Advanced Characterization Techniques for Nanomaterials

and their Applications

A Seminar Report

Submitted for

Partial fulfilment for the Degree of

Masters of Science in Chemistry

Supervised By Submitted By
Dr. Trapti Gupta Rashi Bala Vyas
Associate Professor IISU/2022/ADM/34580
Dept. of Chemistry M.Sc. (Chem.) Sem-I

DEPARTMENT OF CHEMISTRY

IIS (Deemed to be University), JAIPUR

2022-2023
 IIS (Deemed to be University), Jaipur

CERTIFICATE

This is to certify that Rashi Bala Vyas of M.Sc. (Chemistry) Sem. 1, has been
supervised by Dr. Trapti Gupta for her seminar and the report has been submitted
by her.

SUPERVISOR

Dr. Trapti Gupta

Associate Professor
Department of Chemistry
 ACKNOWLEDGEMENT

I would like to acknowledge and express my sincere gratitude towards my teacher, Dr.
Trapti Gupta for introducing me to this Seminar project and for incepting the idea of
how to proceed with the same.

It would not have been a successful project if not for the worthy inputs given by my
mentor, my friends and the Department of Chemistry, IISU. I am deeply thankful for
their kind cooperation and help.

Rashi Bala Vyas

 Content
Introduction............................................................................................................................................1

Classification of nanomaterials..............................................................................................................1

1) Natural & Artificial nanomaterials..........................................................................................1

2) Fullerenes and Nanoparticles..................................................................................................2

3) Intentionally Produced Nanomaterials....................................................................................3

Importance of nontechnology in chemical analysis...............................................................................4

History of nanotechnology.....................................................................................................................5

Techniques of Nanotechnology in Chemical Analysis...........................................................................6

1. Transmission Electron Microscopy (TEM).................................................................................7

2. Scanning Electron Microscopy (SEM).......................................................................................7

3. Auger Electron Spectroscopy (AES)..........................................................................................8

4. X-ray Photoelectron Spectroscopy..............................................................................................9

5. X-ray Fluorescence Spectroscopy...............................................................................................9

6. Atomic Force Microscope (AFM)............................................................................................10

7. Single-particle ICP-MS.............................................................................................................11

8. X-ray Absorption Fine Structure...............................................................................................12

9. Capillary Electrophoretic Separations.......................................................................................12

10. Magnetic Nano Particles and HPLC......................................................................................13

11. Dynamic Light Scattering (DLS)..........................................................................................13

12. Zeta potential.........................................................................................................................14

Application...........................................................................................................................................15

Everyday Materials and Processes...................................................................................................15

Electronics and IT Applications.......................................................................................................17

Medical and Healthcare Applications..............................................................................................18

Energy Applications.........................................................................................................................19

Environmental Remediation.............................................................................................................20
 Foods and bio actives.......................................................................................................................21

Biosensor..........................................................................................................................................22

Challenges and future directions..........................................................................................................23

Safety, Health & Welfare implications for nanomaterials................................................................23

 Risk Assessment........................................................................................................................23

 Control Measures......................................................................................................................24

Nanotechnology Challenges, Risks and Ethics................................................................................24

Future Opportunities and Challenges...............................................Error! Bookmark not defined.

Conclusion............................................................................................................................................26

Reference..............................................................................................................................................28
 Advanced Characterization Techniques for Nanomaterials
and their Applications1

Introduction
Nanotechnology is science, engineering, and technology conducted at the nanoscale, which is about
1 to 100 nanometres.

Nanoscience and nanotechnology are the study and application of extremely small things and can be
used across all the science fields, such as chemistry, biology, physics, materials science, and
engineering.

Nanotechnology can increase the surface area of a material. This allows more atoms to interact with
other materials. An increased surface area is one of the chief reasons nanometer-scale materials can
be stronger, more durable, and more conductive than their larger-scale (called bulk) counterparts.

Nanotechnology is not microscopy. "Nanotechnology is not simply working at ever smaller

dimensions," the National Nanotechnology Initiative says. "Rather, working at the nanoscale enables
scientists to utilize the unique physical, chemical, mechanical, and optical properties of materials that
naturally occur at that scale."

Scientists study these properties for a range of uses, from altering consumer products such as clothes
to revolutionizing medicine and tackling environmental issues.1

Classification of nanomaterials
There are different types of nanomaterials, and different ways to classify them.

1) Natural & Artificial nanomaterials

a) Natural nanomaterials, as the name suggests, are those that occur naturally in the world.
These include particles that make up volcanic ash, smoke, and even some molecules in our
bodies, such as the haemoglobin in our blood. The brilliant colours of a peacock’s feathers are
the result of spacing between nanometer-scale structures on their surface.
b) Artificial nanomaterials are those that occur from objects or processes created by people.
Examples include exhaust from fossil fuel burning engines and some forms of pollution. But

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 while some of these just happen to be nanomaterials—vehicle exhaust, for instance, was not
developed as one—scientists and engineers are working to create them for use in industries
from manufacturing to medicine. These are called intentionally produced nanomaterials.2

2) Fullerenes and Nanoparticles

This classification includes both naturally occurring and man-made nanomaterials.

1. Fullerenes are allotropes of carbon. Allotropes are different molecular forms of the same
element. The most familiar carbon allotropes are probably diamond and graphite, a type
of coal.

Fullerenes are atom-thick sheets of another carbon allotrope, graphene, rolled into spheres or
tubes.

The most familiar type of spherical fullerene is probably the buckminsterfullerene,

nicknamed the buckyball. Buckyballs are nanometer-sized carbon molecules shaped like
soccer balls—tightly bonded hexagons and pentagons.

Buckyballs are very stable—able to withstand extreme temperatures and pressure. For this
reason, buckyballs are able to exist in extremely harsh environments, such as outer space. In
fact, buckyballs are the largest molecules ever discovered in space, detected around planetary
nebula in 2010.

Buckyballs’ cage-like structure seems to protect any atom or molecule trapped within it.
Many researchers are experimenting with "impregnating" buckyballs with elements, such as
helium. These impregnated buckyballs may make excellent chemical "tracers," meaning
scientists could follow them as they wind through a system. For example, scientists could
track water pollution kilometres away from where it entered a river, lake, or ocean.

Tubular fullerenes are called nanotubes. Thanks to the way carbon atoms bond to each other,
carbon nanotubes are remarkably strong and flexible. Carbon nanotubes are harder than
diamond and more flexible than rubber.

Carbon nanotubes hold great potential for science and technology. NASA, for example, is
experimenting with carbon nanotubes to produce "blacker than black" coloration on satellites.
This would reduce reflection, so data collected by the satellite are not "polluted" by light.2

2. Nanoparticles can include carbon, like fullerenes, as well as nanometer-scale versions of

many other elements, such as gold, silicon, and titanium. Quantum dots, a type of

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 nanoparticle, are semiconductors made of different elements, including cadmium and sulphur.
Quantum dots have unusual fluorescent capabilities. Scientists and engineers have
experimented with using quantum dots in everything from photovoltaic cells (used for solar
power) to fabric dye.

The properties of nanoparticles have been important in the study of nanomedicine. One
promising development in nanomedicine is the use of gold nanoparticles to fight lymphoma,
a type of cancer that attacks cholesterol cells. Researchers have developed a nanoparticle that
looks like a cholesterol cell, but with gold at its core. When this nanoparticle attaches to a
lymphoma cell, it prevents the lymphoma from "feeding" off actual cholesterol cells, starving
it to death.2

3) Intentionally Produced Nanomaterials

There are four main types of intentionally produced nanomaterials: carbon-based, metal-
based, dendrimers, and nanocomposites.

i) Carbon-based nanomaterials are intentionally produced fullerenes. These include

carbon nanotubes and buckyballs.

Carbon nanotubes are often produced using a process called carbon assisted vapor
deposition. (This is the process NASA uses to create its "blacker than black" satellite
color.) In this process, scientists establish a substrate, or base material, where the
nanotubes grow. Silicon is a common substrate. Then, a catalyst helps the chemical
reaction that grows the nanotubes. Iron is a common catalyst. Finally, the process requires
a heated gas, blown over the substrate and catalyst. The gas contains the carbon that
grows into nanotubes.

ii) Metal-based nanomaterials include gold nanoparticles and quantum dots.

Quantum dots are synthesized using different methods. In one method, small crystals of
two different elements are formed under high temperatures. By controlling the
temperature and other conditions, the size of the nanometer-scale crystals can be carefully
controlled. The size is what determines the fluorescent colour. These nanocrystals are
quantum dots—tiny semiconductors—suspended in a solution.

iii) Dendrimers are complex nanoparticles built from linked, branched units. Each dendrimer
has three sections: a core, an inner shell, and an outer shell. In addition, each dendrimer

3
 has branched ends. Each part of a dendrimer—its core, inner shell, outer shell, and
branched ends—can be designed to perform a specific chemical function.

Dendrimers can be fabricated either from the core outward (divergent method) or from
the outer shell inward (convergent method).

Like buckyballs and some other nanomaterials, dendrimers have strong, cage-like cavities
in their structure. Scientists and researchers are experimenting with dendrimers as multi-
functional drug-delivery methods. A single dendrimer, for example, may deliver a drug to
a specific cell, and also trace that drug's impact on the surrounding tissue.

iv) Nanocomposites combine nanomaterials with other nanomaterials, or with larger, bulk
materials. There are three main types of nanocomposites: nanoceramic matrix composites
(NCMCs), metal matrix composites (MMCs), and polymer matrix composites (PMCs).

NCMCs, sometimes called nanoclays, are often used to coat packing materials. They
strengthen the material’s heat resistance and flame-retardant properties.

MMCs are stronger and lighter than bulk metals. MMCs may be used to reduce heat in
computer "server farms" or build vehicles light enough to airlift.

Industrial plastics are often composed of PMCs. One promising area of nanomedical
research is creating PMC "tissue scaffolding." Tissue scaffolds are nanostructures that
provide a frame around which tissue, such as an organ or skin, can be grown. This could
revolutionize the treatment of burn injuries and organ loss.2

Importance of nontechnology in chemical analysis

There are typically two main applications for nanotechnology in analytical chemistry. The first is to
analyse nano-scale material and the second is to use nanotechnology for analysis and in
spectroscopic imagine. Spectroscopic instrumentation and other scanning microscopy techniques
supplement the information provided by other techniques such as electron microscopy, atomic force
microscopy, and scanning tunnelling microscopy to help characterize the structure and function of
molecules and chemical or biological objects.

Furthermore, nanotechnology has developed materials that have led to new analytical techniques.

Due to the complexity of the chemical and biological information within biological systems, it is
often thought that a combination of different instruments should be used to capture the full

4
complexity of the system, especially for chemical imaging. The main challenge in using such
instrumentation is translating the nanoscale methods into medically or biologically relevant tools. 3

History of nanotechnology
American physicist Richard Feynman is considered
the father of nanotechnology. He introduced the
ideas and concepts behind nanotech in a 1959 talk
titled "There’s Plenty of Room at the Bottom."
Feynman did not use the term "nanotechnology," but
described a process in which scientists would be
able to manipulate and control individual atoms and
molecules.

Modern nanotechnology truly began in 1981, when

Fig1.Physicist Richard Feynman, the father of
nanotechnology. the scanning tunnelling microscope allowed
scientists and engineers to see and manipulate
individual atoms. IBM scientists Gerd Binnig and
Heinrich Rohrer won the 1986 Nobel Prize in Physics for inventing the scanning tunnelling
microscope. The Binnig and Rohrer Nanotechnology Centre in Zurich, Switzerland, continues to
build on the work of these pioneering scientists by conducting research and developing new
applications for nanotechnology.

The iconic example of the development of nanotechnology was an effort led by Don Eigler at IBM to
spell out "IBM" using 35 individual atoms of xenon.

By the end of the 20th century, many companies and governments were investing in nanotechnology.
Major nanotech discoveries, such as carbon nanotubes, were made throughout the 1990s. By the
early 2000s, nanomaterials were being used in consumer products from sports equipment to digital
cameras.

Modern nanotechnology may be quite new, but nanometre-scale materials have been used for
centuries.

As early as the 4th century, Roman artists had discovered that adding gold and silver to glass created
a startling effect: The glass appeared slate green when lit from the outside, but glowed red when lit
from within. Nanoparticles of gold and silver were suspended in the glass solution, colouring it. The
most famous surviving example of this technique is a ceremonial vessel, the Lycurgus Cup.

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Artists from China, western Asia, and Europe were also using nanoparticles of silver and copper, this
time in pottery glazes. This gave a distinctive "luster" to ceramics such as tiles and bowls.

In 2006, modern microscopy revealed the technology of "Damascus steel," a metal used in South
Asia and the Middle East until the technique was lost in the 18th century—carbon nanotubes. Swords
made with Damascus steel are legendary for their strength, durability, and ability to maintain a very
sharp edge.

One of the most well-known examples of pre-modern use of nanomaterials is in

European medieval stained-glass windows. Like the Romans before them, medieval artisans knew
that by putting varying, small amounts of gold and silver in glass, they could produce bright reds and
yellows.4

Techniques of Nanotechnology in Chemical Analysis

For characterization of nano materials, a numberof researches have been conducted. Among them,
summarizes the Engineered NanoMaterials (ENMs) in foods and the suitability ofexisting
instrumentation for identification andquantification. The recent advances in thedevelopment of
electrochemical sensors andbiosensors are based on the click chemistryfictionalization. There is
development ofnovel drug delivery systems using nano particles. The nano-based analytical methods
havebeen developed to control analytes of interest infoods. As studied by Enisa and Mirjana.Modern
techniques were developed to meet the different requirements in food inspection furthermore,
(Kanchi et al. 2014) reported that,there is novel routes in the development of newnano materials
which are used for the detectionof organic and inorganic pollutants. The small size and large surface
area to volumeratio of nanomaterials results in increased ratesof oxidation and subsequent
dissolutioncompared to larger-scale forms of silver.Researchers had assessed the problem ofselecting
the suitable method for the preparationof nano particles. Nano sensors contribute tothe specificity,
sensitivity, and performance of themethods and improved by using nano materialsfor their
construction. Thenanotechnology-based biosensor or nano biosensor technology is revolutionizing
the healthcare industry such as the nano biosensortechnology which is used in the measurement
ofmetabolites, monitoring of diabetes forensicmedicine, homeland security.
Additionally,methodologies used to characterize thecomposition, morphology and
biologicalproperties of synthesized nano particles bymultiple techniques have been
presented.Different researchers reviewed that, analyticaltools are deleveraged and applied togenerate
predictive modelling determinationsduring development. Techniques for predictive in vivo
information include those that measuresurface chemistry at nano, micro, and macroscales for both

6
inorganic and organic particles. Structural characterization is essentialfor nanomaterials research.
Posth et al.have assessed common magnetic nano particleanalytical techniques under various criteria
inorder to define the methods that can be used aseither standard technique for magnetic particle
orthose that can be used to obtain acomprehensive picture of a magnetic nanoparticle system. 5

1. Transmission Electron
Microscopy(TEM)
Materials that have dimensions
small enough to be electron
transparent, such as powders or
nano tubes, can be quickly
produced by the deposition of a
dilute sample containing the
specimen onto support grids. The
electron microscope uses
electrostatic and electromagnetic
"lenses" to control the electron
beam and focus it to form an image. Researchers have been used a technique whereby a beam of
electrons is transmitted through an ultra-thin-specimen and interacts as passes through the

Fig2 TEM Schematic diagram

sample. An image is formed from
the electrons transmitted through
the specimen, magnified and focused by an objective lens and appears on imaging screen. It is
sensitive to extended crystal lattice defects. The specimens must be prepared as a thin foil so that
the electron beam can penetrate.6

2. Scanning Electron Microscopy (SEM)

This technique creates magnified images
using electrons instead of light waves.When
the beam of electrons interacts with the
atoms of the sample, signals in the form of
secondary electrons, back scattered
electrons and characteristic X- rays are
generated that contain information about the

Fig3 SEM Setup sample’s surface topography, composition

etc. It can also produce very high-resolution
7
images of a sample surface,revealing details about 1-5 nm in size in its primary detection mode
i.e., secondary electron imaging. Detectors collect these X rays, back scattered electrons, and
secondary electrons and convert them into a signal that is sent to a screen similar to a television
screen.6

Fig.4System of detectors in connection with a scanning transmission

electron microscope
3. Auger Electron Spectroscopy (AES)
In this technique, after an inner shell excitation which can be caused by a collision with a primary
electron that has an atom in an energy level above its ground state. The atom returns to its ground
state by filling the empty level created,with an electron from a higher energy level and this leads
to the release of energy and momentum. It uses a primary electron beam to probe the surface of a
sample. The electron impact results in a disturbance of the sample in a region of about 1- 3μm
depth, leading to the emission of secondary electrons, back scattered electrons, Auger electrons
and characteristic X-rays. It focuses only on the small part of secondary electrons that are emitted
because ofthe auger process. The identity and quantity of the elements are determined from the
kinetic energy and intensity of the auger peaks, which occur at specific kinetic energies in the
auger-spectrum. To separate and locate the auger peaks from the intense background of scattered
electrons the signal is deviated. It is used to quantify and qualify the
elements.5

8
 Fig.5 AESSchematic Diagram

4. X-ray Photoelectron Spectroscopy

XPS is used to determine the elements
and the quality of those elements that
are present within~ 10 nm of the
sample surface. It also detects the
contamination, if any, exists in the
surface or the bulk of the sample. If the
material is free of excessive surface
contamination, XPS can generate
empirical formula of the sample and
the chemical state of one or more of
the elements can be identified. It can
be also used to determine the thickness
of one or more thin layers (1-8 nm) of
different materials within the top 10
Fig. 6 X-ray PhotoelectronSpectroscopySchematic
nm of the surface. It can also measure the
Diagram
uniformity of elemental composition of
textile surfaces after nano level etching, finishing, or coating of the surfaces.5

5. X-ray Fluorescence Spectroscopy

It is similar to XPS in terms of the excitationmechanism but differs in its detection mechanism.
While XPS detects photoelectrons, XFSdetects “secondary” or “fluorescent” X-rays froma
material that has been excited by high-energyX-rays (or sometimes γ-rays). Theprinciple behind
XFS is relatively straightforward.When a material is exposed to high energy X-rays, ionization or
electron ejection can takeplace if the X-ray photon energy is greater thanits ionization energy.
Due to the high energy ofX-rays or γ-rays, tightly bound electrons in theinner, low energy
orbitals of the atom in thematerial can be expelled. The resulting ionisedatom is not unstable and

9
electrons in outer,higher energy orbitals may fall or make atransition into the lower orbital to fill
the hole leftbehind. In doing so, energy may be released inthe form of a photon usually with
energy in the X-ray region still with energy equal to the energydifference of the two orbitals
involved. The X-rays penetrates up to a depth of about 1-10 μm.Only photo-ionised electrons of
the first atomiclayers (1-10 μm) can leave the solid withoutsignificance energy loss, pass an
electrostaticenergy analyser and reach the electron detector.The measured kinetic energy of
thes8ephotoelectrons depends on the photonenergyand the binding energy of the atomic orbital
fromwhich the electrons originate.5

Fig.7 X-Ray fluorescence

spectroscopy schematic diagram

6. Atomic Force Microscope (AFM)

AFM is an ideal
for quantitatively
measuring the
nanometer scale
surface roughness
and for
visualizing the
surface nano-
texture on many
types of material surfaces
Fig.8 Atomic force microscope
including polymer nano
composites and nano finished or nano-coated textiles. In AFM a probe consisting of a sharp tip
(nominal tip radius is in the order of 10nm) located near the end of a cantilever beam is raster

10
scanned across the surface of a specimen using piezoelectric scanners. Changes in the tip-
specimen interaction are often monitored using an optical lever detection system, in which a laser
is reflected off the cantilever and onto a position sensitive photo diode. AFM can be used to
explore the nano structures, properties,surfaces, and interfaces of fibres and fabrics. For example,
structural characteristics of nano fibre materials and nano level surface modification. For non-
conductive nano materials, AFMis a better choice for analyses Bennig et al. 1986.5

7. Single-particle ICP-MS
Mitrano et al, reported
that, due to
itssensitivity, flexibility,
and analytical speed,
ICP-MS performed in
single-particle mode
(SP-ICP-MS) is gaining
Fig.9 Schematic diagram of particle transport from sample to ICP-MS popularity for detecting
interface and resulting time-resolved signal generated by the mass
andmeasuring
spectrometer.
inorganic-based
engineered nanomaterials (ENM), as traditional inductivelycoupled plasma mass spectroscopy
(ICP-MS) already does, but with the important distinctionthat single-particle mode has the ability
to detecta difference between ionic and whole-ENMelemental sources (Andrea et al. 2015). In
single-particle mode, ENMs are introduced into an ICPand completely ionised, with the resulting
ionsbeing detected by a mass spectrometer. Toensure that only a single particle is measured,the
sample has to be diluted to have temporalresolution between particles that only a singleparticle is
introduced into the plasma at a time.The mass spectrometer must also be capable ofmaking
extremely rapid measurements to ensureENM detection (data should be acquired at leastevery
100 μs) as the transient signal of a 50-nmgold nano particle can vary, on average, between600
and 800 μs depending on the instrumentoperating conditions and ion optics design.5

8. X-ray Absorption Fine Structure

XAFS is used to
measure the fine
structure of an
analyte near the
absorption edge

11

Fig.10 Schematic diagram of X-ray absorption Fine Structure

when subjectedto X-ray radiation. It is similar to UV-visibleelectronic absorption spectroscopy, in
principle,except that the spectral range is in the X-rayregion and electronic-XAFS focuses on the
finestructure specifically since it provides localstructural information about specific atoms orions.
EXAFS relates to the details of how X-rays are absorbed by an atom at energies near andabove the
core-level binding energies of thatatom. EXAFS measurements reflect themodulation of an atom’s X-
ray absorptionprobability due to the chemical and physical .states of the atom. EXAFS spectra are
especially sensitive to the formal oxidation state, coordination chemistry, and the local atomic
structure of the selected element. One advantage of EXAFS is that it works for crystalline as well as
non-crystalline or even highly disordered materials, including solutions.5

9. Capillary Electrophoretic Separations

Yang-Wei Lin et al. (2005) had used Capillaryelectrophoresis (CE) and microchip
capillaryelectrophoresis (MCE).These are two of the mostpowerful techniques for the analysis of
DNA.They reported about DNA separation using chip-based nanostructures and nano materials
in CEand MCE. Based on the dependence of themobility of DNA molecules on the size and
shapeof nanostructures, several unique chip-baseddevices have been developed for the
separationof DNA, particularly for long DNA molecules.Unlike conventional CE and MCE
methods,sieving matrices are not required when usingnanostructures.7

10. Magnetic
Nano
Particles
and HPLC
Laleh et al.
(2017) had
used a micro

Fig.11 Schematic representation of Capillary electrophoretic separation

extractionmethod using Ag
modified-magnetic nanoparticle
(Ag-MNPs) coupled with
Fig.12 HPLC instrumentation highperformance liquid
chromatography (HPLC) fordetermination of ceftriaxone in plasma. Theyhad synthesized
magnetic nano particles via amild solution route. The prepared nano particleswere modified with
a thin layer of silver andcharacterized with different methods such as X-ray diffraction (XRD),

12
transmission electronmicroscopy (TEM), FTIR and ultraviolet-visible (UV-Vis) spectroscopy.
Effect of severalparameter such as pH of donor and acceptancephase, amount of magnetic
particle andextraction and desorption time were optimized.They reported that, under the optimal
conditionthe enrichment factor was obtained. Thedetection limit was 0.02 mg/mL and a wide
linearrange from 0.06 to 40 μg/mL were obtained.5

11. Dynamic Light Scattering (DLS)

Sovan et al. reviewed that currently, thefastest and most
popular method of determiningparticle size is photon-correlation spectroscopy(PCS) or dynamic
light scattering (DLS). DLS iswidely used to determine the size of Browniannano particles in
colloidal suspensions in thenano and submicron ranges. Shining monochromatic light (laser) onto
a solution ofspherical particles in Brownian motion causes aDoppler shift when the light hits the
movingparticle, changing the wavelength of theincoming light. This change is related to the
sizeof the particle. It is possible to extract the
Fig. 13 DLS instrumentation
sizedistribution and give a description of the
particle’smotion in the medium, measuring the diffusioncoefficient of the particle and using
theautocorrelation function. The photon correlationspectroscopy (PCS) represents the
mostfrequently used technique for accurate estimationof the particle size and size distribution
based onDLS (EPA).5

12. Zeta potential

Zeta potential (also known as the electrokinetic potential) is a measure of the “effective” electric
charge on the nanoparticle surface, and quantifies the charge stability of colloidal nanoparticles.
When a nanoparticle has a net surface charge, the charge is “screened” by an increased
concentration of ions of opposite charge near the
nanoparticle surface. This layer of oppositely
charged ions moves with the nanoparticle, and
together the layer of surface charge and oppositely
charged ions are referred to as the electrical double
layer. The Zeta Potential is a measure of the
difference in potential between the bulk fluid in
which a particle is dispersed and the layer of fluid
containing the oppositely charged ions that is
associated with the nanoparticle surface. Particles

Fig. 14 Zeta potential diagram

13
 with a positive Zeta Potential will bind to negatively charged surfaces, and vice versa. The
magnitude of the Zeta Potential provides information about particle stability, with higher
magnitude potentials exhibiting increased electrostatic repulsion and therefore increased stability.

0-5 mV: Particles tend to agglomerate or aggregate

5-20 mV: Particles are minimally stable

20-40 mV: Particles are moderately stable

40+ mV: Particles are highly stable

It is important to consider that the magnitude of the charge on the nanoparticle surface depends
on the solution pH. In fact, the surface charge can be reduced to zero at a specific pH referred to
as the isoelectric point.

Zeta potential is measured by adding a solution to a cell that contains two gold electrodes. When
a voltage is applied to the electrode, the particles will move towards the electrode with the
opposite charge. A Doppler technique is used to measure the particle velocity as a function of
voltage. A laser passes through the cell and as particles move through the laser beam the intensity
of scattered light fluctuates at a frequency proportional to the particle speed. Particle speed at
multiple voltages is measured, and this data is used to calculate the zeta potential.

At nanoComposix, Zeta Potential measurements are performed using a Malvern Zetasizer Nano
ZS instrument equipped with a HeNe laser operating at 632.8 nm and a scattering detector at 173
degrees.8

Application
Everyday Materials and Processes
Many benefits of nanotechnology depend on the fact that it is possible to tailor the structures of
materials at extremely small scales to achieve specific properties, thus greatly extending the
materials science toolkit.

Using nanotechnology, materials can effectively be made stronger, lighter, more durable, more
reactive, more sieve-like, or better electrical conductors, among many other traits. Many everyday
commercial products are currently on the market and in daily use that rely on nanoscale materials
and processes:

14
 Nanoscale additives to or surface treatments of fabrics can provide lightweight ballistic
energy deflection in personal body armor, or can help them resist wrinkling, staining, and
bacterial growth.
 Clear nanoscale films on eyeglasses, computer and camera displays, windows, and other
surfaces can make them water- and residue-repellent, antireflective, self-cleaning, resistant to
ultraviolet or infrared light, antifog, antimicrobial, scratch-resistant, or electrically
conductive.
 Nanoscale materials are beginning to enable washable, durable “smart fabrics” equipped with
flexible nanoscale sensors and electronics with capabilities for health monitoring, solar
energy capture, and energy harvesting through movement.
 Lightweighting of cars, trucks, airplanes, boats, and space craft could lead to significant fuel
savings. Nanoscale additives in polymer composite materials are being used in baseball bats,
tennis rackets, bicycles, motorcycle helmets, automobile parts, luggage, and power tool
housings, making them lightweight, stiff, durable, and resilient. Carbon nanotube sheets are
now being produced for use in next-generation air vehicles. For example, the combination of
light weight and conductivity makes them ideal for applications such as electromagnetic
shielding and thermal management.

Fig.15 High-resolution image of a polymer-silicate nanocomposite. This material has improved thermal,
mechanical, and barrier properties and can be used in food and beverage containers, fuel storage tanks for
aircraft and automobiles, and in aerospace components. (Image courtesy of NASA.)

Nano-bioengineering of enzymes is aiming to enable conversion of cellulose from wood

chips, corn stalks, unfertilized perennial grasses, etc., into ethanol for fuel. Cellulosic

15
 nanomaterials have demonstrated potential applications in a wide array of industrial sectors,
including electronics, construction, packaging, food, energy, health care, automotive, and
defence. Cellulosic nanomaterials are projected to be less expensive than many other
nanomaterials and, among other characteristics, tout an impressive strength-to-weight ratio.
 Nano-engineered materials in automotive products include high-power rechargeable battery
systems; thermoelectric materials for temperature control; tires with lower rolling resistance;
high-efficiency/low-cost sensors and electronics; thin-film smart solar panels; and fuel
additives for cleaner exhaust and extended range.
 Nanostructured ceramic coatings exhibit much greater toughness than conventional wear-
resistant coatings for machine parts. Nanotechnology-enabled lubricants and engine oils also
significantly reduce wear and tear, which can significantly extend the lifetimes of moving
parts in everything from power tools to industrial machinery.
 Nanoparticles are used increasingly in catalysis to boost chemical reactions. This reduces the
quantity of catalytic materials necessary to produce desired results, saving money and
reducing pollutants. Two big applications are in petroleum refining and in automotive
catalytic converters.
 Nano-engineered materials make superior household products such as degreasers and stain
removers; environmental sensors, air purifiers, and filters; antibacterial cleansers; and
specialized paints and sealing products, such a self-cleaning house paints that resist dirt and
marks.
 Nanoscale materials are also being incorporated into a variety of personal care products to
improve performance. Nanoscale titanium dioxide and zinc oxide have been used for years in
sunscreen to provide protection from the sun while appearing invisible on the skin.9

Electronics and IT Applications

Nanotechnology has greatly contributed to major advances in computing and electronics, leading to
faster, smaller, and more portable systems that can manage and store larger and larger amounts of
information. These continuously evolving applications include:

 Transistors, the basic switches that enable all modern computing, have gotten smaller and
smaller through nanotechnology. At the turn of the century, a typical transistor was 130 to
250 nanometres in size. In 2014, Intel created a 14-nanometer transistor, then IBM created
the first seven nanometer transistor in 2015, and then Lawrence Berkeley National Lab

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 demonstrated a one nanometer transistor in 2016! Smaller, faster, and better transistors may
mean that soon your computer’s entire memory may be stored on a single tiny chip.
 Using magnetic random-access memory (MRAM), computers will be able to “boot” almost
instantly. MRAM is enabled by nanometer‐scale magnetic tunnel junctions and can quickly
and effectively save data during a system shutdown or enable resume‐play features.
 Ultra-high-definition displays and televisions are now being sold that use quantum dots to
produce more vibrant colours while being more energy efficient.
 Flexible, bendable, foldable, rollable, and stretchable electronics are reaching into various
sectors and are being integrated into a variety of products, including wearables, medical
applications, aerospace applications, and the Internet of Things. Flexible electronics have
been developed using, for example, semiconductor nanomembranes for applications in
smartphone and e-reader displays. Other nanomaterials like graphene and cellulosic
nanomaterials are being used for various types of flexible electronics to enable wearable and
“tattoo” sensors, photovoltaics that can be sewn onto clothing, and electronic paper that can
be rolled up. Making flat, flexible, lightweight, non-brittle, highly efficient electronics opens
the door to countless smart products.
 Other computing and electronic products include Flash memory chips for smart phones and
thumb drives; ultra-responsive hearing aids; antimicrobial/antibacterial coatings on keyboards
and cell phone casings; conductive inks for printed electronics for RFID/smart cards/smart
packaging; and flexible displays for e-book readers.
 Nanoparticle copper suspensions have been developed as a safer, cheaper, and more reliable
alternative to lead-based solder and other hazardous materials commonly used to fuse
electronics in the assembly process.9

Medical and Healthcare Applications

Nanotechnology is already broadening the medical tools, knowledge, and therapies currently
available to clinicians. Nanomedicine, the application of nanotechnology in medicine, draws on the
natural scale of biological phenomena to produce precise solutions for disease prevention, diagnosis,
and treatment. Below are some examples of recent advances in this area:

 Commercial applications have adapted gold nanoparticles as probes for the detection of
targeted sequences of nucleic acids, and gold nanoparticles are also being clinically
investigated as potential treatments for cancer and other diseases.

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 Better imaging and diagnostic tools enabled by nanotechnology are paving the way for earlier
diagnosis, more individualized treatment options, and better therapeutic success rates.
 Nanotechnology is being studied for both the diagnosis and treatment of atherosclerosis, or
the build-up of plaque in arteries. In one technique, researchers created a nanoparticle that
mimics the body’s “good” cholesterol, known as HDL (high-density lipoprotein), which helps
to shrink plaque.
 The design and engineering of advanced solid-state nanopore materials could allow for the
development of novel gene sequencing technologies that enable single-molecule detection at
low cost and high speed with minimal sample preparation and instrumentation.
 Nanotechnology researchers are working on a number of different therapeutics where a
nanoparticle can encapsulate or otherwise help to deliver medication directly to cancer cells
and minimize the risk of damage to healthy tissue. This has the potential to change the way
doctors treat cancer and dramatically reduce the toxic effects of chemotherapy.
 Research in the use of nanotechnology for regenerative medicine spans several application
areas, including bone and neural tissue engineering. For instance, novel materials can be
engineered to mimic the crystal mineral structure of human bone or used as a restorative resin
for dental applications. Researchers are looking for ways to grow complex tissues with the
goal of one day growing human organs for transplant. Researchers are also studying ways to
use graphene nanoribbons to help repair spinal cord injuries; preliminary research shows that
neurons grow well on the conductive graphene surface.
 Nanomedicine researchers are looking at ways that nanotechnology can improve vaccines,
including vaccine delivery without the use of needles. Researchers also are working to create
a universal vaccine scaffold for the annual flu vaccine that would cover more strains and
require fewer resources to develop each year.9

Fig.16 This image shows the bamboo-like structure of nitrogen-doped carbon nanotubes for the treatment of
cancer. (Courtesy of Wake Forest and the National Cancer Institute)

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Energy Applications
Nanotechnology is finding application in traditional energy sources and is greatly enhancing
alternative energy approaches to help meet the world’s increasing energy demands. Many scientists
are looking into ways to develop clean, affordable, and renewable energy sources, along with means
to reduce energy consumption and lessen toxicity burdens on the environment:

 Nanotechnology is improving the efficiency of fuel production from raw petroleum materials
through better catalysis. It is also enabling reduced fuel consumption in vehicles and power
plants through higher-efficiency combustion and decreased friction.
 Nanotechnology is also being applied to oil and gas extraction through, for example, the use
of nanotechnology-enabled gas lift valves in offshore operations or the use of nanoparticles to
detect microscopic down-well oil pipeline fractures.
 Researchers are investigating carbon nanotube “scrubbers” and membranes to separate
carbon dioxide from power plant exhaust.
 Researchers are developing wires containing carbon nanotubes that will have much lower
resistance than the high-tension wires currently used in the electric grid, thus reducing

Fig.17 New solar panel films incorporate

transmission power loss.
 Nanotechnology
nanoparticles to create lightweight, can
flexible solar cells. efficiently, promising inexpensive solar power in the
future. Nanostructured solar cells could be cheaper to manufacture and easier to install, since
they can use print-like manufacturing processes and can be made in flexible rolls rather than
discrete panels. Newer research suggests that future solar converters might even be
“paintable.”
 Nanotechnology is already being used to develop many new kinds of batteries that are
quicker-charging, more efficient, lighter weight, have a higher power density, and hold
electrical charge longer.
 An epoxy containing carbon nanotubes is being used to make windmill blades that are longer,
stronger, and lighter-weight than other blades to increase the amount of electricity that
windmills can generate.
 In the area of energy harvesting, researchers are developing thin-film solar electric panels that
can be fitted onto computer cases and flexible piezoelectric nanowires woven into clothing to
generate usable energy on the go from light, friction, and/or body heat to power mobile
electronic devices. Similarly, various nanoscience-based options are being pursued to convert
waste heat in computers, automobiles, homes, power plants, etc., to usable electrical power.

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  Energy efficiency and energy saving products are increasing in number and types of
application. In addition to those noted above, nanotechnology is enabling more efficient
lighting systems; lighter and stronger vehicle chassis materials for the transportation sector;
lower energy consumption in advanced electronics; and light-responsive smart coatings for
glass.9

Environmental Remediation
In addition to the ways that nanotechnology can help improve energy efficiency (see the section
above), there are also many ways that it can help detect and clean up environmental contaminants:

 Nanotechnology could help meet the need for affordable, clean drinking water through rapid,
low-cost detection and treatment of impurities in water.
 Engineers have developed a thin film membrane with nanopores for energy-efficient
desalination. This molybdenum disulphide (MoS2) membrane filtered two to five times more
water than current conventional filters.
 Nanoparticles are being developed to clean industrial water pollutants in ground water
through chemical reactions that render the pollutants harmless. This process would cost less
than methods that require pumping the water out of the ground for treatment.
 Researchers have developed a nano fabric "paper towel" woven from tiny wires of potassium
manganese oxide that can absorb 20 times its weight in oil for clean-up applications.
Researchers have also placed magnetic water-repellent nanoparticles in oil spills and used
magnets to mechanically remove the oil from the water.
 Many airplanes cabin and other types of air filters are nanotechnology-based filters that allow
“mechanical filtration,” in which the fibre material creates nanoscale pores that trap particles
larger than the size of the pores. The filters also may contain charcoal layers that remove
odours.
 Nanotechnology-enabled sensors and solutions are now able to detect and identify chemical
or biological agents in the air and soil with much higher sensitivity than ever before.
Researchers are investigating particles such as self-assembled monolayers on mesoporous
supports (SAMMS™), dendrimers, and carbon nanotubes to determine how to apply their
unique chemical and physical properties for various kinds of toxic site remediation. Another
sensor has been developed by NASA as a smartphone extension that firefighters can use to
monitor air quality around fires.9

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Foods and bio actives
Archaeosomes are a type of microbial lipid membrane resistant to oxidation, chemical and enzymatic
hydrolysis, low pH, high temperature, and the presence of bile salts due to the hostile living
environment of Archaea microbes (Mozafari 2006). Canham (2007) found that the milk protein α-
lactalbumin in certain conditions can undergo self-assembly to form tubular nanostructures. Such
tubes are thousands of nanometres long, their diameter is 20 nm, and the inner cavity diameter is
about 8 nm. These structures are formed in several stages. In the first stage, α-lactalbumin is partially
hydrolysed through the activity of a protease from Bacillus licheniformis. Also, along with other
components, several derivatives with molecular masses varying from 10 to 14 kDa are formed. In the
presence of calcium ions, this mixture self-assembles into helical tubes. Nano cochleates resulting
from soy and calcium have been found to be suitable for the nano-encapsulation of vitamins, omega-
3 fatty acids, and lycopene without affecting the organoleptic properties of foods (Joseph and
Morrison 2006). Dairy products, beverages cereals, and bread are now supplemented with minerals,
vitamins, bioactive peptides, probiotics, plant sterols, and antioxidants. Some of these active
components are being added to foods as nanoparticles or particles of a few hundred nm in size
(Shelke 2008). Gupta and Gupta (2005) demonstrated that nanometer-sized particles could be
produced using food-grade biopolymers, e.g., polysaccharides or proteins, by inducing phase
separation in mixed biopolymer systems, self-association, or aggregation. Nanoparticles are added to
various foods to increase flow properties, colour, and stability during processing, or shelf-life. For
example, aluminosilicate materials are typically used as anticaking agents in powdered processed
foods, whereas anatase titanium dioxide is a normal food whitener and brightener additive employed
in sweets, some cheeses, and sauces (Ashwood et al. 2007). The applications explored here were
particularly chosen because they are the most likely nanofood products to be accepted by consumers
in the short term. Thus, food nanotechnology is still young, and the future of this exciting field is still
largely uncertain. Regardless of how applications of nanotechnology in the food sector are ultimately
marketed, governed, or perceived by the public, it seems clear that the manipulation of matter on the
nanoscale will continue to yield exciting and unforeseen products.9

Biosensor
Biosensors can be used to monitor environmental pollution in air, soil, water, etc.; toxic elements in
food and quality control; biohazardous bacteria or virus, and biomolecules for clinical diagnostics,
etc.; and to necessitate sensitive, fast, and selective equipment or tools. Biosensors have immense
potential due to their inherent simplicity, low cost, fast analysis, and miniaturization, as well as easy
handling. Biosensors have been predicted to have applications in military, health care, industrial

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process control, environmental monitoring, food control, and microbiology—bacterial and viral
studies, etc. Researchers and scientists define a “bio-sensor” in different ways.

A biosensor is an analytical electronic device that generates an electronic signal by receptor–target

analyte interactions. The main component in a biosensor is a bioreceptor or biologically derived
sensing element that is either intimately connected or integrated with a physicochemical transducer.
The function of a biosensor is to produce a digital electronic signal that is directly proportional to the
concentration of a target biomolecules. According to the International Union of Pure and Applied
Chemistry definition, “a biosensor is a self-contained integrated device that is capable of providing
specific quantitative or semi-quantitative analytical information using a biological recognition
element (receptor) which is in direct spatial contact with a transducer element”. In 1962, Clark and
Lyons first fabricated an electrochemical biosensor by immobilizing glucose oxidase (GOD) enzyme
molecules on the surface of an oxygen electrode to detect glucose concentration. In the presence of
GOD, glucose is converted to gluconic acid and produces two electrons and two protons resulting in
a reduction of GOD (oxidized). Again, electrons, protons, oxygen, and reduced GOD react to
produce hydrogen peroxide and GOD (oxidized). The increased hydrogen peroxide or reduction of
oxygen content can be correlated with the glucose quantity.9

Challenges and future directions

Safety, Health & Welfare implications for nanomaterials
 Exposure & monitoring

A key aspect of any risk assessment of hazardous substances is assessing its exposure.
Therefore, it is essential to understand whether and how people may be exposed to
nanomaterials in their daily lives, including at work and at home.

Evaluation of occupational exposure has traditionally been carried out using qualitative and
quantitative tools. However, conventional sampling and detection methods for carrying out
occupational hygiene monitoring may not be adequate for nanomaterial sampling and
detection. Monitoring methods are under review by research organisations and other institutes
such as the Health & Safety Executive (UK) and the National Institute for Occupational
Safety and Health (US) (NIOSH).10

 Risk Assessment
Grouping of nanomaterials based on their physical structure and their classification is
recommended for risk assessment. The following grouping criteria are suggested:

22
  Fibrous nanomaterials (i.e., insoluble and of a high aspect ratio)
 Nanomaterials from CMR substances (i.e., the larger form particle of the substance is already
classified as a carcinogenic, mutagenic or reproductive toxin)
 Insoluble nanomaterials (i.e., insoluble or poorly soluble nanomaterials, but not fibrous or a
CMR)
 Soluble nanomaterials (i.e., soluble nanomaterials not fibrous or a CMR)

As with any chemical substance, inhalable and poorly soluble nanomaterials in addition to
nanomaterials derived from known CMR substances represent the greatest concern. Nano-
sized materials in general have an increased capacity to reach and interact with tissues in the
body, potentially enhancing any adverse effects on health.10

 Control Measures
Although many uncertainties remain, there is concern about the safety and health hazards of
nanomaterials. Therefore, employers together with workers must apply a precautionary
approach to risk management and the choice of prevention measures.10

Nanotechnology Challenges, Risks and Ethics

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.

Closely related to the knowledge barrier is the technical barrier. In order for the incredible
predictions regarding nanotechnology to come true, we have to find ways to mass produce nano-size
products like transistors and nanowires. While we can use nanoparticles to build things like tennis
rackets and make wrinkle-free fabrics, we can't make really complex microprocessor chips with
nanowires yet.

There are some hefty social concerns about nanotechnology too. Nanotechnology may also allow us
to create more powerful weapons, both lethal and non-lethal. Some organizations are concerned that

23
we'll only get around to examining the ethical implications of nanotechnology in weaponry after
these devices are built. They urge scientists and politicians to examine carefully all the possibilities
of nanotechnology before designing increasingly powerful weapons.

If nanotechnology in medicine makes it possible for us to enhance ourselves physically, is that

ethical? In theory, medical nanotechnology could make us smarter, stronger and give us other
abilities ranging from rapid healing to night vision. Should we pursue such goals? Could we continue
to call ourselves human, or would we become transhuman -- the next step on man's evolutionary
path? Since almost every technology starts off as very expensive, would this mean we'd create two
races of people -- a wealthy race of modified humans and a poorer population of unaltered people?
We don't have answers to these questions, but several organizations are urging nano scientists to
consider these implications now, before it becomes too late.11

Future Opportunities and Challenges

In the future, the field of Advanced Characterization Techniques for Nanomaterials holds tremendous
opportunities for innovation across various sectors, including medicine, electronics, cosmetics, and
materials. However, the widespread use of nanomaterials also brings forth concerns regarding their
potential risks to the environment and human health. Addressing these challenges and seizing the
opportunities requires a comprehensive approach.

One of the key challenges is ensuring that economies lacking a strong science base can effectively
compete and adapt to the development of nanotechnology. This includes overcoming obstacles such
as limited industry infrastructure, difficulty in translating investments into economic outcomes, high
costs associated with acquiring intellectual property rights and establishing nanotech infrastructure.
Additionally, factors like low average incomes, limited government spending on investment and
healthcare, and trade barriers contribute to the complexities faced by less developed countries in
adopting and implementing nanotechnology.

Another significant challenge lies in the absence of a comprehensive standards infrastructure, data
repository, and regulatory framework for nanotechnologies on a global scale. The lack of protocols
for risk assessment and life cycle analysis further deters the adoption of nanotechnology in less
developed countries. Furthermore, the scarcity of tools for quality assurance, hazard evaluation, and
risk mitigation compounds the challenges associated with the safe and responsible use of
nanomaterials.

24
In the realm of nanomedicine, there are specific technical challenges that need to be addressed. These
include the development of virus-like systems for intracellular applications, the design of bio-
mimetic polymers, precise control of sensitive drug delivery, efficient drug targeting mechanisms,
and the creation of bio-responsive triggered systems. Additionally, extensive research is being
conducted on drug delivery formulations and dispersions containing nano-sized components.

To overcome these challenges and harness the potential of Advanced Characterization Techniques for
Nanomaterials, concerted efforts are needed. This includes fostering collaborations between
academia, industry, and governments to strengthen the scientific base, promoting knowledge sharing
and capacity building initiatives, establishing regulatory frameworks and standards, and investing in
research and development. Moreover, it is crucial to prioritize ethical considerations, risk
assessment, and environmental sustainability in the advancement of nanotechnology.

By addressing these challenges and embracing the opportunities, the field of Advanced
Characterization Techniques for Nanomaterials can unlock groundbreaking advancements, transform
industries, and contribute to the betterment of society as a whole.

Conclusion
The field of nanotechnology is rapidly gaining global recognition due to its diverse applications.
Nanomaterials, with their unique properties in one or three dimensions at the nanoscale, exhibit
characteristics that are distinct from both bulk materials and molecular compounds. The synthesis of
nano materials plays a crucial role in the development of analytical methods aimed at characterizing
these nanostructures accurately. Nanotechnology has vast potential for application in various fields,
including but not limited to pharmaceutical development, drug delivery systems, biosensing, food
security, and quality assurance. It is important to acknowledge that nanotechnology continues to
evolve and open up new avenues for scientific exploration and innovation.

Furthermore, the ability to manipulate and control nanomaterials at the atomic and molecular levels
provides opportunities for breakthroughs in areas such as energy storage, electronics, environmental
remediation, and medical diagnostics. The precise characterization techniques discussed in this
report, including microscopy, spectroscopy, and surface analysis, enable researchers to understand
the structure, composition, and behavior of nanomaterials with exceptional detail.

As nanotechnology progresses, it is essential to consider the ethical implications and potential

environmental impacts associated with the manufacturing, use, and disposal of nanomaterials.

25
Continued research and development of advanced characterization techniques will facilitate better
understanding, regulation, and responsible implementation of nanotechnology in various industries.

In summary, nanotechnology's growing significance is fuelled by its potential to revolutionize

numerous sectors, providing innovative solutions to enhance life and sustainability. By leveraging
advanced characterization techniques, scientists and engineers can unlock the full potential of
nanomaterials and pave the way for a future filled with groundbreaking applications.

26
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