Presentation on

XRD APPLICATION :
Identification of an Unknown Specimen
Subject : Material Characterization

By,
Mr. Nishant Shashikant Joshi, Roll No.: 192ML014,
Mr. Nitesh Eknath Chaudhari, Roll No.: 192ML015.
First Year M Tech in Materials Engineering, NIT Surathkal, Karnataka.

Under the Guidance of

Dr. Shashi Bhushan Arya
Assistant Professor at NIT Surathkal, Karnataka.
 XRD Methods
1.Laue Method
2.Rotating Crystal Method
3.Powder Diffraction Method

Most suitable – Powder Diffraction Method

With this method we can find out unknown specimens

like,
Ores, Clays, Refractories, Alloys, Corrosion Products, Wear Products, Industrial Dust,
Pharmaceutical Products, minerals, organic compounds etc.
 BASIC PRINCIPLES
Diffraction Pattern – Fingerprint of a
Substance

Collection of known Pattern –

Powder Diffraction file (PDF)organized by
Joint Committee on Powder Diffraction Standards (JCPDS),
later renamed as International Centre for Diffraction Data (ICDD)
It has 8,93,000+ Powder Diffraction Patterns as per 2019 release data
by ICDD.

Matching the known Pattern –

1. Hanawalt Method,
2. Fink Method
 PROCEDURE
1.Sample Preparation
2.Selection of wavelength
3.Recording of Pattern Data
4.Calculation of Plane Spacing ‘d’
5.Calculation of ‘I/I1’
6.Locate the appropriate ‘d’ in the numerical search
manual
7.Compare the all ‘d’ & ‘I/I1’ values with tabulated
8.Full agreement – Identification complete
 EXAMPLE OF ANALYSIS
For unknown specimen we get following data with
Cu-kα radiation & Debye Scherrer camera.
EXAMPLE OF ANALYSIS

We select three strongest

intensity values.
d1 = 2.82 Å,
d2 = 1.99 Å,
d3 = 1.63 Å.
 EXAMPLE OF ANALYSIS
From numerical search manual d1 = 2.84 to 2.80 Å group
From above group – 17 elements have d2 =1.99 Å
But only 4 elements have d1 = 2.82 Å

From this data only NaCl has d3 = 1.63 Å

Therefore unknown sample is NaCl.
Standard JCPDS diffraction data card for NaCl
Where,
1 - File number
2 - Three strongest
intensities
3 - Lowest angle line
4 - Chemical formula &
name of substance
5 - Data on diffraction
method used
6 - Crystallographic
data
7 - Optical & other
data
8 – Data on specimen
9 - Diffraction pattern
 PRACTICAL DIFFICULTIES
1. Errors in the diffraction pattern of the unknown.

2. Errors in the card file.

This method fails when unknown is a substance not listed in a card file
 NEW XRD

THANK
YOU
VERY
MUCH