Experiment #1: Determination of the structure of Iron Metal Powder

Ahmad Moh. Awadallah -9100030 Advanced physics lab-0352712

Procedure:

 The sample was prepared using powder of Iron metal which was stuck on a substrate
using double-scotch tape.

 Then the sample was examined using the XRD machine, and the XRD pattern was
obtained for our sample for 2θ from 40ο to 120ο using x-ray source with λ=1.54Å.

 The obtained data were plot using OriginPro 9.0.0, and the result was as follows:

Peak # 1
Intensity

Peak # 3
Peak # 2 Peaks # 5, 6

Peak # 4
 Experiment #1: Determination of the structure of Iron Metal Powder
Ahmad Moh. Awadallah -9100030 Advanced physics lab-0352712

Data Analysis:
1.

Peak # Position (2θ) Width of each peak (W) FWHM

1 44.85 0.21 0.243
2 65.21 0.27 0.318
3 82.53 0.34 0.405
4 99.14 0.44 0.515
5 116.5 0.63 0.747
 Experiment #1: Determination of the structure of Iron Metal Powder
Ahmad Moh. Awadallah -9100030 Advanced physics lab-0352712

2. ( 2dsinθ=mλ ) [m=1 for the first order reflection] [ 2dsinθ=λ ]

𝜆
𝑑=
2 sin 𝜃

Peak # Position (2θ) Angle (θ) Sin(θ) d-spacing

1 44.85 22.425 0.381619 2.017717308
2 65.21 32.605 0.539037 1.428472739
3 82.53 41.265 0.65976 1.167090192
4 99.14 49.57 0.761425 1.011262266
5 116.5 58.25 0.850567 0.905277966

3.

sin 𝜃 2
Peak # Position (2θ) Angle (θ) Sin(θ) d-spacing ( )
sin 𝜃𝜊
1 44.85 22.425 0.381619 2.017717308 1.00
2 65.21 32.605 0.539037 1.428472739 2.00
3 82.53 41.265 0.65976 1.167090192 2.99≅3.00
4 99.14 49.57 0.761425 1.011262266 3.98≅4.00
5 116.5 58.25 0.850567 0.905277966 4.97≅5.00

4 sin 𝜃2 ℎ 2 +𝑘 2 +𝑙2 sin 𝜃 2 ℎ 2 +𝑘 2 +𝑙 2

Equ.9 says that: = =
𝜆2 𝑎2 sin 𝜃𝜊 2 ℎ𝜊 2 +𝑘𝑜 2 +𝑙𝜊 2

The ratio between sin2θ and sin2θο is equal to the ratio between the sums of the squared indices.
From the table,
sin 𝜃 2
( ) is equal to integers, so (ℎ2 + 𝑘 2 + 𝑙 2 ) is equal to (ℎ𝜊 2 + 𝑘𝑜 2 + 𝑙𝜊 2 ) multiplied by some
sin 𝜃𝜊
integer.

If we multiply this ratio by the integer which is equal to (ℎ𝜊 2 + 𝑘𝑜 2 + 𝑙𝜊 2 ), we can get directly
the quantity: (ℎ2 + 𝑘 2 + 𝑙 2 ) which will lead us to know ℎ, 𝑘, 𝑎𝑛𝑑 𝑙.
 Experiment #1: Determination of the structure of Iron Metal Powder
Ahmad Moh. Awadallah -9100030 Advanced physics lab-0352712

4. The structure is bcc, so the smallest appropriate common multiplier for our ratios is: 2.
2 will make the 1st ratio to be 2, and so the ℎ, 𝑘, 𝑎𝑛𝑑 𝑙 will be (1, 1, 0) which is the 1st
index for our peaks, and we can insure that (ℎ2 + 𝑘 2 + 𝑙 2 ) =even as per bcc structure
has to be. [ ℎ𝜊 2 + 𝑘𝑜 2 + 𝑙𝜊 2 = 2 ]

Peak Position Angle d-spacing sin 𝜃 2 sin 𝜃 2

# (2θ) (θ)
Sin(θ)
(Å) ( ) (ℎ2 + 𝑘 2 + 𝑙 2 ) = 2 ( ) (ℎ, 𝑘, 𝑙)
sin 𝜃𝜊 sin 𝜃𝜊
1 44.85 22.425 0.382 2.018 1.00 2 (1,1,0)
2 65.21 32.605 0.539 1.428 2.00 4 (2,0,0)
3 82.53 41.265 0.660 1.167 2.99≅3.00 6 (2,1,1)
4 99.14 49.57 0.761 1.011 3.98≅4.00 8 (2,2,0)
5 116.5 58.25 0.851 0.905 4.97≅5.00 10 (3,1,0)

1 ℎ 2 +𝑘 2 +𝑙2
5. 𝑑2
= 𝑎2
equ.9

Peak d-spacing sin 𝜃 2

# (Å) (ℎ2 + 𝑘 2 + 𝑙 2 ) = 2 ( ) (ℎ, 𝑘, 𝑙) a (Å)
sin 𝜃𝜊
1 2.018 2 (1,1,0) 2.853
2 1.428 4 (2,0,0) 2.857
3 1.167 6 (2,1,1) 2.859
4 1.011 8 (2,2,0) 2.860
5 0.905 10 (3,1,0) 2.863
aav = 2.858

6. [a (standard)] = 2.866 Å while our [a (average)] = 2.858 Å which is very close to the
standard one.
This light difference could be come from many experimental and analytical uncertainties’
such as:
1. The sample may not be prepared correctly for the XRD, so there may be some
empty areas at the scotch tape where the sample was stuck.
2. May be there is a little bit difference between the used Iron metal powder in our
sample and which used at the standard.
3. The substrate where the sample was put may not be as flat as should be, so there
is a little deviation inside the XRD machine which caused a small shift in the
positions of the peaks.
4. May be there is a personal error from the XRD man in putting the sample inside
the XRD machine.
5. Some uncertainties may appear through the fitting process of the peaks.
Choosing a not appropriate function to fit the peaks may affect the value of the
lattice constant (a). [Gaussian instead of Lorantzian or vice averse]
6. Some iteration through calculations may cause a little bit of uncertainty.
7. The personal error of the student himself through the whole process of treatment
may cause some difference from the standard value.
 Experiment #1: Determination of the structure of Iron Metal Powder
Ahmad Moh. Awadallah -9100030 Advanced physics lab-0352712

7. The crystal size (D) can be determined from Scherrer’s equation:

0.94𝜆
𝐷=
𝐵(2𝜃)cos(𝜃)
Where 𝐵(2𝜃) is the Full Width at Half Maximum (FWHM) of the diffraction peak line.

Peak # Position (2θ) cos(θ) FWHM≡ 𝐵(2𝜃) Crystal size (D) (nm)
1 44.85 0.924 0.004 36.924
2 65.21 0.842 0.006 30.956
3 82.53 0.751 0.007 27.234
4 99.14 0.648 0.009 24.834
5 116.5 0.526 0.013 21.093
D (average) 28.208

The crystallite size is in nano scale. As we saw, we calculate d the size if the crystal using a very
basic information from the XRD pattern. We can see clearly that the crystal size was decreased
when calculated from the later peaks; D is biggest from the 1st peak, then decreased until reaching
the final peak where D is minimum, and that’s appear normally because of the dependence of D
on the position of the peaks (2θ). One can calculate the volume of the crystal which is≈ 𝐷 3.
𝐷
 = 98.698 which give an idea about how many cubic cell in the side if the crystal.
𝑎

𝑠𝑖𝑛𝜃
8. 𝑓 ( 𝜆
) = ∑4𝑖=1 𝑎𝑖 𝑒 −(𝑏𝑖𝑠𝑖𝑛𝜃/𝜆) + 𝑐 [a, b, and c are parameters that can be obtained
from net]

Peak # Position (2θ) Sin(θ) FWHM≡ 𝐵(2𝜃) Crystal size (D) (nm) Atomic form factor
1 44.85 0.382 0.004 36.924 11.271
2 65.21 0.539 0.006 30.956 9.042
3 82.53 0.660 0.007 27.234 8.453
4 99.14 0.761 0.009 24.834 8.273
5 116.5 0.851 0.013 21.093 8.197

9. LP(θ): Lorentz Polarization factor

1 + 𝑐𝑜𝑠 2 2𝜃
𝐿𝑃(𝜃) =
𝑠𝑖𝑛𝜃. 𝑠𝑖𝑛2𝜃
Peak # Sin(θ) Sin2θ Cos22θ FWHM≡ 𝐵(2𝜃) Crystal size Atomic form Multiplicity
LP(θ) (ℎ, 𝑘, 𝑙)
(D) (nm) factor (m)
1 0.382 0.705 0.502 0.004 36.924 11.271 5.580 (1,1,0) 12
2 0.539 0.908 0.175 0.006 30.956 9.042 2.401 (2,0,0) 6
3 0.660 0.992 0.017 0.007 27.234 8.453 1.554 (2,1,1) 24
4 0.761 0.987 0.025 0.009 24.834 8.273 1.364 (2,2,0) 12
5 0.851 0.895 0.200 0.013 21.093 8.197 1.577 (3,1,0) 24
 Experiment #1: Determination of the structure of Iron Metal Powder
Ahmad Moh. Awadallah -9100030 Advanced physics lab-0352712

10. The calculated intensity (𝐼𝑐𝑎𝑙 ) is determined through the equation:

|𝐹|2 𝑚(𝐿𝑃)
(𝐼𝑐𝑎𝑙 = 1000
)

Peak # Crystal size (f) Atomic Multiplicity Structure

LP(θ) (ℎ, 𝑘, 𝑙) |𝐹 2 | 𝐼𝑐𝑎𝑙
(D) (nm) form factor (m) factor (F)
1 36.924 11.271 5.580 (1,1,0) 12 22.542 508.133 34.025
2 30.956 9.042 2.401 (2,0,0) 6 18.084 327.039 4.712
3 27.234 8.453 1.554 (2,1,1) 24 16.906 285.826 10.661
4 24.834 8.273 1.364 (2,2,0) 12 16.547 273.789 4.482
5 21.093 8.197 1.577 (3,1,0) 24 16.395 268.791 10.172

Where 𝐹 (𝑏𝑐𝑐) = 𝑓[1 + 𝑒 𝜋𝑖(ℎ+𝑘+𝑙) ]

11. From the fitting, the integrated intensities for the experimental peaks are: 𝐼𝑒𝑥𝑝

Peak # Percentage error

(ℎ, 𝑘, 𝑙) 𝐼𝑐𝑎𝑙 𝐼𝑒𝑥𝑝 𝐼𝑒𝑥𝑝 (𝑛𝑜𝑟𝑚𝑎𝑙𝑖𝑧𝑒𝑑) (𝐼𝑐𝑎𝑙 − 𝐼𝑒𝑥𝑝
| × 100%|
𝐼𝑐𝑎𝑙
1 (1,1,0) 34.025 330.462 34.025 0
2 (2,0,0) 4.712 79.607 8.196 73.938
3 (2,1,1) 10.661 129.271 13.310 24.844
4 (2,2,0) 4.482 40.708 4.191 6.487
5 (3,1,0) 10.172 122.217 12.584 23.713

Peak # (ℎ, 𝑘, 𝑙) 𝐼𝑐𝑎𝑙 /𝐼𝑐𝑎𝑙 (max) 𝐼𝑒𝑥𝑝 /𝐼𝑒𝑥𝑝 (max)

1 (1,1,0) 1 1
2 (2,0,0) 0.138 0.241
3 (2,1,1) 0.313 0.391
4 (2,2,0) 0.132 0.123
5 (3,1,0) 0.299 0.370