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5.

Transmission Electron
Microscopy

Dr Aïcha Hessler-Wyser
Bat. MXC 134, Station 12, EPFL+41.21.693.48.30.

Centre Interdisciplinaire de Microscopie Electronique


CIME

Intensive SEM/TEM training: TEM January 2009 1 Aïcha Hessler-Wyser

Outline

a. TEM principle


b. A little about diffraction
c. TEM contrasts
d. Examples
e. Structure analysis

Intensive SEM/TEM training: TEM January 2009 2 Aïcha Hessler-Wyser


Intensive SEM/TEM training: TEM January 2009 3 Aïcha Hessler-Wyser

Canon

Illumination

Echantillon
Projection

Intensive SEM/TEM training: TEM January 2009 4 Aïcha Hessler-Wyser


a. TEM principle

Intensive SEM/TEM training: TEM January 2009 5 Aïcha Hessler-Wyser

a. TEM principle
Lenses, general principle of optical geometry
First approximation: thin lens…
plan focal

plan focal
image

objet

Fi F
o

Fi’
Fo

fi fo

In particular, an image of the source placed at the object focal point F0 of the
condensor 2 will give a parallel illumination onto the sample

Intensive SEM/TEM training: TEM January 2009 6 Aïcha Hessler-Wyser


a. TEM principle
Parallel or converging illumination

A third lens is needed to make sure to have a parallel illumination

Intensive SEM/TEM training: TEM January 2009 7 Aïcha Hessler-Wyser

b. a little about diffraction


Interaction of electrons with the sample
Incident beam

Backscattered electrons secondary electrons


BSE SE Characteristic
X-rays

visible light
Auger electrons

“absorbed” electrons electron-hole pairs


Specimen
direct beam

Bremsstrahlung
elastically scattered
X-rays
electrons
inelastically
scattered electrons

Intensive SEM/TEM training: TEM January 2009 8 Aïcha Hessler-Wyser


b. a little about diffraction

How about
diffraction

Incident beam
Backscattered electrons secondary electrons
BSE SE Characteristic
X-rays

visible light
Auger electrons

???
“absorbed” electrons
Specimen
electron-hole pairs

direct beam
Bremsstrahlung
elastically scattered
X-rays
electrons
inelastically
scattered electrons

Intensive SEM/TEM training: TEM January 2009 9 Aïcha Hessler-Wyser

b. a little about diffraction


Mean free path
– It is the distance an electron travels between interactions with
atoms:
1 A
= =
QT N 0 T 
Differential cross section
– This term describes the angular distribution of scattering from an
atom, and is written d/d. The electrons are scattered through an
angle  into a solid angle  and both angles are linked by a simple
geometrical relation:
 = 2 (1 cos  )
d 1 d
– therefore d = 2 sin d =
d 2 sin  d

– We can calculate  for scattering into all angles which are greater
than : 2 2
d The values of  can vary form 0 to
 =  d = 2  d sind , depending on the specific type
  of scattering.

Intensive SEM/TEM training: TEM January 2009 10 Aïcha Hessler-Wyser


b. a little about diffraction
Scatter from isolated atoms
– The interaction cross section represents the chance of a particular
electron to under any kind of interaction with an atom.
– The total scattering cross section is the sum of all elastic and
inelastic scattering cross sections:
 T =  él +  inél  = r 2
Ze
where r depends on the scattering mechanisms. E.g. rél =
V
– If a specimen contains N atoms/vol, it has then a thickness t, the
probability of scattering from the specimen is givent by QTt:
N 0 T  N 0 T ( t)
QT = N T = QT t =
A A

with QT the total cross section for scattering from the specimen in
units of cm-1, N0 the Avogadro's number (atoms/mole), A the
atomic weight (g/mole) and  the atomic density.

Intensive SEM/TEM training: TEM January 2009 11 Aïcha Hessler-Wyser

b. a little about diffraction


The atomic scattering factor
An incident electron plane wave is given by:
  
 ( r ) =  0 e 2 ik  r

When it is scattered by a
scattering centre, a spherical
scattered wave is created, which
has amplitude sc but the same
phase:  
 e 2 ik  r
 sc ( r ) =  0 f ( ) 
r

where f() is the atomic scattering


factor, k the wave vectors of the
incident or scattered wave, and r
the distance that the wave has
propagated.

Intensive SEM/TEM training: TEM January 2009 12 Aïcha Hessler-Wyser


b. a little about diffraction
The atomic scattering factor
The incident electrons wave has a
uniform intensity.

Scattering within the specimen


changes both the spatial and
angular distribution of the emerging
electrons.

The spatial distribution (A) is


indicated by the wavy line.

The change in angular distribution


(B) is shown by an incident beam of
electrons being transformed into
several forward-scattered beams.

Intensive SEM/TEM training: TEM January 2009 13 Aïcha Hessler-Wyser

b. a little about diffraction


The atomic scattering factor
The atomic scattering factor is related to the differential elastic
scattering cross section by d
f ( ) =
2

d
– f() is a measure of the amplitude of an electron wave scattered
from an isolated atom.
– f()2 is proportional to the scattered intensity.

– f() can be calculated from Schrödinger's equations, and we


obtain the following description:
 E0   2
1 +

 m 0c 2  

f ( ) =
(Z  f X )
8 2 a0 sin 

 2 

f() depends on ,  and Z

Intensive SEM/TEM training: TEM January 2009 14 Aïcha Hessler-Wyser


b. a little about diffraction
The atomic scattering factor
fn = 10+14 m fé 10+14 m fX 10+14 m

(sin)/ 0.1 0.5 0.1 0.5 0.1 0.5


1H -0.378 -0.378 4'530 890 0.23 0.02
63Cu 0.67 0.67 51'100 14'700 7.65 3.85

W 0.466 0.466 118'000 29'900 19.4 12

Atomic scattering factors for neutrons (independent of !), electrons


and X rays, as a function of scattering angle and wave length  [Å].

fn : fé fX = 1 : 104 : 10
Tiré de L.H. Schwartz and J.B. Cohen, Diffraction from Materials

Intensive SEM/TEM training: TEM January 2009 15 Aïcha Hessler-Wyser

b. a little about diffraction


The structure factor
The amplitude (intensity) of a diffracted beam depends on the lattice
structure and its atom positions:

with ri th position of an atom i: ri = xi a + yi b + zi c

and K = g: K = h a * + k b* + l c *

The structure factor is given by the sum of all scattering centres (the
atoms) of the crystal that can scatter the incident wave:

Intensive SEM/TEM training: TEM January 2009 16 Aïcha Hessler-Wyser


b. a little about diffraction

Interaction: diffusion and diffraction


Each point of the object re-emits a spherical wavelet.
When all combined together, they are doing the resulting


d iffu -
wave (transmitted, scattered or backscattered)

o
rétr
If wavelets are coherent (phase relation well defined),
resulting wave is the sum of the wavelets (interference)
and the observed intensity Ic is the squared resulting
objet wave modulus (usually called "diffraction").

 e2 ikr +ai  e2 ikr +ai 


Ic (r ) =  * =
 A i' (r ) '
( )



A r

i r
i
r
  i
If wavelet phases are not correlated (uncoherent), they
cannot interfere and the observed intensity Iinc is the
sum of the intensity of each wavelet (usually called
"diffusion").
 ' e2 ikr +ai ' e2 ikr +ai 
Iinc (r ) =  ii * = 
A i (r ) A i (r ) =  Ii (r )
transmis

2
diffu

i  r r
i i

Intensive SEM/TEM training: TEM January 2009 17 Aïcha Hessler-Wyser

b. a little about diffraction


Diffraction:
Coherent elastic scattering plane wave

sample:
nel
random atoms? Fres
lattice?
spherical
wavelets

ity
intens
f
me<<matom<<msample only i
n !!!
The energy transfer (loss) from the electron to the sample is
usually negligible.
If electrons go through a thick sample:
Multiple interaction occur: dynamical effects
Diffraction patterns complex to interpret

Intensive SEM/TEM training: TEM January 2009 18 Aïcha Hessler-Wyser


b. a little about diffraction

Diffraction and Fresnel fringes


Fresnel fringes are a practical way of
measuring the coherency:

On the edge of a hole in a specimen, when the


image is out of focus, alternating dark and
bright fringes appear, they are called Fresnel
fringes. They are a phase-contrast effect.

W crystals

hole in a carbon film, 200 kV field emission gun


... up to 150 fringes visible: very high coherence

Intensive SEM/TEM training: TEM January 2009 19 Aïcha Hessler-Wyser

b. a little about diffraction

Diffraction and Fresnel fringes

Fresnel fringes can also


be used to correct the
astigmatism in the
objective lens.

b) Irregular fringes,


astigmatism.
c) Underfocussed,
uniform fringes
d) Focussed, min of
contrast, no
fringes
e) Overfocussed,
uniform fringes

Intensive SEM/TEM training: TEM January 2009 20 Aïcha Hessler-Wyser


b. a little about diffraction
Fraunhofer diffraction
Parallel illumination
Electrons arriving all parallel onto the objective lens are focussed in a
single point: a transmitted spot or a diffracted spot

a radiation

a sample
(crystal?)

Intensive SEM/TEM training: TEM January 2009 21 Aïcha Hessler-Wyser

b. a little about diffraction


The Bragg's law
Considering an electron wave incident onto a crystal, Bragg's
low shos that waves reflected off adjacent scattering centres
must have a path difference equal to an integral number of
wavelengths if they have to remain in phase (constructive
interference)

In a TEM, the to total path difference is 2dsin if the reflecting hkl


planes are spaced a distance d apart and the wave is incident
and reflected at an angle B.
Faisceau Faisceau
n=2dsin incident diffracté
 
 
d
A C

Intensive SEM/TEM training: TEM January 2009 22 Aïcha Hessler-Wyser


b. a little about diffraction
The Bragg's law
2 sin dhkl = n 

dhkl = n /2 sin



différence de  
chemin parcouru distance
d entre
plan atomiques

Elastic diffraction
k
|k| = |k’| k’

g = k-k’
Periodic arrangement of atoms in the real space:
g : vector in the reciprocal space

Intensive SEM/TEM training: TEM January 2009 23 Aïcha Hessler-Wyser

c. TEM contrasts
Imaging mode

Echantillon

Lentille objectif

Plan focal

Plan image

Intensive SEM/TEM training: TEM January 2009 24 Aïcha Hessler-Wyser


c. TEM contrasts
Diffraction mode

Echantillon

Lentille objectif

Plan focal

Plan image

Intensive SEM/TEM training: TEM January 2009 25 Aïcha Hessler-Wyser

c. TEM contrasts
Diffraction mode
Direct correlation
between the back focal
plane (first diffraction
pattern formed in the
microscope) of the
objective lens and the
screen

Imaging mode
Direct correlation
between the image plane
(first image formed in the
microscope) of the
objective lens and the
screen

Intensive SEM/TEM training: TEM January 2009 26 Aïcha Hessler-Wyser


c. TEM contrasts
Diffraction: Zone axis
Several (hi ki li) planes intersect with a common
direction [u v w] (zone axis) of the crystal.
If electron beam is along [u v w ] direction, they all
will be in Bragg condition. They satisfy the zone
equation:
hu+kv+lw=0

Each family of crystalline plane generates diffract in


a single direction. This corresponds to a single spot
the the focal plane.

picture from Morniroli


Intensive SEM/TEM training: TEM January 2009 27 Aïcha Hessler-Wyser

c. TEM contrasts
Diffraction patterns for fcc

Intensive SEM/TEM training: TEM January 2009 28 Aïcha Hessler-Wyser


c. TEM contrasts
Different type of contrasts

Thickness contrast HAADF


Z contrast (D)STEM

Diffraction contrast => BF and DF Obj. ap.

SA ap.
Phase contrast

The objective aperture allows to


select a transmitted spot to increase
the contrast in image mode

The selected area aperture allows to


select a region from which the
diffraction pattern is considered

Intensive SEM/TEM training: TEM January 2009 29 Aïcha Hessler-Wyser

c. TEM contrasts
Bright field (BF), dark field (DF)
Bright fied (BF) : the
image is formed with
the transmitted beam
only 0
Dark field (DF): the
image is formed with
one selected
diffracted beam hkl
It gives information on
regions from the
sample that diffract in
that particular
direction.
Note the particular
case ot the DF mode:
the incident beam is
tilted.

Intensive SEM/TEM training: TEM January 2009 30 Aïcha Hessler-Wyser


c. TEM contrasts
Bright field (BF), dark field (DF)
100 nm
Bright field Dark field

P.-A. Buffat

Intensive SEM/TEM training: TEM January 2009 31 Aïcha Hessler-Wyser

c. TEM contrasts
Bright field (BF), dark field (DF)

Nickel based
superalloys
Contrast /’

Intensive SEM/TEM training: TEM January 2009 32 Aïcha Hessler-Wyser


c. TEM contrasts
Bright field (BF), dark field (DF)
Segregation of chemical species in OMCVD AlGaAs structures on
patterned substrates

Can vertical
1.1
A B

1 quantum wells emit


0.9
III light?
We need local
c(Ga)normalized
concentrations to
0.8

0.7 model the


0.6
II/2
electronic
properties
II/1

I/1 I/2
0.5
0 50 100 150 200 250 300 350
distance/nm

Because of the Z dependence of the structure factor, we can observe a


chemical contrast in dark field mode!

Intensive SEM/TEM training: TEM January 2009 33 Aïcha Hessler-Wyser

c. TEM contrasts
Polysilicon on Si wafer
Bright field (BF), dark field (DF)
Bright filed image. HRTEM image
The arrows point on stressed parts of the A disorganized layer is present
interface and induced strain in the substrate. between the substrate (left) and
The film has a columnar structure the polysilicon right. The polysilicon
is polycristalline and contains
stacking faults or twins

Intensive SEM/TEM training: TEM January 2009 34 Aïcha Hessler-Wyser


c. TEM contrasts
Thickness fringes
If we admit at this stage that a transmitted
beam and a diffracted beam can interact
in the material, we can calculate the
intensity of each one. It varies periodically
with the thickness t, resulting in equal
thickness fringes.

Champ clair Champ sombre

Intensive SEM/TEM training: TEM January 2009 35 Aïcha Hessler-Wyser

c. TEM contrasts
Exctinction distance

This intensity depends on the g [nm] Al Ag Au


extinction distance: Ve cos B
g = (111) 72 29 23
Fg
(200) 87 33 25
and thus on the crystal orientation
(220) 143 46 35
and the atomic number of the
sample atoms. (400) 237 75 55

We usually admit that kinematic


g calculated for
theory is valid as long as the
metals at 300 kV
diffracted beam intensity/incident
beam intensity is lower than 10%.
Thus, the thickness limit is g g
t < t max   
 10

Intensive SEM/TEM training: TEM January 2009 36 Aïcha Hessler-Wyser


c. TEM contrasts
Thickness fringes and chemical contrast

TEM dark field image g=(200)dyn

HRTEM zone axis [001] HRTEM zone axis [001]

Intensive SEM/TEM training: TEM January 2009 37 Aïcha Hessler-Wyser

TEM: contrastes
Thickness fringes and chemical contrast

Quanum wires InP/GaInAs.

Cleaved wedge method

The bending of the fringes


indicates clearly the
presence of a chemical
concentration gradient
close to the interfaces.

P.-A. Buffat

Intensive SEM/TEM training: TEM January 2009 38 Aïcha Hessler-Wyser


TEM: contrastes
Bended samples

When a sample is deformed, the


diffraction conditions are not the
same in two different regions.

In bright field, the diffracting area


appears in dark.

It is then possible to observe lines


with a different contrast: they are
called bend contour.

Intensive SEM/TEM training: TEM January 2009 39 Aïcha Hessler-Wyser

TEM: contrastes
Bended samples

When a sample is deformed, the


diffraction conditions are not the
same in two different regions.

In bright field, the diffracting area


appear in dark.

It is then possible to observe lines


with a different contrast: they are
called bend contour.

Each line can be associated with a


family of diffracting planes. (tiré de J.V. Edington, Practical Electron
Microscopy in Materials science)

Intensive SEM/TEM training: TEM January 2009 40 Aïcha Hessler-Wyser


c. TEM contrasts
High resolution contrast (HRTEM)

Intensive SEM/TEM training: TEM January 2009 41 Aïcha Hessler-Wyser

c. TEM contrasts
Source project. pot. phase of exit wave
specimen atom pos.
FEG

Illumination
coherent

projected
potential
specimen

exit wave Problems:


defocusing for contrast: delocalization of information, information limit not used
objective lens
Spherical aberration Transfer
Cs Function
thickness

image
image of “projected
potential” defocus
Intensive SEM/TEM training: TEM January 2009 42 Aïcha Hessler-Wyser
c. TEM contrasts High Angle Annular Dark Field =HAADF

Scanning transmission (STEM)


High angle
thermal diffuse
scattering
~z2
= z-contrast

incoherent imaging:
no interference effects

dedicated STEM:
beam size ~0.1-0.2nm

Limitation: beam
formation by magnetic
lens: Cs !!!

Analytical EM: probe-size ~1nm


for EDX and EELS analysis
HRTEM HAADF-STEM
Intensive SEM/TEM training: TEM January 2009 43 Aïcha Hessler-Wyser

d. Structure analysis
Zone axis
Each diffraction spot corresponds to a well defined familly of atomic
planes.
On a diffraction pattern, the distances between the diffracted spots
depend on the lattice parameter, but their ratio is constant for each
Bravais lattice.
Quick structure identification, manual or computer assisted.

Intensive SEM/TEM training: TEM January 2009 44 Aïcha Hessler-Wyser


d. Structure analysis
Diffraction pattern indexing

Simulation: Software JEMS (P. Stadelmann)


If we propose possible crystal, it calulates its
electron diffraction for all orientations and
compares with experimental diffraction
pattern.

Intensive SEM/TEM training: TEM January 2009 45 Aïcha Hessler-Wyser

d. Structure analysis
Camera length
Diffraction spots are supposed to
converge at infinity.

The projective lenses allow us to get this


focal plane into our microscope:

The magnification of the diffraction


pattern is represented by the camera
length CL.

Intensive SEM/TEM training: TEM January 2009 46 Aïcha Hessler-Wyser


d. Structure analysis
Camera length dhkl

Diffraction spots are supposed to


converge at infinity.

The projective lenses allow us to get this


focal plane into our microscope:

2hkl
The magnification of the diffraction
pattern is represented by the camera
length CL. CL
tg(2hkl) = R/CL

For small angles,   sin  tg


and with the Bragg's law 2dhklsinhkl=n
we have: R
dhklR= CL (=cte)

Intensive SEM/TEM training: TEM January 2009 47 Aïcha Hessler-Wyser

d. Structure analysis
Phase identification

The detailed analysis of the diffrated spots gives us the crystalline


structure of the sample.

If the microscope is perfectly calibrated, it is then possible to get


the crystal interplanar distance, and thus its lattice parameter.

However, usually, we have possible strucures and diffraction


allows us to choose between the candidates.

Intensive SEM/TEM training: TEM January 2009 48 Aïcha Hessler-Wyser


d. Structure analysis
Phase identification
0-13
1-2-2

[831]

Hexagonal -(AlFeSi)

40-3

0-20

FIB lamella of  50 nm thickness, GJS600


treated
Bright Field micrograph, 2750x (Philips
CM20) [304]

Simulated diffraction on JEMS software Monoclinic Al3Fe

Intensive SEM/TEM training: TEM January 2009 49 Aïcha Hessler-Wyser

d. Structure analysis
Powder diagram
Polycrystaline TiCl

• All reflexions (i.e. all atomic planes 222


311
with structure facteur) are present
220
200
• They are also called "ring pattern" 111

• Angular relations between the


atomic planes are lost.

Intensive SEM/TEM training: TEM January 2009 50 Aïcha Hessler-Wyser


Intensive SEM/TEM training: TEM January 2009 51 Aïcha Hessler-Wyser

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