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Lecture 3.3 - Introduction To The Synthesis of Nanomaterials - SEM and TEM

This document provides an overview of electron microscopy techniques for characterizing nanomaterials, specifically scanning electron microscopy (SEM) and transmission electron microscopy (TEM). It discusses the components, working principles, and applications of SEM and TEM, including their advantages over optical microscopy in terms of higher magnification, greater depth of field, and higher resolution. Key points covered include electron sources, electromagnetic lenses, electron-sample interactions, detectors, vacuum requirements, and examples of SEM and TEM images.

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Gian Banares
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170 views30 pages

Lecture 3.3 - Introduction To The Synthesis of Nanomaterials - SEM and TEM

This document provides an overview of electron microscopy techniques for characterizing nanomaterials, specifically scanning electron microscopy (SEM) and transmission electron microscopy (TEM). It discusses the components, working principles, and applications of SEM and TEM, including their advantages over optical microscopy in terms of higher magnification, greater depth of field, and higher resolution. Key points covered include electron sources, electromagnetic lenses, electron-sample interactions, detectors, vacuum requirements, and examples of SEM and TEM images.

Uploaded by

Gian Banares
Copyright
© © All Rights Reserved
We take content rights seriously. If you suspect this is your content, claim it here.
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Download as PDF, TXT or read online on Scribd
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ChE ELNT: Nanotechnology

Lecture 3.2
Characterisation of Nanomaterials:
Introduction to Electron Microscopy
(Scanning Electron Microscopy and
Transmission Electron Microscopy)

Dr. Lorico Lapitan Jr.

Department Of Chemical Engineering, CHE ELNT


University Of Santo Tomas, España, Manila 5CHE A-B-C
Imaging Methods
• Light (Optical) Microscopy SEM micrograph
• Electron Microscopy
• TEM
• SEM
• Scanning Probe Microscopy
• STM
• AFM
Resolution Limit in Optical Microscopy

• Light Microscopes
• 500 X to 1500 X magnification
• Resolution of ~0.2 µm
• Limits reached by early 1930’s

Resolution dependent on:


0.612
• wavelength of illumination () d=
• Numerical Aperture (NA) of lens system NA
Magnification
• Degree of enlargement. Number of times the
length, diametre of an object is multiplied

Li, F., Yao, C., Zheng, Y., & Hou, S. (2018). Facile synthesis of wavy carbon
nanowires via activation-enabled reconstruction and their applications towards
nanoparticles separation and catalysis. RSC Advances, 8(37), 20593-20602.
Resolution
• Ability to reveal closely adjacent structural
details as separate and distinct.

Limit of Resolution
• The main distance between two visible bodies at which
they can be seen as separate and not in contact with
each other

LR = (0.61 x lambda) / NA

(lambda is wavelength and NA = numerical aperture)


Resolution

Resolution
allows us
to see

Objects as
separate

From one
another
What is Depth of Field?
• The distance of the nearest and farthest object
from the detector if it appears sharp and with
enough details.
Understanding Depth of Field

https://photographylife.com/what-is-depth-of-field
Optical Microscopy vs Scanning Electron
Microscopy

25mm
radiolarian
OM SEM
Small depth of field Large depth of field
Low resolution High resolution

http://www.mse.iastate.edu/microscopy/
Electron Microscopes
• Wavelength of the electron dependent on:
• Electron mass (m)
• Electron charge (q)
• Potential difference to accelerate electrons (V)

h
=
2mqV
Comparison of OM,TEM and SEM
Light source Source of
electrons
Condenser
Magnetic
lenses
Specimen
Objective

Specimen
Projector CRT
Eyepiece Cathode
Ray Tube

detector
OM TEM SEM

Principal features of an optical microscope, a transmission electron


microscope and a scanning electron microscope, drawn to emphasize
the similarities of overall design.
What is SEM ?
Column
TV Screens
Sample
Chamber
• The SEM is
designed for
direct studying
of the surfaces
of solid objects

• 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 OM.
Scanning Electron Microscope
1. e- beam strikes sample
and electron penetrate
surface
2. Interactions occur
between electrons and
sample
3. Electrons and photons
emitted from sample
4. Emitted e- or photons
detected
SEM Images
SiO2 spheres Conidia of Aspergillus
SEM Images
A “bug” eye A succulent plant
Advantages of Using SEM over OM
Magnification Depth of Field Resolution
OM 4x – 1000x 15.5mm – 0.19mm ~ 0.2mm
SEM 10x – 3000000x 4mm – 0.4mm 1-10nm

• 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 SEM also produces images of high resolution, which means
that closely features can be examined at a high magnification.

• The combination of higher magnification, larger depth of field,


greater resolution and compositional and crystallographic
information makes the SEM one of the most heavily used
instruments in research areas and industries, especially in
semiconductor industry.
Main Applications
• Topography
The surface features of an object and its texture (hardness,
reflectivity… etc.)
• Morphology
The shape and size of the particles making up the object
(strength, defects in IC and chips...etc.)
• Composition
The elements and compounds that the object is composed of
and the relative amounts of them (melting point, reactivity,
hardness...etc.)
• Crystallographic Information
How the grains are arranged in the object (conductivity,
electrical properties, strength...etc.)
Components of the SEM
Electrons emitted by the
gun are accelerated,
typically by 20 kV.

They pass through


condenser and objective
lenses, and then through
a set of scan coils and
an aperture. A scan is
simultaneously
generated on a computer
monitor.

Electrons emitted by the


specimen are detected,
amplified and the signal
is then used to produce
an image.
1- Electron sources
A number of different kinds of electron source are used in
SEM. The microscopes in EMLab use the following sources:

Tungsten thermionic source


This is simply a very fine Characteristics
tungsten wire, through ➢ Low brightness
which a current is ➢ Energy spread ~ 1-2eV
passed.

Schottky Field Emission Source


This is a crystal Characteristics
to which a very ➢ High brightness
high voltage is ➢ Energy spread < 0.5 eV
applied.
Electron Beam Source

W or LaB6 Filament
Thermionic or Field Emission Gun
2- Electromagnetic lenses
All modern SEMs use electromagnetic lenses. These
consist of a coil of copper wires inside iron pole pieces.
solenoid of wire together with a magnetic pole piece that
creates and concentrates a magnetic field.

A current through the coils creates a


magnetic field, symbolized by red lines in
the diagram on the left. Electrons close
to the centre are less strongly deflected
than those passing through the lens far
from the axis.
3- Interaction of electrons with specimen
When high energy electrons impinge on the specimen, a
number of signals are generated:
● Backscattered electrons
These are high energy electrons which
are scattered out of the specimen, losing
only a small amount of energy.

● Secondary electrons
These originate in the specimen itself,
and have a much lower energy than
the backscattered electrons (typically
< 50 V).

● X-rays
These give information about the
elemental composition of the sample.
Information given by secondary and
backscattered electrons

Secondary electrons originate from within a


few nm from the surface. They are therefore
very sensitive to surface structure, and provide
topographic information.

Backscattered electrons originate from much


deeper within the sample (a few mm below the
surface), and interact much more strongly with the
sample. They therefore provide compositional
information, but give lower resolution images.
Detectors: secondary electrons
The detector for secondary
electrons is the Everhart
Thornley Detector (ETD).
This consists of a scintillator that
emits photons when hit by high-
energy electrons. The emitted
photons are collected by a
lightguide and transported to a
photomultiplier for detection.
A metal grid known as a Faraday
cage surrounds the scintillator,
and is usually held at a positive
potential to attract the secondary
electrons.
Electron Detectors and Sample Stage

Objective
lens
Sample stage
Transmission Electron Microscope
1. e-beam strikes
sample and is
transmitted through
the sample
2. Scattering occurs
3. Un-scattered
electrons pass
through sample and
are detected
Transmission Electron Microscope
TEM Copper Grid Sample Holder
Transmission Electron Microscope

Organic Material Inorganic Material


Why Need a Vacuum?
When a SEM or TEM is used, the electron-optical
column and sample chamber must always be at a
vacuum.

1. If the column is in a gas filled environment, electrons will


be scattered by gas molecules which would lead to
reduction of the beam intensity and stability.

2. Other gas 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.
References
Goldstein, J. (Ed.). (2012). Practical scanning electron
microscopy: electron and ion microprobe analysis. Springer
Science & Business Media.

Flegler, S. L., Heckman Jr, J. W., & Klomparens, K. L.


(1993). Scanning and transmission electron microscopy: an
introduction. Oxford University Press(UK), 1993,, 225.

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