Experiment #2: Determinaton of the structure of NaCl Powder

Ahmad Moh. Awadallah -9100030 Advanced physics lab-0352712

1

Abstract
In this work, we had examined the structure of the NaCl powder sample. For this purpose, we
prepared our sample by grinding a small amount of salt via an agate mortar and pestle until
reaching to a very fine powder could be reached. Then we pressed a small amount of NaCl into the
sample holder. The prepared sample then was studied through the XRD machine, where the used x-
rays are Cu-K (=1.5406) and Cu-K2 (=1.5444). The x-ray diffraction pattern was then
treated by the Origin 9 software, and the result was presented in this report. The figures of the fitted
peaks were sited at the appendix.

1. Introduction
The cubic system is one of the most important crystallite systems, it is a wide spread system in the
nature. It was naturally divided into three types of cubes: the simple cubic (sc), the body centered
cubic (bcc), and the face centered cubic (fcc). A lot of crystals were composed from interpenetrating
two of the three basic structures. One of the most important examples of this composition is the
diamond; it is two interpenetrated face centered cubes one shifted from the origin by quarter
diagonal in the direction of the diagonal. The two fcc lattices were filled by a carbon (C) atom at the
corners and faces. In this study, the NaCl structure composed from two fcc sub lattices, the 1
st
one
with Na
+
basis, and the other one is Cl
-
basis, they were shifted through the diagonal by a half
diagonal in which the corner of the Na sublattice is at the origin of the Cl sublattice. The main
object in this job is to calculate the lattice parameter (a), the crystallite size (D). They was
calculated and then compared with the Published ones. The intensities of the peaks were calculated
and compared with the experimental (fitted) ones. The differences were explained due to the texture
of the cells, they prefer to be ordered in a certain direction because of its cubic design.
In general, the following formulae are used in such a study:
To calculate the lattice parameter (a):
4sin
2

2
=

2
+
2
+
2

2


To calculate the crystallite size (D): =
0.94
(2)cos ()

Where B(2): the full width at half maximum (FWHM).

To calculate the intensity of a peak:

=
||
2
()
1000


Where F: structure factor

() = (

(++)
)[1 +
(+)
+
(+)
+
(+)
]

() = {
4(

) , ,
4(

) , ,
0 , ,
}
Eqn. 1.1
Eqn. 1.2
Eqn. 1.3
Eqn. 1.4
Eqn. 1.5
Experiment #2: Determinaton of the structure of NaCl Powder
Ahmad Moh. Awadallah -9100030 Advanced physics lab-0352712
2

m: multiplicity of the indices.
LP (): Lorentz polarization factor () =
1+
2
2
.2


2. Experimental
Natural salt was grinded very well for an enough time to get a fine powder using agate mortar and
pestle, the fine powder then was pressed into the sample holder of 2cm diameter inside the x-ray
machine. The thickness of the powder is about 2mm with a flat surface. The x-ray diffraction
pattern was obtained in an angular position (2) range 20.00

to 120.00

with 0.02 step between

each two succession channels. Then these collected data had been analyzed. The x-ray machine
does not contain a filter for Cu-K2, so it will be in consideration that the peaks are formed from a
super position from both Cu-K1 and Cu-K2. The diffraction pattern was studied and the
intensities of the peaks were analyzed using ORIGIN 9.0.0 software. I had fitted the peaks using the
Gaussian distribution function. The splitted peaks were fitted through a multipeaks fitting routine to
ensure taking in consideration the intensity of peak due to the Cu-K2 rays.

3. Results and Discussion
a. Fig.1 shows the XRD pattern for powdered NaCl, we can see clearly that there are some
SATELLITES appeared through the pattern, which indicates for the odd (hkl) of these
peaks; because the negative sign in (F) formula lowers the value of (F), and
correspondingly the value of the intensity.














Fig.1: XRD paterns for the NaCl sample
Eqn. 1.6
Experiment #2: Determinaton of the structure of NaCl Powder
Ahmad Moh. Awadallah -9100030 Advanced physics lab-0352712
3

The peak positions were determined using the Gaussian fitting, and they were listed at table 3.1.
The d-spacing for the different reflections were calculated using Braggs law:
(2d sin =m) [m=1 for the first order reflection] [2dsin=]
and the results were tabulated in the same table. In order to get the indices for all peaks, we
calculated the ratio between sin and sin

; we found that the common value that makes all the

ratios (
sin
sin

)
2
are integers when multiplied by it is (3) because these ration are integers, one third
of an integer, or two thirds of an integer. The values of these ratios multiplied by 3 and the indices
of each peak correspond to them were also included in table 3.1.Then the values of the indices were
used to obtain the lattice parameter (a) using the relation:
1

2
=

2
+
2
+
2

2


and recorded at the same table. We calculated to compare it with the recorded value.
To find the error in calculating (a):
=

2sin

=

2sin(+)

[for =13.70, =0.02, =1.5406 = 3.252 ,

= 3.248 d=0.004]
= (
2
+
2
+
2
)
1
2

= (0.001)
(d=3.252,(1,1,1)) a=5.633 = 5.633 0.001 = 0.006

Peak
#
Position (2) d+d()
(
sin
sin

)
2
3(
sin
sin

)
2

(, , ) +()
1 27.410.02 3.2500.004 1.000 3 (1,1,1) 5.6290.006
2 31.760.02 2.8140.004 1.334 4 (2,0,0) 5.6280.006
3 45.510.02 1.9910.004 2.666 8 (2,2,0) 5.6300.006
4 53.940.02 1.6980.004 3.664 11 (3,1,1) 5.6310.006
5 56.550.02 1.6260.004 3.997 12 (2,2,2) 5.6310.006
6 66.270.02 1.4090.004 5.323 16 (4,0,0) 4.8800.006
7 73.090.02 1.2930.004 6.317 19 (3,3,1) 5.6370.006
8 75.320.02 1.2600.004 6.651 20 (4,2,0) 5.6360.006
9 84.020.02 1.1500.004 7.980 24 (4,2,2) 5.6360.006
10 90.450.02 1.0850.004 8.977 27 (3,3,3) 5.6360.006
= 5.557 0.006
Table 3.1: Position against d-spacing and lattice parameter.


Experiment #2: Determinaton of the structure of NaCl Powder
Ahmad Moh. Awadallah -9100030 Advanced physics lab-0352712
4

The recorded (real) value of the lattice parameter (a) is: 5.639
The percentage error in calculating (a) is:
. =
|

100% =
|5.639 5.557|
5.639
100% = 1.454%
This small value of P.E indicates how accurate our calculation of lattice parameter is.

b. Using the Origin fitting routine, we found the B (): Full widths at Half Maximum
(FWHM), these values were sited in table 3.2. The crystallite size (D) was calculated
depending on the value of B () through the equation:

=
0.94
(2)cos ()

and tabulated in the same table against the position 2.
Peak # Position (2) FWHM (2) Crystal size (D)
1 27.410.02 0.004 358.7
2 31.760.02 0.004 393.7
3 45.510.02 0.004 384.4
4 53.940.02 0.005 353.9
5 56.550.02 0.005 348.8
6 66.270.02 0.002 712.6
7 73.090.02 0.003 583.3
8 75.320.02 0.003 563.4
9 84.020.02 0.003 563.9
10 90.450.02 0.004 547.9
D (average)=367.9
Table 3.2: the values of FWHM and crystal size with position
The crystallite size is very small; it is in the nano scale; the value of the crystallite size was of the
magnitude of 350. The uncertainty in calculating D was very small and could without loss of
accuracy- be ignored.

c. The last part of our work was to calculate the intensity. The intensity was calculated from
eqn.1.3. For this aim, we calculated the multiplicity (m) and put it in table 3.3, then we
found the value of the structure factor (F) for each position through eqn.1.5, we used the
standard values of the constants a
i
, b
i
, and c from the tables at internet. The atomic form
factor for each ion (Na and Cl) at each position was calculated using the following formula:
(

) =

(/)
2
)
4
=1
+
Experiment #2: Determinaton of the structure of NaCl Powder
Ahmad Moh. Awadallah -9100030 Advanced physics lab-0352712
5

The values of (F) were inserted into table 3.3 too. Then I had evaluated the Lorentz Polarization
Factor (LP) using eqn.1.6, I put these values at table 3.3 to complete the required parameters to find
the intensity.
Peak # 2 f
Na
f
Cl

Structure
factor (F)
|
2
|
Multiplicity
(m)
LP()

1 27.41 8.965 13.46 -17.99 323.6 8 16.38 42.42
2 31.76 8.639 12.68 85.26 7269 6 11.96 521.4
3 45.51 7.609 10.61 72.88 5311 12 5.40 344.1
4 53.94 6.973 9.687 -10.86 117.9 24 3.67 10.39
5 56.55 6.765 9.432 64.79 4197 8 3.30 110.7
6 66.27 6.084 8.711 59.18 3502 6 2.32 48.76
7 73.09 5.641 8.320 -10.72 114.8 24 1.90 5.242
8 75.32 5.508 8.211 54.87 3011 24 1.80 130.0
9 84.02 5.024 7.840 51.45 2648 24 1.52 96.45
10 90.45 4.716 7.606 -11.56 133.7 8 1.41 1.506
Table 3.3: calculated structure factor, multiplicity, LP, and corresponding intensity.
The error in calculating structure Factor is coming only from reading the value of atomic form
factor (f) which is very negligible. The error in calculating LP is also very small.

To compare our experimental values of intensity that obtained from the fitting routine with the
calculated ones, I normalized the calculated intensities to the second peak because it is the larger
one, and so I did for the experimental values of the intensity, then I put it in table 3.4.
Peak # 2 (, , )

()

()
Percentage error (P.E)
|
(

100%|
1 27.41 (1,1,1) 42.42 8.1% 272.0 5.0% 38%
2 31.76 (2,0,0) 521.4 100.0% 5394 100.0% 0%
3 45.51 (2,2,0) 344.1 66.0% 1840 34.1% 48%
4 53.94 (3,1,1) 10.39 2.0% 71.59 1.3% 33%
5 56.55 (2,2,2) 110.7 21.2% 500.3 9.3% 56%
6 66.27 (4,0,0) 48.76 9.4% 429.5 8.0% 15%
7 73.09 (3,3,1) 5.242 1.0% 28.06 0.5% 48%
8 75.32 (4,2,0) 130.0 24.9% 568.8 10.5% 58%
9 84.02 (4,2,2) 96.45 18.5% 367.3 6.8% 63%
10 90.45 (3,3,3) 1.506 0.3% 31.33 0.6% 101%
Table 3.4: Calculated and experimental intensities.
The difference between the normalized calculated intensities and the experimental ones are large,
and that may be for several reasons. One of them is due to the cubic structure of our sample, the
cells prefer to stack on its faces rather than the other directions, so the texture make the intensity for
the some peaks be at a great difference from the calculated one. Another one which is well-known
as: EXTINCTION. Extinction may be due to crystal structure which in our case cancel out the
mixed indices peaks- or rather is related to a phase-shifted reflection; which can occur from the
Experiment #2: Determinaton of the structure of NaCl Powder
Ahmad Moh. Awadallah -9100030 Advanced physics lab-0352712
6

underside of very strongly reflecting planes. Directed towards the incident beam but always 180
out of phase with it, the net effect is to reduce the intensity of the incident beam, and secondarily
the intensity of the diffraction from that plane. Another reason that make this big difference
between calculated and experimental intensities is that the error in reading the integrated intensity
from the fitting routine. In addition, one can get very different normalized intensities if he
normalizes the peaks to another one than the second. Our calculated intensities are close to some of
the recorded patterns, fig.2 shows one of them. One source of error in my work is due to use
1
in
calculating instead of

for the


4. Conclusions
From the XRD pattern, we can decide that the structure of NaCl is fcc structure because all the
peaks of the fcc were appeared. The difference between f
Na
and f
Cl
allowed the satellites to appear.
The lattice parameter were calculated and found to be: = (5.557 0.006). The crystallite size
was obtained and has the order of 350; it was increased when calculated from the last peaks due
to the broadening of the peaks causing the broadening in the crystallite size. The experimental
intensities of the peaks are different from the calculated ones due to the extinction due to the phase-
shifted reflection, and the non-filtered Cu-Kbeam in the x-ray machine.


Fig.2: A recorded XRD pattern for NaCl powder