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Synthesis techniques for preparation of nanomaterials

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DOI: 10.1007/978-3-319-68255-6_149

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Synthesis Techniques for Preparation
of Nanomaterials 4
Sharanabasava V. Ganachari, Nagaraj R. Banapurmath,
Basavaraja Salimath, Jayachandra S. Yaradoddi, Ashok S. Shettar,
Anand M. Hunashyal, Abbaraju Venkataraman, Parvathi Patil,
H. Shoba, and Gurusiddesh B. Hiremath

Contents
Introduction . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 85
Colloidal Methods . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 86
Coprecipitation Method . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 86
Self-Propagating High-Temperature Combustion Method . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 88

S. V. Ganachari · N. R. Banapurmath (*)

Centre for Material Science, Advanced Research in Nanoscience and Nanotechnology, School of
Mechanical Engineering, KLE Technological University (formerly known as B.V. Bhoomaraddi
College of Engineering and Technology), Hubballi, Karnataka, India
e-mail: sharanu14@gmail.com; nrbanapurmath@gmail.com
B. Salimath
Department of Chemistry, Gulbarga University, Kalaburagi, Karnataka, India
Department of Materials Science, Gulbarga University, Kalaburagi, Karnataka, India
Icon Analytical Equipment Pvt. Ltd, Bengaluru, India
e-mail: basu1231@gmail.com
J. S. Yaradoddi
Centre for Material Science, Advanced Research in Nanoscience and Nanotechnology, School of
Mechanical Engineering, KLE Technological University (formerly known as B.V. Bhoomaraddi
College of Engineering and Technology), Hubballi, Karnataka, India
Extremz Biosciences Private Limited (Govt. of Karnataka Funded Startup), KLE Technological
University (formerly known as B.V. Bhoomaraddi College of Engineering and Technology),
Hubballi, Karnataka, India
e-mail: jsybiotech@gmail.com
A. S. Shettar
Centre for Material Science, Advanced Research in Nanoscience and Nanotechnology, School of
Mechanical Engineering, KLE Technological University, B.V. Bhoomaraddi College of
Engineering and Technology, Hubballi, Karnataka, India
Department of Civil Engineering, KLE Technological University, B.V. Bhoomaraddi College of
Engineering and Technology, Hubballi, Karnataka, India
e-mail: ashokshettar@bvb.edu

# Springer Nature Switzerland AG 2019 83

L. M. T. Martínez et al. (eds.), Handbook of Ecomaterials,
https://doi.org/10.1007/978-3-319-68255-6_149
84 S. V. Ganachari et al.

Sol-Gel Technique . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 89
Reverse Microemulsions/Micelles Method . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 89
Spray Pyrolysis . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 90
Thermochemical/Flame Decomposition of Metal-Organic Precursors . . . . . . . . . . . . . . . . . . . . . . . . . 91
Self-Propagating Low-Temperature Synthesis (SPLTS) . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 92
Microwave-Assisted Technique . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 93
Solution Combustion Technique . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 94
Hydrothermal (HT)/Solvothermal (ST) Synthesis . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 94
Alginate Template Technique . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 96
Liquid-Liquid Interface Technique . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 97
Biosynthesis of Biofunctionalized Noble Metal Nanoparticles . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 98
Actinomycetes . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 99
Yeast . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 99
Fungi . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 100
Higher Plants . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 100
Conclusion . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 101
References . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 101

Abstract
Nanotechnology is concerned with the design, development, and application
of nanomaterials and the essential empathizing of the associations among
physical properties or phenomena and material dimensions. It deals with

A. M. Hunashyal
Centre for Material Science, Advanced Research in Nanoscience and Nanotechnology, KLE
Technological University, B.V. Bhoomaraddi College of Engineering and Technology, Hubballi,
Karnataka, India
Department of Civil Engineering, KLE Technological University, B.V. Bhoomaraddi College of
Engineering and Technology, Hubballi, Karnataka, India
e-mail: amhunashyal@bvb.edu
A. Venkataraman
Department of PG Studies and Research in Chemistry, Gulbarga University, Kalaburagi, Karnataka,
India
Department of Materials Science, Gulbarga University, Kalaburagi, Karnataka, India
e-mail: raman.dms@gmail.com
P. Patil
Department of PG Studies and Research in Chemistry, Gulbarga University, Kalaburagi, India
Department of Materials Science, Gulbarga University, Kalaburagi, India
Department of Chemistry, H. K. E. Society’s Smt. Veeramma Gangasiri College for Women,
Kalaburagi, India
e-mail: parvathipatil03@gmail.com
H. Shoba
Department of Agricultural Engineering, University of Horticultural Sciences, Bagalkot, India
e-mail: shobhahugar@gmail.com
G. B. Hiremath
Department of Biotechnology and Microbiology, P. C. Jabin Science College, Hubballi, India
e-mail: guruh22@gmail.com
4 Synthesis Techniques for Preparation of Nanomaterials 85

materials or structures in nanometers and is a novel field or a new technical

area. Analogous to quantum mechanics, on the nanometer scale, materials
or structures may have new physical properties or show new physical
phenomena.
Nanomaterials have an enormously wide range of possible applications from
nanoscale optics and electronics to nano-biological systems and nano-medicine.
However, the study and applications of nanomaterials rely powerfully on the
effective synthesis of nanomaterials. In addition, progress of simple and econom-
ical impending for the preparation of nanomaterials is vital for the applications of
nanomaterials and the progress of nanotechnology.

Keywords
Nanomaterials · Synthesis methods · Sol- gel · Hydrothermal · Colloidal ·
Spray pyrolysis · Self-propagating high- temperature combustion method ·
Self-propagating low- temperature combustion method · Reverse
microemulsions/micelles method · Thermochemical/Flame decomposition of
metal-organic precursors · Microwave-assisted method

Introduction

Synthesis of nanometal and metal oxide (MO) materials involves substantial

synthetic ingenuity. Although one can develop a balanced method to the synthe-
sis of nanomaterials [1, 2], there is continually an element of serendipity. A
verity of nanomaterials has been synthesized in the last several decades by the
old-style ceramic method, which includes mixing and crushing powders of the
constituent oxides, carbonates, and other compounds and heating them at ele-
vated temperatures with transitional grinding when necessary. A varied range of
environments, often bordering on the extreme, have been employed in material
synthesis; these contain high temperatures or pressures, very low oxygen fugac-
ities, and quick quenching. The current trend is to circumvent brute force
impending in direction to achieve better control of structure, stoichiometry, and
phasic purity. The so-called soft chemistry techniques, which the French call
chimie douce, are indeed necessary as they lead to innovative products, any of
which are metastable and can’t otherwise be synthesized. Chimie douce routes
basically make use of simple reactions which are carried out at relatively low
temperatures [3]. Figure 1 shows structure/property relationships: physicochem-
ical properties of materials.
Some of the important chemical methods of synthesis of oxides are
coprecipitation and precursor methods, ion exchange and sol-gel technique,
topochemical methods, hydrothermal/solvothermal approaches, combustion tech-
nique (self-propagating high- and low-temperature method and solution combustion
method), microwave-assisted and liquid-liquid interface method, etc. Some of them
have been briefly described in the following sections.
86 S. V. Ganachari et al.

Fig. 1 Structure/property
relationships:
physicochemical properties of
materials

Colloidal Methods

Colloidal chemical methods are some of the most useful, easiest, and cheapest ways
to create nanoparticles. Colloidal methods may utilize both organic and inorganic
reactants. Typically, a metal salt is reduced leaving nanoparticles evenly dispersed in
a liquid. Aggregation is prevented by electrostatic repulsion or the introduction of a
stabilizing reagent that coats the particle surfaces. Particle sizes range from 1 to
200 nm and are precise by the initial concentrations of the reactants and the action of
the stabilizing reagent. Figure 2 shows the method of formation of gold nanoparticles
as follows: Heat the solution of chloroauric acid (HAuCl4) up to boiling point.
HAuCl4 is a water-solvable gold salt. Add trisodium citrate, which is a reducing
agent. Remain stirring and heating for around 10 min. Throughout time, Na3C6H5O7
(sodium citrate) reduces the gold salt (Au3+) to metal gold (Au0). The neutral Au
atoms cumulate into seed crystals. The seed crystals continue to grow and ultimately
produce Au nanoparticles (Adam D. McFarland et al.):
Examples: Gold

• A common method for preparing colloidal gold nanoparticles involves combining

hydrogen tetrachloroaurate (HAuCl4) and sodium citrate (Na3C6H5O7) in a dilute
solution.
• Upon dissociation, the citrate ions (C6H5O73 ) reduce Au3+ to yield 30–40 nm
gold particles.

Coprecipitation Method

The usage of chemical solution methods permits the formation of high-purity, homog-
enous, multicomponent ceramic precipitates with accurate stoichiometry. The
coprecipitation technique, which has been explored by several investigators [4], can
yield more homogenous powders than those gained by the conventional mixed oxide
technique. However, the essential stoichiometry can be lost throughout the sifting step
when there is a large variance of solubility among the precipitates. Also, as the number
of components rises, it becomes more tough to find an appropriate precipitating agent.
4 Synthesis Techniques for Preparation of Nanomaterials 87

Fig. 2 Formation of gold nanoparticle

These boundaries, to greater extent, can be meticulous by aqueous organic gel tech-
nique which is an alternate way to produce inorganic powder, using polyfunctional
hydroxyl acids and metallic salts to form solvable complexes in aqueous solution. The
clean solution is desiccated to produce the formless solid precursor, which can form the
anticipated compound after firing at higher temperatures. This coprecipitation method
has number of benefits, including homogenous mixing, good stoichiometric control,
and being appropriate for the invention of active residues using less processing times
and commercially existing chemicals. Ethylenediaminetetraacetic acid (EDTA) is a
well-known polyfunctional hydroxyl acid, which is often used in complex-metric
titrations and has fascinated consideration in the creation of a new superconductor
88 S. V. Ganachari et al.

material [5]. EDTA forms constant soluble complexes with most metallic elements
which make this method an adaptable tool in the creation of a new ceramic material.
Sale and co-workers [6] prepared a highly homogenous PZT compound and obtained
optimum electrical properties through EDTA-gel route. These authors also discussed
the remarkable differences observed between the gel-derived and the EDTA-gel-
derived PZT compounds. Our research group has reported the synthesis of monophasic
MoO3 employing this route [7].

Self-Propagating High-Temperature Combustion Method

Conservative synthesis of inorganic ceramic materials habitually involves crushing,

heating, and cooling cycles of appropriate precursors [8]. Reactions typically need
wide-ranging time phases mostly because interdiffusion of responding solids is slow
level at elevated temperatures [9]. Numerous methods have been established
to overcome the solid-state diffusion barrier together with precipitation synthesis [10],
the sol-gel procedure [11, 12], hydrothermal [13], and melt development and creation of
appropriate precursors which have inherent molecular generates or thermal “Achilles
heels” [14]. These developments aim to decrease the diffusion route span of the reacting
mechanisms repeatedly by mixing the essential elements on the atomic scale. They all
have a common relation in that peripheral heating is vital to promote the reaction. These
developments are enormously effective, each method having advantages for certain
applications. Two comparatively new synthetic variations have been established which
contradict the need to superficially heat a reaction; these are based on the self-
propagating reactions which deliver the energy to get over the solid-state spreading
barrier inside, within initial materials, by encouraging an exothermic chemical reaction.
These procedures are named self-propagating high-temperature synthesis (SHS) [15]
and solid-state metathesis reactions (SSM) [16]. SHS permits the synthesis of a wide
variation of materials, such as long-range-ordered alloy compounds, metallic carbides,
nitrides, borides, and oxides [17]. The main property of the self-propagating high-
temperature synthesis also permits innovative practice, for example, inner coating of
pipes, or downregulates radioactive material [18]. Self-propagating high-temperature
synthesis reactions are extremely exothermic. Acceptable heat is liberated in the response
to fire up consecutive coatings of blend; henceforth no outside warming is needed.
The reactions are characterized by fast warming and freezing and may be burnt in two
ways at a point or in substance. From starting point, the reaction takes through circulation
wave which transfers over the reaction mixture. The products necessitate negligible
action to yield single-phase materials. With large commencement, the reactants are
heated in a furnace; once the ignition temperature is reached, the reaction is started in a
variety of places. Regularly this procedure is named “thermal flash.” The main charac-
teristic of SHS is a very less time essential for reaching elevated burning temperatures
due to heat liberated during exothermic reactions. This feature elucidates other detailed
features, such as the high degree of transition, the fractional self-purification from
impurenesses, and the practicability for the shortest preparation of constituents with an
expected structure and undeviating size, shape, and capability constraints.
4 Synthesis Techniques for Preparation of Nanomaterials 89

Sol-Gel Technique

The importance of sol-gel process and chemistry normally in material fabrication has
been growing rapidly. The event of sol-gel process of materials, and particularly of
ceramics, has been defined in various books and reviews [19]. This method is
typically used to formulate MO through the chemical reactions of volatile metal
precursors, routinely alkoxides in association with alcoholic solution, sequent within
the conforming hydroxide.
Hydroxide molecules get condensed and have been associated to eliminate water
that contributes to organize network of robust bases.
Once hydroxide molecules interlinked like structure, then gelation will be
achieved and forms thick porous gel. Chemical compound of a three-dimensional
skeleton adjacent reticular pore indicates the gel. Drying of the gel is based on the
evaporation of solvents and leads to the formation of ultrafine metal OH powder
and will contribute to the conforming ultrafine powder of the MO. Since, this method
is being initiated with a nanosized material and undertakes reactions in nanometer
scale, and that certainly results in nanometer material synthesis.
Sol-gel processes have been suitable for preparing only MO as a result of the
presence of metal-oxygen bonds corresponding to alkoxide precursor, and the
desired gels are basically metal hydroxides or oxides. In recent study [19], a
sol-gel processing technique was developed to produce large number of ceramic
materials, viz., γ-Al2O3, γ-Fe2O3, SiO2, TiO2, etc. However, some studies have
shown that sol-gel processing could be employed to prepare non-oxide powders
from organometallic precursor other than alkoxides [20, 21].
Sol-gel methods have numerous benefits over other methods for synthesizing
nano-powders of MO ceramics. This will contain the creation of superfine poriferous
powder. Therefore, the reproducibility of the invention is the result of stable amal-
gamating of the beginning materials at the molecular level. Sol-gel process is also
having robust potential for creation of employment in industries at higher propor-
tions. Effort has been successfully established for the scaling up of some industrially
important MO nanoparticles.

Reverse Microemulsions/Micelles Method

The revert aggregation method is one among the current assuring ways to nanocrys-
talline materials. Numerous current research have revealed that this impending is a
potential technique for the synthesis of nanocrystalline ceramic powder with specific
and measured properties [22]. Surfactants are dissolved in organic solvent-type
conglomerations known as reverse micelles. Within the existence of water, the
polar head clusters of the surface-active agent molecules organize themselves around
little water polls, resulting in spread of the liquid phase in the uninterrupted oil phase.
Converse aggregates are utilized to formulate nanoparticles through commission-
ing water solution of responsive predecessors and may be modified over to indis-
soluble nanomaterials. Nanoparticle synthesis within the micelles may be modified
90 S. V. Ganachari et al.

over to indissoluble nanoparticles. Nanoparticle synthesis within the micelles may

be achieved by various approaches, letting in hydrolysis of responsive precursors,
like alkoxides and metal salt precipitation. Removal of persisted solvent along with
calcination process can able to form the ultimate product. Spreading of the surfac-
tants could be utilized during accomplishment of these procedures, like
decaoxyethylene nonyl phenyl ether (TNT-10), pentadecaoxyethylene nonyl phenyl
ether (TNP-35), poly(oxyethylene) nonyl phenol ether (NP5), and many other
solvents that are commercially accessible. Various parameters, especially quantity
of the reactive precursor within particle, the mass proportion of the liquid phase in
macroemulsion, particle size, distribution of particle size, and agglomerate size and
phases of the eventual ceramic powder. Through exploration of this method, there
will be an associated advantage. Very small particles can be prepared that have got
the potential to regulate the particle size. Difficulties include low production capacity
and being bound to utilize immense quantity of liquid [23–25].

Spray Pyrolysis

Spray pyrolysis is a helpful technique to synthesize the higher purity and consistent
ceramic powder [26–32]. This technique can be called using different names, such as
solution aerosol thermolysis [29–32], phase transition decomposition of solution,
plasma evaporation of the sample solutions, and aerosol decomposition [29–32]. The
starting materials required during this technique are chemical precursors, generally
acceptable when the solution contains salts, sol, or suspension. Figure 3 shows spray
pyrolysis system overview. Thus, the method comprises formation of aerosol

Cooling Collecting filter

Nitrogen
carrier gas

Flame
Vacuum Spray
pump

Precursor
solution

O2
Feed gas Ultrasonic
vibrator

Fig. 3 Pyrolysis: system overview

4 Synthesis Techniques for Preparation of Nanomaterials 91

droplets by nebulization or “atomization” of the beginning solution, sol, or suspen-

sion. Evaporation of droplets created takes place with concentrated droplet, and the
precipitation of the particle can be carried out through thermolysis process that forms
microporous particles and ultimately that will create dense particle [75–78].
An extensive variability of ceramic materials has been prepared using this
method, including MgO, Al2O3, and ZrO2. Nitrate salts and metal chlorides can be
utilized as precursors, because of their increased solvability. The precursors having
low solubility will influence the impurenesses, like C2H3O2 that contribute to
carbon formation in the product, and it is not well-linked [26–31].
The conversion of the atomizer droplets into the particles comprises many pro-
cedures, properties in solvent disappearance, snow of liquified precursor, and pre-
cipitated particle thermolysis. All of those ways take place in one step that represents
associate degree advantage of this methodology. Different edges contain the assem-
bly of nanosized particles of high purity, reliability of the particles resulting,
similarity of initial resolution, and also the facts that every particle will undergo
corresponding reaction circumstances where no sequent edge is important. One of
the main disadvantages of spray transformation is that it will embrace with massive
amount of solvent requirement and also has problem of scaling up of the assembly.
Using huge amount of nonaqueous solvents will increase the assembly expenses, as
a result of the costly pure solvents to have an acceptable discarding process.

Thermochemical/Flame Decomposition of Metal-Organic

Precursors

Flame procedures are broadly accustomed nanosize powder for synthesizing ceramic
materials. Basically, it is a kind of gas compression technique and the starting constit-
uent is liquid chemical precursor. This method is known as chemical vapor condensa-
tion (CVC). Chemical precursor area unit will be gasified before change in exceeding
combustion process by engaging fuel-oxidant amalgamate like propane-oxygen or
methane-air. This method indicates the fast energy breakdown of a precursor carrier
steam in a remarkably condensed product particle upon the cold substrate. Flame
sometimes delivers much higher temperature (1200–3000 K), and it will enhance the
rapid gas phase chemical reaction. Many forms of flame reaction are being used. One
example of those reactors could be a diffusion flame reactor during which the mix
processes are in the main defined interdiffusion of the oxidizing agent and the fuel. The
utmost flame temperature typically happens at the tip of flame wherever cumulations
coalesce and leave the flame. As they leave the flame, the flame temperature drops
quickly and particles still coalesce while not sintering, leading to large agglomerates of
primary particles. A spread of ceramic nanoparticles is with success ready by this
system, as well as TiO2 and SiO2 [33]. The advantage of a diffusion flame reactor is that
it provides a stable flame over a large range of process conditions.
A diversity of chemical precursors has been used, letting in metal chlorides like
titanium tetrachloride to prepare titanium dioxide and silicon tetrachloride to prepare
silicon dioxide [26–28, 34]; metal alkyl precursors; metal alkoxides; and gaseous
92 S. V. Ganachari et al.

metal hydrides, such as silane as a basis of silicon to prepare silica. Chlorides are the
utmost used precursors within the industry, and process is typically mentioned as
“chloride process.” The high pressure of chlorides and thus the undeniable fact that
they’ll safely be kept and handled build them wonderful possible precursors. The
disadvantages of exploiting chloride precursor lead to development of harmful acidic
gases and pollution of the product with salt residues. Flame processes area unit used
industrially to produce commercial numbers of ceramic particulates, like oxide,
titania, etc. Usually this can be often thanked to the low price of production as
compared to any or all alternative ways. The disadvantage of flame synthesis is that
the control of particle size (both primary particle and aggregate size), surface, and
section composition is tough and restricted.

Self-Propagating Low-Temperature Synthesis (SPLTS)

Combustion synthesis (CS) [35] has appeared as a significant method for the
preparation and process of advanced ceramics (structural and functional), catalysts,
composites, alloys, intermetallics, and nanomaterials. In CS, the exothermicity of the
oxidation-reduction (reduction-oxidation) reaction is used to produce helpful mate-
rials. Contingent upon the character of reactants, elements, or compounds and,
therefore, the exothermicity (adiabatic temperature, T), CS is delineated as self-
propagating high-temperature synthesis (SHS), low-temperature combustion syn-
thesis (LCS), solution combustion synthesis (SCS), gel-combustion, sol-gel com-
bustion, emulsion combustion, bulk combustion, etc. Combustion preparation
processes are characterized by high temperatures, fast heating rates, and short
reaction times. These features create CS an attractive technique for the production
of technologically helpful materials at lower costs compared to traditional ceramic
processes. Other benefits of CS are:

• Use of comparatively easy instrumentation

• Establishment of high-purity products
• Equilibrium of constancy phases
• Development of nearly any size and shape products

The literature on combustion synthesis is large, and most of the materials

prepared and their applications are abridged in recent publications [33,
36–38]. The popularity of the method is reflected within the large number of
publications on metal shown within the Materials Science journals and a decade
of publication of the International Journal of Self-Propagating High-Temperature
Synthesis (Allerton Press, New York).
Combustion synthesis of oxide materials utilizes redox compounds and intermix-
tures (self-propagating low-temperature synthesis). A completely diverse impending
of synthesis involves the utilization of flammable precursors (reduction-oxidation
compounds) and chemical reaction mixtures. It uses cold (<500  C) originated
gas-producing exothermal reactions that are self-propagating and yield large fine
4 Synthesis Techniques for Preparation of Nanomaterials 93

particle oxides in few minutes. Compounds like (NH4)2Cr2O7 that contain every
oxidizing (Cr2O72 ) and reducing (NH4+) groups once properly lit (using
KClO3 sucrose-H2SO4) decompose autocatalytically to yield capacious inexperi-
enced Cr2O3.
The exothermicity of the combustion is attributable to the oxidization of NH4+ to N2
and H2O by the dichromate particle that itself is reduced to Cr3+. The combustion is
smoldering type (flameless) and is escorted by the evolution of gases leading to fine,
voluminous Cr2O3 powder. A brand-new category of precursors containing a carbox-
ylate anion, hydrazide, hydrazine, or hydrazinium groups was unintentionally initiated
to ignite at low temperature (120–350  C) and break down autocatalytically to yield
fine particle, massive extent oxides. The high exothermicity of combustion was
attributed to the chemical reaction of sturdy reducing moieties like COO , N2H3 ,
N2H4, or N2H5+ by atmospheric oxygen to carbon dioxide, H2O, and N2. The prepa-
ration, crystal structure, and reactivity of various ignitible precursors are reported [39].
Although the preparation of fine particle compound materials by the combustion
of reaction compounds is easy and engaging, it sure has limitations. Firstly, the
preparation of the precursors desires many days. Secondly the yield is simply ~20%
of the precursor. To conclude it is not feasible to use the presented system to organize
high temperature oxides like chromites, alumina, etc as metal complexes used with
reducing agent are not fruitful in nature.
A substitute technique to the flammable reaction compounds is the use of the
reaction mixtures (oxidizer – fuel) like gunpowder (KNO3 + C + S) or solid
propellant (NH4ClO4 + CTPB + Al) that once ignited undergo self-propagation
combustion. The temperature of the reaction doesn’t exceed over <500  C, and
therefore the method is also termed self-propagating low-temperature synthesis.

Microwave-Assisted Technique

Microwave (MW) heating has been renowned since the early 1940s and has been
used with success within the food industry. The MW technique has found variety of
applications in chemistry since 1986. As of late, the utilization of microwaves has
been found to offer many benefits for the preparation of many inorganic materials as
compared to traditional impending. The foremost of those benefits are the very short
time periods concerned within the preparation, improved reaction kinetics, and
therefore the reactant selectivity throughout energy transfer from the microwave
field. Moreover, the high reaction rates throughout microwave treatment open up the
possibility, the likelihood, and the chance of retaining the nanostructures from nano-
powders when processed and therefore the possible action of preparing metastable
high-temperature phases. Additionally significantly, the effect of heating is made by
the interaction of the permanent moment of the molecule with the high-frequency
(2.45 GHz) nonparticulate radiation that results in consistent and quick thermal
reactions. Moreover, it’s very simple to use microwave equipment for continuous
synthesis of huge amounts of products. This can be important for getting products in
bulk quantities in industry [40–42].
94 S. V. Ganachari et al.

Numerous inorganic materials are prepared using microwave energy for several
applications. Rao et al. have reviewed this subject very well. Microwave irradiation
as a heating technique, which is usually quite quick, easy, and competent in energy,
has been established and widely utilized in the fields like molecular sieve prepara-
tion, radiopharmaceuticals, preparation of inorganic complexes and oxide, organic
reactions, plasma chemistry, analytical chemistry, catalysis, and, recently, the prep-
aration of nanocrystalline particles [43, 44].
Unfortunately, the precise nature of the fundamental interaction of the micro-
waves with the reactants throughout the preparation of materials is somewhat
unclear and speculative. However, it’s commonplace that the interaction of stuff
materials, liquids or solids, with microwaves ends up in what is usually brought up
as dielectric heating. Electrical dipoles present in such materials resonate in the
applied field. In liquids, this constant reorientation ends up in friction between
molecules that in a while generates heat [45]. Compared with standard methods,
microwave preparation has the advantages of short time interval, small particle size,
slender particle size probability distribution, and eminent pureness.

Solution Combustion Technique

The solution primarily grounded combustion synthesis of advanced materials, pre-

dominantly the nanocrystalline ceramics and composites, has scientific and also
high-tech importance [46]. A series of such solution combustion decomposition
(SCD) methods are supposed to yield single-phase produce of assorted multi-
component ceramics, where the heat created throughout exothermic chemical reac-
tion/chemical change chemical action of combustion process is used to complete the
phase formation of the products. Numerous chemicals like acid, urea, glycol,
glycine, TFTA, etc. are normally getting used as flammable agents for those com-
bustion processes. The solution combustion technique using citric acid, which is
widely referred to as amorphous citrate method, could be an inexpensive method.
It uses readily accessible starting materials, particularly metal nitrates with citric acid
as fuel/complexing agent, and is found to be extremely promising in manufacturing a
spread of amorphous and nanocrystalline ceramic powders [47]. Fascinatingly, some
of the fuels used were found to be specific for a specific category of oxides, e.g.,
carbamide, for aluminum oxide and connected compounds; CH, for zirconium oxide
and related compounds; ODH, for Fe2O3 and ferrites; TFTA, for TiO2 and related
compounds; and glycine, for chromium and related oxides.

Hydrothermal (HT)/Solvothermal (ST) Synthesis

Hydrothermal, coprecipitation, combustion, sol-gel, precursor, spray drying,

freeze-drying, macroemulsion, and reverse particle techniques [48] are some
ways for synthesizing nanosized ceramic materials. Among the mentioned
4 Synthesis Techniques for Preparation of Nanomaterials 95

Fig. 4 Hydrothermal bomb

methods, the method of precipitation from solution under hydrothermal condi-

tions is one among the soft chemical routes; at comparatively low temperatures,
current attention is engaging for the direct preparation of crystalline ceramic
particles. Generally,hydrothermal reactions were conducted in an autoclave at
temperatures between the boiling and significant points of water (100–374  C) at
raised pressure (up to ca. 15 MPa). Recently, the ultra-fine powders of various
ceramics nanoparticles are prepared by the hydrothermal techniques
[49]. Results have excellent consistency and particle uniformity. Figure 4
shows hydrothermal bomb.
Important benefits of synthesis techniques under hydrothermal conditions over
alternative chemical synthesis are as follows: It is simple to regulate morphology
and particle size by various synthesis conditions. Next numerous materials are
continually prepared directly within the anticipated crystalline state at low tem-
perature. Lastly, an elemental oxidation state material may be produced in a very
sol form, and the resulting sol may be used in production of green bodies by
pressure filtration or extrusion [50]. Chemically synthesized nanostructured pow-
ders possess higher chemical consistency and a fine particle size adjacent to higher
control of particle morphology as an outcome of nucleation and particle growth
occur underneath these circumstances. These features of very fine ceramic pow-
ders at lower temperatures enhance the sinterability and in addition produce a
consistent fine-grained sintered microstructure, which possesses higher mechani-
cal or electrical properties.
Several researchers refer this technique as solvothermal [51], in special case
where solvent being water referred to as hydrothermal. To regulate grain size,
particle surface morphology, crystalline state, and surface interaction by control
sol composition, response temperature, pressure, property of solvent, additives,
and aging time solvothermal treatment may be valuable.
96 S. V. Ganachari et al.

Alginate Template Technique

Biomineralization methods have become a source of motivation for the planning

of organic-inorganic hybrid nanomaterials. Diverse biological systems, like pro-
teins, polysaccharide, DNA, or combinatorial phage show peptide libraries, have
already been prepared to direct the growth of such nanoparticles. For nanopar-
ticle growth, alginic acid exhibits many attention-grabbing options which may
vary from possible templates. Algin might be present as di- and trivalent cations
in saccharide that forms rigid cross-linked gels. This natural polymer brown
marine protoctist (Phaeophyceae) is widely found over the planet’s coasts. It is
an inexpensive and eco-friendly chemical agent; however, its use might contrib-
ute to the valorization of a nonconventional biotic resource. Figure 5 shows the
scale-dependent properties of nanoparticles/materials. Figure 6 shows the algi-
nate template technique; alginate solution is dripped, one drop at the time from
an oversized syringe into solution of calcium chloride. The beads are instantly
shaped within the CaCl2 solution.
Recently, combination of micrometer scale iron oxides into the calcium cross-
linked gel magnetic types of alginate is made. Additionally, alginic acid conjunct
with different polysaccharides aided as templates for the preparation of varied
magnetic substrates. Brayner et al. and Kroll and Winnik have recently reported
the in situ preparation of γ-Fe2O3 and alternative magnetic nanoparticles by metal
cross-linked alginate gels [52–55].

Fig. 5 Size-dependent properties

4 Synthesis Techniques for Preparation of Nanomaterials 97

Fig. 6 Alginate template

technique

Liquid-Liquid Interface Technique

By variety of methods, ultrathin films of inorganic materials are developed

[56–58].Thermal evaporation, optical device ablation, vacuum sputtering, and
molecular beam are the physical ways growing essentially which involve the
evaporation of reactants using elevated energy tagged along by condensation on
a substrate yielding thin films of materials. Chemical vapor deposition (CVD) and
electrodeposition typically use milder conditions. In the recent history, thin films of
nanocrystals were prepared using the Langmuir-Blodgett [LB] technique. Thus,
lean films of Au nanocrystals and alternative materials [59] by the LB technique
are at the air-water interface. The properties and features of a thin film typically
rely upon the nature of the substrate and similarly on the conditions and tech-
nique used for making the film. Thus, lean films are made of polycrystalline or
possess island structures usually of inorganic materials. Since it’s not habitually
simple to get vigorous films of nanocrystals through self-assembly, it would be
beneficial to plot an acceptable technique to get ultrathin films that are
98 S. V. Ganachari et al.

continuous over a wide area and are single crystalline in nature. During this
context, the liquid-liquid interface supported in making nanocrystalline films of
metals, metal chalcogenides, and oxides. In contrast to the other ways, crossing
point between unmixable liquids is well-known to be ideal for assembling of
mixture particles. On the other hand, Brust et al. studied the water-organic
solvent unmixable mixture reagents to prepare metal organosols in the presence
of phase transferring. Experiments by Rao et al. unrestrained that it had been so
attainable to arrange nanocrystals of metals and alternative materials at the
liquid-liquid interface through the reaction of an organometallic precursor
taken within the organic layer with an applicable reagent within the liquid
layer. Rao et al. in addition distributed the deep experiments on nanocrystalline
CuS and CuO films obtained at the interface which he found to be basically
single crystalline in nature [60].
Liquid-liquid interface technique may be a single synthesis step, which enables
synthesis of nanocrystal arrays under ambient conditions. In this technique, the
reaction of an organometallic compound dissolved in the organic layer with a
reducing, a sulfiding, or an oxidizing agent is involved within the liquid layer.
The material formed is ultrathin nanocrystalline film at the interface level consisting
of closely packed nanocrystals. Ultrathin nanocrystalline film consisting of closely
packed metal/MO nanocrystals coated with the organic species was carefully
assessed at the interface. The opposite benefits of this invention are as follows:
delicate reaction conditions, straightforward to control, short method period, and
simple to industrialize.

Biosynthesis of Biofunctionalized Noble Metal Nanoparticles

The development of hybrid nanomaterials integrates the exceptionally selective

catalytic and recognition properties of biomaterials, such as with the distinctive
electronic, photonic, and catalytic features of nanoparticles mainly based on
the convergence of biotechnology and engineering science [61–63]. Nano-
biotechnology has a striking space of research in conjugation with nanoparticles
and alternative nanoobjects (e.g., nanorods and nanotubes) with biomolecules [56].
Within the dimensions of 2–20 nm, enzymes, antigens, antibodies, and biomolecular
receptors have their size which is similar to nanoparticles; as a result, both the
categories of materials are structurally compatible.
Nearly all the multicellular organisms have hard tissues, which are composed of
inorganic materials. Minerals of 60 different forms play a significant role in struc-
tural, mechanical, and physiological functioning in the living organisms.
Minerals such as CaCO3, Ca3 (PO4)2, etc. play a vital role in cellular organisms
and living things. Microorganism and protoctist are capable of synthesizing inor-
ganic materials, each intra- and extracellularly [64–66], for instance, sponges syn-
thesize biosilica, magnetic particles are synthesized by magneto-tactic
microorganism, biosilica is synthesized by diatoms, and S-layer microorganism
synthesizes mineral and carbonate as surface layers [67–69].
4 Synthesis Techniques for Preparation of Nanomaterials 99

Actinomycetes

Ahmad and co-workers reported the intracellular biogenesis of gold nanoparticles.

The organism used was Rhodococcus sp. which is an alkalotolerant actinomycete.
The gold nanoparticles obtained showed an honest monodispersity with size starting
from 5 to 15 nm. The particles were found on the cell membrane similarly as on the
plasma membrane however in a very larger quantity within the former. This obser-
vation was in all probability because the presence of enzymes within the cell
membrane results in reduction of the gold ions. The metal ions weren’t poisonous
to the cells, and they remained viable even with the reduction of gold ions.
Ahmad and co-workers have conjointly reported the biomass of chloroaurate ions
involved in the generation of gold nanoparticles by extracellular chemical process. It
was determined that 8 nm is an average size for the formation of nanoparticles at a
high concentration of gold solution. The precise mechanism resulting in the reduction
of the metal ions within the organism has not however been elucidated. In the cluster
of primary step was proteins released into water by the organism were analyzed in
terms of variety of proteins secreted and their molecular weights. Four totally
different proteins with molecular weight of 10–80 KDa were examined in preliminary
gel natural action analysis. It’s believed that one or more copy of those proteins could
also be enzymes that reduce the chloroaurate ions and cap the gold nanoparticles
formed by the reduction method. It’s additionally possible that totally different pro-
teins have an effect on caing and stabilizing of the gold nanoparticles [32, 70, 71].

Yeast

The biogenesis of quantum crystallites in yeast is reported in Candida glabrata

and Schizosaccharomyces pombe refined with the presence of cadmium salt.
Short chelating peptides of general structure control the nucleation and growth
of CdS crystallites (a well-known semiconductor material) to peptide-capped
intracellular particles of diameter 20 nm. Kowshik and co-workers reported the
intracellular synthesis of cadmium sulfide nanoparticles by S. pombe strain once
challenged with 1 mM atomic number 48 solution. The CdS nanoparticles
exhibited an absorbance most at 305 nm. X-ray scattering information showed
that the nanoparticles had Wurtzite sort hexagonal lattice structure and most of the
nanoparticles were within the varying sizes of 1–1.5 nm. The nanoparticles were
employed in the fabrication of heterojunction with poly-(p-phenylenevinylene).
The diode exhibited ~75 mA/cm2 current at 10 V when forward biased and a
breakdown at ~15 V within the reverse biased mode. These characteristics are
considered ideal for a diode. This particular study was the primary of its kind
within the application of biogenic nanoparticles in optoelectronic electronic
devices. Living thing synthesis of silver nanoparticles was observed in silver-
tolerant yeast strains MKY3 once challenged with 1 mM soluble silver within the
log section of growth. It had been shown that silver wasn’t reduced once the
supernatant of MKY3 culture (grown within the absence of silver) was exposed to
100 S. V. Ganachari et al.

an environment of silver ions. It had been reported that though the precise
mechanism resulting in reduction of silver ions to elemental silver is however to
be elucidated, it’s possible that certain organic chemistry reducing agents are
secreted by yeast cells in response to silver stress. TEM and X-ray diffraction
analysis confirmed that gold-bearing silver nanoparticles of size 2–5 nm were
being shaped. Extracellular synthesis of nanoparticles may well be extremely
advantageous from the purpose of view of synthesis in large quantities and easier
downstream processing as compared to the intracellular synthesis [33–35].

Fungi

Cost-effective and eco-friendly method of synthesizing colloidal silver nano-

particles by using the extracellular extract of fungi Penicillium diversum. AgNPs
were synthesized by biomass of P. diversum strain and were evaluated against
pathogenic bacteria drug-resistant E. coli. The nanoparticles were synthesized
extracellularly by P. diversum strain adopting standard conditions, and the synthe-
sized purified particles were characterized by using UV-Vis spectroscopy, FTIR,
XRD, AFM, and TEM. UV-Vis spectroscopy revealed the formation of AgNP with
the range between 5 and 45 nm, and the same is confirmed by AFM as well as
TEM. The antibacterial activity with AgNP shows the distinct effect and minimum
inhibitory concentration (MIC) at a different concentration of 5 μg/ml for E. coli.
In our current investigation, the biological synthesis of AgNP by nonpathogenic
strains of the fungus P. diversum and the synthesized AgNP were found to be most
active against the clinically isolated human pathogenic bacteria. The results proved
that the thus obtained AgNPs showed maximum activity at the least concentration,
which proved these functionalized AgNPs are novel antibacterial agents [72].

Higher Plants

Shankar and co-workers reported use of Geranium leaves (Pelargonium

graveolens) and its endophytic fungus within the extracellular preparation of
gold nanoparticles. Decontaminated Geranium leaves and an endophytic fungus
(Colletotrichum sp.) growing within the leaves were distinctly exposed to liquid
chloroaurate ions. In each case, speedy reduction of the metal ions was ascertained
leading to the development of stable gold nanoparticles of variable size. Within the
case of gold nanoparticles prepared using herb leaves, the reducing and capping
agents appear to be terpenoids, whereas they’re known to be polypeptides/
enzymes within the case of Colletotrichum sp. The biogenic gold nanoparticles
synthesized by using the extracellular extract of fungus were primarily spherical in
shape, whereas the particles grown-up mistreatment the leaves exhibited a range of
shapes that enclosed rods, flat sheets, and triangles. Gardea-Torresdey and
co-workers reported the development of gold nanoparticles within live alfalfa
plants. Alfalfa plants were grown up in HAuCl4-made environment. The seeds
4 Synthesis Techniques for Preparation of Nanomaterials 101

were soaked in the third formaldehyde to avoid contamination by fungus and

completely washed thrice with deionized water. The seeds were then transferred to
nutrient medium to permit plant growth to require place. Gold (III) from K
tetrachloroaurate was further in several concentrations in several jars containing
the seeds. Four replicates of every treatment were ready at the optimum hydrogen
ion concentration of 5.8. The plant growth conditions were maintained at 12-h
photoperiod and dark period. The alfalfa plant was harvested when 2 weeks of
growth, washed totally, frozen in liquid nitrogen, and so placed in a very freeze-
dry system for 2 days. The absorption of Au metal by the plant was confirmed by
X-ray absorption studies (XAS) and TEM. Atomic resolution analysis confirmed
the nucleation and growth of Au nanoparticles within the alfalfa plant. [36–38].
Armendariz and co-workers studied oat (Avena sativa) biomass as an alternate to
convalesce Au (III) ions from liquid solutions and for its capability to scale back Au3+
to Au0 forming Au nanoparticles. To review the binding trend of Au3+ to oat and
therefore the possible formation of Au nanoparticles, the biomass and a solution of
Au3+ were reacted for an amount of one unit of time at hydrogen ion concentration
values ranging from 2 to 6. The results demonstrated that Au3+ ions were certain to
oat biomass in a very pH-dependent manner, with the highest sorption (about 80%) at
hydrogen ion concentration 3. These studies additionally showed that the hydrogen
ion concentration of the reaction influenced the nanoparticle size. The smaller
nanoparticles and therefore the higher occurrence of those were observed at hydrogen
ion concentration values of 3 and 4, while the larger nanoparticles were observed at
hydrogen ion concentration [73, 74].

Conclusion

Nanomaterials are extensively investigated throughout the last decade, thanks to

their large choice of applications. It’s ascertained that field of nanomaterial synthesis
is incredibly dynamic. Several synthesis techniques like colloidal methods,
coprecipitation method, self-propagating high-temperature combustion method,
sol-gel technique, reverse microemulsions/micelles method, spray pyrolysis, ther-
mochemical/flame decomposition of metal-organic precursors, self-propagating
low-temperature synthesis, microwave-assisted technique, solution combustion
technique, hydrothermal (HT)/solvothermal (ST) synthesis, alginate template tech-
nique, liquid-liquid interface technique, and biosynthesis of biofunctionalized noble
metal nanoparticles using microorganisms like actinomycetes, yeast, etc. and higher
plants like plant leaves, flower petals, root, stem, bark, etc. Nanomaterials ready for
exploitation processes include a large variety.

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