• Basics-distinction between molecules, nanomaterials and bulk

materials; size-dependent properties.

• Types –nanoparticle, nanocluster, nanorod, nanowire and
nanotube (definition, properties and uses).
• Preparation of nanomaterials: sol-gel, solvothermal, laser
ablation, chemical vapour deposition, electrochemical
deposition and electro spinning.
• Characterization - Scanning Electron Microscope and
Transmission Electron Microscope:- Principle and
instrumentation (block diagram).
• Properties (optical, electrical, mechanical and magnetic) and
Applications of nanomaterials - medicine, agriculture,
electronics and catalysis (at least 6 in each).
 5.1 BASICS - NANOCHEMISTRY:

Branch of nano science dealing with the study and

application of extremely small sized materials with at
least one dimension in the 1-100 nm range.
5.2 CLASSIFICATION OF NANOMATERIALS:

•Zero dimensional : Have diameter less than 100 nm. Eg :

nanoparticles, nanoclusters and nanocrystals

•One dimensional : One dimension exceeds in nanometer

scale. Eg: nanofibre, nanorod, nanotube.

•Two dimensional : Two dimensions exceeds in

nanometer scale. Eg : films and coatings with nanometer
thickness.

Three dimensional : Three dimensions exceeds in

nanometer scale. Eg : powders, multilayer materials
5.3 DISTINCTION BETWEEN MOLECULES, NANOPARTICLES
AND BULK MATERIALS:
Property Molecules Nanoparticles Bulk materials

collection of
collection of collection of
1 Constitution thousands of
atoms few molecules
molecules.
in the range
less than 100
2 Size of picometer range in microns
nm
(10-12 m)
well defined well defined depends on the
3 Geometrical structure
structures structures crystalline lattices.
Physical properties constant Not constant Constant
4 (eg : melting point, Eg: Gold sheet melting point = 1064 °C
boiling point etc.) Gold nanoparticles melting point = 300 °C
Very high
Low compared to
5 Surface area NA compared to
nanomaterials
bulk materials
In general, Nanomaterials Vs Bulk materials:
Nanomaterials possess:

•Hardness : 5 times more

•Wear resistance : 200 times more
•Electrical resistivity : 3 times more
•Optical : unexpected property
•Mechanical : less defects and hence more strength
mechanical strength
5.4 SIZE DEPENDENT PROPERTIES OF
NANOMATERIALS

Significant change in the following properties are

observed for nanomaterials compared to their bulk
counterparts, due to the reduction in size, without change
in chemical composition.
•Nanomaterials have extremely large surface area to
volume ratio called as Aspect ratio.
•They have large fraction of surface atoms, high surface
energy, spatial confinement and reduced imperfections.
•These enhance the properties of nanomaterials.
Examples of Nanomaterials
 Optical Properties
•Quantum confinement &
•Surface plasma resonance
--- responsible for a change in
optical properties of materials in nm scale.
Eg : 1. Ag : 40 nm size : blue 2. Gold : 25 nm : red
Ag : 100 nm size : yellow Gold : 50 nm : green
Prism shaped Ag nano : Red Gold :100 nm : orange

1 kg of particles of 1 mm3 has the same surface area as 1 mg of particles of 1 nm3

 Quantum confinement

Quantum confinement is change of electronic and

optical properties when the material sampled is of
sufficiently small size - typically 10 nanometers or less.
The bandgap increases as the size of the nanostructure
decreases.
• Surface plasmon resonance (SPR) is the
resonant oscillation of conduction electrons at
the interface between negative and positive
permittivity material stimulated by incident
light.
•Mechanical Properties :

Nanomaterials have lesser voids and defects compared to

bulk materials. Therefore they impart very good
mechanical properties.

Compared to bulk materials, for nanomaterials,

Hardness : 5 times more;
Wear resistance : 200 times more;
Corrosion resistance : higher ;
Toughness and ductility : can be varied according to
requirement.
Eg : Nanocomposites of polymers metals and ceramics.
•Melting points :

Significantly lower for nanomaterials, because most of the

atoms in the material are at the surface.

Eg : Gold – bulk gold has a melting point of 1064 ºC

while 100 nm gold particles have a melting point of 300
ºC.
•Electrical Properties :
Conductivity decreases with decrease in size due to
increased surface scattering. But better ordering of the
particles in micro structure can enhance the conductivity.
Therefore, nanomaterials with the same chemical
composition but different conductivities can be prepared.
Eg :
•Metals --- become non-metallic when the diameter of the
nano crystals is in 1-2 nm range.
•Hg clusters --- shows non-metallic band gap but with the
addition of more Hg atom to clusters , band gap can be
decreased to metallic range.
•Magnetic properties:
With most of the atoms on the surface, the coupling of
magnetic moments of atoms leads to an entirely different
set of magnetic properties for nanomaterial.
Eg : Bulk Au & Pt --- non-magnetic
50 nm Au & Pt --- magnetic
< 25 nm --- super paramagnetic
Paramagnetic materials are materials that tend to get weakly magnetized in the
direction of the magnetizing field when placed in a magnetic field. Paramagnetic
substances are those which are attracted by magnetic field and have impaired electrons.
They lose magnetism in the absence of magnetic field. The greater the number of
unpaired electrons, the greater the magnetic moment of the substance and hence
greater the paramagnetism CuO,Fe3+,Al,Mn,Cu2+
Example Super paramagnetic means that on application of an external magnetic field,
they become magnetized up to their saturation magnetization, and on removal of the
magnetic field, they no longer exhibit any residual magnetic interaction. Eg magnetite
(Fe3O4) and maghemite (Fe2O3)
•Catalytic properties :

Larger surface area : 1000 times more catalytic

efficiency

Particle Size reduction

Increases hardness, strength, toughness and catalytic

properties.

Decreases conductivity, melting point, density, electrical

properties.
5.5 NANOPARTICLES DEFINITION:

They are the simplest nano structures with any collection

of atoms bonded together with a structural radius of < 100
nm. Eg : TiO2 nanoparticles added in paints and sunscreen
lotions.
5.5 CHARACTERISTICS OF NANOPARTICLES:

Characteristics:
•Zero dimentional nanostructures
•Most of their physical properties are not constant
•Have peculiar optical properties.

They are small enough to limit the thickness of

common electron layer metals leading to quantum effects
5.5 USES OF NANOPARTICLES

•Pd nanoparticles are used as H2 storage materials.

•Ag & Au nanoparticles – transmit brilliant coloured light
through glass windows.
•Gold and nanopolymer composites are used for cancer
detection and treatment
•Cu & Ag nanoparticles are used in electronics
•<100 nm sized Ag & TiO2 are used in surgical masks due
to their antimicrobial properties
•Ag & AgO nanoparticles are used in air filters in air
conditioners, sweat-free textiles & sports wears.
•Nanoclusters :
They are zero dimensional nanomaterials with
dimension 1 – 10 nm and narrow size distribution. They
are formed by the aggregation of atoms (or) molecules by
i) Van der Waals,
ii) Metallic,
iii) Ionic (or)
iv) Networking types of interaction.
Eg., Nanocarbon clusters, Au clusters.
•Nanoclusters : Characteristics:

They exhibit quantum electronic properties such as

i) photoluminescence,
ii) ferromagnetism (Ferromagnetism refers to the phenomenon by which
ferromagnetic metals such as iron, nickel, cobalt and certain alloys become magnetized in a
magnetic field and retain their magnetism when the field is removed For Eg Fe, Ni, Co)

iii) semiconduction,
iv) photoconductivity

The growth of nanoclusters proceeds through the

formation of “magic no” clusters that exhibit usual
electronic properties
(The magic numbers for atoms are 2, 10, 18, 36, 54, and 86, corresponding to the total
number of electrons in filled electron shells)
•Nanoclusters Uses:

•Si nanoclusters embedded in wide band gap materials are

used for the construction of microelectronic and optical
devices.

•Core-shell nanoclusters with tunable properties are used

for magnetic recording, magnetic sensor, bioseparation &
drug delivery applications.
•Nanorods :
They are cylindrical, solid nanostructures with the length
in the range: 10 nm to few µm and width in the nano scale
dimensions of 1-100 nm.
The aspect ratio ie., the ratio of length to width is less than
10.
Eg : Gold nanorods as biomedical sensor for cancer
diagnosis.
•Nanorods : Characteristics:
•One dimensional nano structures.

•Exhibit optical absorbance, luminescence of

photodetection property.

•Have anisotropic magnetic properties (Magnetic anisotropy is the

property that confers a preferred direction on the spin of a system which may not
be aligned with an external magnetic field)

•Many of them can be prepared as conducting and

superconducting material.
•Nanorods :
Uses:
•Au nanorods are used for detecting target sequences in
disease like HIV-1, cancer.
•MnO2 rods of 5- 6 nm dia and 20-40 nm length are
excellent electrochemical capacitors.
•ZnO nanorods are used in optoelectronic devices as UV
light emitters.
•MgO nanorods are used in high temperature
superconductors.
•ZnO nanods arrays are used as gas sensors.
•Nanowires :

Cylindrical, solid nanostructures with diameter in the 10 –

100 nm range and length in µm dimension.
Aspect ratio is greater than 10.

Eg :
i) Ag, Au, Ni-nanowires in bar code tags.
ii) p-n junction nano wires made of ZnO, CdO etc. for
LED.
•Nanowires : Properties:

•One dimensional nanostructures.

•Electrical conductivity is less than that of bulk materials.

•High aspect ratio, enhances physical properties.

•Nanowires : Uses:

•Nanowires of Ag, Au, Ni, Pd, etc are used as barcode

tags.

•Semiconductor nanowires are used as junction in

LEDs, transistors, invertors, switches & memory cells.

•In2O3 nanowires are used as chemisensors at room

temperature.
•Nanotubes:
Long, hollow solid structures with the walls formed by one atom
thick sheets of materials. They can be metallic, semiconducting (or)
semiconducting depending on the diameter, length and chirality
(twist).
Eg : Carbon nanotubes (CNT)
•Structures of interest are carbon nanotubes (CNT)
•Consists of graphitic layers seamlessly wrapped to cylinders
•Both single walled CNTs and multi walled CNTs can be prepared

Depending on the hexagonal lattice, SWNTs can have the

following orientation
•Arm chair
•Zig-zag
•Chiral
Nanotubes: Properties
•CNTs are flexible & do not break on bending
•Thermal conductivity of CNTs is several times higher
compared to graphite and bulk materials
•CNTs are 100 times stronger than steel even though they
are 6 times lighter.
•Metallic or semiconducting property of CNTs is
determined by its helicity
Nanotubes : Uses
•Used for H2 storage in fuel cells
•In field emission array for flat-panel display in mobiles &
laptops
•Used in high energy density batteries
•Used in CNT-based cross bar memory called Nano-RAM
•Used in aerospace vehicle construction
•Used for customized fabrication of artificial joints &
body parts for implants

•Used as drug delivery vehicles

Nickel titanium, also known as nitinol, is
a metal alloy of nickel and titanium, where the two elements are
present in roughly equal atomic percentages. Different alloys
are named according to the weight percentage of nickel; e.g.,
nitinol 55 and nitinol 60

Nitinol is deformed at a low temperature, and heated to recover

its original shape through the shape memory effect

Image: A nitinol paperclip bent and recovered after being

placed in hot water

.
5.6 PREPARATION OF NANOMATERIALS
•PREPARATION OF CARBON NANOTUBE (CNT):

• Laser ablation
• Chemical vapour deposition – CVD
•Laser ablation for CNT preparation:

Principle:

A graphite target is vaporized and ablated

(gradually removed from) by a beam of laser. The
evaporated carbon atoms are swept by an inert gas to a
cooler zone. The carbon atoms condense as nanotubes in
presence of nucleation sites.
Reactor:
The reactor consists of a quartz tube filled with an inert gas
like He (or) Ar. One end of a quartz tube is fitted with a laser torch
and the other end has a water-cooled copper collector. A graphite
target containing a small amount of Ni (or) Co is placed in-between
these two ends. The entire quartz tube reactor is placed in an
electric furnace.
Procedure:
•Quartz tube is heated up to 1200˚C using the external
furnace.
•Graphite target at high temperature is exposed to intense
pulsed laser beam.
•Supersonic jet of carbon particles, called plume is
ejected.
•Plume is swept by the inert gas towards the colder copper
collector.
•The plume expands & forms the tube on the copper
surface.
•Co (or) Ni acts as nucleation sites for the formation of
CNT.
Advantages:
•Single-walled CNT of 10-20 nm dia and 100 nm lengths
can be prepared by this method.

•CNT is obtained in high yield.

•Diameter of CNT can be critically controlled.

•Chemical Vapour Deposition (CVD) for CNT
preparation:

Principle:
Hydrocarbon gas is decomposed at a high
temperature in presence of a metal nanoparticle catalyst.
Vapours of carbon atoms travel to a cooler surface
containing metal catalysts & condense to form CNT. The
size of the metal nanoparticles determines the diameter of
CNT.
Schematic representation of chemical vapor deposition (CVD) process. a
Simplified scheme of a CVD reactor for (carbon nanotubes) CNTs
synthesis; b base-growth model of CNT growth mechanism; c tip-growth
model of CNT growth mechanism
Procedure:
•A hydrocarbon gases such as methane (or) acetylene is
sent along with a carrier gas into a quartz reactor tube.
•The tube is heated with an external heater.
•On decomposition, hydrocarbon produces carbon atoms
which are allowed to condense on a cooler surface.
•Ni (or) Co metal nanoparticles mixed with MgO act as
catalyst and also determine the size of CNT.
Advantages:
•Suitable for the continuous production of CNT on
industrial scale.
•High purity of product.

Colorless gem cut from diamond Free-standing single-crystal

grown by chemical vapor deposition CVD diamond disc
Preparation of nanoparticles by sol-gel method:
Principle:
[Sol- is a colloidal (or) a molecular suspension of
solid particles in a solvent. Gravity does not act on it and
size is 1-100 nm. Gel- is a semi-rigid mass that is formed
when the sol begins to evaporate. The particles then join
together to form a continuous network.]

•The sol of the nanoparticle is prepared by dispensing the

solid (or) hydrolysis of precursor compound in a suitable
solvent.
•Sol is aged to form a gel.
•Gel is subjected to heat treatment to form crystalline
nanoparticles.
Advantages:
•Porous as well as dense solids can be prepared.
•Both amorphous and crystalline (silica, alumina, zeolites)
materials can be prepared.
SOLVOTHERMAL METHOD FOR NANOPARTICLE
PREPARATION
Procedure:
•Reaction vessel is an autoclave made of steel and lined inside with
Teflon.
•Metal salt + an organic template + a reducing agent are dissolved
in a suitable solvent. The solvent can be water (hydrothermal) (or)
methanol, toluene, cyclohexane, etc.
•The function of the template is to provide nucleating sites of
desired size & shape around which nanoparticle can grow.
•The sol is stirred, aged and converted into a gel.
•The gel is placed in an autoclave. Autoclave is tightly closed &
heated in an oven at a controlled rate up to a temperature above the
boiling point of the solvent.
•Temperature & pressure created by the super-heated solvent
vapours and the action of the reducing agent convert the starting
material to the nanocrystals.
•After sometime, the product crystals are collected on a filter,
washed and dried.
(1)stainless steel autoclave
(2)precursor solution
(3)Teflon liner
(4)stainless steel lid
Advantages of solvothermal method:

•Single crystals can be grown.

•Autoclave can be fitted with baffle stirrers to control the

growth of crystals.

•High yield

•Nanoparticle can be prepared at relatively low

temperature.
PREPARATION OF NANOWIRES:

•Preparation of nanowires by Electrospinning method:

Electrospinning is suitable for the preparation of

nanowires and nanofibers of polymers, ceramics &
composite materials.
•PREPARATION OF NANOWIRES:

Principle
When a high voltage is applied to a polymer fluid taken
in a syringe, charges are induced within the fluid. When
the charges within the fluid reach a critical amount, the
fluid can overcome the surface tension forces and hence is
ejected as a jet from the tip of the needle, forming a
Taylor cone. This jet is allowed to travel to a region of
lower potential where a grounded collector in the form of
a drum or sheet is placed. The jet solidifies into
nanofibers or nanowires of desired dimensions.
Procedure
A pipette with a syringe is filled with the chosen polymer
fluid. Two electrodes are fitted - one to the syringe and
another to the collector. When a high DC voltage in kV
range is applied to the fluid, a jet of nanofibers is ejected.
Factors that influence electro spinning are:

•Nature & viscosity of polymer fluids

•Applied voltage
•Temperature
•Needle diameter
•Flow rate
•Needle to collector distance
Advantages
1. Uniform nanofibers and nanowires can be prepared.
2. High product purity.
3. Highly aligned fibers can be prepared.
Preparation of nanowires by elecrodeposition method:

Principle
A porous metal oxide acts as a cathode as well as a
template. On electrolysis, metal from metal salt solution
get deposited into the porous of the cathode. When the
cathodic template is dissolved, the deposited nanowires
can be separated.
Procedure
A porous template of alumina with desired pore
dimension is made as the cathode. A thin film of silver or
gold is deposited onto it by evaporation. On electrolysis,
the metal from the electrolytic solution gets deposited in
the pores of the alumina template. On dissolution of
alumina, individual nanowires are released.
Advantages
•Easy to operate and low cost
•Densely packed continuous nanowires are obtained.
The aspect ratio of metal nanowires can be easily
controlled
 Applications of Nanomaterials
• Medicine
• Agriculture
• Electronics
• Catalysis
 Nanomedicine
Nanotechnology provides a wide range of new technologies for
developing customized solutions that optimize the delivery of
pharmaceutical products. Today, harmful side effects of treatments
such as chemotherapy are commonly a result of drug delivery methods
that don't pinpoint their intended target cells accurately. Researchers
at Harvard and MIT, however, have been able to attach
special RNA strands, measuring nearly 10 nm in diameter, to nano-
particles, filling them with a chemotherapy drug. These RNA strands
are attracted to cancer cells. When the nanoparticle encounters a
cancer cell, it adheres to it, and releases the drug into the cancer
cell. This directed method of drug delivery has great potential for
treating cancer patients while avoiding negative effects (commonly
associated with improper drug delivery)
 Nano Chemistry for... Gadgets
1956, IBM launched the 305
RAMAC, the first “SUPER”
computer with a hard disk drive
(HDD). The HDD weighed over a
ton and stored 5 MB of data.

hard disk drive sizes have changed

since the ‘80s until today, an old 8-
inch drive all the way down to
today’s 3.5-inch, 2.5-inch and 1.8-
inch drives.
Nano Chemistry for... Gadgets
"There's Plenty of Room at the Bottom" was a
lecture given by physicist Richard Feynman at
an American Physical Society meeting
at Caltech on December 29, 1959. Feynman
considered the possibility of direct manipulation of
individual atoms as a more powerful form of
synthetic chemistry than those used at the time.
The talk went unnoticed and did not inspire the
conceptual beginnings of the field. In the 1990s it
was rediscovered and published as a seminal event
in the field, probably to boost the history of
nanotechnology with Feynman's reputation
TEM (a, b, and c) images of prepared mesoporous silica nanoparticles with mean outer
diameter: (a) 20nm, (b) 45nm, and (c) 80nm. SEM (d) image corresponding to (b). The
insets are a high magnification of mesoporous silica particle.
The Nobel Prize in Chemistry 2016 is awarded to Jean-Pierre Sauvage, Sir J.
Fraser Stoddart and Bernard L. Feringa for their design and production of
molecular machines. They have developed molecules with controllable
movements, which can perform a task when energy is added.
 Nanorobotics

Nanorobotics is the emerging technology field creating machines or robots whose

components are at or close to the scale of a nanometer (10−9 meters). More
specifically, nanorobotics refers to the nanotechnology engineering discipline of
designing and building nanorobots, with devices ranging in size from 0.1–10
micrometers and constructed of nanoscale or molecular components.[ The
names nanobots, nanoids, nanites, nanomachines or nanomites have also been used
to describe these devices currently under research and development.
Diode:
The nanotube is used here to connect two
electrodes (yellow) on a silicon dioxide base (green)
[Diodes allow a current to travel in one direction only]
Bacteria can be used to carry drugs, DNA or sensors attached
to nanoparticles into cells for treatment, gene therapy or
diagnosis.
Replacing Antibiotics
Scanning Electron Microscopy (SEM)
 Outline

• What can we use a SEM for?

• How do we get an image?
• Electron beam-sample interactions
• Signals that can be used to characterize the
microstructure
– Secondary electrons
– Backscattered electrons
– X-rays
• Components of the SEM
• Some comments on resolution
• Summary
 The most versatile instrument for a
materials scientist?
What can we study in a SEM? “Easy” sample
preparation!!
• Topography and morphology
“Big” samples!

Morphology studies the shape, texture and distribution of materials at a

surface, The shape and size of a line, an area, or a volume, the distribution
of phases in a system (material)

; whereas topography focuses on the quantitative dimensional

measurement of features on a surface (study of surface of materials)
The instrument in brief
SEM block diagram
• electron gun (filament)
• electromagnetic optics
• scan coils
• sample stage
• detectors
• vacuum system
• computer hardware and
software (not trivial!!)
• How does SEM work?
• To obtain a high-resolution image, an electron source
(also known as an electron gun) emits a stream of high-
energy electrons towards a sample. The electron beam is
focused using electromagnetic lenses. Once the focused
stream reaches the sample, it scans its surface in a
rectangular raster.
• The interaction between the electron beam and the
sample creates secondary electrons, backscattered
electrons, and X- rays. These interactions are captured
to create a magnified image.
How do we get an image?
215868eelleeccttrroonnss!!

Electron gun

Detector

Image
 Electron guns

• We want many electrons per

time unit per area (high current
density) and as small electron
spot as possible
• Traditional guns: thermionic
electron gun (electrons are
emitted when a solid is heated)
– W-wire, LaB6-crystal
• Modern: field emission guns
(FEG) (cold guns, a strong
electric field is used to extract
electrons)
– Single crystal of W, etched to a
thin tip
 Electron guns
• With field emission guns we get a smaller spot
and higher current densities compared to
thermionic guns
• Vacuum requirements are tougher for a field
emission guns

Single crystal of LaB6 Tungsten wire Field emission tip

 Detectors
Backscattered electron
detector:
(Solid-State Detector)

Secondary electron detector:

(Everhart-Thornley)
 Our traditional detectors
• Secondary electrons: Everhart-Thornley
Detector
• Backscattered electrons: Solid State
Detector
• X-rays: Energy dispersive spectrometer
(EDS)

MENA3100
 Electron beam-sample interactions
• The incident electron beam is scattered in the sample,
both elastically and inelastically
• This gives rise to various signals that we can detect
(more on that on next slide)
• Interaction volume increases with increasing acceleration
voltage and decreases with increasing atomic number

MENA3100
Images: Smith College Northampton, Massachusetts
 Signals from the sample
Incoming electrons
Secondary electrons
Auger electrons
Backscattered Cathodo-
electrons luminescence (light)

X-rays

Sample
Where does the signals come from?

•Diameter of the interaction

volume is larger than the
electron spot
 resolution is poorer than the
size of the electron spot
 Secondary electrons (SE)
• Generated from the collision
between the incoming electrons
and the loosely bonded outer
electrons
• Low energy electrons (~10-50 eV)
• Only SE generated close to
surface escape (topographic
information is obtained)
• Number of SE is greater than the
number of incoming electrons
• We differentiate between SE1 and
SE2
 SE1

• The secondary electrons that are

generated by the incoming electron beam
as they enter the surface
• High resolution signal with a resolution
which is only limited by the electron beam
diameter
 SE2
• The secondary electrons that are generated by the
backscattered electrons that have returned to the surface
after several inelastic scattering events
• SE2 come from a surface area that is bigger than the spot
from the incoming electrons  resolution is poorer than for
SE1 exclusively
SE2
Incoming electrons
Sample surface
 Backscattered electrons (BSE)

• A fraction of the incident

electrons is retarded by the
electro-magnetic field of the
nucleus and if the scattering
angle is greater than 180 ° the
electron can escape from the
surface
 Backscattered electrons (BSE)

• High energy electrons (elastic scattering)

• Fewer BSE than SE
• We differentiate between BSE1 and BSE2
 BSE2

• Most BSE are of BSE2 type

BSE2
Incoming electrons
Sample surface
 Why do we need vacuum?
• Chemical (corrosion!!) and thermal stability
is necessary for a well-functioning
filament (gun pressure)
– A field emission gun requires ~ 10-10 Torr
– LaB6: ~ 10-6 Torr
• The signal electrons must travel from the
sample to the detector (chamber pressure)
– Vacuum requirements is dependant of the
type of detector
 Summary
• Signals:
– Secondary electrons (SE): mainly
topography
• Low energy electrons, high resolution
• Surface signal dependent on curvature
– Backscattered electrons (BSE): mainly
chemistry
• High energy electrons
• “Bulk” signal dependent on atomic number
– X-rays: chemistry
• Longer recording times are needed

MENA3100
 Topography and morphology

• High depth of focus

 Depth of focus
Optical microscopy vs SEM

Screw length: ~ 0.6 cm

Images: the A to Z of Materials

• A SEM typically has orders of magnitude better

depth of focus than a optical microscope making
SEM suitable for studying rough surfaces
• The higher magnification, the lower depth of focus
 Chemistry Images: Harald Fjeld, UiO

Ce

Fe Sr
Blood Clot
SEM image of a fly's eye
Pollen from a variety of common plants including the sunflower, primrose
and lily
Butterfly Wing Scales
a plant leaf stem in cross section
blue cheese
 Transmissions Electron Microscopy (TEM)

Part I:
The microscope
Sample preparation
Imaging/Contrast
Part II: Diffraction
Defects
Part III

Spectroscopy
•What is TEM?
TEM can stand for Transmission Electron
Microscopy or Transmission Electron Microscope
(TEM). A TEM is a type of electron microscope that
uses a broad beam of electrons to create an image of
a sample’s internal structure. A beam of electrons is
transmitted through a sample, creating an image that
details a sample’s morphology, composition, and
crystal structure.
TEM
Condenser lens:
Converges the beam to a spot –
spot size (beam diameter) and
convergence angle

Objective lens (before and after

specimen):
Image formation (inverts image)
and magnification

Intermediate lens:
Magnifies the initial image that is
formed by the objective lens
-- Image or diffraction mode
Projector lens:
Controls the magnification

TEM block diagram

 The Transmission Electron Microscope

•Electrons scatter when they pass through thin

sections of a specimen
•Characterization of materials crystal structure
and microstructure simultaneously by diffraction
and imaging techniques.
•Denser regions in specimen, scatter more electrons
and appear darker
•Transmitted electrons (those that do not scatter)
are used to produce image
Samples must be incredibly thin, often less than 150 nm
thick, to allow electrons to pass through them. After the
transmission of the electrons through the sample, they
arrive at a detector below and a 2-D image is created.

TEMs have an incredible magnification potential of

10-50 million times.The details provided are at the
atomic level, the highest resolution of any electron
microscope. TEMs are often used to examine
molecular and cellular structures
Microscope outline
Electron gun

illumination Condenser lenses

Condenser aperture

Sample holder Objective aperture

Objective lens
Selected area aperture
Intermediate lens
Magnification
Projector lenses

Fluorescent screen

Gatan Imaging Filter

For EELS
Imaging
Parallel incoming electron beam

Sample

sample
Objective lens

Diffraction plane
(back focal plane)

Image plane
Electron source / Filament

1. Thermionic emission:
• W or LaB6
• Robust
• Relatively cheap
• Does not requite ultra high vacuum

2. Field emission

• Cold FEG, ZrO/W or Schottky FEG

• High brightness
• Require high vacuum,
Polymers

Technology for a better society 16

Technology for a better society 22
 Diffraction Pattern in TEM

Ring Kikuchi Spot CBED

Pattern Pattern Pattern Pattern
 Transmission Electron Microscopes (TEM)
Scanning Electron Microscopes (SEM)

Electron stream Fine, focused beam Broad beam

Image taken Topographical/surface Internal structure

Resolution Lower resolution Higher resolution

Magnification Up to 2,000,000 times Up to 50,000,000 times

Image dimension 3-D 2-D

Sample thickness Thin and thick samples okay Ultrathin samples only

Penetrates sample No Yes

Sample restriction Less restrictive More restrictive

Sample preparation Less preparation required More preparation required

Cost Less expensive More expensive

Speed Faster Slower

Operation Easy to use More complicated; requires training