-C, Station 12 CH-1015 Lausanne High

Questions : where are the atoms ? Do we see the oxygen

Aberrations corrected TEM

Transfer function limited by gun and objective lens current

P. Stadelmann CIME-EPFL Bât. MX-C, Station 12 CH-1015 Lausanne High

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i (k ) image wavefunction (back focal plane)