Transmission electron microscopy (A textbook for materials science)

David B. Williams and C. Barry Carter

Practical electron microscopy in materials science

J. W. Edington

Electron microscopy of thin crystals

P. B. Hirsch and A. Howie, R. B. Nicholson, D. W. Pashley, and M. J. Whelan

Transmission electron microscopy: Physics of image formation and microanalysis

L. Reimer

Transmission electron microscopy of metals

G. Thomas and M. J. Goringe

Bright field image

Dark field image

High-resolution TEM image

(a)


(source)

(aperture)

(high voltage)

(anode)

(double lens)

(condenser lens)

(specimen)

(objective lens)

(aperture)

(aperture)

(intermediate
electron lens)

(projector lens)

(light optical system)

(final image)

(electron optical system)

q'

(electron source)

(focal plane of
condenser lens)

(condenser lens)

(object)

(objective lens)

(diffraction plane)

f(x)

f(k)

f(x')

(Bight field image)

(Dark field image)
(High-resolution TEM image)

k0

2-

2-

2B
k'

g*

000

hkl

000

hkl

k'

k0

(objective aperture)

(object)

(lens) (back focal plane)

(image plane)

k'
k0



2B

2B
k
k'

g*

000

hkl

000

hkl

k'
k

k0

(x, y)

(kx, ky)

(kx, ky)T (kx, ky)

T(kx, ky) :

m (x, y)



x- (EDS, WDS)

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

(Bragg diffracted electron)
(TEM, STEM)

(TEM, STEM)
SEM

(secondary electron)

(backscattered electron)

(cathodoluminescence, CL)

(REM)

(EELS)

(kV)

(pm)

0.1

120

1.0

39

10

12

102

3.7

2102

2.51

3102

1.97

4 102

1.64

5 102

1.42

6 102

1.26

8 102

1.03

103

0.87

h
2me eV0

eV0

1 +
2
2me c

1 / 2

1.226
6

Vo (1.09788 10 Vo )

nm

Three principal sources operating at 100 kV

Work function
Richardsons constant
Operating temperature
Current density
Crossover size
Brightness
Energy spread
Emission current
stability
Vacuum
Lifetime

units

Tungsten

LaB6

Field
Emission

eV
A/m2K2
K
A/m2
m
A/m2/sr
eV
%hr

4.5
6 105
2700
5 104
50
109
3
<1

2.4
4 105
1700
106
10
5 1010
1.5
<1

4.5

Pa
hr

10-2
100

10-4
500

10-8
>1000

300
1010
<0.01
1013
0.3
5

 3.72 pm 100kV
k 5nm-1 ?
(3.7 10 3 nm)(5 nm 1 )
sin =
10 2
2
2

= 10 2 rad

= 2 10 2 rad = 1o

x-

elatom
4
=
10
x
atom

= 2d sin B


(lattice) + (basis or motif)


r
r
r
r
, rn = ua + b + wc
r r r
a , b , c :
,

r r
r r
r*
b c
b c
a = r r r =

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

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

c (a b )

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

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

r* r r* r
b c = b a = 0
r* r r* r
c a = c b = 0

r
r
r
r,b r* c a ,
r * a b
c
(orthorhombic) , (tetragonal) , (cubic)

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

If abc,

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 | cos

r r r r
a * a =| a * || a |cos 1 = 1
r
1
|a * | = r
| a |cos 1

r*
1
r
|b | =
|b |cos 2
r*
1
|c | = r
|c |cos 3
r
r
| a * |= 1 / | a |,
r*
r
| b |= 1 / | b |,
r
r
| c * |= 1 / | c |


r* r*
r*
v*
g hkl = ha + kb + lc h, k , l
r
r
r
c
a
b OC =
OA =
OB =
l
h
k

v *
g hkl

r r
v*
v * b a
g hkl AB = g hkl

k h

r r
r
r*
r * b a
*
= (ha + kb + lc )

=0
k h

v*
g hkl
BC = 0
v * (hkl)
g hkl

d hkl =| OA|cos

r*
g hkl
cos =
r*
| OA| | g hkl |
OA

d hkl

r*
g hkl
= OA r *
| g hkl |
r* r*
r r*
a ha + kb + lc
=
r*
h
| g hkl
|
1
= r*
| g hkl |

r*
1
| ghkl
|=
d hkl

r*
g (hkl) (lattice plane)
(interplanar spacing)

r* r*
r*
v
*
123 g hkl = 1a + 2b + 3c

hkl
(indexing)


3
(
)

r
k = k 'k
r r*
k = g

| k | = 2k 'sin
2
r

1
| k | = 2 sin
2

r
1
| k | = 2 sin B

r*
1
| g |=
d hkl

r r*
k = g
1
1
2 sin B =

d hkl
Bragg

2d hkl sin B =


- :
- :

, ,

(hkl)

=2B k '

a=0.1~0.5 nm
a*=2~10 nm-1
X-
=0.1 nm
r=1/0.1 nm=10nm-1

=10-3 nm
r=1/10-3 nm=1000nm-1



r
r
r r
F ( k ) = f j ( k ) exp( 2ik r j )
j

r
r
r
r
r j = ua + b + wc , ( u, , w < 1)

r r*
r* r*
r*
k = ghkl = ha + kb + lc

F=

exp{2i( hu + k + lw)}

0 0
.

hkl hkl

B = z = [001]

B:
z: hkl

B = z = [001]

B = z = [001]

B = z = [001]

NaCl
NaCl (lattice) (fcc) (basis) 000
Na 1/2 1/2 1/2 Cl (space group)
Fm3m (unit cell) 4 NaCl
F=

exp{2i( hu + k + lw)}

= f Na [1 + exp{i( h + k )} + exp{i( h + l )} + exp{i( k + l )}]

+ f Cl [exp{i( h + k + l )} + exp( il ) + exp( ik ) + exp( ih )]
= f Na [1 + exp{i( h + k )} + exp{i( h + l )} + exp{i( k + l )}]
+ f Cl exp{i( h + k + l )}[1 + exp{i( h + k )} + exp{i( h + l )} + exp{i( k + l )}
= f Na [1 + exp{i( h + k )} + exp{i( h + l )} + exp{i( k + l )}]
+ f Cl exp{i( h + k + l )}[1 + exp{i( h + k )} + exp{i( h + l )} + exp{i( k + l )}]
F = [ f Na + f Cl exp{i( h + k + l )}]
[1 + exp{i( h + k )} + exp{i( h + l )} + exp{i( k + l )}]

F = [ f Na + f Cl exp{i( h + k + l )}] 0
=0
I = F2 = 0

hkl
(h + k + l) = ()

F = 4( f Na + f Cl )
I = F 2 = 16( f Na + f Cl ) 2

(h + k + l) = ()

F = ( f Na f Cl ) 4
= 4( f Na f Cl )

I = F 2 = 16( f Na f Cl ) 2

KCl
K+ Cl-
K 19, Cl 17
. K+ = Cl

f Kx+ f Clx
h, k, l F = 4( f Kx+ f Clx ) = 0
111, 311 x-

(atomic scattering amplitude)

[GaAs/AlGaAs ]

[ReSi2/Si(001) ]

(deviation parameter)

:
:

(a)

r r* r
k = g + s

(b)

Si (plasma enhanced chemical vapor

deposition) Ta2O5

304 M23C6


L/k = L :

r = L tan L sin 2 B L2 B

= 2d sin B

k' = 1/

k = 1/

2d B

rd = L
r*
1
r = L =| g | L
d

g*

hkl

000

hkl

B
___
hkl
1

hkl
2

hkl =hkl +hkl

C
3

b
000
O

hkl
1

___
hkl
2

1. r1, r2,
L .
hkl
hkl
hkl .
557/771 300/221 hkl
d .

2. ,
h,k,l
,

h1, k1, l1
*

g h1k1l1 = h1 a + k1 b + l1 c

h2, k2, l2
*

g h 2 k 2l 2 = h2 a + k 2 b + l2 c
*

g h1k1l1 g h 2 k 2l 2 = g h1k1l1 g h 2 k 2l 2 cos

*

cos =

g h1k1l1 g h 2 k 2l 2
*

g h1k1l1 g h 2 k 2l 2

:
*

(h1 a + k1 b + l1 c ) (h2 a + k 2 b + l2 c )
*

g h1k1l1 g h 2 k 2l 2

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

a b c,
*

a b c

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

h2 + k 2 + l 2
1
g = =
d
a
*

cos =

h1 h2 + k1k 2 + l1l2
h12 + k12 + l12 h22 + k 22 + l22

h,k,l

 .
r* r* r*
g3 = g1 + g2

h3 = h1 + h2, k3 = k1 + k2, l3 = l1 + l2

h3 = mh1 + nh2
k 3 = mk1 + nk 2
l3 = ml1 + nl2

m n
h1k1l1, h2k2l2
(beam) B = [uuw]

u = k1l2 k 2 l1
= l1 h2 l2 h1
w = h1 k 2 h2 k1

 hkl

hu + k + lw = 0
[uuw] (hkl) (zone axis)

r
r
r
r2 | g 2* | d1
r3 | g 3* | d1
r4 | g 4* | d1
,L
,
,
= r =
= r =
= r =
r1 | g1* | d 2
r1 | g1* | d 3
r1 | g1* | d 4

hkl dhkl .
hkl .
h,k,l
.

45o
SC

45o
rC

rB

010

011

000

100

Z=B=[001]

rA

rB
=1
rA
rC
= 1.414
rA

FCC

020

022

000

200

Z=B=[001]

45o
BCC

45o
rB

rC

rA

rB
=1
rA
rC
= 1.414
rA

020

022

000

200

Z=B=[001]

 Ratio of interplanar spacings

111

200

220

311

331

420

422

511

531

111

200

1.155

220

1.63

1.41

311

1.92

1.66

1.17

222

2.00

1.73

1.225

1.045

400

2.31

2.00

1.415

1.21

331

2.52

2.18

1.54

1.31

420

2.58

2.235

1.58

1.35

1.027

422

2.85

2.45

1.73

1.48

1.124

1.096

333,511

3.00

2.60

1.84

1.57

1.19

1.16

1.06

440

3.27

2.83

2.00

1.71

1.30

1.217

1.156

1.09

531

3.42

2.96

2.09

1.785

1.36

1.32

1.21

1.14

442

3.46

3.00

2.12

1.81

1.38

1.34

1.225

1.157

1.014

620

3.66

3.16

2.24

1.91

1.45

1.42

1.29

1.22

1.07

k'

(Ew

(
000

100

(rings from double diffraction)

000
0

24

32

12

in
(R

gsfro

do
m

ledbu

ifrac

ion)t

400
222
311
220
200
111

(Rings from double diffraction)

[001]

001 a
101

011 b

021

111

121

000
O

211

c
110

100

020

010
120
g

(reciprocal lattice circ

(a)

[001]
,
[001]
306o

{001}
{011}
{020}
{021}
{110}
{111}
{120}
{121}

(b)

b d

c e


(second phase), (twin), (martensite),
(double diffraction), (ordering)
(twin)


(HKL) [UVW]
180 (twin) (matrix)
(h1k1l1) (h2k2l2)

Uh1 + Vk1 + Wl1

h2 = h1 2 H
HU + KV + LW
, k2 l2

(cubic)

h2 = h1 2 H

Hh1 + Kk1 + Ll1

H 2 + K 2 + L2

k2 l2 .

(fcc) (twin) (111)

h1 + k1 + l1
h2 = h1 2
3
h1k1l1 = 333 h2k2l2 = .
(twin spot)
, <111> 1/3

 111, 200, -244 (111)

1
1
1 11 ( 511) T = 200 + (111),
3
3
1
1
200 ( 244 ) T = 1 1 1 (111),
3
3
244 ( 600 ) T

(hkl)T hkl .
(twin spot)

hkl:
[pqr]: (pqr)
hkl [pqr] 180o
hkl
pqr

[hkl ] + [h' k ' l ' ] = n[ pqr ]

(hkl)

(hkl)

h + h' = np
k + k ' = nq
l + l ' = nr

[hkl ] + [h' k ' l ' ] = n[ pqr ]

h + h' = np
k + k ' = nq
l + l ' = nr
a, b, c

h 2 k 2 l 2 h'2 k '2 l '2

+ 2+ 2 = 2 + 2 + 2
2
a
b
c
a
b
c
np h nq k nr l
=
+
+

a b c
ph qk rl
2 2 + 2 + 2
a
b
c

n=
2

h k l
2 + 2 + 2
a b c
2

 h, k, l
2
r2
ph 2qk 2rl q
p 2 + 2 + 2 h 2 + 2
c
b
c b
a
h' =
p2 q2 r 2
2 + 2 + 2
a b c
2
r2
2 ph qk 2rl p
q 2 + 2 + 2 k 2 + 2
c
b
c a
a
k'=
p2 q2 r 2
2 + 2 + 2
a b c
2
q2
2 ph 2qk rl p
r 2 + 2 + 2 l 2 + 2
b
b
c a
a
l' =
p2 q2 r 2
2 + 2 + 2
a b c

For cubic (a=b=c)

p( ph + 2qk + 2rl ) h(q 2 + r 2 )

h' =
p2 + q2 + r 2

(double diffraction)

B 1

1 D1

B 2

2
,

B 2

(a)

2 D3
D3 D1
1/d2

(c)

(b)

(d)

(e)

diamond: 002
hcp: 0001
(f)

(a)

(b)

(superlattice reflection)
.

(extra spot)
(unit cell) .

(superlattice reflection)
(dark-field image) ,
(superlattice)
(domain)
.

ah
g*
= 2
h + k 2 + l 2 g *

< 100 >

(a)

020

220

000

200
g*
g *
(b)

CdxZn1-xTe

ZnTe rich

CdTe rich