ACCE-5202: Nanoscience and Nanotechnology

Introduction to Nanotechnology

Dr. Sumaya Farhana Kabir

Associate Professor
Dept. of ACCE
University of Dhaka
 What is Microscopy
• Microscopy is any technique for producing visible images of structures or details too small to otherwise be seen by the
human eye.
What is microscope magnification and resolution?
Magnification is the ability to make small objects seem larger, such as making a microscopic organism visible. Resolution
is the ability to distinguish two objects from each other. Light microscopy has limits to both its resolution and its
magnification
Microscopic Techniques
Resolution/Resolving power

Angular Aperture
Optical Microscope
 Electron Microscopes
Electron Microscopes are scientific instruments that use a beam of highly energetic electrons to examine objects on
a very fine scale.
The high resolution of EM images results from the use of electrons (which have very short wavelengths) as the
source of illuminating radiation.
Electron Microscopes can yield information about the topography (surface features of an object), morphology
(shape and size of the particles making up the object), composition (the elements and compounds that the
object is composed of and the relative amounts of them) and crystallographic information (how the atoms are
arranged in the object).
Electron Microscopes were developed due to the limitations of Light Microscopes which are limited to 500x or
1000x magnification and a resolution of 0.2 micrometers whereas electron microscope has magnification of
1000000x and a resolution of 0.2 nm.
Electron Microscopes (EMs) function exactly as their optical counterparts except that they use a focused beam of
electrons instead of light to "image" the specimen and gain information as to its structure and composition. The
basic steps involved in all Ems are the following: A stream of electrons is formed in high vacuum (by electron
guns).
The Transmission Electron Microscope (TEM) was the first type of Electron Microscope to be developed and is
patterned exactly on the Light Transmission Microscope except that a focused beam of electrons is used instead
of light to "see through" the specimen. It was developed by Max Knoll and Ernst Ruska in Germany in 1931
 Properties of Electrons
1.Electrons are used as a source of illumination.
2.They are negatively charged subatomic particles.
3.When atoms of metal (tungsten) are excited by energy (current of high
voltage; 20KV,/20000V; in household 220V), the electron velocity is
increased to a rate at which electrons leave the orbit, enter the space,
and are lost to the atom.
4.Electrons emitted from electron guns are passed through an aperture
to form a well-defined beam.
5.Electrons interact with the atoms of the specimen to form the image.
6.The transmitted electrons form the image while the rest of the
electrons get scattered.
 Transmission electron Microscopy
TEM is a microscopic technique whereby a beam of electrons is transmitted through an ultra thin specimen (<200 nm)
and interacts as passes through the sample. An image is formed from the electrons transmitted through the
specimen, magnified and focused by an objective lens and appears on an imaging screen.

Optical microscopes use simple glass lens, whereas electron

microscopes use an electrostatic or electromagnetic lens,
because electron can’t pass through glass.
Optical microscopes have a maximum magnification power of
1,000, compared to the better resolving power of the electron
microscope that can reach 1,000,000 times.

Electromagnetic Lens:
They simply consist of coils of wires inside metal pole
pieces. When electricity passes through a wire rolled into a
tight coil, the center is filled with a strong force called
magnetism. This force pushes inwards on the electron beam.
This device is called a magnetic lens because it bends the beam
of electrons the same way that a glass lens bends a beam of
light
Electrons can be focus or deflected by use of the magnetic Lorentz force.

The Lorentz force (or electromagnetic force) is the combination of electric and magnetic force on a point charge due
to electromagnetic fields. A particle of charge q moving with a velocity v in an electric field E and a magnetic field B
experiences a force of
TEM instrumentation
TEM requires a vacuum inside the microscope column.
An electron source: The source of electrons is the electron gun and is located at
the top of the microscope body. It consists of a hot tungsten filament cathode as
the electron source forming the beam.
Electromagnetic lenses/coils : The Electromagnetic lens/ coils correspond to the
Electricity runs through a wire rolled into a tight coil, the center is filled with a
strong force called magnetism. This force focus or deflect moving charged
particles, such as electrons or ions, by use of the magnetic Lorentz force.
Condenser lens: To focus electron
Objective lens: The main magnifying lens
Projector lens: The final lens in a TEM. Used to assist in magnifying the image and
to project the magnified image onto the phosphorus screen

Phosphorescent screen-The screen at the bottom of the electron column,

where the specimen is viewed. The screen is coated with a phosphor
material such as zinc sulfide.
Computer-A high-resolution phosphor is coupled by means of a lens optical system
to the sensor of a digital camera. The image detected by the digital camera is
displayed on a monitor of the computer.
The magnification is determined mainly by the value of the current (for magnetic lenses) through the intermediate
and projector lens coils. The image is focused by changing the current through the objective lens coil. Another
difference is that the optical microscope is usually operated so that the image is a virtual one, while in the electron
microscope the final image is invariably real and is visualized on a fluorescent screen or recorded for study on a
photographic plate in traditional instruments or—more usually in today’s laboratory—on a digital imaging system.
Electron lenses are the magnetic equivalent of the glass lenses in an optical microscope and to a large
extent, we can draw comparisons between the two.
A strong magnetic field is generated by passing a current through a set of windings. This field acts as a
convex lens, bringing off axis rays back to focus. The image is rotated, to a degree that depends on the
strength of the lens. Focal length can be altered by changing the strength
Objective lens
Most important lens in the microscope since it generates the first intermediate
image, the quality of which determines the resolution of the final image. The
objective lens forms an inverted initial image, which is subsequently magnified.

Intermediate lens
The first intermediate lens magnifies the initial image that
is formed by the objective lens:
Projector lens

Magnification in the electron microscope can be varied from hundreds to several hundred thousands of times.
This is done by varying the strength of the projector and intermediate lens.
Working Principle of TEM
❑ The specimen is bombarded by a beam of electrons, the primary electrons.

❑ The electrons in the form of a beam pass through a condenser coil and fall on the
object.

❑ They get scattered and transmitted through the object and pass through the
objective coil which magnifies the image of the object.

❑ In order to have maximum magnification, an intermediate coil is fitted between

the objective and the projector coils. If the magnification of the objective is 100
and the projector coil is 200, the total magnification becomes 20,000. This can be
increased up to 1,60,000 by fitting the intermediate coil.

❑ The projector coil further magnifies the image and projects it on the fluorescent
screen.

❑ Electrons which reach the fluorescent screen form the bright spots while the
areas where electrons do not reach the fluorescent screen form the dark spots.

❑ The varying degree of the intensity of electrons forms the image with varying
degrees of grey. The lighter areas of the image represent the places where a
greater number of electrons were able to pass (transmitted) through the sample
and the darker areas reflect the dense areas of the object.
How does the final image in a transmission electron microscope become visualized?

The fluorescent screen is coated with phosphor chemical like Zinc

sulfide, which appears as bright spot when electrons come into
contact. The intensity of the bright spot depends on how much
energy the electrons have when they hit the fluorescent screen.
The camera under the fluorescent screen capture the image
made from bright spot which is displayed on a computer screen.
Electron Scattering for TEM
All electrons released by the tungsten
filament hits a fluorescent screen or
photographic print which generates an
image that looks like one from an xray.
 Scanning electron microscopy
A scanning electron microscope is a type of electron microscope that
produces images of a sample by scanning the surface with a focused
beam of electrons. The electrons interact with atoms in the sample,
producing various signals that contain information about the surface
topography and composition of the sample. The entire electron column
needs to be under vacuum.
In scanning electron microscopy, the electron beam scans the sample
in a raster pattern.
First, electrons are generated at the top of the column by
the electron source.
They are then accelerated and attracted by the positively-
charged anode.

Electromagnetic lenses
Condenser lens: This is the first lens that electrons meet as they travel towards the sample. This lens converges the
beam. The condenser lens defines the size of the electron beam (which defines the resolution).
Scanning coils: Scanning coils are used to raster the beam onto the sample.
Objective lens:
The beam is converged once again by the objective lens before hitting the sample, while the main role of the objective
lens is to focus the beam onto the sample.
 Electron Scattering for SEM
When an electron beam strikes a sample a large number of signals are generated. One possible signal could be
from electrons. There are two types of electrons used to produce an image in a SEM, namely, secondary and
backscattered electrons.
Backscattered Electrons
When the electron beam strikes the sample some of the electrons will interact with the nucleus of the atom in much the
same way a space craft will interact with the gravity of a planet. The negatively-charged electron will be attracted to the
positive nucleus but if the angle is just right instead of being captured by the “gravitational pull” of the nucleus it will
circle the nucleus and come back out of the sample without slowing down. These electrons are called backscattered
electrons because they come back out of the sample. The electrons are moving so fast, so they travel in straight lines.
In order to form an image with BSE (backscattered electrons), a detector is placed in their path. When they hit the
detector a signal is produced which is used to form the TV image. All the elements have different sized nuclei. As the size
of the atom nucleus increases, the number of BSE increases.
 Secondary Electron (SE)
The bombarding electrons (=primary electrons) can penetrate in the electron shells of the atoms composing the
surface of the sample. The energy (negative charge, mass, velocity) of these incident electrons can be converted
to eject local electrons, so-called secondary electrons.

They are a result of inelastic interactions between the primary electron beam and the sample and have lower
energy than the backscattered electrons. Secondary electrons are very useful for the inspection of the
topography of the sample's surface.

Because BSEs come from deeper regions of the sample whereas SEs originate from surface regions, the two
carry different types of information. BSE images show high sensitivity to differences in atomic number; the
higher the atomic number, the brighter the material appears in the image. SE imaging can provide more
detailed surface information.

How electrons are detected

BSEs and SEs are detected by different types of detectors. For the detection of BSEs, solid state detectors are
placed above the sample, concentrically to the electron beam, to maximize BSE collection.
01. At the surface of the sample, electrons in the deeper electron shells (shell K in C) can be ejected by primary
electrons (Pe- indicated in red), resulting in an electron hole (D).
02. When this lower-shell (e.g; K shell) position is filled by an electron from a higher shell (e.g; L shell) energy is
released.
03. This can be as light (photons; the phenomenon is also called cathode luminescence) or as X-ray. Because each
element emits an own characteristic energy value.
Another phenomenon is that

1. The energy released upon filling a hole in the K shell by an electron from the L shell is used to
expulse an electron from the external M shell: a so-called Auger electron.

2. The released energy is characteristic for the type of atom. Auger electrons are produced in the
outermost surface layer (at nanometer depth) of the sample.
 SEM sample Preparation

1. Cleaning the surface of the specimen

2. Stabilizing the specimen
3. Rinsing the specimen
4. Dehydrating the specimen
5. Mounting the specimen
6. Coating the specimen.

Why are samples coated for SEM?

It is commonly necessary to coat the sample with a thin layer of gold or gold-palladium alloy in order to prevent
charging of the surface, to promote the emission of secondary electrons so that the specimen conducts evenly,
and to provide a homogeneous surface for analysis and imaging.