0 Voturi pozitive0 Voturi negative

1 (de) vizualizări9 paginiLioutas2

Nov 05, 2016

© © All Rights Reserved

PDF, TXT sau citiți online pe Scribd

Lioutas2

© All Rights Reserved

1 (de) vizualizări

Lioutas2

© All Rights Reserved

Sunteți pe pagina 1din 9

a

t

u

Ch. B. Lioutas

Microscopy (HRTEM)

o

i

L

.

s

a

t

u

o

on growth and structural characterization

of advanced materials

B

.

h

C

Geometrical optics

ELECTRON-OPTICS

Description completely analogous to the light rays

.

h

.

B

4

1

0

2

THE MICROSCOPE

Imaging & Diffraction

i

L

(linear

(linear optics)

optics)

Projector

Diffraction

s

a

t

u

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

o

i

L

.

B

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

a

t

u

(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

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

.

h

C

Electrons

Electrons source

Condensor

specimen

Objective

.

h

Objective aperture

1st intermediate image

Intermediate

2nd intermediate image

Projector

Screen

2 mo e

h2

4

1

0

2

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)

s

a

t

u

o

A(K) are Fourier components spatial frequencies corresponding to diffracted

beams

i

L

(working

(working modes)

modes)

.

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

i

L

.

that describes the imaging object

Electron

Electron diffraction

diffraction

SAD

selective area

diffraction

condensor

aperture

Back focal plane

Selective

area

aperture

Final

diffraction

image

s

a

t

u

Imaging modes

the number of the

diffracted beams used

for image formation

Insertion of aperture on

the back focal plane of

the objective lens

o

i

L

.

B

diffraction image

(imaging

(imaging modes)

modes)

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

II

4

1

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

.

Fraunhofer diffraction proves

that the diffraction image

represents the Fourier

Transform of the objects

transparence function

o

i

L

.

information details of the object

n-th order beam corresponds to a grading with

period d/n beams.

h

C

s

a

t

u

(imaging

(imaging modes)

modes)

.

B

Continuous object gives rise to continuous diffraction pattern

II

II

i

L

second step

The final image is produced from the interference of the diffracted beams on the

back focal plane of the eyepiece lens.

.

h

inverse Fourier Transform of

the diffraction image

(x,y)= F -1[Q(u,v)]

image is

Iuv ~ |(x,y)|2

s

a

t

u

o

Q(u,v)=F [q(x,y)]

correspond to the diffracted

beams with intensities

Fuv = |Q(u,v)|2

0

2

Imaging in TEM

s

a

t

u

Bright

Bright Field

Field (BF)

from the undiffracted

beam

o

i

L

.

B

11

10

(imaging

(imaging modes)

modes)

Dark

Dark Field

Field (DF)

High

High Resolution

Resolution (HRTEM)

from one of the

diffracteed beams

undiffracted as well from a

number of diffracted beams.

12

s

a

t

u

4

1

The minimum distance to distinguish two points of the observed object

= 0.61/

wavelength,

an instruments parameter ~1

Optical microscope

~ 492nm

o

i

300 nm

Electron microscope

=100keV

=0.0037nm

L

.

2.3 10-3 nm

B

.

h

C

lenses aberrations

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

.

h

q(x)=exp[i(x)]

performing two Fourier Transforms

|q(x)|2=|exp[i(x)]|2=1

There is NO CONTRAST

.

B

q(x)=exp[i(x)]

Q(u)=F [q(x)]

(x)=F 1[Q(u)]

(x)= exp[i(x)]

s

a

t

u

o

0.1 nm

13

i

L

0

2

PHASE

MICROSCOPY

14

s

a

t

u

(x) << 1

o

i

L

.

B

|(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

between two adjacent areas C=I / Io

15

16

s

a

t

u

In the case of a Weak Phase Object (WPO)

(x) << 1

Q1(u)=

(x)+ iF [(x)]ei/2=

(x) - F [(x)]

L

.

(x) << 1, (x)2 ~ 0

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

B

.

h

C

.

B

17

i

L

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)=

along electron beam, direction Oz

V(x,y,z)dz = (x,y)

.

h

two dimensional transparency function

We can take account of electrons absorption

by including a function (x,y)

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

= /

18

s

a

Electron

Electron Microscope

Microscope -- Optical

Optical System

System

t

u

Imaging

It can be represented with a function H(u) including three factors

(in reciprocal space)

u=sin()/ /

( the diffraction angle)

o

i

L

.

B

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 )

without any difference

1/ 2

2 (E +V)1/2 = 2 + V

1

1

1

dz

E1/2

E

s

a

t

u

o

dx(z) =

(x)~1 - (x)

PERFECT REPRESENTATION of the objects

phase

0

2

1 1

2

dx( z ) = 2 dz = 1 dz

o

i

(x)+ iF [(x)]

in diffracted beams only

4

1

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 envelope function E(u)

The aberration function 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:

19

Ch. . Lioutas AISMAT 2014, HRTEM

20

s

a

t

u

The

The Electron

Electron Microscope

Microscope as

as phase

phase contrast

contrast microscope

microscope

transparency function proportional to the

projection of the structures potential

is a function of the diffraction angle mainly affected by:

Spherical

aberration

() = 2 Cs +

(x,y)=

o

i

electrons wavelength

Accelerating voltage

given instruments manufacturer

q(x,y)=exp[i

(x,y)]

z

Defocus

Cs

s

a

t

u

o

h

C

.

B

the minimum distance between to points of the object

in order to be resolved in the image plane

.

h

electron diffraction

diffracting object (crystal)

the instruments parameters

i

L

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)]

exact representation of the objects phase

proportional to the projection of specimens

potential

Direct illustration of structural characteristics

of the specimen

21

|(x,y)|2=[1-(x,y)]2 ~1-2(x,y)

B

.

Q(u)=F [q(x)]=

F [1+ i(x)]=

defocus value

selected during observation

L

.

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

(x)~1 - (x)

22

s

a

t

u

III

IMAGE SIMULATION

& PROCESSING

o

i

L

.

B

23

4

1

q(x)=exp[i(x)]

~ 1+ i(x)

0

2

V(x,y)dz= (x,y)

() takes the value of /2 or equivalent sin[()] = -1

for a large range of values

High

High Resolution

Resolution Electron

Electron Microscopy

Microscopy

24

Structural Analysis

s

a

t

u

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 ?

B

.

h

C

L

.

Specimen Thickness & Defocus Values

.

h

series of Thickness &

Defocus Values

conditions by comparison

with experimental images

0

2

Cerius2

by Accerlys

Runs on UNIX

s

a

t

u

o

EMS & jEMS

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

i

L

Thickness

Thickness -- Defocus

Defocus Matrix

Matrix

.

B

4

1

reproducing

Interaction Electron Beam - specimen (Diffraction)

Diffraction)

Interaction Electron Beam Lenses , Apertures (Imaging)

Imaging)

COMPUTER CALCULATION

o

i

Experimental requirements

Very thin specimen

Defocus close to that of Scherzer value

Appropriate projection

interpretation

interpretation of

of HRTEM

HRTEM micrographs

micrographs

s

a

t

u

Computer

Image Processing

o

i

L

.

B

REAL image

from the microscope

Digitized Image

Processed Image

27

26

data than we can obtain by eye

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

.

28

s

a

t

u

HRTEM examples

4

1

IV

EXAMPLES

& CASE STYDIES

B

.

h

C

HRTEM micrograph

dislocation in SiGe

.

h

o

i

L

.

HRTEM examples

projection of the

crystal structure

29

s

a

t

u

o

.

B

10

10

i

L

II

HRTEM

HRTEM image

image simultion

simultion

intense dots Si complex

less intense dots Fe-I

very weak dots Fe-II

HRTEM examples

30

s

a

t

u

stacking faults in CdTe

o

i

L

.

B

6

0

2

II

II

31

32

s

a

t

u

HRTEM examples

V

V

Grain boundaries

B

.

h

C

o

i

L

.

.

B

.

h

s

a

t

u

o

33

i

L

Microscopy (HRTEM)

V

V

4

1

Polycrystalline Si

in amorphous SiO2 matrix

Ch. B. Lioutas

HRTEM examples

34

s

a

t

u

o

i

L

.

B

on growth and structural characterization

of advanced materials

0

2

## Mult mai mult decât documente.

Descoperiți tot ce are Scribd de oferit, inclusiv cărți și cărți audio de la editori majori.

Anulați oricând.