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c X-ray diffraction and applications

DOA: 18-02-2010

DOR: 02-04-2010

DOS: 08-05-2010



Deptt. Of Physics Roll. No.:-- RD6902B60

Reg.No. -- 10903598

Class: -- D6902





X-radiation (composed of X-rays) is a form of electromagnetic radiation. X-rays have a

wavelength in the range of 10 to 0.01 nanometers, corresponding to frequencies in the range 30
petahertz to 30 exahertz (3 × 1016 Hz to 3 × 1019 Hz) and energies in the range 120 eV to 120
keV. They are shorter in wavelength than UV rays. In many languages, X-radiation is called
Röntgen radiation, after Wilhelm Conrad Röntgen, who is generally credited as their discoverer,
and who had named them X-rays to signify an unknown type of radiation.X-rays from about 0.12
to 12 keV (10 to 0.10 nm wavelength), are classified as "soft" X-rays, and from about 12 to 120
keV (0.10 to 0.010 nm wavelength) as "hard" X-rays, due to their penetrating abilities.


X-ray diffraction (XRD) is a versatile, non-destructive technique that reveals detailed information about
the chemical composition and crystallographic structure of natural and manufactured materials In an X-
ray diffraction measurement, a crystal is mounted on a goniometer and gradually rotated while
being bombarded with X-rays, producing a diffraction pattern of regularly spaced spots known as
reflections. The two-dimensional images taken at different rotations are converted into a three-
dimensional model of the density of electrons within the crystal using the mathematical method
of Fourier transforms, combined with chemical data known for the sample. Poor resolution
(fuzziness) or even errors may result if the crystals are too small, or not uniform enough in their
internal makeup

Diffraction occurs as waves interact with a regular structure whose repeat distance is about the
same as the wavelength. The phenomenon is common in the natural world, and occurs across a
broad range of scales. For example, light can be diffracted by a grating having scribed lines
spaced on the order of a few thousand angstroms, about the wavelength of light.

It happens that X-rays have wavelengths on the order of a few angstroms, the same as typical
interatomic distances in crystalline solids. That means X-rays can be diffracted from minerals
which, by definition, are crystalline and have regularly repeating atomic structures.
When certain geometric requirements are met, X-rays scattered from a crystalline solid can
constructively interfere, producing a diffracted beam. In 1912, W. L. Bragg recognized a
predicatable relationship among several factors.

1. The distance between similar atomic planes in a mineral (the interatomic spacing) which we
call the d-spacing and measure in angstroms.

2. The angle of diffraction which we call the theta angle and measure in degrees. For practical
reasons the diffractometer measures an angle twice that of the theta angle. Not surprisingly, we
call the measured angle '2-theta'.

3. The wavelength of the incident X-radiation, symbolized by the Greek letter lambda and, in our
case, equal to 1.54 angstroms.


A diffractometer can be used to make a diffraction pattern of any crystalline solid. With a
diffraction pattern an investigator can identify an unknown mineral, or characterize the atomic-
scale structure of an already identified mineral.

There exists systematic X-ray diffraction data for thousands of mineral species. Much of these
data are gathered together and published by the JCPDS-International Centre for Diffraction Data.
The diffractometer in the IPFW Geosciences Department is a Philips APD3520 built in 1986. It
consists of several parts.

i The chiller provides a source of clean water to cool the X-ray tube.
i The regulator smooths our building current to provide a steady and dependable source of
electricity to the diffractometer and its peripherals.
i The computer sends commands to the diffractometer and records the output from an
analysis. We are currently using a 486-100 running DR-DOS7 to run the diffractometer,
and provide interfacing with this web page. We process most of the information digitally,
although we can make hardcopy analog patterns directly on the;
i Strip-chart recorder.
i The tube provides an X-ray source. (An old tube, shown upside down, is on the counter
top.) Inside there is a 40,000 volt difference between a tungsten filament and copper
target. Electrons from the filament are accelerated by this voltage difference and hit the
copper target with enough energy to produce the characteristic X-rays of copper. We use
one part of the copper spectrum (with a wavelength of 1.54 angstrom) to make the
diffraction pattern. The radiation is monochromatized by a graphite crystal mounted just
ahead of the scintillation counter.
i The theta compensating slit collimates the X-rays before they reach the sample.
i The sample chamber holds the specimen. We grind our samples to a fine powder before
mounting them in the diffractometer, and then close the chamber to allow the collimated
X-rays to enter from the left. The X-rays hit and scatter from the sample. The diffracted
beams leave the chamber to the right where they can be detected by the;
i Scintillation counter which measures the X-ray intensity. It is mounted on the;
i Goniometer which literally means angle-measuring device. The goniometer is motorized
and moves through a range of 2-theta angles. Because the scintillation counter is
connected to the goniomter we can measure the X-ray intensity at any angle to the
specimen. That's how we determine the 2-theta angles for Braggs's Law.

A diffraction pattern records the X-ray intensity as a function of 2-theta angle. All the diffraction
patterns you'll see on this web site were prepared as step-scans. To run a step-scan we mount a
specimen, set the tube voltage and current, and enter the following parameters:

--A starting 2-theta angle.

--A step-size (typically 0.005 degrees).
--A count time per step (typically 0.05-1 second).
--An ending 2-theta angle.

Once started, the goniometer moves through its range, stopping at each step for the alotted time.
The X-ray counts at each step are saved to a file on the computer. Once finished, the data are
smoothed with a weighted moving average and a diffractogram like the one below is printed or
Consider the following areas on the diffractogram.

A. The diffraction pattern is labelled with the sample name and other information pertinent to the
experiment. This happens to be a pattern of ground calcite from the France Stone Quarry in Fort
Wayne, Indiana. The sample was randomly mounted using the backpack technique. The
diffraction pattern was prepared on March 24, 1993. The diffractometer was running at 40 kv
and 30 ma. Steps were in increments of 0.005 degrees, and counts were collected for 0.25
seconds at each step. The data were smoothed with a 15-pt (weighted, moving average) filter.

B. The vertical axis records X-ray intensity. The horizontal axis records angles in degrees 2-
theta. Low angles (large d-spacings) lie to the right.

C. This is one of the X-ray peaks. It happens to be the one with the smallest angle which I
measured as 23.04 degrees. Solving Bragg's Law (with n=1 and wavelength=1.54 ang) we find
that 23.04 degrees 2-theta corresponds to a d-spacing of 3.86 angstrom.

D. This is another peak picked for no special reason. I measured the peak at 39.37 degrees 2-
theta. This corresponds to a d-spacing of 2.287 angstrom.
E. This is the largest peak on the pattern. It actually extends several times the height of this
image. Many factors affect the intensity of a given peak. Some of these factors are intrinsic to the
mineral under study; some of these factors are peculiar to the way a specimen is mounted in the
diffractometer. (The random/backpack mounting method limits, but does not eliminate, these
peculiarities). You can see a partial list of calcite peaks.

When solving scientific problems it is often useful to ask three questions: What do I Know?
What can I measure? What do I want to find out?
In Bragg's law:

1. we know lambda (the wavelength) = 1.54 angstrom and we assume n=1.

2. We can measure 2-theta from the diffraction pattern. Divided by 2, these values become theta.

3. That leaves us with an equation with one unknown -d- the d-spacing we want to find out.


X-ray diffraction finds the geometry or shape of a molecule using X-rays. X-ray diffraction
techniques are based on the elastic scattering of X-rays from structures that have long range
order. The most comprehensive description of scattering from crystals is given by the dynamical
theory of diffraction.

i Single-crystal X-ray diffraction is a technique used to solve the complete structure of

crystalline materials, ranging from simple inorganic solids to complex macromolecules,
such as proteins.
i Powder diffraction (XRD) is a technique used to characterise the crystallographic
structure, crystallite size (grain size), and preferred orientation in polycrystalline or
powdered solid samples. Powder diffraction is commonly used to identify unknown
substances, by comparing diffraction data against a database maintained by the
International Centre for Diffraction Data. It may also be used to characterize
heterogeneous solid mixtures to determine relative abundance of crystalline compounds
and, when coupled with lattice refinement techniques, such as Rietveld refinement, can
provide structural information on unknown materials. Powder diffraction is also a
common method for determining strains in crystalline materials. An effect of the finite
crystallite sizes is seen as a broadening of the peaks in an X-ray diffraction as is
explained by the Scherrer Equation.
i Thin film diffraction and grazing incidence X-ray diffraction may be used to characterize
the crystallographic structure and preferred orientation of substrate-anchored thin films.
i High-resolution X-ray diffraction is used to characterize thickness, crystallographic
structure, and strain in thin epitaxial films. It employs parallel-beam optics.
i X-ray pole figure analysis enables one to analyze and determine the distribution of
crystalline orientations within a crystalline thin-film sample.
i X-ray rocking curve analysis is used to quantify grain size and mosaic spread in
crystalline materials.

This is an X-ray diffraction pattern formed when X-rays are focused on a crystalline material, in
this case a protein. Each dot, called a reflection, forms from the coherent interference of scattered
X-rays passing through the crystal.

APPLICATIONS:-- X-ray diffraction is a very important method to characterize the structure

of crystalline material. The technique can typically be used for the lattice parameters analysis of
single crystals, or the phase, texture or even stress analysis of polycrystalline materials (like
powders). The technique is widely used in research and development applications and its use for
production or quality control issues is also growing, benefiting from developments in hardware
and software for high throughput capability.
Most of the applications of X-ray diffractometry require a beam with well defined spatial and
spectral characteristics. X-ray optics is a critical component for obtaining the required beam
specifications at the sample. Multilayer X-ray optics are now widely used in X-ray diffraction
due to their balanced performance in terms of divergence, spectral purity, and flux.

X-ray diffraction can be used in many ways for the study of new materials, often only available
in very small amounts. Recent breakthroughs in X-ray diffraction instrumental development,
such as RTMS detection technology and the implementation of mono-capillary have reduced
measurement times and minimum amounts of material required considerably. Many X-ray
diffraction techniques are at disposal of the nanoscientist for the structural characterization of the
nanomaterials, such as high-resolution diffraction, reflectometry, small-angle X-ray scattering
and line profile analysis.

A very large reflecting diffraction grating.

In optics, a diffraction grating is an optical component with a regular pattern, which splits and
diffracts light into several beams travelling in different directions. The directions of these beams
depend on the spacing of the grating and the wavelength of the light so that the grating acts as
the dispersive element. Because of this, gratings are commonly used in monochromators and

A photographic slide with a fine pattern of black lines forms a simple grating. For practical
applications, gratings generally have grooves or á  on their surface rather than dark lines.
Such gratings can be either transparent or reflective. Gratings which modulate the phase rather
than the amplitude of the incident light are also produced, frequently using holography.
The principles of diffraction gratings were discovered by James Gregory, about a year after
Newton's prism experiments, initially with artifacts such as bird feathers. The first man-made
diffraction grating was made around 1785 by Philadelphia inventor David Rittenhouse, who
strung hairs between two finely threaded screws. This was similar to notable German physicist
Joseph von Fraunhofer's wire diffraction grating in 1821.

Other applications

i Protein Crystallography - with Xenocs optics on RAG

i Protein Crystallography - with Xenocs source
i Small molecule Crystallography
i High Pressure
i High Resolution
i Microdiffraction