TITLE: X -RAY ANALYSIS OF CERAMIC MATERIALS.

AIM: Identifying the given sample using the results obtained from the x-ray
diffractometer.

INTRODUCTION

X-ray scattering techniques are a family of non-destructive analytical techniques

which reveal information about the crystallographic structure, chemical composition, and
physical properties of materials and thin films. These techniques are based on observing
the scattered intensity of an X-ray beam hitting a sample as a function of incident and
scattered angle, polarization, and wavelength or energy.

THEORY

Bragg's Law and Diffraction:-

The relationship describing the angle at which a beam of x-ray of a particular

wavelength diffracts from a crystalline surface was discovered by Sir William H.
Bragg and Sir W. Lawrence Bragg and is known as Bragg’s Law

2dsin= n

= wavelength of the x-ray

= scattering angle
n = integer representing the order of the diffraction peak.
d = inter-plane distance of (i.e. atoms, ions, molecules)

MATERIALS AND APPARATUS

Apparatus: X-ray diffractometer
Glass plate

Materials: Ceramic powder sample

PROCEDURE:

The diffractometer was set to the suitable parameters previously. Then the unknown
specimen powder was placed on the glass plate compacting it with enough pressure to
cause cohesion between the powder and the glass plate. Then the surface was smoothened
by removing the excess powder. The slide was then fixed on the sample holder of the x ray
diffractometer and the scanning unit was moved continuously over a circular scale and the
variation of intensity was obtained against the changing angle on a strip chart.

CALCULATIONS

2θ(degree) d= λ__ (ºA)

2sinθ
20.8 4.2704
26.6 3.3510
27.5 3.2434
36.6 2.4551
39.5 2.2813
40.3 2.2379
42.5 2.1279
45.8 1.9811
50.2 1.8273
54.9 1.6723
55.4 1.6584
60.0 1.5418
64.0 1.4547
67.7 1.3839
68.1 1.3868
68.3 1.3732

RESULTS
According to the result obtained & comparing to the Hainault manual and the JCPPS card,
the given sample as identified & closely set with “Quartz or Belemnite”
DISCUSSION:

Some of the d values of Quartz and Berlinite that closely match the tested sample and their
intensities (within brackets) are as follows:

Sample quartz Berlinite

4.2704 4.257 (22) 4.28 (25)
3.3510 3.342 (100) 3.369 (100)
2.4551 2.457 (8) 2.471 (12)
2.2813 2.282 (8) 2.287 (6)
2.2379 2.237 (4) 2.252 (6)
2.1279 2.127 (6) 2.140 (10)
1.9811 1.9792 (4) 1.994 (6)
1.8273 1.8021 (<1) 1.835 (16)
1.6723 1.6591 (2) 1.679 (6)
1.5418 1.5418 (9) 1.552 (14)

Other details of the matching candidates are:

Candidate Crystal structure Colour

Quartz Hexagonal Colourless
Berlinite Hexagonal Colourless

From the value given above it can be seen that there is not much of a difference (almost a
negligible one) between the d values of the sample that was subjected to the experiment
and the samples that were selected from the Hanwalt manual and JCPPS card (especially
for Quartz).

For quartz it was to be seen that there is an additional d value between 3 and 4 ºA other
than 3.342 which is contrary to the single d value seen between 3 and 4 ºA. This may be
due to the ceramic being not properly powderised thereby revealing all the possible
orientations of the crystal faces.

It can also be seen that in most of the d values for both quartz and Berlinite, the expected
values for intensity are half of that of the obtained values. This may occur due to several
reasons such as using a powder which contains a considerable no of particles whose size is
greater than 10 microns, mixing of other impurity materials that have d values as those in
which the intensity has shown a considerable increase. Another reason for the difference
between the data collected from the Intensity~2θ graph and the data obtained from the
cards maybe due to the error that may have occurred in calculating the maximum intensity.
As this intensity was calculated by projecting it beyond the boundaries of the paper an
error may have occurred in calculating this value and this value may have been in turn
been transferred to the other intensities as the other intensities are calculated relative to the
maximum intensity. Another error that may have occurred is in selecting the average curve
from which the height of a peak is calculated. Applying a high pressure without using a
binder to cause cohesion while inserting the powder into the recess in the glass plate can
also result in the particle taking certain orientations. This can also lead to high intensities
for certain d values (this error can be avoided by using a binder to cause cohesion between
the powder and the glass face.
CONCLUSIONS

The powder method is an extremely effective method foe identifying crystalline materials
provided that the errors that can occur during calculation of d values, powder preparation
and other experimental techniques be minimized.

REFERENCES:
Cullity, B. D., Elements of X-Ray Diffraction, Addison-Wesley Publishing Company Inc.,
Second edition, 188-196p.