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Transmission Electron

Microscopy

Dr. G. P. Chaudhari
Metallurgical and Materials Engineering
Microscope- transforms an object into an image
Our interest: make image larger magnify!
diverse ways to magnify
TEM: most efficient and versatile tools for the characterization of
materials over spatial ranges from the atomic scale, through the
ever-growing nano regime (from < 1 nm to 100 nm) up to the m
level
WHAT MATERIALS TO STUDY IN THE TEM?
Metals, alloys, ceramics, glasses, polymers, semiconductors, and
composites
Nanotechnology
the ability to understand and control matter at dimensions of roughly 1
to 100 nanometers, where unique phenomena enable novel applications
WHY USE ELECTRONS?
limited image resolution in light microscopes imposed by the wavelength
many other equally sound reasons
Introduction- TEM
Same principles as light microscope- uses
electrons to produce image
Lower wavelength of electrons allows for much
higher resolution than is possible with light
microscope.
Electrons accelerated to defined energy behave as a
wave.
Objects to order of 10-10 m are visible
The total volume of the material investigated by
TEM since it started in the fifties, is less than 1
cm3!
Electron Microscopy
Scanning EM (SEM) an electron beam falls on
the specimen and the image is derived from
the scattered and reflected electrons.
Surface relief (external morphology)
reflection method
scanning technique, pixels (picture elements)

TEM: the diffraction and absorption of


electrons as the electron beam passes
normally through the specimen is imaged to
provide information on the specimen.
internal structure mainly defects!
optical technique
Imaging or Diffraction
0.03 theoretical resolution
1.0 practical resolution lens aberration/diffraction
Image formation in reflected illumination
Image formation in transmission illumination
Condenser Lens

Collects light to direct it at the small area of the


object which is to be examined. It makes the
object brighter (better contrast) and enables to
control the angle at which the illumination reaches
the object.

The condenser lens can converge the light beam on


object or can illuminate it with parallel rays.

Condenser aperture: controls the area of specimen


to be illuminated
Comparison of OM, TEM and SEM
Transmission Electron Microscope

Similar to an optical instrument in that lenses are


used to form images

Scanning Electron Microscope

Not similar to an optical instrument (no image


forming lens) but uses electron optics to form a
fine probe on the specimen and the signals emitted
are detected and characterised.
Resolution
Resolution
Limited by diffraction effect
Light must pass through a series of
restricted openings
Lenses
Apertures
Whenever light passes through an
aperture, parallel beam is transformed into
a series of cones Airy rings
Dia of the central spot is inversely
proportional to the dia of aperture from
which diffraction is occurring
Diffraction effect limits the resolution
because light from every small point in the
object suffers diffraction
Airy rings and resolution
Each point in the object is represented by series of airy rings
-Resolved if Rayleigh criterion is met

Variation of intensity across a set of airy


rings. 84% lies within the central spot of
dia d1

http://photo.stackexchange.com/question
s/8304/what-is-a-diffraction-limit

http://www.olympusmicro.com/primer/techniques/confocal/resoluti
onintro.html

Rayleigh criterion
When the maximum of intensity of an airy disc coinsides with the first
minimum of the second, then the two points can be just distinguished
Resolution
Closest spacing (r) of two points which can be clearly seen
through the microscope to be separate entities
Resolution is limited by diffraction effect- restricted openings-
lenses and apertures esp. objective aperture: light from every
small point in the object suffers diffraction!= Airy ring/disc

wavelength

0.61 0.61
r
sin N . A.
Refractive Semi-angle subtended
by the aperture at the
Index specimen
Resolution limit of a light microscope
can decrease to 400 nm (green light)
sin is limited to ~ 1.6
Thus R. P. = 0.61 /N.A. = 0.61x 400/1.6 = 152 nm

The resolution is about 150 nm (0.15 m)


Resolution limit of an electron microscope
can be as small as 0.001 nm; sin is very small,
because is unity and is about a degree.
0.61
R.P.

For wavelength of 0.0037 nm and = 0.1 radians,


the resolution is about 0.02 nm
Important Features for Imaging
Wavelength of the electrons accelerated by a
potential of V volts is given by the expression,

h
2meV
h is Plancks constant (6.626x10-34 Js), m is electronic
mass (9.11x10-31kg) and e is electronic charge
(1.602x10-19C).
Variation of wavelength with applied voltage
Applied voltage, keV Wave length, nm

20 0.0086

50 0.0054

80 0.0042

100 0.0037

200 0.0025

500 0.0014

1000 0.00087
Light VS Electrons

Light Microscope Electron Microscope

= 0.5m 150
~ 0.055A (@ 50kV )
V
0
= 1.5 (glass) = 1.0 (Vacuum)
= 70 = 1
r = 0.2m=2000 r = 0.00016m=1.6A
Lens Aberrations
Analogies:
Best electromagnetic lens ~ bottom of a coke bottle used as magnifying glass
If your eye lens was ~ best electromagnetic lens => legally blind!

Spherical aberration

Chromatic aberration

Astigmatism
Chromatic Aberration

Occurs when a spectrum of wavelengths is present


Short (blue) is focused nearer.
Compromise position C where smallest image is formed- disc of
least confusion.
Loss of resolution, and quality of image!

Energy spread E = 0.1 eV for 100 keV incident beam


E = 15-25 eV for beam emerging from the specimen
Thin specimen => low E
Spherical Aberration

Portion of the lens farthest from the optic axis, brings


rays to a focus nearer the lens.
i.e. marginal rays are focused nearer than the
paraxial rays.
A point object is imaged as a disc
Electrons sense non-uniform
magnetic field as they spiral down

Reasons:

Soft iron pole piece not


perfectly symmetric
Soft iron-
inhomogeneous
microstructure
Imperfectly centred
apertures
Unclean apertures- get
charged and deflect the
beam

For object points off the optic axis, the path length criterion shows that, there
will be a focus for rays traveling in the horizontal plane at a different position
from the focus for the rays traveling in the vertical plane.
All monochromatic aberrations can be reduced if only the central portion of
the lens is used.
no astigmatism overfocused underfocused

images with astigmatism

Scanning electron micrograph of magnetic tape


Some Definitions
Depth of field: range of positions for the object for
which our eye can detect no change in sharpness
0.61
h
sin tan

aperture

h Plane of
optimum focus

d1

d1 is limited by diffraction and


aberrations
Micrographs of blood
corpuscles
(a) optical, (b) scanning
How to increase DOF in SEM
Smaller HOW? 0.61
h
sin tan

But
resolution
decreases!
Trade-off

AND/OR increase the Working Distance !


Depth of Field

Magnification Depth of field, m


Optical SEM
10 60 1000
100 8 100
1000 0.2 10
10000 -- 1

Depth of focus: range of positions at which the


image can be viewed, without appearing out-of-focus.
Electron Optics
Electrons are charged particles, they can be
accelerated in a E field.
The trajectory of an accelerated charged particle
can be deflected by E and/or B field.
According to de Broglie, the accelerated (high
energy) particles also behave like waves.
Basic e- optics
Magnetic field
Electromagnetic lenses are universally used
Lorentz force on the moving e-
F = - e v B;
v = electron velocity; B = magnetic field
Vary I through the coil, change the magnetic field
and hence the focal length
Spiraling of e- occurs as they travel through the
microscope lenses.
Rarely travel an integral number of turns =>
rotation of image
Important when correlating the diffraction pattern
with the image in TEM
Electron Source

Generation of electrons that can be accelerated by


high tension to obtain the illuminating electron beam.

Thermionic gun:

triode or self-biasing gun,


W, LaB6, CeB6

Field Emission Gun:

Single crystal W
Electron Sources

Thermionic Emitters

Field Emitters
Thermionic Electron Gun
Electrons are emitted from a heated tungsten
filament and then accelerated towards an anode; a
divergent beam of electrons emerges from the
anode hole.

Commonly used electron source

Robust, cheap and does not require relatively high


vacuum
A short LaB6 rod is supported by a ribbon or strip through
which an electrical current is passed for heating. The rod is
heated by conduction from the ribbon.
The ribbon material is chosen to be chemically inactive with
the LaB6, such as graphite or tantalum
Thermionic Gun Electron Source

Energy Spread:

filament imperfections
High tension instability
Surface temperature
Boersch effect (mutual interaction)

Source spot size


30 m for W
5 m for LaB6
Field Emission Gun

Very strong electrical fields (109V/m-1) used to


extract electrons from a metal filament.

Temperatures are lower than those required for


thermionic emission

Requires very good vacuum


Electron Sources

Field Emitter

Single oriented
crystal of tungsten
etched to a fine tip

The emission of electrons that are stripped


from parent atoms by a high electric field
//Work Function:
Min. energy (or work) required to withdraw an electron
completely from a metal surface. This energy is a measure of
how tightly a particular metal holds its electrons//

FEG: The emission process itself depends on the


work function of the metal, which can be affected
by adsorbed gases. This is the reason a very high
vacuum is required.

Sustaining high electrical field gradients is also


essential to emission, so a tip that is well worn
might not emit electrons at all.
From Fultz, Howe:

Features of e- sources Transmission electron


microscopy &
diffractometry of materials
Electron-specimen interactions

High energy electrons are focussed to a fine probe


on a sample (bulk or specially prepared thin)

The interaction between high energy electrons and


the atoms of the sample gives rise to a variety of
signals.

Detection and quantitative characterization of the


signals form the basis of SEM and TEM.
Why electrons?

Wave behavior
Images and diffraction patterns
Wavelength can be tuned by energies
Charged particle behavior
Strong electron specimen interactions
Chemical analysis is possible
INFORMATION AVAILABLE

Morphology size, shape and distribution of phases


and their relationship to one another, high
resolution, m to nm (or fraction of it) level

Crystallography - arrangement of atoms and their


degree of order, detection of equilibrium and
metastable precipitates, orientation relationship

Composition elements present in the sample and


their local variation - high resolution
e-atom interactions
Scattering of e
Mean free path of scattering processes ~thickness of TEM
specimen
Hence an e is scattered only once or never while passing through the
TEM specimen
SEM- thick specimen=> multiple scattering

Elastic scattering
Coulombic interaction
Primary e energy does not change
Direction may change
Strongly forward peaked distribution of scattered e
Probability of scatter through angle
p() 1/(E02sin4); for small , p() is high
Importance of elastic scattering in EM
It is the major mechanism by which e are deflected
Scattered e mainly contribute to the diffraction patterns
Inelastic scattering
Primary e loses detectable amount of energy
K.E. of primary e
Heat (almost all)
X-rays
Secondary e very small energy
Light useful for imaging or analysis
Electron-specimen interactions
Inelastic scattering & absorption
Interaction volume: 95
% of primary e are
brought to rest by
inelastic processes.
A few primary e are
backscattered and
leave the specimen
Thick specimen & the interaction
volume
Electron beam-sample interactions

Interaction volume increases with increasing acceleration


voltage and decreases with increasing atomic number
Secondary effects
Secondary e
e escape from the surface with energies <50 eV
e- to which small amount of energy has been transferred
within a short distance of the surface
Yield = number of emitted e/number of primary e ~ 1 or >1
Hence SE are abundant => for imaging in SEM
Backscattered e
Some primary e may escape the surface before giving up
all their energy
Not as numerous
Carry high energy
Use: imaging, diffraction and analysis in SEM
X- rays (relaxation of excited atoms)
X- rays are characteristic
Energy of X-ray = f( ~ in energy of the two excited
states and is characteristic of the particular atom
species)
TEM
The TEM Column
Gun
(thermionic) Tungsten
filament, LaB6
Tungsten crystal (field
emission) 100x brighter
Condenser lens:
control beam intensity,
density, convergence

Objective lens:
magnification,
introducing contrast

Intermediate lens:
further magnification,
imaging or diffraction

Projector lens: final


magnification
Schematic
of SEM
Imaging Hardware

Film: 3.5 x 4 cm, small grain size


CCD: fast readout, good dynamic range, poor
resolution
Imaging plates: excellent dynamic range, high
cost
Factors affecting TEM image contrast
Ray diagram showing the imaging process at the objective
Lens in a TEM
Common Modes of Operation of TEM

Bright Field (BF) Microscopy

Selected Area Diffraction

Dark Field (DF)


Formation of Diffraction Spots from
Different Planes
(a) (b)

Formation of (a) Bright Field (BF) and


(b) Dark Field (DF) Images
Imaging in (a) BF mode, (b) DF mode with shift of
objective aperture and (c) DF mode with beam tiltin
BF DF
Spherical precipitates in an Al-Li alloy at 80,000 X
magnification.
Left: BF image.
Right: DF image from (100) diffraction spot, unique to
precipitates.
Electron Diffraction
Elastically scattered electrons produce
electron diffraction patterns
DP is spatial distribution of scattered
electrons- tell about atomic arrangement
DP- 2 parameters
Angular distribution of scattered e
Intensity
Diffracted beams are indexed with Miller
Indices without parenthesis, e.g. 110
Strong diffraction from atomic planes that
are almost parallel to the e beam.
For XRD, theta can be very large!
Structure Factor
Predicts planes that will not diffract-
Forbidden reflections (Intensity = 0)
Geometry of Pattern

r r Incident beam
tan 2 ,2 ,since is very small
L L specimen

Braggs Law 2d sin


2
r Diffracted beam
Hence, or rd L L
L d undiffracted
beam
1
or r
d r

Distance of diffraction spot from the direct beam varies inversely


as the d spacing of the diffracting plane!
Remember, planes with higher indices have lower d spacing
Diffraction
Spot pattern
Single crystal within the illumination area
The regular arrangement of spots 2
Spot brightness relates to the structure factor I F

f = atomic scattering factor (= scattering from a single atom)


uvw = unit cell position where atom is located
hkl = plane that diffracts
Spot position relates to the d-spacing

bcc
Imaging Defects
Diffraction Contrast- dominant mechanism for
imaging dislocations and defects in the specimen
The size of the objective aperture in bright-field
mode directly determines the information to be
emphasized in the final image. When the size is
chosen so as to exclude the diffracted beams-
so-called diffraction contrast .
a crystalline specimen is oriented to excite a
particular diffracted beam (g vector), or a
systematic row of reflections, and the image is
sensitive to distortion of crystal lattices due to
defects, strain and bending. (g.b#0 )
The resolution of this imaging technique is 1-3
nm. Diffraction contrast mainly reflects the long-
range strain field in the specimen.
Diffraction Pattern- Spot to Ring

Polycrystalline Au
Ring Patterns- what information?
Amorphous materials

Diffused ring pattern


Reflecting the short range ordered structure
Often seen at contamination layer or on
carbon support film
TEM Specimen Preparation
The major part of any TEM investigation is
the specimen preparation!
thin enough and containing the defects to
be investigated
Beware of artifacts!
TEM sample preparation

Bulk ceramics
Mechanical grinding, polishing, dimpling
Ion erosion, focused ion thinning

Metals
Mechanical grinding, polishing
Electrolytic thinning

Organic Materials
Freeze drying, embedding,
ultramocrotomy
Preparation of powder samples
Small particles:
Direct transfer to carbon film mounted on Cu grid
Ultrasonic dispersion of suspension on C/Cu
Membrane filtration and subsequent dissolution
of the filter
Large particles:
Embedding in resin (phenyl formaldehyde)

La2RuO5 particles
In resin
Powder Samples
Dimpling
3 mm diameter disc- punch/ultrasonic cutter
Ion beam thinning
Electrothinning- Twin-jet electropolisher

specimen punch

sample
grids
Drawbacks
Can take a lot of time to make sample thin
enough to be transparent to electrons
Viewing area only shows a small section of the
sample being analyzed, which can differ from
the rest of the sample
The sample can be damaged by the electrons,
especially when dealing with biological samples
Uses optical system lens aberration
Vibration of stage
Reference Books
Transmission Electron Microscopy: A Textbook
for Materials Science (4-Vol Set) by David B.
Williams, C. Barry Carter
Transmission Electron Microscopy and
Diffractometry of Materials by Brent Fultz, James
Howe
Electron Microscopy of Thin Crystals by Peter B.
Hirsch
Electron Microscopy and Analysis, 3rd ed. (2000)
by Peter J. Goodhew, John Humphreys, and
Richard Beanland