1/71

May12, 2011 KRISS

Incident Electron
Matter
Transmitted Electron
Eye

(Young Heon KIM)

young.h.kim@kriss.re.kr
T. 042-868-5449, 010-9389-1606

2/71

I. ?
II. ?
(1) , ,

III. ?
(1)
(2)

IV. ?
(1)
(2)

3/71

I. ?

1. ?
-> (1)
(2)

2. ?
-> (1)
(2)

3. ?

4/71

: ?

5/71

6/71

Satellite camera

http://www.peakoil.net/images/PetitPrince.jpg

My Office

?
http://earty.google.com

7/71

8/71

9/71

(1) ?

II. ?

[]
1 . .
2 <> . .

[]
<> .
9.109010-31 kg, 0.511 MeV. .
19 , .
e.

[]
<> . , ,
, () , () , ,
.

[]
1 <> ,
. . .
:
2 <>=.

10/71

(S)TEM

http://nobelprize.org/educational_games/physics/microscopes/1.html
http://nobelprize.org/educational_games/physics/microscopes/tem/tem.html

11/71

TEM

Philips CM30

JEOL 3010

Hitachi H9000

(filament)

: thermionic guns,
: 100 kV, 200 kV (low voltage TEM),
300 kV, 400 kV (medium voltage TEM), field emission guns
> 1 MV (high voltage TEM)

: medical TEM,
bio TEM,
materials TEM

12/71

- ()
-

13/71

http://nobelprize.org/educational_games/physics/microscopes/1.html

,
.
Hardware advances in imaging microscopes
H. Rose. In Advances in Imaging and Electron Physics Vol. 153 (ed. P. Hawkes) (Elsevier, 2009)

14/71

History of visible light microscopy (VLM)

(~):
13 :
(Roger Bacon, 1214-1294):
(Conrad Gesner, 1516-1565):
17:
1590 (Hans Janssen, Zacharis Janssen) :
- (10-30):
1609 -> .
- :
=>
.
: (Robert Hooke, 1635-1703)
-> 1665 (Micrographia)
=>
. ( )
(Nehemiah Grew, 1641-1712) , , ,

(Marcellko Malpighi 1628-1694), (Jan Swammerdam, 1637-1680),
(Antony van Leeuwenhoek, 1632-1723)
1830 ( )
- (Giovanni Battista Amici: 1786-1863),
1827 (achromatic system) .
- (Ernest Abbe, 1840-1905):
(Abbe sine )
1878 (Zeiss)
1886 -
20 (Khler) :

15/71

History of electron microscopy

1855
1897
1900
1912
1913
1914
1926
1927

Geisler
Tompson
Quantum theory by Max plank
Laue P. Ewald -> X-ray diffraction theory
Bragg Diffraction Condition
kinematical diffraction theory (Darwin)
Schrdinger
Davisson and Germer interference
electron diffraction pattern
1928 Bethe Dynamical diffraction theory
1933 Ruska -> first EM
1939 first commercial EM (100 )
1947 RCA, Simens, AEI, Hitachi, JEOL, Phillips
1955-57 Cambridge Univ. Cavendish Lab.
-> Dislocation and defects imaging based on
Diffraction Contrast (Kinematical theory)
1961 100 kV TEM
1962 1,000 kV TEM (1MV) -> France (Dynamical theory )
1966-70 1 MV (Japan), 3MV (France)
1983 300-400 kV -> 1.8
1986 Nobel Prize (Ruska, 1906-1988)
1995 3MV (Japan) -> 0.88
First Electron Microscope with Resolving Power
2009 ~50 pm ()
Higher than that of a Light Microscope
Ernst Ruska, Berlin 1933 Replica by Ernst Ruska,
1980
For the first time the apparatus had a condensor
in front of the specimen and two magnifying
lenses. Magnification around 12,000

16/71

= + + + + + .

C
A

, (threading dislocation),

InSb

Si

,
Nb Mapping

Cu Mapping

17/71

(S)TEM
Image Analysis

Electron Diffraction

Chemical Analysis

a-Si
HfOx

~ 3 nm

SiO2

Si

GaSb

Twin I
Twin II

5.43 = aSi
by Young H KIM

CTEM image
Bright-field image
Dark-field image
HRTEM micrograph
(HA)ADF image
Energy-filtered TEM image

GaSb/Si

B=z=[110]

by Young H KIM

Selected Area Electron Diffraction

(SAED)
Kikuchi Patterns
Convergent Beam Electron Diffraction
(CBED)

Single Atom Spectroscopy

M. Varela et al, Physical Review Letters 92,
095502 (2004)

Energy-Dispersive X-ray Spectroscopy

(EDS)
Electron Energy Loss Spectroscopy
(EELS)

18/71

Size of an atom

: 20 ~ 300 pm

III. ?

http://en.wikipedia.org/wiki/Atomic_size

Resolution of Transmission Electron Microscope

Wavelengths of the electrons in TEMs
Voltage (kV)

Relativistic
Wavelength (pm)

0.1

120

1.0

39

100

3.7

200

2.51

300

1.97

400

1.64

1000

0.87

l= 1.226/[E(1+0.978810-6E]1/2 nm
(E: accelerating voltage (V))

(dr)Scherzer Cs1/4l3/4
Cs: Spherical Aberration
l: Wavelength

19/71

Interactions of Electrons and Material (Specimen)

x- (EDS, WDS)

(electron-beam-induced current, EBIC)
(AES)

(Bragg diffracted electron)
(TEM, STEM)

(TEM, STEM)

(EELS)

SEM (secondary electron)

(backscattered electron)

(cathodoluminescence, CL)

(REM)

.
Edited by young h kim
(, , (2002))

20/71

(S)TEM

Source

Condenser Lens

Specimen

Objective Lens

Objective Aperture

Selected Area Aperture

Intermediate Lens

Projector Lens

Optical Microscope

Transmission Electron Microscope

Edited by young h kim

(, , (2002), , , (1996) )

21/71

Fundamental Properties of Electrons

de Brogiles ideas of the wave-particle duality
: particle momentum p, wavelength , Plancks constant h

(non-relativistic electron wavelength)

(relativistic electron wavelength)

22/71

Electron Sources
1. Thermionic source

2. Field emission source

- Anode 1 provides the
extraction voltage to
pull electrons out of
the tip.
- Anode 2 accelerates
the electrons to 100 kV
or more (appropriate
voltage).

23/71

Lenses
Roles

-
. ( )
- .
-
.
-
. ( )

24/71

Apertures
-

e
(electron wave)

k'
k

k0

(imginary aperture)

(objective aperture)

(lens)

(back focal plane)

(image plane)

.

.

.


.

.


.

25/71

Spherical aberration
:

q
q

(object)

M dr

(objective lens)

(disc of confusion)

(Gaussian image plane)

.

(disc of confusion) .
q

dr = C sq 3
Cs (spherical aberration coefficient)
mm

26/71

Chromatic aberration

Depth of focus and depth of

field

27/71

Depth of focus & depth of image

S

T
q
q' = M

dr = T q

M dr

A B C

A'

B'

(specimen)

(objective lens)

(image plane)

C'

OM vs SEM

dr
2

T=

T
tanq
2
dr

Depth of focus

Mdr S
S
= tan q = q
2
2
2
Mdr M 2 dr
S=
=

q
q
Depth of image
Screw length: ~ 0.6 cm
Images: the A to Z of Materials

28/71

Illumination system: gun + condenser lenses

29/71

Imaging system: 1. TEM

30/71

Imaging system: 1. TEM Bright and Dark field image

<DF>

<BF>
-

k0

k'

e
k

k0

k
q

(objective aperture)

(object)

(lens)

(back focal plane)

(image plane)

31/71

Imaging system: 2. STEM

32/71

Imaging system: 2. STEM BF and DF

33/71

Spectrometry:
Energy Dispersive X-ray Spectroscopy Analysis

(32)

Quantized energy of an electron in a

4
2
3/2

2
M

(18)

5/2
3/2

3
1

1/2
0

1/2

1
L

(8)
Lb

Lg

D l =+- 1
Dj=0

K
Kb

Ka

Kb
Kb

1/2

+- 1

(2)

1/2

For m=2, n=1

2 2 - 12
3
3
2
DU = U 1
=
U
=
13
.
6
Z

eV
1
22
4
4

Kb

Transition energy from m-level to n-level

m2 - n2
Z 2 m2 - n2
DU = U m - U n = U n
= - 13.6 2
eV
m2
n m2

''

3/2
1/2

La

'

Ka

hydrogenic atom
13.6
U n = - 2 Z 2 eV
n

< >

Edited by young h kim

(, , (2002))

34/71

Spectrometry:
Energy Dispersive X-ray Spectroscopy Analysis

Types of X-rays
- Characteristic x-rays
elemental identification
quantitative analysis

- Continuum x-rays
background radiation
must be subtracted for
quantitative analysis

Example of EDS x-ray spectrum

from Goldstein et al., Scanning Electron Microscopy and X-ray

Microanalysis, Springer, 2003.

35/71

Generation of Characteristic X-rays

Mechanism

Fast beam electron has enough energy

to excite all atoms in periodic table
Ionization of electron from the K-, L-,
or M-shell
X-ray is a product of de-excitation

Example

Vacancy in K-shell
Vacancy filled from L-shell
Emission of a Ka x-ray
(or a KLL Auger electron)

Important uses
Qualitative use x-ray energy to
identify elements
Quantitative use integrated peak
intensity to determine amounts of
elements

36/71

Spectrometry:
Energy Dispersive X-ray Spectroscopy Analysis

37/71

Spectrometry:
Electron Energy Loss Spectroscopy Analysis
-

r=

(screen) (aperture)

m eu
eH

(uniform field
sector magnet)

100

U0 - DU

U0

(electron loss spectrum)

Edited by young h kim

(, , (2002))

38/71

The energy of a transmitted or elastically scattered

electrons, even diffracted ones, remains relatively
unchanged. The energy of an inelastically
scattered electron is always less than that of the
primary electron.

Every primary electron has one

of three possibilities in terms of
its interactions with atoms of the
specimen.

From website

For most of the

electrons, the change in
energy is not random
but is directly related to
which electron, from
which atom, from which
orbital shell the
inelastic collision took
place.

39/71

Spectrometry:
Energy filters

40/71

Basic Principles for Diffraction

and Imaging

Edited by young h kim

(, , (2002))

41/71

S
R

< >

y
M

Y
O

O'
A

B
H

X
Q

<>

(lattice)+ (basis or motif)

=

< ( )>
: +
: +

(lattice)
:
(structure factor)
Edited by young h kim
(, , (2001))

< >

(periodic atom array)

r r r
a, b , c :
r r
r r
b c
b c
r
a* = r r r =
V
a (b c )
r
r
r
r
r*
ca
ca
b = r r r =
V
b (c a )
r r
r r
a b
a b
r*
c =r r r =
V
c (a b )

42/71

< >

r r
r
r
b c
r
a* b = r r r b = 0
a (b c )
r
r
r r r r r r r r r r
a* b = a* c = b * a = b * c = c * a = c * b = 0
If

r r r r r r
a ^ b ^ c, a * // a , b * // b , c * // c

< >

r r
r* r
r
b c
a a = r r r a =1
a (b c )
r* r r* r
b b = c c = 1
r r r r
a * a =| a * || a | cosq

If a^b^c,

r
r
| a * |= 1 / | a |,
r
r
| b * |= 1 / | b |,
r
r
| c * |= 1 / | c |

Edited by young h kim

(, , (2001))

43/71

< >
(3 Ewald >

r
q
| Dk |= 2k sin
2
r
1
q
| Dk | = 2 sin
l
2
q=2qB

r
1
| Dk | = 2 sin q B

|k'|=1/l

sin q B =

(Ewald sphere)

g*

(reciprocal lattice points)
qB

(hkl)

Dk = g*

qB qB

|k'| =
F G
qB

qB

qB
O
qB qB

|k| =

1
l

1
l

d
B

l = 2d hkl sin q B
Edited by young h kim
(, , (2002))

1
d hkl

l = 2d hkl sin q B

|k|=1/l
=
Dk

r
1
| g *|=
d hkl

|Dk| = |g*| =

44/71
S
R
y
M

Y
O

O'
A

B
H

X
Q

F
(Structure Factor)

r
r
~
F (Dk ) = m(Dk )

(lattice translation) r

r
m( r ) =

r
r
r
r
rn = ua + ub + wc

r
D(r ) =

~ r
D(Dk ) =

r r
f j * d (r - r j )

r
F (Dk ) =

r r

r
r r
f j (Dk ) exp(-2piDk rj )

f j (Dk ) exp(-2piDk r j )
j

r
f j ( Dk )
~

exp( -2piDk r ) = u exp{-2piDk (ua + ub + wc )}

n

u w

r r
exp( -2piuDk a )

r r
exp(
2
p
i
D
k
rn ) @

r
r
= D ( r ) * m( r )

m
j

r
r
~ (Dk ) =
F (Dk ) = m

r r
exp(-2piDk rn )

, 1, 2, 3, ..., j, ... r

r r
d (r - rn )

f crystal

r r

r r
exp( -2piuDk b )

r r
exp( -2piwDk c )

1
1
r r
r r
r r
1 - exp( -2piDk a ) 1 - exp( -2piDk b ) 1 - exp( -2piDk c )

r
~ r ~ r
y (Dk ) = D(Dk )m(Dk )

r
f j ( Dk )

r
r ~ r
y (Dk ) = F (Dk ) D(Dk )
r
r r ~ r
= f j (Dk ) exp(-2piDk r j ) D(Dk )
j
r r
r k
r h
r l
n exp(-2piDk rn ) = h d Dk - ar k d Dk - br l d Dk - cr
r
r
r
r r
r
= d (Dk - ha * ) d (Dk - kb * ) d (Dk - lc * )
h
k
l
r
r* r*
r*
= d (Dk - ha - kb - lc )
h , k ,l

r r
= d (Dk - g * )
h , k ,l

45/71

TEM
:

(1) (amplitude contrast)

- (diffraction contrast)
: BF, DF, WBDF images
- (absorption contrast)
: amorphous, topography

(2) (phase contrast)

: HRTEM

46/71
46/80

TEM : 1. (kinematical theory)

: .

(assumption) (limit)
1.
* ,

=> . (fg<<f0)
-> , Bragg
.
( )

2.
fg , .
s=0 ,
= p2t2/ (xg)2 .
*
I g ( x , y ) = y gy g

pt sin 2 (pst )
=
x (pst ) 2
g
1
= 2 2 sin 2 (pst )
s xg

t > xg/p , 1 1 ,
.

47/71
47/80

(kinematical theory)
yg =

k0

k0 k
(a)

k0 k'

k0

ip

xg

t
2 exp( 2pisz ) dz
t
2

ip sin(pst )
t
xg
pst

:
(kinematical integral)

I g ( x , y ) = y gy g*
2

k0 k'

k0 k k' k k' k'

(b)

pt sin 2 (pst )
=
x (pst ) 2
g
1
= 2 2 sin 2 (pst )
s xg

48/71
48/80

TEM : 2. (dynamical theory)

:
:
: Howie-Whelan equation

k0

dy 0 ip
r
r r
ip
= y 0 + y g exp{2pi ( g * + s ) rn }
dz
x0
xg

dy g
dz
k0 k
(a)

ip

xg

r r

y 0 exp{2pi( - g * - s ) rn } +

ip

x0

yg

k0 k'

dy 0 ip
ip
= y0 +
y g exp( 2pisz )
dz
x0
xg

k0

k0 k'

dy g
dz

k0 k k' k k' k'

(b)

ip

xg

y 0 exp( -2pisz ) +

ip

x0

yg

49/71
49/80

TEM : 3. (high-resolution image)

(weak-phase approximation: dz
.)

Df 2

I = yy = 1 +
b ( x , y )
4pk

Df 2
@ 1+
b (x , y )
2pk
*

Dfdz r ( x , y )
I @ 12V0
e

r
V (r )
b ( x, y ) = 2pk 0
dz
2V0

V0 , dz, Df ,

2 b ( x, y ) = 2pk 0

r(x, y)

r
r
2V ( r ) = e

r(x, y).

dz
2V0

2 b ( x, y ) = -2pk 0

r
2V (r )

dz r
2V0 e

-> .
, .
=> (high-resolution transmission electron microscopy, HRTEM)
.

: - .
1 nm .

50/71
50/80

dz -> 0 dz (proper differential) dz

t .

I = yy *
@ 1+

Df 2
b (x , y )
2pk

2pk 0 2 t
b ( x, y ) =
V ( x , y , z )dz
0
2V0
2

Df 2
I @ 1+
b (x , y )
2pk
Df 2 t
= 1+
V ( x , y , z )dz
0
2Vo

Si 100

(projected potential)

Si 110

51/71

TEM Working Process

1. Sample Preparation
2. TEM Observation
3. Data Analysis

Preparation Methods
Ion milling, Tripod polishing,
FIB, Ultramicrotomy, replica
...

Materials
Metals
Ceramics
Semiconductors
Powders, Fibers, ...
Nanomaterials

IV. ?

Analysis Methods
Image Analysis
Electron Diffraction
Chemical Analysis
in-situ Analysis
.

Data Analysis
Image Processing
Simulation
.

http://www.google.com/

52/71

(1) - Specimen requirements

TEM specimen must be ...
thin : less than ~ 1000
shape : 3 disk type
representative of, and unchanged, from bulk
flat, not rugged
amount of transparent area
stable in the electron beam
very clean : free from extraneous particles or debris
(possibly from specimen preparation)
conductive, non magnetic

TEM specimens with varying thicknesses will affect x-ray

quantitative analyses.

53/71

Specimen preparation

54/71

1. Cross-sectional TEM sample preparation

disc cutting

slicing

cutting & bonding

3
100

EPOXY

Ion milling

dimpling

polishing

50~60

50~60
< 5

100

55/71

2. TEM sample preparation of Powders:

(1) Dispersion Technique ()

Mesh Grid

Carbon Support Film

Mesh Grid

Carbon Support Film Mesh Grid with Holes

56/71

3. Focused Ion Beam (FIB) Technique a. Overview

Produce cross-section TEM specimens

of individual devices
(site-specific).
Can provide ion beams with lateral res
olution less than 10nm.
Provide a large area of uniform thickn
ess; Possible to detect the localized int
ernal stress around features
Good for materials that are not suitabl
e for mechanical grinding and polishin
g.
less preferential milling is observed , e
nabling the preparation of cross-sectio
n specimens from samples composed
of different materials

57/71

(2) -
i. InSb

Sample A
(a)

Sample B
(b)

RMS: 7.162E+00 nm

RMS: 4.237E+00 nm

Surface morphologies of samples A and B

58/71

- Plan-view image

Sample B

Sample A
(a)

(b)
Region B

Region A

Region C
500 nm

110

110

001

Y.H. KIM et al, Appl. Phys. Lett. 89 031919 (2006)

500 nm

110

001

110

59/71

- Cross-section image Sample A

Centered bright field image

Y.H. KIM et al, Appl. Phys. Lett. 89 031919 (2006)

Microtwin

InSb

AlSb GaSb
Si
004 2-beam bright field image

220 2-beam bright field image

60/71

- Cross-section image Sample B

Centered bright field image

Y.H. KIM et al, Appl. Phys. Lett. 89 031919 (2006)

InSb

AlSb GaSb
Si
004 2-beam bright field image

220 2-beam bright field image

61/71

- High-Resolution Transmission Electron Microscopy (HRTEM) image

Y.H. KIM et al, Appl. Phys. Lett. 89 031919 (2006)

B
Region I

001 plane

15.8

B = z = [110]

62/71

- Cross-section image & SAED

A

Microtwins

Y.H. KIM et al, Appl. Phys. Lett. 89 031919 (2006)

Dislocation

A
C
A

C
A

InSb

Si

63/71

(a)

(b)

(a)

3
2
(b)

Edited by young h kim

(, , (2002))

1, 2 : Epitaxial
3 : (twin)
4 :

64/71

000

400
222
311
220
200
111

(Rings from double diffraction)

O
(hkl)
qB

qB

hkl

000

Kikuchi pattern

Edited by young h kim

(, , (2002))

65/71

Spectrometry:
Energy Dispersive X-ray Spectroscopy Analysis

H. Ryu et al, Jpn. J. Appl. Phys. 48, 091405 (2009)

66/71

H. Ryu et al, Jpn. J. Appl. Phys. 48, 091405 (2009)

67/71

Spectrometry:
Electron Energy Loss Spectroscopy Analysis

68/71

- Energy-Filtered Transmission Electron Microscopy (EFTEM) image

www.gatan.com/answers/answer1.php

69/71

1.
2.
3.
4.

Theres Plenty of Room for TEM at the Bottom!!

69

70/71

1. , ( 115), , , (1998).
2. , , , , (2001).
3. , , , , (1999).
4. , , , , (2002).
5. , , , , , , (1996).
6. D.B. Williams and C.B. Carter, Transmission Electron Microscopy, Vol. I-IV, Plenum
Press, New York and London, (1996).
7. B. Fultz and J.M. Howe, Transmission Electron Microscopy and Diffractometry of

Materials, Springer, Berlin (2001).

71/71

Theres Plenty of Room for TEM at the Bottom!!

..

5 nm

100 nm

100 nm

-> ->