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Methods of Chemical Synthesis in the Synthesis of Nanomaterial

and Nanoparticles by the Chemical Deposition Method: A Review
Kadda Hachem1 · Mohammad Javed Ansari2 · Raed Obaid Saleh3 · Hamzah H. Kzar4 · Moaed E. Al‑Gazally5 ·
Usama S. Altimari6 · Shaymaa Abed Hussein7 · Halah T. Mohammed8 · Ali Thaeer Hammid9 · Ehsan Kianfar10,11

Accepted: 23 May 2022

© The Author(s), under exclusive licence to Springer Science+Business Media, LLC, part of Springer Nature 2022

Abstract
Chemical vapor deposition (CVD) is a vacuum deposition method used to produce high-quality and high-performance solid
materials. The process is often used in the semiconductor industry to produce thin films. Microfabrication processes widely
use CVD to deposit materials in various forms, including monocrystalline, polycrystalline, amorphous, and epitaxial. These
materials include silicon (dioxide, carbide, nitride, oxynitride), carbon (fiber, nanofibers, nanotubes, diamond, and graphene),
fluorocarbons, filaments, tungsten, titanium nitride, and various high-k dielectrics. Chemical deposition takes advantage of
the chemical reaction where the product self-assembles and deposits on a suitable substrate. Chemical deposition is com-
monly used for generating thin nanostructured blend films of crystalline inorganic materials, such as ZnS, CuSe, InS, CdS,
etc. Depending on the deposition conditions, several terms have been used, such as chemical bath deposition, CVD, and
ECD. Depending on the material and the deposition conditions, different surface morphologies have been obtained, from
nanopins to nanotubes to nanorods. Reagents in sedimentary reactions are usually water-soluble ionic compounds. When
these compounds are dissolved in water, they separate from each other to form anion and cation ions. If a cation of one com-
pound forms an insoluble compound with an anion of another compound, precipitation occurs. Applications of this method
include the removal of heavy metals and anions from wastewater, reducing water hardness, and metal recovery. Synthesis
processes occur by chemical deposition based on deposition reactions (substitution), co-precipitation, oxidation–reduction,
thermolysis, hydrolysis, polymerization, and condensation. The control of various variables in a synthetic system plays an
important role in controlling particle size and morphology. The products of sedimentary processes under various synthetic
conditions range from coarse crystals to nanostructured colloidal particles. Co-precipitation chemical methods allow the
synthesis of metal nanoparticles, metal oxides, as well as many metal semiconductor compounds. Also, a wide range of
properties and characteristics can be achieved by changing the synthesis conditions. The basis of these methods is the prepa-
ration of products from soluble precursors using different systems such as electrochemical equipment, microwave radiation,
ultrasound, and high-energy beams.

Keywords Nanoparticles · Chemical deposition · Chemical synthesis · Electrochemical

1 Introduction have deposited zinc tetradecanoate film via potentiostatic

electrolysis of tetradecanoic acid using zinc as the work-
A chemical deposition involves a reaction wherein the prod- ing electrode [1]. Deposition of Zn(CH3(CH2)12(COO)2)
uct self-assembles and coats the substrate. It can be further on the zinc surface caused its contact angle to change from
divided into chemical vapor deposition, chemical bath depo- 62° ± 3° for bare zinc to 152.5° ± 3°. The petal structures
sition, and electrochemical deposition. Recently, Wang et al. (see Fig. 1) with low surface energy found on the zinc
surface caused superhydrophobicity. They observed a five
order-of-magnitude decrease in capacitance and a dramatic
* Kadda Hachem
kadda46@[Link] increase in the resistance because of the air trapped between
these structures.
* Ehsan Kianfar
ehsan_kianfar2010@[Link] The carbonyl method is one of the most widely used
methods of chemical deposition [3–7]. Physical and
Extended author information available on the last page of the article

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Fig. 1  Contact angle photo-

graphs of zinc coated with
superhydrophobic film (left)
and surface morphology of
the superhydrophobic coating
(right) [2]

chemical techniques of gas-phase manufacturing of metal

Table 1  Advantages and disadvantages of “top–down” synthesis [22]
powders have a common theoretical basis. A chemical
reaction may account for the formation of the metal vapor; Advantages Disadvantages
its precipitation may occur because of simple condensa- Large-scale production Size distribution (10–100 nm)
tion. At the same time, the evaporation–condensation pro- It is possible to deposit on a large Expensive technique
cesses also involve chemical interactions. The process of substrate
chemical vapor deposition (CVD), mainly of high-purity No chemical purification is required Various particle shapes
refractory metals, requires reagents that are able to vapor-
ize without decomposition, form a sufficient concentra-
tion of the vapor of the metal-containing compound, and
give, upon decomposition of the latter and deposition of 2 Methods of Elaboration
the metal, only gaseous and chemically inert substances.
The products obtained from the various chemical depo- 2.1 Sol–gel Method
sition reactions cover a wide range of material structures
(from coarse crystals to nanostructured colloidal parti- The sol–gel method was first described by the chemist
cles). Solutions containing colloidal fine particles remain Ebelmen [23] in the mid-nineteenth century. The soil is a
stable for days and months without precipitation (due to colloidal suspension of oligomers (“oligomer = monomer
brown movement) [3–5]. In contrast, coarse-grained par- molecular complex” whose diameter is several nanom-
ticles precipitate rapidly. Coarse sediments can be easily eters). Thereafter, this “soil” may be developed by chemi-
separated by processes such as filtration, centrifugation, cal reactions, i.e. polycondensation or polyesterification,
or decantation. Chemical deposition processes have a forming alcohol molecules in the bridges until gel for-
complex mechanism, so in many cases, their mecha- mation. This freezing process offers many advantages for
nisms are still unknown. In this article, the mechanisms producing large materials with homogeneity and purity at
of such processes are described separately and in simple lower temperatures than conventional methods. Thus, the
language [6, 7]. By choosing the right reaction variables, gel obtained is subjected to the drying process, and the
different stages of synthesis can be controlled and nano- resulting product is transformed into xerogel, followed by
structures with the desired size and morphology can be a heat treatment that will eventually form powder [5, 6].
produced [8–12]. In this paper, some of the most impor- The sol–gel method does not involve melting or sintering
tant methods of synthesis of metal nanoparticles, metal powders to produce ceramic but uses a solution contain-
oxides, and metal chalcogenides using chemical deposi- ing reactive precursors such as alkoxides or metal salts.
tion methods from aqueous and non-aqueous solutions, The precursors for the preparation of a colloid consist
as well as methods of thermal decomposition, microwave of a metal or metalloid element surrounded by various
radiation, and ultrasonic radiation are discussed [13–21]. ligands. Metal alkoxides (R-O-M) are similar to alcohols
The methods of synthesis of nonmetric structures include (ROH) with a metal atom M, replacing hydrogen H in the
two approaches, depending on the precursors used: (a) hydroxyl group. They are the class of chemical precursors
top–down and (b) bottom–up. The advantages and disad- most commonly used in sol–gel synthesis because they are
vantages are presented in Tables 1 and 2. subject to hydrolysis depending on the amount of water
and the catalyst present. The advantages and disadvantages
of this process are presented in Table 3.

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Table 2  Advantages and Advantages Disadvantages

disadvantages of “bottom-up”
synthesis [22] Obtained nanoparticles, nanotubes • Large-scale production is difficult
The deposit parameters can be controlled • Chemical purification of nanoparticles is required
It is possible to distribute the narrow size (1–20 nm)
Cheaper technique

Table 3  Advantages and disadvantages of the sol–gel method [23]

Advantages Disadvantages

Can produce a thin coating to ensure excellent adhesion between the substrate and the top layer The contraction that occurs during processing
Can produce a thick coating to provide protection against corrosion Residual hydroxyl and/or carbon groups
It has the capacity of sintering at low temperatures, between 200 and 600 °C Long processing time
Simple, economical, and efficient method to produce high-quality coverage Fine pores

Table 4  Advantages and disadvantages of the Pechini method [24]

Advantages Disadvantages

Versatility Use of toxic ethylene glycol and organic reagents

Almost complete independence of the process conditions of the posi- The lack of stable citric complexes of elements (bismuth, silicon, etc.),
tive ion chemistry contained in the final material as well as the partial or complete regeneration of one of the compo-
The relatively low temperature of the precursor, due to which the nents during the pyrolysis of the polymer gel (for example copper,
process can occur almost completely without sintering lead, zinc, ruthenium, etc.)

Table 5  Advantages and Advantages Disadvantages

disadvantages of the
microemulsion method [28] They are easy to prepare and do not require an energy contribution during A large amount of surfactants
synthesis
The preparation is due to better thermodynamic stability Temperature stability is
influenced by microemul-
sion, pH
The formation of the microemulsion is reversible Limited solubility capacity
for substances with high
melting points

2.2 Polymer Precursor Method—Pechini Method 2.3 Microemulsion Method

The method was proposed in 1967 as a technique for depos- Microemulsions are isotropic solutions, macroscopically
iting titanium and niobium dielectric films and alkaline- homogeneous and thermodynamically stable, containing
earth metals in condensation production. Later, the process at least three components, namely, a polar phase (usually
was customized for the synthesis of oxide materials in the water), a nonpolar phase (usually oil), and a surfactant.
laboratory. The method is based on the intense mixing of the At the microscopic level, the surfactant molecules form
positive ions in a solution, the controlled transformation of an interphase film that separates the polar and nonpolar
the solution into a polymeric gel, the removal of the poly- domains. This interface layer forms different microstruc-
meric matrix, and the development of an oxide precursor tures, ranging from oil droplets dispersed in a continuous
with a high degree of homogeneity [24]. During the syn- aqueous phase (oil/water microemulsion) to a bicontinuous
thesis process, metal salts or alkoxides are introduced into a phase with water droplets dispersed in a continuous oil phase
solution of citric acid with ethylene glycol. The advantages (water/oil microemulsion) [25–28]. The advantages and dis-
and disadvantages of the polymeric precursors’ method are advantages of the microemulsion method are summarized
presented in Table 4. in Table 5.

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2.4 Hydrothermal Method 3 Methods of Chemical Synthesis

in the Synthesis of Nanomaterial
The hydrothermal method consists of obtaining nanomateri-
als through hydrolysis reactions at high temperatures of the In the process of synthesizing nanomaterials, the production
various compounds directly in an autoclave. The synthesis can of nanoparticles whose size distribution range is very small
have precursor products obtained previously at room tempera- (their particle size is very close to each other, monodisperse)
ture based on the crystallization of the phases under high tem- is very important, and the synthesis process is valuable when
peratures and pressures. Hydrothermal synthesis can be per- the difference in particle size is less than 5%. Nanoparticles
formed both at temperatures and at pressures below the critical that are very close to each other in size have homogene-
point for a specific solvent, over which the differences between ous and special properties that make them widely used in
liquid and vapor disappear, and under supercritical conditions. industrial products [13–15]. Therefore, providing methods
The solubility of many oxides in hydrothermal salt solutions is for the synthesis of nanoparticles with a range of small and
much higher than in pure water (such salts are called mineral- homogeneous size changes on an industrial scale is very
izers). There is also a group of solvothermal synthesis meth- important [33, 34]. In general, chemical synthesis involves
ods related to hydrothermal methods; this group of methods is the process by which a product precipitates from a liquid (or
based on the use of organic solvents and supercritical C ­ O2 [2]. solution) phase containing a precursor. Chemical syntheses
Substantial improvement of the hydrothermal method facili- are opposed to mechanical methods of nanomaterial produc-
tates the use of additional external factors to control the reac- tion (top-down approach) and physical methods (gas-phase
tion environment during the synthesis process. From now on, synthesis methods) [16]. Chemical synthesis methods are
this approach is implemented in the methods of microthermal also referred to as wet synthesis methods or solution-phase
hydrothermal synthesis, hydrothermal, ultrasonic, hydrother- synthesis. During this process, soluble species become insol-
mal-electrochemical, and hydrothermal-mechanochemical. uble or insoluble and precipitate. Since chemical methods
The hydrothermal method is a simple and versatile method of nanomaterial synthesis have a bottom–up approach, so
for the synthesis of inorganic nanomaterials at high tempera- with the help of this method, nanostructured engineering,
tures and pressures. The advantages and disadvantages of the as well as surface modification, can be done easily [35, 36].
hydrothermal method are summarized in Table 6. Chemical methods do not require complex and expensive
equipment compared to physical methods, which is a great
2.5 Sonochemical Method advantage on the scale of laboratory research and industrial
production. Soluble phase synthesis methods, like physical
The sonochemical method is one of the recently discovered methods, in addition to the production of nanopowders, are
techniques that offer a versatile way to obtain nanostructures also used to create thin films [35–37]. The types of chemical
for different applications. This represents the use of high- synthesis methods include the following: chemical precipita-
intensity ultrasounds, which induce synthesis conditions dis- tion, thermal decomposition, solvothermal, hydrothermal,
tinct from other conventional methods such as hydrothermal microemulsion or reverse micro-emulsion, and reverse
synthesis, spray pyrolysis method, and wet chemical method. micelle sol–gel. One of the main methods among chemical
Sonochemical synthesis resulted in the formation of methods of nanoparticle synthesis is the chemical deposition
α-Fe2O3 spherical nanoparticles with an average diameter of
60 nm. ZnO microspheres were prepared by sound-chemical
synthesis at room temperature using carbon spheres as a tem-
plate. The diameter of the hollow spheres obtained is about Table 7  Advantages and disadvantages of the sonochemical method
500 nm, and the walls are composed of numerous nanocrys- [29–32]
talline ZnO aggregates with diameters of 90 nm. A growth Advantages Disadvantages
mechanism has been proposed for the formation of ZnO
microspheres, in which carbon spheres play a crucial role Improves reaction rate Extension of problems
in the formation of hollow ZnO microspheres [29–32]. The Involves high energies and pressures in a Inefficient energy
short time
advantages and disadvantages of the sonochemical method are
No additives needed Low yield
summarized in Table 7.

Table 6  Advantages and Advantages Disadvantages

disadvantages of the
hydrothermal method [2] The ability to synthesize substances that are unstable near the melting point High cost of equipment
The ability to synthesize large crystals of high quality

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method [38, 39]. The formation of low-solubility products shifts from point 1 to point 2. Therefore, the point that was
from the aqueous phase forms the basis of the sedimenta- initially in the solubility range is located in the supersatu-
tion process. The deposition process can be classified into rating region. Raising the pH of the solution is the easiest
two categories: (1) chemical deposition (2) sedimentation/ way to precipitate. In order to obtain nanoparticles with very
absorption. This process is a complex process that occurs small amplitude changes, the germination and growth stages
under supersaturated solution conditions [40–43]. This pro- must be closely monitored. This is done by changing the
cess is rarely used in the deposition of organic compounds reaction parameters such as changing the ratio of the reac-
from solution. tants, adding a surfactant, changing the solvent, and also pro-
viding conditions such as (a) a high level of supersaturating
3.1 Chemical Deposition Process of the system (b) uniform concentration distribution inside
the reactor and (c) uniform growth time It is possible for
The chemical deposition process consists of three main all particles or crystals. Among the above, the appropriate
stages: (1) germination, (2) crystal growth, and (3) aggre- reaction rate plays a key role. Rapid nucleation and relatively
gation. In general, chemical deposition is not a controlled low particle growth rates usually lead to the formation of
process in terms of reaction kinetics, germination processes, monodisperse nanoparticles [46].
and solid-phase growth. Thus, solids obtained by chemical
deposition synthesis have a wide particle size distribution 3.2 Co‑precipitation Process
range, uncontrollable morphology, and agglomerated par-
ticles [42]. In order to start the germination process in the Another common method of synthesis in solution is the
solution, the solution must be supersaturated with precipi- co-precipitation method, which is used to synthesize multi-
tated compounds. The parameters that affect the supersatura- component oxide ceramics. In this method, a mixture of
tion of the solution are given in Fig. 2. In the supersaturated sediment is formed which contains two or more insoluble
zone, the system is unstable and sedimentation occurs with species, which are separated from the solution simulta-
the slightest change in the system. As shown in the diagram, neously [47, 48]. The precursors used in this method are
factors such as increasing the concentration of the solution mainly mineral salts (nitrate, chloride, sulfate, etc.), which
by evaporation, decreasing the temperature, or increasing the dissolve in water or other suitable environments and form
pH, bring the solution to the supersaturated region [43–45]. a homogeneous solution of ionic clusters. The solution is
It is also known that the dissolution of a compound increases then subjected to changes in solution pH or evaporation to
with increasing temperature. The dissolution curve is also act as a force for the deposition of salts (hydroxides, aqueous
a function of the pH of the solution, so that as the pH of oxides, or oxalates). Crystal growth and agglomeration are
the solution increases, its solubility decreases and the curve affected by factors such as salt concentration, temperature,
the true pH of the solution, and the rate of pH change [49].
After deposition, the solid mass is collected and washed and
then gradually dried by heating to the boiling point. The
washing and drying steps in hydroxide materials that are
synthesized by the precipitation process affect the degree
of agglomeration of the final powder. If the purpose of syn-
thesis is to prepare nanoscale powders, this point should be
very much considered. Many of the compounds produced by
this method (especially at low temperatures) are amorphous,
and secondary heat treatment is required to achieve products
with a suitable crystal structure [50–53]. A calcination step
is usually performed to convert hydroxides to crystalline
oxides. Most single-component, two-component, or three-
component systems require a crystallization step, usually
by calcination or hydrothermal processing in high-pressure
autoclaves [53–58]. Numerous papers have been reported
on the synthesis of ultra-fine oxide powders, oxide-oxide
composites, and biomaterials by co-precipitation reactions.
The advantages of homogeneous reactions include:

Fig. 2  Factors affecting the initiation of the germination process in Homogeneity of component distribution.
solution [3] Relatively low reaction temperature.

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Fine and uniform particle size. AG+ = (aq) + CL− (aq) → AgCl(S) (1)
Poor agglomeration intensity in the particles, as well as
its low cost. Silver chloride is sparingly soluble in the aqueous
medium, and very few silver and chloride ions are formed
Since these reactions depend on the conditions in the when dissolved in the aqueous medium. Considering the
reaction, it is difficult to control the stoichiometry of the stoichiometric coefficients, a simple sediment substitution
precursors due to the incomplete deposition of metal ions. In reaction is expressed as follows:
addition, co-precipitation reactions do not appear to be suit-
able for some oxide/hydroxide materials (e.g., in amphoteric
XA(aq) + YB(aq) ↔ AX BY (S) (2)
systems) [59–63]. The product of solubility product is expressed as follows:

KSP = [A]X [B]Y (3)

4 Chemical Reactions in the Synthesis
of Nanomaterial The expressions inside the brackets indicate the concen-
tration of species A and B. The levels of KSP or solubility of
The synthesis of nanoparticles using chemical methods is compounds such as hydroxides, carbonates, oxalates, and
based on fundamental chemical reactions. These reactions chalcogenides in an aqueous solvent are low. In contrast, the
are precipitation reactions, oxidation–reduction, hydroly- solubility of salts with ions of nitrate, chlorate, perchlorate,
sis, thermolysis, polymerization, and condensation. Each of and acetate in an aqueous solvent is high [29, 74–77].
these methods is briefly described in the rest of this article
[64–68]. 4.2 Redox Reactions

4.1 Precipitation Reactions Oxidation–reduction reactions are reactions in which the

oxidation number of the components used in a reaction
When the concentration of the solute exceeds its solubility, changes. These reactions can also produce low-solubility
the substance precipitates. The deposition process some- compounds. Reduction reactions usually result in the forma-
times takes place under supersaturated conditions, and tion of insoluble compounds of metal ions in aqueous media
sometimes by performing metathesis reactions, a low-sol- [30–32, 78, 79]. The following is an example of a reduction
uble ionic solid is formed, which subsequently precipitates. reaction half:
This reaction is also called the metathesis reaction [59]. Fig- Mn+ (aq) + ne− → M0 (S) (4)
ure 3 shows an overview of the dual substitution reaction
in the reaction between silver nitrate and sodium chloride. where ­Mn+ is a metal ion and ­ne− represents the number
Silver chloride is a low-solubility substance and precipi- of electrons used in the reduction reaction of a chemical
tates as soon as it is produced (indicated by the letter (S) oxidizing agent [80–82]. In an oxidation–reduction reaction,
in the equation). Sodium nitrate (shown in the equation as two chemical compounds are always oxidized and reduced
(aq)) is soluble in an aqueous medium and exists as separate together. The compound that oxidizes loses its electron and
­Na+ ions and ­NO−3 ions in the solution. In fact, these ions is therefore called the reducing agent, and the second com-
have only the role of contour ions or spectator ions and do pound (here, metal ion as an oxidant) oxidizes the reducing
not participate in the reaction themselves. By removing the agent [83, 84]. Which of the two materials plays the roles of
observer ions, the general reaction can be written as follows electron giver and electron receiver depends on their stand-
[60, 61, 69–73]: ard electrode potential (­ E0). Quantity (­ E0) is a measure of a

Fig. 3  Gives an overview of

the dual substitution reaction
and the reaction between silver
nitrate and sodium chloride [4]

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chemical compound’s tendency to capture or release elec- of this process. In this case, depending on the pH of the
trons [66, 67]. environment, the water-coated metal ion is usually converted
to metal hydroxide. The obtained metal hydroxide is a suit-
4.3 Hydrolysis Process able precursor for the synthesis of metal oxides that can
be converted to metal oxide by thermal decomposition pro-
The breaking down of a molecule by the reaction of that cesses [85–89]. For example, titanium oxide ­(TiO2) can be
molecule with a molecule of water is called hydrolysis. produced by hydrolysis of titanium chloride (­ TiCl3) in the
Hydrolysis is derived from the Greek word “hydro,” mean- presence of ­NH4OH.
ing water, and the word “lysis,” meaning to separate a bond.
In fact, by adding water molecules to the structure of the
molecule, certain bonds of the original molecule are broken. 4.4 Thermolysis Process
In many cases, the bonds of water molecules themselves are
broken, and each part of them is attached to a part of the Thermal decomposition is the irreversible chemical decom-
original molecule [68]. Even in the pure aqueous medium, position of a substance at high temperatures. If the residual
water is broken down into hydroxyl ions ­(OH−) and hydro- product of this process is a solid precipitate, this process can
nium ­(H3O+), which are sometimes displayed for conveni- be used to synthesize nanomaterials. The thermal degrada-
ence with protons ­(H+). The dissociation reaction of water tion method has been proposed as one of the ways to synthe-
molecules is as follows: size nanomaterials [90–92]. In general, in thermal decompo-
sition, the material is degraded in its chemical structure after
H2 O + H2 O ↔ H3 O+ + OH− (5) reaching a certain temperature. Because the chemical bonds
The general state of a hydrolysis reaction is expressed usually have to be broken during thermal degradation, the
as follows: whole process is usually endothermic. This process is also
known as thermolysis and sometimes pyrolysis. More spe-
AB + H2 O → AH + BOH (6) cifically, pyrolysis refers to chemical degradation reactions
of chemicals in which oxygen is not involved [93–95]. The
Figure 4 shows the hydrolysis process on the surface of
process of thermal degradation is an irreversible process. In
a fullerene molecule. Hydrolysis is one of the main steps in
the thermal degradation method, organometallic compounds
the sol–gel process [69]. The hydrolysis process also occurs
are used as precursors [3].
in many cases for metal cations. Figure 5 shows an outline

Fig. 4  Overview of the hydroly-

sis process of a functional
group present on the surface of
fullerene [5]

Fig. 5  Hydrolysis process in

metal ions [6]

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4.4.1 Precursors of Thermal Degradation precursors (metal salts) along with suitable completing
agents for synthesis.
The synthesis of pure metal nanoparticles (Ag or Au metal
nanoparticles) is usually performed using complexes in 4.5 Synthesis of Nanoparticles by Thermal
which the metal uses a low or zero degree of oxidation. Degradation Method
When carbon monoxide (CO) binds as a ligand to met-
als, it is called a carbonyl ligand. Usually, carbonyl com- 4.5.1 A Variety of Synthetic Approaches
plexes with central metals are formed in the zero-oxidation
state and are therefore suitable for heat degradation syn- Synthesis using organic-metal compounds can generally
theses. During degradation, carbonyl ligands are easily be done by two different approaches: In the first approach,
removed from the solution as carbon monoxide gas mol- the complex compound is injected into a hot solvent (with
ecules (Fig. 6). The formation of iron nanoparticles was a high boiling point). In this case, heat is cooled rapidly
synthesized by heating the pentacarbonyl iron (Fe(CO) 5) and nuclei are formed during the injection phase (nuclea-
complex in the presence of octyl ether as a solvent and tion). Because the formation of nuclei in the hot solvent
oleic acid as a stabilizer at temperatures above 100 °C [4]. is intense, the growth process is limited relative to nuclea-
Many nanoparticles such as nickel, chromium, tungsten, tion, and the size of the solid particles resulting from the
and cobalt nanoparticles have also been synthesized by thermal degradation will be in the nanometer range [102,
this method [96–98]. Thus, the heat recovery of the cobalt 103]. In the second approach, the reagents, which are the
carbonyl complex at 130 to 170 °C under the atmosphere same as the complex compounds, are first mixed together in
has been reported to be ineffective. In this method, PVP the solvent, and the temperature of the solvent rises gradu-
polymer is used as a stabilizer. The reaction of this process ally and in a programmed manner. When the temperature
is given below [5]: of the solvent reaches the point of thermal degradation, the
nuclei begin to form (nucleation stage). Due to temperature
CO2 (CO)8 → 2CO(S) + 8CO (7) controls, subsequent solid particles can either become new
nuclei or settle on the surface of the original nuclei (leading
Alkenes (olefins) are other functional ligands. Complex to the growth process) [104, 105]. Therefore, in the second
compounds with alkenes are also degraded at relatively approach of nanoparticle synthesis by the thermal decom-
low temperatures to form pure metal along with olefin position method, the growth process proceeds with more
ligands. Ligands such as cyclooctane, cyclooctadiene, and control and the final particle size is more controllable. By
π-allyl ligands are mentioned as examples. It is also com- suddenly cooling the reaction vessel, the growth process
mon to use complexes made with acetate ligand (acac). can be completely prevented. In some cases, two different
In general, the use of metal–organic precursors is often precasting complexes are used. Each of these complexes
expensive. Many of these compounds are also toxic and has its own degradation temperature and therefore begins
can be highly flammable. All of these can be accounted to degrade within a certain temperature range [67, 68]. In
for by the disadvantages of synthesis with this method. this case, the primary nuclei usually occur due to thermal
Therefore, the development of this method to large scale degradation of the first complex (with lower degradation
and industrial scale requires special skills in defining the temperature) and the growth process occurs due to the degra-
process and selecting appropriate precursors [99–101]. In dation of the second complex (more thermally stable). Usu-
this process, efforts should be made to use simpler metal ally, the products of both approaches can be aged. At this
stage, the product particles are exposed to the solvent for a

Fig. 6  Complex structures of

iron carbonyl and carbonyl
cobalt as precursors of heat
degradation synthesis [7]

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relatively long time at high temperatures. This causes the Accordingly, the selection of precursors in which the metal
particles to coalesce over time to form larger particles. This has a high oxidation number (the central metal is a cation,
phenomenon is called Ostwald ripening. If parameters such such as iron(III) complexes) can lead to the synthesis of
as temperature, concentration, and time are set correctly, metal oxide products [7], including complexes used for the
particles with the desired uniformity and homogeneity are direct synthesis of oxide magnetic nanoparticles. Iron is an
obtained by this method [106–109]. It should be noted that organic metal structure containing the acetyl acetate ligand
in order to obtain higher quality products, stabilizing com- (acetylacetonate-acac), expressed as Fe(acac)3. In this struc-
pounds can also be used in the reaction medium. In some ture, the oxidation number of iron (III) and The structure of
cases, the heat source can be supplied from different sources this complex is shown in Fig. 7. Thermal degradation of iron
[69]. Thermal degradation using son chemical reactions in complexes with oleic acid, olamine, fatty acids (fatty acids),
the presence of high-energy ultrasonic radiation or the use and phenols in non-aqueous solutions can also be used for
of microwave radiation is in this category. the direct synthesis of magnetic iron oxides. In general, the
initial ratio of reactants (organic–metallic precursors, sur-
4.5.2 Chemical Additives in Heat Degradation Method factants, and solvents) plays an essential role in controlling
the size and morphology of the final product [114–116].
As with other chemical methods (wet methods) of nano- TEM images of ­Fe2O3 nanoparticles synthesized by heat
materials, the addition of specific chemical compounds can degradation are shown in Fig. 8. The homogeneity in the size
lead to control of the size, shape, and structure of the prod- distribution (size distribution), as well as the monodispersity
uct. Although these compounds are not directly involved in of the particles, is clearly shown in Fig. 8.
chemical processes, they exert their effects through differ-
ent interactions with the product particles. Such polymeric 4.5.4 Synthesis of Other Compounds
materials play an essential role in the synthesis process
through the thermocouple process [6]. Initially, polymers In addition to pure metal nanoparticles as well as oxide
were considered only stabilizing agents. Further research nanoparticles, nanoparticles of semiconductor compounds
has shown that polymers act as catalysts and act as sites (quantum dots) can also be prepared by heat degradation.
for particle nucleation. It can be said that in this process, For example, the synthesis of cadmium selenide (CdSe)
special polymers with special heteroatoms play the role of nanoparticles by this method has been reported [14]. In
nucleophiles. Therefore, different functional groups on the this report, a mixture of both metal–organic precursors in
polymer surface can change the kinetics of the whole reac- a suitable solvent is used. Nanoparticles are formed at 230
tion in interaction with different metals and intermediates to 260 °C. Also, in some cases, heat degradation methods
and lead to different products. The type of polymer used and have been combined with the polyol reduction method as
the concentration of the precursor are two important factors one of the most practical methods of nanoparticle syn-
in determining particle size. In addition to polymers, the thesis. In these cases, in addition to the metal–organic
presence of capping ligands and surfactants can control the precursor of one metal, a salt of another metal is added to
growth process and prevent oxidation as well as aggrega- a polyol compound (such as ethylene glycol) as a solvent
tion [3–6].

4.5.3 Synthesis of Magnetic Nanoparticles (Metal Oxide)

by Thermal Degradation Method

If the process of thermal degradation takes place at high

temperatures, part of the product is usually obtained in oxi-
dized form. Although this approach can be a drawback to
the production of pure (non-oxidized) nanoparticles, it also
can be a pathway for the production of many metal oxides
[110–113]. The oxidation process can take place in the
presence of various oxidizing agents such as air or chemi-
cal oxidants. One of the important factors in determining
the chemical structure of the final product is the choice of
the primary metal–organic precursor. As mentioned above,
the use of precursors with zero (or lower) oxidation num-
bers for the central element leads to the synthesis of non-
oxide particles (for example, iron carbonyl complexes [7]. Fig. 7  Molecular structure of Fe(acac)3 [13]

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5 Polymerization Process

During the polymerization process, the primary molecules

are chemically bonded together to form a large molecule.
The initial molecules are called monomers, and the final
molecule is called a polymer. Polymerization processes are
performed in two ways: addition polymerization or conden-
sation polymerization [120–122]. In compression polymeri-
zation, polymers are formed through compression reactions,
and as the monomers bind together, some of the elements
in the monomers combine to form small molecules such as
water or methanol as a by-product. In incremental polymeri-
zation, the monomers are simply blended together, without
producing another by-product. Figure 9 shows an overview
of both types of polymerization processes [35–37].
Fig. 8  Iron oxide nanoparticles are synthesized by the heat degrada-
tion method [13]

6 Condensation Process
[117–119]. Therefore, at high temperatures, the process of
degradation of the metal–organic complex occurs simul- By attaching monomeric molecules to each other, molecules
taneously with the reduction of the salt of another metal, are created as a by-product in the compaction process. If the
and bimetallic compounds with different structures are molecule is released in water, this process is considered the
formed. In this case, the polyol solvent is used as a mild opposite of the hydrolysis reaction because in the hydrolysis
reducing agent in the conversion of metal salts (metal process, the chemical bond in the molecule is broken due to
ions) to metal nanoparticles. Polyols also usually have a the absorption of water molecules, and in the compaction
high boiling point that can be used as a solvent in thermo- process, bond formation causes the water molecule to be
couple processes. This synthetic process has been used to released. This process is the main step in the sol–gel process.
prepare Fe-Pt nanoparticles [14]. This step usually occurs simultaneously or after the hydroly-
sis process and results in the formation of large molecular
structures as a product. Due to this phenomenon, the viscos-
ity of the initial solution (tuberculosis) gradually increases.

Fig. 9  Schematic of incremental

polymerization and cumulative
polymerization reactions [37]

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The process of condensation of silanol (Si–OH) groups and concentration of solutes in the equilibrium state. The larger
the formation of the S­ iO2 network is one of the most com- the ratio, the faster the solution precipitates. In some cases,
mon examples in this regard. The silanol groups themselves the term “relative supersaturation” is used, which is defined
are the result of the hydrolysis of alkoxide (Si-OR) groups as follows:
[37, 67, 68]. Figure 10 shows an example of this reaction.
Relative supersaturation = (Q − S)∕S (8)
In the above relation, Q is the concentration of solute
7 Mechanism of Deposition Processes at any moment and S indicates its equilibrium solubility.
The relationship between particle size and relative super-
Several different processes occur during the deposition saturation in solution is inversely related. Thus, colloidal
processes, including the main stages in the deposition pro- sediments (small particle size) are obtained in large relative
cesses, which are (1) nucleation, (2) crystal growth, and (3) supersaturation, and crystalline sediments are obtained in
accumulation [3–6]. small supersaturation [69–71].

7.1 Nucleation
7.2 Growth
The bud is defined as the smallest solid phase consisting of
atoms, molecules, or ions that are formed during the deposi- As mentioned above, germination begins with the forma-
tion process and have the ability to grow spontaneously [63, tion of clusters. By adding a monomer to the solution and
64]. As mentioned in the previous article, the need to start increasing the size of the clusters formed until they reached a
germination is to be supersaturated with the solution. Only critical size, the clusters will be able to grow spontaneously.
when the concentration of the solution exceeds a critical Smaller-than-critical clusters tend to re-dissolve, while
level does the initial bud form and the deposition process larger clusters continue to grow. Growth occurs through the
begin. New particles are formed as long as the concentra- adsorption of ions on the surface of primary bud particles
tion of the species is above the critical germination limit. [72]. The growth process is a function of the concentration,
Because the supersaturation of the solution is high for most temperature, and pH of the solution. The rate of germina-
metal hydroxide or carbonate base materials, germination tion and growth processes can be controlled independently.
occurs spontaneously in these solutions [65–68]. The degree If the germination process is faster than the growth process,
of supersaturation of a solution is equal to the ratio of the small particles of the same size are produced. Rapid growth
concentration of solutes in the supersaturated state to the will also lead to the production of large particles. In many

Fig. 10  Condensation and

hydrolysis reactions as the main
reactions of the sol–gel process
[14]

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cases, crystal growth occurs so rapidly that crystal orienta- is controlled by processes such as mass transfer or related
tions may not be performed properly and the crystal may reaction kinetics, in which mass transfer processes play a
have defects such as dislocation defects (Fig. 11). more important role. In many cases, the growth process is
If the growth takes place in only one crystal direction, controlled by the phenomenon of infiltration. In this case,
the properties of the crystal will be different in different the degree of supersaturation of the solution at the edges of
directions, which is called anisotropic. The growth process the crystal is greater than its aspects, so the germination of

Fig. 11  Schematic diagrams and corresponding high-resolution trans- boundaries. i, l Nanoprecipitates. The insets in (e), (j), and (l) show
mission electron microscope images of common defects in solids. a, the morphology of a dislocation, dislocation (on the grain boundary),
d Vacancies. b, e Dislocations. c, f Stacking faults (SFs). g, j Grain and nanoprecipitate, respectively [123]

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the crystal is done from the corners and prevents the forma- higher the ratio of atoms (or molecules) on the surface
tion of a regular polyhedral structure. In the advanced state, to the total atoms, and therefore the higher the energy of
this process leads to the formation of dendritic crystals. Fig- the larger particles. For this purpose, small particles are
ure 12 shows polyhedral crystals and dendrimers. absorbed by large particles to reduce their energy, and over
time, large particles are formed. In cases where large crys-
7.3 Accumulation tals need to be formed, colloidal precipitates are placed
in the presence of solvent and heat for several hours to
In addition to germination and growth processes, the accu- allow Ostwald to be processed and larger coarse crystals
mulation stage is also an important stage in the deposition to grow. Figure 13 shows an overview of Ostwald pro-
process. Particle aggregation results in smaller, larger, but cessing. Ostwald’s processing process not only causes a
more porous particles. In this process, nanoscale primary deviation in the expected size for the product particles, but
particles can be converted to microscale secondary par- also changes the particle size distribution and sometimes
ticles. Physical and chemical forces hold these particles even produces two separate particle size ranges: a range of
together. In a colloidal solution, after a certain period of fine-sized particles and a range of large-sized particles. It
time, the smaller particles are gradually removed and the should be noted that in addition to Ostwald ripening, sec-
remaining particles become larger. This process is known ondary processes such as agglomeration are also involved
as Ostwald ripening. In fact, smaller particles are sacri- in the final product size. At low growth rates, nanoparticle
ficed to make larger particles grow. Ostwald processing is molecules usually follow the Ostwald processing process,
based on the inherent tendency of soluble particles to form while rapid growth always results in irregular morphology
a structure with less energy. The smaller the particles, the and variable particle sizes [37, 73, 74].

Fig. 12  a The structure of poly-

hedral crystals and b dendrim-
ers [15]

Fig. 13  Ostwald processing

process. The absorption of fine
particles into large particles
leads to the production of larger
particles [16]

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8 Particle Size Control the deposition reaction, and by increasing the amount of
supersaturation, smaller crystals are formed. If the ger-
8.1 Control of Synthesis Variables mination process dominates the growth process, a large
number of small nuclei are formed, and also a small num-
Because the complex processes of germination, growth, ber of large particles are formed when the growth process
and aggregation take place almost simultaneously, pre- is predominant [37].
cise control is required to produce single-particle particles.
For this purpose, and in order to obtain a high-quality 8.2 Nanoparticle Surface Stabilization
product, in many cases, it is tried to complete the ger-
mination process completely before the growth process. Due to the very high surface energy in nanoparticles, these
In this case, one can hope to create particles of the same particles have a strong tendency to stick to each other and
size [124–126]. But if the processes of germination and aggregate to reduce their energy. However, since the syn-
growth overlap, we will have a wide range of particle thesis of nanoparticles requires stable colloidal solutions as
sizes. To produce particles of approximately the same well as nanopowders separated from the solution, stabili-
size, severe conditions are first applied to the solution so zation of the nanoparticle surface and thus prevention of
that germination can be completed in a short time despite the phenomenon of agglomeration seems to be absolutely
the high supersaturation of the solution. In the growth necessary [127–131]. There are two approaches to achieving
phase, milder conditions are applied so that germination this goal [37]:
does not occur too much and the growth process domi-
nates. Under these conditions, the nuclei formed in the 1. Steric repulsion between nanoparticles: accordingly, the
initial stage grow homogeneously, resulting in particles of particles remain separate in the solution and no agglom-
approximately similar size [37]. As mentioned, the degree eration occurs. For this purpose, chemical compounds
of supersaturation of the solution plays a very key role such as surfactants, polymers, or some other organic
in the beginning and progress of the process as well as compounds are used in the nanoparticle formation
in the quality of the final product. In general, any factor medium. These compounds are also commonly known
that increases the supersaturation in the solution causes as capping agents.
the final product to become finer. It has been experimen- 2. Electrostatic repulsion (van der Waals) among nanopar-
tally proven that factors such as precipitate solubility, ticles: in many cases, this phenomenon occurs due to the
temperature, the concentration of reagents, the intensity chemical adsorption of ions such as hydroxyl (− OH)
of solution collision, as well as the presence of complet- and protons (+ H) or other charged agents on the surface
ing agents and stabilizers are very effective in determin- of nanoparticles. Therefore, the formed nanoparticles
ing the final particle size. When the product is inherently will be constant and repel each other. Absorption of
a water-insoluble compound (with a very low K SP), the hydroxyl ions or protons usually occurs at very high or
degree of supersaturation of the solution is also practically very low pH in aqueous solutions. An example of both
high. However, for compounds that have good solubility in approaches is given in Fig. 14. Sometimes the stabilizing
the aqueous medium, it is absolutely necessary to control agent plays both roles simultaneously.
the conditions to achieve the desired quality products. For
example, as mentioned in the previous article, the solubil- Without the presence of a stabilizing agent, a layer of
ity of the product can be changed and optimized by con- ions, called a double layer, surrounds the colloidal particles.
trolling the pH and temperature of the solution. In some This layer itself consists of two layers: (1) the primary ion
cases, the application of higher temperatures accelerates layer and (2) the counter ion layer. The primary ion layer and
the opposing ion layer have opposite names to each other,

Fig. 14  Nanoparticle surface

stabilizers [33]

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so the double layer is electrically neutral. Due to its elec- for hydrazine and borohydride are − 230 and − 480 mV,
trostatic repulsion, the double layer prevents particles from respectively. For example, Aucl-4 ions are used to syn-
approaching each other and prevents them from clumping thesize gold nanoparticles from an aqueous solution. The
[37]. Therefore, the thickness of this layer plays an impor- standard reduction potential of this ion is + 1 V. Therefore,
tant role in preventing the agglomeration of nanoparticles. it is a strong oxidant. In addition to the above-mentioned
Reducing the thickness of the double layer increases the reductases, compounds with a standard reduction potential
likelihood of clumping (Fig. 15). of fewer than + 1 V can be used as a suitable reluctance for
this ion and oxidize themselves to produce metallic gold.
Gold nanoparticles have attracted a lot of attention due
9 Synthesis of Metal Nanoparticles to their unique properties and applications. Alcohols are
from Aqueous Solution another reducing agent used in the synthesis of gold nano-
particles [135–138]. The choice of reducing or reducing
9.1 Synthesis with Chemical Reducers agent has a significant effect on determining the properties
of metal nanoparticles, so the appropriate reducing agent
Metal nanoparticles (MNPs) are one of the simplest nano- should be selected taking into account the available facili-
structures used in various industries. Most metal salts are ties and expectations of the final properties of the reduced
soluble in water. Therefore, by adding reducing or reduc- metal [76]. A schematic of the synthesis of gold nanopar-
ing compounds (reducing agents), they can be obtained as a ticles using an aqueous solution containing ­Aucl−4 ions is
solid metal structure from the aqueous medium [132–134]. shown in Fig. 16.
Hydrogen gas ­(H2), hydrazine ­(N2H4), and borohydrides
with the general formula A ­ BH4 (where A represents an 9.2 Reduction of Metals by Electrochemical
alkali metal such as sodium) are common chemical reduc- Processes
ers [75]. The standard reduction potential (Eo) of hydrogen
is zero, and the reduction chemical reaction is as follows: The reduction of metals by electrochemical processes is
only suitable if the number of electrons required to reduce
2H+ + 2e− ↔ H2 (9) metal ions is provided by the reducing agent on the electrode
Therefore, hydrogen can be used as a reducing agent for surface. As discussed above, the ability of different materi-
all compounds that have the potential to reduce the positive als to reduce metal actions depends on the amount of their
standard. Since most water-soluble metal salts have a posi- standard reduction potential [139, 140]. In electrochemical
tive reduction potential, hydrogen gas is a suitable and cost- processes, the reducing power of an electrode, as well as
effective reducing agent. The standard reduction potentials the nucleation processes and the growth of nanoparticles on
them, depend on several factors, including [77]:

• The electrical potential applied to the electrode surface

• Current density

In electrochemical processes, there are usually two elec-

trodes called anode and cathode. The oxidation process takes
place on the anode and the reduction process takes place on
the cathode. In electrochemical methods, as well as synthe-
sis methods with chemical reducers, the use of stabilizing
agents is necessary and significantly improves the nanopar-
ticles resulting from the process [29].

9.3 Reduction of Metals Using Optical Processes

When an energetic light beam strikes an aqueous solution,

the water molecules in it decompose, releasing electrons
unstable and transient into the solution. If metal actions are
present in the aqueous solution under irradiation, they react
with the released electrons and are reduced without the need
for any other reducing agent. The products of the decompo-
Fig. 15  Layer—the two structures around colloidal particle [34] sition of water molecules are gaseous hydrogen, hydrogen

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Fig. 16  Schematic of the

synthesis of gold nanoparticles
using an aqueous solution con-
taining Aucl.−4 ions [37]

peroxide ­(H2O2), hydroxyl radical (­ OH−), hydrogen radical annealing and calcination, the stabilizers cannot completely
­(H−), and so on. Studies on the reduction of metals using prevent agglomeration, and usually some particle aggrega-
high-energy light beams have grown significantly in recent tion is seen. To prevent the formation of lumps during the
years. For example, ultraviolet light (ultraviolet (UV)) has synthesis of oxide nanoparticles with the second method,
been used to reduce metals such as silver. Of course, the there is a need for excellent skills and control over the pro-
use of more powerful beams such as gamma rays seems to cess. In general, there are various processes for the synthesis
increase the efficiency of the process. An illustration of the of metal oxide nanoparticles, the most important of which
process of reducing silver sulfide to silver and silver sulfide are [37]:
using high-energy beams is shown in Fig. 17. The reduction
method using high-energy energetic beams has the ability to • Calcination in which synthesis is done by thermal pro-
synthesize all noble metals and some electronegative metals. cesses.
To improve the synthesis efficiency with this method, the • Thermal decomposition of carbonate, bicarbonate, and
use of stabilizing agents and short-chain alcohols such as metal oxalate deposits.
methanol is recommended [77]. • Direct synthesis of some metal oxides such as titanium
dioxide ­(TiO2) by hydrolysis.
9.4 Synthesis of Metal Oxides from Aqueous • Synthesis using reduction of soluble salts with higher
Solution oxidation number for the central atom.

The synthesis of metal oxides is a more complex process For example, the salts ­K2Cr2O7 and ­KMnO4 are soluble in
than the synthesis of metal nanoparticles. There are two water and after reduction are converted to ­Cr2O3 and ­Mn2O3
main methods for synthesizing metal oxides from an aque- compounds, respectively. The resulting compounds are spar-
ous solution, which are: (1) direct synthesis of metal oxide ingly soluble, so they can be formed as sediment.
from solution; (2) the synthesis of metal oxides indirectly, in
which nanoparticles are first synthesized as a precursor and 9.5 Metal Chalcogenides
then converted to oxide nanostructures by processes. In the
direct synthesis method (the first method), stabilizing agents Elements such as selenium (Se) and tellurium (Te) and
are used to control the structure, increase the homogeneity at other elements in the periodic table with sulfur are known
the nanoscale, and prevent agglomeration. However, in the as chalcogen. The combination of chalcogens with metals
second method, which requires thermal processes such as is called “metal chalcogenides.” In recent years, the use

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Fig. 17  Schematic of the pro-

cess of reducing silver sulfide
to silver and silver sulfide using
high-energy energetic beams
[37]

of metal chalcogenides has increased due to their unique

properties. The synthesis of metal chalcogenides takes place
through two types of reactions: (1) the reaction of mineral
salts and (2) the reaction of organic substances (or metals).
CdSe is a metal chalcogenide that has been widely used in
optoelectronic applications in the form of quantum dots due
to its semiconductor properties. Direct synthesis of metal
chalcogenides is possible using the precipitating reaction
between cacogenic salts such as ­Na2S and metal cations.
Methods such as microemulsion are used to prevent agglom-
eration and to control the size distribution. Another solution
for the synthesis of metallic chalcogenide nanoparticles is to
use a reaction between metallic organic precursors such as
(Cd(CH3)2) and cacogenic organic precursors such as ­R3PSe
and ­R3Si2S. The reaction between these two precursors is
usually nucleophilic, which eventually results in the synthe-
sis of metal chalcogenide nanoparticles. This type of reac-
tion usually occurs between two organic substances. Unlike
the mineral salt reaction, the reaction between metallic and
precursor organic precursors requires high activation energy.
Therefore, these reactions occur with the application of heat
and their kinetics are heat dependent. Therefore, nucleation
and growth processes are regulated by temperature control. Fig. 18  Scheme of synthesis of metal chalcogenide nanoparticles [35]
In the synthesis of metal chalcogenide nanoparticles using
the reaction of organic materials (or metals), a strong coor- of this solvent is to stabilize the formed nanocrystals [77].
dinating solvent such as trioctylphosphine (TOP) and trio- Figure 18 shows a schematic of the synthesis of metal chal-
actylphosphine oxide (TOPO) is usually used. Another role cogenide nanoparticles [37].

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9.6 Synthesis of Metal Nanoparticles and Oxides standard methods for synthesizing gold nanoparticles are the
from Non‑aqueous Solutions citrate reduction method and the thiol stabilized synthesis in
aqueous solvent [22–24, 145, 146]. Thiol has a functional
Water is not the only solvent used in chemistry, and it is pos- group (SH −). In addition to thiol-coating ligands, amine,
sible to use non-aqueous solvents in the synthesis of nano- phosphine, and silane ligands are also used to modify the
particles. Organic solvents make up the bulk of non-aqueous properties of nanoparticles synthesized by organic solvents.
solvents. The main differences between aqueous solvents and The wide range of ligands used can lead to the synthesis
non-aqueous solvents are: of different nanoparticles with unique properties. Figure 19
shows a diagram of gold nanoparticles stabilized by aro-
• Dielectric constant matic thiols. Because the aqueous phase (usually containing
• Polarity a metal salt or chemical reducing agent) and the organic
• The ability to create protons, according to which the phase (usually containing a stabilizing agent or surface-
properties of solvents are divided into two categories: modifying ligand) are insoluble, the reaction between the
protic and aprotic. Protic solvents, unlike non-protic compounds within the two phases is difficult [25–28]. The
ones, have the ability to produce ­H+ ions. phase mixing process (phase transfer catalyst (PTC)) is usu-
• Coordination ability. ally used to advance the reaction between these two phases.
Phase transfer catalyst is a general method for reactions in
Organic substances, depending on their chemical compo- which organic, inorganic anions, and other active species
sition, can be dissolved in water in certain proportions (such react with organic compounds. Unlike reactions that take
as short-chain alcohols, acetone, etc.) or insoluble in water place in a homogeneous environment, reactions performed
(such as toluene, chloroform, etc.). The mentioned differ- with a phase transfer catalyst take place in a heterogeneous
ences in the properties of aqueous and non-aqueous solvents biphasic system in which the first phase is a source of reac-
change the synthesis process and affect the final properties tion anions (organic anions) and the second phase is organic
of the product [73–76]. reactants and catalysts (a source of fat cations). The metal
ion is placed in the central cavity or hydrophilic part of the
9.7 Synthesis of Metal Nanoparticles phase transfer catalyst. Catalyst molecules have an organic
in Non‑aqueous Medium structure and are soluble in the organic phase, so they easily
transport the metal with them to the organic phase. Crown
Since the salts of different metals and reducing agents used ethers are among these catalysts [1, 2, 8, 9, 71–76].
in the aqueous medium are usually soluble, the synthesis in Alcohols are also said to be a subset of non-aqueous sol-
the aqueous medium is monophasic. However, the synthe- vents. Polyol is a type of alcohol that consists of several
sis of metal nanoparticles in a non-aqueous medium takes groups of hydroxyls. Polyols are used to reduce (reduce)
place in a two-phase medium (aqueous and organic solvents many metal salts, so they can be used as a non-aqueous sol-
together) [141–144]. The main application of this type of vent in the synthesis of metal nanoparticles. One of the main
synthesis is in the production of modified nanoparticles with challenges when using common alcohols is the agglomera-
organic molecules. For example, alkane thiol R-SH coat- tion of the synthesized nanoparticles, even in the presence
ing compounds are used to synthesize gold nanoparticles of stabilizing agents. However, the use of polyol compounds
using non-aqueous solvents. In general, the two common significantly reduces the amount of agglomeration due to

Fig. 19  Scheme of gold nano-

particles stabilized by aromatic
thiols [37]

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the presence of several hydroxyl functional groups. Also, desired properties. The use of aqueous solvent in such pro-
these alcohols themselves can play the role of stabilizing cesses, due to poor control over the reaction, cannot achieve
agents and chelating agents or chelating agents. The syn- the desired results. Figure 20 shows TEM images of oxidized
thesis of metal nanoparticles using a non-aqueous polyol nanoparticles (ZnO) synthesized using a non-aqueous sol-
solution is called a polyol synthesis procedure [76]. Ethyl vent (alkylamine).
glycol is the most well-known polyol used in this method. In
materials whose standard reduction potential is very nega- 9.9 Production of Nanoparticles by Thermal
tive, it is not possible to use a strong reducing agent in an Decomposition Processes
aqueous medium, because in these conditions the reducing
agent used, which has a lower standard reduction potential The synthesis of nanoparticles occurs by thermal decompo-
than water, reduces it to hydrogen gas. Therefore, the syn- sition methods based on thermolysis reactions. If the product
thesis process is problematic and not successful [10–12]. of the thermocouple reaction in the reaction medium is in
One way to overcome this challenge is to use some non- the form of a precipitate, this process is a co-precipitation
prosthetic organic solvents. These solvents have the abil- reaction and can be used to synthesize nanoparticles (in the
ity to dissolve alkaline metals as well as to separate them, presence of stabilizing agents, of course). For the synthesis
creating solvated electrons (es). Solutions with non-aqueous of nanoparticles by this method, organometallic complexes
solvents that contain solvent electrons are called alkalides with low thermal stability and a solvent with high thermal
and electrides. However, due to the extreme instability of stability are used. Whether the synthesized nanoparticles
these solutions, the preparation of these solutions is very are metallic or oxidized depends on several factors, includ-
complex and requires conditions of high purity and a neutral ing [73–76]:
atmosphere. However, the reducing power of these solutions
is very high, and they have the ability to perform impossible • Type of precursor (in terms of oxidation number of the
reduction processes in aqueous solutions. central metal and type of ligand attached to the central
metal).
9.8 The Synthesis of Metal Oxides in a Non‑aqueous • Type of solvent.
• Additive compounds.
In metal oxides, like metal nanoparticles, it is possible to • The atmosphere used in the synthesis reactor.
synthesize many compounds with non-aqueous media.
Lithium hydroxide (LiOH) is one of these compounds. To Figure 21 shows TEM images of spherical iron oxide
synthesize lithium hydroxide with a non-aqueous solvent, nanoparticles synthesized by thermal decomposition.
first, the metal salt alone, or with the salt of other metals (if
required) is precipitated as hydroxide in a suitable solvent, 9.10 Microwave‑Assisted Synthesis Processes
and then the final product for the production of lithium oxide
­(Li2O) is thermally decomposed. Also, in processes such as Electromagnetic waves whose wavelengths are in the range
sludge based on hydrolysis, the use of a non-aqueous sol- of radio waves and infrared waves are called microwaves.
vent improves control over the evolution of hydrolysis and Sediment synthesis by microwave radiation is used to syn-
ultimately leads to the formation of nanoparticles with the thesize materials that use a polar solvent (water, polyols

Fig. 20  TEM images of oxi-

dized nanoparticles (ZnO) syn-
thesized using a non-aqueous
solvent (alkylamine) [123]

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Fig. 21  TEM images of spherical iron oxide nanoparticles synthesized by thermal decomposition ([13] with permission from Battocchio, 2014)

(polyols), etc.), because polar materials have the ability to For this reason, the nanoparticles obtained by this method
absorb the energy of the emitted microwave. Of course, the are usually amorphous and non-crystalline. This method can
study of the mechanism of microwave radiation absorption be used to synthesize oxide nanoparticles such as titanium
is very complex and its description is beyond the scope of dioxide. It is also possible to combine this method with pro-
this article. Microwave radiation acts as an energy source cesses such as thermal decomposition [73–76].
for the development of sedimentary reactions. This radia-
tion is not concentrated to a single point and can uniformly
affect the entire reaction medium. This causes a uniform 10 Conclusion
precipitate to form throughout the volume of the solution.
The advantages of using microwave radiation in the syn- 1. `Methods based on chemical synthesis are among the
thesis of nanoparticles are the production of particles with suitable methods for the production of nanoparticles.
very small size, high reaction speed, and consequently short These methods, also known as more synthetic methods,
process time. In addition to their solvent properties, polyols are based on the deposition of low-soluble compounds
can act as a reducing agent and affect the final properties from aqueous and non-aqueous solutions. In the synthe-
of the synthesized nanoparticles more than a conventional sis of nanoparticles by chemical deposition, reactions
solvent. On the other hand, polyols are polar and have the such as co-precipitation, oxidation–reduction, hydroly-
ability to absorb microwave radiation. Recently, by com- sis, compaction, polymerization, and thermos grafting
bining these two methods, the process of polyol-microwave are used. Each of these methods is described in detail in
synthesis has been introduced. This process simultaneously specific articles. The chemical deposition process can
has the advantages of two microwave methods (low time and also be divided into two categories: chemical deposition
uniformity of the product) and the polyol method (controlled and co-deposition/adsorption. This process consists of
and special structure) [71–76]. three main stages: (1) germination, (2) crystal growth,
and (3) accumulation. In order to obtain nanoparticles
9.11 Sonication‑Assisted Synthesis Processes with a very small size distribution range, the germina-
tion and growth stages must be carefully controlled,
Ultrasonic synthesis is also a subset of the thermal methods which is done by changing the reaction parameters as
of nanoparticle synthesis. The entry of ultrasound waves well as providing special conditions in the system. The
into the solution causes very small bubbles to form in it. By right response rate plays a key role in this. Rapid nuclea-
destroying these bubbles, a lot of energy is released in a very tion and relatively low growth rate usually lead to the
short period of time (in the range of nanoseconds and even formation of monodisperse nanoparticles. The co-pre-
less) in a very small volume of solution. These energetic cipitation method is used to synthesize multi-component
points in the solution are called hot spots. The temperature of oxide ceramics. In this method, a mixture of sediment
these points even reaches 5000 K. The energy released dur- containing two or more insoluble species is simultane-
ing the ultrasound radiation collides with the solution, and ously separated from the solution and precipitated. The
spreads at a constant speed throughout the solution, causing advantages of co-precipitation reactions include (1)
the reaction (nucleation) and the formation of fine particles. homogeneity of component distribution, (2) relatively

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low reaction temperature, (3) uniform and fine particle released in a very short period of time (in the range of
size, and (4) poor agglomeration intensity in the parti- nanoseconds and even less) in a very small volume of
cles as well as its low cost. solution and causes Progress reacts.
2. In this paper, the mechanisms of the deposition process, 4. Thermal degradation method can be used as one of the
which include germination, growth, and accumulation, nanoparticle synthesis approaches. The main compo-
are examined and discussed. The role of each of them in nents in this synthetic method are one or more organic–
the synthesis of nanoparticles was also expressed. The metallic precursors, a solvent with a high boiling point,
types of nanoparticle surface stabilizers and their role in and various additives (such as stabilizing agents, oxi-
the production of nanoparticles with the same particle dizing or reducing agents, etc.). To produce pure com-
size were investigated. Secondary processes such as steel pounds (for example, non-oxide metal nanoparticles),
processing, annealing, and calcination cause the parti- lower temperatures and an inert gas atmosphere are
cles to clump and grow unintentionally. Precise control commonly used. Synthesis of pure metal nanoparticles,
of synthesis variables as well as the use of stabilizing metal oxide nanoparticles (especially magnetic oxide
agents will increase the quality of the final product. nanoparticles), and semiconductor nanoparticles are
3. Co-precipitation chemical methods enable the synthesis mentioned as the capabilities of this method.
of metal nanoparticles, metal oxides, as well as many
metal semiconductor compounds. In this paper, vari-
ous methods of synthesis of metal nanoparticles, metal Acknowledgements The author acknowledges the support of the Dean-
ship of Scientific Research at Prince Sattam bin Abdulaziz University;
oxides, and metal chalcogenides using chemical deposi- Department of Chemical Engineering, Arak Branch, Islamic Azad Uni-
tion methods from aqueous and non-aqueous solutions versity, Arak, Iran; and Young Researchers and Elite Club, Gachsaran
have been introduced and also, and nanoparticle syn- Branch, Islamic Azad University, Gachsaran, Iran.
thesis methods by thermal decomposition, microwave,
and ultraviolet radiation processes are studied. Synthesis Author Contribution Kadda Hachem, Mohammad Javed Ansari, Raed
Obaid Saleh, Hamzah H. Kzar, and Moaed E. Al-Gazally: investiga-
of metal nanoparticles from aqueous solutions includes tion, concept and design, experimental studies, and writing—original
synthesis with chemical reducers, synthesis with elec- draft, reviewing, and editing. Usama S. Altimari, Shaymaa Abed Hus-
trochemical processes, and synthesis with optical pro- sein, Halah T. Mohammed, Ali Thaeer Hammid, and Ehsan Kianfar:
cesses. The synthesis of metal oxides is a more complex investigation, concept and design, data curation, conceptualization, and
writing—original draft, reviewing, and editing. All authors read and
process than the synthesis of metal nanoparticles. Two approved the manuscript. All authors reviewed the manuscript.
main methods for the synthesis of metal oxides were
introduced. Then the synthesis of metal chalcogenides Funding Statement The funders had no role in the design of the study;
was studied and it was said that the synthesis of metal in the collection, analyses, or interpretation of data; in the writing of
chalcogenides is done through two types of reactions: the manuscript, or in the decision to publish the results.
(1) the reaction of mineral salts and (2) the reaction of
organic substances (or metals). Water is not the only Declarations
solvent used in chemistry, and it is possible to use non-
Research Involving Humans and Animals Statement Data Availability
aqueous solvents such as organic solvents and alcohols and Ethical statement we considerate the submitted is original and
in the synthesis of nanoparticles. Then, various meth- unique work and it has not been submitted to another journal sim-
ods of synthesis of metal and oxide nanoparticles using ultaneity. The work is single study and it’s not up into several parts
non-aqueous solvents were studied and it was said that and results are presented clearly, honestly, and without, falsification or
inappropriate the data manipulation.
the main application of this type of synthesis is in the
production of nanoparticles modified with organic mol-
ecules. It was emphasized that the synthesis of nanopar- Conflict of Interest The authors declare no conflict of interest.
ticles occurs by thermal decomposition methods based Informed Consent Additional informed consent was obtained from all
on thermocouple reactions, if the product of the thermo- individual participants for whom identifying information is included
couple reaction in the reaction medium is in the form of in this paper.
sediment, this process is a co-precipitation reaction and
can be used to synthesize the nanoparticles. Sediment
synthesis with microwave radiation is used to synthesize
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version: In book: Advances in chemistry research, Volume 59: gasoline conversion over CuO/ZSM-5 catalyst synthesized and
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chemistry research. Volume 62, Edition: James C. Taylor. Chap- 140. Kianfar, E. (2020). Magnetic nanoparticles in targeted drug deliv-
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1186/​s12951-​021-​00896-3

Authors and Affiliations

Kadda Hachem1 · Mohammad Javed Ansari2 · Raed Obaid Saleh3 · Hamzah H. Kzar4 · Moaed E. Al‑Gazally5 ·
Usama S. Altimari6 · Shaymaa Abed Hussein7 · Halah T. Mohammed8 · Ali Thaeer Hammid9 · Ehsan Kianfar10,11

1 7
Laboratory of Biotoxicology, Pharmacognosy and Biological Al-Manara College for Medical Sciences, Amarah (Maysan),
Valorization of Plants (LBPVBP), Faculty of Sciences, Iraq
University of Saida - Dr Moulay Tahar, 20000 Saida, Algeria 8
Anesthesia Techniques Department, Al-Mustaqbal University
2
Department of Pharmaceutics, College of Pharmacy, Prince College, Babylon, Iraq
Sattam Bin Abdulaziz University, Al‑Kharj, Saudi Arabia 9
Computer Engineering Techniques Department, Faculty
3
Department of Pharmacy, Al-Maarif University College, of Information Technology, Imam Ja’afar Al-Sadiq
Al‑Anbar, Iraq University, Baghdad, Iraq
4 10
Veterinary Medicine College, Al-Qasim Green University, Department of Chemical Engineering, Arak Branch, Islamic
Al‑Qasim, Iraq Azad University, Arak, Iran
5 11
College of Medicine, University of Al-Ameed, Karbala, Iraq Young Researchers and Elite Club, Gachsaran Branch,
6 Islamic Azad University, Gachsaran, Iran
Department of Pathology, Al-Nisour University College,
Baghdad, Iraq

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