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X-RAY DIFFRACTION

Submitted by Pranav Diwakar


2014B5PS711P
Introduction:

XRD analysis is a non-destructive technique that provides extensive information on the chemical
composition and crystallographic structure of natural and manufactured materials. Various
characteristics of the material are determined by measuring the intensities and angles of diffraction of
X-ray beams that are shone upon the material. The crystalline structure of the material’s lattice causes
this diffraction. Through XRD analysis, one can characterise the phases, particle size, interplanar
spacing and other quantities of a sample.

Objective:

- To index the crystal structures found in a sodium chloride sample.


- To calculate the interplanar spacing and lattice parameter of the lattice structure.
- To find the particle size.
- To obtain the XRD pattern of polyethylene oxide (PEO) film.

Theory:

A beam is comprised of many scattered rays mutually reinforcing one another. Light waves are
scattered and undergo diffraction on striking a set of regularly spaced obstacles whose dimensions are
of the order of wavelength.

Consider two incident beams falling on the surface of a sample. For the two beams to constructively
interfere, their path difference (∆) must be an integral multiple of the wavelength (λ) i.e. Δ = nλ. If d
is the spacing and θ is the scattering angle, we have Δ = 2dsinθ. This gives Bragg’s condition.

2dsinθ = nλ

sinθ <= 1
=> nλ/2d <= 1
n = 1 (first order) => λ <= 2d (necessary condition)

(Note: X-ray beams have an average wavelength of 1.54Å, which is generally lesser than most
interplanar spacings, making the X-ray diffraction method viable.)
The relation between the cell parameter (a) and the interplanar spacing is given by

d = a
(h2 + k2 + l2)1/2
, where (hkl) are the Miller indices of the plane.
The extinction rules for cubic crystals are as follows.

- If the sum (h+k+l) is even: BCC


- If all three quantities are either even or odd: FCC

Working principle:

In an X-Ray diffractometer, the sample is placed in a holder and an X-ray beam is shined upon it. The
angle made by the reflected beam with respect to the incident beam is measured. Since each plane only
reflects 10-3 to 10-5 of the incident radiation, it would take 103 to 105 planes to contribute to a reflected
beam. These are detected by an X-ray detector, which measures their intensities. When multiple
reflected beams interfere constructively at a particular angle, a peak is formed. By plotting the angular
positions and intensities of the resultant diffracted radiation, a pattern of these peaks is produced,
which is characteristic of the crystallographic phases present in the sample.

The intensity of a reflection and, hence, a peak, depends on the number of atoms present on the
reflecting plane. As a direct result of Bragg’s law, the position of the peak depends on the interplanar
spacing. The width of a peak depends on the number of planes that are contributing to that particular
reflection. However, this is also affected by instrumental error and imperfections in the crystal.

The Debye-Scherrer equation provides a relation between the mean size of the particles present in a
sample and the full width at half maximum (β) and position (θ) of a peak in the sample’s XRD graph.
The relation is as follows.

Particle Size (P.S.) = 0.9λ


βcosθ
Results and calculations:

Sodium Chloride (NaCl)


Intensity (A.U.)

2θ (degrees)

Taking λ to be 1.54Å, assuming first-order diffraction (n = 1).

d = λ
2sinθ

Interplanar FWHM
Peak position Plane Cell parameter Particle Size
θ (degrees) sinθ spacing (d) (β)
(2θ) (degrees) (hkl) (a) (Å) (Å)
(Å) (degrees)

27.7894 13.8947 0.2401 3.2065 (111) 5.5538 0.2813 290.8130

32.2005 16.1003 0.2773 2.7766 (200) 5.5532 0.1761 469.3572

45.7769 22.8885 0.3889 1.9797 (220) 5.5996 0.1625 530.4549

45.9111 22.9556 0.3900 1.9743 (220) 5.5841 0.1319 653.8410

54.3175 27.1588 0.4565 1.6869 (113) 5.5948 0.1598 558.5260

56.7246 28.3623 0.4750 1.6209 (222) 5.6150 0.1724 523.4618

66.3790 33.1895 0.5474 1.4066 (400) 5.6265 0.2583 367.3722

66.6532 33.3266 0.5494 1.4015 (400) 5.6060 0.1024 928.1373

73.4199 36.7100 0.5978 1.2881 (330) 5.4651 0.1337 740.8970

75.6223 37.8112 0.6131 1.2560 (331) 5.4747 0.1651 608.8244

84.2932 42.1466 0.6710 1.1475 (422) 5.6215 0.1365 784.6624

Average cell parameter 5.5722


Polyethylene oxide (PEO)

Taking λ to be 1.54Å, assuming first-order diffraction (n = 1).

d = λ
2sinθ

Interplanar FWHM
Peak position Plane Cell parameter Particle Size
θ (degrees) sinθ spacing (d) (β)
(2θ) (degrees) (hkl) (a) (Å) (Å)
(Å) (degrees)

19.3818 9.6909 0.1683 4.5743 (220) 12.9380 0.2678 300.8273

22.2503 11.1252 0.1930 3.9906 (220) 11.2872 0.3946 205.1010

23.5189 11.7595 0.2038 3.7782 (300) 11.3345 0.7456 108.7908

26.3261 13.1631 0.2277 3.3813 (222) 11.7132 0.5244 155.5201

Average cell parameter 11.8182

Results:

- The XRD analyses of NaCl and PEO film was performed.


- The cell parameters and particle sizes were found for both samples.
- The mean cell parameter for NaCl was measured to be 5.5722 Å, which is 1.2% above the theoretical
value of 5.6402 Å.
- The mean cell parameter for PEO was measured to be 11.8182 Å, which is 0.44% below the
theoretical value of 11.8714 Å.

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