• The following diffraction pattern was acquired from an aluminum matrix and a Mg2Si

precipitate which have an orientation relationship.

• Solve the diffraction pattern and determine

the orientation relationship between the
crystals (lL=2.4nm):

-1-
 ⇓
ത
Both Z.A. = 210

𝐴𝑙 002 ∥ 𝑀𝑔2 𝑆𝑖 002

OR=
𝐴𝑙 21ത 0 ∥ 𝑀𝑔2 𝑆𝑖 21ത 0
-2-
 -3-
Courtesy of W.D. Kaplan
Zero Order Laue Zone (ZOLZ)
First Order Laue Zone (FOLZ)
Second Order Laue Zone
(SOLZ)
….

-4-
W&C page 338
-5-
• The intensity (amplitude) of the ring will be
even for random distribution of particles and
not even when a preferred orientation exists.

-6-
A textured ring pattern where the DP from polycrystalline foil DP from polycrystalline foil
rings are more intense over a with relatively small grains with relatively large grain
certain angular range randomly oriented randomly oriented

-7-
W&C page 291-292
-8-
• The following ring pattern was acquired from a polycrystalline sample with Al and Fe grains.
Determine which rings are from which phase and what is the family of planes it represents.
𝜆𝐿 = 10[Å ∙ cm]

-9-
• The DP from an amorphous material looks similar to that from polycrystalline
material but the rings are broader and there is no speckle.

Ring patterns from Ring patterns from

amorphous Carbon polycrystalline Aluminum

-10-
• assuming that the electron beam is only scattered once (kinematical conditions).
Which is more realistic than for crystals at the Bragg condition:

If the material is isotropic, we can simplify the equation to:

where

-11-
⇒ the RDF can be obtained directly from DPs. This process is
enhanced if the patterns are energy-filtered to remove inelastic
contributions

The Radial distribution function (RDF) = ρ(r) :

the locations of the neighboring atoms are defined by the probability
per unit volume that an atom will be found at a distance r from it.

-12-
 X-ray Powder Diffraction Selected Area Electron Diffraction
(https://images.app.goo.gl/CaMw2MpGQqk2MM2N (https://images.app.goo.gl/yZ74rJ1RdAYBniCLA)
6)
-14-
-15-
 List of selection rules for different crystals

Some Useful Relations (Needed for structure factor calculations) :

-16-
 1/2 atom 1/8 atom on 1 atom in 1/8 atom on
on 6 faces 8 corners the center 8 corners

The position of the atoms in a unit cell:

𝟏 𝟏 𝟏 𝟏 𝟏 𝟏 𝟏 𝟏 𝟏
𝟎, 𝟎, 𝟎 , ,𝟎 , 𝟎, 𝟎, 𝟐 , 𝟐 = 4 𝟎, 𝟎, 𝟎 , , = 2 atoms
𝟐 𝟐 𝟐 𝟐 𝟐 𝟐 𝟐
atoms
-17-
 𝟏 𝟏 𝟏 𝟏 𝟏 𝟏
The position of the atoms in a unit cell: 𝟎, 𝟎, 𝟎 , ,𝟎
𝟐 𝟐 𝟐
, 𝟎,
𝟐
𝟎, ,
𝟐 𝟐

Substitute in a few values of 𝒉, 𝒌, 𝒍 and you will find the following:

(111), (200), (220),
(h, k, l) unmixed 𝐹 = 4𝑓 𝐹 2 = 16𝑓 2 (333), (420)
h,k,l → all even or all odd
(100), (211); (210),
(h, k, l) mixed 𝐹=0 𝐹2 = 0 (032), (033)
Two odd and one even (e.g. 112); two even and one odd (e.g. 122)
-18-
 For GaSb
(a) Find the position of the atoms in a unit cell.

GaSb – JCPDS 32-389; AlAs – JCPDS 17-915

ITC No. 216, Pearson F-43m

Generating
Wycoff
sites occupancy
positions
x y Z
4a Sb 0 0 0 100% 4 atoms Si
4c Ga 1/4 1/4 1/4 100% 8 atoms Mg
𝟏 𝟏 𝟏 𝟏 𝟏 𝟏
𝑺𝒃: 𝟎, 𝟎, 𝟎 , ,𝟎 , 𝟎, 𝟎, ,
𝟐 𝟐 𝟐 𝟐 𝟐 𝟐
𝟏 𝟏 𝟏 𝟑 𝟑 𝟏 𝟑 𝟏 𝟑 𝟏 𝟑 𝟑
𝑮𝒂: , , , , , , , ,
𝟒 𝟒 𝟒 𝟒 𝟒 𝟒 𝟒 𝟒 𝟒 𝟒 𝟒 𝟒
-19-
 For GaSb
𝟏 𝟏 𝟏 𝟏 𝟏 𝟏
(b) In which cases the structure 𝑺𝒃: 𝟎, 𝟎, 𝟎 , ,𝟎 , 𝟎, 𝟎, ,
𝟐 𝟐 𝟐 𝟐 𝟐 𝟐
𝟏 𝟏 𝟏 𝟑 𝟑 𝟏 𝟑 𝟏 𝟑 𝟏 𝟑 𝟑
factor is zero ? 𝑮𝒂: , , , , , , , ,
𝟒 𝟒 𝟒 𝟒 𝟒 𝟒 𝟒 𝟒 𝟒 𝟒 𝟒 𝟒

In this case 𝐹 2 will be zero for mixed indexes

(like the FCC structures).
-20-
 For GaSb
(c) Calculate the structure factor (including the atomic scattering factors
for electrons at 200keV) for the first two reflections.

𝑬
𝟏+ 𝝀
𝟐
𝑬𝟎
𝒇 𝜽 = 𝒁 − 𝒇𝒙 𝜽
𝟖𝝅𝟐 𝒂𝟎 𝒔𝒊𝒏𝜽
𝜀 ℎ2
where 𝑎0 = 𝜋𝑚0 2 = 0.529Å = Bohr radius and 𝑓𝑥 = Scattering factor for x-rays.
0𝑒

-21-
 For GaSb
𝐸
1+𝐸 𝜆
2
1 + 200Τ511 1 2
0
𝑓𝑒− 𝜃 = 𝑍 − 𝑓𝑥 𝜃 = 𝑍 − 𝑓𝑥 𝜃 =
8𝜋 2 𝑎 0 𝑠𝑖𝑛𝜃 8𝜋 2 ∙ 0.529 𝑆𝑖𝑛𝜃
𝜆
2 2
1.391 1 1
= 𝑍 − 𝑓𝑥 𝜃 = 0.033 𝑍 − 𝑓𝑥 𝜃
41.77 𝑆𝑖𝑛𝜃 𝑆𝑖𝑛𝜃
𝜆 𝜆

𝟏/𝟐𝒅 𝒇𝒓𝒐𝒎 𝒕𝒉𝒆 𝒕𝒂𝒃𝒍𝒆

𝒅 𝑺𝒊𝒏𝜽/𝝀 𝒇𝑺𝒃
𝒙 𝒇𝑮𝒂
𝒙 𝒇𝑺𝒃
𝒆− 𝒇𝑮𝒂
𝒆− 𝑰= 𝑭 𝟐

111 3.532 0.141 46.523 27.673

200 3.059 0.163 42.73 24.96

-22-
 For GaSb
𝒅 𝑺𝒊𝒏𝜽/𝝀 𝒇𝑺𝒃
𝒙 𝒇𝑮𝒂
𝒙 𝒇𝑺𝒃
𝒆− 𝒇𝑮𝒂
𝒆− 𝑰= 𝑭 𝟐

111 3.532 0.141 46.523 27.673 7.43 5.52

200 3.059 0.163 42.73 24.96 10.27 7.5

2
1
𝒇𝑺𝒃
𝒆− 𝜃111 = 0.033 51 − 46.523 = 1.66 × 4.477 ≈ 7.43
0.141
2
1
𝒇𝑮𝒂
𝒆− 𝜃111 = 0.033 31 − 27.673 = 1.66 × 3.327 ≈ 5.52
0.141
2
1
𝒇𝑺𝒃
𝒆− 𝜃200 = 0.033 51 − 42.73 = 1.242 × 8.27 ≈ 10.27
0.163
2
1
𝒇𝑮𝒂
𝒆− 𝜃200 = 0.033 31 − 24.96 = 1.242 × 6.04 ≈ 7.5
0.163
-23-
 For GaSb
0
3𝜋
𝑭𝟏𝟏𝟏 𝟐 2
= 16 𝑓𝑆𝑏 2
+ 𝑓𝐺𝑎 + 2𝑓𝑆𝑏 𝑓𝐺𝑎 𝑐𝑜𝑠 = 𝟏𝟔 𝒇𝟐𝑺𝒃 + 𝒇𝟐𝑮𝒂 = 16 × 85.67 ≈ 𝟏𝟑𝟕𝟎. 𝟖
2

𝑭𝟐𝟎𝟎 𝟐 2
= 16 𝑓𝑆𝑏 2
+ 𝑓𝐺𝑎 + 2𝑓𝑆𝑏 𝑓𝐺𝑎 𝑐𝑜𝑠 𝜋 = 𝟏𝟔 𝒇𝟐𝑺𝒃 + 𝒇𝟐𝑮𝒂 − 𝟐𝒇𝑺𝒃 𝒇𝑮𝒂 = 16 × 7.673 ≈ 𝟏𝟐𝟐. 𝟕

𝒅 𝑺𝒊𝒏𝜽/𝝀 𝒇𝑺𝒃
𝒙 𝒇𝑮𝒂
𝒙 𝒇𝑺𝒃
𝒆− 𝒇𝑮𝒂
𝒆− 𝑰= 𝑭 𝟐

111 3.532 0.141 46.523 27.673 7.43 5.52 1370.8

200 3.059 0.163 42.73 24.96 10.27 7.5 122.7

-24-
 For GaSb
(d) How the answer would change for the AlAs (which has the same
crystallographic structure) ? How the intensity of the two first reflections
will change ?

⇒ 𝑰𝑨𝒍𝑨𝒔
𝟏𝟏𝟏 < 𝑰𝑮𝒂𝑺𝒃
𝟏𝟏𝟏 & 𝑰𝑨𝒍𝑨𝒔
𝟐𝟎𝟎 > 𝑰𝑮𝒂𝑨𝒔
𝟐𝟎𝟎

-25-
 For GaSb
(e) Will there be any change in the intensity if we switch the positions of
the two species of atoms ?

There will be no difference since the expression for the intensity is at

the power of 2 and the two types of atoms are totally equivalent:

𝜋𝑖 𝜋𝑖
𝟐
𝑰 ∝ 𝑭 = 𝑓𝑆𝑏 + 𝑓𝐺𝑎 𝑒 2 ℎ+𝑘+𝑙 𝑓𝑆𝑏 + 𝑓𝐺𝑎 𝑒 − 2 ℎ+𝑘+𝑙 2
∙ 𝐹𝐹𝐶𝐶
𝝅𝒊 𝝅𝒊
= 𝑭𝟐𝑺𝒃 + 𝑭𝟐𝑮𝒂 + 𝒇𝑺𝒃 𝒇𝑮𝒂 𝒆 𝟐 𝒉+𝒌+𝒍 + − 𝒉+𝒌+𝒍
𝒇𝑺𝒃 𝒇𝑮𝒂 𝒆 𝟐 ∙ 𝑭𝟐𝑭𝑪𝑪

-26-
We were asked to characterize a polycrystalline BaTiO3 sample which
contains two types of precipitates as shown in the figure. One type is
TiO2 and the second one is BaO.

A schematic representation of the polycrystalline

BaTiO3 sample containing two types of precipitates.

-27-
 Cubic

Tetragonal

Cubic

-28-
Two SAD patterns were acquired using a TEM operated at 200KeV using
the same acquisition conditions from the areas marked as SAD #1 and
SAD #2.

SAD pattern acquired from the SAD pattern acquired from the
area marked as SAD #2 -29-
area marked as SAD #1
A. Determine the camera constant 𝝀𝑳 .

The light gray pattern is similar in both SADs therefore it belongs to the
matrix which is the BaTiO3.

We don’t know the 𝝀𝑳 so we will use the ratio

method
𝑎
For a cubic 𝑑=
ℎ2 + 𝑘 2 + 𝑙 2
structure:
{hkl}BaTiO3 d di/dmax
100 4.006 1
110 2.832 0.707
111 2.313 0.577

-30-
A. Determine the camera constant 𝝀𝑳 .

i 2Ri [mm] Angle (α) 2Ri/2Rmin {hkl} (hkl)

1 41 1 100 100
45º 2R3 2R2
2 58 0.707 110 110
45º 45º
3 41 1 100 010 45º
2R1

𝑥 𝑦 𝑧
𝑍. 𝐴. = 1 0 0 = 𝑥 0 − 0 + 𝑦 0 − 0 + z 1 − 0 = 001
1 1 0

2𝑅𝑑 41 ∗ 4.006
𝜆𝐿 = = = 82 𝑚𝑚 ⋅ Å
2 2
-31-
B. Solve the SAD patters (two reflections and Z.A.).
i 2Ri [mm] Angle (α) d=2𝜆𝐿/2R {hkl} (hkl)
1 86 1.907 020 200
45º
SAD #1: 2 122
45º
1.344 220 220  Z. A.
= [001]
TiO2
3 86 1.907 020 020

i 2Ri [mm] Angle (α) d=2𝜆𝐿/2R {hkl} (hkl)

1 52 3.154 111 111
~70º
2 52 3.154 111 1 1 -1
SAD #2: ~30º  Z. A. =
[1ത 10]
BaO
3 99 1.656 113 1 1 -3
~25º
4 60 2.733 002 0 0 -2
-32-
D. Determine the O.R. between each of the precipitates and the matrix.

SAD #1: Red = BaTiO3 ; Black = TiO2 SAD #2: Red = BaTiO3 ; Blue = BaO
OR: 𝟎𝟎𝟏 𝑩𝒂𝑻𝒊𝑶𝟑 ∥ 𝟎𝟎𝟏 𝑻𝒊𝑶𝟐 & (𝟐𝟎𝟎)𝑩𝒂𝑻𝒊𝑶𝟑 ∥ (𝟐𝟎𝟎)𝑻𝒊𝑶𝟐 OR: 𝟎𝟎𝟏 𝑩𝒂𝑻𝒊𝑶𝟑
ഥ𝟏𝟎
∥ 𝟏 𝑩𝒂𝑶 & (𝟏𝟎𝟎)𝑩𝒂𝑻𝒊𝑶𝟑 ∥ (𝟏𝟏𝟏)𝑩𝒂𝑶

-33-
Low Index Zone Axes in Cubic Structures:

Z.A. [ 1 0 0 ] Z.A. [ 1 1 0 ] Z.A. [ 1 1 1 ]

-34-