X-Ray Diffraction

Introduction
X-rays are a form of radiation that can pass through solid and semi-solid
substances. X-radiation (composed of X-rays) is a form of electromagnetic
radiation.X-rays are electromagnetic radiation of wavelength about 1 (1010 m), which is about the same size as an atom.X-ray wavelengths are
shorter than those of UVrays and typically longer than those of gamma
rays.

X-rays are produced when electrons strike a metal target. The electrons
are liberated from the heated filament and accelerated by a high voltage
towards the metal target. The X-rays are produced when the electrons
collide with the atoms and nuclei of the metal target.
Since X-rays are emitted by electrons, they can be generated by an X-ray
tube, a vacuum tube that uses a high voltage to accelerate
the electrons released by a hot cathode to a high velocity. The high velocity
electrons collide with a metal target, the anode, creating the X-rays.

The discovery of X-rays in 1895 enabled scientists to probe crystalline

structure at the atomic level. X-ray diffraction has been in use in two main
areas, for the ngerprint characterization of crystalline materials and the
determination of their structure.

Each crystalline solid has its unique characteristic X-ray powder pattern
which may be used as a "ngerprint" for its identication. Once the material

has been identied, X-ray crystallography may be used to determine its

structure.

X-ray diffraction is one of the most important characterization tools used in

solid state chemistry and materials science.We can determine the size and
the shape of the unit cell for any compound most easily using X-ray
diffraction.

Phenomenon
The atomic planes of a crystal cause an incident beam of X-rays to
interfere with one another as they leave the crystal. The phenomenon is
called X-ray diffraction.

X-ray diffraction relies on the dual wave/particle nature of X-rays to obtain

information about the structure of crystalline materials.

The dominant effect that occurs when an incident beam of monochromatic

X-rays interacts with a target material is scattering of those X-rays from
atoms within the target material. In materials with regular structure (i.e.

crystalline), the scattered X-rays undergo constructive and destructive

interference. This is the process of diffraction.

X-rays are generated by a cathode ray tube, filtered to produce

monochromatic radiation, collimated to concentrate, and directed toward
the sample. The interaction of the incident rays with the sample produces
constructive interference (and a diffracted ray) when conditions satisfy
Bragg's Law (n=2d sin ).These diffracted X-rays are then detected,
processed and counted.

The directions of possible diffractions depend on the size and shape of the
unit cell of the material. The intensities of the diffracted waves depend on
the kind and arrangement of atoms in the crystal structure. However, most
materials are not single crystals, but are composed of many tiny crystallites
in all possible orientations called a polycrystalline aggregate or powder.

//
Traditional XRD systems are often based on bulky equipment with high
power requirements as well as employing high powered X-ray sources to
increase X-ray flux on the sample, therefore increasing the detected
diffraction signals from the sample. These sources also have large
excitation areas, which are often disadvantageous for the diffraction
analysis of small samples or small sample features.
//

Powders of crystalline materials diffract x-rays. A beam of x-rays passing

through a sample of randomly-oriented microcrystal produces a pattern of
rings on a distant screen. Powder x-ray diffraction provides less information
than single-crystal diffraction, however, it is much simpler and faster.
Powder x-ray diffraction is useful for confirming the identity of a solid
material and determining crystallinity and phase purity.

Applications of X-Ray
Diffraction
X-ray diffraction is now a common technique for the study of crystal
structures and atomic spacing.A primary use of the technique is the
identification and characterization of compounds based on their diffraction
pattern.
One of the best methods of determining a crystal's structure is by Xray diffraction.
X-ray powder diffraction is most widely used for the identification of
unknown crystalline materials (e.g. minerals, inorganic compounds).
Determination of unknown solids is critical to studies in geology,
environmental science, material science, engineering and biology.
//Other applications include:
-characterization of crystalline materials
-Identification of fine-grained minerals such as clays and mixed layer clays
that are difficult to determine optically
-determination of unit cell dimensions
-measurement of sample purity
XRD is a nondestructive technique
To identify crystalline phases and orientation

 To determine structural properties: Lattice parameters (10-4),thermal

expansion
To measure thickness of thin films and multi-layers
To determine atomic arrangement//

Pharmaceutical industry
X-ray diffraction (XRD) can be used to unambiguously characterize the
composition of pharmaceuticals.XRD is the key technique for solid-state
drug analysis, benefiting all stages of drug development, testing and
production.
Forensic science
XRD is used mainly in contact trace analysis. Examples of contact traces
are paint flakes, hair, glass fragments, stains of any description and loose
powdered materials
Geological applications
XRD is the key tool in mineral exploration. Each mineral type is defined by
a characteristic crystal structure, which will give a unique x-ray diffraction
pattern.
Microelectronics industry
As the microelectronics industry uses silicon and gallium arsenide single
crystal substrates in integrated circuit production, there is a need to fully
characterize these materials using the XRD. XRD topography can easily
detect and image the presence of defects within a crystal

//////////////////paste the pic - ----------------Glass industry

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
texture, crystallite size and crystallinity.

Instruments based on X-ray

diffraction
ExoMars X-ray Diffraction
Instrument
ExoMars is a robotic mission developed by the European Space Agency.
As part of the Mars Joint Exploration Initiative with NASA, ExoMars will
launch in 2018 and land on the surface of Mars

Mars analogue sample being loaded into the Space Research

Centre laboratory XRD chamber between the X-ray source and CCD.

The instrument's ability based on XRD allows identification of mineral

structure.
Using a radioactive Fe-55 source, the X-ray beam is targeted at the martian
soil sample with the observing CCD(Charge Coupled
Device(Semiconductor device; CCDs are sensitive to light, and are
therefore used as the light-detecting components) positioned to receive the
X-ray diffraction and fluorescence from the sample.

pic
X-ray diffractometer-

How Does It Work?

X-ray diffractometers consist of three basic elements: an X-ray tube, a
sample holder, and an X-ray detector.
X-rays are generated in a cathode ray tube by heating a filament to
produce electrons, accelerating the electrons toward a target by applying a
voltage, and bombarding the target material with electrons. When electrons
have sufficient energy to dislodge inner shell electrons of the target
material, characteristic X-ray spectra are produced.

Copper is the most common target material for single-crystal diffraction.

These X-rays are collimated and directed onto the sample. As the sample
and detector are rotated, the intensity of the reflected X-rays is recorded.
When the geometry of the incident X-rays impinging the sample satisfies
the Bragg Equation, constructive interference occurs and a peak in
intensity occurs. A detector records and processes this X-ray signal and

converts the signal to a count rate which is then output to a device such as
a printer or computer monitor.