Michael Carton

11352077
MTE 481: Analytical Methods for Materials

Lab 3: X-Ray Diffraction and Peak Indexing

Date of Experiment: 11/13/2014

Submission Date: 12/01/2014
Instructor: Dr. Jinhui Song
TA: Chaolong Tang

2
Abstract
The purpose of this experiment was to record the diffraction spectra for various samples
and to index their peaks using mathematical and analytical methods. These methods use a
combination of Braggs law and the plane spacing equations in order to determine the lattice
parameters.1 A sample of nickel with a cubic structure and a sample of titanium with a hexagonal
structure were analyzed. The peak values, cubic structures, and lattice parameters determined by
the mathematical and analytical methods agree with each other and with the ICDD values
confirming that the materials indexed were FCC nickel and HCP titanium.

3
Experimental Apparatus and Procedure
To begin the experiment a sample of pure nickel powder was acquired and placed in a
sample holder. The Ni powder and holder was loaded into the chamber of the Philips MPD XRD
machine. The doors were closed and secured and chiller checked to ensure that cool water was
running through the system. The operating computer was turned on and the Data Collector
program on the desktop was opened.
Once the program was opened, the software was connected to the hardware by clicking
Instrument then Connect and then OK. The Tension button was clicked and the voltage
and current were changed to 45kV/40mA. Test program 4 was run by selecting File Open
Program Test program 4. The start angle was set to 20, the end angle to 100, and the step
size to 0.05/step. The program was initiated by clicking Measure Program and giving the
file a unique name.
Once initiated, the shutter opened and scanned the sample according to the parameters set
in program 4. When the scan was complete, the shutter opened and the sample was removed
from the chamber. The data points from the scan were automatically saved by the computer and
exported to a .XRDML file.
To shut tool down, the voltage and current were reset to 30kV/10mA under the Tension
button on the program interface. The hardware was disconnected by clicking Instrument
Disconnect. The .XRDML file was converted to a .ASC file to be read by Excel and plotted.
The same procedure was repeated for the titanium powder. Standard XRD peak files
(ICDD) for both nickel and titanium samples were pulled for comparison. All of the peaks for
both samples were indexed using mathematical and analytical methods.

4
Results and Discussion
Once the data was collected, it was plotted in Excel. The Nickel sample was analyzed
first and its peaks can be seen below in Figure 1.

Figure 1: Experimentally obtained XRD peaks for the Nickel sample

As seen above, there are five distinct peaks between the 2 values of 20 and 100.
These values and their relative intensities are recorded in Table I below.
Table I: Peaks from the Nickel sample and their relative intensities
Normalized Intensity
Angle Intensity
100
44.56
15630
30.8
51.88
4820
12.4
76.38
1940
8.83
92.90
1380
2.94
98.30
460

Next, the each of the peaks of the Nickel sample was indexed using both analytical and
mathematical methods. Following the methods learned in class, Tables II IV below were
constructed and used to determine the crystal structure and lattice parameter of the Nickel.

Table II. Mathematical method for determining the lattice parameter and structure of a cubic material
Peak
No.
1
2
3
4
5

sin()

sin()^2

44.56
51.88
76.38
92.90
98.30

0.38
0.44
0.62
0.72
0.76

0.14
0.19
0.38
0.53
0.57

1*sin()^2/
sin(min)^2
1.00
1.33
2.66
3.65
3.98

2*sin()^2/
sin(min)^2
2.00
2.66
5.32
7.31
7.96

3*sin()^2/
sin(min)^2
3.00
3.99
7.98
10.96
11.94

(h^2)+(k^2)+(l^2)
3.00
4.00
8.00
11.00
12.00

hkl

a (angstroms)

111
200
220
311
222
Average:

3.52
3.52
3.52
3.52
3.53
3.52

Table III. Analytical method for determining the K value for a cubic material
Peak
No.
1
2
3
4
5

sin()

sin()^2

sin()^2/2

44.56
51.88
76.38
92.90
98.30

0.37913
0.43743
0.61827
0.72477
0.75642

0.14374
0.19134
0.38226
0.52530
0.57218

0.07187
0.09567
0.19113
0.26265
0.28609

sin()^2/3 sin()^2/4 sin()^2/5 sin()^2/6

0.04791
0.06378
0.12742
0.17510
0.19073

0.03594
0.04784
0.09556
0.13132
0.14304

0.02875
0.03827
0.07645
0.10506
0.11444

0.02396
0.03189
0.06371
0.08755
0.09536

sin()^2/7

sin()^2/8

0.02053
0.02733
0.05461
0.07504
0.08174

0.01797
0.02392
0.04778
0.06566
0.07152

K = 0.04784
Table IV. Analytical method for determining the lattice parameter and structure of a cubic material
Peak
No.
1
2
3
4
5

(rad)

sin()

44.56
51.88
76.38
92.90
98.30

22.28
25.94
38.19
46.45
49.15

0.39
0.45
0.67
0.81
0.86

0.38
0.44
0.62
0.72
0.76

sin()^
2
0.14
0.19
0.38
0.53
0.57

sin()^2/
K
3.00
4.00
7.99
10.98
11.96

(h^2)+(k^2)+(l^2)

hkl

a (angstroms)

3.00
4.00
8.00
11.00
12.00

111
200
220
311
222

3.52
3.52
3.52
3.52
3.52

These methods depend on the plane spacing equations and Braggs law in order to
determine the crystal structures and lattice parameters. Specifically, these equations can be
2

combined to make the relationship: 2 () = (42 )(2 + 2 + 2 ). This equation can then be
solved either mathematically or analytically.2

As seen in Table II, the h2+k2+l2 for each peak from the mathematical model are 3, 4, 8,
11, and 12. This indicates that the nickel has a face-centered cubic (FCC) structure.3 The lattice
parameter was also calculated and found to be 3.52 .
Analytical methods were also used to confirm the crystal structure of the nickel. As seen
in Table IV, the h2+k2+l2 for each peak from the analytical method are 3, 4, 8, 11, and 12. This
agrees with the mathematical model and also indicates that nickel has an FCC structure.3 The
lattice parameter was once again calculated and found to be 3.52 which also agrees with the
mathematical model. The value of these lattice parameters are very close to the ICDD value for
nickel which is 3.54 . The ICDD data card is attached at the end of the report.
Overall, the peak angles, the FCC structure, and lattice parameter from both the
mathematical and analytical methods of indexing the peaks confirm that the material is in fact
nickel.

7
Next, the experimental spectrum data for the titanium sample was plotted in Excel. This
can be seen below in Figure 2.

Figure 2: Experimentally obtained XRD peaks for the Titanium sample

As seen above, there are eleven clear peaks between the 2 values of 20 and 100.
These values and their relative intensities are recorded in Table V below.
Table V: Peaks from the titanium sample and their relative intensities
Normalized Intensity
Angle Intensity
22.5
34.96
625
30.1
38.30
835
100
40.06
2770
13.7
52.86
380
13.7
62.78
380
14.1
70.52
390
13.0
76.08
360
10.5
77.20
290
3.25
82.16
90
2.89
86.60
80
2.52
92.64
70

These peaks are very close to the expected ICDD peaks and were indexed using the
mathematical method in order to determine the crystal structure and lattice parameters. For
hexagonal structures, Braggs law can be combined with the plane spacing equations to get the

8
2

following relationship: 2 () = 42 [3 (2 + + 2 ] + (
be used to determine c and a, which are the lattice parameters.
First determine the possible values of

4
3

). This relationship can then

[2 + + 2 ] using all of the possibilities for h

and k. These values can be seen below in Table VI.

Table VI: Values for

4
3

[2 + + 2 ] for all possible values of h and k

k

0
0.000
1.333
5.333
12.000

0
1
2
3

Next, the possible values of

( )2

1
1.333
4.000
9.333
17.333

2
5.333
9.333
16.000
25.333

3
12.000
17.333
25.333
36.000

were determined for all possible values of l and using the

lattice parameter ratio (c/a) of 1.5871. These are below in Table VII.
Table VII: Values for
l
0
1
2
3
4
5
6

( )2

for all values of l and c/a = 1.5871

l^2
0
1
4
9
16
25
36

l^2/(c/a)^2
0.000
0.397
1.588
3.573
6.352
9.925
14.292
4

Then the solutions from Tables VI and VII were used to determine the 3 [2 + +

2] + (

) for every allowed hkl value. These were placed in order from smallest to largest in

Table VIII.

9
4

Table VIII: All allowed hkl values and corresponding 3 [2 + + 2 ] + (

hkl
100
002
101
102
110
103
200
112
201
004
202
104
203
210
211
114
212
105
204
300
213
302
006
205
106

value
1.333
1.588
1.73
2.921
4.000
4.906
5.333
5.588
5.73
6.352
6.921
7.685
8.906
9.333
9.73
10.352
10.921
11.258
11.685
12.000
12.906
13.588
14.292
15.258
16.625

) values.

This order of hkl values was then used to assign indices to the peaks from the diffraction
pattern. The a values for the hk0 type reflections was calculates and the c values for the 00l type
reflections were calculated. These values were averaged in order to determine the a, c and c/a
values. This can all be seen below in Table IX.

10
Table IX: Calculations of the c and a lattice parameters for the experimental spectrum
Peak
No.
1
2
3
4
5
6
7
8
9
10
11

2
34.96
38.3
40.06
52.86
62.78
70.52
76.08
77.2
82.16
86.6
92.64

Relative
d
sin()^2
hkl
Intensity
(nm)
22.5
0.0902 2.563 100
30.1
0.1076 2.347 002
100
0.1173 2.248 101
13.7
0.1981 1.730 102
13.7
0.2713 1.478 110
14.1
0.3333 1.334 103
13
0.3797 1.250 200
10.5
0.3892 1.234 112
3.25
0.4318 1.172 201
2.89
0.4703 1.123 004
2.52
0.5230 1.065 202

a()

c ()

2.960

(h^2)+hk+(k^2)

l^2

1
4.695

2.957

2.886

4.491

16

As seen in the table above the average values for a is 2.934 , the average value for c is
4.593 , and the average value for c/a is 1.565. These are close to the ICDD values for titanium
which are a = 2.951 , c = 4.670 , c/a = 1.583.
Summary and Conclusions
In conclusion, the experimental spectra of the nickel and titanium match the expected
spectra according to the ICDD data. The mathematical and analytical methods of indexing the
spectra agree with each other and result in crystal structures and lattice parameters that also agree
with the expected results. The experimental results indicate the nickel has an FCC structure and
the titanium has an HCP structure. The experimental value for the lattice parameter of nickel is
3.52 which is very close to the ICDD value of 3.54 . The experimental values for titaniums
lattice parameters are: a = 2.934 , c = 4.593 , c/a = 1.565 which is very close to the ICDD
values of: a = 2.951 , c = 4.670 , c/a = 1.583. The small variations can be accounted for by
the different systems used to generate the spectra and slight rounding errors.

11
References
1. Callister, William D., Rethwisch, David G, Fundamentals of Materials Science and
Engineering, 3rd Ed., John Wiley and Sons, Inc., Hoboken, NJ, 2008
2. Suryanarayana, C., Experimental Techniques in Materials and Mechanics, Taylor & Francis
Group, Boca Raton, FL, 2011
3. Leng, Yang, Materials Characterization: Introduction to Microscopic and Spectroscopic
Methods, John Wiley & Sons, Ltd., Hoboken NJ, 2008

Nov 13, 2014 5:56 PM (CAF User)

00-001-1258

Status Deleted
QM: Blank
Pressure/Temperature: Ambient
Chemical Formula: Ni
Weight %: Ni100.00
Atomic %: Ni100.00
Compound Name: Nickel
Radiation: MoK

Empirical Formula: Ni

0.7093

SYS: Cubic
SPGR: Fm-3m (225)
Author's Cell [ AuthCell a: 3.54
AuthCell Vol: 44.36
AuthCell Z: 2.00
AuthCell MolVol: 22.18 ]
Density [ Dcalc: 4.394g/cm
Dmeas: 8.72g/cm ]
SS/FOM: F(12) = 7.9(0.117, 13)
Temp: 298.000K (Ambient temperature assigned by ICDD editor)
Melting Point: 1728 K
Space Group: Fm-3m (225)
Molecular Weight: 58.70
Crystal Data [ XtlCell a: 3.540
XtlCell b: 3.540
XtlCell c: 3.540
XtlCell : 90.00
XtlCell : 90.00
XtlCell : 90.00
XtlCell Vol: 44.36
XtlCell Z: 2.00 ]
Crystal Data Axial Ratio [ a/b: 1.000
c/b: 1.000 ]
Reduced Cell [ RedCell a: 2.503
RedCell b: 2.503
RedCell c: 2.503
RedCell : 60.00
RedCell : 60.00
RedCell : 60.00
RedCell Vol: 11.09 ]
Crystal (Symmetry Allowed): Centrosymmetric
Pearson: cF2.00
Subfile(s): Common Phase, Forensic, Inorganic, Deleted Pattern, Metals & Alloys
Last Modification Date: 01/11/2013
Cross-Ref PDF #'s: 04-001-0091 (Alternate)
References:
Type
Primary Reference
Optical Data
Unit Cell

DOI

Reference
Hull. Phys. Rev. 17, 571 (1921).
Data on Chem. for Cer. Use, Natl. Res. Council Bull. 107.
The Structure of Crystals, 1st Ed.

Database Comments: Color: White. Deleted Or Rejected By: Deleted by NBS card. Melting Point: 1728 K.
d-Spacings (8) - 00-001-1258 (Fixed Slit Intensity) - Cu K(Avg) 1.54184
2
d()
I
h k l *
2
d()
I
h k
44.4076
92.1892
3 1
2.040000 100 1 1 1
1.070000 60
51.6403
2 0 0
98.1913
1.020000 10
2 2
1.770000 50
76.1563
1.250000 40
2 2 0
122.3379 0.880000 2
4 0

l
1
2
0

2014 International Centre for Diffraction Data. All rights reserved.

2
144.2592
154.7640

d()
0.810000
0.790000

I
20
16

h
3
4

k
3
2

l
1
0

Page 1 / 1

Nov 13, 2014 3:29 PM (CAF User)

00-001-1197

Status Deleted
QM: Blank
Pressure/Temperature: Ambient
Chemical Formula: Ti
Weight %: Ti100.00
Atomic %: Ti100.00
Compound Name: Titanium
Radiation: MoK

Empirical Formula: Ti

0.7093

SYS: Hexagonal
SPGR: P63/mmc (194)
Author's Cell [ AuthCell a: 2.951
AuthCell c: 4.67
AuthCell Vol: 35.22
AuthCell Z: 2.00
AuthCell MolVol: 17.61 ]
Author's Cell Axial Ratio [ c/a: 1.583 ]
Density [ Dcalc: 4.517g/cm
Dmeas: 4.49g/cm ]
SS/FOM: F(15) = 5.1(0.162, 18)
Temp: 298.000K (Ambient temperature assigned by ICDD editor)
Melting Point: 2093 K
Space Group: P63/mmc (194)
Molecular Weight: 47.90
Crystal Data [ XtlCell a: 2.951
XtlCell b: 2.951
XtlCell c: 4.670
XtlCell : 90.00
XtlCell :
XtlCell : 120.00
XtlCell Vol: 35.22
XtlCell Z: 2.00 ]
Crystal Data Axial Ratio [ c/a: 1.583
a/b: 1.000
c/b: 1.583 ]
Reduced Cell [ RedCell a: 2.951
RedCell b: 2.951
RedCell c: 4.670
RedCell : 90.00
RedCell : 90.00
RedCell : 120.00
RedCell Vol: 35.22 ]

90.00

Atomic parameters are cross-referenced from PDF entry 04-001-8963

Crystal (Symmetry Allowed): Centrosymmetric
SG Symmetry Operators:
Seq Operator
Seq
1
x,y,z
5
2
-x,-y,-z
6
3
-y,x-y,z
7
4
y,-x+y,-z
8
Atomic Coordinates:
Atom Num Wyckoff
Ti
1
2c

Operator
-x+y,-x,z
x-y,x,-z
-y,-x,z
y,x,-z

Symmetry
-6m2

Seq
9
10
11
12
x
0.33333

Operator
x,x-y,z
-x,-x+y,-z
-x+y,y,z
x-y,-y,-z

y
0.66666

z
0.25

Seq
13
14
15
16
SOF
1.0

IDP

Operator
-x,-y,z+1/2
x,y,-z+1/2
y,-x+y,z+1/2
-y,x-y,-z+1/2

Seq
17
18
19
20

Operator
x-y,x,z+1/2
-x+y,-x,-z+1/2
y,x,z+1/2
-y,-x,-z+1/2

Seq
21
22
23
24

Operator
-x,-x+y,z+1/2
x,x-y,-z+1/2
x-y,-y,z+1/2
-x+y,y,-z+1/2

AET
12-d

Pearson: hP2.00
Subfile(s): Metals & Alloys, Inorganic, Deleted Pattern, Common Phase, Forensic, Explosive
Last Modification Date: 01/11/2013
Cross-Ref PDF #'s: 04-001-8963 (Primary)
References:
Type
Primary Reference
Crystal Structure
Optical Data
Unit Cell

DOI

Reference
Phys. Rev. 26, 56 (1925).
Crystal Structure Source: LPF.
Data on Chem. for Cer. Use, Natl. Res. Council Bull. 107.
The Structure of Crystals, 1st Ed.

Database Comments: Color: White. Deleted Or Rejected By: Deleted by NBS. Melting Point: 2093 K.
d-Spacings (15) - 00-001-1197 (Fixed Slit Intensity) - Cu K(Avg) 1.54184
2
d()
I
h k l *
2
d()
I
h k l
35.0522
1 0 0
70.2432
1 0 3
2.560000 40
1.340000 50
38.4712
2.340000 40
0 0 2
76.1563
1.250000 40
1 1 2
40.2611
77.6236
1.230000 30
2 0 1
2.240000 100 1 0 1
52.9258
1.730000 40
1 0 2
81.5851
1.180000 10
0 0 4
62.7842
1.480000 40
1 1 0
86.0363
1.130000 10
2 0 2

2014 International Centre for Diffraction Data. All rights reserved.

2
92.1892
102.2847
110.1952
113.8499
122.3379

d()
1.070000
0.990000
0.940000
0.920000
0.880000

I
20
30
30
30
10

h
1
2
2
1
1

k
0
0
1
1
0

l
4
3
1
4
5

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