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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

Ch. . Lioutas AISMAT 2014, HRTEM

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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

Ch. . Lioutas AISMAT 2014, HRTEM

Electron diffraction

A( ) =

2 mo e
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(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

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Ch. . Lioutas AISMAT 2014, HRTEM

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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

Ch. . Lioutas AISMAT 2014, HRTEM

2 mo e
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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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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

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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

Ch. . Lioutas AISMAT 2014, HRTEM

The electron Microscope

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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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.

Ch. . Lioutas AISMAT 2014, HRTEM

The electron Microscope


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

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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.

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Ch. . Lioutas AISMAT 2014, HRTEM

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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(imaging
(imaging modes)
modes)

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Periodic objects diffraction image consists of sharp spots


Continuous object gives rise to continuous diffraction pattern

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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

Ch. . Lioutas AISMAT 2014, HRTEM

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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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Ch. . Lioutas AISMAT 2014, HRTEM

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.

Ch. . Lioutas AISMAT 2014, HRTEM

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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

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2.3 10-3 nm

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Ch. . Lioutas AISMAT 2014, HRTEM

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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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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

Ch. . Lioutas AISMAT 2014, HRTEM

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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

Ch. . Lioutas AISMAT 2014, HRTEM

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Phase Contrast 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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Ch. . Lioutas AISMAT 2014, HRTEM

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Phase Contrast Microscopy


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)]

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Ch. . Lioutas AISMAT 2014, HRTEM

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V << E (energy of the incident electrons)

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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)

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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

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(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

Ch. . Lioutas AISMAT 2014, HRTEM

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

Ch. . Lioutas AISMAT 2014, HRTEM

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
E

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dx(z) =

(x)~1 - (x)

The CONTRAST on the image plane is a


PERFECT REPRESENTATION of the objects
phase

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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

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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
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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


Ch. . Lioutas AISMAT 2014, HRTEM

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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)=

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electrons wavelength
Accelerating voltage

spherical aberration coefficient


given instruments manufacturer

q(x,y)=exp[i
(x,y)]
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Defocus

Cs

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The Resolving Power of the Microscope

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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

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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
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Ch. . Lioutas AISMAT 2014, HRTEM

(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

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Q(u)=F [q(x)]=
F [1+ i(x)]=

Induced by spherical aberration & defocus

defocus value
selected during observation

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(x)=F 1[Q1(u)]
(x)~1 - (x)

Ch. . Lioutas AISMAT 2014, HRTEM

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III
IMAGE SIMULATION
& PROCESSING

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q(x)=exp[i(x)]
~ 1+ i(x)

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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

Ch. . Lioutas AISMAT 2014, HRTEM

High
High Resolution
Resolution Electron
Electron Microscopy
Microscopy

Ch. . Lioutas AISMAT 2014, HRTEM

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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)

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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

Ch. . Lioutas AISMAT 2014, HRTEM

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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)

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Thickness
Thickness -- Defocus
Defocus Matrix
Matrix

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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

Ch. . Lioutas AISMAT 2014, HRTEM

HRTEM micrographs Simulation

interpretation
interpretation of
of HRTEM
HRTEM micrographs
micrographs

Ch. . Lioutas AISMAT 2014, HRTEM

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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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Ch. . Lioutas AISMAT 2014, HRTEM

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HRTEM examples

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FeSi2 along [012]

IV
EXAMPLES
& CASE STYDIES

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Ch. . Lioutas AISMAT 2014, HRTEM

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HRTEM micrograph
dislocation in SiGe

Burgers vector determination

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Ch. . Lioutas AISMAT 2014, HRTEM

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HRTEM examples

projection of the
crystal structure

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HRTEM
HRTEM image
image simultion
simultion
intense dots Si complex
less intense dots Fe-I
very weak dots Fe-II

Ch. . Lioutas AISMAT 2014, HRTEM

HRTEM examples

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HRTEM images from


stacking faults in CdTe

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Ch. . Lioutas AISMAT 2014, HRTEM

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HRTEM examples

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Grain boundaries

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Ch. . Lioutas AISMAT 2014, HRTEM

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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

Ch. . Lioutas AISMAT 2014, HRTEM

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Autumn International School


on growth and structural characterization
of advanced materials

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