Scribd Logo
Upload

Welcome to Scribd!

  • 23 views

    X-Ray Diffraction

    Uploaded by

    vinushakaveripakam26
    This document discusses X-ray diffraction, including the Bragg equation, instrumentation used in XRD, and various X-ray diffraction methods and applications. Key topics covered include how X-rays are generated, the components of an X-ray diffractometer, and common techniques like powder diffraction and rotating crystal methods.

    Copyright:

    © All Rights Reserved
    Download as PPTX, PDF, TXT or read online from Scribd

    X-Ray Diffraction

    Uploaded by

    vinushakaveripakam26
    23 views29 pages
    This document discusses X-ray diffraction, including the Bragg equation, instrumentation used in XRD, and various X-ray diffraction methods and applications. Key topics covered include how X-rays are generated, the components of an X-ray diffractometer, and common techniques like powder diffraction and rotating crystal methods.

    Original Description:

    Easy to read

    Original Title

    x-ray diffraction

    Copyright

    © © All Rights Reserved

    Available Formats

    PPTX, PDF, TXT or read online from Scribd

    Did you find this document useful?

    Is this content inappropriate?

    This document discusses X-ray diffraction, including the Bragg equation, instrumentation used in XRD, and various X-ray diffraction methods and applications. Key topics covered include how X-rays are generated, the components of an X-ray diffractometer, and common techniques like powder diffraction and rotating crystal methods.

    Copyright:

    © All Rights Reserved
    Download as PPTX, PDF, TXT or read online from Scribd
    Download as pptx, pdf, or txt
    23 views29 pages

    X-Ray Diffraction

    Uploaded by

    vinushakaveripakam26
    This document discusses X-ray diffraction, including the Bragg equation, instrumentation used in XRD, and various X-ray diffraction methods and applications. Key topics covered include how X-rays are generated, the components of an X-ray diffractometer, and common techniques like powder diffraction and rotating crystal methods.

    Copyright:

    © All Rights Reserved
    Download as PPTX, PDF, TXT or read online from Scribd
    Download as pptx, pdf, or txt
    of 29

    X-Ray Diffraction

    CONTENTS
    INTRODUCTION
    BRAGG EQUATION
    INSTRUMENTATION
    X-RAY DIFFRACTION METHODS
    APPLICATIONS
    ELECTROMAGNETIC
    SPECTRUM
    INTRODUCTION
    X-Rays :
     X-rays are short wave length electromagnetic radiations
    produced by the deceleration of high energy electrons or by
    electronic transitions of electrons in the inner orbital of atoms
     X-ray region 0.1to100 A˚
     Analytical purpose 0.7 to 2 A˚
     More energetic (i.e. can penetrate deeper into a material).
     Emitted in a continuous band of white radiation as well as a
    series of discrete lines that are characteristic of the target
    material.
    Characteristic Radiation:
     The characteristic lines in an atom's emission spectra are called K, L, M, ... and
    correspond to the n = 1, 2, 3, ... quantum levels of the electron energy states,
    respectively.
     α lines (n = 2 to n = 1, or n = 3 to n = 2).
     β lines (n = 3 to n = 1 or n = 4 to n = 2).
     Moseley found that :1/λ = K2 [Z - σ]2.

    Electronic energy levels of an atom


    GENERATION OF X-RAYS

     Generated by bombarding a metal target with an energetic beam of electrons.

     Synchrotrons:
    Very expensive to build and maintain.

     By use of radioactive source like 55Fe.

     A new method of generating X rays that is not yet commercially available


    uses an electron-impact beam impinging on a stream of liquid gallium.

     X rays may also be produced while unrolling adhesive tape from a tape
    dispenser.
    X-RAY TECHNIQUES
    X-ray absorption methods
     Fraction of X-ray photons absorbed is considered.
     Used in elemental analysis and thickness measurements.
    X-ray fluorescence methods
     Wavelength and intensity of generated X-rays are measured for
    qualitative and quantitative analysis.
     Non-destructive and requires little sample preparation.
    X-ray diffraction methods
     Scattering of X-rays by crystals.
     Determines crystalline structure.
    X-RAY DIFFRACTOMETER

    The Bruker-D8 diffractometer


    BRAGG’s EQUATION
    Constructive interference of the reflected beams emerging from two different planes will
    take place if the difference in path lengths of two rays is equal to whole number of
    wavelengths.
    Deviation = 2

    Ray 1

    Ray 2  

     d

    dS
    in

     The path difference between ray 1 and ray 2 = 2d Sin


     For constructive interference: n = 2d Sin
    INSTRUMENTATION
     X-ray source:1.Crooke’s tube
    2.Coolidge tube

     Collimator

     Monochromator-1.Filter type
    2.Crystal type
     Detectors:
    a)Photographic methods
    b)Counter methods:
    1.Geiger-muller counter
    2.Proportional counter
    3.Scintillation counter
    4.Solid-state semi-conductor detector
    5.Semi conductor detectors
    INSTRUMENTATION OF XRD
    X-RAY SOURCE
    Crookes tube
    Called as cold cathode tube.
    Electrons are generated by ionization of
    the residual air in the tube, instead of
    heated filament.
    An aluminum cathode plate at one end of
    the tube created a beam of electrons, which
    struck a platinum anode target at the center
    generating X-rays.
    Advantage
    Point source X-rays, which resulted in
    sharper images.
    Crookes tube
    Disadvantage :Unreliable
    Coolidge tube
    Called as hot cathode tube.
    Works with a very good quality vacuum (about 10-4 Pa,
    The electrons are produced by thermionic effect from a tungsten filament heated
    by an electric current.
    There are two designs:
    1.End-window tubes: Have thin "transmission target" to allow X-rays to pass
    through the target
    2.side-window tubes:An Electrostatic Lens to focus the beam onto a very small spot
    on the anode.
    • A window designed for escape of the generated X-ray photons.
    • Power 0.1 to 18 kW.
    COLLIMATOR

    Inserted in the diffracted-beam to get a


    narrow x-ray beam.
    It consists two sets of closely
    packed metal plates seperated by a gap.
    The left end of the collimator shown is
    mounted on the X-ray tube.
     The yellow-colored region at the left
    end determines the the size of the beam.
    The green region at the right end
    removes parasitic radiation.
    MONOCHROMATOR

    Filter
    MATERIALS USED:NACL,LIF,QUARTZ ETC,.
    type
    A window that absorbs undesirable radiation and
    allows required wavelength to pass.
    Eg:Zr absorbs x-rays emitted by Mo.
    Crystal type
    Positioned in the x-ray beam so that the angle of
    the reflecting planes satisfied the Bragg’s equation
    for the required wave length.
    Characteristics of a crystal:
    Mechanically strong and stable
    The mosaicity and resolution of the crystal,
    should be small.
    DETECTORS
    Photographic methods
    Contains photographic plate
    Blackening of developed film is expressed in terms of density ,D
    D=Log Io/I.

    Photostimulable phosphors
    An increasingly common method is the use of photo stimulated luminescence
    Photostimulable phosphor plate (PSP plate) is used in place of the photographic plate.
    After the plate is X-rayed, excited electrons in the phosphor material remain ‘trapped'
    in'colour centres' in the crystal lattice until stimulated by a laser beam passed over the plate
    surface.
    The light given off during laser stimulation is collected by a photomultiplier tube

    ADVANTAGE:The PSP plate can be reused


    Counter methods
    1.Geiger-muller counter:
    Filled with an inert gas like argon.
    Measures ionizing radiation.
    Detect the emission of nuclear
    radiation: alpha particles,
    beta particles or gamma rays
    Advantages:
    a)Trouble free
    b)Inexpensive
    Disadvantages:
    a)Cannot be used to measure
    energy of ionizing radiation.
    b)Used for low counting rates
    2.Proportional counter:
    Filled with heavier gas like xenon
    or krypton as it is easily ionized.
    Output pulse is dependent on
    intensity of X-rays falling on
    counter.
    Count the particles of ionizing
    radiation and measures their energy.
    Advantages:
    a)Count high rates with out
    significant error.
    Disadvantages:
    a)Associated electronic circuit is
    complex.
    b)Expensive.
    3.Scintillation counter:
    Measures X-rays of shorter
    wavelengths.
    The sensor, called a scintillator,
    consists of a transparent crystal,
    usually phosphor, plastic (usually
    containing anthracene), or
    organic liquid that fluoresces when
    struck by ionizing radiation.
    The PMT is attached to an
    electronic amplifier to count and
    possibly quantify the amplitude of
    the signals.
    Advantages:
    a)Count high rates.
    4.Solid state semi-conductor detector:
     The electrons produced by X-ray beam are promoted into
    conduction bands and the current which flows is directly
    proportional to the incident X-ray energy.
    Disadvantage:
     Maintainted at very low Temp to minimise the noise and prevent
    deterioration of the detector.
    5.Semi-conductor detectors:
     Silicon-lithium drifted detector.

     The principle is similar to gas

    ionization detector.
     Voltage of pulse=Q/C

    Application: In neutron activation


    Semi-conductor detector
    analysis
    X-RAY DIFFRACTION METHODS
    1.LAUE PHOTOGRAPHIC METHOD:
    The Laue method is mainly used to determine the orientation of large single
    crystals. White radiation is reflected from, or transmitted through, a fixed
    crystal.
     Back-reflection Laue  Transmission Laue
    In the back-reflection method, The film is placed behind the
    the film is Placed between X- crystal to record beams which are
    transmitted through the crystal.
    ray source and crystal.
    The beams which are diffracted
    in a backward direction are
    recorded.

    Disadvantage: Big crystals are required


    Back-reflection Laue Transmission Laue

    Crystal orientation and perfection is determined from the position of spots.


    2.BRAGG X-RAY SPECTROMETER METHOD:

    Bragg analysed the


    structures of Nacl,Kcl and
    ZnS.

    Method is based on Bragg’s


    law.

    The strength of ionisation


    current is directly proportional
    to intensity of entering
    reflected X-rays.

    SO2 or CH3I increases


    ionisation in the chamber.
    3.ROTATING CRYSTAL METHOD:

    Shaft is moved to put the


    crystal into slow rotation.
    This cause sets of planes
    coming successively into their
    reflecting position.
    Each plane will produce a
    spot on the photographic plate.
    Can take a photograph of the
    diffraction pattern in two ways
    1.complete rotation method

    2.oscillation method
    4.POWDER CRYSTAL METHOD:

    1mg material is sufficient for study.


    Applications: useful for
    Cubic crystals.
    Determining complex structures of metals and alloys.
    Making distinction between allotropic modification of the same substance.
    APPLICATIONS
    Structure of crystals
    Polymer characterization
    State of anneal in metals
    Particle size determination
    Spot counting method
    v=V.δθ.cosθ/2n
    Broadening of diffraction lines
    Low-angle scattering
    Applications of diffraction methods to complexes
    Determination of cis-trans isomerism
    Eg:Bis(pyridine-2-carboxamido)nickel(II) chloride
    Determination of linkage isomerism
    Eg:Biuret+copper(II)=pottassium bis(biureto)cuprate(II)
    tetrahydrate
    MISCELLANEOUS APPLICATIONS
     Soil classification based on crystallinity.
     Analysis of industrial dusts.

     Assessment of weathering & degradation of minerals &


    polymers.
     Study of corrosion products.

     Examination of tooth enamel & dentine.

     Examination of bone state & tissue state.

     Structure of DNA&RNA.

     X-ray Diffraction on aerosol drugs -


    Measurements on small quantities of pharmaceutical
    samples using the X'Celerator detector.
    REFERENCES
    1)Instrumental methods of chemical analysis ,B.K.sharma,17 th

    edition 1997-1998,GOEL publishing house.page no:329-359

    2)Principles of instrumental analysis,5th edition ,by Dougles


    a.skoog,f.James holles,Timothy A.Niemen.page no:277-298

    3)Instrumental methods of chemical analysis ,Gurudeep


    R.chatwal,sham k.anand,Himalaya publications page no:2.303-
    2.332

    4) Instrumental Methods Of Chemical Analysis –


    H. Kaur pg.no:727-729,737

    5) http://www.scienceiscool.org/solids/intro.html

    6) http://en.wikipedia.org/wiki/X-ray_crystallography
    Thank you

    You might also like