Introduction
Definition
History
Principle
Instrumentation
Methods
Applications
Advantages
Limitation
Conclusion
References
X-ray diffraction (XRD) is one of the most important non-destructive tools to analyze all kinds of matter—ranging from fluids, to powders and crystals. From research t...
Introduction
Definition
History
Principle
Instrumentation
Methods
Applications
Advantages
Limitation
Conclusion
References
X-ray diffraction (XRD) is one of the most important non-destructive tools to analyze all kinds of matter—ranging from fluids, to powders and crystals. From research to production and engineering, XRD is an indispensable method for materials characterization and quality control.
X-ray diffraction techniques are used for the identification of crystalline phases of various materials and the quantitative phase analysis subsequent to the identification.
X-ray diffraction techniques are superior in elucidating the three-dimensional atomic structure of crystalline solids.
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1 x-ray diffraction By KAUSHAL KUMAR SAHU Assistant Professor (Ad Hoc) Department of Biotechnology Govt. Digvijay Autonomous P. G. College Raj-Nandgaon ( C. G. )
INTRODUCTION X-ray diffraction (XRD) is one of the most important non-destructive tools to analyze all kinds of matter—ranging from fluids, to powders and crystals. From research to production and engineering, XRD is an indispensable method for materials characterization and quality control . X-ray diffraction techniques are used for the identification of crystalline phases of various materials and the quantitative phase analysis subsequent to the identification. X-ray diffraction techniques are superior in elucidating the three-dimensional atomic structure of crystalline solids. 3
DEFINITION The atomic plans 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. 4
HISTORY X-ray were discovered in 1895 by the German physicist Wilhelm Conrad Rontgen and were so named because their nature was unknown at the time. He was awarded the Nobel Prize for physics in 1901. 1912: Max Theordor Felix von Laue (1879-1960) (U of Munich) thought that X-ray has a wavelength similar to interatomic distances in crystals and the crystal should act like a 3D diffraction grating. Along with Walter Friedrich (research assistant) and Paul Knipping (PhD grad student), he did the first diffraction experiment on CuSO4 crystal – Nobel Prize in Physics. 5
PRINCIPLE X-ray diffraction is based on constructive interference of monochromatic x-rays and a crystalline sample. These x-rays are generated by a cathode ray tube, filtered to produce monochromatic radiation, collimated to concentrate and directed towards the sample. The interaction of incident rays with the sample produces constructive interference when conditions satisfy Bragg’s law . 6
BRAGG’S LAW In physics , Bragg's law , or Wulff –Bragg's condition , a special case of Laue diffraction , gives the angles for coherent and incoherent scattering from a crystal lattice. When X-rays are incident on an atom , they make the electronic cloud move as does any electromagnetic wave . The movement of these charges re-radiates waves with the same frequency , blurred slightly due to a variety of effects; this phenomenon is known As Rayleigh scattering (or elastic scattering). These re-emitted wave fields interfere with each other either constructively or destructively (overlapping waves either add up together to produce stronger peaks or are subtracted from each other to some degree), producing a diffraction pattern on a detector or film. The resulting wave interference pattern is the basis of diffraction analysis. This analysis is called Bragg diffraction . 7
BRAGG’S EQUATION nΛ = 2d sinΘ where, Λ = the wavelength of the x-ray d = the spacing of the crystal layers (path difference) θ = the incident angle (the angle between incident ray and the scatter plane) n = an integer 8
production of x- rays collimator Monochromator Filter Crystal monochromator Detectors Photographic methods Counter methods INSTRUMENTATION 9
PRODUCTION OF X- RAYS 10
COLLIMATOR 11
MONOCHROMATORS In order to do monochromatization 2 methods are available:- Filter Crystal monochromator Flat crystal monochromator Curved crystal monochromator 12
The x-ray intensities can be measured and recorded either by Photographic methods Counter methods Geiger – Muller tube counter Proportional counters Scintillation detector Solid state semiconductor detector Semi-conductor detectors DETECTORS 13
Geiger – Muller tube counter 14
Scintillation detector 15
Semi –conductor detectors 16
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X- RAY DIFFRACTION METHODS These are generally used for investigating the internal structures and crystal structures of various solid compounds. They are Laue’s photographic method Transmission method Back reflection method Bragg’s x- ray spectrometer method Rotating crystal method Powder method 18
Transmission Laue method 19
Bragg’s x-ray spectrometer method 20
Rotating crystal method 21
Powder crystal method 22
APPLICATION Structure of crystal Polymer characterization State of anneal in metals Particle size determination 23
ADVANTAGE It is a powerful and rapid technique. Less sample required. Unknown determination. 24
LIMITATION XRD also has size limitations. It is much more accurate for measuring large crystalline structures rather than small ones. 25
CONCLUSION For materials including metals, minerals, plastics, pharmaceuticals and semiconductors XRD apparatus provide highly accurate tools for non-destructive analysis. The diffraction systems are also supported by an extensive range of application software. 26