MATERIAL CHARACTERISATIONS
XRD,SEM AND AFM
BY
CHANDAN
M150478ME
MATERIALS SCIENCE
AND TECHNOLOGY
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X RAY DIFFRACTION
• A technique used to determine the atomic and molecular structure
of a crystal, in which the crystalline atoms cause a beam of
incident x-rays to diffract into many specific directions.
• 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.
• A stream of x-rays directed at a crystal diffract and scatter as they
encounter atoms. the scattered rays interfere with each other and
produce spots of different intensities that can be recorded on film.
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BRAGG’S EQUATION
WORKING PRINCIPLE
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the path difference between ray 1 and ray 2 = 2d sin
“constructive interference of the reflected beams emerging from two
different planes will take place if the path lengths of two rays is equal
to whole number of wavelengths”.
for constructive interference,
nλ=2dsin
this is called as bragg’s law
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SETUP OF INSTRUMENTS
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DIFRACTION FROM SINGL CRYSALS
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DIFRACTION FROM POWDER CRYSTALS
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APPLICATION OF XRD
• Structure of crystals
• Polymer characterization
• Particle size determination
• Applications of diffraction methods to complexes
I. Determination of cis-trans isomerism
II. Determination of linkage isomerism
• Miscellaneous applications
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SCANNING ELECTRON MICROSCOPE
• Electron microscopes (SEM) are scientific instruments that use
a beam of energetic electrons to examine objects on a very
fine scale.
• Electron microscopes (SEM) were developed due to the
limitations of light microscopes which are limited by the
physics of light.
• Electron microscopes (SEM) have a greater resolving power than
a light-powered optical microscope, because electrons have
wavelengths about 100,000 times shorter than visible light .
• Magnifications of up to about 10,000,000x.
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PRINCIPLE OF WORKING
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LIMITATIONS
• SEM cannot detect very light elements (H, He, and Li).
• Samples must be solid and they must fit into the microscope chamber.
maximum size in horizontal dimensions is usually on the order of 10
cm, vertical dimensions should not exceed 40 mm.
• Very high vacuum, vibration free, large space.
• An electrically conductive coating must be applied to electrically
insulating samples .
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E COLLISION SCATTERING AUGER EFFECT
INTERACTION OF ELECTRON WITH
SAMPLE
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APPLICATIONS
• Topography and morphology
• Chemistry
• Crystallography
• Orientation of grains
• In-situ experiments
I. Reactions with atmosphere
II. Effects of temperature
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Morphology and
Topography
Fe Ce Sr
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IN-SITU IMAGING
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ATOMIC FORCE MOCROSCOPY
• AFM works by scanning a probe over the sample surface,
building up a map of the height or topography of the surface as it
goes along
• No need of focusing, illumination, depth of field.
• It also have height information that make it simple to quickly
measure the height, volume, width of any feature in the sample.
• It physically feels the sample’s surface with a sharp probe,
building up a map of the height of samples surface.
• It provides single atomic level structure so provide high
resolution.
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18
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LIMITATIONS
• AFM can only image a maximum height on the order of 10-20
micrometers and a maximum scanning area of about 150×150
micrometers.
• The scanning speed of an AFM is also a limitation.
• Highly dependent on AFM probes.
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COMPARISIONS
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SR. NO. XRD SEM AFM
SAMPLES CONDUCTIVE /
INSULATING /
SEMI CONDUCTER
MUST BE
CONDUCTIVE
CONDUCTIVE/
INSULATING
MAGNIFICATION 2 DIMENSIONAL 2 DIMENSIONAL 3 DIMENSIONAL
ENVIORNMENT VACUUM VACUUM VACUUM/ AIR/
LIQUID
TIME FOR IMAGE 3- 5 min 0.1 - 1 min 1-5 min
HORIZONTAL
REVOLUTION
5 nm 5 nm 2 nm
VERTICAL
REVOLUTION
- - 0.05 nm
FIELD OF VIEW 1 mm 1mm 0.01 mm
DEPTH OF FIELD GOOD GOOD POOR
CONTRAST ON
FLATE SURFACE
POOR POOR GOODNITC MED
THANK YOU……
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Material characterisations

  • 1.
    MATERIAL CHARACTERISATIONS XRD,SEM ANDAFM BY CHANDAN M150478ME MATERIALS SCIENCE AND TECHNOLOGY 1 NITC MED
  • 2.
    X RAY DIFFRACTION •A technique used to determine the atomic and molecular structure of a crystal, in which the crystalline atoms cause a beam of incident x-rays to diffract into many specific directions. • 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. • A stream of x-rays directed at a crystal diffract and scatter as they encounter atoms. the scattered rays interfere with each other and produce spots of different intensities that can be recorded on film. NITC MED 2
  • 3.
  • 4.
    the path differencebetween ray 1 and ray 2 = 2d sin “constructive interference of the reflected beams emerging from two different planes will take place if the path lengths of two rays is equal to whole number of wavelengths”. for constructive interference, nλ=2dsin this is called as bragg’s law 4 NITC MED
  • 5.
  • 6.
    DIFRACTION FROM SINGLCRYSALS 6 NITC MED
  • 7.
    DIFRACTION FROM POWDERCRYSTALS 7 NITC MED
  • 8.
    APPLICATION OF XRD •Structure of crystals • Polymer characterization • Particle size determination • Applications of diffraction methods to complexes I. Determination of cis-trans isomerism II. Determination of linkage isomerism • Miscellaneous applications NITC MED 8
  • 9.
    SCANNING ELECTRON MICROSCOPE •Electron microscopes (SEM) are scientific instruments that use a beam of energetic electrons to examine objects on a very fine scale. • Electron microscopes (SEM) were developed due to the limitations of light microscopes which are limited by the physics of light. • Electron microscopes (SEM) have a greater resolving power than a light-powered optical microscope, because electrons have wavelengths about 100,000 times shorter than visible light . • Magnifications of up to about 10,000,000x. NITC MED 9
  • 10.
  • 11.
    LIMITATIONS • SEM cannotdetect very light elements (H, He, and Li). • Samples must be solid and they must fit into the microscope chamber. maximum size in horizontal dimensions is usually on the order of 10 cm, vertical dimensions should not exceed 40 mm. • Very high vacuum, vibration free, large space. • An electrically conductive coating must be applied to electrically insulating samples . NITC MED 11
  • 12.
    E COLLISION SCATTERINGAUGER EFFECT INTERACTION OF ELECTRON WITH SAMPLE 12 NITC MED
  • 13.
  • 14.
    APPLICATIONS • Topography andmorphology • Chemistry • Crystallography • Orientation of grains • In-situ experiments I. Reactions with atmosphere II. Effects of temperature NITC MED 14
  • 15.
  • 16.
  • 17.
    ATOMIC FORCE MOCROSCOPY •AFM works by scanning a probe over the sample surface, building up a map of the height or topography of the surface as it goes along • No need of focusing, illumination, depth of field. • It also have height information that make it simple to quickly measure the height, volume, width of any feature in the sample. • It physically feels the sample’s surface with a sharp probe, building up a map of the height of samples surface. • It provides single atomic level structure so provide high resolution. NITC MED 17
  • 18.
  • 19.
  • 20.
    LIMITATIONS • AFM canonly image a maximum height on the order of 10-20 micrometers and a maximum scanning area of about 150×150 micrometers. • The scanning speed of an AFM is also a limitation. • Highly dependent on AFM probes. NITC MED 20
  • 21.
    COMPARISIONS 21 SR. NO. XRDSEM AFM SAMPLES CONDUCTIVE / INSULATING / SEMI CONDUCTER MUST BE CONDUCTIVE CONDUCTIVE/ INSULATING MAGNIFICATION 2 DIMENSIONAL 2 DIMENSIONAL 3 DIMENSIONAL ENVIORNMENT VACUUM VACUUM VACUUM/ AIR/ LIQUID TIME FOR IMAGE 3- 5 min 0.1 - 1 min 1-5 min HORIZONTAL REVOLUTION 5 nm 5 nm 2 nm VERTICAL REVOLUTION - - 0.05 nm FIELD OF VIEW 1 mm 1mm 0.01 mm DEPTH OF FIELD GOOD GOOD POOR CONTRAST ON FLATE SURFACE POOR POOR GOODNITC MED
  • 22.