High Resolution Electron Microscopy (HRTEM) Techniques

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Ch. B. Lioutas
High Resolution Electron

Microscopy (HRTEM)
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Autumn International School

on growth and structural characterization
of advanced materials
Oludeniz, Turkey - October 2014
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The Optical Microscope
Geometrical optics
Dual character of electrons

ELECTRON-OPTICS
Description completely analogous to the light rays
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Ch. . Lioutas AISMAT 2014, HRTEM
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THE MICROSCOPE
Imaging & Diffraction
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(linear
(linear optics)
optics)
Projector
Diffraction
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Diffraction
general effect of wave phenomena occurring whenever a portion
of a wavefront (elastic, electromagnetic or matter wave) is
obstructed in some way
The wavefront is modified from one point to the next one
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Final Result on the observed image

Deviation of the intensity distribution that is predicted from the
linear propagation
Increasing or decreasing of the intensity at unexpected points
that give rise to bright or dark fringes
Electron diffraction
A( ) =
2 mo e
h2
s
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u
(Fourier
(Fourier Transform)
Transform)
V (r) exp[i 2 K r]d
The integral gives the Fourier Transform of the function that describes the
potential of the material that induces the electrons diffraction
The intensity of every diffracted beam
in Fraunhofer diffraction conditions
is proportional to Fourier Transform
and is observed on the back focal plane of the
imaging lens
A lens visualizes
B
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C
The electron Microscope
Electrons
Electrons source
Condensor
specimen
Objective
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Objective aperture
1st intermediate image
Intermediate
2nd intermediate image
Projector
Final image (x 1.5M)
Screen
2 mo e
h2
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V (r) exp[i 2 K r]d
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According to J.B. Fourier:

A periodic function V(x) with period a can be written as
a sum of harmonic functions A(u)
Fourier components with frequencies u=n/a
Every Fourier component contains
information about the details of order a/n of V(x)
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For crystals V(r) is a periodic function in three dimensions

A(K) are Fourier components spatial frequencies corresponding to diffracted
beams
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(working
(working modes)
modes)
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B
A(K ) =
(Inverse
(Inverse Fourier
Fourier Transform)
Transform)
The integral gives the Fourier Transform of the function that describes the
potential of the material that induces the electrons diffraction
o
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.
the Fourier Transform of the function

that describes the imaging object
Electron
Electron diffraction
diffraction
SAD
selective area
diffraction
condensor
aperture
Back focal plane
Selective
area
aperture
Final
diffraction
image
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Imaging modes
final image depends on

the number of the
diffracted beams used
for image formation
Insertion of aperture on
the back focal plane of
the objective lens
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B
diffraction image
(imaging
(imaging modes)
modes)
Higher order diffracted beams contain

information details of the object
n-th order beam corresponds to a grading with
period d/n beams.

Imaging modes
final image depends
on the number of the
diffracted beams used
for image formation
Insertion of
aperture on the back
focal plane of the
objective lens
Imaging Theory & Diffraction
II
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Ernst Abbes Imaging Theory, 1872
first step
In every single case the interaction of the light beam (or incident wave) with the
object can be described by the diffraction of the lights wavelet.
A Fraunhofer diffraction image appears on the back focal plane of the objective lens.
B
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Imaging Theory & Diffraction
Ernst Abbes Imaging Theory, 1872
Mathematical analysis of the

Fraunhofer diffraction proves
that the diffraction image
represents the Fourier
Transform of the objects
transparence function
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Higher order diffracted beams contain

information details of the object
n-th order beam corresponds to a grading with
period d/n beams.
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C
s
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(imaging
(imaging modes)
modes)
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B
Periodic objects diffraction image consists of sharp spots

Continuous object gives rise to continuous diffraction pattern
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II
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second step
The back focal plane acts as a set of Huyghens sources

The final image is produced from the interference of the diffracted beams on the
back focal plane of the eyepiece lens.
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Image formation represents the

inverse Fourier Transform of
the diffraction image
(x,y)= F -1[Q(u,v)]
The intensity of the observed

image is
Iuv ~ |(x,y)|2
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Q(u,v)=F [q(x,y)]
The spatial frequencies

correspond to the diffracted
beams with intensities
Fuv = |Q(u,v)|2
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Imaging in TEM
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Bright
Bright Field
Field (BF)
image formation only

from the undiffracted
beam
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(imaging
(imaging modes)
modes)
Dark
Dark Field
Field (DF)
High
High Resolution
Resolution (HRTEM)
image formation only

from one of the
diffracteed beams
image formation from the

undiffracted as well from a
number of diffracted beams.
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Electrons versus Light
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Magnification of an optic instrument is related with to the resolution limit.

The minimum distance to distinguish two points of the observed object
= 0.61/
wavelength,
an instruments parameter ~1
Optical microscope
~ 492nm
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300 nm
Electron microscope
=100keV
=0.0037nm
L
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2.3 10-3 nm
B
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(Rayleigh 19th century )
lenses aberrations
Phase Contrast Microscopy
A lot of objects change the phase rather than

the intensity of the incident beam
In the simple case of an one dimensional
object the wave function at the exit surface of
the specimen is
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h
q(x)=exp[i(x)]
(x) the phase change at the point x
The ideal Microscope produces an image

performing two Fourier Transforms
The intensity distribution on the image plane
|q(x)|2=|exp[i(x)]|2=1
There is NO CONTRAST
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q(x)=exp[i(x)]
Q(u)=F [q(x)]
(x)=F 1[Q(u)]
(x)= exp[i(x)]
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0.1 nm
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PHASE
MICROSCOPY
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In the case of a Weak Phase Object (WPO)
(x) << 1
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The intensity on the image plane
|(x)|2=(1+i(x))(1-i(x))=1- (x)2 ~ 1
(x) << 1,
(x)2
~0
((WPO)
WPO)
q(x)=exp[i(x)]
~ 1+ i(x)
Q(u)=F [q(x)]
F [1+ i(x)]=
(x)+ iF [(x)]
(x)=F 1[Q(u)]
(x)~1+i(x)
There is NO CONTRAST
CONTRAST is the difference in intensity (I)

between two adjacent areas C=I / Io
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s
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In the case of a Weak Phase Object (WPO)
(x) << 1
Q1(u)=
(x)+ iF [(x)]ei/2=
(x) - F [(x)]
(in the optical microscope by inserting a glass plate )
The intensity on the image plane
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|(x)|2=[1-(x)]2=1- 2(x)+(x)2 ~1-2(x)

(x) << 1, (x)2 ~ 0
(x)=F 1[Q1(u)]
B
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V << E (energy of the incident electrons)
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B
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The total phase shift in any point at the exit surface of the specimen is
calculated by integration over all the thickness of the specimen
(x,y)=
(x,y) yields the potentials projection

along electron beam, direction Oz
V(x,y,z)dz = (x,y)
.
h
The specimen interacts as pure phase object with

two dimensional transparency function
We can take account of electrons absorption
by including a function (x,y)
q(x,y)=exp[i (x,y) (x,y)]
(x,y) varies from point to point on the unit cell projection

For a very large number of materials (x,y) << 1 when z 10 nm
q(x,y) 1 + i (x,y)] the specimen acts as Weak Phase Object
vacuum
h
(2meE )1/ 2
= /
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Electron
Electron Microscope
Microscope -- Optical
Optical System
System
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The transfer of the information from the object
Imaging
(exit face of the specimen)
to the image plane

It can be represented with a function H(u) including three factors
(in reciprocal space)
u=sin()/ /
( the diffraction angle)
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q(x,y)=exp[i (x,y)]
specimen
Apertures
Attenuation of the wave
Aberrations of the lens
The absorption term does not affect the result in the final image contrast in the first order approximation
2 1 V
dz = Vdz
2 E
dx(z )
Extension in two dimensions

without any difference
The specimen as Phase Object
1/ 2
2 (E +V)1/2 = 2 + V
1
1
1
dz
E1/2
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dx(z) =
(x)~1 - (x)
The CONTRAST on the image plane is a

PERFECT REPRESENTATION of the objects
phase
0
2
1 1
2
dx( z ) = 2 dz = 1 dz

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(x)+ iF [(x)]
It is possible to induce a phase shift of /2

in diffracted beams only
4
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Any specimen is characterized by a three-dimensional

potential V(x,y,z) that induces a phase shift dx(z) along the
propagation of the electrons wave
h
in a distance dz (relative to the propagation in the vacuum) (r ) = {2me[ E + V (r )]}1/ 2
q(x)=exp[i(x)]
~ 1+ i(x)
Q(u)=F [q(x)]
F [1+ i(x)]=
The specimen as Phase Object
The aperture function A(u)

The envelope function E(u)
The aberration function B(u)
H(u) = A(u) E(u) B(u)
Describe the cut off all values of u greater than some selected value
A(u) imposed by objective diaphragm (radius of the aperture)
E(u) property of the lens itself (may be either more or less restricting than A(u))
B(u) is usually expressed as:
B(u)= exp[i (u)]
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(u) the phase sift induced by the electron microscope

20
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The
The Electron
Electron Microscope
Microscope as
as phase
phase contrast
contrast microscope
microscope
The specimen acts as pure phase object with

transparency function proportional to the
projection of the structures potential
The phase sift induced by the electron microscope

is a function of the diffraction angle mainly affected by:
Spherical
aberration
() = 2 Cs +
(x,y)=
o
i
electrons wavelength
Accelerating voltage
spherical aberration coefficient

given instruments manufacturer
q(x,y)=exp[i
(x,y)]
z
Defocus
Cs
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The Resolving Power of the Microscope
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B
Point or structural resolution s

the minimum distance between to points of the object
in order to be resolved in the image plane
projection of a crystals structure
.
h
electron diffraction
diffracting object (crystal)
the instruments parameters
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V=200 kV s=0.19 0.3 nm

V > 200kV s=0.12 nm
Line resolution
the minimum distance between two parallel lines on the object
in order to be resolved in the image plane.
atomic planes
V=200 kV =0.14 0.2 nm
l
(x)+ iF [(x)]
Q1(u)=
(x)+ iF [(x)]ei/2=
(x) - F [(x)]
HRTEM image Contrast

exact representation of the objects phase
proportional to the projection of specimens
potential
Direct illustration of structural characteristics
of the specimen
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s 0.66 Cs1/4 3/4
Intensity on the image plane
|(x,y)|2=[1-(x,y)]2 ~1-2(x,y)
Electron Microscope Phase Contrast Microscope
B
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Q(u)=F [q(x)]=
F [1+ i(x)]=
Induced by spherical aberration & defocus
defocus value
selected during observation
L
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(x)=F 1[Q1(u)]
(x)~1 - (x)
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III
IMAGE SIMULATION
& PROCESSING
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q(x)=exp[i(x)]
~ 1+ i(x)
0
2
V(x,y)dz= (x,y)
phase sift of -/2
For an optimum defocus value (Scherzer defocus)

() takes the value of /2 or equivalent sin[()] = -1
for a large range of values
High
High Resolution
Resolution Electron
Electron Microscopy
Microscopy
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Structural Analysis
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The contrast on the HRTEM micrograph has lost the phase of the electrons
wavefunction that holds the projection of the 3D potential of the
specimen
How is possible to have interpretable structural details ?
(electron beam aligned along a low-index zone axis)
B
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HRTEM micrographs Simulation
The parameters for every structure model:

Specimen Thickness & Defocus Values
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A set of images for a

series of Thickness &
Defocus Values
Selection of the optimum

conditions by comparison
with experimental images
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HRTEM IMAGE SIMULATION SOFTWARE
Cerius2
by Accerlys
Runs on UNIX
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EMS & jEMS
by Pierre Stadleman (Very widely used and user-friendly)
Multi-platform: Mac, Unix, Windows. The j denotes the java version
Kirkland
by Earl Kirkland. Well described in his book on the subject
MacTEMPAS
by Roar Kilaas
Runs on a Mac (so its very user-friendly)
WinHREM & MacHREM
by HREM Research Inc. (Kazuo Ishizuka)
25
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Thickness
Thickness -- Defocus
Defocus Matrix
Matrix
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B
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Mathematical relations (analytical or numerical) accurately reproducing

reproducing
Interaction Electron Beam - specimen (Diffraction)
Diffraction)
Interaction Electron Beam Lenses , Apertures (Imaging)
Imaging)
COMPUTER CALCULATION
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Experimental requirements
Very thin specimen
Defocus close to that of Scherzer value
Appropriate projection
HRTEM micrographs Simulation
interpretation
interpretation of
of HRTEM
HRTEM micrographs
micrographs
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Image Processing on HRTEM micrographs
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Computer
Image Processing
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REAL image
from the microscope
Digitized Image
Processed Image
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extract more information from the

data than we can obtain by eye
Transfer the image directly from the TEM to the

computer via CCD camera
Record the image on film, then digitize it using scanner
Print out the recorded on the film image and use a
scanner
Fourier filtering & Reconstruction
Averaging and pattern recognition
Reconstructing the Phase
.
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HRTEM examples
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FeSi2 along [012]
IV
EXAMPLES
& CASE STYDIES
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HRTEM micrograph
dislocation in SiGe
Burgers vector determination
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HRTEM examples
projection of the
crystal structure
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s
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10
10
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II
HRTEM
HRTEM image
image simultion
simultion
intense dots Si complex
less intense dots Fe-I
very weak dots Fe-II
HRTEM examples
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HRTEM images from

stacking faults in CdTe
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II
II
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HRTEM examples
V
V
Grain boundaries
B
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C
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High Resolution Electron

Microscopy (HRTEM)
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Polycrystalline Si
in amorphous SiO2 matrix
Ch. B. Lioutas
Oludeniz, Turkey - October 2014
HRTEM examples
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Autumn International School

on growth and structural characterization
of advanced materials
0
2

High Resolution Electron Microscopy (HRTEM) Techniques

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High Resolution Electron

Autumn International School

Oludeniz, Turkey - October 2014

The Optical Microscope

Dual character of electrons

Ch. . Lioutas AISMAT 2014, HRTEM

Ch. . Lioutas AISMAT 2014, HRTEM

Final Result on the observed image

Ch. . Lioutas AISMAT 2014, HRTEM

V (r) exp[i 2 K r]d

Ch. . Lioutas AISMAT 2014, HRTEM

The electron Microscope

Final image (x 1.5M)

Ch. . Lioutas AISMAT 2014, HRTEM

V (r) exp[i 2 K r]d

According to J.B. Fourier:

For crystals V(r) is a periodic function in three dimensions

the Fourier Transform of the function

Ch. . Lioutas AISMAT 2014, HRTEM

The electron Microscope

final image depends on

Higher order diffracted beams contain

Ch. . Lioutas AISMAT 2014, HRTEM

The electron Microscope

Imaging Theory & Diffraction

Ernst Abbes Imaging Theory, 1872

Ch. . Lioutas AISMAT 2014, HRTEM

Imaging Theory & Diffraction

Ernst Abbes Imaging Theory, 1872

Mathematical analysis of the

Higher order diffracted beams contain

Periodic objects diffraction image consists of sharp spots

The back focal plane acts as a set of Huyghens sources

Image formation represents the

The intensity of the observed

Ch. . Lioutas AISMAT 2014, HRTEM

The spatial frequencies

Ch. . Lioutas AISMAT 2014, HRTEM

image formation only

image formation only

image formation from the

Ch. . Lioutas AISMAT 2014, HRTEM

Electrons versus Light

Magnification of an optic instrument is related with to the resolution limit.

Ch. . Lioutas AISMAT 2014, HRTEM

(Rayleigh 19th century )

Phase Contrast Microscopy

A lot of objects change the phase rather than

(x) the phase change at the point x

The ideal Microscope produces an image

The intensity distribution on the image plane

Ch. . Lioutas AISMAT 2014, HRTEM

Ch. . Lioutas AISMAT 2014, HRTEM

Phase Contrast Microscopy

In the case of a Weak Phase Object (WPO)

The intensity on the image plane

CONTRAST is the difference in intensity (I)

Ch. . Lioutas AISMAT 2014, HRTEM

Phase Contrast Microscopy

(in the optical microscope by inserting a glass plate )

The intensity on the image plane