Faculty of Engineering

Scanning, Transmission electron

microscopes and Differential thermal
analyzer
Scanning electron microscope:
Scanning electron microscope (SEM) is a type of electron
microscope that produces images of a sample by scanning the
surface with a focused beam of electrons

How it works?

The scanning electron microscope (SEM) uses a focused beam of

high-energy electrons to generate a variety of signals at the
surface of solid specimens. The signals that derive from electron-
sample interactions reveal information about the sample including
external morphology (texture), chemical composition, and
crystalline structure and orientation of materials making up the
sample. In most applications, data are collected over a selected
area of the surface of the sample, and a 2-dimensional image is
generated that displays spatial variations in these properties.
Areas ranging from approximately 1 cm to 5 microns in width can
be imaged in a scanning mode using conventional SEM
techniques (magnification ranging from 20X to approximately
30,000X, spatial resolution of 50 to 100 nm). The SEM is also
capable of performing analyses of selected point locations on the
sample; this approach is especially useful in qualitatively or semi-
quantitatively determining chemical compositions (using EDS),
crystalline structure, and crystal orientations (using EBSD). The

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design and function of the SEM is very similar to the EPMA and
considerable overlap in capabilities exists between the two
instruments.

ELECTRON BEAM – SAMPLE INTERACTION

The image formation in a scanning electron microscope is

different from that in a conventional optical microscope. In SEM
a focused mono-energetic electron beam scans the sample surface
producing various “products” from the surface. These are
secondary electrons, backscattered electrons and X-ray photons
(see Fig. 2.). These products are collected by dedicated detectors
and utilizing their signals, an intensity map is constructed on the
screen; this is the microscopic image. Due to this image formation
mechanism in SEM there is no need to have a transparent to the
electrons specimen as in case of a transmission electron
microscope (TEM). The sample thickness is arbitrary within
reasonable limits and quite often sample preparatory measures are
not needed at all. Of course, the sample should be cleaned in
order to remove the surface contamination, dust and grease if they
are. In case of microstructural or micromechanical analysis the
sample can need more sophisticated cleaning and polishing. The
proper preparation method is extremely important because the
true microstructure of the sample may be obscured or altered by
the use of poor technique.

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As the energies of emerging products are different, they provide
information from different depths. The secondary electrons (SE)
are specimen electrons, knocked out of the surface by inelastic
collisions with the incoming beam electrons and their majority are
emitted with energies of a few electron volts (3-5 eV) providing
only near-surface information. In this case, the resolution is
determined by the diameter of the focused electron beam. The
ultimate resolution in case of secondary electrons is ~1 nm.

Fig. 2. The products due to the electron-material interaction

The backscattered electrons (BSE) are beam electrons

experiencing large angle (or multiple) elastic scattering. The order
of magnitude of their energy is some tens of kilo electron volts
(10-30 keV). Owing to their energy range they provide

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information from deeper layers. Accordingly, in this case the
resolution is poorer, ~2-4 nm.

The energy of X-ray photons is characteristic of the atoms they

originate from, thus measuring their energy allows for local
elemental analysis. The analysis can be point- or surface analysis
(elemental mapping).

THE SET-UP OF A SCANNING ELECTRON MICROSCOPE

The main parts of the scanning electron microscope are as

follows: electron source, focusing- and scanning magnets,
detectors and sample stage. The diagram of the set-up can be seen
in Fig. 3. The source of electrons in an electron microscope is the
electron gun. In the gun the electrons are emitted from the
cathode either due to heating (thermionic source) or due to
expelling electric field (field emission gun = FEG).

In the Quanta 3D FEG microscope the electron source is a field

emission gun which is heated as well, called Schottky source. The
material of the filament is tungsten covered by zirconium oxide

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(ZrO2) in order to lower the work function of the cathode
material.

The electrons emitted from the cathode are accelerated by an

electric field up to the required energy. The maximum electron
energy in scanning electron microscopes is usually 30 keV which
can be adjusted towards the smallest energies.

After acceleration the electrons are focused and scanned by

magnetic lenses. The electron lenses work on the basis of the
Lorentz force. The focal length of magnetic lenses and the size of
the beam spot can be changed by changing the current flowing
through the coils. The minimum diameter of the beam spot is ~1
nm.

The beam scans the sample surface point by point and row by
row. The detectors positioned above the sample surface collect
the generated by the beam secondary electrons (SE),
backscattered electrons (BSE) and the X-ray photons. The
simplest scanning electron microscopes have only SE detector,
but the SEM installed at ELTE has all of these three ones.

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IMAGE FORMATION IN SEM

Sample preparation
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SEM samples have to be small enough to fit on the specimen
stage, and may need special preparation to increase their electrical
conductivity and to stabilize them, so that they can withstand the
high vacuum conditions and the high energy beam of electrons.
Samples are generally mounted rigidly on a specimen holder or
stub using a conductive adhesive. SEM is used extensively for
defect analysis of semiconductor wafers, and manufacturers make
instruments that can examine any part of a 300 mm
semiconductor wafer. Many instruments have chambers that can
tilt an object of that size to 45° and provide continuous 360°
rotation.

Nonconductive specimens collect charge when scanned by the

electron beam, and especially in secondary electron imaging
mode, this causes scanning faults and other image artifacts. 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. Metal objects
require little special preparation for SEM except for cleaning and
conductively mounting to a specimen stub. Non-conducting
materials are usually coated with an ultrathin coating of

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electrically conducting material, deposited on the sample either
by low-vacuum sputter coating or by high-vacuum evaporation.

Transmission electron microscope

Transmission electron microscopes (TEM) are microscopes

that use a particle beam of electrons to visualize specimens
and generate a highly-magnified image. TEMs can magnify
objects up to 2 million times. In order to get a better idea of
just how small that is, think of how small a cell is. It is no
wonder TEMs have become so valuable within the
biological and medical fields.

How does it work?

TEMs employ a high voltage electron beam in order to

create an image. An electron gun at the top of a TEM emits
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electrons that travel through the microscope’s vacuum
tube. Rather than having a glass lens focusing the light (as
in the case of light microscopes), the TEM employs an

electromagnetic lens which focuses the electrons into a

very fine beam. This beam then passes through the
specimen, which is very thin, and the electrons either
scatter or hit a fluorescent screen at the bottom of the
microscope. An image of the specimen with its assorted
parts shown in different shades according to its density
appears on the screen. This image can be then studied
directly within the TEM or photographed. Figure 1 shows
a diagram of a TEM and its basic parts.
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TEM is complex and sophisticated but the basic principle
behind its operation can be readily understood.

A heated tungsten filament in the electron gun generates a

beam of electrons that is then focused on the specimen by
the condenser.

Since electrons cannot pass through a glass lens ,magnetic

lenses are used to focus the beam.

The column containing the lenses and specimen must be

under high vacuum to obtain a clear image because
electrons are deflected by collisions with air molecules.

The specimen scatters electron passing through it, and the

beam is focused by magnetic lenses to form an enlarged ,
visible image of the specimen on a fluorescent screen.

A denser region in the specimen scatters more electron and

therefore appears darker in the image.

In contrast, electron-transparent regions are brighter.

The screen can also be moved aside and the image captured
on photographic film as a permanent record.

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What Are the Differences Between a TEM and a Light
Microscope?

Although TEMs and light microscopes operate on the same

basic principles, there are several differences between the
two. The main difference is that TEMs use electrons rather
than light in order to magnify images. The power of the
light microscope is limited by the wavelength of light and
can magnify something up to 2,000 times. Electron
microscopes, on the other hand, can produce much more
highly magnified images because the beam of electrons has
a smaller wavelength which creates images of higher
resolution. (Resolution is the degree of sharpness of an
image.) Figure 2 compares the magnification of a light
microscope to that of a TEM.

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Fig. 2 [left] Cotton stem; area in the circle is the phloem tissue. Light microscope x250. Photo by K. Esau.
[right] Enlarged image of cotton phloem tissue showing a sieve element (top cell) and a companion cell
(bottom cell), TEM x8,000. Photo by J. Thorsch.

How Are TEM Specimens Prepared?

Specimens must be very thin so that electrons are able to

pass through the tissue. This may be done by cutting very
thin slices of a specimen’s tissue using an ultramicrotome.
The tissue must first be put in a chemical solution to
preserve the cell structure. The tissue must also be
completely dehydrated (all water removed).

Once preserved and dehydrated, tissue samples are placed

in hard, clean plastic. The plastic supports the tissue while
it is being thinly cut with the ultramicrotome

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After sections are cut and mounted on grids, (tiny circular
disks with openings,) a solution of lead is used to stain the
tissue. The lead provides contrast to the tissue by staining
certain cell parts. When placed in the electron microscope,
the electrons are scattered by the lead. They do not
penetrate the tissue or hit the fluorescent screen, leaving
those areas dark.

Advantages of TEM

TEMs offer very powerful magnification and resolution.

TEMs have a wide range of applications and can be

utilized in a variety of different scientific , educational and
industrial fields.
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TEMs provide information on element and compound
structure, Images are high qualified and detailed.

Disadvantages of TEM

TEMs are large and very expensive.

Laborious sample preparation.

Operation and analysis require special training.

Samples are limited to those that are electron transparent.

Images are black and white.

Differential thermal analysis

A technique in which the difference in temperature
between the sample and a reference material is monitored
against time or temperature while the temperature of the
sample, in a specified atmosphere, is programmed.

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Figure 1 shows the block diagram of DTA.

The sample and the reference are placed symmetrically in

the furnace. The furnace is controlled under a temperature
program and the temperature of the sample and the
reference are changed. During this process, a differential
thermocouple is set up to detect the temperature difference
between the sample and the reference.

Also, the sample temperature is detected from the

thermocouple on the sample side

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 Graph (a) shows the temperature change of the furnace,
the reference and the sample against time.

Graph (b) shows the change in temperature difference (ΔT)

against time detected with the differential thermocouple.

ΔT signal is referred to as the DTA signal.

Matters that do not change in the measurement temperature

range (usually α-alumina) are used as reference.

When the furnace heating begins, the reference and the

sample begin heating with a slight delay depending on their
respective heat capacity, and eventually heat up in
according to the furnace temperature.

ΔT changes until a static state is reached after the heating

begins, and after achieving stability, reaches a set amount
compliant with the difference in heat capacity between the
sample and the reference. The signal at the static state is
known as the baseline.

When the temperature rises and melting occurs in the

sample, for example, the temperature rise stops as shown in

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graph (a) and the ΔT increases. When the melting ends, the
temperature curve rapidly reverts to the baseline.

At this point, the ΔT signal reaches the peak, as shown in

graph (b).

From this, we can detect the samples transition temperature

and the reaction temperature from the ΔT signal (DTA
signal).

In graph (b), the temperature difference due to the samples

endothermic change is shown as a negative direction and
the temperature difference due to the samples exothermic
change is shown as a positive direction.

Applications
A DTA curve can be used only as a finger print for
identification purposes but usually the applications of this
method are the determination of phase diagrams, heat
change measurements and decomposition in various
atmospheres

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DTA is widely used in the pharmaceutical and food
industries.

DTA may be used in cement chemistry, mineralogical

research and in environmental studies.

DTA curves may also be used to date bone remains or to

study archaeological materials. Using DTA one can obtain
liquidus & solidus lines of phase diagrams.

Resources 
https://serc.carleton.edu

https://www.technoorg.hu

http://www.biosciencenotes.com

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https://www.ccber.ucsb.edu

https://www.hitachi-hightech.com

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