Additive Manufacturing

Naveen A Kalal
Department of Mechanical Engineering
 Module 4
Nanomaterials
and
Characterization Techniques

Naveen A Kalal
Department of Mechanical Engineering
 Definition
Additive Manufacturing (AM) refers to a process by which
digital 3D design data is used to build up a component in
layers by depositing material.

“Nanotechnology is the understanding and control of matter at

dimensions of roughly 1 to 100 nanometers, where unique
phenomena enable novel applications.”

(from the National Nanotechnology Initiative, 2007)

 Module 4
NANO MATERIALS & CHARACTERIZATION
TECHNIQUES:
• Introduction: Importance of Nano-technology,
Emergence of Nanotechnology, Bottom up and Top-down
approaches, challenges in Nanotechnology
• Nano-materials Synthesis and Processing:
Methods for creating Nanostructures; Processes for
producing ultrafine powders- Mechanical grinding; Wet
Chemical Synthesis of Nano-materials- sol-gel process;
Gas Phase synthesis of Nano-materials-Furnace, Flame
assisted ultrasonic spray pyrolysis; Gas Condensation
Processing (GPC), Chemical Vapour Condensation(CVC).
 Module 4
NANO MATERIALS & CHARACTERIZATION TECHNIQUES:
• Optical Microscopy - Principles, Imaging Modes, Applications,
Limitations.
• Scanning Electron Microscopy (SEM) - Principles, Imaging
Modes, Applications, Limitations.
• Transmission Electron Microscopy (TEM) - Principles, Imaging
Modes, Applications, Limitations.
• X- Ray Diffraction (XRD) - Principles, Imaging Modes,
Applications, Limitations.
• Scanning Probe Microscopy (SPM) - Principles, Imaging Modes,
Applications, Limitations.
• Atomic Force Microscopy (AFM) - basic principles,
instrumentation, operational modes, Applications, Limitations.
• Electron Probe Micro Analyzer (EPMA) - Introduction, Sample
preparation, Working procedure, Applications, Limitations.
 Module 4
NANO MATERIALS & CHARACTERIZATION
TECHNIQUES:
• Introduction: Importance of Nano-technology,
Emergence of Nanotechnology, Bottom up and Top-
down approaches, challenges in Nanotechnology
 Module 4
NANO MATERIALS & CHARACTERIZATION
TECHNIQUES:
• Introduction: Importance of Nano-technology
 Module 4

• The earliest systematic discussion of nanotechnology is

considered to be a speech given by Richard Feynman
(American physicist, 1918-1988) in 1959. It was titled:
"There's Plenty of Room at the Bottom." In this speech
Feynman discussed the importance "of manipulating and
controlling things on a small scale" and how they could "tell us
much of great interest about the strange phenomena that
occur in complex situations." He described how physical
phenomena change their manifestation depending on scale,
and posed two challenges: the creation of a nanoomotor, and
the scaling down of letters to the size that would allow the
whole Encyclopedia Britannica to fit on the head of a pin.
 Module 4
• The term 'nanotechnology' was used first by
the Japanese scientists Norio Taniguchi (1912-
1999) in a 1974 paper on production
technology that creates objects and features
on the order of a nanometer.
What is Nanotechnology?
Module 4
Nanotechnology is the understanding and control of matter at the nanoscale, at
dimensions between approximately 1 and 100 nanometers, where unique
phenomena enable novel applications. Encompassing nanoscale science, engineering,
and technology, nanotechnology involves imaging, measuring, modeling, and
manipulating matter at this length scale. Matter such as gases, liquids, and solids can
exhibit unusual physical, chemical, and biological properties at the nanoscale,
differing in important ways from the properties of bulk materials and single atoms or
molecules. A nanometer is one-billionth of a meter. A sheet of paper is about 100,000
nanometers thick; a single gold atom is about a third of a nanometer in diameter.

(Source: The Laboratory for Multiscale Regenerative Technologies at MIT, 2015)

 Module 4

Damascus steel swords from the Middle East were made between AD300 and AD1700
and are known for their impressive strength, shatter resistance and exceptionally
sharp cutting edge. The steel blades contain oriented nanoscale wire-and-tube-like
structures, which almost certainly enhanced the material's properties.
 Module 4

There are a number of relatively famous examples of ancient artefacts which were
created using nanocomposites. The Lycurgus cup, for example, is a stunning decorative
Roman treasure from about AD400; it is made of a glass that changes colour when light
is shone through it. The glass contains gold-silver alloyed nanoparticles, which are
distributed in such a way to make the glass look green in reflected light but, when light
passes through the cup, it reveals a brilliant red.
Module 4

Medieval stained glass windows are an

example of how nanotechnology was used in
the pre-modern era. (Courtesy: NanoBioNet)
 Module 4
UNDERSTANDING SIZE
How big (small) are we talking about?
Module 4
UNDERSTANDING SIZE
• 1 meter
UNDERSTANDING SIZE
• 10 centimeters
UNDERSTANDING SIZE
• 1 centimeter
UNDERSTANDING SIZE
• 100 micrometers
UNDERSTANDING SIZE
• 10 micrometers
UNDERSTANDING SIZE
• 1 micrometer
UNDERSTANDING SIZE
• 100 nanometers
UNDERSTANDING SIZE
• 10 nanometers
UNDERSTANDING SIZE
• 1 nanometer
 NANOMETER………..(nm)
 A nanometer is one billionth of a meter (10-9
m). This is roughly ten times the size of an
individual atom.
 Module 4
• Emergence of Nano-technology
The emergence of nanotechnology has led to the
design, synthesis, and manipulation of particles in
order to create a new opportunity for the utilization
of smaller and more regular structures for various
applications. In recent years, nanosized metal oxide
particles have gotten much attention in various fields
of application due to its unique optical, electrical,
magnetic, catalytic and biomedical properties
 Module 4

SALIENT FEATURES
 SALIENT FEATURES

• At atomic and molecular scales, in the length scale

of approximately 1 - 100 nanometer range

• Fundamentally new properties and functions

because of their nanoscale structure
 SALIENT FEATURES

• Ability to control , to see, measure, and manipulate

matter on the atomic scale to exploit those
properties and functions

• Ability to integrate those properties and functions

into systems spanning from nano- to macro-scopic
scales
 How does Nanotechnology work?

1.Atoms are the building blocks for all matter in our

universe.

2. Atoms and molecules stick together because they have

complementary shapes that lock together, or charges that
attract. Just like with magnets, a positively charged atom
will stick to a negatively charged atom.
3. Every atom has a exhibits different property at various
conditions

4. The goal of nanotechnology is to manipulate atoms

individually and place them in a pattern to produce a
desired structure.
 APPROACHES..
• Two approaches can be taken when making
something at the nano scale:

 Top-Down approach

 Bottom-Up approach
 TOP DOWN APPROACH
• The top-down approach is analogous to making a
stone statue.

• The process involves wastage.

• Used in fibres

• Seldom used in MNT

 BOTTOM UP APPROACH
• Approach one would take to building a house

• Less wastage, as strong covalent bonds will hold the

constituent parts together.

• Limited in how big the structures can be made

• Approach used currently

The most immediate challenge in nanotechnology is that we need to learn
more about materials and their properties at the nanoscale. Universities
and corporations across the world are rigorously studying how atoms fit
together to form larger structures. We're still learning about how quantum
mechanics impact substances at the nanoscale.
Because elements at the nanoscale behave differently than they do in their
bulk form, there's a concern that some nanoparticles could be toxic. Some
doctors worry that the nanoparticles are so small, that they could easily
cross the blood-brain barrier, a membrane that protects the brain from
harmful chemicals in the bloodstream. If we plan on using nanoparticles to
coat everything from our clothing to our highways, we need to be sure that
they won't poison us.
Despite the rapid developments and escalating publications in this field,
there remain a number of challenges in product development and
commercialization. The key issues are the health, safety and environmental
aspects of some nanomaterials and their regulatory status.
APPLICATIONS
Medical and Healthcare Applications

Electronics and IT Applications

Energy Applications

Environmental Remediation

Future Transportation Benefits

 Module 4
NANO MATERIALS & CHARACTERIZATION
TECHNIQUES:
• Introduction: Importance of Nano-technology,
Emergence of Nanotechnology, Bottom up and Top-down
approaches, challenges in Nanotechnology
• Nano-materials Synthesis and Processing:
Methods for creating Nanostructures; Processes for
producing ultrafine powders- Mechanical grinding; Wet
Chemical Synthesis of Nano-materials- sol-gel process;
Gas Phase synthesis of Nano-materials-Furnace, Flame
assisted ultrasonic spray pyrolysis; Gas Condensation
Processing (GPC), Chemical Vapour Condensation(CVC).
 Nano-materials Synthesis and
Processing
Nanoparticle production / Methods for creating
nanostructrures
• Nanomaterials and/or nanoparticles are used in a
broad spectrum of applications. Today they are
contained in many products and used in various
technologies. Most nanoproducts produced on
an industrial scale are nanoparticles, although
they also arise as byproducts in the manufacture
of other materials. Most applications require a
precisely defined, narrow range of particle sizes
(monodispersity).
• Two basic strategies are used to produce
nanoparticles: 'top-down' and 'bottom-up'.
The term 'top-down' refers here to the
mechanical crushing of source material using a
milling process. In the 'bottom-up' strategy,
structures are built up by chemical processes
(Figure 1). The selection of the respective
process depends on the chemical composition
and the desired features specified for the
nanoparticles.
Figure 1. Methods of nanoparticle production: top-down and bottom-up. (Image: Laboratory for
Micro and Nanotechnology, Paul Scherrer Institut)
• Top-Down/mechanical-physical production
processes
• 'Top-down' refers to mechanical-physical
particle production processes based on
principles of microsystem technology. The
traditional mechanical-physical crushing
methods for producing nanoparticles involve
various milling techniques (Figure 2).
• mechanical-physical crushing methods
• Milling processes
• The mechanical production approach uses milling to
crush microparticles. This approach is applied in
producing metallic and ceramic nanomaterials. For
metallic nanoparticles, for example, traditional
source materials (such as metal oxides) are
pulverized using high-energy ball mills..
• These mills are equipped with grinding media
composed of wolfram carbide or steel.
• Ball mills rotate around a horizontal axis ,partially
filled with the material to be ground plus the
grinding medium.
• Milling processes
• The balls rotate with high energy inside a container and then
fall on the solid with gravity force and kinetic and hence crush
the solid into nano crystallites.
• Milling involves thermal stress and is energy intensive.
Lengthier processing can potentially abrade the grinding
media, contaminating the particles. Purely mechanical milling
can be accompanied by reactive milling: here, a chemical or
chemo-physical reaction accompanies the milling process.
• Compared to the chemo-physical production processes (see
below), using mills to crush particles yields product powders
with a relatively broad particle-size ranges. This method does
not allow full control of particle shape.
• Bottom-up/Chemo-physical production
processes
• Bottom-up methods are based on
physicochemical principles of molecular or
atomic self-organization. This approach produces
selected, more complex structures from atoms or
molecules, better controlling sizes, shapes and
size ranges. It includes aerosol processes,
precipitation reactions and solgel processes
(Figure 3).
Figure 3. Chemo-physical processes in nanoparticle production
Wet Chemical Synthesis of Nano-materials- sol-gel process
The encapsulated liquid can be removed from a gel by either
evaporative drying or with supercritical drying /extraction. The
resulting solid products are known as xerogel and
aerogel respectively. When gels are dried by evaporation, the
dried product is called xerogel. When the gels are dried by
supercritical drying, the dried gel is called aerogels. The aerogel
retains high porosity and has very high pore volume.
Gas phase Synthesis of Nano-materials- Furnace process

Fig:Schematic representation of gas phase process of synthesis of single phase

nanomaterials from a heated crucible
Energy is normally introduced into the precursor by arc heating, electronbeam heating or
Joule heating. The atoms are evaporated into an atmosphere, which is either inert (e.g.
He) or reactive (so as to form a compound). To carry out reactive synthesis, materials with
very low vapour pressure have to be fed into the furnace in the form of a suitable
precursor such as organometallics, which decompose in the furnace to produce a
condensable material. The hot atoms of the evaporated matter lose energy by collision
with the atoms of the cold gas and undergo condensation into small clusters via
homogeneous nucleation
Gas phase Synthesis of Nano-materials- Furnace process

Fig:Schematic representation of gas phase process of synthesis of single phase

nanomaterials from a heated crucible
In case a compound is being synthesized, these precursors react in the gas phase and
form a compound with the material that is separately injected in the reaction chamber.
The clusters would continue to grow if they remain in the supersaturated region. To
control their size, they need to be rapidly removed from the supersaturated environment
by a carrier gas.
Gas phase Synthesis of Nano-materials-
Furnace process
The simplest fashion to produce nanoparticles is by heating the desired material in a heat
resistant crucible containing the desired material. This method is appropriate only for
materials that have a high vapour pressure at the heated temperatures that can be as high
as20000 c.

Fig:Schematic representation of gas phase process of synthesis of single phase

nanomaterials from a heated crucible
Gas phase Synthesis of Nano-materials-
Furnace process
The simplest fashion to produce nanoparticles is by heating the desired material in a heat
resistant crucible containing the desired material. This method is appropriate only for
materials that have a high vapour pressure at the heated temperatures that can be as high
as20000 c.

Fig:Schematic representation of gas phase process of synthesis of single phase

nanomaterials from a heated crucible
Gas phase Synthesis of Nano-materials
Flame assisted ultrasonic spray pyrolysis
Gas phase Synthesis of Nano-materials
Flame assisted ultrasonic spray pyrolysis(FSP)
Gas phase Synthesis of Nano-materials
Flame assisted ultrasonic spray pyrolysis
In this process, precusrsors are nebulized and then unwanted components are burnt in a
flame to get the required material, eg. ZrO2 has been obtained by this method from a
precursor of Zr(CH3 CH2 CH2O)4.
Flame hydrolysis that is a variant of this process is used for the manufacture of fused
silica. In the process, silicon tetrachloride is heated in an oxy-hydrogen flame to give a
highly dispersed silica. The resulting white amorphous powder consists of spherical
particles with sizes in the range 7-40 nm. The combustion flame synthesis, in which the
burning of a gas mixture, e.g. acetylene and oxygen or hydrogen and oxygen, supplies the
energy to initiate the pyrolysis of precursor compounds, is widely used for the industrial
production of powders in large quantities, such as carbon black, fumed silica and titanium
dioxide.
However, since the gas pressure during the reaction is high, highly agglomerated powders
are produced which is disadvantageous for subsequent processing. The basic idea of low
pressure combustion flame synthesis is to extend the pressure range to the pressures used
in gas phase synthesis and thus to reduce or avoid the agglomeration. Low pressure flames
have been extensively used by aerosol scientists to study particle formation in the flame.

Zirconium dioxide
 Gas phase Synthesis of Nano-materials
Gas Condensation Processing (GPC)

Fig. Schematic representation of typical set-up for gas condensation synthesis of

nanomaterials followed by consolidation in a mechanical press or collection in an appropriate
solvent media.
 Gas phase Synthesis of Nano-materials
Gas Condensation Processing (GPC)

Fig. Schematic representation of typical set-up for gas condensation synthesis of

nanomaterials followed by consolidation in a mechanical press or collection in an appropriate
solvent media.
Gas phase Synthesis of Nano-materials
Gas Condensation Processing (GPC)
In this technique, a metallic or inorganic material, e.g. a suboxide, is vaporised
using thermal evaporation sources such as crucibles, electron beam evaporation
devices or sputtering sources in an atmosphere of 1-50 mbar He (or another inert
gas like Ar, Ne, Kr). Cluster form in the vicinity of the source by homogenous
nucleation in the gas phase and grow by coalescence and incorporation of atoms
from the gas phase.
Originally, a rotating cylindrical device cooled with liquid nitrogen was employed
for the particle collection: the nanoparticles in the size range from 2-50 nm are
extracted from the gas flow by thermophoretic forces and deposited loosely on
the surface of the collection device as a powder of low density and no
agglomeration. Subsequenly, the nanoparticles are removed from the surface of
the cylinder by means of a scraper in the form of a metallic plate. In addition to
this cold finger device several techniques known from aerosol science have now
been implemented for the use in gas condensation systems such as corona
discharge, etc. These methods allow for the continuous operation of the
collection device and are better suited for larger scale synthesis of nanopowders.
Gas phase Synthesis of Nano-materials
Chemical Vapour Condensation (CVC)
Gas phase Synthesis of Nano-materials
Chemical Vapour Condensation (CVC)
Gas phase Synthesis of Nano-materials
Chemical Vapour Condensation (CVC)
As shown schematically in Figure, the evaporative source used in GPC is replaced by a hot
wall reactor in the Chemical Vapour Condensation or the CVC process. Depending on the
processing parameters nucleation of nanoparticles is observed during chemical vapour
deposition (CVC) of thin films and poses a major problem in obtaining good film qualities.
The original idea of the novel CVC process which is schematically shown below where, it
was intended to adjust the parameter field during the synthesis in order to suppress film
formation and enhance homogeneous nucleation of particles in the gas flow
 Module 4
NANO MATERIALS & CHARACTERIZATION
TECHNIQUES:
• Introduction: Importance of Nano-technology,
Emergence of Nanotechnology, Bottom up and Top-down
approaches, challenges in Nanotechnology
• Nano-materials Synthesis and Processing:
Methods for creating Nanostructures; Processes for
producing ultrafine powders- Mechanical grinding; Wet
Chemical Synthesis of Nano-materials- sol-gel process;
Gas Phase synthesis of Nano-materials-Furnace, Flame
assisted ultrasonic spray pyrolysis; Gas Condensation
Processing (GPC), Chemical Vapour Condensation(CVC).
 Module 4
NANO MATERIALS & CHARACTERIZATION TECHNIQUES:
• Optical Microscopy - Principles, Imaging Modes, Applications,
Limitations.
• Scanning Electron Microscopy (SEM) - Principles, Imaging
Modes, Applications, Limitations.
• Transmission Electron Microscopy (TEM) - Principles, Imaging
Modes, Applications, Limitations.
• X- Ray Diffraction (XRD) - Principles, Imaging Modes,
Applications, Limitations.
• Scanning Probe Microscopy (SPM) - Principles, Imaging Modes,
Applications, Limitations.
• Atomic Force Microscopy (AFM) - basic principles,
instrumentation, operational modes, Applications, Limitations.
• Electron Probe Micro Analyzer (EPMA) - Introduction, Sample
preparation, Working procedure, Applications, Limitations.
 Module 4
NANO MATERIALS & CHARACTERIZATION
TECHNIQUES:
• Optical Microscopy - Principles, Imaging
Modes, Applications, Limitations.
 OPTICAL MICROSCOPY
Fig: Basic optical transmission
microscope elements
The optical microscope, often referred to as the light
microscope, is a type of microscope that commonly
uses visible light and a system of lenses to magnify
images of small objects.
Basic optical microscopes can be very simple,
although many complex designs aim to
improve resolution and sample contrast.
Types of compound optical microscope.
Stereo microscope, a low-powered microscope which
provides a stereoscopic view of the sample,
commonly used for dissection.
Comparison microscope, which has two separate light
paths allowing direct comparison of two samples via
one image in each eye.
Inverted microscope, for studying samples from
below; useful for cell cultures in liquid, or for
metallography.
 OPTICAL MICROSCOPY
• Principles
Optical Microscopy is a surface investigation
technique that relies on the use of light in
the visible spectrum to image the
topography of a sample.
It is usable for feature sizes down to the
micron range and can also be used to obtain
information about the lateral structure, that
is the height differences occurring on the
sample.

Fig: Basic optical transmission

microscope
 OPTICAL MICROSCOPY
Principles
An optical microscope creates a magnified image of an object specimen with an
objective lens and magnifies the image further more with an eyepiece to allow the
user to observe it by the naked eye. Assuming a specimen as AB in the following figure,
primary image (magnified image) A'B' of inverted real image is created with objective
lens

Diagram of a simple microscope Diagram of a compound microscope

 OPTICAL MICROSCOPY
• Imaging Modes
• Different schemes of illumination of the
sample resulting in different aspects of the
images being amplified, often resulting in
better image quality.
– Bright field illumination
– Dark field illumination
– Color filtering
 OPTICAL MICROSCOPY
• Imaging Modes
 OPTICAL MICROSCOPY
• Applications
• Optical microscopy is used extensively in
microelectronics, nanophysics,
biotechnology, pharmaceutics research,
mineralogy and microbiology.
• Optical microscopy is used for medical
diagnosis, the field being
termed histopathology when dealing with
tissues, or in smear tests on free cells or
tissue fragments.
 OPTICAL MICROSCOPY
• Limitations
• At very high magnifications with
transmitted light, point objects are seen as
fuzzy discs surrounded by diffraction rings.
These are called Airy disks.

Two points showing the limits of detection

 OPTICAL MICROSCOPY
• Limitations
• At very high magnifications with
transmitted light, point objects are seen as
fuzzy discs surrounded by diffraction rings.
These are called Airy disks.
• The resolving power of a microscope is
taken as the ability to distinguish between
two closely spaced Airy disks.
• It is these impacts of diffraction that limit
the ability to resolve fine details.
Scanning Electron Microscopy (SEM)
 Scanning Electron Microscopy (SEM)
Principles
SEM can produce images with high resolution at
high magnification. Comparing to the light
microscopy, the high resolution in SEM is about
10 nm while a typical light microscopy can
produce images with the best resolution about
200 nm.
Moreover, SEM has depth of field, which is the
height of a sample that appears in focus in an
image, approximately 300 times more than the
light microscopy. This feature can be used to
obtain great topographical information.
 Scanning Electron Microscopy (SEM)
Principles
Scanning electron microscopy is a machine that is
used to characterize objects with size between 1
micron to 1 nanometer.
The basic idea of the SEM is the use of a focused
beam of electrons. By using the beam of high-
energy electrons, SEM can reveal levels of detail
and complexity that are inaccessible by using light
microscopy.
In addition, SEM has the ability to magnify objects
from about 10 times up to 300,000 times with
high resolution.
 Scanning Electron Microscopy (SEM)
Principles
The basic idea of the SEM is the use of a focused
beam of electrons. By using the beam of high-
energy electrons,
 Scanning Electron Microscopy (SEM)
SEM works by creating an electron beam with high energy produced
by an electron gun. The electron beam will be controlled by a series
of lenses and apertures. When the electron beam arrives to the
surface of the specimen, electron-sample interaction will occur and
several types of signals will be generated. Different types of
detectors to produce a SEM image can detect these signals. SEM
machine operates at a high vacuum level to avoid the
contamination.

SEM contains five major parts that work together to analyze a sample.
Each one of these five components has its specific function in the SEM
system (Figure1).
Electron gun
Electron column
High Voltage
Optics
Scan coils
Stage
Detector
Vacuum chamber
 Scanning Electron Microscopy (SEM)
Electron gun consisting of
cathode and anode.
• The condenser lens
controls the amount of
electrons travelling down
the column
• The objective lens focuses
the beam into a spot on the
sample.
• Deflection coil helps to
deflect the electron beam.
• SED attracts the secondary
electrons.
• Additional sensors detect
backscattered electrons and
Fig:1. Schematic of a Scanning Electron Microscope X-rays.
 Scanning Electron Microscopy (SEM)

Fig: 1. Schematic of a Scanning Electron Microscope

 Scanning Electron Microscopy (SEM)
Imaging Modes
For better understanding, we need to know the roles of the four
scattered events above in SEM system and how they are formed.
Visible light.
Because of some specimens molecules has the ability to emit
light photons when they are exposed to an electron beam, the
visible light will be produced in this case. Some information
about the compound and the structure of the specimen can be
obtained from this event.
Backscattered electrons.
When the primary electron beam hits the surface of the
specimen and cannot go through the specimen; therefore, it
will be reflected back to produce a backscattered electrons with
high energy level approximately the same as the gun energy.
This event will provide great information about the chemical
component information of the sample in addition to some
information relates to the topographical analysis. For
backscattered electron, the detector will be the same as for the
secondary electron detectors.
Fig: Schematic of a Scanning Electron Microscope
 Scanning Electron Microscopy (SEM)
• Limitations
• SEMs are expensive and large.
• Special training is required to operate an
SEM.
• The preparation of samples can result in
artifacts.
• SEMs are limited to solid samples.
• SEMs carry a small risk of radiation
exposure associated with the electrons
that scatter from beneath the sample
surface.
 Scanning Electron Microscopy (SEM)
• Applications
• Virology - for investigations of virus structure
• Cryo-electron microscopy – Images can be made of
the surface of frozen materials.
• 3D tissue imaging -
– Helps to know how cells are organized in a 3D
network
– Their organization determines how cells can interact.
• Forensics - SEM reveals the presence of materials on
evidences that is otherwise undetectable
• SEM renders detailed 3-D images
– extremely small microorganisms
– anatomical pictures of insect, worm, spore, or other
organic structures
 Scanning Electron Microscopy (SEM)
• Applications

SEM image of pollen grains Drosophila's eye.

SEM image of blood cells

Transmission Electron Microscopy (TEM)
 Transmission Electron Microscopy (TEM)
Principles
Transmission electro microscopy
(TEM) is a microscopy technique in
which a beam of electrons is
transmitted through an ultra-thin
specimen.
Transmission Electron Microscopy (TEM)
 Transmission Electron Microscopy (TEM)
Working
• Specimen is bombarded by a beam of electrons, the primary electrons .
The bombarding electrons are focussed to a bundle onto the object.
• In areas in the object where these electrons encounter atoms with a heavy
atomic nucleus, they rebound.
• In regions where the material consists of lighter atoms , the electron are
able to pass through.
• The fine pattern of electrons leaving the object , reaches the objective lens
forms the image
• It is then greatly enlarged by projector lens.
• Eventually, the traversing electrons (transmission) reach the scintillator
plate at the base of the column of the microscope.
• The scintillator contains phosphor compounds that can absorb the energy of
the stricking electrons and convert it to light flashes.
• Thus a contrasted image is formed on this plate.
 Transmission Electron Microscopy (TEM)
• Advantages
• TEMs offer the most powerful magnification,
potentially over one million times or more.
• TEMs have a wide range of applications and can be
utilized in a variety of different scientific, educational
and industrial fields.
• TEMs provide information on element and compound
structure
• Images are high-quality and detailed.
• TEMs are able to yield information of surface features,
shape, size and structure.
• They are easy to operate with proper training.
 Transmission Electron Microscopy (TEM)
• Limitations
• TEMs are large and very expensive.
• Laborious sample preparation.
• Potential artifact from sample preparation.
• Operation and analysis requires special training.
• Samples are limited to those that are electron
transparent, able to tolerate the vacuum chamber and
small enough to fit in the chamber.
• TEMs require special housing and maintenance
• Images are black and white.
 Transmission Electron Microscopy (TEM)
• Applications
• A Transmission Electron Microscope is ideal for a
number of different fields such as life sciences,
nanotechnology, medical, biological and material
research, forensic analysis, gemology and metallurgy
as well as industry and education.
• TEMs provide topographical, morphological,
compositional and crystalline information.
• The images allow researchers to view samples on a
molecular level, making it possible to analyze structure
and texture.
• This information is useful in the study of crystals and
metals, but also has industrial applications.
 Transmission Electron Microscopy (TEM)
• Applications
• TEMs can be used in semiconductor analysis and
production and the manufacturing of computer and
silicon chips.

TEM image of golgi complex E. coli bacteria

X- Ray Diffraction (XRD)
 X- Ray Diffraction (XRD)
X-ray powder diffraction (XRD) is a rapid analytical
technique primarily used for phase identification of a
crystalline material and can provide information on
unit cell dimensions
The analyzed material is finely ground, homogenized,
and average bulk composition is determined.
 X- Ray Diffraction (XRD)
Principles
X-ray diffraction is based on constructive interference of
monochromatic x-rays and a crystalline sample. These x-
rays are generated by a cathode ray tube, filtered to
produce monochromatic radiation, collimated to
concentrate and directed towards the sample. The
interaction of incident rays with the sample produces
constructive interference when conditions satisfy Bragg’s
law.
 X- Ray Diffraction (XRD)
Principles

Production of X-rays:
X-rays are generated when high velocity electrons impinge on a
metal target. Approximately 1% of the total energy of the electron
beam is converted into x-radiation. The remainder being
dissipated as heat. Many types of x-ray tubes are available which
are used for producing x-rays.
 X- Ray Diffraction (XRD)
• Applications
• The electron density and accordingly, the position of
the atoms in complex structures, such as penicillin may
be determined from a comprehensive mathematical
study of the x-ray diffraction pattern.
• The elucidation of structure of penicillin by XRD paved
the way for the later synthesis of penicillin.
• The powder XRD pattern may be thought of as finger
print of the single crystal structure, and it may be used
conduct qualitative and quantitative analysis.
• XRD can also be used to determine whether the
compound is solvated or not.
Scanning Probe Microscopy (SPM)
 Scanning Probe Microscopy (SPM)
• Scanning probe microscopy covers several related
technologies for imaging and measuring surfaces on a
fine scale, down to the level of molecules and groups
of atoms.
• SPMs are a very powerful family of microscopes,
sometimes with a resolution of less than a nanometer.
(A nanometer is a billionth of a meter.)
• SPMs can detect differences in height that are a
fraction of a nanometer, about the diameter of a single
atom.
 Scanning Probe Microscopy (SPM)
• Principle
• An SPM has a probe tip mounted on the end of a
cantilever. The tip can be as sharp as a single atom. It
can be moved precisely and accurately back and forth
across the surface, even atom by atom.
• When the tip is near the sample surface, the cantilever
is deflected by a force. SPMs can measure deflections
caused by many kinds of forces, including mechanical
contact, electrostatic forces, magnetic forces, chemical
bonding, van der Waals forces, and capillary forces.
 Scanning Probe Microscopy (SPM)
• Principle

Scanning probe microscope

 Scanning Probe Microscopy (SPM)
• Working
• SPM technologies share the concept of
scanning an extremely sharp tip(3-50
nm radius of curvature)across the
object surface. The tip is mounted on a
flexible cantilever, allowing the tip to
follow the surface profile (see Figure).
• When the tip moves in proximity to the
investigated object, forces of
interaction between the tip and the
surface influence the movement of the
cantilever.
• The tip is moved across the sample
many times. This is why these are
called
• “scanning” microscopes. A computer
combines the data to create an image.
 Scanning Probe Microscopy (SPM)
• Advantages
• Advantages of Scanning Probe Microscopy Technology
• Scanning Probe Microscopy provides researchers with
a larger variety of specimen observation environments
using the same microscope and specimen reducing the
time required to prepare and study specimens.
• Specialized probes, improvements and modifications
to scanning probe instruments continues to provide
faster, more efficient and revealing specimen images
with minor effort and modification.
 Scanning Probe Microscopy (SPM)
• Limitations
• Unfortunately, one of the down sides of scanning
probe microscopes is that images are produced in
black and white or gray scale which can in some
circumstances exaggerate a specimens actual shape or
size.
• Computers are used to compensate for these
exaggerations and produce real time color images that
provide researchers with real time information
including interactions within cellular structures,
harmonic responses and magnetic energy.
 Scanning Probe Microscopy (SPM)
• Applications
• In Scanning Tunneling Microscopy(STM)
• To measure the electron density of material surface
Atomic Force Microscopy (AFM)
Atomic Force Microscopy (AFM)
 Atomic Force Microscopy (AFM)
• Principle
• The atomic force microscope(AFM) was developed to
over come a basic draw back with STM–it can only
image conducting or semi conducting surfaces.
• The AFM has the advantage of imaging almost any
type of surface, including polymers, ceramics,
composites, glass, and biological samples.
 Atomic Force Microscopy (AFM)
• Advantages
• AFM has several advantages over the scanning
electron microscope (SEM).Unlike the electron
microscope which provides a two-dimensional
projection or a two-dimensional image of a sample,
the AFM provides a three-dimensional surface profile.
• Additionally, samples viewed by AFM do not require
any special treatments (such as metal/carbon
coatings)that would irreversibly change or damage the
sample.
 Atomic Force Microscopy (AFM)
• Limitations
• AFM can only image a maximum height on the order
of 10-20 micrometers and a maximum scanning area
of about 150 × 150 micrometers.
• Highly dependent on probes.
• Error occurring due to interaction.
 Atomic Force Microscopy (AFM)
• Applications
• To investigate properties of surfaces
• To investigate topology of surfaces
• To investigate properties of single molecules
• To investigate forces within molecules

AFM topography of Scan of glass

Electron Probe Micro Analyzer (EPMA)
 Electron Probe Micro Analyzer (EPMA)
An electron microprobe (EMP), also known as an electron
probe microanalyzer (EPMA) or electron micro probe
analyzer (EMPA), is an analytical tool used to non-
destructively determine the chemical composition of small
volumes of solid materials. It works similarly to a scanning
electron microscope: the sample is bombarded with
an electron beam, emitting x-rays at wavelengths
characteristic to the elements being analyzed. This enables
the abundances of elements present within small sample
volumes (typically 10-30 cubic micrometers or less) to be
determined. The concentrations of elements
from beryllium to plutonium can be measured at levels as low
as 100 parts per million (ppm). Recent models of EPMAs can
accurately measure elemental concentrations of
approximately 10 ppm.
 Electron Probe Micro Analyzer (EPMA)
• Principle
• Electrons emitted from the electron source are
accelerated at a certain accelerating voltage and
collimated through electron lenses. When this electron
beam hits a specimen, X-rays are generated from the
specimen. By dispersing this X-ray using a dispersive
element, the composition of the specimen can be
examined. This type of spectrometer is called a
wavelength dispersive X-ray spectrometer (WDS).
 Electron Probe Micro Analyzer (EPMA)
• Principle
 Electron Probe Micro Analyzer (EPMA)
• Principle
 Electron Probe Micro Analyzer (EPMA)
• Principle

When accelerated electrons hit a specimen,

in addition to the X-rays, particles and
electromagnetic waves carrying various
kinds of information are emitted. With
EPMA, signals such as the characteristic-X-
rays, secondary electrons, backscattered
electrons, etc. are detected by the
appropriate detectors and that information
is utilized to find the area of interest on a
specimen, and for analysis.
 Electron Probe Micro Analyzer (EPMA)
• Principle

When accelerated electrons hit a specimen, in addition to the X-rays, particles

and electromagnetic waves carrying various kinds of information are emitted.
With EPMA, signals such as the characteristic-X-rays, secondary electrons,
backscattered electrons, etc. are detected by the appropriate detectors and that
information is utilized to find the area of interest on a specimen, and for
analysis.
 Electron Probe Micro Analyzer (EPMA)
• Advantages
This shows the result of area analysis (where is each element
distributed?) for Sn, and Si, which were detected in the
preceding qualitative analysis. In area analysis, the more
concentrated the red color on the color bar is, the more
concentrated the element being analyzed is. It is clear that there
is a difference in distribution concentration between Sn and Si.
 Electron Probe Micro Analyzer (EPMA)
• Limitations
Electron Probe Micro Analyzer (EPMA)
 Electron Probe Micro Analyzer (EPMA)
• Applications
• Geochemistry, mineralogy, geochronology, physical metallurgy,
nuclear metallurgy, materials science including glass, ceramics,
superconductors, cements, microelectronics, and biochemistry.
• EPMA provides much better results than standard SEM/EDS
systems. Because of the internal properties of WDS, the general
sensitivity, analysis of light elements and risks of erroneous
interpretation of qualitative spectra are all superior with EPMA.
• Spectral resolution and detector dead time are much better
than EDS (Energy Dispersive Spectroscopy).
• The excitation beam regulation system and sophisticated
sample stage capabilities guarantee that this technique provides
outstanding stability and measurement repeatability.
That’s all for the day.

Any Questions.