Transmission Electron Microscopy
Chapter 4
Diffraction (I)
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Outline
• Reciprocal Space
• The Ewald Sphere
• The Thin-Foil Effect on Diffraction Spots
• Zone Law
• The Excitation Error
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Real Space and Reciprocal Space
• TEM optics and sample are similar to grating in Fraunhofer far-
field diffraction geometry.
Incident plane wave (far-field) on diffraction grating
=> Periodic array of spots on diffraction plane
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Real Space and Reciprocal Space
Bragg Condition
2 sin
= = =
Crystal
Real Space Reciprocal Space
• The lattice represents the • The points in the lattice are
arrangements of the unit associated with particular
cells of atoms in the crystal. sets of planes in the crystal.
+
Basis Real Lattice Reciprocal Lattice
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Reciprocal Lattice
• In real space, lattice vector is
defined by the equation, =
= + +
=
, , and are the translational vectors of the
unit cell.
=
• In reciprocal space, reciprocal-lattice
vector is defined as
= + +
, , and are the reciprocal-lattice translational
vectors of the unit cell.
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Reciprocal Lattice
• The Volume of the unit cell is
= × = ×
1 ×
=
×
• So, the reciprocal-lattice translational
vectors are defined as,
× × ×
= = =
× × ×
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Reciprocal Lattice
1. Orthonormal Relation
= = = = = =
is normal to and , etc.
= ; = ; =
The projection of on multiplied by the length
of is unity, etc.
2. The dot product of and is integer.
=( + + ) ( + + )=
+ + = integer
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Reciprocal Lattice
3. The reciprocal-lattice vector is normal to the ( ) plane.
• Defining = + + ,
is the reciprocal-lattice vector.
=
=
4. The length of the vector, , is given by .
• Assuming the unit vector, n, normal to the
plane (parallel to ),
+ +
= = = =
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Interplanar Spacing (d-spacing)
For cubic material
=
+ +
a: the lattice parameter (lattice constant)
Lattice arrays of the crystal
in the real space
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Interplanar Spacing (d-spacing)
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Reciprocal Lattice
Real Space Reciprocal Space
• For transmitting object t(x,y) can be proved that diffraction pattern
in X, Y plane has amplitude
This is the Fourier transform of the object
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Reciprocal Lattice
Real Space Reciprocal Space
• The transform between the fringes in the real space and the spot array
in the reciprocal space is based on the Fourier Transform.
• For a crystal (3-D), the reciprocal lattices are 3-D spot arrays.
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Reciprocal Lattice
Real Space
Fourier Transform
Reciprocal
Space
FCC BCC
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Ewald Sphere
• The reciprocal lattice of the crystal is a 3D array of points, each
point represents a set of particular plane of the crystal.
• Ewald sphere, also known as the sphere of reflection, is
constructed with the radius of 1/ .
Bragg
Condition
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Ewald Sphere
Real space
Origin of Ewald sphere
Reciprocal space
Draw a sphere using Ko 3th layer
vector as the radius, the
sphere is called Ewald Sphere nd 2 layer
The change of the Ewald
sphere is followed by the 1th layer
change of Ko vector
Oth layer
Real and reciprocal spaces are
co-existed together. If the real
space is titled, the reciprocal
Ewald sphere
space is also titled.
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Bragg Condition
G 1
Ewald K = =
Sphere O 2 sin 1
= 2 sin =
2 sin
K
= , ,
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A spot in the reciprocal space
represents the plane (hkl) in the
real space.
The distance in reciprocal space is
revise proportional to the distance
in each plane.
Zero “Laue Zone” in reciprocal
space.
ZOLZ nearly locates at Ewald sphere, which can satisfy Bragg’s
diffraction condition.
Bragg‘s condition:
Atoms on the plane
Under the electron diffraction condition, we can see the two dimensional ZOLZ
at back focus plane.
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Radius of Ewald Sphere
TEM XRD
For 100 kV gun For Cu k source
= 0.154 nm
= 0.0037 nm 1
= 0.65
d = 0.2 nm
A near plane can be achieved once the Ewald sphere interests with
the Laue Zone in the reciprocal space.
If K vectors satisfy the G vectors, the Bragg’s condition can be
satisfied.
In fact, the symmetric spots appeared in the plane is caused by the
intersection between the Ewald sphere and the Laue zone.
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Laue Zone
Empty space Empty space
Diffraction patterns can be obtained by the Ewald sphere
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[110]
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Reciprocal Lattice
Real Space
Reciprocal
Space
BCC
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Outline
• Reciprocal Space
• The Ewald Sphere
• The Thin-Foil Effect on Diffraction Spots
• Zone Law
• The Excitation Error
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The Thin-Foil Effect on Diffraction Spots
• The reciprocal spot is a point only if the specimen is perfect and
infinite in all directions.
• The specimen is very thin (< few hundred nm) in the parallel direction
to the electron beam, the intensity of reciprocal spot can be
represented as a relrod stretched parallel to the electron beam in the
reciprocal space.
Relrod: Reciprocal-Lattice Rod
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Diffraction from Single Slit
sin
Uncertainly principle (1927 heisenbergs’ principle)
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Diffraction from Small Volumes
Diffraction from Particles (Shape Effect)
Real Space Reciprocal Space Real Space Reciprocal Space
• Small size in the real space becomes large in the reciprocal space.
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Diffraction from Small Volumes
Diffraction from Particles (Shape Effect)
Streaks
110 200
110
GP zones
[100] 020
[010]
Guinier–Preston (GP) zone: fine-scale solute enriched regions of the material
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Each spot in the reciprocal space along Z axis can be replaced
by a rod (rel-rod) function because of the shape effect (thin
film effect).
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The length of the rel-rod is reversely proportional to the
thickness of the sample.
Intersected line can be found from all planes, which can be
called zone axis.
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Zone Law
• If the crystal plane (hkl) contains the direction [UVW].
[ + + ]·[ + + ]= + + =0
Zone Law
[ ] Zone Axis: [ ]
[ ]
[ ]
Real Space Reciprocal Space
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Practice_Plot a Diffraction Pattern
1. Find two lowest index vectors • Plot the DP for FCC along [001]
g1 and g2 satisfying zone law and and (110] direction
selection rule.
2. Plot the two vectors with inter-
angles satisfying
cos =
3. Obtain the algebraic sums of g1
and g2, i.e. mg1 ± ng2, and plot the
resulting vectors.
4. Remove the vectors not
obeying the selection rules, and
add the possibly omitted vectors.
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Zone Law
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Ewald Sphere, Relrods and Diffraction Pattern
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Laue Zone
Empty space Empty space
Diffraction patterns can be obtained by the Ewald sphere
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Laue Zone
• Zero-order Laue Zone (ZOLZ)
• First-order Laue Zone (FOLZ) • Second-order Laue Zone (SOLZ)
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Tilting Effect on DP
Analyzable
Condition
(on the zone axis) *
Tilting
Condition
*
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Tilting Effect on DP
Analyzable Tilting High Tilting
Condition Condition Condition
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Zone axis
The titling of samples makes the
titling of the reciprocal space.
Zone axis
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The Excitation Error
• A vector, s, known as the
excitation error or the
deviation parameter is
introduced to explain the
emergence of diffraction
spot even when the Bragg
condition is not exactly
satisfied.
• The excitation error, s, is
expressed as
= +
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The Thin-Foil Effect on Diffraction Spots
• The intensity of diffraction beam is given by
sin
= = : Extinction Distance
: Effective Excitation Error
• The shape (intensity
distribution) of relrod
is proportional to
, which is the
same as that of
single-slit diffraction
pattern.
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The Excitation Error
• We can change the s value in two ways.
1. Tilting the Specimen. The row of spots moves but the Ewald sphere
does not.
2. Tilting the Beam. The Ewald sphere moves, because kI tilts and moves.
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The Excitation Error
3. s > 0
2. s < 0 The G point is inside the
The G point is outside the sphere.
sphere.
1. s = 0
The G point intersects the
surface of the Ewald sphere.
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In general, S>0, the reciprocal lattices are located in the Ewald sphere;
S<0, the reciprocal lattices are outside the Ewald sphere.
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Excitation Error
s=0 s<0
The larger the S is, the stronger the intensity of the diffraction spot is
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The Extinction Distance
• The extinction distance ( ) is the characteristic length for the
diffraction vector g.
• depends on the lattice parameters, the atomic number and the
accelerating voltage of TEM.
: The volume of the
cos unit cell
• can be expressed as = : The structure factor
for reflection g
• will be small, if the structure factor is large. Similarly, the will
increase as the accelerating voltage is increased.
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Any Questions?
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