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CHAPTER 3 CHARCTERISATION TECHNIQUS

3.1 DIFFRACION METHODS

Diffraction methods have become a fundamental tool for the structural characterization
and they have also been applied to the samples studied in this project. The X-ray
diffraction (XRD) allows studying the long range ordering and determination of the
crystallographic structure on the one hand and deviation from a perfect ordering on the
other hand. The usefulness of the short x-rays arises from the possibility to tune their
wavelength so that it closely matches the interatomic distances in the solid(i.e bcomes
of order~ 1A.

3.1.1 X-RAY DIFFRACTION


X-ray diffraction is a widely used technique to determine the crystalline phase in the
bulk material. The wavelength of X-ray is comparable to the separation (d) between the
crystal planes. Diffraction occurs when the Bragg condition which states that the X-rays
reflected from two neighboring planes of atoms must coherently interfere, is satisfied.
This condition is fulfilled when the extra distance traveled by the x-rays to the farther
plane of atoms is equal to the multiple of the X-ray wavelength, i.e. 2dSinϴ = nλ, where
n is an integer ( as illustrated in Fig. 3.1 below) giving rise to diffraction in solids[1,2].
An x-ray diffraction can be carried out on the polycrystalline (powder) sample or single
crystals. The XRD pattern is a plot of the intensity of diffracted rays versus Bragg angle

Fig: 3.1. The Bragg condition, 2dSinϴ = nλ, where n is an integer, the extra distance
traveled by the X-rays to the farther plane of atoms is equal to the multiple of the X-ray
wavelength.
and contains information about the structure and composition of the basis. This
information needs to be extracted from the pattern by employing a proper analysis
procedure such as Full Prof suite.

In the present study, the powder method is made use off wherein the samples were
crushed into fine powder in an agate pestle and mortar and placed in a beam of
monochromatic X-rays. The powder X-ray diffraction measurements are performed on
powder samples using Rigaku X-ray diffractometer system at the Department of
Physics, St. Xaviers College of Arts and Science. The intensity of the Copper K α (λ =
1.5418A°) radiation diffracted from the powdered specimen was detected by a
scintillation counter and recorded as a function of 2ϴ, where ϴ is the angle of
incidence. The patterns were recorded in continuous mode in the 2ϴ range of 20° ≤ 2ϴ

25
≤ 80° with a step size of 0.02 at a speed of 2°/min. The diffraction peaks were indexed
using a commercially available Power diffraction package.

3.2 FTIR(FOURIER TRANSFORM INFRARED ANALYSIS)

The FTIR technique is used for knowing the infrared spectra in terms of absorbance,
reflection and photoconductivity [3].FTIR collects spectral data in wide spectral range.
This technique is utilized for knowing the molecular bonding between atoms present in
the sample, resulting in confirmation about its structure. In this technique, the sample
cannot be directly characterized, but a few samples like thin films may be done by
direct measurement. For the ceramic sample, there is a base of potassium bromide
(KBr). The light source falls on the sample surface that is placed in front of the base
KBr. The IR spectrum forms in the form of stretching peaks. Each peak forms at a
different wave number. These peaks give the bonding range between the atoms present
in the material. The FTIR principle is based on the Michelson’s Interferrometer as seen
in Fig. 3.2 below. Data acquisition for FTIR was carried out at the Research centre of
the college.

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