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What is XRD ?

NANOSAINS DAN NANOMATERIAL

X-RAY DIFFRACTIONS (XRD)

Mostuseful in the characterisation of crystalline

materials; Ceramics, metals, intermetallics,
minerals, inorganic compounds

Rapid and nondestructive techniques

Providei nformation on unit cell dimension

Structural Analysis
Evi Fitri (3325122134)

Universitas Negeri Jakarta

2015

X-ray diffraction provides

structural information

Interatomic distances and bond angles

Introduction

most

definitive

Electromagnetic Spectrum

X-ray diffraction is used to obtain structural information about

crystalline solids.

Useful in biochemistry to solve the 3D structures of complex

bio-molecules.

Bridge between physics, chemistry, and biology.

X-raydiffractionis important for

Solid-state physics

Biophysics

Medical physics

Chemistry and Biochemistry

What Is X-Rays ?

Beams of electromagnetic radiation

*smallerwavelength than visible light,

*higher energy

*more penetrative

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History of X-Ray Diffraction

X-Ray Production

Wilhelm Conrad Rntgen discovered 1895 the X-rays. 1901 he

was honoured by the Noble prize for physics. In 1995 the
German Post edited a stamp, dedicated to W.C. Rntgen.

History of X-Ray Diffraction

(1895) X-rays discovered by Roentgen

(1914) First diffraction pattern of a crystal

made by Knippingand von Laue

(1915) Theory to determine crystal structure

from diffraction pattern developed by
Bragg.

(1953) DNA structure solved by Watson and

Crick

Now Diffraction improved by computer

technology; methods used to determine
atomic
structures
and
in
medical
applications

The prime componen in X-Ray tube are

filamen (catode), vacum room, anode,
and high voltage

When high energy electrons strike an

anodein a sealed vacuum, x-raysare
generated. Anodes are often made of
copper, iron or molybdenum.

High energy electron come from heated

filamen in X-Ray tube.

X-rays are electromagnetic radiation.

They have enough energy to cause

ionization.

Generation of X-Rays

The First X-Ray

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Braggs Law

Braggs Law

n = 2d sin
Constructive interference occurs only when

English physicists Sir W.H. Bragg and his son Sir W.L. Bragg developed a relationship in 1913 to
explain why the cleavage faces of crystals appear to reflect X-ray beams at certain angles of
incidence (theta, q). The variable d is the distance between atomic layers in a crystal, and the
variable lambda l is the wavelength of the incident X-ray beam; n is an integer. This observation is
an example of X-ray wave interference (Roentgen strahl interferenzen), commonly known as X-ray
diffraction (XRD), and was direct evidence for the periodic atomic structure of crystals postulated
for several centuries.

Braggs Law

n = AB + BC

AB=BC

n = 2AB

Sin =AB/d

AB=d sin

n = 2 d sin

= 2 dhkl sin hkl

How Diffraction Works ?

The Braggs were awarded the Nobel Prize in

physics in 1915 for their work in determining
crystal structures beginning with NaCl, ZnS
and diamond.
The Braggs were awarded the Nobel Prize in physics in 1915
for their work in determining crystal structures beginning with
NaCl, ZnS and diamond.

Wave Interacting with a Single Particle

Wave Interacting with a Solid

Incident beams scattered uniformly in all directions

Scattered beams interfere constructively in some directions, producing

diffracted beams
Random arrangements cause beams to randomly interfere and no
distinctive pattern is produced

Crystalline Material
Regular pattern of crystalline atoms produces regular diffraction
pattern.
Diffraction pattern gives information on crystal structure

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Components XRD

X-ray source

Device for restricting wavelength range

goniometer

Sample holder

Radiation detector

Signal processor and readout

How XRD works ?

A continuous beam of X-rays is incident on

the crystal

The diffracted radiation is very intense in

certain directions

How XRD works: Braggs Law

The beam reflected from the lower

surface travels farther than the one
reflected from the upper surface

If the path difference equals some

integral multiple of the wavelength,
constructive interference occurs

Braggs Law gives the conditions for

constructive interference

How Diffraction Works: Schematic

These directions correspond to constructive

interference from waves reflected from the
layers of the crystal

The diffraction pattern is detected by

photographic film

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Single Crystal Diffraction

A single crystal at random orientations and its corresponding diffraction
pattern. Just as the crystal is rotated by a random angle, the diffraction
pattern calculated for this crystal is rotated by the same angle

Single Crystal Diffraction

Single Crystal Diffraction

Used to determine

crystal structure

orientation

degree of crystalline perfection/imperfections (twinning, mozaicity,

etc.)

Sample is illuminated with monochromatic radiation

Easier to index and solve the crystal structure because it diffraction

peak is uniquely resolved

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X-ray Powder Diffraction

More appropriately called polycrystalline X-ray diffraction, because it can

also be used for sintered samples, metal foils, coatings and films, finished
parts, etc.
Used to determine

phase composition (commonly called phase ID)-what phases are

present?

quantitative phase analysis-how much of each phase is present?

unit cell lattice parameters, crystal structure

average crystallite size of nanocrystallinesamples

crystallite microstrainandtexture

residual stress (really residual strain)

X-ray Powder Diffraction

A 'powder' composed from 4 single
crystals in random orientation (left)
and the corresponding diffraction
pattern (middle). The individual
diffraction patterns plotted in the
same color as the corresponding
crystal start to add up to rings of
reflections. With just four reflection
its difficult though to recognize the
rings. The right image shows a
diffraction pattern of 40 single
crystal grains (black). The colored
spots are the peaks from the 4 grain
'powder' shown in the middle
image.

Applications of X-Ray Diffraction

Determinationof Crystalstructure

Phaseidentification/ transition

Grainsize / micro-strain

Texture/stress( i.e.polymer, fiber )

Determination of thin film composition

Industry Identification of archeological materials

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Advantages of XRD

Fastidentification of materials,

Easysample preparation,

Computer-aidedmaterial identification,

Large library of known crystalline structures.

What are the dangerousareas?

Safetyin XRD

Exposure types
o

Short-term high-dose

Long-term low-dose

Invisible, odorless,colorless (most exposures undetectable)

Lab users must understand radiation safety issues and pass an exam to use
lab

Safeguards present in lab do not substitute for knowledge and following

safe procedures

Thank you