Scanning Electron Microscopy

Field
emitting tip

2kV
100kV

Grid
Anode

ZEISS SUPRA
Variable Pressure FESEM

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Workshop 2012

Dr Heath Bagshaw CMA

bagshawh@tcd.ie

Why use an SEM?

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Fig 1. Examples of features resolvable using different imaging techniques

Improving Resolution
Firstly, the wavelength of the imaging source is important.
In an optical microscope white light is used ( 380-700-nm)
In an Electron Microscope the imaging source is a beam of electrons which has a
shorter wavelength ( ~0.0025nm at 200kV) .
This is approximately five times smaller than visible light and twice as small as a
typical atom this is why electrons can see atoms but white light cant :the analysis probe must be smaller than the feature being analysed
The wavelength of electrons is dependent on the accelerating voltage, i.e.:kV

Wavelength (pm)

20

8.588

100

3.702

200

2.508

300

1.968

The higher the accelerating voltage the shorter the wavelength.

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The Parts of an EM
Electron Microscopes (EMs) are similar in operation to optical microscopes except
that they use a focused beam of electrons instead of light to "image" the specimen and
gain information about its structure and composition.
There are four major regions in an Electron Microscope:(1) A stream of electrons is formed (by the electron source/gun) and
accelerated toward the specimen using a positive electrical potential
(2) This stream is confined and focused using metal apertures and magnetic
lenses into a thin, focused, monochromatic beam.
(3) This beam is focused onto the sample using a magnetic lens. In an SEM
the beam is then also scanned across the surface of the sample.
(4) Interactions occur inside the irradiated sample, affecting the electron
beam which are detected and transformed into an image or signal.
The above happens in all EMs regardless of type.
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Layout of a Generic SEM

Gun

Aperture
Holder

Deflection
coils

3
Objective Lens

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Electron Gun
There are two main types of gun Thermionic and Field Emission (FEG).
Thermionic gun :- Simplistically, a material (often a piece of twisted tungsten) is heated
to a high temperature so that it will emit electrons.
Can also use LaB6 crystal grown to a tip gives a brighter beam than W for same kV.

Tungsten filament

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Tungsten filament assembly

LaB6 filament tip

Thermionic Gun
Filament

Wehnelt
cylinder

10-10000kV
+

Anode
earth

Filament is heated and begins to produce electrons.

Electrons leave the filament tip with a negative potential so accelerate towards the
earthed anode and into the microscope column.
A small negative bias on the Wehnelt then focuses the beam to a crossover which acts as
the electron source.
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Field Emission Gun (FEG)

FEG source W tip

A very strong magnetic field (~109Vm-1) draws electrons from a very fine metallic tip
(usually W).
An extraction voltage of around 2kV is applied to the first anode to create an intense
electric field to allow electrons to escape from the tip.
The second anode is then used to accelerate the electrons into the microscope at the
required energy.
Combination of the two anodes focuses the beam into a crossover creating a fine
beam source.

Comparison of Sources
W filaments are very simple and inexpensive.
LaB6 filaments give greater brightness than W (approximately X10), but cost more.
FEGs give much more brightness than thermionic systems.
FEGs give a more monochromatic electron source and finer probe (i.e. better resolution).
Temperatures used are much lower than for thermionic sources (particularly cold cathode
FEGs).
FEGs require better vacuum systems and are more expensive.

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Comparison of the three types of source

operating at 100kV

Focusing the Beam

After the beam is formed it is focused by a condenser lens system to form a probe.
The lenses are electromagnetic the focal length changes as current in the coil changes.
After focusing, the beam is passed through an aperture which excludes electrons which are
not on the optical axis improving resolution.
Inconsistencies in the beam are corrected by stigmators and the beam focused onto the
sample.

A typical Electro
Magnetic Lens

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Scanning the Beam\Beam Interactions

Deflector coils move the beam back and forth over the sample and the signal
generated from each area is collected simultaneously, building up the final image
shown on the monitor.
Many signals are generated at the surface of the
sample and many different forms of analysis may be
performed.
The interaction volume is the area of the sample
excited by the electron beam to produce a signal.
Incident Electrons
(Electron Probe)
Secondary Electrons
AugerElectrons
Electrons
Auger
Backscattered Electrons
Continuum X-Rays
Characteristic X-Rays
Fluorescence X-Rays

Signals generated in the interaction volume

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Interaction Volume
The interaction volume is the area of the sample excited by the electron beam to
produce a signal.
The penetration of the electron beam into the sample is affected by the accelerating
voltage used, the higher the kV the greater the penetration.
The effective interaction volume can be calculated using the electron range, R:-

0.0276 A E
=
R
Z
0.89

1.67
0

( m)

Where A is the atomic weight (g/mole), Z is the atomic number, is the density (in g/cm3) and Eo is the energy of
the primary electron beam (in kV).
Take the example of iron:
A=55.85, Z=26, r=7.87 g/cm3
Accelerating voltage (kV)
30
15
5
1

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Primary Electron Range (m)

3.1
0.99
0.16
0.01 (10nm!)

Signals generated in the interaction volume

Signal Detection
The Everhard Thornley Detector (ETD) is the most common detector used to detect
secondary electrons to image surface topography.
Electrons are attracted to a +ve charge on a grid in front of the detector. The captured
electrons are then amplified by a photo-multiplier before being digitised and sent to a screen.
The signal detected is transferred to a viewing screen as the beam is scanned building up the
image.

Everhard Thornley Detector

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Scanning to produce an image

Biological Samples
Biological samples are not conductive and are particularly vulnerable to beam damage and
other heating effects when examined in an Electron Microscope.
The level of exposure is referred to as Electron Dose and is a measure of the number of
electrons per unit area (e/nm2).
Samples are either stained with conductive materials (e.g. OsO4) or coated with Au or C.
Samples are viewed under vacuum, so they are dried to remove all water.
a)

b)

a) SEM image of Pneumonia, and b) SEM image of Diatom (Pictures from University of Iowa)
Preparing the samples fixes, and alters them need a way to look at samples whilst they are
still wet.
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Variable Pressure SEM

Localised charging is removed by the presence of gas in the sample chamber, effectively allowing the
examination of non conductive samples
In Low vacuum mode the chamber is isolated from the high vacuum system(A) and is instead pumped
by the additional rotary pump system(B).

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Variable Pressure SEM (2)

This allows analysis of non conducting samples as charge is compensated by gas in the
chamber.
Use of an SEM in VP mode does lead to some limitations in its operation:-

Because the vacuum is lower in a VPSEM chamber, some resolution of the instrument is
lost due to scattering of the electron beam by the gas particles in the chamber.
In situ heating and or cooling (with the appropriate sample stage) is possible in VPSEM
to allow direct observation of sample changes.
Compositional analysis is still possible.
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Compositional Analysis Back Scattered Imaging

As mentioned previously, when the electron beam hits the sample a number of signals
are generated. Secondary electrons are used for looking at surface detail (topography).
EM is also a very powerful technique for analysing composition and compositional
distribution in a material\sample.

Signals generated in the interaction volume

Back Scattered electrons are produced just below the surface of the sample (B) and are
scattered more by heavier elements than by lighter elements.
The backscattered coefficient, = (Z-1.5)/6 So, as Z increases, so does the degree of
backscatter.
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Back Scattered Electrons

0.5

Backscattered
electrons

Electron yield

0.4
0.3
0.2
Secondary electrons

0.1

20

40

60

80

Atomic number (Z)

Electron yield (i.e. intensity) as a function of atomic number for backscattered and Secondary
electrons.

Back Scattered electron have approximately the same energy as the primary electron
beam and are therefore easy to detect - simply by a semiconductor placed above the
sample :-

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Schematic of a backscattered electron detector.

BackScattered Imaging
Back scattered electrons are deflected more by heavier atoms leading to a brighter
contrast in BEI images the lighter the region the heavier the element present.
a)

b)

Dark
region

White
region

Grey
region

a)Secondary image of a cement showing surface morphology

b)Backscattered image of same area showing compositional inhomogeneity
Three distinct regions in b), EDS analysis can then be used to find the different
compositions of the these regions.
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Example EDS of a Cement

There were 3 distinct regions in the Backscattered Image
Light region is made up predominantly of
Fe. (i.e. the heaviest element)

Grey region is made up predominantly of

Ca.

Dark region is made up predominantly of Si

and Al. (i.e. the lightest elements)

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Examples Images

Imaged using ET Detector

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Imaged using InLens Detector

Low kV image of platelets

Examples Images

SE image of nano tubes

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SE Image of nano structure

BE image of nano tubes

Conclusions
Scanning Electron Microscopes (SEMs) are very useful tools for looking at a range of
samples\materials.
Surface detail, homogeneity and elemental composition can be determined in one
experiment on the same sample.
Newer Variable Pressure SEMs allow the imaging of non conducting samples.
ESEMs, with cold stages and other peripherals allow imaging at 100% relative humidity
allowing imaging of wet samples
Electron Microscopy based analysis when used with other analysis techniques can
assist in complete characterisation\identification of materials.
Electron Microscopes provide a very powerful analysis tool in both Materials and
biological fields.

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