Synthesis of nanoparticles: Classification, characterization,

and their application

Nanotechnology is science, engineering, and technology conducted at the nanoscale (about 1 to
100 nanometers). The term Nano is derived from the Greek word “dwarf” and is usually
combined with a noun to form words such as nanometer, nanobot and nanotechnology.
Nanobot: Nanobots are robots that are microscopic in nature, measured largely on the scale of
nanometers. They are currently in the research and developments phase, but on realization they
are expected to do specific tasks at the atomic, molecular and cellular levels and help in bringing
about breakthroughs, especially in engineering science and medical science.
Nanobots are also known as nanomachines, nanorobots, nanomites,

nanites or nanoids.
NANO CAN REFER TO TECHNOLOGIES, MATERIALS, PARTICLES, OBJECTS-WE
ARE FOCUSING ON NANOMATERIALS AS THESE ARE ALREADY BEING USED IN
WORK PLACES MORE WIDELY.
Examples: A sheet of paper is about 100,000 nanometers thick, a human hair is
around 80,000-100,000 nanometers wide.
A nanometer is defined as one-billionth of a meter. Since it is not easy to visualize the scale of a
nanometer, a comparison with concepts and objects of appreciable dimensions is helpful. To get
a perspective of the scale used in nanotechnology, representative structure and materials found in
nature are typically referenced to have the following dimension:
Examples of Biological Structures Dimension in Nanometers (nm)
Leukocytes 10,000 nm
Bacteria 1,000-10,000 nm
Virus 75-100 nm
Protein 5-50 nm
DNA(width) 2 nm
Atom 0.1 nm

Nanoparticles have unique chemical and physical properties as compared to their solid
bulk materials because of their
High surface area
High surface to volume ratio
Defects level/surface defects/embedded defects
 Absorbing behavior
Frictional properties
Conductivity behavior
Electronic properties
Classification of Nanoparticles
The nanoparticles are generally classified into the organic, inorganic and carbon based.
Organic nanoparticles:
Dendrimers, micelles, liposomes and ferritin, etc. are commonly knows the organic
nanoparticles or polymers.
These nanoparticles are biodegradable, non-toxic, and some particles such as micelles and liposomes
has a hollow core (Fig. 1), also known as nanocapsules and are sensitive to thermal and
electromagnetic radiation such as heat and light.
The drug carrying capacity, its stability and delivery systems, either entrapped drug or adsorbed drug
system determines their field of applications and their efficiency apart from their normal
characteristics such as the size, composition, surface morphology, etc. The organic nanoparticles are
most widely used in the biomedical field for example drug delivery system as they are efficient and
also can be injected on specific parts of the body that is also known as targeted drug delivery.

Fig. 1: Organic nanoparticles: a – Dendrimers, b – Liposomes and c – micelles.

Inorganic nanoparticles:
Inorganic nanoparticles are particles that are not made up of carbon. Metal and metal
oxide based nanoparticles are generally categorized as inorganic nanoparticles.
Metal based: Nanoparticles that are synthesized from metals to nanometric sizes either by
destructive or constructive methods are metal based nanoparticles. Almost all the metals can
be synthesized into their nanoparticles. The commonly used metals for nanoparticle synthesis
are aluminium (Al), cadmium (Cd), cobalt (Co), copper (Cu), gold (Au), iron (Fe), lead (Pb),
silver (Ag) and zinc (Zn).
Metal oxides based: The metal oxide based nanoparticles are synthesized to modify the
properties of their respective metal based nanoparticles, for example nanoparticles of iron (Fe)
instantly oxidizes to iron oxide (Fe2O3) in the presence of oxygen at room temperature that
increases its reactivity compared to iron nanoparticles. The commonly synthesized are
Aluminium oxide (Al2O3), Cerium oxide (CeO2), Iron oxide (Fe2O3), Magnetite (Fe3O4),
Silicon dioxide (SiO2), Titanium oxide (TiO2), Zinc oxide (ZnO). These nanoparticles have
possessed exceptional properties when compared to their metal counterparts.
Carbon based:
The nanoparticles made completely of carbon are knows as carbon based. They can be
classified into fullerenes, graphene, carbon nano tubes (CNT), carbon nanofibers and carbon
black and sometimes activated carbon in nano size and are presented in Fig. 2.
Fullerenes: Fullerenes (C60) are a carbon molecule that is spherical in shape and made up of
carbon atoms held together by sp2 hybridization. About 28 to 1500 carbon atoms form the
spherical structure with diameters up to 8.2 nm for a single layer and 4 to 36 nm for multi-
layered fullerenes.
Graphene: Graphene is an allotrope of carbon. Graphene is a hexagonal network of honey
comb lattice made up of carbon atoms in a two dimensional planar surface. Generally the
thickness of the graphene sheet is around 1 nm.
Carbon Nano Tubes (CNT): Carbon Nano Tubes (CNT), a graphene nanofoil with a honey
comb lattice of carbon atoms is wound into hollow cylinders to form nanotubes of diameters as
low as 0.7 nm for a single layered and 100 nm for multi-layered CNT and length varying from
a few micrometres to several millimetres. The ends can either be hollow or closed by a half
fullerene molecule.
Carbon Nanofiber: The same graphene nanofoils are used to produce carbon nanofiber as
CNT but wound into a cone or cup shape instead of a regular cylindrical tubes.
Carbon black: An amorphous material made up of carbon, generally spherical in shape with
diameters from 20 to 70 nm. The interactions between the particles are so high that they bound
in aggregates and around 500 nm agglomerates are formed.
Fig. 2: Carbon based nanoparticles: a – fullerenes, b – graphene, c – carbon nanotubes, d – carbon
nanofibers and e – carbon black
Synthesis of Nanoparticles:
The nanoparticles are synthesized by various methods that are categorized into bottom-up or
top-down method. A simplified representation of the process is presented in Figure3.

Top-down method:
Top-down or destructive method is the reduction of a bulk material to nanometric scale
particles. Mechanical milling, nanolithography, laser ablation, sputtering and thermal
decomposition are some of the most widely used nanoparticle synthesis methods.
– Chips and processors
 Bottom-up method:
Bottom-up or constructive method is the build-up of material from atom to clusters to nanoparticles.
Sol-gel, spinning, chemical vapor deposition (CVD), pyrolysis and biosynthesis are the most
commonly used bottom-up methods for nanoparticle production.
– Nanoparticles such as C60, carbon nanotubes, quantum dots

Scheme 1: Synthesis of Au and Ag Nanoparticles

Applications:
These materials have been utilized in electrochemistry, photochemical, and biomedicine.
Nanoparticles have many functional platforms that can be utilized forimaging and
therapeutic functions.
High drug loading capacity and stability.
Studies of metal nano particles:
Metal nanoparticles (NPs) in the range of one to a few hundred nanometers are stated to have
novel magnetic, electronic and optical properties dependent on their shape, size and composition.
Characterization Tools [Structural, morphological and optical]
• XRD
• FESEM-EDS
• AFM
• TEM
• DLS
• UV-Vis spectrophotometry and
• Photoluminescence
Importance of Gold Nanoparticles
There are a number of advantages to the use of Au-NPs, particularly in
biological systems including the following:
1) Bind readily to sulfhydryl groups which allow for simple NP functionalization by the
conjugation of various biomolecules and other ligands
2) Resistant to oxidation
3) Possess surface plasmons (in some cases multiple plasmon peaks depending on their
morphology)
4) Biocompatible
5) Size tunable
6) Electron dense due to the high atomic number of gold, making the Au-NPs easily identifiable
by analysis with electron-microscopes and
7) Laser illumination of the particles results in an increase in particle temperature due to energy
absorption by the surface plasmons.
8) Nanoparticles are good therapeutic agents due to their ease transport in the diseased cell and
carrier-loading drug.
9) Colloidal Au/NPs have the very small size to introduce in the tissues and cells of biological
molecules such as proteins and DNA.
10) Because of their electronic properties, Au/NPs have been commonly utilized in analytical
methods and used as an electrode in an electrochemical sensor of different samples.
Nature of Gold nanoparticles
The gold nanoparticles properties are the wine-red solution. The interactions of gold
nanoparticles play an important role in their properties. There are different sizes of gold
nanoparticles start from 1 nm to 8 µm, and various shapes; for example, spherical ring, sub-
octahedral, icosahedral tetrahedral, decahedral, octahedral, nanorods etc. have been observed.
These shapes depend upon the nature of solvents and the other reaction conditions at the time of
preparation.

Importance of Silver nanoparticles

There are a number of advantages to the use of Ag-NPs, particularly in the
practical applications as well as medicinal fields in the following ways:
1) The potential of Ag/NPs has been widely utilized in nano-medicine, drug delivery, cosmetics,
electronic application, and environmentalprotection.
2) Ag/NPs have special chemical and physical properties, such as surface enhanced Raman
scattering and optical behavior, electrical conductivity, high thermal, chemical stability,
nonlinear, and catalytic activity.
3) Ag/NPs are commonly used in the antimicrobial field to treatment microbes such as fungi,
virus, and bacteria.
4) Due to their proven antimicrobial properties, Ag/NPs are widely used in the daily used
commercial products; Ag/NPs are used in different applications, such as colloidal coating, and in
paints, or in a solid material such as polymer scaffolds.
5) In addition, Ag/NPs used in textile industry, where Ag/NPs are utilized in the filtration
membranes of water due to the slow release rate of the membrane to be utilized as a protective
bulk head against different bacteria and other microbes present in the water.
Synthesis of Gold and Silver Nanoparticles
Different methods have been used to synthesize gold and silver nanoparticles. The techniques
used for the preparation of nanoparticles involved biological, physical, and chemical methods.

Bare nanoparticles cannot exist?

Because of high tendency to agglomerate to change their size and shapes and starts
distortion from the nano dimensions. Use of protective layers or capping agents on to the
bare nano particles so that the interactions between the adjacent particles have been
minimized to avoid agglomeration tendency. Usually macro ligands like polyethers,
polyamines, polyphenols, polythiols, alkylated amines, surfactants are used as stabilizer
during preparation or after the preparation as protective agents.
֍ The preparation of Au and Ag-NPs by the chemical method is based
on three factors:
(a) Stabilizing agents (b) Reducing agents and (c) Au and Ag precursors (d)
Physiochemical conditions
By Chemical methods: Gold nanoparticles
Au/NPs can be grown in encapsulated immersed in polyethyl eneglycol dendrimers and reduced
by formaldehyde under near infrared rays. The dendrimers/Au nanoparticles can be prepared by
the reduction of a solution of HAuCl4 and sodium borohydride. The synthesis of Au/NPs with
size less than 10 nm can be by two various thiols involved ethylene glycol and dodecanethiol.
By Chemical methods: Silver nanoparticles
The chemical methods are important to synthesize of Ag-NPs because of the simplicity of
preparation in aqueous solution. Monodisperse silver nanocubes were prepared by polyol
process, by using a polyvinyl pyrrolidone (PVP) polymer with AgNO3 in the presence of
ethylene glycol as reducing agent. On the other hand, monodispersed Ag-NPs were prepared by
using AgNO3, oleylamine, and liquid paraffin. Oleylamine-paraffin was utilized to control
temperature and liquid paraffin was utilized in avoiding the solvents.
 ☻ The factors like metal precursor, pH, temperature, and reducing agents for the
synthesis of Au and Ag/NPs can be utilized by HAuCl4 and AgNO3 and
sodium borohydride and trisodium citrate as reducing and stabilizing agents.

Preparation and assembly of Au NPs and Au@Ag NPs

Au-NPs and bimetallic core shell Au@Ag NPs have designed by three-step process
in the following manner:
Citrate stabilized Au-NPs with diameter of 3.5 nm were prepared by adding NaBH4 (0.1
M, 0.3 mL) solution into 10 mL of HAuCl4 (0.25 μM) and sodium citrate (0.25 μM) aqueous
solution. The resultant solution was stirred for 2 min and stored at ambient temperature for 3 h.
Au-NPs with diameter of 8 nm were subsequently prepared by adding 5.0 mL of the
obtained Au-NP (3.5 nm) solution into the mixture of HAuCl4 (10 mM, 1.125 mL), ascorbic acid
aqueous solution (0.1 M, 0.25 mL) and CTAC solution (80 mM, 45 mL), which was stirred for
10 min. Au-NPs with diameter of 19 nm were prepared by employing these 8 nm Au-NPs as the
seeds following the same protocol as the previous growth step. The average diameter of the
obtained Au-NPs was 19.0 ± 0.9 nm based on the TEM images.
Au@Ag NPs were prepared by coating the prepared 19 nm Au-NPs with Ag shells.
Briefly, 19 nm Au-NPs (0.75 nM, 2 mL) were washed and re-dispersed in CTAC solution (80
mM, 10 mL) before adding ascorbic acid (0.1 M, 0.3 mL) and AgNO3 (10 mM, 0.1 mL) under
vigorous stirring. The resultant solution was then kept at 60 °C for 1 h. Au@Ag NPs were
formed, indicated by the change of the color of solution from wine red to orange yellow. The
thickness of Ag shells was estimated to be 3.5 ± 0.3 nm based on the TEM images. Au-NPs (26
nm) were prepared by using a similar protocol for the synthesis of Au@Ag NPs, but HAuCl4 was
used instead of AgNO3.
Conclusion:
Nanotechnology is improving our everyday lives by enhancing the performance and efficiency of
everyday objects. It provides a clean environment by providing safer air and water, and clean
renewable energy for a sustainable future. Nanotechnology has gained a wide attention where
more investment is made for the research and development by top institutions, industries and
organizations. Nanotechnology has established to be an advanced field of science where
extensive research is carried out to implement the technology. It is being tested for various new
applications to increase the efficiency and performance of the object or process and subsequently
reduce the cost so that it is accessible for everyone. The nanotechnology has a great future due to
its efficiency and environmental friendly property.