Kimia Analisis Instrumen 2

X-Ray Diffraction (XRD)

 Introduction to XRD
 How does it Works?
 Function
 Instrumentation
 Sample Preparation
Tentang Cahaya…
“Allah cahaya langit dan bumi. Perumpamaan cahaya Allah
adalah seperti sebuah lubang yang tak tembus, yang di
dalamnya ada pelita besar. Pelita itu di dalam kaca (dan)
kaca itu seakan-akan bintang (yang bercahaya) seperti
mutiara, yang dinyalakan dengan minyak dari pohon yang
banyak berkahnya, (yaitu) pohon zaitun yang tumbuh tidak
di sebelah timur dan tidak pula di sebelah barat, yang
minyaknya (saja) hampir-hampir menerangi, walaupun
tidak disentuh api. Cahaya di atas cahaya (berlapis-lapis),
Allah membimbing kepada cahaya-Nya siapa yang Dia
kehendaki, dan Allah membuat perumpamaan-
perumpamaan bagi manusia, dan Allah Maha Mengetahui
segala sesuatu.” (QS. An-Nuur [24]:35)
Introduction
X-rays were discovered in 1895 by
the German physicist Wilhelm
Conrad Röntgen

And were so named because their

nature was unknown at the time.
Wilhelm Conrad Röntgen
(1845-1923)

• He was awarded the Nobel prize for

physics in 1901.
Inner electron
 X-rays are electromagnetic radiation with photon
energies ranging from 100 eV to 100 keV.

Civil Security
Medical Science

Analyzing the composition of chemical

elements, phase, and the crystal structure
of a material
• Rontgen was awarded the Nobel prize for
physics in 1901.
 Illustration
Do you know about allotropes of carbon (C)?
Carbon has a lot of allotropes.
Three of them are graphite, diamond, and regular.
How can we know the difference between the three allotropes?

Graphite C60 Diamond

Diamond

C60

Grafit
 X ray diffraction

• Is a method for analyzing a cystalline solid

• Inspection that does not damage the material or
humans  
• Qualitative and quantitative analysis of material.
 Diffraction
Diffraction is a wave bending event when passing through an
object (for example in the form of a slit).

Not diffracted Diffracted

The process by which a beam of light or other system of waves is spread

out as a result of passing through a narrow aperture or across an edge,
typically accompanied by interference between the wave forms produced
X-RAY DIFFRACTION
• Monochromatic x-rays falling on a crystal will be scattered in
all directions, but because of the regularity of the location of
the atoms, in certain directions the scattering waves will
interfere constructively, while others have negative
interference.
 X ray diffraction
• X-rays that reinforce each other are called diffraction beams.
XRD observes the pattern of refraction of light as a result of
the beam of light refracted by the material that has the
arrangement of atoms in the crystal lattice.
•

• X-ray diffraction is a technique used to analyze crystalline

solids. X-rays are electromagnetic radiation with a wavelength
of about 1 Å, between wavelengths of gamma rays (γ) and
ultraviolet rays.
Formation of x-ray
1. Characteristic x-rays
X-rays are produced if high-speed electrons hit a target metal.
This occurs in the instrument section called x-ray tubes or
cathode tubes. High-speed electrons hitting electrons in the 1s
orbitals will cause the electrons to excite causing vacancies (□) in
the 1s orbitals, by charging electrons in these empty orbitals
from higher energy orbitals giving X-ray rays.
The K Lines
The L Lines
The X-rays obtained give a certain peak intensity which depends
on the probability of the electron transition occurring. Kα
transitions are more likely to occur and have a higher intensity
than Kβ transitions, so Kα radiation is used for X-ray diffraction
purposes.
 2. Bremsstrahlung x-
rays
X-rays can also be produced by
the process of slowing down
electrons as they penetrate
the target metal.
When high-energy and high-
speed electrons hit atoms in
the metal target, the electrons
slow down while releasing x-
ray radiation with a continuous
spectrum called
Bremsstrahlung radiation or
white radiation.
2. Bremsstrahlung x-
rays

The result of all these

processes for a particular
metal is the typical spectrum
of X-rays. There is a basic
shape formed by white
radiation and a sharp
characteristic peak that
depends on the quantization
of electron transitions.
 2. Bremsstrahlung x-
rays

The continuous spectrum of x-rays arises due to the braking of electrons

with high kinetic energy by the anode. During the braking, some of the
kinetic energy is converted into x-rays. This braking process can take
place either suddenly or slowly, so that the x-ray energy it produces
will have a very wide energy range.
 There are several types of wavelength emitted with
different intensities, where the wavelength Kα1 has a
higher intensity, so it is used in X-ray diffraction.

Continuous X-Ray vs. Characteristic X-Ray

Bragg's Law and Diffraction

A crystal has an arrangement of

atoms arranged in an orderly
and repetitive manner, having a
distance between atoms whose
ideas are the same as the
wavelength of X-rays.
Bragg's Law and Diffraction
...consequently, if a beam of X-rays is shot at a crystalline
material, the ray will produce a typical diffraction pattern. The
resulting diffraction pattern matches the arrangement of atoms
in the crystal.
Bragg's Law and Diffraction
According to the Bragg approach, crystals can be seen to consist
of flat fields (crystal lattices), each of which functions as a semi-
transparent mirror. If X-rays are fired into the stack of flat planes,
then some of them will be reflected by these fields with the
same reflecting angle as the incident angles, while the rest will
be continued through the plane.
Bragg's Law and
Diffraction

The mathematical formulation can be expressed by relating the wavelength of

X-rays, the distance between fields in the crystal, and the diffraction angle:

nλ = 2d sin θ (Bragg equation)

λ = wavelength of X-rays, d = distance between the crystal lattices, θ = angle of

incidence of rays, and n = 1, 2, 3, and so on is the order of diffraction.
The Bragg equation is used to determine the parameters of the crystal cell.
Meanwhile, to determine the crystal structure, using crystallographic
computation methods, the intensity data is used to determine the positions of
the atoms.
Bragg's Law and Diffraction:
If two parallel X-ray beams pertaining to the same crystal plane, it will diffracted at a certain
angle, and the difference in distance traveled by the two rays is proportional to the wavelength of
the X-ray
Bragg's Law and Diffraction:
•
Based on Bragg's Law, if the wavelength of the colliding ray is
known, then we can control the angle of impact, then the
distance between atoms / geometry of the d-spacing can be
determined.

• By calculating the d-spacing obtained from the Bragg formula

and knowing the value of the Miller Index (hkl) which states
the position of the atoms in the crystal, the lattice parameters
(a, b and c) can be determined according to the crystal shape.
Based on the Bragg equation, if a beam of X-rays is dropped on
a crystal sample, then the crystal field will refract X-rays that
have wavelengths equal to the distance between the lattice
in the crystal.
The refracted beam will be captured by the detector and then
activated as a diffraction peak.
The more crystalline planes found in a sample, the stronger the
refraction intensity it produces.
Each peak that appears in the XRD pattern represents one
crystal plane that has certain predetermined three-
dimensional motions.
The peaks obtained from this measurement data are then
matched to the X-ray diffraction standard for almost all types
of material.