‫دانشگاه صنعتی سهند تبریز‬

‫دانشکده مهندسی مواد‬

‫گزارشکار ‪XRD‬‬

‫استاد ‪:‬‬

‫پروفسور یزدانی‬

‫دانشجویان‪:‬‬

‫امین جوادی‬

‫مهدی قلیزاده‬

‫خرداد‪09‬‬

‫‪0‬‬
 X-ray Diffraction

The atomic planes of a crystal cause an incident beam of X-rays to interfere with
one another as they leave the crystal. The phenomenon is called X-ray diffraction.

1. Measure the average spacings between layers or rows of atoms

2. Determine the orientation of a single crystal or grain
3. Find the crystal structure of an unknown material
4. Measure the size, shape and internal stress of small crystalline regions

Bragg’s Law and Diffraction

n λ = 2dsinθ
Diffraction occurs only when Bragg’s Law is satisfied Condition for constructive
interference from planes with spacing d.

1
 Applications of XRD

1. XRD is a nondestructive technique

2. To identify crystalline phases and orientation
3. To determine structural properties:
Lattice parameters (10-4Å), strain, grain size, expitaxy, phase composition,
preferred orientation (Laue) order-disorder transformation, thermal expansion
4. To measure thickness of thin films and multi-layers*
5. To determine atomic arrangement
6. Detection limits: ~3% in a two phase mixture; can be
~0.1% with synchrotron radiation
Spatial resolution: normally none

2
 Determination of Volume Fraction of Austenite
When an austempered ductile iron (ADI) specimen is irradiared by x-ray it
produces a characteristic difrfraction pattern which is determined by the structure
of phases present.Quantitive determination of the relative volume fraction of ferrite
and austenite phases can be made because the intensity diffracted from each phase
is proportional to the volume fraction of that phase. If the phases are randomly
oriented the measurement of the integrated intensity of one austenite and one
ferrite (hkl) line will accurately establish the volume fraction of each phase. By
using each pair of austenite and ferrite lines one independent measurement can be
obtained. The integrated intensity of a particular (hkl) reflection in the ferrite or
austenite can be expressed as:

Ihkl = KRhklα Vα /2µ

R = (1/V2) [F2 P (1+Cos2θ)/(Sin2θCosθ)]e-2M

Where

Ihkl is the integrated intensity per angular diffraction peak in α or γ phase

F is the structure factor

P is the multiplicity

θ is the bragg angle

e-2M is the temperature factor

Vα is the volume fraction of α-phase

Calculation of the Theoretical Relative Intensity Factor, R

R factor is a fanction of θ, hkl and crystal stracture.θ is the Bragg angle of

reflectin for each ferrite and austenite hkl line and depends on λ, the caracteristic
wavelength of X-ray radiatin and chemical composition of the crystal. It is derived
from the 2θ position of the peak maximum of the diffraction pattern. Each θ value
can be used to calculate the temperature factor, e-2M,and the atomic scattering
2
factors, f, which are used in the calculation of the structure factor, ,from the
equation

3
 2 2
=

Where

f is the atomic scattering factor

is a correction for anomalous scattering

E is the number of atoms per cell, four for BCC,two for FCC

The integrated intensity from the (hkl) planes of ferrite and austenite phases which
generally exist in an ADI matrix, is expressed as:

Ihkl = KRhklα Vα /2µm

Where µm is the linear absorption coefficient for the mixture of ferrite and
austenite. A similar equation applies to the austenite phase.

For any pair of ferrite and austenite peaks

Ihklα/ Ihklγ = (Rhklα/Rhklγ)( Vα/ Vγ)

The above ratio holds if ferrite and austenite are the only phases present in a
specimen of austempered ductile iron. Then

Vα + Vγ = 1

The volume fraction of austenite, Vγ, is determined using the ratio of measured
integrated intensities of ferrite and austenite and the following equation.

Vγ = (Iγ/Rγ)/( Iα/Rα) + (Iγ/Rγ)

Several pairs can be used for comparing the obtained values and cover the errors
arising from the low preferred orientation of phases. For numerous ferrite and
austenite peaks each ratio of measured integrated intensity to the R value can be
summed

Vγ =

4
Where

q is the number of austenite diffracted peaks

p is number of ferrite diffracted peaks

93
Results

400-2
20
2.0
d=

600

500

400
Lin (Counts)

6
90
2.08

300
d=

200
62
26

68
13

1.1
50

35
1.8

0
31

99
82

d=

34
d=

90
1.4

12
1.2

9
100

46
1.0

1.0
d=

d=

1.0
d=

d=
d=

40 50 60 70 80 90 100 110

2-Theta - Scale
400-2 - File: 400-2.raw - Type: 2Th/Th locked - Start: 38.000 ° - End: 110.000 ° - Step: 0.020 ° - Step time: 1.5 s - Temp.: 25 °C (Room) - Time Started: 6 s - 2-Theta: 38.000 ° - Theta: 19.000 ° - Chi: 0.00 ° -
Operations: Background 1.000,1.000 | Import

Intensity % Intensity Angstrom d value Angle 2-Theta

42.9 256 2.08906 43.275
100.0 598 2.02093 44.811
13.3 79.7 1.81326 50.278
7.7 45.8 1.43150 65.110
6.9 41.3 1.28235 73.839
14.2 84.9 1.16862 82.470
5.2 30.9 1.09340 89.578
4.1 24.5 1.01299 99.003
2.1 12.3 1.04690 94.748

5
 recognize of ferrite and austenite peaks

aFccγ = 3.6469 aBccα = 2.863 a=d√(h2+k2+l2)

Pick 1 γ (111) a = 2.08906 √3  a = 3.618

Pick 2 α (110) a = 2.02093 √2  a = 2.86
Pick 3 γ (200) a = 1.81326 √4  a = 3.627
Pick 4 α (200) a = 1.43150 √4  a = 2.863
Pick 5 γ (220) a = 1.28235 √8  a = 3.63
Pick 6 α (211) a = 1.16862√6  a = 2.863
Pick 7 γ (311) a = 1.09340 √11  a = 3.63
Pick 8 α (220) a = 1.01299√8  a = 2.86
Pick 9 γ (222) a = 1.04690 √12  a = 3.63

According to following equation:

R = (1/V2) [F2 P (1+Cos2θ)/(Sin2θCosθ)]e-2M

2 2
=

θ V= a3 Sinθ/λ f F2 p e-2M R
21.6375 48.50 0.2 18.9 1428.84 8 1 (γ) 71.89
22.4055 23.55 0.3 15.6 3893.76 12 0.99 (α) 1154.45
25.139 48.50 0.3 15.6 973.44 6 0.99 (γ) 27.95
32.555 23.55 0.4 13.3 2830.24 6 0.98 (α) 210.3
36.9195 48.50 0.4 13.3 707.56 12 0.98 (γ) 20.1
41.235 23.55 0.4 13.3 2830.24 24 0.98 (α) 575.1
44.789 48.50 0.5 11.6 538.24 24 0.97 (γ) 22.74
49.5015 23.55 0.5 11.6 2152.96 12 0.97 (α) 171.08
47.374 48.50 0.5 11.6 538.24 8 0.97 (γ) 7.06

Iγ1 = 44.26 Rγ1 = 71.89

Pair picks 1
Iα1 = 116.6 Rα1 = 1154.45
Iγ2 = 20.75 Rγ2 = 27.95
Pair picks 2
Iα2 = 17.05 Rα2 = 210.3
Iγ3 = 13.15 Rγ3 = 20.1
Pair picks 3
Iα3 = 36.33 Rα3 = 575.1

6
By using following equation:

Vγ =

Vγ =

Vγ = 0.89

Determination of Austenite Carbon Content

The unit volume of austenite is a function of carbon and alloy content. The effects
of alloying elements can be ignored.The effect of carbon on the dimension of the
austenite unit cell is expressed by the following equation.

a= 3.548 + 0.044%C

where

a( ) is the unit cell dimension

C is the carbon weight percent

The lattice parameter of austenite varies whit the concentration of carbon

according to equation above. Therefore, precise measurement of the austenite
lattice parameter the carbon composition is determined. By measuring the Bragg
angle θ for a set of planes and using the Bragg law to determine d, the lattice
parameter , a, is determined.It has been shown that the error in calculation of lattice
parameter , a, can be expressed by the following equation

= = - cot .

7
Since cot θ approaches zero as θ approaches 90º , , the fractional error in a,

caused by a given error in θ ,also approaches zero as θ approaches 90º. So, use of
peaks having 2θ as near as possible to180º makes it possible to measure the lattice
parameter presicely. Since there is no reflected beam at this angle the true values of
a can be calculated by piotting the measured values against 2θ and extrapolating to
2θ =180º. This curve is not linear and extrapolation of a non-linear curve is not
accurate.

hkl d a Cos2θ
111 2.08906 3.6184 0.8640
200 1.81326 3.6265 0.8195
220 1.28235 3.6270 0.6392
311 1.09340 3.6264 0.5037
222 1.04690 3.6266 0.4586

a
4
3.8
3.6
3.4
3.2
3
2.8
2.6
2.4
2.2
2
1.8
1.6
1.4
1.2
1
0.8
0.6
0.4
0.2
0
0 0.1 0.2 0.3 0.4 0.5 0.6 0.7 0.8 0.9 1

8
After extrapolation to 2θ=180:

a = 3.69 C = 3.4%

a= 3.548 + 0.044%C

Determination of Pure Cu Lattice Parameter

Cu lattice is fcc and a=d√(h2+k2+l2):

hkl 2θ d a Cos2θ
111 41.901 2.15429 3.7313 0.8722
200 43.761 2.06696 4.1339 0.8611
220 50.785 1.79634 5.0808 0.8161
311 90.302 1.08651 3.6035 0.4974
222 95.912 1.04137 3.674 0.4528

9
 cu
6
5.8
5.6
5.4
5.2
5
4.8
4.6
4.4
4.2
4
3.8
3.6
3.4
3.2
3
2.8
2.6
2.4
2.2
2
1.8
1.6
1.4
1.2
1
0.8
0.6
0.4
0.2
0
0 0.1 0.2 0.3 0.4 0.5 0.6 0.7 0.8 0.9 1

After extrapolation to 2θ=180:

a = 3.2 A0

10
11