3

Transmission Electron
Microscopy
magni
Electron microscopes generate images of material microstructures with much higher
fication and resolution than light microscopes. The high resolution of electron microscopes
The wave
results from short wavelengths of the electrons used for microscope illumination.
shorter than that of visible
length of electrons in electron microscopes is about 10,000 times
of 0.1 nm if lens aberra
light. The resolution of electron microscopes reaches the order
microscopes extremely use
tions can be minimized, Such high resolution makes electron
There are two main types of
ful for revealing ultrafine details of material microstructure.
clectron microscopes: transmission electron microscopes (TEM) and scanning electron mi
conventional transmission light
croscopes (SEM). The optics of the TEM is similar to the microscopes.
scanning confocal laser
microscope, while that of SEM is more like that of
features of transmission electron
This chapter introduces the basic working principles and
microscopes.

3.1 Instrumentation
microscope, has the fol
Atransmission electron microscope, similar to atransmission light
lens, specimen stage, ob
lowing components along its optical path: light source, condenser differences are that, in a
main
jective lens and projector lens as shown in Figure 3.1. The
lenses for visible light
TEM, the visible light ray is replaced by an electron ray and glass has more lenses (the
are replaced byelectromagnetic lens for the electron beam. The TEM
aperture). The TEM con
intermediate lens) and more apertures (including the selected area
For example, a vacuum
tains further features arising from using electrons as illumination.
energy electrons and air
environment is required in a TEM because collisions between high
comparison of aTEM with
molecules significantly absorb electron energy. Table 3.1 provides a in detail in the following
microscope. Structural features of the TEM are introduced
a light
sections.

Muterials Characterization Yang Leng

O 2008 John Wiley & Sons (Asia) Pte Ltd
 Matcrials Characterization
80

Light and Transmission Elcctron Microscopcs

Table 3.1 Comparison Between
Transmission electron
Transmissionlight microscope microscope

scction Thin section (<200 nm)

Polished surface and thin
Specimen requirements
(<100 um)
~200 nm
~0.2nm
Best resolution 500-1,000,000 ×
2-2000 >x
Magnification range High-specd electrons
Sourcc of illumination Visible light
Glass
Electromagnetic
Lens
Operation environment Air or liquid High vacuum
On phosphorescent plate
Image formation for vicwing By cyc

High vacuum

Electron gun

Accelerator

Illumination 1st condenser lens

2nd condenser lens

Specimen stage Specimen

Imaging Objective lens

Intermediate lens

Magnification

Projector lens

Fluorescent screen
Photographic tilm
Data recording CCD camera

optical path.
Figure 3.1 Structure of atransmission electron mieroscope and the
 81
Transmission Electron Microscopy

Resolution
Table 3.2 Correlation betwcen Acccleration Voltage and
TEM resolution (nm)
Electron wavelength (nm)
Acceleration voltage (kV)
0.56
0.0060 1
40 0.46
0.00487
60 0.00418 0.39
80 0.00370 0.35
100 0.00251 0.24
200 0.00142 0.13
500

3.1.1 Electron Sources

illumination.
generates a high energy electron beam for
In a TEM system, an electron gun accelerated by
from acathode, a solid surface, are
In the electron gun, the electrons emitted electron
electron beam with energy E= eVo. Because
high voltage (Vo) to form a high energy determines resolution
and wavelength largely
energy determines the wavelength of electrons voltage determines the resolution to a large
accelcration
of the microscope (Equation 1.3), the between the acceleration voltage and wavelength. It
extent. Table 3.2 gives the relationship which is
acceleration voltage and the TEM resolution,resolution,
also provides the correlation between
6.5 x 10-5 radians. To achieve a high
calculated with a realistic a angle of about practice,
acceleration voltage of greater than 100 kV. In
the TEM is usually operated under an most resolution requirements. High-voltage electron
200 kV is commonly used and meets damage
(~1000 kV) requires extremely expensive instrumentation, and also it may
microscopy defects in it during observation.
microstructural
a specimen by generating gun is composed of three main
parts: cathode or electron
general structure of an electron emitted from
The
Wehnelt electrode and anode, as illustrated in Figure 3.2. Electrons are Wehnelt
source, an electric field toward the cathode. The
cathode and accelerated by
the surface of the hundred volts negative
is placed between the cathode and the anode. It is biased a few fluctuation by
electrode the electron beam against voltage
cathode in order to stabilize
with respect to the

Cathode

Wehnelt
electrode

Anode

Figure 3.2 General structure of an electron gun.

 Materials Characterization
82

nccessary. There are two basic types of electron

reducing the electronbeam current whenever
field emission.
guns: thermionic emission and
Thermionic Emission Gun
the
and includes the tungsten filament gun and
This is the most common typc of clectron gun tungsten filament as the cathode. During
lanthanum hexaboride gun. The tungsten gun uses a
(filament current) to high temperature
operation, the filament is heated by electrical current
energy for electrons to overcome the surface
(2800 K). The high tempcraturc provides kinetic The
electrons in the filament to leave the surface.
cnergy barrier, enabling the conduction
clcctric voltage between the filament
clcctrons leaving the surface are acccleratcd by a high
of the clectron beam is determined by the
and anode to a high energy level. The intensity
filament temperature and acceleration voltage. and it is more widely used
Lanthanum hexaboride (LaBo) is a better cathode than tungsten
kinetic energy to escape from the LaBo
in modern clectron microscopes. Electrons require less smaller than the 4.5 eV of tungsten.
surface because its surface work function is about 2eV,
can generate a higher intensity
Thus, a lower cathode temperature is required. A LaB6 cathode disadvantage is that a higher
clcctron beam and has a longer life than a tungsten filament. One
tungsten filament gun.
level of vacuum is requircd for a LaB6 gun than for a
Field Emission Gun
thermal energy for electrons to overcome
This typc of clectron gun does not necd to provide
out by applying a very high
the surface potential barrier of electrons. Electrons are pulledthermionic effect, makes metal
of a
clectric ficldtoa metal surface. A tunncling effcct, instead electrons are
barrier. During operation,
electrons in the conducting band cross the surface
physically drawn off from avery sharp tip of tungsten crystal (~100 nm tip radius) by an
the highest intensity electron beam,
applied voltage field. The field emission gun generates and 10 timnes greater than that of the
10° times greaterthan that of the tungsten filament gun
emission guns: thermal and cold guns. The thermal
LaB, gun. There are tWo kinds of field
temperature of about 1600-1800 K, lower than that
field emission gun works at an elevated noise. The
thermionic emission. It provides a stable emission current with less emission
of
temperature. It provides a very narrow energy spread
coldfield emission gun works at room
in air. The bombardment of the tungsten tip
(about (0.3-0.5 eV), but it is very sensitive to ions maintenance (called
of the emission. Thus, regular
by residualgaseous ions causes instability torr is required to operate the
vacuum of 10-0
flashing ) of the tip is necessary. Generally, a
comparison of various kinds of electron guns.
coldfield emission gun. Table 3.3 shows a

Guns
Table 3.3 Comparison of Electron
Field emission
Tungsten Cold
filament LaBo Thermal

L600~ I800 ~300

~2800 n800
Operalion temperature (K) ~5x 0
~5x 10
Brightness At 200kV (A Cm s) 10-10 10-9 t0-10-0
Requirement to vacuum (Tor)
angle.
Intensiiy eimilled per unit cathode surface in unit sohd
bi orT = 133 Pa.
 Mateiais Characterizatin

33T Mass-Density Contnast

nucieus
The defvtonof elvtons can esult from interaction between electrons and an atomic cicctron.
mass than an
DetiecuOn of an elovton by an atomic nucicus, which has much more
changes its path atter
is like a collision ewen a particle and a wall. The particle (clectron)
colision. The amount of elevOn scattering at any specific point in a specimen depends on the
Thus, ditterence in thickness and
mass-density (protuct of density and thickness} at that point. rveived by an image screen
eiecton intensity
density in a specmen will generate vanation in
beam to pass the objective aperture as shown
in the TEM. if we only allow the transmittedscatterning angle larger than the a angle (in the
in Figur 3.13. The defiected electron with by the aperture nng.
obiective aperture will be blocked
order of0.01 radians) controlled by the transmission beam as the beam passes through
duces the intensity of the
Thus, the aperture beam leaving the
bnghtness of the image is determined by the intensity of the electron intensity of the
it. The through the objective aperture. The
lower surtace of the specimen and passing primary beam (l,)less the intensity of beam
deflected
ransmited beam (7;) is the intensity of
by object (lg) in a specimen. (3.1)

deined by Equation 3.2.

The contrast (C) in a TEM is (3.2)
C= (l, - )/1,
mechanism
contrast exists in all types of materials. It is the main
Thistype of mass-density and biological
materials such as amorphous polymers
non-crystalline
for image formation for
Primary beam

Sample

Scattered
beams Objective lens

Objective aperture

Additional magnitying
lenses
A Fluorescent screen

Intensity profile Bright

on the Screen Dark
with permission
mass-density contrast in the TEM.(Reproduced 1980 Elsevier
arrangement of York. O
Figure 3.13 Optical Electron Microscopy ofMaterials, Academic Press, New
from M. von Heimandahl,
B. V.)
 91
Transmission Electron Microscopy

described as 'absorption contrast', which is rather

specimens. The mass-density contrast is also
absorption by the specimen.
misleading because there is little electron biological specimens often are stained by solu
to increase contrast, polymeric and oxides
Inorder heavy mnetal oxides. The ions of metal
such as
tions containing high density substances constituents of the microstructure, and thus increase
in solution selectively penetrate certain
mass-density. Figure 3.14 is an example of a TEM image showing mass-density contrast in
its polycarbonate (PC) and polybutylene terephthalate
a specimen of polymer blend containing
rich in staining substance, RuO4. Besides
(PBT).The PC phase appears darker because it is
contrast include using a smaller objective
staining, common effective techniques to increase
negative side of using such techniques is
aperture and using a lower acceleration voltage. The
reduction of total brightness.

PC

PBT

Crack

1um
Crack Tip

PBT

PC

Crae

specimen is
Figure 3.14 TEM image of PC-PBT polymer blends with mass-density contrast. The
stained with RuO4. (Reproduced with permission of Jingshen Wu.)
92 Materials Characterization

3.3.2 Diffraction Contrast

We can also generate contrast in the TEM by adiffraction nethod. Diffraction contrast is
the primary mechanism of TEM image formation in crystalline specimens. Diffraction can
collaboratively
be regarded as collective deflection of electrons, Electrons can be scattered
by parallel crystal planes similar to X-rays. Bragg's Law (Equation 2.1), which applies to
conditions are satis
X-ray diffraction, also applies to electron diffraction. When the Bragg
orientation, constructive diffraction
fied at certain angles between electron beams and crystal
specimen results, as schematically illustrated in
OCcurs and strong electron deflection in a when the objective aperture
Figure 3.15. Thus, the intensity of the transmitted beam is reduced

Primary beam lo
lo
Sample

201 Objective lens

(Back focal plane
Objective aperture
LPlane of diffraction pallern

Transmitted beam L
I, =Diffracted beam

Image plane (single-slage

magnified image)
(a)

Crystalline objcct.
containing inclusion

Bragg
diffraction

Diffraction
(b) from inclusion

diffraction of a crystalline specimen: (a)

image formation
Figure 3.15 Electron deflection by Bragg contours of inclusions.
(b) diffraction at crystal lattice planes and at the
Electron Microscopy of Materials, Academic
in crystalline samples; and
Heimandahl,
(Reproduced with permission from M. von
Press, New York. © 1980 Elsevier B. V.)
 93
Transmission ElectronMicOscopy

the situation of
mass-density contrast. Note that the
similar to
the diftraction beanms, contrasts is that the diffraction contrast is very sensitive to
blocks between the (wo sensitive to total mass
main difterence mass-density contrast is only
specimen holder but
specimentiltingin the area. from a
in thickness per
surface
very small (<1°) and the diffracted beam
The diftraction angle (20)
in aTEM is on the back-focal plane of
the
focused as a single spot
crystallographicplane (hkl) can be useful for interpreting electron diffraction in
is particularly
objective lens. The Ewald spherebeam is parallel to a crystallographic axis, all the diffraction
the TEM. When the transmitted form a diffraction pattern (a
reciprocal lattice) on the
will
points from the same crystal zone
2.9 and 2.11.
back-focal plane as shown in Figures bright-field and dark-field TEM images. In order to
generate
The diffraction contrast can dark-field images, the diffraction mode in a TEM
bright-field and
understand the formation of modes: the image mode and the diffraction
can be operated in two
must be mentioned. A TEM changing the optical path in the TEM as illustrated
between the modes by
mode. We can switch specimen is focused and projected onto a
image mode, the image of the
in Figure 3.4. In the mode, the diffraction pattern formed on the
back-focal
fluorescent screen. In the diffraction diffraction
projected onto a fluorescent screen as shown in Figure 3.16. The TEM
plane is reciprocal lattice of crystal (Section 2. 1.1).
pattern shown in Figure 3.16 exhibits a plane of the contains a
a selected area in the specimen that
Such a pattern is obtained by diffraction from selected-area diffraction (SAD), which is
single crystal. The diffraction mode is designed for
discussed further in Section 3.4.
the transmitted beam to pass the objective
A bright-field image is obtained by allowing only dark-field image, however, is obtained
aperture, exactly the same as in mass-density contrast. A
aperture. Figure 3.17 illustrates the
by allowing one diffraction beam to pass the objective switch between bright- and dark
optical arrangement of bright- and dark-field contrast. To
first in order toselect one diffraction
field modes, we need to operate in the diffraction mode
center of that spot (Figure 3.18).
spot in the diffraction pattern by moving the aperture to the of the incident beam is moved,
direction
However, what really happens in the TEM is that the 3.17c).
to the central axis (Figure
rather than the aperture, to shift the selected diffraction spot polycrystalline A-Cu alloy
Figure 3.19 shows an example of a bright-field image of aresults from the strong diffrac
with grain boundaries. The darker appearance of certain grains
specimen we change the diffraction
tion from their crystallographic planes. When we tilt the brighter grains will become darker.
angle, and the darker grains will become brighter and the

single crystal. The transmitted spot

Figure 3.16 Photograph of a typical electron diffraction pattern of
at the center is much brighter than the diffraction spots.
 TraC
Dirae
dark-ieid imaging
wh oetve paure fr
Figure313 Seleia ae a dirzatO Ot

oducowth pemIs
 95
Transmission Electron Microscopy

300nm

Figure 3.20 Bright-field image of fine grained Al-Fe Si alloy. Only a few grains are visible at certain
specimen orientations.

Diffraction contrast is very sensitive to specimen tilting. Even atilt of less than 1° can cause the
contrast to change from bright to dark. On the other hand, note that the grains are not always
obvious in diffraction contrast. At certain diffraction angles, only a few grains might satisfy
the Bragg conditions and be revealed (Figure 3.20).

image of AI-Fe-Si alloy: (a) bright-field; and (b)

Figure 3.21 Comparison of bright- and dark-field
dark-field images.
 Materials Characterization
Dark-field
reveal
is not as
commonly used as bright-field imaging,
may more fine features that are bright when the However, the dark-ficld image
shows compar1son between bright- and
a background becomes dark. Figure 3.21
alloy. The dark-hcld image (Figure 3.2lb) dark-field images for the same area in an Al-Fe- Si
reveals finer details inside the
corresponding to a single bright-fieldgrains.
there are several dark-field images Interestingiy.
can select different diffraction spots (hkl) in Figure image because we
3.18 to
different from light microscopy in which there is a one-to-oneobtain a dark-field image. ms
dark-fieldimages. When tlting a specimen to generate a high correlation between brignr d
intensity diffraction spot (nkI
we may chose the spot of (hkl), wvhich must exhibit low intensity in this circumstance, to torm
a dark-field image. This type of dark-field image is called the weak-beam dark-held mags
Weak-beam imaging is useful for increasing the resolution of fine features such as dislocations
in crystallinematerials.

3.3.3 Phase Contrast

amplitude contrast because they use only
Both mass-density and diffraction contrasts are change
amplitude change of transmitted electron waves. Chapter 1 mentions that phase
difference in
the Similarly, a TEM can also use phase
generates contrast in light microscopy.
mechanism, however, is much more
The phase contrast
electron waves to generate contrast. highest
that of light microscopy. The TEM phase contrast produces the is
complicated than for crystalline materials. Thus,
phase contrast
lattice and structure images
resolution of microscopy (HRTEM).
to high resolution transmission electron phase.
often referred as
at least two electron waves that are different in wave
Phase contrast must involve beam) to
two beams (the transmitted beam and a diffraction
Thus, we should allow at
least specimen
TEM. Formation of phase contrast in a crystalline
participate in image formation in a crystalline specimen with a periodic lattice
structure
Figure 3.22. A objective lens
is illustrated simply in between the transmitted and diffracted beams. Thetransmitted and
generates a phase difference Recombination of
difference among the beams.
generates additional phase
interference pattern with periodic dark-bright changes on
diffracted beams willgenerate an interferences, as shown in Figure 3.23. An interference
of beam
the image plane because reveals the periodic nature of a crystal.
when more
pattern isa fringe type that of phase contrast images is complicated, particularly illustration in
Theoretical interpretation image formation. The schematic
participates in theory of
than one diffraction spot the complexity of phase contrast. The electron wave
Figure 3.22 does not refiectexplained briefly in the following section.
phase contrast formation is

Theoretical Aspects TEM is illustrated by Figure 3.24. The properties

phase contrast in a
The electron wave path of represented by an object function, fr), which
exiting the specimen are position vector from the
of electron waves wave amplitude and phase. r is the
Equation 3.3.
includes the distributions of function may be represented as a function in
centraloptical axis. Theobject
(3.3)
fr) = [1- sr)] exp (id(r))