TEM

Electron Diffraction
Nataly Belman (2003)
Lilah Goshen (2005)

Lecturer: Prof. Jacob Zabicky

 Outline
 Motivation for using TEM electron diffraction analysis
 Diffraction geometries:
 The Reciprocal Lattice
 The Reciprocal Vector ghkl
 Bragg's Law
 Ewald’s Sphere
 Calculation of the dhkl Spacing
 The Zone Axis
 Diffraction pattern types
 Application of the method to nanomaterials
 Advantages and disadvantages of TEM electron
diffraction analysis
 DIFFRACTION IN THE TEM
TEM diffraction characterization is useful to
answer the following questions:
 Is the specimen crystalline or amorphous?
 What are the crystallographic characteristics of the
specimen?
 lattice parameters
 symmetry
 Is the specimen made of single crystals?
 What is the orientation of the specimen or of
individual grains with respect to the electron beam?
 The Real Lattice
 This model gives a physical picture of diffraction geometries
that is extremely helpful. The best approach is to think of
any crystal as having two lattices:
 The Real Lattice describes the arrangement of the unit
cells of atoms in the crystal (the specimen). In real space,
we can define any lattice vector, r, by the equation:

r = n1 a + n 2 b + n 3 c c

r
•Vectors a, b, and c are the b
unit-cell translations a
•n1, n2, n3 are all integers.

Real Lattice
 The Reciprocal Lattice
 The Reciprocal Lattice is an array of points which is
uniquely defined for a given crystal but does not correspond
to arrays of atoms; instead, each point is associated with a
particular set of planes in the crystal.
 A reciprocal lattice vector, r*, can be defined in a similar
manner:

r = m1 a + m 2 b + m 3 c
* * * * *c

•Vectors a*, b*, and c* are the

unit-cell translations b*
r*
•m1, m2, m3 are all integers.
a*
The scalar products of the
vectors behave as follows::
a*b=a*c=b*c=b*a=c*a=c*b=0
a*a=1; b*b=1; c*c=1 Reciprocal Lattice
 The Reciprocal Vector ghkl
 A particularly important reciprocal lattice vector is the
reciprocal vector ghkl in the reciprocal lattice. It is normal to the
plane (hkl) in the real lattice :

g hkl = h a* + k b* + l c*
 The distance between parallel y Vector in
(hkl) planes: Plane (hkl)
ghkl the
reciprocal
1 in the real
d hkl =  lattice
lattice
g hkl
z
 g - reciprocal vector
 h, k and l are all integers and together x
define the plane (hkl)
 d - crystal lattice spacing between atomic
planes Real and Reciprocal Lattices
 Bragg's Law
Diffraction from a Single Crystal
A crystalline specimen will diffract the electron beam strongly
through well-defined directions dependent on the electron
wavelength and the crystal lattice spacing, according to Bragg's
Law:
nλ
=2d sin θ
Incidence
The direction of the reflected beam
beam is in a 2θ angle relatively to
the incident beam. This relation
gives the conditions for
constructive interference of the
scattered electron waves.

θ
n = integer Reflection
λ = electron wavelength beam
dhkl
d = crystal lattice spacing between atomic planes
θ = angle of incidence and reflection
 Ewald’s Sphere
 Ewald’s sphere is a sphere of
radius 1/λ in the reciprocal space. θ Beam
Specimen
(hkl)
 The reciprocal lattice is a tool used
together with Ewald’s Sphere for
geometrical interpretation of the 2θ
Bragg law that describe the /1λ
diffraction conditions: if a point P in
the reciprocal lattice lies on the ghkl
surface of the sphere, the set of P
planes corresponding to that point O*
must satisfy the Bragg equation and Ewald Sphere
Origin of the
hence the planes will diffract Reciprocal Lattice
strongly.
 The reciprocal vector ghkl points from The reciprocal lattice and
the origin O’ to point P. Ewald’s Sphere contain the
origin O*
 Ewald’s sphere can be represented
in practice as a plane, because 1/λ
is very large.
 Each spot in the diffraction pattern
is an image of the electron source, Beam
since the imaging system is set to (λ(=0.072Å
show the image of the electron Specimen
(hkl)
source on the viewing screen.
 The diffraction pattern lies in the
planar section of the reciprocal
lattice, perpendicular to the beam
direction
A diffraction pattern is, in the
simplest sense, a Fourier transform
of the crystal lattice, giving O*
information on the periodicity of the
lattice, and hence the atomic sites.
 Each spot [hkl] in the reciprocal
space in the diffraction pattern is a Ewald’s
Plane (hkl) in the Sphere
diffraction from plane (hkl) reciprocal space
 Calculation of the dhkl Spacing
 Calculation of the dhkl spacing (crystal lattice spacing
between atomic planes) provides valuable information on
the crystal structure and orientation. From the
calculation of d spacings we can identify:
 The (hkl) planes
 The orientation of the specimen or of individual grains
with respect to the electron beam
 The lattice parameters of the specimen (spacing
between the atoms)
 The symmetry of the specimen (atomic structure)
The camera constant is defined as λL, where L is the camera
length L (both are constants for a specific microscop) . The d
spacings in the crystal can be calculated when r is measured
from the Diffraction Pattern. From the microscope structure we
can get the equation (1):

1/λ g Specimen Beam

= (1)
L r
/1λ
Reciprocal
We can use the equation: lattice
g
1 Diffraction Pattern
d hkl =  (2) L
g hkl
r
From (1) and (2) => (3):
L λ
rdhkl =L λ⇒dhkl = (3) Photographic
r r plate
 Zone Axis
 A Zone Axis is an axis that defines the orientation of
the specimen or of individual grains with respect to the
electron beam
 The zone axis is parallel to the beam
 The zone axis is perpendicular to the g vectors, so it
can be calculated as the vectorial product of two
planes in the diffraction pattern
Beam || Zone axis
g1

O* g2

g3

Reciprocal Lattice
 The zone axis || (hikili) planes in the Real Lattice
 The spots on the diffraction pattern represent the (hkl)
planes
 In the diffraction pattern we see only the spots which
represent planes that belong to the same zone axis

[h1k1l1] Beam (h1k1l1)

[h2k2l2] (h2k2l2)

[h3k3l3] (h3k3l3)

Planes in the
Diffraction Pattern
Real Lattice
TEM viewing

When the electron

beam strikes the
specimen part of the
beam is transmitted,
other parts are
diffracted, scattered,
absorbed, etc.
 TEM viewing

With the objective

aperture one may
choose to view the
diffraction pattern of
the specimen
 Diffraction pattern types
A diffraction pattern of the crystal lattice gives us
information on the periodicities of the lattice.
Depending on the nature of the specimen, a diffraction
pattern usually consists of:

 SAD (selected area diffraction, spots from a single

crystal)
 Rings (from multiple crystals)
 Diffuse rings (from amorphous materials)
 CBED (convergent beam electron diffraction)
 )SAD )spots
This diffraction pattern is typical to a single crystal (all the
grains or crystals have the same orientation).
Sets of parallel (hkl) atomic planes are represented by a
single point.

Schematic explanation of a
spots diffraction from 4 grains
with same orientation A single crystal
 )SAD )spot alignment
SAD from zone axis [100] – with or without deviation

Beam normal to a lattice plane of Beam has off-axis angle of

<1 0 0> direction incidence
)SAD )beam effects
)SAD )grain size effects

Single crystal Textured Fine grained

sample sample or
nanomaterial
 Rings
If the sample is not a single crystal (polycrystalline), in the
diffraction pattern different crystals or grains will diffract on
different places and their connection forms rings. The ring
radiuses represent different (hkl) planes.

Schematic explanation of
rings diffraction from 3 grains
with different orientations
)Rings )polycrystalline Au
 Diffuse rings
There are no (hkl) planes in an amorphous specimen, so it
won’t diffract strongly. If there are no spots or rings in the
diffraction pattern the material is amorphous.

Amorphous Carbon
 CBED
convergent beam electron diffraction

Si Al

dislocations
Example: Diffraction fromPbS
Nanocrystals

(200) (220)

(220)

zone axis<<100 zone axis<<111

There are two types of PbS Nanocrystals:
 right-angled triangle
 equilateral triangle
We can see above the relation between the crystal
morphology and crystallography.
The pictures show the electron diffraction, from which
we can define the zone axis of each nanoparticle
There are two types of PbS nanocrystals, large ones
(≈ 25nm, d220=2.131 Å ) and small ones (≈ 7nm,
d220=1.981 Å ). The diffraction pattern below shows
doublet spots of (220) planes. We can conclude that
the lattice parameter (a) of PbS nanocrystals
depends directly on their size.
 )220(

r2
r1

Diffraction Pattern PbS nanocrystals

2
a
For a cubic lattice the dependence of d
hkl =
d on a follows from the equation: h +k +l
2 2 2
 Advantages of electron diffraction
 The ability to see in the image pattern the area we want to
diffract,
 The ability to determine crystallographic orientations
locally (down to the nm level)
 The ability to get a diffraction pattern from specific grains

Disadvantages
 No TEM diffraction can be obtained from the
whole specimen, but only from selected areas.
Therefore, there could be areas in the
specimen that were not diffracted and phases
that were not identified. Unlike X-ray diffraction
that can be obtained from the whole specimen
 References
 David B. Williams and C. Barry Cartor,
“Transmission Electron Microscopy
Diffraction”, pp.179-199.
 http://em-outreach.sdsc.edu/web-course/
toccontents.html
 http://
www.mete.metu.edu.tr/FACILITIES/TEM/TEM