6.

2 Scanning Electron
Microscope (SEM)

 A scanning electron microscope (SEM) is a type of electron

microscope that produces images of a sample by scanning it
with a focused beam of electrons.
The electrons interact with electrons in the sample, producing
various signals that can be detected and that contain
information about the sample's surface topography and
composition.

The electron beam is generally scanned in a raster scan

pattern, and the beam's position is combined with the detected
signal to produce an image.
Specimens can be observed in high vacuum, low vacuum and
an environmental SEM specimens can be observed in wet
condition.
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 The most common mode of detection is by secondary

electrons emitted by atoms excited by the electron beam.
The number of secondary electrons is a function of the angle
between the surface and the beam.

On a flat surface, the plume of secondary electrons is mostly

contained by the sample, but on a tilted surface, the plume is
partially exposed and more electrons are emitted.
By scanning the sample and detecting the secondary
electrons, an image displaying the tilt of the surface is created.

Principles & Capacities of SEM

The types of signals produced by a SEM include:
secondary electrons (SE),
back-scattered electrons (BSE),
characteristic X-rays,
light (cathodoluminescence) (CL),
specimen current and
transmitted electrons.

Secondary electrons (SE)

Secondary electron detectors are standard equipment in all
SEMs, but it is rare that a single machine would have detectors
for all possible signals.
The signals result from interactions of the electron beam with
atoms at or near the surface of the sample.

In the most common or standard detection mode, secondary

electron imaging (SEI), the SEM can produce very highresolution images of a sample surface, revealing details less
than 1 nm in size.
Due to the very narrow electron beam, SEM micrographs have
a large depth of field yielding a characteristic three-dimensional
appearance useful for understanding the surface structure of a
sample.
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Back-scattered electrons (BSE)

Back-scattered electrons (BSE) are beam electrons that are
reflected from the sample by elastic scattering.
BSE are often used in analytical SEM along with the spectra
made from the characteristic X-rays, because the intensity of
the BSE signal is strongly related to the atomic number (Z) of
the specimen.
BSE images can provide information about the distribution of
different elements in the sample.

Characteristic X-rays
Characteristic X-rays are emitted when the electron beam
removes an inner shell electron from the sample, causing a
higher-energy electron to fill the shell and release energy.
These characteristic X-rays are used to identify the
composition and measure the abundance of elements in the
sample.

Sample Preparation
All samples must be in an appropriate size to fit in the
specimen chamber and are generally mounted rigidly on a
specimen holder called a specimen stub.
For conventional imaging in the SEM, specimens must be
electrically conductive, at least at the surface, and electrically
grounded to prevent the accumulation of electrostatic charge
at the surface.
Metal objects require little special preparation for SEM except
for cleaning and mounting on a specimen stub.

 Nonconductive specimens tend to charge when scanned by

the electron beam, and especially in secondary electron
imaging mode, this causes scanning faults and other image
artifacts.
They are therefore usually coated with an ultrathin coating of
electrically conducting material, deposited on the sample
either by low-vacuum sputter coating or by high-vacuum
evaporation.
Conductive materials in current use for specimen coating
include gold, gold/palladium alloy, platinum, osmium, iridium,
tungsten, chromium, and graphite.

A spider coated in gold, having been

prepared for viewing with an SEM.

Low-voltage micrograph (300 V) of

distribution of adhesive droplets on Post-It
note.
No conductive coating was applied: such a
coating would alter this fragile specimen.

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Schematic Diagram of an SEM

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 In a typical SEM, an electron beam is thermionically emitted from an

electron gun fitted with a tungsten filament cathode.

Normally used in thermionic electron guns

Has the highest melting point and lowest vapour pressure of all metals.
Can be heated for electron emission.
Low cost.

The electron beam, which typically has an energy ranging from 0.2
keV to 40 keV, is focused by one or two condenser lenses to a spot
about 0.4 nm to 5 nm in diameter.
The beam passes through pairs of scanning coils or pairs of deflector
plates in the electron column, typically in the final lens, which deflect
the beam in the x and y axes so that it scans in a raster fashion over
a rectangular area of the sample surface.
When the primary electron beam interacts with the sample, the
electrons lose energy by repeated random scattering and absorption
within of the specimen (interaction volume).
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SEM Images

SEM image of normal circulating human

blood. This is an older and noisy micrograph
of a common subject for SEM micrographs:
red blood cells.

SEM image of a photoresist layer used in

semiconductor manufacturing taken on a field
emission SEM. These SEMs are important in the
semiconductor industry for their high-resolution
capabilities.

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6.3 Infrared Spectroscopy

Infrared spectroscopy (IR spectroscopy) is the spectroscopy
that deals with the infrared region of the electromagnetic
spectrum, that is light with a longer wavelength and lower
frequency than visible light.

It covers a range of techniques, mostly based on absorption

spectroscopy.
As with all spectroscopic techniques, it can be used to identify
and study chemicals. A common laboratory instrument that
uses this technique is a Fourier transform infrared (FTIR)
spectrometer.

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6.3.1 FTIR (Fourier Transform Infrared

Spectroscopy)
Fourier transform infrared spectroscopy (FTIR) is a
technique which is used to obtain an infrared spectrum of
absorption, emission, photoconductivity or Raman scattering
of a solid, liquid or gas.
An FTIR spectrometer simultaneously collects spectral data in
a wide spectral range.
The term Fourier transform infrared spectroscopy originates
from the fact that a Fourier transform (a mathematical
process) is required to convert the raw data into the actual
spectrum.

The Components of FTIR Spectrometers

A common FTIR spectrometer consists of a source,
interferometer, sample compartment, detector, amplifier, A/D
convertor, and a computer.
The source generates radiation which passes the sample
through the interferometer and reaches the detector.

Then the signal is amplified and converted to digital signal by

the amplifier and analog-to-digital converter, respectively.
Eventually, the signal is transferred to a computer in which
Fourier transform is carried out.
Figure below is a block diagram of an FTIR spectrometer.
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Block diagram of an FTIR spectrometer

 The goal of any absorption spectroscopy is to measure how well a

sample absorbs light at each wavelength.
The most straightforward way to do this, is to shine a monochromatic
light beam at a sample, measure how much of the light is absorbed,
and repeat for each different wavelength.
FTIR technique shines a beam containing many frequencies of light
at once, and measures how much of that beam is absorbed by the
sample.
The beam described above is generated by starting with a broadband
light source one containing the full spectrum of wavelengths to be
measured.

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 The light shines into a Michelson interferometera certain

configuration of mirrors, one of which is moved by a motor.
As this mirror moves, each wavelength of light in the beam is
periodically blocked, transmitted, blocked, transmitted, by the
interferometer, due to wave interference.

Different wavelengths are modulated at different rates, so that at

each moment, the beam coming out of the interferometer has a
different spectrum.

Schematic of the Michelson interferometer

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 Computer processing is required to turn the raw data (light absorption

for each mirror position) into the result of light absorption for each
wavelength.
The processing required a common algorithm called the Fourier
transform. The raw data is sometimes called an "interferogram".

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 In FTIR Analysis, is a failure analysis technique that provides

information about the chemical bonding or molecular structure
of materials, whether organic or inorganic.

It is used in failure analysis to identify unknown materials

present in a specimen, and is usually conducted to
complement Energy Dispersive X-Ray (EDX) analysis.

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 Unlike SEM inspection or EDX analysis, FTIR spectroscopy

does not require a vacuum, since neither oxygen nor nitrogen
absorb infrared rays.
FTIR analysis can be applied to minute quantities of
materials, whether solid, liquid , or gaseous.

When the library of FTIR spectral patterns does not provide

an acceptable match, individual peaks in the FTIR plot may
be used to yield partial information about the specimen.

22

A scan of an FTIR Spectrum Plot

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