Identification of NaCl Monocrystals (with X-ray unit)
Jeet Bhattacharjee, Int. PhD - 24483
August 2024
1 OBJECTIVE
1. Determine the intensity of the X-rays that are reflected by the NaCl monocrystals
with the orientations [100],[110],[111] as a function of the bragg angle.
2. Assign the reflections to the corresponding lattice planes that are given by way of
their respective Miller indices.
3. Determine the lattice constant and calculate interplanar spacing.
4. Determine the mass of a cell and the number of atoms in the cell.
2 APPARATUS
XRD unit, Goniometer, Geiger-Muller counter tube, X-ray tube, NaCl monocrystals of
orientations [100],[110],[111], crystal holder, Measure software and a Laptop.
3 THEORY
3.1 Principle
The spectra of the X-rays that are reflected with various different orientations by the NaCl
moncrystals are analysed. The associated interplanar spacings are determined based on the
Bragg angles of the characteristic lines.
3.2 Bragg’s Law
The entire experiment is characterized by the Bragg’s Law, for constructive reflected ra-
diation. The law explains the relationship between an x-ray light shooting into and its
reflection off from crystal surface.
1
The law states that when the x-ray is incident onto a crystal surface, its angle of inci-
dence, will reflect back with a same angle of scattering, when the path difference is equal
to a whole number of wavelength, a constructive interference will occur.
2dsin(θ) = nλ
where
• n = 0, 1, 2, 3, . . .
• d : interplanar spacing
• θ : glancing angle
• λ : Wavelength of the incident photon (herein, X-ray)
Figure 1: Bragg’s Law
Source: [Link]
3.3 Miller Indices
Miller indices [1] form a notation system in crystallography for lattice planes in crystal
(Bravais) lattices.
In particular, a family of lattice planes of a given (direct) Bravais lattice is determined by
three integers h, k, and l, the Miller indices. They are written (hkl), and denote the family of
(parallel) lattice planes (of the given Bravais lattice) orthogonal to ghkℓ = hb1 + kb2 + ℓb3 ,
where bi are the basis or primitive translation vectors of the reciprocal lattice for the given
Bravais lattice.
2
The lattice spacing, d is determmined by the lattice constant, a and the miller indices hkl
a
d= √
h2 + k 2 + l 2
Using the form of the Bragg’s Law, this can be expressed as
p λ
sin(θhkl ) = h2 + k 2 + l2
2a
3.4 Structure Factor
In condensed matter physics [2] and crystallography, the static structure factor (or struc-
ture factor for short) is a mathematical description of how a material scatters incident
radiation. The structure factor is a critical tool in the interpretation of scattering patterns
(interference patterns) obtained in X-ray, electron and neutron diffraction experiments.
The relative intensity of reflected radiation is determined by scattering power / atomic
factor f and position of individual atoms in unit cell of crystal. It is given by geometrical
factor F (hkl) as follows
X
F (hkl) = fn exp[−2πi(hun + kvn + lwn )]
n
where
• fn : atomic form factor
• un , vn , wn : co-ordinates of nth atom
The total back scattered intensity is given by
I = F ∗ ∗ F = |F (hkl)|2
With the co-ordinates (000), (0, 21 , 12 ), ( 12 , 0, 12 ), ( 21 , 21 , 0)
F (hkl) = 1 + eiπ(h+k) + eiπ(k+l) + eiπ(h+l)
which is non-zero when all the miller indices are either odd or even.
3.5 Crystal Structures (used in experiment)
We used monocrystals with three orientations [100],[110],[111].
(100) → F = f (1 + e−πi + 1 + e−πi ) = 0(200) → F = f (1 + 1 + 1 + 1) = 4f
3
Similarly for others.
Figure 2: The Planes
Source: [Link]
4 Procedure
1. First we will calibrate the setup using LiBr crystal
• On X-ray unit we will click on Menu
• Select Goniometer
• Select auto-calibration and switch on X-ray and then start
• Ensure that you get two peaks
2. Then switch of the X-ray and unlock the chamber and insert one of the samples
3. Open Measure software. A virtual X-ray unit will be opened on screen. We can control
X-ray unit by clicking various features and under virtual X-ray unit. Alternatively,
we can change the parameters of the unit. The program unit will automatically adopt
to the settings.
4. Click the experimental chamber to change parameter. We set the crystal type, and
the corresponding lattice parameters.
5. Settings of the goniometer as follows :-
• 2:1 coupling mode
• Scanning Range : 5◦ - 60◦
4
5 Observations
The intensity of the characteristic lines is always the highest for the order 1 reflections in
case of [100] and [110]. But in case of [111] crystal it is highest for order 2, because in
[111] the lattice planes are occupied by either N a+ or Cl− ions, and they have different
scattering factors, so intensities also differ.
For solely odd hkl indices :-
F = 4(fN a+ − fCl− ) & I ∝ |F |2 = 16 (fN a+ − fCl− )2
For solely even hkl indices :-
F = 4(fN a+ + fCl− ) & I ∝ |F |2 = 16 (fN a+ + fCl− )2
Intensity vs Bragg’s angles plot
Figure 3: The [100] Planes
5
Figure 4: The [110] Planes
Figure 5: The [111] Planes
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6 Plots and table for lattice spacing and interplanar distance
for Kα and Kβ
For [100] plane
Bragg’s Angle Interplanar Spacing Lattice Constant
(hkl) (h2 + k 2 + l2 )
(in Degrees) d (in pm) a (pm)
17.1 200 4 263.4 525.2
Kα 34.3 400 16 137.2 548.0
56.2 600 36 93.5 557.4
[100] 15.5 200 4 258.7 517.6
crystal Kβ 30.7 400 16 136.3 546.4
48.9 600 36 92.5 555.0
Mean Value 541.7 pm
For [110] plane
Bragg’s Angle Interplanar Spacing Lattice Constant
(hkl) (h2 + k 2 + l2 )
(in Degrees) (in pm) a (pm)
22.5 220 8 194.3 545.7
Kα
[110] 53.2 440 32 98.2 556.4
20.2 220 8 187.6 545.3
Kβ
crystal 44.5 440 32 99.3 552.9
Mean Value 550.2
For [111] plane
Bragg’s Angle Interplanar Spacing Lattice Constant
(hkl) (h2 + k 2 + l2 )
(in Degrees) (in pm) a (pm)
14.6 111 3 340.2 547.5
Kα
[111] 29.4 222 12 161.3 546.2
8.7 111 3 258.7 545.1
Kβ
crystal 26.5 222 12 136.3 548.3
Mean Value 546.5
Mean lattice constant = 548.7 pm.
7
7 Calculations
Mass of a cell and unit cell and the number of unit cell.
Mass (m) of a unit cell is given by
m = ρV
Number of unit cells (n) is calculated using
n NA ρ
3
=
a m
Using these formula, mass of NaCl is found to be 58.675u.
No. of NaCl in the crystal is = 3.8 ≈ 4
7.1 Error Analysis
|Theoretical value - Experimental value|
Error = Theoretical value ∗ 100
7.1.1 Error in Lattice Constant
Error in a = 2.7
7.1.2 Error in Mass
Error in m = 8.9
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8 Results
• Lattice constant of NaCl monocrystal is found to be to 548.7 pm or 5.487 µm.
• Interplanar spacing are found for various (hkl) planes and it is reported in the table.
• Number of NaCl in a unit cell is found to be 3.8 ≈ 4.
• Mass of 1 unit cell is found to be 216u.
• Experimental error is lattice constant is 2.7%.
• Experimental error in mass is 8.9%.
9 Discussion
The experiment illustrates the use of Bragg’s Law to observe the fundamental structures of
the crystal lattice. This experiment demonstrates the use of intensity diffraction patterns
to understand the internal structure of solid state structures
10 SOURCES OF ERROR
1. Impurity and structural deformity inside the crystal.
2. Settings of Goniometer must be precise
11 PRECAUTIONS
1. Crystal should be mounted properly.
2. Setup should be properly calibrated.
3. The GM counter must not be exposed to the X-ray radiation for prolonged time.
4. There is initially a large intensity, which must be ignored, due to stray radiation.
9
References
[1] [Link]
[2] SRIVASTAVA, J. P. Elements of Solid State Physics, Fourth Edition, PHI India
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