Do Minh Nghiep

Materials Science Center

Electron Microscopy
and Diffraction
8. Electron difraction

Part of the figures, texts are quoted from internet resources. All the copyrights belong to the original authors.
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

William Henry Bragg: Like an X-ray an electron beam has its

1862 – 1942 own wavelength which is inversely
Nobel Prize in Physics: 1915
proportional to its energy: E = hν =
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hc/λ 6
 Vulf-Bragg’s diffraction

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

If a known wavelength λ is used and the Bragg’s

angle θ can be measured or inferred then the d-
spacing of a crystal of unknown composition can be
calculated.
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 Diffraction law

For a given wavelength λ there is a specific angle θ (Bragg’s angle) at which

diffraction will occur. Bragg’s angle is determined by the d-spacing
(interplanar spacing) of the crystal and the order of diffraction (n = 1, 2, 3….).
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 X-ray diffraction

Diffraction
pattern

This is the principle behind X-ray diffraction (XRD) in which an X-ray of

known wavelength is focussed onto a crystal that can be aligned until a
diffraction pattern is created. A blanker on the optical access blocks
the transmitted wavelengths.
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 Diffraction pattern

An XRD pattern of
silicon single crystal
is discrete spots.

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 Diffraction pattern

If a polycrystal diffracted the resultant pattern will be a set of

distinct concentric rings, not discrete spots.
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 Powder
method
 X-ray source:
Xray tube
 Debye chamber:
powder sample,
film winded
around sample

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 Electron
diffraction

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21.05.10 15
 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

The result is an electron diffraction (ED) pattern. The pattern one

obtains is completely dependent on the d-spacing and composition of
the crystal that is being analyzed.
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 ED pattern of
single crystal
Diffraction spots

An ED from a single crystal will result in a series of diffraction spots

arranged in concentric rings around the central bright spot which is
comprised of transmitted electrons.
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 ED pattern of
polycrystal
Diffraction rings

If an ED is made of field of many crystals, some of which are oriented

at the Bragg’s angle while others are not, a pattern with well defined
concentric rings, but not spots, will result.
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 ED pattern of
amorphous
ED diffusion ring
material
If an ED is made of an
amorphous structure (i.e. no
crystalline formation) then one
simply gets a central bright
spot comprised of transmitted
electrons and a single ring of
randomly forward scattered
electrons.
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 Sample position by tilt
holder to Bragg’s angle

Sample
holder

So that individual crystals can be oriented to the appropriate Bragg’s

angle one uses a double tilt specimen holder, which allows for
positioning in X, Y, and Z directions.
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 Calculation
of d-spacing
P - photographic plane
L - distance of specimen from P
T - forward transmitted beam
O - point where T strikes P
S - Bragg diffracted beam
G - point where S strikes P
R - distance from O to G

Calculation d from ED image:

image R / L = tan2θ and from Bragg’s law we
know that 2d.sinθ = λ .
Thus R / L ≈ 2θ ≈ 2λ / 2d which simplifies to R = λ .L / d. If we can
measure R and both λ and L are constants then d can be calculated.
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Exact R and L values required
 The R values for different
order diffraction events
can be measured directly
from a diffraction pattern,
but it is crucial that it not
be enlarged or reduced.
 It should always be
compared to a pattern of
a crystal with a known d-
spacing, so that the value
Index of ED spots
for the camera length L is
accurate.
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 Application

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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

Mg3Si2O5(OH)4 EDS hologram of

Mg3Si2O5(OH)4
Magnesium 26,31 % Mg
Silicon 20,27 % Si
Hydrogen 1,45 % H
Oxygen 51,96 % O

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Selected Area Electron
Virtual
Diffraction (SAED) Aperture

Specimen

Lower Objective
Lens

Back Focal Plan

b*
a*

SA Aperture

SAED use parallel illumination and

SAED pattern of a crystal limits the sample volume by an
aperture in the image plane of the
lower objective lens.
Lattice plane have K+g
θ
spacing of d K
D
= tan( θ ) = tan( 2θ B ) ; 1 D
Camera length
≈
L
L
Ewald Sphere
2dSinθ B = λ d Lλ
D
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31
ELECTRON DIFFRACTION PATTERNS

MOSAIC SINGLE PLATELIKE TEXTURE POLYCRYSTA

CRYSTAL L

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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

Specimen prep important: surface must

have damaged layer (esp from coarse
polishing) removed, e.g. with colloidal silica
(which is also chemical etching action);
carbon coat must be very very thin (≈ 10 Å)

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 Summary

Electron diffraction is a technique which allows

users to determine the atomic arrangement of
crystals. When combined with other analytical
techniques such as EDS it can aid in the
identification of unknown crystals and/or determine
the d-spacing of newly described crystals.

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