Electron Diffraction Analysis: Chapter (1

Electron diffraction analysis
Ch
The$probes:$phot
description
of+their+interactio
2 nm
Isocahedral AlFeCu modulated AlFeCu
FFT
2-fold zone axis 5-fold zone axis
1"1" The&useful&quantities&to&describe&th
1"1"1" Electromagnetic&waves
1"1"2" Neutrons
1"1"3" Electrons
1"2" Interaction&processes
1"2"1" Two&fundamental&interactions
1"2"2" Interaction&cross&section
1"2"3&" Different&mechanisms&of&scatte
1"2"4&– Examples&of&methods&based&on
1"3" The&specific&case&of&X"rays
1"3"1" X"ray&sources&
! hot&cathode&tube,&rotating
1"3"2" Classical&vs&&quantum&mechanica
1"3"3" Basic&concepts&of&X"ray&scatterin
! differential&cross&section,&T
1"3"4" Basic&concepts&of&X"ray&absorptio
! Beer"Lambert&law,&absorpt
(Pbx-La1–x)TiO3 (Pb(Zrx-Ti1–x)O3 (PZT)

[112] zone axis [001] zone axis
Institut de Minéralogie, de Physique des Matériaux et de Cosmochimie
dhkl measurements
Ch
The$probes:$phot
Example #1: single crystal diffraction
description
of+their+interactio
® h i
® k
k0
e f g M
c d
a b
® +
Ghkl 000
L : camera length
® ® 1"1" The&useful&quantities&to&describe&th
|k0| |Ghkl| 1"1"1" Electromagnetic&waves
= 1"1"2" Neutrons
L rhkl
1"1"3" Electrons
lL a: 2.70 Å e: 1.90 Å 1"3"3" Basic&concepts&of&X"ray&scatterin

dhkl =
rhkl b: 1.35 Å f: 1.65 Å ! Beer"Lambert&law,&absorpt
000 c: 3.10 Å g: 1.10 Å

rhkl d: 1.65 Å h: 1.25 Å
i: 1.05 Å

dhkl measurements
Ch
The$probes:$phot
description
of+their+interactio
0.485
+ 2 rhkl
0.295
0.255 1"1"1" Electromagnetic&waves
1"1"2" Neutrons
1"1"3" Electrons
0.240 1"2" Interaction&processes
0.210 1"2"2" Interaction&cross&section

0.170 1"3" The&specific&case&of&X"rays

0.160 ! hot&cathode&tube,&rotating
0.148 ! differential&cross&section,&T
0.142
0.133
dhkl (nm)

Iraw = f(r) with r in pixels Ch
The$probes:$phot
description
of+their+interactio
® Radial integration of
diffracted intensity
1"1"2" Neutrons
1"1"3" Electrons
Icorr = f(q) with q in Å–1 1"2"1" Two&fundamental&interactions
1. conversion r ® q 1"3"1" X"ray&sources&
q = r / (l·L) 1"3"2" Classical&vs&&quantum&mechanica

2. Background estimation: bkgd ®

bkgd = A·q–B

Background substraction Ch
The$probes:$phot
description
of+their+interactio
Peak indexation 1"1"1" Electromagnetic&waves
1"1"2" Neutrons
1"1"3" Electrons

Ch
Application
The$probes:$phot
description
of+their+interactio
1"1"2" Neutrons
1"1"3" Electrons
• coexistence of nano-rods
and very small particles
Ch
The$probes:$phot
description
of+their+interactio
nano-particules
NPs
1"1"2" Neutrons
1"1"3" Electrons
• ≈ same structure, i.e. 1"3"1" X"ray&sources&
gold fcc NRs 1"3"2" Classical&vs&&quantum&mechanica

• ≠ peak FWHM
® ≠ size & cristallinity
nano-rods

Ch
• detailed analysis of the NPs diffraction pattern
The$probes:$phot
description
of+their+interactio
Gold fcc
M
1"1"2" Neutrons
1"1"3" Electrons
• unexpected peaks observed ! • presence of non-fcc Gold particles 1"2"4&– Examples&of&methods&based&on

Zone axis identification
Ch
Reciprocal lattice of a fcc (direct) lattice is a bcc lattice
The$probes:$phot
description
e– // [101] e– // [111] of+their+interactio
e– // [001] – –
202 222 – –
022 202
M
000 000 –
200 020 020 000 220
1"1"2" Neutrons
1"1"3" Electrons
Corresponding reciprocal planes 1"2"4&– Examples&of&methods&based&on
– – ! hot&cathode&tube,&rotating
202 222 – – 1"3"2" Classical&vs&&quantum&mechanica
022 202 1"3"3" Basic&concepts&of&X"ray&scatterin
–
000 020 000 020 000 220
200

Ch
The$probes:$phot
description
of+their+interactio
Direct space
4mm mm2 3m 1"1" The&useful&quantities&to&describe&th

1"1"2" Neutrons
1"1"3" Electrons
Reciprocal space
4mm mm2 6mm
• Diffraction patterns reveal the crystal symmetry

• Reciprocal lattice is centrosymmetric (Friedel’s law)
Ch
Each diffraction pattern has its own geometric characteristics
The$probes:$phot
description
<001> <011> of+their+interactio
M
022
020 220
111 54.74°
A B 45° A
200
B
200
C C
1"1"2" Neutrons
1"1"3" Electrons
4mm symmetry 2mm symmetry 1"3"1" X"ray&sources&
A 8 1"3"4" Basic&concepts&of&X"ray&absorptio
• = ≈ 1.414
C 4
B 8
• = = 2 ≈ 1.414
C 4 A 8
• = ≈ 1.633
B 3
A 4
• = =1 C 4
C 4 • = ≈ 1.155
B 3

Ch
Each diffraction pattern has its own geometric characteristics
The$probes:$phot
description
<111> <112> <123>- - - of+their+interactio
511 313
31.48°
–
022 60° 220 M
311
– B 82.39°
202
A B 58.52° 56.25° A
A
B – –
111 111
60° C C
C –
220
1"1"2" Neutrons
1"1"3" Electrons
41.36° 1"2" Interaction&processes

6mm symmetry mm2 symmetry 2-fold symmetry 1"3" The&specific&case&of&X"rays

A 8 A 27 1"3"4" Basic&concepts&of&X"ray&absorptio
A B 4 • = ≈ 1.633 • = =3
• = = =1 C 3 C 3
C C 4
B 11 B 19
• = ≈ 1.172 • = ≈ 2.517
A 8 C 3
B 11
• = ≈ 1.915
C 3
Ch
The$probes:$phot
• Diffraction patterns of simple structures
description
• face-centered cubic (cF), Al, Cu, Ni, Sr, Rh, Pd, Ag, Ce, Tb, Ir, Pt, Au, Pb, Th, … of+their+interactio
• body-centered cubic (cI), Na, K, V, Cr, Fe, Rb, Nb, Mo, Cs, Ba, Eu, Ta, …
M
• diamond cubic, Si, Ge, Sn, C (diamant), …

• hexagonal close packed (hcp), Be, Sc, Te, Co, Zn, Y, Zr, Tc, Ru, Gd, Tb, Py, Ho, Er,
Tm, Lu, Hf, Re, Os, Tl, …
are existing in tables
1"1"2" Neutrons
1"1"3" Electrons
• For other complex structures, softwares are needed !

Zone axis identification & Indexing

• zone axis determination Ch
The$probes:$phot
• Symmetry : mm2 description
of+their+interactio
A A C
• ≈ 1.44 • ≈ 1.65 • ≈ 1.15
A C B B M
B • Angle between B and C ≈ 55°

C
Þ Zone axis <110>

1"1"2" Neutrons
• Indexing
1"1"3" Electrons
022 1"3"3" Basic&concepts&of&X"ray&scatterin
000
d111 ≈ 0.315 nm
111
222
200
In agreement with silicon cell parameter
(0.5431 nm)
Relation between diffraction and direct space
Ch
The$probes:$phot
description
of+their+interactio
022
-- (220)
000
(111)
111
222
--
(111)
(111)
200
(200) 1"1"1" Electromagnetic&waves
1"1"2" Neutrons
1"1"3" Electrons
[110] 1"2" Interaction&processes
[111] 1"3" The&specific&case&of&X"rays

--
[100] 1"3"3" Basic&concepts&of&X"ray&scatterin
[111] ! differential&cross&section,&T
® Interface plane between Pyrex and silicon is a {100} type


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Electron diffraction analysis

(Pbx-La1–x)TiO3 (Pb(Zrx-Ti1–x)O3 (PZT)

Institut de Minéralogie, de Physique des Matériaux et de Cosmochimie

lL a: 2.70 Å e: 1.90 Å 1"3"3" Basic&concepts&of&X"ray&scatterin

rhkl b: 1.35 Å f: 1.65 Å ! Beer"Lambert&law,&absorpt

000 c: 3.10 Å g: 1.10 Å

Institut de Minéralogie, de Physique des Matériaux et de Cosmochimie

0.210 1"2"2" Interaction&cross&section

0.170 1"3" The&specific&case&of&X"rays

Institut de Minéralogie, de Physique des Matériaux et de Cosmochimie