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Chapter

Preparation of Nanoparticles
Takalani Cele

Abstract

Innovative developments of science and engineering have progressed very fast

toward the synthesis of nanomaterials to achieve unique properties that are not
the same as the properties of the bulk materials. The particle reveals interesting
properties at the dimension below 100 nm, mostly from two physical effects. The
two physical effects are the quantization of electronic states apparent leading to
very sensitive size-dependent effects such as optical and magnetic properties and
the high surface-to-volume ratio modifies the thermal, mechanical, and chemical
properties of materials. The nanoparticles’ unique physical and chemical properties
render them most appropriate for a number of specialist applications.

Keywords: nanoparticles, physical methods, chemical methods, synthesis,

metal nanoparticles

1. Introduction

Several methods have been developed to produce metal nanoparticles. Two syn-
thesis approaches have been identified that is top-down and bottom-up approach.
Top-down methods comprise of milling, lithography, and repeated quenching. This
approach does not have good control of the particle size and structure. Bottom-up
method is the approach that is mostly used by scientists in the synthesis of nanopar-
ticles as it involves building up a material from bottom: atom-by-atom, molecule-by-
molecule, and cluster-by-cluster [1, 2]. Several chemical routes have been identified
to synthesize the colloidal metal nanoparticles from different precursors using
chemical reductants in solvents (aqueous and nonaqueous). The chemical routes
that have been studied for various applications include electrochemical method [3],
sonochemical method [4], radiolytic [5] and photochemical [6] method.

2. Methods of synthesis of metal nanoparticles

2.1 Chemical methods

2.1.1 The polyol method

The Polyol method is a chemical method for the synthesis of nanoparticles.

This method uses nonaqueous liquid (polyol) as a solvent and reducing agent.
The nonaqueous solvents that are used in this method have an advantage of mini-
mizing surface oxidation and agglomeration. This method allows flexibility on
controlling of size, texture, and shape of nanoparticles. Polyol method can also be
used in producing nanoparticles in large scale [7].

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Engineered Nanomaterials - Health and Safety

The polyol process can be taken as a sol-gel method in the synthesis of oxide, if
the synthesis is conducted at moderately increased temperature with accurate par-
ticle growth control [8]. There are several reports that have studied the synthesis of
oxide sub-micrometer particles and these include Y2O3, VxOy,Mn3O4, ZnO, CoTiO3,
SnO2, PbO, and TiO2 [9–16].
The solvent that is mostly used in polyol method in metal oxide nanoparticles
synthesis is ethylene glycol because of its strong reducing capability, high dielectric
constant, and high boiling point. Ethylene glycol is also used as a crosslinking
reagent to link with metal ion to form metal glycolate leading to oligomerization
[17]. It has been reported that as-synthesized glycolate precursors can be converted
to their more common metal oxide derivatives when calcined in air, while maintain-
ing the original precursor morphology [8].
The polyol synthesis process has also been used for the synthesis of bimetal-
lic alloys and core-shell nanoparticles [18–20]. Yang and co-workers used polyol
method to produce icosahedral and cubic gold particles on the order of 100–300 nm
by careful regulation of the growth rate for each crystallographic direction [21].
Xia and co-workers reported the production of controlled morphologies such as
nanocubes and nanowires by controlling the molar ratio between silver nitrate and
PVP [22].

2.1.2 Microemulsions

An emulsion is a liquid in liquid dispersion. A solution of polymers can produce

emulsions as it is liquid. Emulsions are divided according to the size of droplet, i.e.,
macro-emulsions, mini-emulsions, and micro-emulsions [23].
Micro-emulsion synthesis method is widely used for the production of inorganic
nanoparticles [24]. When oil and water are mixed, they separate into two phases
as they are immiscible [25]. The energy input is required to mix the two phases to
create water-oil.
An attempt to combine the two phases requires energy input that would estab-
lish water-oil connection replacing the water-water/oil-oil contacts. The interfacial
tension between bulk oil and water can be as high as 30–50 dynes/cm and this can
be avoided by using surfactants (surface-active molecules). Surfactants contain
hydrophilic (water-loving) and lipophilic (oil-loving) groups [26]. The interface
can be aligned and established between oil and water by reducing the interfacial
tension if there are enough surfactant molecules.
The preparation procedure of metallic nanoparticles in water in oil microemul-
sion commonly consists of mixing of two microemulsions containing metal salt and
a reducing agent, respectively as shown in Figure 1.
Brownian motion is formed after the exchange of reactants (collision) between
micelles that happens after mixing two microemulsions. Good collisions result into
coalescence, fusion, and mixing well of the reactants. Metal nuclei are formed from
the reaction between solubilizates. Bönnemann et al. reported the formation of
zerovalent metal atoms at nucleation stage from reducing a metal salt, which can
collide with additional metal ions, metal atoms, or clusters to form an irreversible
seed of stable metal nuclei [28].
The growth stage happens around the nucleation point, where successful colli-
sion occurs between a reverse micelle moving a nucleus and another one moving the
product monomers with the arrival of more reactants due to intermicellar exchange.
The morphology and size of nanoparticles are based on the size and shape of the
nanodroplets and the type of the surfactant. The surfactant is usually used to
stabilize the particle and protect them from proceeding to grow [28].

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Figure 1.
Schematic illustration of nanoparticles preparation using microemulsion techniques: Particle formation steps.
Kchem is the rate constant for chemical reaction, kex is the rate constant for intermicellar exchange dynamics, kn
is the rate constant for nucleation, and kg is the rate constant for particle growth [27].

Wongwailikhit et al. reported the formation of iron (III) oxide, Fe2O3 using
water in oil microemulsion by combining the required amount of H2O in a stock
solution of Sodium Bis (2-Ethylhexyl) Sulfosuccinate (AOT) in n-heptane. The
solution was left overnight, then the concentrated Hydroxylamine (NH2OH) and
FeCl3 were mixed into the water in oil microemulsion. Suspension of Fe2O3 was
filtered and washed with 95% ethanol and dried at 300°C for 3 h. The product was
spherical, monodisperse nanoparticles with diameter of about 50 nm. The size of
particles depended on the water content in microemulsion system. The increase of
particles size was achieved with increasing the water fraction in water in oil micro-
emulsion [29].
Sarkar et al. reported the formation of pure monodispersed zinc oxide nanopar-
ticles of different shapes. Microemulsion was composed of cyclohexane, Triton
X-100 as surfactant, hexanol as cosurfactant and aqueous solution of zinc nitrate
or ammonium hydroxide/sodium hydroxide complex. The molar ratio of TX-100
to hexanol was maintained at 1:4. The microemulsion containing ammonium
hydroxide/sodium hydroxide was added to microemulsion containing zinc nitrate
and stirred. The nanoparticles were then separated by centrifuging at 15,000 rpm
for 1 h. The particles were washed with distilled water and alcohol and dried at 50°C
for 12 h [30].
Maitra was the first to establish Chitosan nanoparticles by microemulsion
technique. Chitosan nanoparticles were prepared in the aqueous core of reverse
micellar droplets and crosslinked through glutaraldehyde. Surfactant dissolved in
N-hexane was also used with chitosan in acetic acid and glutaraldehyde was added
in the surfactant at room temperature. The mixture was stirred continuously and
nanoparticles were produced [31].

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2.1.3 Thermal decomposition

Thermal decomposition also known as thermolysis is a chemical decomposition

that is caused by heat. In this method, the heat is required to break chemical bonds
in the compound undergoing decomposition and the reaction is endothermic.
If decomposition is sufficiently exothermic, a positive feedback loop is created
producing thermal runaway [32].
Arshad et al. reported on thermal decomposition of metal complexes of type
MLX2 [M = Co (II), Cu (II), Zn (II), and Cd (II);L = DIE; X = NO31−] by TG-DTA-
DTG techniques in air atmosphere. They synthesized nitrate complexes of transi-
tion metals with 1,2-diimidazoloethane (DIE) of the general formula M(DIE)
(NO3)2. The study was conducted by thermoanalytical techniques in static air
atmosphere to study the thermal behavior of these complexes and to determine
their mode of decomposition. The complexes and ligands decomposed in a two-step
process when heated to 740°. Above 740°, the residue was found to correspond with
metal oxide. The thermal stability of the complexes increases in the following series:
Co(II) < Cu(II) < Zn(II) < Cd(II) [33].
Patil et al. studied infrared spectra and thermal decompositions of metal
acetates and dicarboxylates. The study was done to determine the metal-acetate
bonding and the thermal decomposition of lead, copper, and rare earth acetates was
studied by means of thermogravimetric analysis and differential thermal analysis.
The investigations on decomposition products yielded good results [34].
George et al. reported on the mechanism of thermal decomposition of n-Buty l
(tri-n-butylphosphine) copper (I). This study provided the first easily interpretable
example in which succeeding reaction of a metal hydride and its parent metal alkyl
was found to be vital in determining the products of a thermal decomposition [35].
Thermal decomposition of bismuth and silver carboxylates was investigated by
means of TG, DSC, mass spectrometry, X-ray analysis, and electron microscopy
Logvinenko et al. [36]. Non-isothermal thermogravimetric data were used for
kinetic studies. All decomposition processes had multi-step character [36].
Ewell et al. investigated nearly pure talc both unheated and after heating at vari-
ous temperatures ranging up to 1,435°C. The research included the measurement of
heat effects, weight losses, and changes in true specific gravity occurring on heating
talc. There was no change in the crystal structure of the talc heated up to 800°C. At
the temperature between 800 and 8400°C, the talc decomposed to enstatite,
amorphous silica, and water vapor. At the temperature approximately 1,200°C,
the enstatite steadily changed to clinoenstatite and the amorphous silica changed
to cristobalite approximately 1,300°C, giving clinoenstatite and cristobalite as end
products [37].

2.1.4 Electrochemical synthesis

Electrochemical synthesis is the synthesis of chemical compounds in an electro-

chemical cell. The main advantage of electrochemical synthesis over an ordinary
chemical reaction is rejection of the potential wasteful alternative half-reaction and
the ability to accurately tune the preferred potential [38].
Electrochemical synthesis of silver nanoparticles has been extensively studied
in the previous years. The method of electrochemical that was used was based on
the dissolution of a metallic anode in an aprotic solvent. The silver nanoparticles
that were produced by electroreduction of anodically solved silver ions in aceto-
nitrile containing tetrabutylammonium ranged from 2 to 7 nm. The particle size
was obtained by varying the current density. Different types of counter electrodes
were used to study the effect of the different electrochemical parameters on the

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end particle size. The UV-Vis spectra showed the presence of two different silver
clusters [39].
Dobre et al. also reported on the electrochemical synthesis of colloidal silver
solutions using “sacrificial anode” technique conducted with a home-built current
pulse generator with alternating polarity and a stirrer. Poly (N-vinyl-2-pyrrolidone)
(PVP) and sodium lauryl sulfate (Na-LS) were used as a stabilizer and co-stabilizer,
correspondingly. Spherical Ag particles with the size approximately 10–55 nm were
synthesized. The UV/Vis spectra showed the absorption band at 420 nm, which is
the evidence of the presence of Ag nanoparticles. The zeta potential values between
−17 and −35 mV suggested a presence of particles covered by stabilizer with a slight
agglomeration [40].
More research was done on the electrochemical synthesis of silver nanopar-
ticles in aqueous poly (vinyl alcohol) solution (PVA). PVA is a low price widely
used synthetic polymer with properties such as nontoxicity, water solubility, bio-
compatibility, biodegradability, and excellent mechanical properties. The experi-
ment was conducted at a constant current density of 25 mA cm−2 for a synthesis
time of 10 min. Silver nanoparticles with an average diameter of 15 ± 9 nm were
obtained [41].
The electrochemical synthesis of red fluorescent Silicon (Si) nanoparticles sta-
bilized with styrene. Si nanoparticles emit fluorescence under UV excitation, which
is great for optics applications, etc. It was found that the liberated silicon particles
in ethanol solution interact with styrene, which resulted in the substitution of Si-H
bonds with those of Si-C. The developed styrene-coated Si nanoparticles exhibited
a stable, bright, red fluorescence under excitation with a 365 nm UV light, and
resulted into approximately 100 mg per Si wafer with a synthesis time of 2 h [42].
More investigations were done on the preparation of long-lived silver nanopar-
ticles in aqueous solutions and silver powders using electrochemical method. The
produced silver nanoparticles had a size distribution ranging from 2 to 20 nm and
the nanoparticles remained stable for more than 7 years. Silver crystals containing
agglomerated silver nanoparticles with sizes below 40 nm was found growing on
the surface of the cathode [43].
The research was conducted on using electrochemical method to synthesize
highly pure silver nanoparticles. This method was used as it is one-step less expen-
sive procedure and easy to control at room temperature and it does not use danger-
ous chemicals. The experimental setup brought up the oxidation of the anode and
reduction of the cathode. The silver nanoparticles synthesized were spherical and
had a particle size below 50 nm [44].
Islam et al. explored on the synthesis of platinum nanoparticles by electrochemi-
cal deposition method. The particle size was controlled by varying electrolysis
parameters and homogeneity of platinum particles was improved by varying the
composition of electrolytic solutions. Platinum nanoparticles were deposited on
electrode surfaces and the particle sizes were found to be larger than 10 nm and had
wide particle size distribution [45].

2.2 Physical methods

2.2.1 Plasma

Plasma method is another method that is used to produce nanoparticles. The

plasma is generated by radio frequency (RF) heating coils. The initial metal is
enclosed in a pestle and the pestle is enclosed in an evacuated chamber. The metal
is then heated above its evaporation point by high voltage RF coils wrapped around
the evacuated chamber. The gas that is used in the procedure is Helium (He), which

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Engineered Nanomaterials - Health and Safety

forms a high-temperature plasma in the region of the coils after flowing into the
system. The metal vapor nucleates on the helium gas atoms and diffuses up to a cold
collector rod, this is where nanoparticles are collected and they are passivated by
oxygen gas (Figures 2 and 3) [46].
Classification of plasma methods based on the feeding materials to reactor and
also the heating source (electrodeless/ electrode containing), see (Figures 2 and 3).

2.2.2 Chemical vapor deposition

The chemical vapor deposition method (CVD) involves a chemical reaction.

CVD procedure is mostly used in semiconductor manufacturing for depositing
thin films of different materials. The method involves one or more volatile precur-
sors, the substrate is exposed to those precursors that decompose on it and form
the desired deposit. The vaporized precursors are inserted into a CVD reactor and
adsorb onto a substance being placed at high temperature. The molecules that get
adsorbed react with other molecules or decompose to form crystals. The three steps
in CVD method are:

1. Reactants are transported on the growth surface by a boundary layer.

2. Chemical reactions occur on the growth surface.

3. By products produced by the gas-phase reaction has to be removed from the

surface. Homogeneous nucleation occurs in gas phase and heterogeneous
nucleation happens in a substrate.

The CVD method can synthesize ultrafine particles of less than 1 μm by the
chemical reaction taking place in the gaseous phase. The reaction can be controlled
to produce nanoparticles of size ranging from 10 to 100 nm [46, 47].

2.2.3 Microwave irradiation

Microwave irradiation is a synthesis method that has been widely used in the
synthesis of organic, inorganic, and inorganic–organic hybrid materials because of
its well-known advantages over conventional synthetic routes [48].
A research was conducted on a rapid and efficient oxidation of organic
compounds in microwave condition with new phase transfer oxidative agent:
CTAMABC. CTMABC (1 mmole) was suspended in acetonitrile (2 ml) and an alco-
hol (l mmole in 0.5–1.5 ml of acetonitrile) was quickly added at room temperature
and the resulting mixture was stirred vigorously. The mixture was then irradiated
by microwave radiation (3.67 GHz, 300 W). The solution became homogeneous
for a short time before the black-brown reduced reagent precipitated. Thin layer
chromatography (TLC) and UV/VIS spectrophotometer (at 352 nm) were used to
monitor the progress of reactions [49].
In another experiment conducted by Sahoo Biswa Mohan et al., o-Phenylenedi-
amine (1.08 g, 0.01 mole) and anthranillic acid (1.37 g, 0.01mole) were dissolved in
ethanol (15 ml). And K2CO3 was added to a mixture and the reaction mixture was
put in microwave oven and refluxed at power (140 Watt) for 10 min. TLC was used
to monitor the reaction. After the reaction was complete, ethanol was removed by
distillation process and the residue was poured into crushed ice. Then the reaction
was made alkaline by using 10% NaOH to get the solid product. The product was
filtered, dried, and recrystallized from ethanol [50].

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Figure 2.
Flow diagram for production plant based on plasma burners. The recirculation system is of special importance
in the case of expensive reaction or carrier gases.

Figure 3.
Different plasma classification.

Sahoo Biswa Mohan et al. conducted another experiment where N-(2-(1H-

benzo[d]imidazol-2-yl) phenyl) acetamide (2.51 g, 0.01 mole) was dissolved in
ethanol (30 ml) and various aromatic aldehydes (0.01 mole) were taken and then
an aqueous solution of KOH (2%, 5 ml) added to it. The reaction was then put in

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Engineered Nanomaterials - Health and Safety

a microwave oven and refluxed at power (210 Watt) for 10–20 min. The excess
solvent was removed by vacuum distillation and then poured into crushed ice and
acidified with dilute HCl. The product was filtered, dried, and recrystallized from
ethanol [51].
Microwave-assisted organic synthesis has been widely used due to enhanced
reaction rates, higher yields, improved purity, ease of work up after the reaction
and eco-friendly reaction conditions compared to the conventional methods. In
above experiments, microwave irradiated synthesis of chalcone was carried out to
get higher yield with less reaction time period as compared to conventional method.
The synthesized benzimidazolyl chalcone produces yield around 60% (conven-
tional) and 80% (microwave) [52].
Another study was conducted to synthesize silver nanoparticles (AgNPs) in
aqueous medium by a simple, efficient, and economic microwave-assisted syn-
thetic route using hexamine as the reducing agent and the biopolymer pectin as
stabilizer. The synthesized AgNPs were characterized by UV-VIS, Spectroscopy,
Energy dispersive X-ray (EDX), X-ray diffraction (XRD), and Transmission
electron microscopy (TEM) techniques. The nanoparticles were found to be spheri-
cal shape with an average diameter of 18.84 nm. The rate of reaction was found to
increase with increasing temperature and the activation energy was found to be
47.3 kJ mol−1 [53].
ZnS nanoparticles were synthesized by microwave-assisted irradiation method.
The produced ZnS nanoparticles were characterized by XRD, SEM, and UV-Vis
spectroscopy. The average size of the nanocrystallites was measured by Debye-
Scherrer formula as per the XRD spectrum, and there were found to be approxi-
mately 6 nm [54].

2.2.4 Pulsed laser method

Pulsed laser method is a method that is mostly used in the synthesis of silver
nanoparticles, at a high rate of production of 3 gm/min. Silver nitrate solution and
a reducing agent are poured into a blender-like device. The device is composed of
a solid disc that rotates with the solution. The disc is exposed to pulses from a laser
beam to create hot spots on the surface of the disc. Hot spots are where the silver
nitrate reacts with reducing agent to produce silver particles that can be separated
by centrifuge. The particle size is controlled by the energy of the laser and angular
velocity of the disc [46] (Figures 4 and 5).

2.2.5 Sonochemical reduction

Sonochemical method has been studied in the synthesis of metal nanoparticles.

The synthesis of different types of metal nanoparticles has been studied by use of
the sonochemical reduction of the corresponding metal ions. The sonochemical
reduction of MnO4−, Au3+, Au+, and Pd2+ in the absence and presence of organic
additives were investigated in relation to the synthesis of size and shape controlled
metal nanoparticles. The rates of reduction were controlled to control the size
and shape of metal nanoparticles. The size of the Au nanoparticles formed from
the sonochemical reduction of Au3+ was controlled in the presence of an organic
stabilizer citric acid [55].
Obreja et al. conducted a study on alcoholic reduction platinum nanoparticles
synthesis by sonochemical reduction. H2PtCl6 was reduced with methanol, ethanol,
and propanol working as solvents and reducing agents, in the presence of capping
polymers such as chitosan, polyethylene glycol, and poly (amidehydroxyurethane).
The produced nanoparticles size was found to be approximately 3 nm [56].

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Figure 4.
Synthesis of nanoparticles using a pulsed laser method [46].

Figure 5.
Apparatus to produce silver nanoparticles using a pulsed laser beam that makes hot spots on the surface of a
rotating disk [54].

2.2.6 Gamma radiation

Gamma radiation is the preferred method for metallic nanoparticles synthesis

because it is reproducible, may control the shape of the particles yields monodis-
perse metallic nanoparticles, is easy, cheap, and use less toxins precursors: in water
or solvents such as ethanol, it uses the least number of reagents, it uses a reaction
temperature close to room temperature with as few synthetic steps as possible
(one-pot reaction) and minimizing the quantities of generated by-products and
waste [57].
The radiolytic reduction has been proven to be a powerful tool to fabricate
monosized and highly dispersed metallic clusters [58]. The primary effects of the
interaction of high-energy gamma photons with a solution of metal ions are the
excitation and the ionization of the solvent [59]. The different reactions that are
observed are well explained in the paper by Abidi and Remita. In particular, water
can be produce upon irradiation of a series of reducing and oxidizing agents as
shown in the following equation.
−
H2 O ⇒ e aq, H 3 O + , H • , OH • , H 2, H 2 O 2 (1)

For the production of metallic nanoparticles from metallic salt solutions, the
reducing agents e−aq and H• are the cornerstones of the process. Unfortunately,
the production of hydroxyl radicals OH• hampers the efficiency unless some

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Engineered Nanomaterials - Health and Safety

specific hydroxyl scavengers are used. Among them, isopropanol is frequently

used [60].
This technique has been widely used so far to produce solutions of MNP pri-
marily gold and silver that were further investigated by UV-Visible spectroscopy
with the aim to analyze their plasmonic absorption band. A wealth of literature
can be found on this topic [61, 62]. Additionally, γ rays irradiation was also used to
trap MNP inside polymers or inside porous frameworks like mesoporous silica for
instance [63–65].

3. Conclusions

Nanoparticles have gained significant interest due to their unique chemical and
physical properties and are applicable to diverse areas. Various methods of prepa-
ration of nanoparticles have been developed and they are suitable for synthesis
of nanoparticles in different sizes and shapes. The methods that were discussed
include gamma irradiation, chemical reduction photochemical method, thermal
decomposition, and microwave irradiation among others.

Acknowledgements

The author is particularly grateful to National Research Foundation, University

of South Africa, iThemba LABS and L’Oreal For Women in Science for their support
and funding.

Author details

Takalani Cele
University of South Africa, Pretoria, South Africa

*Address all correspondence to: [email protected]

© 2020 The Author(s). Licensee IntechOpen. This chapter is distributed under the terms
of the Creative Commons Attribution License (http://creativecommons.org/licenses/
by/3.0), which permits unrestricted use, distribution, and reproduction in any medium,
provided the original work is properly cited.

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DOI: http://dx.doi.org/10.5772/intechopen.90771

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