Seminar On Methods of Synthesis of

Nanoparticles

Chapter 01
INTRODUCTION
Nanotechnology refers to the creation and utilization of materials whose constituents
exist at the nanoscale; and, by convention, be up to 100 nm in size. Nanotechnology explores
electrical, optical, and magnetic activity as well as structural behavior at the molecular and
submolecular level. It has the potential to revolutionize a series of medical and biotechnology
tools and procedures so that they are portable, cheaper, safer, and easier to administer.
Nanoparticles are being used for diverse purposes, from medical treatments, using in various
branches of industry production such as solar and oxide fuel batteries for energy storage, to wide
incorporation into diverse materials of everyday use such as cosmetics or clothes, optical
devices, catalytic, bactericidal, electronic, sensor technology, biological labelling and treatment
of some cancers. Due to their exceptional properties including antibacterial activity, high
resistance to oxidation and high thermal conductivity, nanoparticles have attracted considerable
attention in recent years. Nanoparticles can be synthesized chemically or biologically. Metallic
nanoparticles that have immense applications in industries are of different types, namely, Gold,
Silver, Alloy, magnetic etc.

The man in his quest for knowledge has been conceiving and developing physical world
and its components in bigger than the biggest and smaller than the smallest dimensions of mass,
length and time. Though the smallest entity with individual characteristic features that was
established happened to be an atom of an element but realization of the single atom in physical
form and serving mankind remained a dream till recently. It is achieved through the development
of nanocrystaline materials, discovery of concept of quantum confined atom and synthesis of
doped nanocrystaline materials. Investigation of growth mechanism of nanoparticles is present
large scientific and practical interest. As, nanoparticles with given size and characteristics are
required in nanotechnology. Nanoparticles growth mechanism determines distribution function
of nanoparticles on size, physical-chemical properties of nanoparticles medium and etc. Because
of, known of growth mechanism give possibility control of preparation of nanoparticles and to
obtain nanoparticles with given parameters (mean diameter, standard deviation, coefficient

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polydispersity and other) and characteristics (magnetic moment). Nanoparticles growth

mechanism is enough complex process and depended from many conditions (temperature,
viscosity, concentration of medium and etc.). Conditions determinant of nanoparticle growth are
changed in the dependence on method preparation of nanoparticles. Materials scientists and
engineers have made significant developments in the improvement of methods of synthesis of
nanomaterial solids. A brief review is given in this article.

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Chapter 02
ROLE OF TOP DOWN & BOTTOM UP
APPROACHES IN NANOTECHNOLOGY

Fig 2.1: Schematic representation of the building up of Nanostructures.

There are two approaches for synthesis of nano materials and the fabrication of nano
structures. Top down approach refers to slicing or successive cutting of a bulk material to get
nano sized particle. Bottom up approach refers to the buildup of a material from the bottom:
atom by atom, molecule by molecule or cluster by cluster.

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Both approaches play very important role in modern industry and most likely in nano
technology as well. There are advantages and disadvantages in both approaches.

Attrition or Milling is a typical top down method in making nano particles, whereas the
colloidal dispersion is a good example of bottom up approach in the synthesis of nano particles.

The biggest problem with top down approach is the imperfection of surface structure and
signicant crystallographic damage to the processed patterns. These imperfections which in turn
leads to extra challenges in the device design and fabrication. But this approach leads to the bulk
production of nano material. Regardless of the defects produced by top down approach, they will
continue to play an important role in the synthesis of nano structures.

Though the bottom up approach oftenly referred in nanotechnology, it is not a newer

concept. All the living beings in nature observe growth by this approach only and also it has been
in industrial use for over a century. Examples include the production of salt and nitrate in
chemical industry.

Although the bottom up approach is nothing new, it plays an important role in the
fabrication and processing of nano structures. There are several reasons for this and explained as
below.

When structures fall into a nanometer scale, there is a little chance for top down
approach. All the tools we have possessed are too big to deal with such tiny subjects. Bottom up
approach also promises a better chance to obtain nano structures with less defects, more
homogeneous chemical composition.

On the contrary, top down approach most likely introduces internal stress, in addition to
surface defects and contaminations.

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Chapter 03
NUCLEATION & GROWTH
3.1 Nucleation:
Nucleation is the rst step in the formation of either a new thermodynamic phase or a new
structure via self-assembly or self-organization. Nucleation is typically dened to be the process
that determines how long an observer has to wait before the new phase or self-organized
structure appears. For example, if a volume of water is cooled (at atmospheric pressure) below
0 C, it will tend to freeze into ice. Volumes of water cooled only a few degrees below 0 C often
stay completely ice free for long periods of time. At these conditions nucleation of ice is either
slow or does not occur at all. However, at lower temperatures ice crystals appear after little or no
[1][2]
delay. At these conditions ice nucleation is fast . Nucleation is commonly how rst-order
phase transitions start, and then it is the start of the process of forming a new thermodynamic
phase. By contrast new phases at continuous phase transitions start to form immediately.

Nucleation is often found to be very sensitive to impurities in the system. These impurities
may be too small to be seen by the naked eye, but still can control the rate of nucleation. Because
of this, it is often important to distinguish between heterogeneous nucleation and homogeneous
nucleation. Heterogeneous nucleation occurs at nucleation site on surface on the system.
Homogeneous nucleation occurs at away from the surface.

In nucleation of crystals, in many cases, liquids and solutions can be cooled down or
concentrated up to conditions where the liquid or solution is signicantly less thermodynamically
stable than the crystal, but where no crystals will form for minutes, hours, weeks or longer.
Nucleation of the crystal is then being prevented by a substantial barrier. This has consequences,
for example cold high altitude clouds may the nucleation of crystals contain large numbers of
small liquid water droplets that are far below 0C.

In small volumes, such as in small droplets, only one nucleation event may be needed for
crystallisation. In these small volumes, the time until the rst crystal appears is usually dened to

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[3]
be the nucleation time . In larger volumes many nucleation events will occur. A simple for
crystallisation in that case that combines nucleation and growth is the KJMA or Avrami model.

3.1.1 Examples of the nucleation of crystals

The most common crystallisation process on Earth is the formation of ice. Liquid water
does not freeze at 0C unless there is ice already present, cooling signicantly below 0C
is required to nucleate ice and so for the water to freeze. For example, small droplets of
very pure water can remain liquid down to below -30C although ice is the stable state
below 0C.
Many of the materials we make and use are crystalline, but are made from liquids, eg
crystalline iron made from liquid iron cast into a mold. So the nucleation of crystalline
materials is widely studied in industry. It is used heavily in the chemical industry for
cases such as in the preparation of metallic ultradispersed powders that can serve as
catalysts. For example, platinum deposited onto TiO2 nanoparticles catalysis the
liberation of hydrogen from water. It is an important factor in the semiconductor industry,
as the gap width in semiconductors is inuenced by the size of metal nanoclusters.

3.2 Crystal Growth

A crystal is a solid material whose constituent atoms, molecules, or ions are arranged in an
orderly repeating pattern extending in all three spatial dimensions. Crystal growth is a major
stage of a crystallization process, and consists in the addition of new atoms, ions, or polymer
strings into the characteristic arrangement of a crystalline Bravais lattice. The growth typically
follows an initial stage of either homogeneous or heterogeneous (surface catalyzed) nucleation,
unless "seed" crystal, purposely added to start the growth, was already present.

There are many types of different substances that will produce crystals grown from an
aqueous solution: sugar and salt for example. Crystals begin to grow when the amount of the
substance that is dissolved (the solute) exceeds the amount that in this case the water (the
solvent) is capable of dissolving. The maximum amount of solute dissolved in the water
produces a solution that is saturated. If additional solute is added, it will not dissolve. By raising
the temperature of the water it is possible to dissolve more solute such as sugar in hot coffee than

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would be possible at lower temperatures. Each substance will have a characteristic solubility that
can be experimentally determined.

Crystal growth is partly art, partly science. Crystals can be grown from solution using seed
crystals, which involves putting a small crystal into the presence of more of its component
materials (usually in solution) and allowing those components to uniform the pattern of the small
crystal, or seed. Silicon bottles, the blocks used for making microchips, are made or drawn in
this way.

Fig 3.1: Nucleation and Growth

Chapter 04
METHOD OF SYNTHESIS OF NANOPARTICLES

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Nanotechnology is an important field of modern research dealing with design, synthesis, and
manipulation of particle structures ranging from approximately 1-100 nm. Nanoparticles (NPs)
have wide range of applications in areas such as health care, cosmetics, food and feed,
environmental health, mechanics, optics, biomedical sciences, chemical industries, electronics,
space industries, drug-gene delivery, energy science, optoelectronics, catalysis, single electron
transistors, light emitters, nonlinear optical devices, and photo-electrochemical applications

Nowadays, there is a growing need to develop eco-friendly processes, which do not use toxic
chemicals in the synthesis protocols. Green synthesis approaches include mixed-valence
polyoxometalates, polysaccharides, Tollens, biological, and irradiation method which have
advantages over conventional methods involving chemical agents associated with environmental
toxicity. Selection of solvent medium and selection of eco-friendly nontoxic reducing and
stabilizing agents are the most important issues which must be considered in green synthesis of
NPs.

Some of the important chemical methods for synthesis of nanoparticles which are widely
used are as follows:

1. Coprecipitation method
2. Sol gel method
3. Solution reduction method
4. Microemulsion method
5. Hydrothermal method
6. Polyol method

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4.1 Coprecipitation method

On the other hand, in the analysis of trace elements, as is often the case in radiochemistry,
coprecipitation is often the only way of separating an element. Since the trace element is too
dilute (sometimes less than a part per trillion) to precipitate by conventional means, it is typically
coprecipitated with a carrier, a substance that has a similar crystalline structure that can
incorporate the desired element. An example is the separation of francium from other radioactive
elements by coprecipitating it with caesium salts such as caesium perchlorate. Otto Hahn is
credited for promoting the use of coprecipitation in radiochemistry.

There are three main mechanisms of coprecipitation: inclusion, occlusion, and

adsorption. An inclusion occurs when the impurity occupies a lattice site in the crystal structure
of the carrier, resulting in a crystallographic defect; this can happen when the ionic radius and
charge of the impurity are similar to those of the carrier. An adsorbate is an impurity that is
weakly bound (adsorbed) to the surface of the precipitate. An occlusion occurs when an adsorbed
impurity gets physically trapped inside the crystal as it grows.

Besides its applications in chemical analysis and in radiochemistry, coprecipitation is also

"potentially important to many environmental issues closely related to water resources, including
acid mine drainage, radionuclide migration in fouled waste repositories, metal contaminant
transport at industrial and defense sites, metal concentrations in aquatic systems, and wastewater
treatment technology"

Coprecipitation is also used as a method of magnetic nanoparticle synthesis.

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Fig 4.1: Coprecipitation Method

Advantages of coprecipitation method:

1) Simple and rapid preparation.
2) Easy control of particle size and composition.
3) The process is lower temperature synthesis.
4) Environmental friendly process.

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4.2 Sol gel method

The sol-gel method is a versatile process used for synthesizing various oxide materials. This
synthetic method generally allows control of the texture, the chemical, and the morphological
properties of the solid. This method also has several advantages over other methods, such as
allowing impregnation or coprecipitation, which can be used to introduce dopants. The major
advantages of the sol-gel technique includes molecular scale mixing, high purity of the
precursors, and homogeneity of the sol- gel products with a high purity of physical,
morphological, and chemical properties. In a typical sol-gel process, a colloidal suspension, or a
sol, is formed from the hydrolysis and polymerization reactions of the precursors, which are
usually inorganic metal salts or metal organic compounds such as metal alkoxides. A general
flowchart for a complete sol-gel process is shown in Figure.

Any factor that affects either or both of these reactions is likely to impact the properties of
the gel. These factors, generally referred to as sol-gel parameters, includes type of precursor, type
of solvent, water content, acid or base content, precursor concentration, and temperature. These
parameters affect the structure of the initial gel and, in turn, the properties of the material at all
subsequent processing steps.

After gelation, the wet gel can be optionally aged in its mother liquor, or in another solvent,
and washed. The time between the formation of a gel and its drying, known as aging, is also an
important parameter. A gel is not static during aging but can continue to undergo hydrolysis and
condensation.

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Fig 4.2: Flowchart for Sol Gel Method

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Advantages of sol gel method:

1) Simple, economic & effective
2) Highly pure product form.
3) Uniform nanostructure obtained.
4) Low temperature preparation saving energy.

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4.3 Solution reduction method

This is a new method for the preparation of metal nanoparticles (MNPs). This method is
mostly used for the synthesis of silver nanoparticles (AgNPs) from different precursors such as
silver chloride (AgCl) and silver nitrate (AgNO3). AgNP layers exhibiting strong infrared
surface enhancement were prepared by reacting silver chloride discs in a solution containing
hydrazine, which acts as a reducing agent. The silver ions in the outer layer could be reduced
under proper conditions and the reduced silver coagulated to form suitable AgNPs.

Chemical reduction method involves the reduction of AgNO3 in aqueous solution by an

effective reducing agent in the presence of appropriate stabiliser, which is necessary in shielding
the growth of silver particles through aggregation. During the formation of silver nanoparticles
by the chemical reduction method, some of the parameters like the particle size and aggregation
state of silver nanoparticles are affected by initial AgNO 3 concentration, reducing agent, AgNO3
molar ratios and stabilizer concentrations. So many methods are suggested for the chemical
synthesis of silver nanoparticle formation; chemical reduction method, polyol method and
radiolytic process have been developed for the synthesis of silver nanoparticles. The best and
most easy method of yielding nanoparticles without aggregation, high yield and low preparation
cost is chemical reduction method.

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Fig 4.3: Flowchart for Solution Reduction Method

Advantages of solution reduction method:

1) Simple, convenient, flexible.
2) Producing metal nanoparticles like molybdenum, tungsten.
3) Economical method.

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4.4 Microemulsion method

Micro-emulsion method is one of the recent and ideal techniques for the preparation of
inorganic nano-particles. Oil and water are immiscible and they separate into two phases when
mixed, each saturated with traces of the other component. An attempt to combine the two phases
requires energy input that would establish water-oil association replacing the water-water/oil-oil
contacts. The interfacial tension between bulk oil and water can be as high as 30-50 dynes/cm.
This can be overcome by the use of surface-active molecules known as surfactants. Surfactants
contain water- loving (hydrophilic) and oil-loving (lipophilic) moieties. Owing to this
characteristic, they tend to adsorb at the water-oil interface. If enough surfactant molecules are
present, they align and create an interface between the water and the oil by decreasing the
interfacial tension.

An emulsion is formed when a small amount of an appropriate surfactant is mechanically

agitated with the oil and water resulting in a two-phase dispersion where one phase exists as
droplets coated by surfactant that is dispersed throughout the continuous, other phase. These
emulsions are milky or turbid in appearance due to the fact that the droplet sizes range from 0.1
to 1 micron. As a general rule, the type of surfactant used in the system determines which phase
is continuous. If the surfactant is hydrophilic, oil will be emulsified in droplets throughout a
continuous water phase. The opposite is true for more lipophilic surfactants. Water will be
emulsified in droplets that are dispersed throughout a continuous oil phase in this case.
Emulsions are kinetically stable, but are ultimately thermodynamically unstable, and will begin
to separate back into their two phases. The droplets would merge together, while the dispersed
phases will sediment. At this point, they degrade back into bulk phases of pure oil and pure water
with some of the surfactant dissolved preferentially in one of the two.

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Fig 4.4: Preparation of nanoparticles in Microemulsion

Advantages of microemulsion process:

1) Process is simple and economic.
2) Better size controlled possible in microemulsion process.

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4.5 Hydrothermal method

Water is an excellent solvent for many ionic compounds. It can even dissolve non-ionic
covalent compounds under high pressure and high temperature. In hydrothermal synthesis, the
above property of water has been effectively exploited for the preparation of fine powders of
metal oxides. Under these hydrothermal conditions, water plays two roles: 1) as pressure
transmitting medium and 2) as a solvent for reacting solids. Such hydrothermal conditions
effectively brings down the activation energy for the formation of final phase, which can also
speed up the reaction between the solids which otherwise would occur only at very high
temperatures. An autoclave is invariably employed to achieve hydrothermal conditions. The
pressures attained are in the range of 10 to 150 kilobar which depends on the chosen temperature
of water (>373 K). Powders are either crystalline or amorphous depending on chosen
hydrothermal temperature.

Fig 4.5: Hydrothermal process

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Advantages of hydrothermal process:

1) Powders are formed directly from the solution.
2) It is possible to control particle size and shapes by using different starting materials and
hydrothermal conditions.
3) Resulting powders are highly reactive which aid in low temperature sintering.

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4.6 Polyol method

Ethylene glycol has been widely used in the polyol process for the synthesis
of metal (both pure and alloyed) nanoparticles due to its strong reducing power and
relatively high boiling point (~197 C). Recently, it has been widely used for the
synthesis of nanocrystaline ceramic powders that involved, complexation with
ethylene glycol, followed by polymerization. In addition, ethylene glycol has been
used to fabricate meso structures of titania, tin dioxide, zirconia, and niobium
oxide by forming glycol ate precursors because of its coordination ability with
transition metal ions. This route involves hydrolysis and inorganic polymerization
carried out on the salts dissolved in a polyol medium. The polyol acts as a solvent
for the precursor salts because of its high relative permittivity, and allows one to
carry out hydrolysis reactions under atmospheric pressure in a large temperature
range up to the boiling point of the polyol.

Fig 4.6: Polyol Method with formation of possible structure

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Advantages of polyol process

1) Low temperature process which can able to control the properties of the
particles such as size, shape and uniformity, etc.
2) It yields high pure organic free powders.

Chapter 05
CHARACTERIZATION OF NANOPARTICLES
When the dimensions of materials are reduced to nano scale, they demonstrate unique
properties which are far different from those of their bulk counterparts. For example, their
electronic and optical properties change, their chemical properties can be increased or decreased
and mechanical/structural stabilities are changed dramatically. These features make
Nanoparticles attractive for unique sensing applications, and also at the same time cause
complications in their characterization processes. Therefore, the challenge lies in finding the

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right characterization techniques that have the optimum capabilities for studying the
characteristics of nanomaterials generated by these techniques.
Common techniques are Transmission Electron Microscope (TEM), Scanning Electron
Microscope (SEM), Atomic Force Microscopy (AFM), Dynamic Light Scattering (DLS), X-ray
Photoelectron Spectroscopy (XPS), Powder X-ray Diffraction (XRD), Fourier Transform
Infrared Spectroscopy (FTIR), Matrix-assisted Laser Desorption/ionization Time-of-Flight Mass
Spectrometry(MALDI-TOF), Ultraviolet-Visible Spectroscopy, dual polarisation.
Characterization of nanoparticles is based on the size, morphology and surface charge,
using such advanced microscopic techniques as atomic force microscopy (AFM), scanning
electron microscopy (SEM) and transmission electron micros- copy (TEM). Properties such as
the size distribution, average particle diameter, charge affect the physical stability and the in vivo
distribution of the nanoparticles. Properties like surface morphology, size and overall shape are
determined by electron microscopy techniques. Features like physical stability and
redispersibility of the polymer dispersion as well as their in vivo performance are affected by the
surface charge of the nanoparticles.

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Chapter 06
CONCLUSION
Nanomaterials have been extensively investigated during the last decade due to their
Wide variety of applications. It is observed that field of nanomaterial synthesis is very dynamic.
Many process such as gas condensation, chemical vapor synthesis, mechanical attrition, chemical
precipitation, Sol-Gel technique, electrodeposition, some other methods widely used are
molecular beam epitaxy, ionised cluster beam, liquid metal ion source, consolidation, sputtering
and gas aggregation of monomers chemical precipitation in presence of capping agents, reaction
in microemulsion and autocombustion are commonly used techniques for synthesis of
nanophosphors. Nanomaterials prepared using the processes include a wide variety.

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