Applying X-Ray

Diffraction in Material
Analysis
Dr. Ahmed El-Naggar

Outline
Introduction
X-Ray diffraction techniques
Some X-Ray diffraction applications
Summary

I) Introduction

II) X-Ray diffraction techniques

I- High-resolution
Mostly used for near-perfect epitaxial thin films and
single crystals.

2- Medium resolution
Primarily used for thin films that are textured
epitaxial, textured polycrystalline.
Also can be used for polycrystalline and amorphous
materials.

3- Low resolution
Mostly used for polycrystalline as well as
amorphous materials

motorized movements of the Sample 6

 Low Resolution applications: Texure

analysis, Stress analysis, and -2 scan,
phase analysis
Medium Resolution applications: -2 scan,
phase analysis, Stress analysis, and
Reflectivity.
High Resolution applications: Rocking
curve (-scan), Reciprocal space map, -2
scan, phase analysis, Stress analysis, and
Reflectivity

III) Some X-Ray diffraction applications

/2-scan, phase analysis

From -2 ( -2) scan the ensemble of d- spacings (" d"

s) (Using Bragg's law to get them) and intensities (" I" s)
is sufficiently in order to identify phases

Phase determination can be performed by a comparison

of a set of experimental d's and I'swith a database of d-I
files

Database of d-I files were named Powder Diffraction File

(PDF) database (started 1919 and was containing 4000
compounds) , but from 1978 the name changed to be
International Center for Diffraction Data (ICDD) which
contains about 300,000 pattern

Indexing and lattice constants determination

 N.B. The unit cell volume V( for Cubic) = a 3, for

tetragonal = a2c, and for hexagonal = 0.866 a2c

Reflectivity

It is proceeded at low angles of incidence () to study the

surface only (GIXRD)

Reciprocal Space Maps

From reciprocal space mapping (RLM): composition,

thickness (at least 50 nm), mismatch, mosacity, and defects
profile.

Rocking curve measurement;

composition and thickness
determination

 HRXRD (004) Rocking curve for sample 1683 of

In0.53Al0.47As on InP substrate

For example: To measure layer composition for InyAl1-yAs we need

only B (difference between Bragg angle of the substrate and epilayer)
and use the following relation (comes from Vegard's law) for symmetric
measurements:

Symmetric measurement is only sensitive to the lattice mismatch

perpendicular to the substrate/layer interface
Where, for symmetric measurements:

Also, one can use

:The

layer thickness can be determined from the relation

The best way to determine layer compositions and

thicknesses : is to compare the experimental rocking curve to
simulated curves. There are some commercial programs for that purpose
(i.e. RADS (Rocking curve Analysis by Dynamical Simulation)

Summary
XRD is the main method for crystallographic
characterization for both bulk and thin film materials
The diffraction pattern is like a finger print of the crystal
structure.
From the diffraction pattern of -2 ( -2) scan : phase
analysis
From rocking curves: composition, thickness (30- 1000
nm), mismatch.
From reciprocal space mapping(RLM): composition,
thickness (at least 50 nm), mismatch, mosacity, and
defects profile.
From Reflectivity measurements: composition, thickness
(5-150 nm), and interface roughness.
From Pole figures: Composition, orientation with respect
to substrate and phase analysis