STRUCTURE DETERMINATION BY DIFFRACTION

AND SCATTERING

Presented by
Shawhab Ali Jaber
University of Technology
2019-2020
Outlines:
• X-Rays form part of the electromagnetic spectrum, and are characterized by energies
lying between ultra-violet and gamma radiation.
• XRD is used to uniquely identify the crystalline phases present in materials
and to measure the structural properties (strain state, grain size, phase
composition, preferred orientation, and defect structure)
• It is also used to determine the thickness of thin films and multilayers, and
atomic arrangements in amorphous materials and at interfaces.
• Useful in biochemistry to solve the 3D structures of complex
biomolecules.

•
 A-Classification

 The techniques can be broadly classified into two

groups:
1. those which directly identify the atomic species present and
then provide structural information about the identified
species from diffraction or scattering effects (EXAFS,
SEXAFS, and XPD)
2. and those which are purely diffraction-based and do not
directly identify the atoms involved, but give long-range
order information on atomic positions from diffraction
patterns (XRD, LEED, and RHEED).
 B-Bragg’s law

n=2d.sin
Where
d: Plane spacing
: Bragg Angle
n: Order of reflection from (hkl) planes of
spacing d
• The space between diffracting planes of atoms determines peak positions.
• The peak intensity is determined by what atoms are in the diffracting plane.
C-
 D-Grain Size

L=crystallite size
Crystallite size can be calculated using
Scherrer Formula
E-Lattice Strain (strain state)

do

No Strain 2

Uniform Strain
  d  strain 2

Non-uniform Strain
2
d
Broadeing b   2  2 tan 
d
 2-XRD Techniques and Applications

• powder diffraction
• single-crystal diffraction

XRD is a non destructive technique to identify crystalline phases.

The powder XRD pattern may be thought of as finger print of the single crystal
structure, and it may be used conduct qualitative and quantitative analysis.
 XRD is a technique used to determine the orientation of the given crystal compound.
 Obtain XRD pattern are used to measure d-spacing of the given compound.
 To measure thickness of thin films and multi-layers.
 To determine atomic arrangement.
Diffraction from a variety of materials
 3-Extended X-Ray Absorption Fine Structure, EXAFS

*EXAFS is a nondestructive, element-specific

spectroscopic technique with application to all elements
from lithium to uranium. It is employed as a direct probe
of the atomic environment of an X-ray absorbing element
and provides chemical bonding information. Although
EXAFS is primarily used to determine the local
structure of bulk solids (e.g., crystalline and amorphous
materials), solid surface, and interfaces.

*The EXAFS spectrum results from the constructive and

destructive interference between the outgoing and incoming
photoelectron waves at the absorbing atom.
Principle Of Mechanism
XAFS spectrum (Mo-K)
 4-Surface Extended X-Ray Absorption Fine Structure and
Near Edge X-Ray Absorption Fine Structure, SEXAFS/NEXAFS

A-SEXAFS is a research technique providing the most precise values

obtainable for adsorbate-substrate bond lengths, plus some
information on the number of nearest neighbors (coordination
numbers).
B-NEXAFS has become a powerful technique for probing the
structure of molecules on surfaces. Observation of intense resonances
near the X-ray absorption edge can indicate the type of bonding. The
energies of resonances to estimate the intermolecular bond length.

The principles and analysis of EXAFS and SEXAFS are the same.
 5-X-Ray Photoelectron and Auger Diffraction, XPD and AES

A-X-ray Photoelectron Diffraction (XPD) and Auger Electron Diffraction

(AED) are well-established techniques for obtaining structural information on
chemically specific species in the surface regions of solids.
B-Auger Electron Spectroscopy (AES), is a widely used technique to
investigate the composition of surfaces.

* Ultrahigh-vacuum conditions are necessary to maintain surface cleanliness

* The x-Ray photoelectron diffraction (XPD) and Auger electron diffraction
(AED) from a single crystal surface may be provide information about the
surface atomic structure.
 6-Low-Energy Electron Diffraction, LEED

Low-energy electron diffraction (LEED) is a technique for the determination of the surface

structure of single-crystalline materials by bombardment with a collimated beam of low
energy electrons (20–200 eV)

Advantages
High surface sensitivity
Easy information on symmetry
and shape of surface unit-cell
Atomic structure can be retrieved
with high accuracy
 7-Reflection High-Energy Electron Diffraction, RHEED

Reflection high-energy electron diffraction (RHEED) is a technique used to

characterize the surface of crystalline materials. RHEED systems gather
information only from the surface layer of the sample, which distinguishes
RHEED from other materials characterization methods that also rely on
diffraction of high-energy electron.