Scanning Electron Microscopy

Content

1. Introduction and History .......................... 1

1.1 Comparison of OM, TEM and SEM……………………………………...1

1.2 Characteristic Information: SEM…………………………………………2

1.3 Identification of Fracture Mode…………………………………………..2

1.4 OM vs. SEM………………………………………………………….……..2

1.5 How Fine can you see? ......................................................................3

1.6 Scale and Microscopy Techniques………………………………………4

1.7 Advantages of Using SEM over OM……………………………………..4

2. What is SEM? .......................................................................4

3. How the SEM works and How to use it…....5

3.1 Forces in a Cylindrical Magnetic Lens……………………………………..6

3.2 Beam's Path through the Column……………………………………….…7

3.3 SEM Ray Diagrams…………………………………………………………..8

3.4 Electron Beam/Specimen Interactions……………………………………...9

3.5 Using a Vacuum……………………………………………………...…….....9

3.6 Specimen Chamber…………………………………...………………….…10

3.7 Objective Lens……………………………….………..………………….....10

3.8 Stage…………………………………………………..………….…………..11

4. Fundamental Principles of Scanning Electron Microscopy (SEM)

………………………………12

5. Principle of Operation……………………………………13
5.1 Secondary Electron Imaging…………………………………...…….…….13

5.2 Backscattered Electron Imaging………………….………………….…….13

5.3 Data Output………………………………….……………………………….13

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 5.4 Breakdown of an Electron Microscope………………………………...….14

5.5 Electron vs. Optical Lenses……………………………………………...…14

6. Electron source SEM.....................................................14

7. Specimen Preparation..........................................….....16

8. Infrastructure Requirements………………………..16

9. Strengths and Limitations of Scanning Electron Microscopy (SEM)

……………………….…..….16
9.1. Strengths………………………………………………………………..….16

9.2. Limitations.....................................................................................…...17

10. Applications include…………………………………...…18

10.1 Materials evaluation………………………………….…………….........18

10.2 Failure analysis……………………………………………….………......18

10.3 Quality Control screening………………..… ………….…………...……18

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1. Introduction and History:
 Electron microscopes are scientific instruments that use a beam of
energetic electrons to examine objects on a very fine scale.
 Electron microscopes were developed due to the limitations of
Light Microscopes which are limited by the physics of light.

 In the early 1930's this theoretical limit had been reached and
there was a scientific desire to see the fine details of the interior
structures of organic cell (nucleus, mitochondria...etc.).

 This required 10,000x plus magnification which was not possible

using current optical microscopes.

 The first scanning electron microscope (SEM) debuted in 1938

(Von Ardenne) with the first commercial instruments around 1965.
Its late development was due to the electronics involved in
"scanning" the beam of electrons across the sample.

1.1 Comparison of OM, TEM and SEM:

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  Principal features of an Optical Microscope, a Transmission
Electron Microscope and a Scanning Electron Microscope, drawn
to emphasize the similarities of overall design.

1.2 Characteristic Information: SEM

1.2.1. Topography:
 The surface features of an object or "how it looks", its texture;
direct relation between these features and materials properties.
1.2.2. Morphology:
 The shape and size of the particles making up the object; direct
relation between these structures and materials properties.
1.2.3. Composition:
 The elements and compounds that the object is composed of and
the relative amounts of them; direct relationship between
composition and materials properties.
1.2.4. Crystallographic Information:
 How the atoms are arranged in the object; direct relation between
these arrangements and material properties.
1.3 Identification of Fracture Mode:

SEM micrographs of fractured surface of two BaTiO3 samples.

1.4 OM vs. SEM:

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1.5 How Fine can you see?
 The resolution of human eyes is of the order of mm, 100μm ≈ 4
mils.
 However, something vital to human beings are of sizes Smaller
than 0.1mm, e.g. our cells, bacteria, microstructural details of
materials, etc.

1.6 Scale and Microscopy Techniques:

XRD, TEM SEM OM

Microstructure ranging from crystal structure to engine components (Si 3N4)

1.7 Advantages of Using SEM over OM:

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 Magnifications Depth of Field Resolution

OM: 4x – 1400x 0.5mm ~ 0.2mm

SEM: 10x – 500Kx 30mm 1.5nm

 The SEM has a large depth of field, which allows a large amount of
the sample to be in focus at one time and produces an image that
is a good representation of the three-dimensional sample.
 The combination of higher magnification, larger depth of field,
greater resolution, compositional and crystallographic information
makes the SEM one of the most heavily used instruments in
academic/national lab research areas and industry.

2. What is SEM?
 The Scanning Electron Microscope (SEM) is a microscope that
uses electrons rather than light to form an image.
 There are many advantages to using the SEM instead of a light
microscope.
 The SEM has a large depth of field, which allows a large amount of
the sample to be in focus at one time.
 The SEM also produces images of high resolution, which means
that closely spaced features can be examined at a high
magnification.
 Preparation of the samples is relatively easy since most SEMs any
require the sample to be conductive.
 The combination of higher magnification, larger depth of focus,
greater resolution, and ease of sample observation makes the
SEM one of the most heavily used instruments in research areas
today.
 A microscope is very similar to a telescope or, for that matter, a
pair of eye glasses. All microscopes, telescopes, and glasses have
something in common - lenses.
 Since you can't really see electrons with your eyes we have to use
some other equipment to produce a television signal that shows an
image on a TV screen. Your TV at home uses electrons to produce
an image, too.
 A scanning electron microscope really is a big fancy TV attached to
some magnets!

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  The SEM is designed for direct studying of the surfaces of solid
objects.
 By scanning with an electron beam that has been generated and
focused by the operation of the microscope, an image is formed in
much the same way as a TV.
 The SEM allows a greater depth of focus than the optical
microscope. For this reason the SEM can produce an image that is
a good representation of the three-dimensional sample.

 As in any microscope the main objective is for magnification and

focus for clarity. An optical microscope uses lenses to bend the
light waves and the lenses are adjusted for focus.

 In the SEM, electromagnets are used to bend an electron beam

which is used to produce the image on a screen. By using
electromagnets an observer can have more control in how much
magnification he/she obtains.

 The electron beam also provides greater clarity in the image

produced.

3. How the SEM works and How to use it

 The electron beam comes from a filament, made of various types
of materials.
 The most common is the Tungsten hairpin gun. This filament is a
loop of tungsten which functions as the cathode.

 A voltage is applied to the loop, causing it to heat up. The anode,

which is positive with respect to the filament, forms powerful
attractive forces for electrons.

 This causes electrons to accelerate toward the anode. Some

accelerate right by the anode and on down the column, to the
sample.

 Other examples of filaments are Lanthanum Hexaboride filaments

and field emission guns.

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3.1 Forces in a Cylindrical Magnetic Lens:

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3.2. Beam's Path through the Column:

 A beam of electrons is generated in the electron gun, located at

the top of the column, which is pictured to the left.
 This beam is attracted through the anode, condensed by a
condenser lens, and focused as a very fine point on the sample by
the objective lens.

 The scan coils are energized (by varying the voltage produced by
the scan generator) and create a magnetic field which deflects the
beam back and forth in a controlled pattern.

 The varying voltage is also applied to the coils around the neck of
the Cathode-ray tube (CRT) which produces a pattern of light
deflected back and forth on the surface of the CRT.

 The pattern of deflection of the electron beam is the same as the

pattern of deflection of the spot of light on the CRT.

 The electron beam hits the sample, producing secondary electrons

from the sample. These electrons are collected by a secondary

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 detector or a backscatter detector, converted to a voltage, and
amplified.
 The amplified voltage is applied to the grid of the CRT and causes
the intensity of the spot of light to change.

 The image consists of thousands of spots of varying intensity on

the face of a CRT that correspond to the topography of the sample.

3.3. SEM Ray Diagrams:

 The following schematics show the ray traces for two probe-
forming lens focusing conditions: small working distance (left) and
large working distance (right).
 Both conditions have the same condenser lens strength and
aperture size. However, as the sample is moved further from the
lens, the following occurs,

 The working distance S is increased

 The demagnification decreases
 The spot size increases
 The divergence angle alpha is decreased.

 The decrease in demagnification is obtained when the lens current

is decreased, which in turn increases the focal length f of the lens.

Figure: The Ray Traces for two probe-forming lenses.

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  The resolution of the specimen is decreased with an increased
working distance, because the spot size is increased.
 Conversely, the depth of field is increased with an increased
working distance, because the divergence angle is smaller.

3.4. Electron Beam/Specimen Interactions:

 While all these signals are present in the SEM, not all of them are
detected and used for information. The signals most commonly
used are the Secondary Electrons, the Backscattered
Electrons and X-rays.

3.5. Using a Vacuum:

 When a SEM is used, the column must always be at a vacuum.
 There are many reasons for this. If the sample is in a gas filled
environment, an electron beam cannot be generated or maintained
because of a high instability in the beam.

 Gases could react with the electron source, causing it to burn out,
or cause electrons in the beam to ionize, which produces random
discharges and leads to instability in the beam.

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  The transmission of the beam through the electron optic column
would also be hindered by the presence of other molecules.

 Those other molecules, which could come from the sample or the
microscope itself, could form compounds and condense on the
sample.

 This would lower the contrast and obscure detail in the image.

 A vacuum environment is also necessary in part of the sample

preparation. One such example is the sputter coater.

 If the chamber isn't at vacuum before the sample is coated, gas

molecules would get in the way of the argon and gold. This could
lead to uneven coating, or no coating at all.

3.6. Specimen Chamber:

 The photo on the left shows the sample chamber located at the
base of the column. The second photo shows the lens and
detectors located inside the sample chamber.

3.7. Objective Lens:

 The lens that focuses the beam of electrons towards the sample is
in the center of the picture.
 The parts off to the right of the sample are different detectors. One
is for detecting the secondary electrons and the other is for

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 detecting the backscattered electrons. The operator has the power
to choose and switch detectors for use on each sample.
 Using the secondary electron detector produces a clear and
focused topographical image of the sample.

 The backscatter electron detector produces an image that is useful

when determining the make-up of the sample.
 Each element in the sample appears as a different shade, from
almost white to black.
3.8. Stage:

 A prepared sample is mounted on a specimen stub and placed on

the stage.

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4. Fundamental Principles of Scanning Electron
Microscopy (SEM):
 Accelerated electrons in an SEM carry significant amounts
of kinetic energy, and this energy is dissipated as a variety
of signals produced by electron-sample interactions when
the incident electrons are decelerated in the solid sample.
 These signals include secondary electrons (that produce SEM
images), backscattered electrons (BSE), diffracted
backscattered electrons (EBSD that are used to determine
crystal structures and orientations of minerals), photons
(characteristic X-rays that are used for elemental analysis and
continuum X-rays), visible light (cathodoluminescence-CL), and
heat.

 Secondary electrons and backscattered electrons are

commonly used for imaging samples:

 Secondary electrons are most valuable for showing morphology

and topography on samples and backscattered electrons are
most valuable for illustrating contrasts in composition in
multiphase samples (i.e. for rapid phase discrimination).

 X-ray generation is produced by inelastic collisions of the

incident electrons with electrons in discrete orbital’s (shells) of
atoms in the sample.

 As the excited electrons return to lower energy states, they yield

X-rays that are of a fixed wavelength (that is related to the
difference in energy levels of electrons in different shells for a
given element).

 Thus, characteristic X-rays are produced for each element in a

mineral that is "excited" by the electron beam.

 SEM analysis is considered to be "non-destructive"; that is, x-

rays generated by electron interactions do not lead to volume
loss of the sample, so it is possible to analyze the same
materials repeatedly.

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5. Principle of Operation:
 A finely focused electron beam scanned across the surface of the
sample generates secondary electrons, backscattered electrons,
and characteristic X-rays.
 These signals are collected by detectors to form images of the
sample displayed on a cathode ray tube screen.

 Features seen in the SEM image may then be immediately

analyzed for elemental composition using EDS or WDS.

5.1 Secondary Electron Imaging:

 Shows the topography of surface features a few nm across.
 Films and stains as thin as 20 nm produce adequate-contrast
images. Materials are viewed at useful magnifications up to
100,000 XS without the need for extensive sample preparation and
without damaging the sample.

 Even higher magnifications and resolution are routinely obtained

by our Field Emission SEM.

5.2 Backscattered Electron Imaging:

 Shows the spatial distribution of elements or compounds within
the top micron of the sample.
 Features as small as 10 nm are resolved and composition
variations of as little as 0.2% determined.

5.3 Data Output:

 Data output is generated in real time on the CRT monitor. Images
and spectra can be printed here, recorded on CD ROM and/or
emailed for insertion into your own reports.

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 5.4 Breakdown of an Electron Microscope

 In simplest terms, an SEM is really nothing more than a television.

We use a filament to get electrons, magnets to move them around,
and a detector acts like a camera to produce an image.

5.5 Electron vs. Optical Lenses:

 e-’s don’t actually touch the lens

No definite interface.
 e-’s rotate in the magnetic field.
 e-’s repel each other.
 f∞H∞I
- Focus and magnification controlled
Electronically.
- No physical movements
 e- lenses can only be positive elements
(Converging).
 Can’t correct e- lens aberrations like you can
With compound optical lenses.
 e- Lenses always operate at small apertures

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6. Electron source SEM:
 In standard electron microscopes electrons are mostly generated
by heating a tungsten filament by means of a current to a
temperature of about 2800°C (electron gun).
 Sometimes electrons are produced by a crystal of lanthanum
hexaboride (LaB6) that is mounted on a tungsten filament.
 This modification results in a higher electron density in the beam
and a better resolution than with the conventional device. In a field
emission (FE) scanning electron microscope no heating but a so-
called "cold" source is employed.

 An extremely thin and sharp tungsten needle (tip diameter 10 -7 -

10-8 m) functions as a cathode in front of a primary and secondary
anode.
 The electrons are accelerated in the direction of the column by a
voltage gradient (see example left for a traditional SEM).
 The voltage between cathode and anode is in the order of
magnitude of 0.5 to 30 KV. Because the electron beam produced
by the FE source is about 1000 times smaller than in a standard
microscope, the image quality is markedly better.
 As field emission necessitates an extreme vacuum (10 -8 Torr) in
the column of the microscope, a device is present that regularly
decontaminates the electron source by a current flash.

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  In contrast to a conventional tungsten filament, a FE tip last
theoretically for a lifetime, provided the vacuum is maintained
stable.

7. Summary of Electron Microscope Components:

 Electron optical column consists of:
– Electron source to produce electrons
– Magnetic lenses to de-magnify the beam
– Magnetic coils to control and modify the beam
– Apertures to define the beam, prevent electron spray,etc.
 Vacuum systems consists of:
-chamber which “holds” vacuum, pumps to produce vacuum
-valves to control vacuum, gauges to monitor vacuum
 Signal Detection & Display consists of:
-detectors which collect the signal
– Electronics which produce an image from the signal

8. Infrastructure Requirements:
 Power Supply
 Vacuum System
 Cooling system
 Vibration-free floor
 Room free of ambient magnetic and electric fields
 SEMs always have at least one detector (usually a secondary
electron detector), and most have additional detectors.
 The specific capabilities of a particular instrument are critically
dependent on which detectors it accommodates.

9. Strengths and Limitations of Scanning Electron

Microscopy (SEM):
9.1. Strengths:
 There is arguably no other instrument with the breadth of
applications in the study of solid materials that compares
with the SEM.
 The SEM is critical in all fields that require characterization
of solid materials.
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 While this contribution is most concerned with geological
applications, it is important to note that these applications
are a very small subset of the scientific and industrial
applications that exist for this instrumentation.
 Most SEM's are comparatively easy to operate, with user-
friendly "intuitive" interfaces.
 Many applications require minimal sample preparation.
For many applications, data acquisition is rapid (less than
5 minutes/image for SEI, BSE, spot EDS analyses.)
Modern SEMs generate data in digital formats, which are
highly portable.

9.2. Limitations:
 Samples must be solid and they must fit into the microscope
chamber.
 Maximum size in horizontal dimensions is usually on the order of
10 cm; vertical dimensions are generally much more limited and
rarely exceed 40 mm.
 For most instruments samples must be stable in a vacuum on the
order of 10-5 - 10-6 torr.
 Samples likely to outgas at low pressures (rocks saturated with
hydrocarbons, "wet" samples such as coal, organic materials or
swelling clays, and samples likely to decrepitate at low pressure)
are unsuitable for examination in conventional SEM's.
 However, "low vacuum" and "environmental" SEMs also exist, and
many of these types of samples can be successfully examined in
these specialized instruments.
 EDS detectors on SEM's cannot detect very light elements (H, He,
and Li), and many instruments cannot detect elements with atomic
numbers less than 11 (Na).
 Most SEMs use a solid state x-ray detector (EDS), and while these
detectors are very fast and easy to utilize, they have relatively poor
energy resolution and sensitivity to elements present in low
abundances when compared to wavelength dispersive x-ray
detectors (WDS) on most electron probe microanalyzers (EPMA).
 An electrically conductive coating must be applied to electrically
insulating samples for study in conventional SEM's, unless the
instrument is capable of operation in a low vacuum mode.
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10. Applications include:
10.1 Materials evaluation:
 Grain size
 Surface roughness
 Porosity
 Particle size distributions
 Material homogeneity
 Intermetallic distribution and diffusion

10.2 Failure analysis:

 Contamination locate
 Mechanical damage assessment
 Electrostatic discharge effects
 Micro-crack location

10.3 Quality Control screening:

 "Good" to "bad" sample comparison
 Film and coating thickness determination
 Dimension verification
 Gate width measurement
 Mil Std. screening
10.4 other Applications
 Microscopic feature measurement
 Fracture characterization
 Microstructure studies
 Thin coating evaluations
 Surface contamination examination
 IC failure analysis

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