SAED in TEM

Selected area electron diffraction
Parallel incoming electron beam and a

selection aperture in the image plane.
Diffraction from a single crystal in a

polycrystalline sample if the aperture is
small enough/crystal large enough.
Orientation relationships between

grains or different phases can be
determined.
~2% accuracy of lattice parameters
Convergent electron beam better
Image plane
Diffraction with large SAD aperture, ring and

spot patterns
Poly crystalline sample
Similar to XRD from polycrystalline samples.
Four epitaxial phases
The orientation relationship between the

phases can be determined with ED.
Higher order reflections, Laue zones

2d sin = n
200kV = 0.00251
nm
~1o
I(k-)I=(2/)sinB=g
From one set of planes we only
get one reflected beam
-The Bragg angle increases with
increasing order (n)
-Tilt sample or beam to satisfy
Bragg condition of higher order
reflections.
Ewald sphere
(Reflecting sphere)
The intensity distribution

around each reciprocal
lattice point is spread out
in the form of spikes directed
normal to the specimen
2
k=1/
First order Laue zone

Zero order Laue zone
(see figure 2.35 text book)
Double diffraction, extinction thickness
Double electron diffraction leads to

oscillations in the diffracted intensity
with increasing thickness of the
sample
Incident beam
No double diffraction with XRD,

kinematical intensities
Forbidden reflection may be observed
t0: Extinction thickness
Periodicity of the oscillations

t0=Vc/IF(hkl)I
Wedge shaped TEM sample

t0
Transmitted
Diffracted beam Doubly
diffracted beam beam
Kikuchi lines
Deficient
Used for determination of:

-crystal orientation
Excess
B
B
-lattice parameter
-accelerating voltage
2B
-Burgers vector
Objective lens
Diffraction plane
Excess
line
Deficient
line
1/d
http://www.doitpoms.ac.uk/index.html
http://www.doitpoms.ac.uk/tlplib/diffraction-patterns/kikuchi.php
Camera constant
R=L tan2B ~
2LsinB
2dsinB =
R=L/d
Camera constant:
K=L
Film plate
Indexing diffraction patterns

The g vector to a reflection is normal to the
corresponding (h k l) plane and IgI=1/dnh nk nl
(h2k2l2)
Measure Ri and the angles between

the reflections
Calculate di , i=1,2,3
Compare with tabulated/theoretical

calculated d-values of possible phases
Compare Ri/Rj with tabulated values for

cubic structure.
g1,hkl+ g2,hkl=g3,hkl (vector sum must be ok)
Perpendicular vectors: gi gj = 0
Orientations of corresponding
planes in the real space
(=K/Ri)
Zone axis: gi x gj =[HKL]z

All indexed g must satisfy: g [HKL]z=0
Example: Study of unknown phase in a BiFeO3 thin film

Metal organic compound on Pt
BiFeO3
Heat treatment at 350oC (10 min) to

remove organic parts.
Pt
TiO2
Lim
Process repeated three times before final

heat treatment at 500-700 oC (20 min) .
(intermetallic phase grown)
SiO2
Bi
Bi
O
O
Si
Bi
Bi
Fe
O
Bi
Fe
Fe
O
O
O
O
200 nm
Fe
Bi
Fe
Fe
Bi
Bi
O
O
O
Bi
Bi
Bi
Fe
Goal:
Fe
Fe
O
O
BiFeO3 with space grupe: R3C

and celle dimentions:
a= 5.588 c=13.867
c
O
Fe
Bi
Fe
Bi
Bi
O Fe
Bi
Bi
Po wd erCell 2 .0
Determination of the Bravais-lattice of an unknown

crystalline phase
Tilting series around common axis
27o
15o
50 nm
10o
0o
Determination of the Bravais-lattice of an unknown

crystalline phase
Tilting series around a dens row of
reflections in the reciprocal space
0o
50 nm
19o
Positions of the
reflections in the
reciprocal space
25o
40o
52o
Bravais-lattice and cell parameters
011
111
001
c
101
b
010
a
110
100
[011]
[100]
[101]
d=L/R
6.04
From the tilt series we find that the unknown phase

has a primitive orthorhombic Bravias-lattice with
cell parameters:
a= 6,04 , b= 7.94 og c=8.66
7.94
= = = 90o
Chemical analysis by use of EDS and EELS

Ukjent fase
BiFe2O5
BiFeO3
x 1000
counts
CCD
x 1000
counts
CCD
1_1evprc.PICT
Nr_2_1evprc.PICT
40
14
35
12
O-K
Fe - L2,3
30
10
25
8
20
6
BiFeO3
Ukjent fase
4
15
2
10
-0
5
500
1 eV pr.600
kanal 800
-0 eV forskyvning,
200
400
-0
200
Energy
(eV)
400 Loss 600
Energy Loss (eV)
800
1000
1000
Published structure
A.G. Tutov og V.N. Markin
The x-ray structural analysis of the antiferromagnetic Bi2Fe4O9 and the isotypical combinations Bi2Ga4O9 and Bi2Al4O9
Izvestiya Akademii Nauk SSSR, Neorganicheskie Materialy (1970), 6, 2014-2017.
Romgruppe: Pbam nr. 55,
celleparametre: 7,94 , 8,44 , 6.01

Bi
O
Bi
Bi
Fe
Fe
O
O
O
O
4g
4h
4f
4g
8i
4h
2b
x
0,176
0,349
0
0,14
0,385
0,133
0
y
0,175
0,333
0,5
0,435
0,207
0,427
0
Bi
z
0
0,5
0,244
0
0,242
0,5
0,5
Bi
Fe
O
Fe
Fe
O
Fe O
O
Fe
O
O
Fe
O
Fe
O
Fe
O
Fe
O
O
Fe
Fe
O
Fe
Bi
O
Bi
Bi
O
Bi
c
b
Po wd erCell 2 .0
Celle parameters found with electron diffraction (a= 6,04 , b= 7.94 and c=8.66 ) fits reasonably well with the
previously published data for the Bi2Fe4O9 phase. The disagreement in the c-axis may be due to the fact that we
have been studying a thin film grown on a crystalline substrate and is not a bulk sample. The conditions for
reflections from the space group Pbam is in agreement with observations done with electron diffraction.
Conclusion: The unknown phase has been identified as Bi2Fe4O9 with space group Pbam with cell parameters a=
6,04 , b= 7.94 and c=8.66 .

SAED in TEM

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SAED in TEM

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Selected area electron diffraction

Parallel incoming electron beam and a

Diffraction from a single crystal in a

Orientation relationships between

~2% accuracy of lattice parameters

Convergent electron beam better

Diffraction with large SAD aperture, ring and

Similar to XRD from polycrystalline samples.

Four epitaxial phases

The orientation relationship between the

Higher order reflections, Laue zones

The intensity distribution

First order Laue zone

Double diffraction, extinction thickness

Double electron diffraction leads to

No double diffraction with XRD,

t0: Extinction thickness

Periodicity of the oscillations

Wedge shaped TEM sample

Used for determination of:

Indexing diffraction patterns

Measure Ri and the angles between

Compare with tabulated/theoretical

Compare Ri/Rj with tabulated values for

g1,hkl+ g2,hkl=g3,hkl (vector sum must be ok)

Zone axis: gi x gj =[HKL]z

Example: Study of unknown phase in a BiFeO3 thin film

Heat treatment at 350oC (10 min) to

Process repeated three times before final

BiFeO3 with space grupe: R3C

Determination of the Bravais-lattice of an unknown

Determination of the Bravais-lattice of an unknown

Bravais-lattice and cell parameters

From the tilt series we find that the unknown phase

Chemical analysis by use of EDS and EELS

celleparametre: 7,94 , 8,44 , 6.01

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