Transmission

Electron Microscopy
and Electron
Diffraction
The Philips CM200
transmission electron
microscope

Accelerating voltages is 200

kV

Can achieve resolution upto

 Why Electron Microscope?
Light Microscopes are limited by the physics of light
to 500x or 1000x magnification and a resolution of
0.2 micrometers.

In the early 1930's there was a scientific desire to

see the fine details of the interior structures of
organic cells (nucleus, mitochondria...etc.).

This required 10,000x plus magnification which was

just not possible using Light Microscopes.
 LM, resolving power
~0.25µm, maximum
(useful) magnification is
about 250µm/0.25µm =
1000X.
Any magnification above
this value represents
empty magnification

TEM at 60,000 volts has a resolving power

of about 0.0025 nm. Maximum useful magnification
of about 100 million times!!!
COMPARISION OF LIGHT AND ELECTRON MICROSCOPE

LIGHT MICROSCOPE

Optical glass lens, Small depth of

Field, lower magnification, do not
Require vacuum, Low price.

ELECTRON MICROSCOPE

Magnetic lens, Large depth of field,

Higher magnification and better
Resolution, Operates in HIGH
vacuum, Price tag.
 Electron Microscopy
What are electron microscopes?

Electron Microscopes are scientific instruments that use a

beam of highly energetic electrons to examine objects on a
very fine scale which yield the following information:
1. Topography :
The surface features of an object (hardness, reflectivity...etc.)
2. Morphology:
The shape and size of the particles(ductility, strength,
reactivity...etc.)
3. Composition:
The elements and compounds that the object is composed of
and the relative amounts of them.
4. Crystallographic Information:
 SPECIMEN INTERACTION IN
ELECTRON MICROSCOPY
REACTIONS ON THE TOP SIDE VARIOUS REACTIONS CAN
ARE UTILIZED FOR EXAMINING
OCCUR WHEN ENERGETIC
THICK OR BULK SPECIMENS
(SEM) ELECTRONS STRIKE
THE SAMPLE

RECTIONS ON THE BOTTOM SPECIMEN

SIDE ARE EXAMINED INTERACTION
IN THIN OR FOIL SPECIMEN VOLUME FOR VARIOUS
(TEM) REACTIONS
 THIN SPECIMEN INTERACTIONS
REACTION UTILIZATON
PRODUCT
SOURCE

INCIDENT ELECTRONS TRANS- UNSCATTERED ELECTRON INTENSITY IS

MITTED(NO DEFLECTON FROM INVERSELY PROPORTIONAL TO THE
UNSCATTERED
THE ORIGINALPATH) THROUGH SPECIMEN THICKNESS. THICKER PORTION
ELECTRONS
THE SPECIMEN WITHOUT ANY OF THE SPECIMEN WILL APPEAR DARKER
INTERACTION AND CONVERSE IS ALSO TRUE.

INCIDENT ELECTRONS FOLLOW BRAGG’S LAW. SIMILAR ANGLE

SCATTERED(DEFLECTED FROM
ELASTICALLY
THE ORIGINAL PATH) BY THE
SCATTERED
ATOMS IN THE SPECIMEN IN
ELECTRONS
AN ELASTIC FASHION
(NO LOSS OF ENERGY)
SCATTERING OF THE ELECTRONS FROM THE
PLANE OF SAME ATOMIC SPACING FORM
PATTERN OF SPOTS WHICH YIELDS INFOR-
MATION ABOUT THE ORIENTATION, ATOMIC
ARRANGEMENTS AND PHASES PRESENT.

UTILIZED IN TWO WAYS:

ELECTRONS INTERACT WITH THE • KIKUCHI BANDS: BANDS OF ALTER-
SPECIMEN ATOM IN AN INELASTIC NATING DARK AND BRIGHT LINES RELATED
INELASTICALLY
FASHION (BY LOOSING ENERGY TO THE ATOMIC SPACING OF THE SPECIMEN.
SCATTERED
DURING INTERACTION) 2. ELECTRON ENERGY LOSS SPECTROSCOPY:
ELECTRONS
LOSS OF ENERGY ARE UNIQUE TO
EACH BONDING STATE OF EACH ELEMENT.
 Transmission Electron
Microscopy
TEM is a unique tool in characterization of materials
crystal structure and microstructure simultaneously by
diffraction and imaging techniques.
TEM is analogous to a Slide Projector
 Transmission Electron
Microscopy
In a conventional transmission electron microscope, a thin
specimen is irradiated with an electron beam of uniform current
density.
Electrons are emitted from the electron gun and illuminate the
specimen through a two or three stage condenser lens system.
Objective lens provides the formation of either image or
diffraction pattern of the specimen.
The electron intensity distribution behind the specimen is
magnified with a three or four stage lens system and viewed on a
fluorescent screen. The image can be recorded by direct exposure
of a photographic emulsion or an image plate or digitally by a
CCD camera.
The acceleration voltage of up to date
routine instruments is 120 to 200 kV.

Medium-voltage instruments work at

200-500 kV to provide a better transmission
and resolution, and in high voltage electron
microscopy (HVEM) the acceleration voltage
is in the range 500 kV to 3 MV.

Acceleration voltage determines the

velocity, wavelength and hence the
resolution (ability to distinguish the
neighbouring microstructural features) of
the microscope
 Depending on the aim of the investigation
and configuration of the microscope,
transmission electron microscopy categorized
as:
Conventional Transmission Electron Microscopy

High Resolution Electron Microscopy

Analytical Electron Microscopy

Energy-Filtering Electron Microscopy

High Voltage Electron Microscopy

Dedicated Scanning Transmission Electron Microscopy

IMAGING
The image of the specimen in conventional microscopy, ,
is formed selectively allowing only the transmitted
beam (Bright Field Imaging) or one of the diffracted
beams (Dark Field Imaging) down to the microscope
column by means of an aperture.

The origin of the image contrast is the variation of

intensities of transmitted and diffracted beams due to
the differences in diffraction conditions depending on
the microstructural features on the electron path.
BRIGHT FIELD IMAGING
ALLOWING TRNSMITTED BEAM
DARK FIELD IMAGING ALLOWING
DIFFRACTED BEAM
Bright-field TEM micrographs of the as-prepared ZnO
powders after annealing for 1 h at various temperatures: a
300 .C, b 400 .C and c 500 .C, respectively.
DIFFRACTION
Electrons of 0.072 Angstrom wavelength at 100 kV
excitation transmitted through about 0.1 micrometer thin foil
specimen are diffracted according to Bragg's Law, forming a
diffraction pattern (consisting of a transmitted and diffracted
beam spots).

Although diffraction phenomena is a complex interactions of

charged electrons with the periodic potential field of the
lattice, Bragg's Law or Laue Conditions are sufficient
approximations for usual practical applications.

A diffraction pattern is, in the simplest sense, a Fourier

transform of the periodic crystal lattice, giving us information
on the periodicities in the lattice, and hence the atomic
positions.
Some fancy
Diffraction
Patterns
 BASIC DESIGN OF TRANSMISSION ELECTRON
MICROSCOPE

Evacuated metal cylinder within which are aligned,

one under another:
1. Tungsten filament (the cathode)
2. A Metal plate with central aperture (the anode)
3. A number of magnetic lenses
4. A Fluorescent screen
5. A photographic plate
 DESIGN OF TRANSMISSION
ELECTRON MICROSCOPE

A simplified ray diagram of a

TEM consists of an electron
source, condenser lens with
aperture, specimen, objective
lens with aperture, projector
lens and fluorescent screen.
In actuality a modern
TEM consists of
many more
components including
a dual condenser
system, stigmators,
deflector coils, and a
combination of
intermediate and dual
projector lens
Electron Gun
Electron beam is generated in the electron gun.
Two basic types of guns are used:

1. Thermionic Gun:
Based on two types of filaments: Tungsten(W) and
Lanthanum-Hexaboride(LaB6).

2. Field Emission Gun(FEG):

Employs either a thermally assisted cold field emitter
or Schottky emitter.
Functioning of the Thermionic Gun
An positive electrical potential is applied to the anode.
The filament (cathode) is heated until a stream of electrons is
produced .
A negative electrical potential (~500 V) is applied to the Whenelt
Cap.
A collection of electrons occurs in the space between the filament
tip and Whenelt Cap. This collection is called a space charge.
Those electrons at the bottom of the space charge (nearest to the
anode) can exit the gun area through the small (<1 mm) hole in the
Whenelt Cap .
These electrons then move down the column to be later used in
imaging
Field Emission Gun (FEG)
In recent years cold field-emission and thermally-assisted field
emission guns have become increasingly common.

In these a very fine point on the pointed

filament is formed.

Electrons are emitted by tunnelling through

the potential barrier at the tip surface when
a very high potential field gradient is formed
at the surface.
FEG requires a different gun design as well as
much better vacuum in the gun area (~10e-8
Pa instead of the ~10e-5 Pa).

Consists of a small single-crystal tungsten

needle that is put in a strong extraction voltage
(2-5 kV). In the case of a cold FEG, the needle
is so sharp that electrons are extracted directly
from the tip. For the Schottky FEG a broader tip
is used which has a surface layer of zirconia
(ZrO2). The zirconia lowers the work function of
the tungsten and can use the broader tip.

Unlike the thermionic gun, the FEG does not produce a small cross-over
directly below the emitter, but the electron trajectories seemingly
originate inside the tip itself, forming a virtual source of electrons for the
microscope.
Electron Optics Elements
Lense: Focus(or defocus) the beam on the
specimen and change the magnification.

Deflection Coil: Shift or tilt the beam.

Stigmators: Correct the lenses. Ideally lenses

are round and symmetrical but in practice
there are small deviation which is corrected
by the stigmators.
Electron Optics Elements

Magnetic Lenses
 MAGNETIC LENSES
1.Coil of several thousand turns of wire through which a current
of less than or equal to one amp is passed --- creates a magnetic
field.
2.. Electrons are deflected by magnetic field
3. To concentrate field further a soft iron pole piece is
inserted into the bore of the objective lens.
5. To focus an electron beam onto a given plane the current
through the coils must be set to a precise value.
.
current – beam focus closer to lens
current – beam focus further from lens
Depth of Field: the range of distance at the specimen parallel to
the illuminating beam in which the object appears to be in focus.

Depth of Focus: the range of distance at the image plane (i.e.

the eyepiece, camera, or photographic plate) in which a well
focussed object appears to be in focus.
 CONDENSER LENS

Illuminates the specimen.

Relatively weak lens.

Longer focal length than objective or projector

lens.

May bring electron beam into focus directly upon

specimen, above the specimen (over focusing) or
below the specimen (under focusing).
As magnification increases the condenser lens
must be adjusted to properly illuminate the
specimen. When the lens is brought to its
smallest spot the beam is said to be at the
crossover point
Holey Formvar is used to critically adjust the stigmation of a
TEM. When the beam is under or over focused on the specimen
a Fresnel fringe becomes visible due to the effects of diffraction
around the edges of the hole. When this Fresnel fringe is evenly
distributed then the beam is said to be stigmated
OBJECTIVE LENS

Strong lens
Highly concentrated magnetic field and short focal
length.Causes electron beam, which has passed
through specimen, to focus at a point a few mm
below specimen.
Magnification of image produced a short distance
below focused point.
Projector Lens

Magnification produced by projector lens dependent

on current passing through the coil of the lens (ie
increase current spreads beam further = higher
mag.)

Projector lens has great depth of focus (several

meters). Therefore distance at which fluorescent
screen or photographic plate are placed is not
critical.
Total magnification in the TEM is a
combination of the magnification from the
objective lens times the magnification of the
intermediate lens times the magnification of
the projector lens. Each of which is capable
of approximately 100X.

Mob X Mint X Mproj = Total Mag

 Deflection Coils

In older TEMs functions such as gun and beam alignment

were accomplished by physically moving components in
the column. Today they are achieved by use of
electromagnetic deflection coils that are positioned
throughout the column
Using the deflection coils the beam can be shifted so
that the focused beam is centered in the back focal plane
of the lens and tilted so that the beam is centered on the
specimen.
 Fluorescent Screen
Fluorescence: Property of emitting radiation under the
influence of electromagnetic or electron beam bombardment.

In the TEM, screen coated with a material in the visible range,

eg zinc sulphide, is installed beneath the projector lens in the
path of the electron beam.

Screen emits visible light when bombarded with electrons.

The resolution of the fluorescent screen is limited to

70-100µm by the grain size of the fluorescent material and by
light scattering within this material.
Vacuum System
Electron can’t travel more than a few angstrom
without colliding with gas molecules.

Distance between photographic plate and electron

gun is approximately 1 meter.

Electron gun must be evacuated (10-4 torr).

Two types of vacuum pump are used

 Rotary (mechanical) fore-pump.

 Diffusion pump (Oil or Mercury)
 BASICS OF ELECTRON
DIFFRACTION
Simplifications:

No absorption
No thermal vibration
No multiple scattering
Distance between crystal and film >> λ
the wavelength of electron
Large object (macroscopic single
crystal)
 The de Broglie wavelength of electron is given by

or

Diffraction intensity in a given direction is the sum over

contribution from all location of the specimen taking into
account their relative phases.
Bragg’s conditions for constructive
interference:

In vector form:
The scattering vector(not necessarily a
Lattice vector) = Reciprocal lattice vector
ELECTRON DIFFRACTION UNDER THE
CONDITION OF TEM

Special conditions for TEM:

“wavelength λ << interatomic distances

transmission” ⇒ specimen thin along

the viewing direction

consequence of limited thickness: “relaxation” of the

diffraction condition
S = g ∈ REL along the viewing direction (z-axis)
ELECTRON DIFFRACTION UNDER THE
CONDITION OF TEM
• Consider a row of N unit cell along the z-axis

• The topmost unit cell scattered with amplitude F0[s]

• S=s-s0 is the scattering vector

• Scattered wave from the next unit cell below is

Where c is the lattice vector along the z-axis

Final scattered wave intensity is given by

Where I0[s] =

Lattice factor
It has sharp maximum for S.c = l an integer
 EXCITATION ERROR
Assume that the diffraction condition is not exactly satisfied:

Where s is the excitation error

g is a lattice translation of the REL, satisfying the 3rd Laue equation:

s is not a lattice translation of the REL, and we assume that

This yields, the diffraction intensity

TEM thin foil: Small extension in the z-direction, large extension in the x
And y direction.
Thus 1st and 2nd Laue equation satisfies exactly,

Excitation error only have z-component, thus

 I[s] >0 is represented by ‘rods’ parallel to z* in every REL point (REL rods).

And the scalar product, N.c.s =

This yields following expression of intensity

Since s is small

First minimum of I occurs at ± 1/t. Thus

diffraction Occurs although S is not a
 Ewald Construction for Electron
Diffraction in TEM
Special Ewald construction for diffraction of electrons at thin foils:
1. Replace REL points by REL rods!

2. Direction of the rods: normal to the plane of the foil (parallel to z*)

3. Length of the rods: ± 1/t

• special conditions:

1. Very small wavelength (compared to

X-ray diffraction, for example)
⇒ Ewald sphere has a very large radius
1/λ
2. REL points “rods” normal
to the TEM foil
Specimen, transmitted and diffracted beam forming the
diffraction pattern. Also see the Ewald sphere construction
in Reciprocal Space.
 CONSEQUENCES:
1. Even for a “sharp” wavelength, λ = const., a TEM foil generates
diffracted beams, irrespective of the orientation of the foil versus the
primary beam!
2. Very small Bragg angles ( 1°)
3. Reflecting planes are approximately parallel to the
primary beam
4. = Reduces the Bragg condition to

5. Ewald sphere “flat” in the angular region of ±1° around the direction of
the primary beam
6. Curvature of the sphere is negligible compared to length ±1/t of the
REL rods
Consequence:

Example: Diffraction pattern of f.c.c lattice in <hkl> direction

(hkl) plane of b.c.c lattice and vise versa.
 EXAMPLE OF DIFFRACTION PATTERN

In this case incident beam direction B [100] in an Aluminum (f,c.c),

single crystal specimen. Transmitted beam is marked as T and the
arrangement of the diffracted beams D around the transmitted beam
is the characteristic of the four fold symmetry of the [100] cube axis
of Aluminum.
SINGLE CRYSTAL DIFFRACTION PATTERN

Single crystal are most ordered (lattice type such as f.c.c, b.c.c, s.c etc.)
among the three structures.
Electron beam passing through a single crystal will produce a
pattern of spots.
Type of crystal structure (f.c.c., b.c.c.) and the "lattice parameter"
(i.e., the distance between adjacent planes) can be determined.
Also, the orientation of the single crystal can be determined: if the
single crystal is turned or flipped, the spot diffraction pattern will
rotate around the centre beam spot in a predictable way.
 DIFFRACTION FROM POLYCRYSTALLINE
MATERIALS
• Polycrystalline materials are made up of
many tiny single crystal.
• Not ordered, single crystal grains in a
polycrystal have random distribution of all
possible orientations.
• Diffraction patterns will therefore will look
like superposition of single crystal spot
pattern: a series of concentric ring resulting
from many spots very close together at
various rotation around the central spot.

From the diffraction rings type of crystal structure and the "lattice
parameter“ can be determined.
One cannot determine the orientation of a polycrystal, since there is no
single orientation and flipping or turning the polycrystal will yield the
same ring pattern.
 Contribution of Inelastic
Scattering
Conventional high-energy electron diffraction:
elastic scattering
But in thick enough specimen: also inelastic
scattering
Inelastically scattered electrons:

1. Travel in all directions

2. Distribution peaks in forward direction

3. Grey background around central spot

Bragg Reflection of Inelastically
Scattered Electrons
Inelastically scattered electrons can
subsequently be diffracted
But only if they are now traveling at the Bragg
angle, to a set ( hi) of lattice planes
Consider (hi) inclined by angle versus
primary beam
Bragg reflection can occur with two sets of
inelastically scattered electrons at

Result: intensity changes in the b ackground

Kikuchi Lines
Diffraction of inelastically-scattered electrons:
In all directions for which
In 3D (from Laue equations) we know
Diffracted electrons will form a cone , not a
beam
Intersection of cones with viewing plane:
hyperbola, not spots!
Usually:
Camera length (magnification) >>radius of
curvature
Only small sections visible straight lines

KIKUCHI LINES
Features of Kikuchi Lines
Kikuchi lines belong to particular lattice planes
hiai and can be indexed.
Spacing , distance of diffraction spot
from center spot
Mirror line in the center between excess and
deficiency line trace of planes
Specimen tilt lines rotate as if “attached” to
specimen
Position sensitive to small specimen tilts
Adjust crystal orientation and excitation error
Accuracy: ±0.10
Compare accuracy using spot intensities:
± 20
 TYPES OF DIFFRACTION PATTERNS AND THEIR USE
TYPE OCCURENCE USE
RING POLYCRYSTALL- Identification of phases and determination of
PATTERN INE AND AMOR- grain size of polycrystalline sample produced
PH0US SPECIMEN by electro-deposition or CVD
Magnified images of the planar section of RL
pace perpendicular to the beam direction and
can be used to determine
SPOT SINGLE CRYSTAL 4. Specimen orientation in the microscope
PATTERN 5. Tilt axis by tilting about the bright spot
6. Orientation relationship between phases
7. Precipitates, twin etc. can be identified
8. Quick survey of orientation and hence the
diffraction vectors.
KIKUCHI INELASTIC SCATT-
1. Accurate crystal orientation
LINES ERING BY A THICK 2. Incident beam direction
SPECIMEN. 3. Define the sense of tilt
SADP FROM SING- 4. Crystal symmetry
LE CRYSTAL
 INDEXING DIFFRACTION PATTERNS

C am e ra is the distance between and screen and the crystal

Le ngth (without imaging lens).

With imaging lenses effective L is considered.

From the figure:

Using the reduced Bragg condition:

and the above relation we have,
 DETERMINATION OF LATTICE PLANE SPACING
AND INDEXING DIFFRACTION PATTERNS
Ring Patterns: Radius of each ring is characteristics of inter-planar spacing.
Steps are: • Measure the diameter of the ring.
• Convert the distances into interplanar spacing using

3. Use ASTM index to identify the phases.

4. If the material is known, one can measure the ratio’s of the square of
the diameters of the outer ring to that of the 1st or 2nd (lower index) ring.
5. Check the ratio’s against a table of ratio’s for the crystal structure of
interest.
Spot Patterns: 1. Measure the distances R1, R2,… of the diffracted spots from
the central spot. These distances correspond to the interplanar spacing of the
reflecting planes and hence related to the camera length L.

2. The angles between the lines drawn from the central spot to the diffracted
spots (h1k1l1), (h2k2l2) are the angle between the planes.
 INDEXING DIFFRACTION PATTERNS
General Method:
1. Measure R of the fundamental reflection.
2. Calculate the corresponding plane spacing dhkl.
3. Index the reflections with (hkl).

In a good approximation primary beam is parallel to the reflecting planes.

That is primary beam corresponds to the zone axis of the reflecting plane.

Addition Rule:

If a zone includes the plane hi and ki , then it also

includes the plane (hi + ki).

For the diffraction pattern of a single crystal this implies that after
indexing two non-collinear fundamental reflections, the indices of the
entire pattern follow from vector addition.
DETERMINATION OF BEAM DIRECTION

The zone axis [uvw]=Z=B can be determined

by using the relations,

u=k1l2-k2l1
v=l1h2-l2h1
w=h1k2-h2k1
Where the spot (h1l1k1) is positioned counter clockwise
around the central spot relative to the spot (h2k2l2).

If the spots are expressed in terms of reciprocal lattice

vector g1 and g2 then

B= g1 g2