Beruflich Dokumente
Kultur Dokumente
Electron Microscopy
and Diffraction
8. Electron difraction
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All the references made here are for educational purpose only.
Content
Diffraction in crystals
• Diffraction law
•Diffraction patterns
Electron diffraction in TEM
Application
Diffraction
in crystals
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Light interference
4
What is diffraction?
Diffraction – the spreading out of waves as they encounter a barrier
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Diffraction in crystals
Bragg’s law reminds us that for any given wavelength λ it will be diffracted
by a crystal if it strikes the crystal at precisely the correct angle θ .
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Diffraction law
nλ
d=
2 sinθ
Diffraction
pattern
An XRD pattern of
silicon single crystal
is discrete spots.
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Diffraction pattern
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Electron
diffraction
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Electron diffraction
If a monochromatic e-beam
of known λ strikes a crystal
at the appropriate Bragg’s
angle θ a number of the
diffracted electrons will be
forward scattered.
Like the transmitted
electrons these diffracted
electrons will have nearly
their same energy, but will
have been significantly
altered from their trajectory.
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ED in TEM
The transmitted electrons will
be brought to convergence in
the back focal plane of the
objective lens at point Y.
Likewise the diffracted
electrons will also be brought
to convergence in the back
focal plane of the lens but at
a different spot X.
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ED in TEM
Normally an aperture is
placed in the back focal
plane of the objective lens
to stop widely scattered
electrons from reaching
the viewing screen.
But in the case of
diffraction it is these same
scattered electrons that
contain the information
about the diffraction event.
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ED in TEM
To operate the TEM in
diffraction mode the
objective aperture is
removed from the beam
path and the scope is
adjusted to focus an image
of the back focal plane of
the objective lens, not the
image plane.
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Back
focal
plane
ED in TEM
This is most easily
accomplished by
adjusting the
strength of the
objective lens so that
an image of the back
focal plane is
projected onto the
viewing screen.
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ED pattern
ED spots
Sample
holder
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Microstructure + structure
Crysotile is a monocyclic crystal that tends to
Hollow
form a hollow tube. This results in a distinctive
tube
diffraction pattern with smeared spots.
TEM of
Crysotile fiber
Diffraction of Crysotile
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and composition
TEM of
Crysotile fiber
Diffraction of Crysotile
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Selected Area Electron
Virtual
Diffraction (SAED) Aperture
Specimen
Lower Objective
Lens
SA Aperture
31
ELECTRON DIFFRACTION PATTERNS
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Electron Backscatter Diffraction-EBSD
Electron backscatter diffraction (EBSD) is a technique for determining
crystallographic information of submicron regions of flat polished samples. It
has made possible studies of microtextures, phase identification (of
polymorphs), grain boundary distribution, and deformation microstructures.
EBSD is also known by the names backscatter Kikuchi diffraction BKD, or
electron backscatter pattern EBSP. The phenomenon has been known since
1928 by Kikuchi, who noted ‘remarkable lines’ resulting from electron diffraction
thru a thin mica crystal. Two research groups (in UK) started working on EBSD
~1973, and it has only been commercially available since 1994.
In many cases it replaces more time-consuming/difficult TEM or XRD, or
possibly electron channeling studies, with the benefit of SEM’s point by point
high spatial resolution (<1 mm) together with its ability to scan large areas
(~cm). It is relatively inexpensive ($50-100K), in being an add-on attachment to
a previously existing SEM.
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EBSD
Kikuchi recognized the importance of a divergent electron
beam being diffracted - how the spreading of the incident
beam (by inelastic scattering in upper surface of sample)
Orientation mapping (OIM, orientation imaging microscopy)
Phase identification by step-by-step deduction of pattern
point group symmetry, though some problems; other
technique is to determine approx value of unit cell volume
from measured lattice spacing and interplanar angles,
together with EDS, searching a database for possible
matches, then match angles
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EBSD
The sample is tilted steeply (70°, so beam is 20° to
sample) which enhances the number of BSEs able to
undergo diffraction and escape the surface. The HV
electrons are scattered by the electrons of the atoms
in the top unit cells of the material, scattering from
electrons in crystallographic planes producing
intersecting bands imaged by film or a phosphor
screen immediately adjacent.
The pattern and bands provide information about the
crystal structure:
• Symmetry of crystal lattice
• Width and intensity of bands are a measure of the
plane spacing (and unit volume)
• Angles between bands are related to the angles
between planes in the lattice.
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From Microscopy
Today, Jan/Feb 1993
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Specimen preparation
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Summary
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