Electron microscopy

M. Sathish
Functional Materials Division
CECRI-Karaikudi

Contents (Overall)
Introduction to Surfaces
Surface modification
Characterization techniques
Catalysis and surface reactions
Electrochemical Energy storage
systems ???
???????

Contents
Introduction to Surfaces
Adsorption Vs Absorption
Langmuir-Blodgett Adsorption
Self-assembled monolayer
Surface modification
BET Analysis

Microscopy-Dimension

Resolution magnification
is the ability to separate two objects optically

Unresolved

Partially resolved

Resolved

The human eye can separate 0.25 mm (250 m)

at a normal viewing distance of 25 cm
The light microscope can separate 0.25 m
(0.00025mm) depending on wavelength of light
used
Electrons have a smaller wavelength than light
therefore provide the highest resolving power
about 2 nm (0.000002mm)

Useful magnification

= Naked Eye resolution/Resolving power

= 250/0.25
= 1000 X , (X means diameter)

For electron microscope

Resolving power = 0.0027 mm for 50,000 V
So the order of magnification will be 1,00,000

Aberrations of the electron lenses, complex nature of

electron-sample interaction

Origin of Electron Microscope

Year

NAME

1897

J. J. Thompson

Discovers the electron

1924

Louis deBroglie

Identifies a wavelength to moving electrons

=h/mv where
= wavelength
h = Planck's constant
m = mass
v = velocity
(For an electron at 60kV, = 0.005 nm)

1926

H. Busch

Magnetic or electric fields act as lenses for electrons

1929
1931

E. Ruska
Knoll & Ruska

Ph.D thesis on magnetic lenses

First electron microscope built

1931

Davisson &
Calbrick
Driest & Muller

Properties of electrostatic lenses

von Borries &

Ruska
RCA

First practical EM (Siemens) - 10 nm resolution

1934
1938
1940
1945

EVENT

Surpass resolution of the LM

Commercial EM with 2.4 nm resolution

1.0 nm resolution

Basics
de Broglie wavelength of electron

h
h

p mv

If electron is passing through the potential V, it acquires KE

1 2
KE mv eV
2

; m 2v 2 2meV ; mv 2meV

Now, wavelength of electron

h
h

mv
2meV

If V = 60,000 volts,

h
6.626 1034

2meV
2 9.110 31 1.6 10 19 60000
0.005 nm

Basics

1.23 / V
V

(nm)

v(X1010 cm/sec)

v/c

50000

0.0055

1.326

0.442

100000

0.0039

1.875

0.625

1000000

0.0012

5.930

1.977

1.23 /(V 10 V )nm

6

Relativistic correction when electron

velocity approaches the speed of light
mass increases

v(X1010 cm/sec)

v/c

50000

1.283

0.414

100000

1.699

0.548

1000000

2.917

0.941

speed of light in vacuum

(c = 3 X 1010 cm/sec)

Types of Microscopes
Transmitting - the probe beam is passed through the sample
differently refracted and absorbed beam area analysed

Scanning - the probe beam is scanned over the surface and the
image is created point-by point

Other kinds of Scanning microscope

Scanning Ion microscope charged ions are used, the process etches
away the top surface

Scanning Acoustical microscope ultrasonic waves are used

wavelength limited- good for biological sample

Scanning light microscope Visible light is used, colour enhancement

Scanning confocal microscope finely focused beam of
monochromatic light is used

Components of Microscopes

1.Illumination source
2.Condenser lens to converge the beam onto sample
3.Objective lens to magnify the image

4.Projector lens to project the image to screen

Analogy between LM and EM

Source

Condenser Lens
Specimen
Objective Lens

Projector Lens

Screen

Components of EM
1.Electron Gun
2.Electron Lenses
3.Scan Coils

4.Electron Detector

Electron Gun
Provides a stable beam of electrons
Thermionic emitter the work function of metal is
overcome by the surface temperature of the
filament

Components of SEM-Electron gun

Function Provides a stable beam of electrons

W wire radius ~100 m

Temp = 2000-2700 K

Components of SEM - Electron Lens

Cu coil enclosed in iron casting

Lorentz formula

F is the force
E is the electric field
B is the magnetic field
q is the electric charge of the particle
v is the instantaneous velocity of the
particle

Two kinds of lens :

Condenser lens
Objective lens

Electromagnetic Lenses
An electromagnetic lens is essentially
soft iron core wrapped in wire
As we increase the current in the wire
we increase the strength of the
magnetic field

Recall the right hand rule electron will

move in a helical path spiralling towards
the centre of the magnetic field

Lens aberrations
Electron optics suffers from aberrations. Unlike light optics,
there is no way to solve it, but we can reduce

Spherical aberration
Electrons in far away trajectories from the optic axis are
bent more strongly

Chromatic aberration

The extent of deflection of electron by converging lens

depends on energy of the electron shorter wavelength
less deflection (opp to light optics)

Aperture diffraction

Due to the wave nature electron beam diffract

upon passing through a narrow slit

Astigmatism

Improper shape of beam

Lens aberrations

Spherical aberration

Aperture diffraction

Chromatic aberration

Astigmatism

The Scanning Electron Microscope is analogous to

the stereo binocular light microscope because it
looks at surfaces rather than through the
specimen

Diagram of Scanning Electron Microscope

In cross section view - the electrons are in green

Electron beam
produced here
Cross section of
electromagnetic
lenses

Sample

Beam passes down

the microscope
column
Electron beam now
tends to diverge

But is converged by
electromagnetic
lenses

Electron beam Specimen Interaction

Note the two types of electrons produced.

Electrons from the focused beam interact with the

sample to produce a spray of electrons up from the
sample. These come in two types either secondary
electrons or backscattered electrons.
As the beam travels across (scans across) the
sample the spray of electrons is then collected little
by little and forms the image of our sample on a
computer screen.

We can look more closely at these two types of

electrons because we use them for different
purposes.

Inelastic scattering Vs Elastic scattering

A new electron is
knocked out (as a
secondary electron) -

An incoming electron
rebounds back out (as a
backscattered electron)
-

Inelastic scattering

Energy of electron from

beam is lost to atom

Elastic scattering

Secondary electrons Vs backscattered electrons

Secondary electrons

Contrast of these grains

is all quite similar three-dimensional image
of the surfaces.

backscattered electrons

Grain containing of
silica - darker

Grain containing
titanium - whiter

The differing contrast of the

grains tells us about composition

Working principle
Composition from backscattered electrons

The higher the atomic number of the atoms the

more backscattered electrons are bounced back
out

This makes the image brighter for the larger atoms

Titanium Atomic
Number 22

Silica Atomic
Number 14

Understanding compositional analysis using X-rays

and the scanning electron microscope

Inelastic scattering

If the yellow electron

falls back again to the
inner ring, that is to a
lower energy state or
valence, then a burst of
X-ray energy is given
off that equals this
loss.
This is a characteristic
packet of energy and
can tell us what
element we are dealing
with

EDS output from X-rays

Amount of
packets

1050
900

Characteristic oxygen peak

CKa

1200

Characteristic carbon peak

006

Characteristic chlorine peak

ClKa

600

OKa

Counts

750

450
300
150
0
0.00

1.00

2.00

3.00

4.00

5.00

6.00

keV

Energy of packets
in thousands of electron volts

7.00

8.00

9.00

10.00

Using X-rays to investigate composition in this

way is called Energy Dispersive Spectroscopy
(EDS) since it produces a spectrum graph

We can get detailed information about mass

and atomic percentages in materials from EDS