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X-rays are high energy electromagnetic radiation .

Diffraction occurs when each object in periodic array scatters radiation coherently producing concerted constructive interference at specific angles

X-ray diffraction (XRD) is a non-destructive technique that operates on the nanometre scale based on the elastic scattering of X-rays from structures that have long range order. Or Using the principle of diffraction Measurement of crystal geometry by using X-rays as a source. 2

Wave length of X-ray in EMR is of about 0.1 100 A Analytical scale wavelength ranges from 0.7 2 A

1895 X-rays discovered by Roentgen 1914 First diffraction pattern of a crystal made by Knipping and 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 first X-ray

Motivation: X-ray diffraction is used to obtain structural information about crystalline solids. Useful in biochemistry to solve the 3D structures of complex biomolecules. Bridge the gaps between physics, chemistry, and biology.

X-ray diffraction is important for: Solid-state physics Biophysics Medical physics Chemistry and Biochemistry
X-ray Diffractometer

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X-rays are high energy electromagnetic radiation . X-rays are in the wavelength range of 0.1 to 100 A. For analytical purpose 0.7 to 2 Aare used. X-ray technique are of 3 types:

X-ray absorption method X-ray diffraction method X-ray fluorescence method


By striking a metal target

Beam of electrons Metal Target X-rays

2. 3.

From radioactive source Production of x-rays by striking of a substance to a primary beam of x-rays & causes liberation of secondary beam of x-rays.

Energy level diagram for a hypothetical atom Electronic structure of an atom

Interaction of x-ray with matter: They are 3 types: 1. Absorption 2. Fluorescence 3. Scattering & diffraction

If a beam of x-rays is allowed to pass through matter , it loses energy partly by scattering & partly by true absorption. X-rays means that the electron of the atoms constituting the matter absorbs energy from these rays & get excited. These excited electrons emit secondary radiation characteristic of those atoms. 9

The absorption of x-rays follows the BEERS LAW ; I=Io e


I0=Incident intensity of x-rays I=Intensity after passing through the absorbing sample L = thickness of material, cm =mass absorption co-efficient ,cm2/g P= the density of the absorbing material


If a sample is irradiated with an x-ray beam, the sample sometimes emits other x-ray beams; this process is called x-ray fluorescence . Its WAVELENGTH enables us to determine Qualitative aspect Its INTENSITY enables us to determine Quantitative aspect

when a beam of x-radiation is incident upon a substance , the electrons constituting the atoms of the substance become as small oscillators. These, on oscillating at the same frequency as that of incident x-radiation, emit electromagnetic radiations at the same frequency as the incident x-radiation

n = AB + BC n = 2d sin

The space between diffracting planes of atoms determines peak positions. The peak intensity is determined by what atoms are in the diffracting plane.

William Henry Bragg

William Lawrence Bragg

BRAGGS were awarded NOBEL PRIZE in PHYSICS in 1915 for their work in determining crystal structure beginning with Nacl, ZnS and Diamond.


Laue photographic method Bragg s method Rotating crystal method



1. 2. 3. 4.

Cobalt Copper Molybdenum Chromium


These are used to get narrow beam of X-rays from an X ray tube. These are made of a series of closely spaced parallel metal plates. These are placed in between the analyzing crystals.


A filter is a window of material that absorbs undesirable wavelength but allows radiation of required wavelength to pass.

Crystal monochromator:

crystals are used as grating monochromator. It splits the beam into component wavelength in same as that of prism. This crystalline substance is called as analyzing crystal.


Soller slits after the monochromator keep divergence of the beam to a minimum. The discriminator is a crystal monochromator such as graphite.

Are used to limit the divergence of the incident X-ray beam.

y The size of the divergence slit influences peak intensity and peak shapes. y
Reduce the intensity of the X-ray beam y Reduce the length of the X-ray beam hitting the sample y Produce sharper peaks

The instrumental resolution is improved so that closely spaced peaks 20 can be resolved.

Solid samples are used. Amorphous Crystalline Solids are used Sample holders are glass plates and samples are adhered by glue on the glass plate


Photographic detector:
It is used to quantitative comparison of X-ray intensities & for diffraction studies. A photographic film is used to record diffraction pattern. D = log Io / I Io = incident X-rays I = transmitted X- rays And D is calculated by densitometer.

It is useful for measuring the X-rays of shorter wavelength. Crystals used in these detector include sodium iodide, anthracene,

naphthalene and p- terphenol in xylene


 comprises a cylindrical metallic tube in the middle of which a thin wire (counting wire) is mounted.  This tube is filled with a suitable gas (e.g. Ar + 10% CH4)  Positive ions move to the cathode (the metallic tube),  The free electrons to the anode (the wire).  The number of electron-ion pairs created is proportional to the energy of the X-ray quantum 24

Used to record the signal obtained form detector And the unknown compound is identified by comparing with the library / data base


y Useful for determination of cubic crystal. y Used for determination of complex structure of metals & alloys. y Used to make distinction between the allotropic modifications of the same

y X-ray powder diffraction used for identification of crystalline compunds by

their diffraction patterns.

y Identification & structural analysis of clay materials. y Identification of multiple phases in microcrystalline mixtures.

y X- ray crystallography is a method of determining the arrangement of atoms within a crystal, in which a beam of Xrays strikes a crystal and diffracts into many specific directions. y From the angle and intensities of these diffracted beams, a crystallographer can produce a 3-D picture of the density of electrons within a crystal. y Materials of crystals such as salts, metals, minerals, semiconductors.


y To determine the size of atoms y Length and types of chemical bonds y It also reveals the structure and function of biological molecules including vitamins, drugs, proteins and nucleic acids.


y Structure of crystals y Polymer Characterization y State of anneal in metals y Particle size determination y Determination of Cist- Trans isomerism y It is also used to asses the weathering & degradation of natural & synthetic minerals.


y In determination of linkage isomerism. y The solids are classified based on the degree of crystallinity. y Corrosion products can be studied by this method. y Tooth enamel & dentine have been examined by X-ray diffraction. y X-ray diffraction was a major tool in elucidating the structure of RNA & DNA.


y H. Kaur Instrumental Methods Of Chemical Analysis Published by

Pragathi prakashan, meerut, 2006, third edition,737

y GURDEEP R. CHATWAL SHARM K. ANAND Instrumental Methods Of

Chemical Analysis published by Himalaya publishing house New Delhi , 2006 5th edition.
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