X - r a y d i ff r a c t i o n E x p e r i m e n t

Introduction
Objective

: To determine the crystal structure

of various samples using x-ray diffraction
technique.
X-ray crystallography is a technique used for determining the atomic and
molecular structure of a crystal, in which the crystalline atoms cause a beam of
incident X-rays to diffract into many specific directions. By measuring the angles
and intensities of these diffracted beams, a crystallographer can produce a threedimensional picture of the density of electrons within the crystal. From this
electron density, the mean positions of the atoms in the crystal can be determined,
as well as their chemical bonds, their disorder and various other information.
It is well known that, for visible electromagnetic radiation to be diffracted, the
spacing between lines in a two-dimensional grating must be of the same order as
that of the same order as the wavelength range for light (3900-7800). The same
principle holds good for diffraction by the three-dimensional grating of the
periodic array of atoms in crystals. The typical interatomic spacing in crystals is 23 A. So, the wavelength of the radiation used for crystal diffraction should be in the
same range. X-rays have wavelengths in this range and are, therefore, diffracted by
crystals. This property is widely used for the study of crystal structures

1 | Page

T H A PA R U N I V E R S I T Y

X - r a y d i ff r a c t i o n E x p e r i m e n t

Cystallograpic
Determination
SAMPLE 1
Measurement Conditions:
Dataset Name

5
Goniometer=PW3050/60 (Theta/Theta); Minimum step
size 2Theta:0.001; Minimum step size Omega:0.001
Sample stage=Reflection-Transmission Spinner
PW3064/60; Minimum step size Phi:0.1
Measurement Date / Time 11/9/2016 10:42:11 AM
Scan Axis
Gonio
Start Position [2Th.]
20.0066
End Position [2Th.]
79.9886
Step Size [2Th.]
0.0130
Scan Step Time [s]
38.8871
Scan Type
Continuous
PSD Mode
Scanning
PSD Length [2Th.]
3.35
Offset [2Th.]
0.0000
Divergence Slit Type
Automatic
Irradiated Length [mm]
10.00
Specimen Length [mm]
10.00
Measurement Temperature [C] 25.00
Anode Material
Cu
K-Alpha1 []
1.54060
Generator Settings
40 mA, 45 kV
Diffractometer Type
0000000011059259
Diffractometer Number
0
Goniometer Radius [mm] 240.00
Dist. Focus-Diverg. Slit [mm]
100.00
Incident Beam Monochromator No
Spinning
Yes
2 | Page

T H A PA R U N I V E R S I T Y

X - r a y d i ff r a c t i o n E x p e r i m e n t

Main Graphics, Analyze View:

Counts
5

20000

10000

0
30

40

50

60

Position [2Theta]

Peak List:
Pos.
[2Th.]
43.3617
50.4206
74.1234

Height
[cts]
20234.01
7378.70
3545.32

FWHM [2Th.]
0.2303
0.2047
0.1872

d-spacing
[]
2.08507
1.80846
1.27813

Rel. Int.
[%]
100.00
36.47
17.52

Pattern List:
Document History:
Default properties:
- Measurement step axis = "None"
- Internal wavelengths used from anode material: Copper (Cu)
- Original K-Alpha1 wavelength = "1.54060"
- Used K-Alpha1 wavelength = "1.54060"
- Original K-Alpha2 wavelength = "1.54443"
- Used K-Alpha2 wavelength = "1.54443"
- Original K-Beta wavelength = "1.39225"
- Used K-Beta wavelength = "1.39225"
- Incident beam monochromator = "No"
- Fixed div. slit size = "1.00000"
- Receiving slit size = "0.10000"
3 | Page

T H A PA R U N I V E R S I T Y

70

X - r a y d i ff r a c t i o n E x p e r i m e n t

Step axis value = "0.00000"

Offset = "0.00000"
Sample length = "10.00000"
Modification time = "11/18/2016 2:59:46 PM"

Interpolate Step Size:

- Step Size = "Derived"
- Modification time = "2/1/2006"
Determine Background:
- Correction method = "Search Peaks"
- Minimum significance = "1.00"
- Minimum tip width = "0.00"
- Maximum tip width = "1.00"
- Peak base width = "2.00"
- Add to net scan = "Nothing"
Search Peaks:
- Minimum significance = "20.00"
- Minimum tip width = "0.10"
- Maximum tip width = "0.50"
- Peak base width = "1.00"
- Method = "Minimum 2nd derivative"
- Modification time = "11/18/2016 2:59:13 PM"

Strip K-Alpha2:
- Method = "Rachinger"
- Intensity ratio = "0.50"
- Delta wavelength ratio = "0.000000"
- Modification time = "2/1/2006"

Observation and Calculation :4 | Page

T H A PA R U N I V E R S I T Y

X - r a y d i ff r a c t i o n E x p e r i m e n t

2*theta

theta

Sin2(theta)

Ratio

of

Sin2(theta)

Approx.
whole
number

43.3617

21.68085

0.976121

3.0000

50.4206

25.21
03
37.06
17

0.001503

3.9879

0.098181

7.9838

74.1234

4
8

Since, for determination of face-centered crystal , the whole number

ratios comes out to be

FCC:-

3 : 4 : 8 : 11 : 12 : 16 : 19

Therefore we conclude that the structure of

sample-1

face-centered cubic (FCC)

within the limits of

experimental error

5 | Page

T H A PA R U N I V E R S I T Y

crystal

is a

X - r a y d i ff r a c t i o n E x p e r i m e n t

SAMPLE 2
Measurement Conditions: (Bookmark 1)
Dataset Name

Chalk
Goniometer=PW3050/60 (Theta/Theta); Minimum step
size 2Theta:0.001; Minimum step size Omega:0.001
Sample stage=Reflection-Transmission Spinner
PW3064/60; Minimum step size Phi:0.1
Diffractometer system=XPERT-PRO
Creation date=2/5/2010 5:38:09 PM
Measurement Date / Time 11/9/2016 11:17:38 AM
Raw Data Origin
XRD measurement (*.XRDML)
Scan Axis
Gonio
Start Position [2Th.]
15.0066
End Position [2Th.]
79.9936
Step Size [2Th.]
0.0130
Scan Step Time [s]
38.8852
Scan Type
Continuous
PSD Mode
Scanning
PSD Length [2Th.]
3.35
Offset [2Th.]
0.0000
Divergence Slit Type
Automatic
Irradiated Length [mm]
10.00
Specimen Length [mm]
10.00
Measurement Temperature [C] 25.00
Anode Material
Cu
K-Alpha1 []
1.54060
Generator Settings
40 mA, 45 kV
Diffractometer Type
0000000011059259
Diffractometer Number
0
Goniometer Radius [mm] 240.00
Dist. Focus-Diverg. Slit [mm]
100.00
Incident Beam Monochromator No
Spinning
Yes

Main Graphics, Analyze View: (Bookmark 2)

6 | Page

T H A PA R U N I V E R S I T Y

X - r a y d i ff r a c t i o n E x p e r i m e n t

Counts
Chalk
6000

4000

2000

0
20

30

40

50

60

70

Position [2Theta]

Peak List: (Bookmark 3)

Pos.
[2Th.]
23.1398

Height
[cts]
363.56

FWHM [2Th.]
0.3070

d-spacing
[]
3.84068

Rel. Int.
[%]
6.85

29.4737
36.0446
39.4943
43.2185
47.5656
48.5707
56.6211
57.4462
64.6842
65.6499
73.0341

5304.41
737.59
1073.60
859.29
981.23
993.25
159.48
407.04
253.81
152.96
115.85

0.1535
0.1791
0.2047
0.2047
0.2047
0.2303
0.2558
0.3070
0.3070
0.2558
0.4992

3.02815
2.48976
2.27987
2.09165
1.91013
1.87293
1.62425
1.60286
1.43988
1.42102
1.29449

100.00
13.91
20.24
16.20
18.50
18.73
3.01
7.67
4.78
2.88
2.18

Document History: (Bookmark 5)

Insert Measurement:
- File name = "Chalk.xrdml"
- Modification time = "11/18/2016 2:57:03 PM"
- Modification editor = "Dell"
Default properties:
- Measurement step axis = "None"
- Internal wavelengths used from anode material: Copper (Cu)
7 | Page

T H A PA R U N I V E R S I T Y

X - r a y d i ff r a c t i o n E x p e r i m e n t

Original K-Alpha1 wavelength = "1.54060"

Used K-Alpha1 wavelength = "1.54060"
Original K-Alpha2 wavelength = "1.54443"
Used K-Alpha2 wavelength = "1.54443"
Original K-Beta wavelength = "1.39225"
Used K-Beta wavelength = "1.39225"
Incident beam monochromator = "No"
Fixed div. slit size = "1.00000"
Receiving slit size = "0.10000"
Step axis value = "0.00000"
Offset = "0.00000"
Sample length = "10.00000"
Modification time = "11/18/2016 2:57:03 PM"
Modification editor = "Dell"

Interpolate Step Size:

- Step Size = "Derived"
- Modification time = "2/1/2006"
- Modification editor = "PANalytical"
Determine Background:
- Correction method = "Search Peaks"
- Minimum significance = "1.00"
- Minimum tip width = "0.00"
- Maximum tip width = "1.00"
- Peak base width = "2.00"
- Add to net scan = "Nothing"
- Modification time = "10/26/2016 4:55:04 PM"
- Modification editor = "Dell"
Search Peaks:
- Minimum significance = "30.00"
- Minimum tip width = "0.10"
- Maximum tip width = "0.50"
- Peak base width = "1.00"
- Method = "Minimum 2nd derivative"
- Modification time = "11/18/2016 2:57:50 PM"
- Modification editor = "Dell"
Strip K-Alpha2:
- Method = "Rachinger"
- Intensity ratio = "0.50"
- Delta wavelength ratio = "0.000000"
- Modification time = "2/1/2006"
- Modification editor = "PANalytical"

Observation and Calculation :8 | Page

T H A PA R U N I V E R S I T Y

X - r a y d i ff r a c t i o n E x p e r i m e n t

2*the

Sin2(th

theta

ta

eta)

Ratio
2

Sin (theta)

of

Approx.
whole
number

23.13
98
29.47
37
36.04
46
39.49
43
43.21
85
47.56
56
48.57
07

11.569
9
14.736
85
18.022
3
19.747
15
21.609
25
23.782
8
24.285
35

0.70485
9
0.68147
4
0.54180
9
0.61125
7
0.13889
3
0.95201
1
0.56183
4

3.0000
3
4.8260
5
7.1388
7
8.5137
8
10.1149
10
12.1286
12
12.6153

Since, for determination of face-centered crystal , the whole number

ratios comes out to be

FCC:-

3 : 4 : 8 : 11 : 12 : 16 : 19

Therefore we conclude that the structure of

sample-2

face-centered cubic (FCC)

within the limits of

crystal

is a

experimental error, although the values are very flucuating here.

9 | Page

T H A PA R U N I V E R S I T Y

X - r a y d i ff r a c t i o n E x p e r i m e n t

SAMPLE 3
Measurement Conditions: (Bookmark 1)
Dataset Name
1
File name
C:\Users\Dell\Desktop\1.xrdml
Comment
Configuration=Spinner Reflection-Transmission,
Owner=User-1, Creation date=6/25/2009 11:03:49 AM
Goniometer=PW3050/60 (Theta/Theta); Minimum step
size 2Theta:0.001; Minimum step size Omega:0.001
Sample stage=Reflection-Transmission Spinner
PW3064/60; Minimum step size Phi:0.1
Diffractometer system=XPERT-PRO
Measurement program=Thapar_Spinner Stage,
Owner=User-1, Creation date=2/5/2010 5:38:09 PM
Measurement Date / Time 11/9/2016 11:01:45 AM
Operator
Administrator
Raw Data Origin
XRD measurement (*.XRDML)
Scan Axis
Gonio
Start Position [2Th.]
15.0066
End Position [2Th.]
79.9936
Step Size [2Th.]
0.0130
Scan Step Time [s]
38.8852
Scan Type
Continuous
PSD Mode
Scanning
PSD Length [2Th.]
3.35
Offset [2Th.]
0.0000
Divergence Slit Type
Automatic
Irradiated Length [mm]
10.00
Specimen Length [mm]
10.00
Measurement Temperature [C] 25.00
Anode Material
Cu
K-Alpha1 []
1.54060
Generator Settings
40 mA, 45 kV
Diffractometer Type
0000000011059259
Diffractometer Number
0
Goniometer Radius [mm] 240.00
Dist. Focus-Diverg. Slit [mm]
100.00
Incident Beam Monochromator No
Spinning
Yes

10 | P a g e

T H A PA R U N I V E R S I T Y

X - r a y d i ff r a c t i o n E x p e r i m e n t

Main Graphics, Analyze View: (Bookmark 2)

Counts
8000

6000

4000

2000

0
20

30

40

50

60

Position [2Theta]

Peak List: (Bookmark 3)

Pos.
[2Th.]
38.4724
44.7109
65.0463
78.2087

Height
[cts]
7091.19
3807.97
1604.94
1559.67

FWHM [2Th.]
0.2303
0.2558
0.2303
0.3432

d-spacing
[]
2.33804
2.02523
1.43274
1.22127

Rel. Int.
[%]
100.00
53.70
22.63
21.99

Pattern List: (Bookmark 4)

Document History: (Bookmark 5)
Insert Measurement:
- File name = "1.xrdml"
- Modification time = "11/18/2016 2:58:59 PM"
- Modification editor = "Dell"
Default properties:
- Measurement step axis = "None"
- Internal wavelengths used from anode material: Copper (Cu)
- Original K-Alpha1 wavelength = "1.54060"
- Used K-Alpha1 wavelength = "1.54060"
11 | P a g e

T H A PA R U N I V E R S I T Y

70

X - r a y d i ff r a c t i o n E x p e r i m e n t

Original K-Alpha2 wavelength = "1.54443"

Used K-Alpha2 wavelength = "1.54443"
Original K-Beta wavelength = "1.39225"
Used K-Beta wavelength = "1.39225"
Incident beam monochromator = "No"
Fixed div. slit size = "1.00000"
Receiving slit size = "0.10000"
Step axis value = "0.00000"
Offset = "0.00000"
Sample length = "10.00000"
Modification time = "11/18/2016 2:58:59 PM"
Modification editor = "Dell"

Interpolate Step Size:

- Step Size = "Derived"
- Modification time = "2/1/2006"
- Modification editor = "PANalytical"
Determine Background:
- Correction method = "Search Peaks"
- Minimum significance = "1.00"
- Minimum tip width = "0.00"
- Maximum tip width = "1.00"
- Peak base width = "2.00"
- Add to net scan = "Nothing"
- Modification time = "10/26/2016 4:55:04 PM"
- Modification editor = "Dell"
Search Peaks:
- Minimum significance = "20.00"
- Minimum tip width = "0.10"
- Maximum tip width = "0.50"
- Peak base width = "1.00"
- Method = "Minimum 2nd derivative"
- Modification time = "11/18/2016 2:59:13 PM"
- Modification editor = "Dell"
Strip K-Alpha2:
- Method = "Rachinger"
- Intensity ratio = "0.50"
- Delta wavelength ratio = "0.000000"
- Modification time = "2/1/2006"
- Modification editor = "PANalytical"

12 | P a g e

T H A PA R U N I V E R S I T Y

X - r a y d i ff r a c t i o n E x p e r i m e n t

Observation and Calculation :2*the

theta

ta
38.47
24
44.71
09
65.04
63
78.20
87

19.236
2
22.355
45
32.523
15
39.104
35

Sin2(th

Ratio

eta)

Sin2(theta)

number

0.14219
1
0.12694
7

3.0000

of

Approx.

3.9983

7.9890

whole

0.80006
10.9951

11

0.97284

Since, for determination of face-centered crystal , the whole number

ratios comes out to be

FCC:-

3 : 4 : 8 : 11 : 12 : 16 : 19

Therefore we conclude that the structure of

sample-3

face-centered cubic (FCC)

within the limits of

experimental error

13 | P a g e

T H A PA R U N I V E R S I T Y

crystal

is a