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1. XRD analysis, a focused X-Ray beam is shot at the sample at a specific angle of
incidence.
2. The X-Rays deflect or "diffract" in various ways depending on the crystal
structure (inter-atomic distances) of the sample. The locations (angles) and
intensities of the diffracted X-Rays are measured.
3. Crystalline substances have an ordered three-dimensional arrangement with a
particular spacing of atoms.
4. When x rays strike the atoms within the crystal, the atoms absorb and reemit
the energy from the x rays in the form of spherical wave fronts emanating from
each atom. The waves travelling outward from each atom interact with other
waves in the processes known as constructive and destructive interference
which results a diffraction pattern. The patterns are controlled by the spacing of
atoms within the matrix and are unique to that substance.
Every compound has a unique diffraction pattern. In order to identify a
substance, the diffraction pattern of the sample is compared to a library
database of known patterns.
Instrument component
1. Source
The source come from the X- ray Tube.
What does the source produce?
The source produces X- ray that will be used for analyzing the sample.
What is an X ray Tube?
An X ray tube is usually made from evacuated ceramic or glass vessel. A x
ray tube contain a tungsten filament which is located in the cathode. From the
cathode, electron are emitted. The x ray tube also contain an anode where
these electrons are accelerated with a potential of several ten thousand volt.
Filaments
-
Anode
-
positive end of the x-ray tube, target for stream of electron that are
emitted by the cathode
The process
accelerated electrons hit inner shell electrons from atoms of the target metal
material, remove them and leave holes behind. These holes are quickly filled
from higher level electrons of the same atom. On falling down to the lower
energy level the atoms emit characteristic radiation ( X ray) with sharply
defined frequencies associated with the difference between the atomic energy
levels of the target atoms.
2. Primary Optic
Function
controls the beam produced by the X-ray source, and manipulates it into forms
more useful for diffraction experiments
Soller Slit
reduce the axial divergence of the X- Ray beam to less than 6 = to
collimate the X ray Beam
Monochromator
Prevent the passing of other lights ( in nm) except for the chosen
wavelength
3. Sample holder
Function
Place to put the sample.
The best result is obtained when the sample is a rotating sample holder.
In the sample holder, the most common error that might occurred is due
to overfilled or underfilled of the sample in the sample holder. This will
cause error on the result.
4. Detectors
The detectors based on the image above is the photographic plate.
Function
allows the diffracted X-rays to be detected
Mechanism
The photographic plate is sensitive to light, this happened since there is
coating of emulsion of silver salts. When the x- rays emits its beam, the
photographic plate will absorbs it beams and undergo chemicals changes
which can capture the diffracted X ray patterns
The data obtained from XRD are in the form of DIFFRACTION PATTERN,
During XRD analysis the X-ray will attack the atom in the crystal lattice
and then diffracted off set of planes that are present inside the unit cell
(smallest constituent that make up the crystal lattice or repeating unit of
crystal lattice).
Bragg equation
How constructive interference occurs?
During analysis, same wavelength of X-ray will attack different atom in
Therefore for the same wavelength of the X-ray to attack the atom
located in a deeper atomic plane and thus reflected, it needs to travel
extra 2dsin
If the extra distance is equal to the wavelength of two waves they will
In general the direction where the light are reflected depends on the
orientation of planes inside the unit cell. Different orientation of planes
Indices
Which is a set of numbers that show the intercepts of the planes in
crystal and thus may be used to uniquely identify the plane or surface.
o It is because different miller indices represent planes with different
orientation.
pattern
will
represent
the
Wavelength is known
constructive
interference
occur
Solving Bragg's Equation gives the dspacing between the crystal lattice
planes of atoms that produce the
constructive interference
Applications of XRD
The main function of XRD application are:
To identify the unknown crystalline materials
To determine the charcteriation of crystalline materials
To measure the samplepurity.
There are 4 example of XRD application in real life:
Pharmaceutical insustry
o X-ray diffraction (XRD)
can
be
used
to
unambiguously
Forensic Sccience
o XRD is used mainly in analysis. Examples of contact traces are paint flakes,
hair, glass fragments, stains of any description and loose powdered
materials. Identification and comparison of trace quantities of material can
help in the conviction or exoneration of a person suspected of involvement in
a crime.
Geological Application
o XRD is the key tool in mineral exploration. Mineralogists have
been amongst the foremost to develop and promote the new field
of X-ray crystallography after its discovery. Thus, the advent of
XRD has literally revolutionized the geological sciences to such a
degree that they have become unthinkable without this tool.
Nowadays,
mineralogical
any
geological
studies
would
group
be
actively
lost
involved
without
XRD
in
to
Microelectics Industry
o As the microelectronics industry uses silicon and gallium arsenide
single crystal substrates in integrated circuit production, there is a
need to fully characterise these materials using the XRD. XRD
topography can easily detect and image the presence of defects
within a crystal, making it a powerful non-destructive evaluation
Glass industry
o While glasses are X-ray amorphous and do not themselves give X-ray
diffraction patterns, there are still manifold uses of XRD in the glass industry.
They include identification of crystalline particles which cause tiny faults in
bulk
glass,
and
measurements
of
crystalline
coatings
for