Nanomaterial by Sol-Gel Method: Synthesis and Application: Advances in Materials Science and Engineering December 2021

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Nanomaterial by Sol-Gel Method: Synthesis and Application
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Advances in Materials Science and Engineering
Volume 2021, Article ID 5102014, 21 pages
https://doi.org/10.1155/2021/5102014
Review Article
Nanomaterial by Sol-Gel Method: Synthesis and Application
Dmitry Bokov ,1 Abduladheem Turki Jalil ,2,3 Supat Chupradit ,4

Wanich Suksatan ,5 Mohammad Javed Ansari,6 Iman H. Shewael,7
Gabdrakhman H. Valiev,8 and Ehsan Kianfar 9,10
1
Institute of Pharmacy, Sechenov First Moscow State Medical University, 8 Trubetskaya Street, Bldg. 2, Moscow 119991, Russia
2
Faculty of Biology and Ecology, Yanka Kupala State University of Grodno, 230023 Grodno, Belarus
3
College of Technical Engineering, Islamic University, Najaf, Iraq
4
Department of Occupational Therapy, Faculty of Associated Medical Sciences, Chiang Mai University, Chiang Mai 50200,
Thailand
5
Faculty of Nursing, HRH Princess Chulabhorn College of Medical Science, Chulabhorn Royal Academy, Bangkok, Thailand
6
Department of Pharmaceutics, College of Pharmacy, Prince Sattam Bin Abdulaziz University, Al-Kharj, Saudi Arabia
7
Department of Optics, College of Health and Medical Technology, Al-Ayen University, Thi-Qar, Iraq
8
Kazan Federal University, Kazan, Russia
9
Department of Chemical Engineering, Arak Branch, Islamic Azad University, Arak, Iran
10
Young Researchers and Elite Club, Gachsaran Branch, Islamic Azad University, Gachsaran, Iran
Correspondence should be addressed to Ehsan Kianfar; [email protected]
Received 19 September 2021; Revised 23 October 2021; Accepted 12 November 2021; Published 24 December 2021
Academic Editor: Zhongchang Wang
Copyright © 2021 Dmitry Bokov et al. This is an open access article distributed under the Creative Commons Attribution License,
which permits unrestricted use, distribution, and reproduction in any medium, provided the original work is properly cited.
The sol-gel process is a more chemical method (wet chemical method) for the synthesis of various nanostructures, especially metal
oxide nanoparticles. In this method, the molecular precursor (usually metal alkoxide) is dissolved in water or alcohol and
converted to gel by heating and stirring by hydrolysis/alcoholysis. Since the gel obtained from the hydrolysis/alcoholysis process is
wet or damp, it should be dried using appropriate methods depending on the desired properties and application of the gel. For
example, if it is an alcoholic solution, the drying process is done by burning alcohol. After the drying stage, the produced gels are
powdered and then calcined. The sol-gel method is a cost-effective method and due to the low reaction temperature there is good
control over the chemical composition of the products. The sol-gel method can be used in the process of making ceramics as a
molding material and can be used as an intermediate between thin films of metal oxides in various applications. The materials
obtained from the sol-gel method are used in various optical, electronic, energy, surface engineering, biosensors, and phar-
maceutical and separation technologies (such as chromatography). The sol-gel method is a conventional and industrial method for
the synthesis of nanoparticles with different chemical composition. The basis of the sol-gel method is the production of a
homogeneous sol from the precursors and its conversion into a gel. The solvent in the gel is then removed from the gel structure
and the remaining gel is dried. The properties of the dried gel depend significantly on the drying method. In other words, the
“removing solvent method” is selected according to the application in which the gel will be used. Dried gels in various ways are
used in industries such as surface coating, building insulation, and the production of special clothing. It is worth mentioning that,
by grinding the gel by special mills, it is possible to achieve nanoparticles.
1. Introduction the production and synthesis of nanoparticles. Although all

the mentioned methods have the ability of producing large
Today, various methods such as sol-gel method (solution volumes of nanomaterial, the sol-gel method has a higher
method), vapor phase compression method, mechanical popularity and industrial application than other existing
alloying method or collision with high-energy pellets, methods [1–5]. Due to its unique properties and charac-
plasma method, and electrochemical methods are used for teristics, this method is capable of producing high quality
2 Advances in Materials Science and Engineering
nanoparticles of the same size on an industrial scale [6–8]. or molding are used as filters or membranes. It is possible to
This method is capable of producing two or more types of create thin films with a thickness of 50–500 nm by sol-gel
nanoparticles simultaneously, meaning that alloy products method [79, 82–84]. For this purpose, different coating
are synthesized in one step by mixing two or more metal (or methods can be used: (a) dipping coating method and spin
metal oxide) precursors in certain proportions [9–11]. Of coating, (b) spray coating process, (c) flow coating process,
course, there are other methods such as plasma method and (d) capillary coating process, and (e) the climbing cover
electrochemical methods that have the ability of synthesizing process [85–88]. Sol-gel thin films have a wide range of
alloy products in one step, but their main difference with sol- applications in the electronics and chemical industries [89].
gel method is the industrial scale of sol-gel method [12–15]. In addition, coatings obtained from the sol-gel process also
In addition, the sol-gel method makes it possible to make affect the optical properties of the material. Figure 3 shows
highly homogeneous composites with very high purity an overview of the various sol-gel coating processes [90–94].
(99.99% purity) [16–20]. Another advantage of this method The sol-gel method can be used in the production of
compared to conventional methods is the lower temperature composite or nanocomposite materials [95–97]. For this
of the process in it, so that the production of metal and purpose, continuous porosity at the nanoscale is used as a
ceramic nanomaterial with this method is possible in the place for loading secondary materials [98–100]. Loading
temperature range between 70 and 320°C [21–24]. The other means adding a substance into the cavities. This is done
methods mentioned produce nanomaterial in the temper- using methods such as purification in the molten phase or
ature range of 1400–3600°C [25–28]. The sol-gel process is a chemical reactions. Nanoporous materials are classified into
bottom-up synthesis method. In this process, the final nanocomposites [101–104]. One of the applications of
products are formed by performing a number of irreversible nanoporous materials is their use in catalytic industries
chemical reactions [29–31]. During these reactions, the [105, 106]. The pores of nanoporous materials are filled with
primary homogeneous molecules (sol) become an infinite, a variety of industrial catalysts, and due to the very large
heavy, three-dimensional molecule called a gel [32–35]. The active surface area of these materials the catalytic efficiency
conversion of tuberculosis to gel is done through a process increases and the cost of the product decreases [107–109].
called “compaction process” and leads to the production of Figure 4 shows a diagram of the loading of secondary
wet gel [36–38]. Figure 1 shows an overview of the different particles into the nanoporous material [110–114]. In order to
stages of sol-gel process from precursor to aerogel. For the produce denser parts, the synthesized or produced parts are
synthesis of binary or tertiary hybrid systems, a mixture of subjected to sintering operations [115]. The high specific
salts with different chemical compositions is used [39–41]. surface area increases the rate of compaction or compaction
Each of the primary salts has a unique reaction rate [42–45]. of the structure, so the nanoporous gels compact better and
The rate of reaction of salts depends on various factors such faster during the sintering process [116–119]. On the other
as pH, concentration, type of solvent, and temperature hand, it should be noted that increasing the temperature
[46, 47]. The polymer gel formed from the density of the cell during this process causes the growth of grains and creates a
is a three-dimensional structure and is formed by joining the microstructure consisting of coarse grains [120–123]. Fig-
cavities [48–50]. After drying the gel, due to volumetric ure 5 shows an overview of the types of processes that can be
shrinkage, a solid and rigid structure is obtained [51]. It performed by the sol-gel method and the products derived
should be noted that, by controlling the drying conditions of from them.
the gel, it is possible to achieve nanosized porosity [52, 53].
The advantage of nanoporosity is the very large specific 2. Aerogels
surface area compared to normal porosity [54–56]. For
example, nanoporous carbon materials are used to store Aerogels are gels with nanometer pores, low density, po-
hydrogen, so that hydrogen is trapped and stored in the rosity, and high internal area. Due to these properties,
porosity of the carbon material [57–61]. Figure 2 shows the aerogels are widely used in applications that require sound
SEM image of these nanoporous materials. In the sol-gel insulation as well as high light transmittance. The aerogel
process, the conversion of sol to gel is usually done by synthesis process consists of two stages; in the first stage or
changing the pH or changing the concentration of the so- the gel-making stage, the solvent penetrates the gel and in
lution [62–67]. The main advantages of the sol-gel process the next stage the solvent is removed or dried. In general, the
are the high purity of the product, the narrow particle size term aerogel refers more to the internal structure of a
distribution, and the achievement of uniform nanostructure substance than to its constituent materials; therefore, it is
at low temperatures. This method is commonly used to possible to synthesize aerogels by a wide range of raw
synthesize metal nanooxides [68–70]. As mentioned, the sol- materials with different chemical compositions [124–127].
gel process involves changing the state from sol to gel using a The raw materials used to synthesize aerogels include
variety of techniques; most of which use gentle drying to minerals, organic, and composite. Aerogels were first in-
remove the solvent [71–74]. Since the drying of the gel is troduced in 1931 by Cuce et al. [76–78]. The chemical
accompanied by its shrinkage, providing suitable conditions composition of the first aerogel introduced was silica. The
to prevent the formation of cracks is one of the most im- word “aerogel” is made up of the words air and gel. In
portant issues in this process [75–78]. The produced gel has general, aerogel is a very light, porous substance derived
the ability of casting and by molding and drying it is possible from a gel. In aerogel synthesis, the liquid phase of the gel is
to produce integrated pieces [79–81]. Products from casting replaced by gas (air), which results in a material with low
Advances in Materials Science and Engineering 3
ng
Precursors + Solvents
D r yi Aerogel
cal
riti
up erc
S
Thermal Drying
Xerogel
Fre
ez eD
Sol Formation Connected porous r yi Final Products
ng
(Colloidal Structures in Sol) structure (gel)
Cryogel
Step: 1 (Hydrolysis) Step: 2 (Condensation) Step: 3 and 4 (Aging & Drying) Step: 5 (Calcination)
Figure 1: Schematic of different stages of sol-gel process: from precursor to aerogel [1–5].
Figure 2: SEM image of a dried gel after the sol-gel process: this image confirms the presence of nanometer porosity with a very high specific
surface area [1–5].
density and thermal conductivity [79, 80]. About 99.8% of structure prevents continuous and proper flow of heat. An-
this nanomaterial is composed of air, so their structure is other reason for the insulation of aerogels is the limited heat
solidly porous with a network of porous materials in the transfer mechanisms in them. In general, there are three
form of gas packets, which makes the aerogels almost mechanisms for heat transfer, radiation, convection, and
weightless. Aerogels are known to be the lightest and least conduction. Aerogels neutralize the two mechanisms of
dense solids, with about 50–99.5% of their volume being air convection and conduction in heat transfer [82]. The main
[77, 78, 128–130]. These gels have a surface area of 250–3000 reason for the elimination of the conduction mechanism is the
square meters per gram so that the surface of an aerogel with presence of excessive gas porosity in the structure of aerogels
a volume of one cubic inch is about a football field [81]. and the reason for the elimination of the convection mech-
Aerogels usually have amorphous structures and lack anism is the inability of air of circulating throughout their
crystalline order in their microstructure. For this reason, crystal lattice [131–134]. However, heat transfer by radiation
these nanomaterials are very brittle and have very high is possible due to the possibility of infrared waves (these waves
transparency [82]. have the ability of transferring heat) through the aerogels.
Silica aerogels are used in the manufacture of insulated
windows due to their low heat transfer. The thermal con-
2.1. Properties of Aerogels ductivity of aerogels is even lower than that of their con-
stituent gases. This effect occurs when the size of the gas
2.1.1. Thermal Conductivity Aerogels. Aerogels are known as cavities is approximately equal to their mean free path [83].
the best thermal insulation material. The main reason for the Yang et al. [134] concluded, in an experimental study on
low thermal conductivity of these nanomaterials is their the thermal conductivity of aerogel-enhanced insulating
porous structure, in such a way that the porosity in their materials under various hygrothermal environments, as
Hydrolysis Condensation of the sol particles

polymerisation Gelation
Solution of Sol Gel

precursors
Spin-coating Dip-coating
Evaporation
of solvent
Substrate
gelation and
Xerogel film Xerogel film
evaporation Xerogel
of solvent
Heat
Heat Heat
treatment
treatment treatment
Dense film Dense film
Dense ceramic
(a) (b)
Figure 3: Scheme of synthesis of samples by sol-gel method: (a) films synthesized from colloidal sol and (b) powder synthesized from gel
[1–5].
(A)
Fibers of KCC-1 KCC-1-NH2

(A) NH2(CH2)3Si(OEt)3,
Reflux in toluene;
(B) (i) RuCl3, H2O, RT (B)
(ii) H2, 400 oC
Ru
KCC-1-NH2/Ru
Figure 4: Image of porous nanomaterial that after modification of the surface, the desired catalyst is loaded into its cavities [1].
nanostructured material, that aerogel insulation materials based insulation materials, various aerogel-enhanced insu-
are widely used due to their outstanding thermal conduc- lating materials were exploited, and their pore distributions
tivity. To improve the hygrothermal performance of aerogel- and hygrothermal performance under different moisture
Coating Heating
Xerogel film Dense film
Sintering
Gelation Evaporation
Sphere
Hydrolysis & Su
polycondensation pe
dry rcriti
ing cal Xerogel
Rod
Precipitation
Metal Alkoxide Sol
Solution
Uniform powder Aerogel
Spinning
Fibers
Figure 5: An overview of the types of processes that can be done with the sol-gel method and the products of each process [1].
contents, environmental temperatures, and moisture levels supercritical methanol. In this method, the drying process is
were analyzed and evaluated. The results show that (1) the performed at high temperatures and leads to hydrophobicity
higher the content of aerogel, the lower the density and the of the surface of the aerogels. Figure 6 shows an overview of
thermal conductivity of an aerogel-enhanced HGB, and a the synthesis steps of hydrophobic silica aerogels. Aerogels
64% aerogel-enhanced HGB had the optimal thermal per- with at least 20% methyl methotrexate remain floating on the
formance and density (λ∼0.0465 W/mk, ρ ∼ 233.35 kg/m3 at water, so they are considered hydrophobic. Figure 7 shows
20°C) in the dry state; (2) a power function relation was the structural differences between hydrophobic and hy-
adopted to fit the thermal conductivity and mass MC of the drophilic silica aerogels [76–83].
specimens, and with increasing aerogel content the greater Li et al. [135] concluded that hydrophobic silica aerogels
the MC was, the slower the specimens’ thermal conductivity were produced by the -Si(Me)3 (trimethylsilyl substituent:
increased; (3) the humidity-driven changes in the thermal TMS) modification of alcogels followed by CO2 supercritical
conductivity of aerogel-enhanced materials are significantly drying. The structure of trimethylsilyl modified silica aerogel
greater than temperature-driven changes. For example, as (TMSA) was the silica matrix produced by hydrolysis and
the temperature increased from 20 to 70°C, the thermal condensation of only tetramethoxysilane (TMOS). TMS was
conductivity increased linearly (high correlation) in the modified on the surface of the silica matrix. TMSA was
range of 9.28–13.97%; however, when the RH increased from extremely moisture-resistant. The density, size, and trans-
0% to 98% at 35°C, the increase in the coefficient of thermal parency of TMSA samples were maintained after the
conductivity of the 64% aerogel-enhanced HGB was the moisture-resistance test. The moisture resistance of trime-
highest (61.54%); (4) the higher the content of aerogels was, thylsilyl modified silica aerogels (TMSAs) was superior to
the more sensitive the humidity was to the thermal con- that of conventional aerogels supercritically dried by the
ductivity of the materials. ethanol method. Another feature of TMSA was the small
shrinkage during supercritical drying. The shrinkage ratio of
TMSA was less than 3% by comparison with 5% for con-
2.1.2. Hydrophobicity of Aerogels. In general, aerogels are ventional aerogels. TMSA had the same transparency as
composed of particles with a diameter of 2–5 nm. After the conventional aerogels, with a transmittance of 90% at a
aerogel is synthesized, large amounts of hydroxyl groups are thickness of 1 cm. The existence of TMS was observed using
formed on its surface. These groups cause the aerogel to react infrared, 13C nuclear magnetic resonance (NMR) and 29Si
with water and cause it to dissolve severely in it. One way to NMR.
make hydrophilic aerogels hydrophobic is to replace their
hydroxyl (-OH) group with nonpolar (-OR) groups
[76, 80, 135, 136]. Therefore, it can be concluded that 2.1.3. Mechanical Properties of Aerogels. One of the main
aerogels are inherently hydrophilic, but they can be dehy- features of aerogels is their lightness and brittleness.
drated by chemical operations. In these groups, R indicates However, they are strong enough to be carried by hand. In
aliphatic compounds. To hydrophobicize silica aerogels, general, the compressive strength, tensile strength, and
these structures are synthesized from methyltrimethox- elasticity of these materials are very low. The mechanical
ysilane and tetraethoxysilane in play conditions and dried in properties of aerogels are highly dependent on their
3 h aging at
Gelation 50 oC
4 times gel
50 oC washing with
water in 24 h
(b) Hydrogel (c) Aged hydrogel
(a) Hydrosol
Na2SiO3 solution
+Tartaric acid
(d) Salt free
hydrogel
Drying at room
temp. for 24 h MeOH:TMCS:Hexane.
and 50 oC, 200 oC 1 : 1 : 1 volume ratio
for 1 h,
Surface Exchange the water
respectively modification with methanol 1
time in 24 h
(g) Hydrophobic (f) Modified gel (e) Alcogel

Silica Aerogel
Figure 6: Synthesis steps of hydrophobic silica aerogels [135]. (a) Hydrosol Na2SiO3 solution + tartaric acid. (b) Hydrogel. (c) Aged
hydrogel. (d) Salt free hydrogel. (e) Alcogel. (f ) Modified gel. (g) Hydrophobic silica aerogel.
OH OH R R
HO Si O Si OH R Si O Si R
O O O O
HO Si O Si OH R Si O Si R
OH OH R R
(a) (b)
Figure 7: Structural differences between hydrophobic and hydrophilic silica aerogels [135]. (a) Hydrophilic. (b) Hydrophobic.
structural conditions such as the quality of cavity cohesion Dynamical

and density. One way to increase the structural integrity of Ultrasounds Mechanical Analysis Brillouin Scattering
aerogels and improve their mechanical properties is to place
the gels in alkoxide solutions during the aging process. In Bending Test Hg Porosimeter
this way, the gels become more resistant to capillary pressure
[76–83]. Figure 8 shows the techniques for characterizing Toughness
Weibull analysis
the mechanical properties of aerogels.
Feng et al. [136] in a study of mechanical properties Nano Uniaxial
Double Cleavage Drilled
and thermal conductivity of aerogel-incorporated alkali- Indentation compression compression
activated slag mortars concluded that compressive
Figure 8: Techniques for characterizing the mechanical properties
strength, thermal conductivity coefficient, and porosi-
of aerogels [136].
metric properties of alkali-activated slag (AAS) mortars
containing silica aerogel were investigated experimentally
in this study. For this purpose, slag mortar mixtures at Li2CO3 on the gel, capillary, and macropore distributions
0.75% and 1.0% aerogel content ratios were prepared, and and the effect of changing porosimetric properties on
these mortar mixtures were activated with lithium car- compressive strength and thermal conductivity coefficient
bonate (Li2CO3) at 0.03% and 1.50% dosage rates. Mortar were analyzed in detail. Experimental studies have shown
samples were exposed to curing process in water for 2, 7, that AAS mortars including an optimum 0.75% aerogel
and 28 days, and the samples, which completed the curing content rate and 0.03% Li2CO3 activation provided a
stage, were subjected to the compressive strength test. The compressive strength of 34.1 MPa and a thermal con-
porosimetry test and the thermal conductivity coefficient ductivity coefficient of 1.32 W/mk. Aerogel addition
measurement were carried out following the compressive provides a partial compressive strength increase at 7- and
strength test on 28-day samples. The varying aerogel 28-day samples while it also causes maximum strength
content rate in the mixtures and the effects of the dosage of loss of 5.0% at 2-day samples.
3. Methods of Synthesis of Aerogels proper solvents [21, 22]. Alkoxides are the most common
sol-gel precursor, since they are commonly available.
In general, the methods of synthesis of aerogels are based on Bradley et al. have well explained the basic chemistry of the
their production by polymerization reactions of various precursor [23]. It is very difficult to predict the type of
compounds in the form of gels. The wet gels produced are precursor to be used for a given purpose. The reactivity of
then dried by various methods. The final product is a dry precursor depends not only on its chemical nature but also
material with a very porous and light texture [137–139]. on the applied reaction condition [24]. Compared to the
precursors of other elements, the network forming power of
3.1. Sol-Gel Process. The sol-gel process is performed at low Si is more to build up a gel [18]. That is why other expensive
temperatures (usually less than 100°C) and in the liquid state. alkoxide precursors can be substituted by cheaper ones like
Of course, the final product is solid, and these solids are silicon alkoxide such as TEOS and TMOS and water-soluble
formed as a result of the polymerization process, which precursor such as Na2SiO3 for sol-gel processing.
involves the establishment of M-OH-M or M-O-M (where
M represents the metal atom) between the metal atoms in
3.4. Methods of Converting Wet Gel to Aerogel
the raw materials. The synthesis of aerogels using the sol-gel
process consists of two steps, which are as follows [140–143]: 3.4.1. Drying by Supercritical Method. This method involves
(i) The first stage involves the formation of separate heating wet gels in a closed space with controlled pressure.
colloidal solid particles with nanometer dimensions. Of course, the temperature and pressure of this medium
must be adjusted so that these values are in the critical area of
(ii) The second stage involves colloidal particles in the
the liquid trapped in the pores of the gel [80, 82, 144–147].
solvent joining together to form a gel.
As a result, the solvent can be removed from the system as
Figure 9 shows an overview of the process of synthe- gas. Figure 10 shows how to find the critical point using
sizing silica aerogels using the sol-gel process [76–83]. pressure-temperature diagrams, and Figure 11 shows a di-
agram of an autoclave used for supercritical drying.
Supercritical solvents are similar to both liquids and
3.2. Chemistry of Sol-Gel Process. There are several param- gases in that they are dispersed like gases and have the same
eters which influence the hydrolysis and condensation re- density and thermal conductivity as liquids. These solvents
actions (sol-gel process), including the activity of the metal usually have high pressure and heat. Also, supercritical
alkoxide, the water/alkoxide ratio, solution pH, temperature, solvents have less surface tension than liquids, which pre-
nature of the solvent, and additive used. Another consid- serves the porous structure of aerogels and prevents their
eration is that catalysts are frequently added to control the structure from collapsing during the drying process
rate and the extent of hydrolysis and condensation reactions. [76, 83, 148–150]. Figure 12 shows the names and properties
By varying these processing parameters, materials with of some common supercritical fluids.
different microstructures and surface chemistry can be
obtained. Further processing of the “sol” enables the fab-
rication ceramic materials in different forms. Thin films can 3.4.2. Drying Methods. It is possible to dry organic gels
be produced on a piece of substrate by spin coating or dip- produced in organic solvents by using solvent evaporation at
coating. When the “sol” is cast into a mold, a wet “gel” will ambient pressure (without severe contraction). Also, in these
form. With further drying and heat treatment, the “gel” is conditions, surfactants can be used to reduce capillary
converted into dense ceramic or glass particles. If the liquid pressure. Other common drying methods include the fol-
in a wet “gel” is removed under supercritical conditions, a lowing [76–83]:
highly porous and extremely low density material called an
“aerogel” is obtained. The evidence of silicate hydrolysis and (i) Use of chemical additives that control the drying
condensation to form polysilicate gel and particles is seen in process such as glycerol, formaldehyde, oxalic acid,
many natural systems like opals and agates [18]. The first and tetramethylammonium hydroxide;
metal alkoxide was prepared from SiCl4 and alcohol by (ii) Drying processes at ambient pressure: these
Ebelmen, who found that the compound gelled on exposure methods can be used on an industrial scale;
to the atmosphere and Si-(OC2H5)4 can therefore be (iii) Freeze drying method: the liquid inside the gel is
regarded as the first “precursor” for glassy materials [19]. first frozen and then dried by sublimation. The
material obtained from this method is called
3.3. Precursors for Sol-Gel Processing. The precursor is Cryogel.
nothing but the starting materials for the sol-gel process. Xylogels are substances that have dried under normal
(1) Precursors should be soluble in the reaction media conditions. These materials are not much different from
aerogels and the main difference between them is the
(2) They should be reactive enough to participate in the
number and size of cavities, as the aerogels have more and
gel forming process[20]
larger cavities due to drying by supercritical method
Some salts, oxides, hydroxides, complexes, alkoxides, [151–153]. Figure 13 shows a flowchart of the synthesis steps
acrylates, and amines are used as precursors if soluble in of aerogels, carbogels, and subgels.
H3C
CH3
O Si Si CH3
Sol-gel O
O
O
process Si CH3 O O
Si Si CH3
O O
CH3 CH Si
O 3
Si CH3
O O
H3C Si
CH3 O Si
CH3
Drying at room
Fiber network is Silica composite-gel CH3 O
temperature
impregnated on solution
of silica precursors
-OH is substituted by -CH3
Figure 9: Scheme of the process of synthesis of silica aerogels using sol-gel process [79].
3.4.3. Types of Aerogels. Aerogels are classified into four

groups according to the chemical composition of their gels:
Pressure
inorganic aerogels including silica aerogels and alumina

solid phase compressible supercritical fluid aerogels, organic aerogels, carbon aerogels, and hybrid
liquid
critical pressure
aerogels [76, 77].
P critical point
liquid
phase (1) Inorganic Aerogels. Silica gels were the first mineral gels
synthesized under acidic conditions. Of course, natural
triple point gaxous phase
P organic gels are more common today. It is possible to
vapour convert all metals or semiconductor oxides to gels. The most
critical
temperature common mineral aerogels are silica aerogels, titanium,
T P
zirconium, tin, aluminum, vanadium, chromium, iron,
Temperature tantalum, molybdenum, and niobium-based aerogels. Bi-
Figure 10: How to find the critical point using pressure-tem- nary or ternary oxide aerogels can also be synthesized. Of
perature diagrams [80–82]. course, these aerogels are very fragile due to their ceramic
nature [78–81].
(2) Organic Aerogels. Organic aerogels are synthesized

Pressure gauge using organic precursors, which produce strong polymer
Inlet N2 gas covalently bonded (C-C) organic polymers. The most
Thermo
common organic compounds used to synthesize these
couple aerogels are resorcinol-formaldehyde and melamine-
formaldehyde (resin-formaldehyde). Condensation of the
Vapour mentioned organic compounds in alkaline aqueous so-
outlet lution is used for the synthesis of organic aerogels. The
alkaline aqueous solution usually used is sodium hy-
droxide, in which sodium hydrogen carbonate is used as a
catalyst [82, 154–159]. Figure 14 shows the melamine-
formaldehyde density reaction for the synthesis of organic
aerogels.
Heater
(3) Carbon Aerogels. Carbon aerogels were first synthesized
in 1990. A common method for synthesizing these aerogels
Gels is the pyrolysis of organic aerogels at temperatures above
500°C, as a result of which the organic aerogels become
Alcohol
electrically conductive carbon air gel. During the ther-
mocouple process, the area and amount of pores and pores
of the carbon air gel are preserved. Studies show that the
Figure 11: Scheme of an autoclave used for supercritical drying pyrolysis process at temperatures below 1000°C increases
[80–82]. the number of microspores, so that the largest surface area
Critical Critical
S.No Compound
temperature (°C) pressure (bar)
1 Carbon dioxide 31.3 72.9
2 Ammonia 132.4 112.5
3 Water 374.15 218.3
4 Nitrous oxide 36.5 71.7
5 Xenon 16.6 57.6
6 Krypton -63.8 54.3
7 Methane -82.1 45.8
8 Ethane 32.28 48.1
9 Ethylene 9.21 49.7
10 Propane 96.67 41.9
11 Pentane 196.6 33.3
12 Methanol 240.5 78.9
Figure 12: Names and properties of some common supercritical fluids [79].
TEOS, EtOH,
Dl water, catalyst
10 min gelation
Hydrogel aged
in EtOH
Ageing 24 hours
Hydrogel immersed
in sodium
bicarbonate
Solvent exchange
for 24 hours
50oC, x3
Wet Gel Heat at 70oC,
4 hours
Followed by
Silica aerogel APD at 150oC
Immersion in Ni
ion solution
Aerogel + EG + NiCl2
+ NaOH + N2H4
Autoclave 110oC
Ni-SiO2 aerogel
(a)
+NiCl2 +NaOH, N2H4

Aerogel immersed in In situ reduction
Ni ion solution to prepare Ni
(b)
Figure 13: (a) A flow diagram depicting the aerogel preparation process; (b) a schematic depicting the in situ synthesis of Ni within the
aerogel, which corresponds to the final two stages in the process (a) [79].
H2N N NH2
H
H 2O +
2 N N + 2 O C
H H H
H 2N N N C O C N N NH2
NH2 H2 H2
N N N N
NH2 NH2
Figure 14: Melamine-formaldehyde density reaction for organic aerogel synthesis [82].
of these aerogels is obtained at a temperature of 600°C. As (xiii) Precise control of material structure with the
the temperature gradually increases, the amount of cavities possibility of adjusting the variables of the early
decreases and at temperatures above 2100°C the volume of stages of tuberculosis and network formation
cavities reaches zero, which indicates the formation of (xiv) Low initial investment while having high quality
closed cavities. Carbon aerogels are synthesized in various products
forms such as monoliths, powders, films, and granules, the
properties of which are shown in Figure 15 The sol-gel process is a common and almost old method
[76, 83, 160, 161]. [161]. In the mid-nineteenth century, the tendency to use the
sol-gel process to synthesize mineral ceramics and glass
(4) Hybrid Aerogels. The synthesis of aerogels using materials began with the efforts of the likes of Ebelman and
organic-mineral compounds, also known as hybrid Graham and the study of silica gels. In the 1950s, extensive
aerogels, significantly increases the applications of aer- studies began on the synthesis of ceramics and glass
ogels. For example, with the introduction of organic structures using the sol-gel method. This method has the
structures into the silica surface, their hydrophobic and ability of synthesizing many mineral oxides such as TiO2,
elastic properties are improved. Hybrid aerogels are SiO2, and ZrO2. Depending on the drying conditions of the
usually synthesized by the sol-gel method. One of the wet gel, two types of dry gels are obtained, aerogels and
main advantages of hybrid aerogels over other aerogels is xerogels. By definition, an aerogel is a dry gel obtained by
their lower fragility [149]. removing moisture from a wet gel. Depending on the
moisture removal method, the structure of this gel largely
preserves the structure of the wet gel (primary gel). Wet gel is
4. Advantages of Sol-Gel Method the gel that results from the conversion of tuberculosis to gel
(i) Simplicity of the process during the compaction process. The sol-gel process involves
the transfer from the liquid phase of the “cell” (colloidal
(ii) Preparation of high purity products;
solution) to the “gel” phase. Figure 16 shows the types of gel
(iii) Very high production efficiency processing methods and techniques presented to turn it into
(iv) Production of optical components with complex products. As can be seen, the products can be produced both
shapes in powder and thin layers and in porous or dense materials
(v) Synthesis of uniform compounds in the form of [76–83].
composite oxides Inorganic metal salts or organic metal compounds such
(vi) bility of designing and controlling chemical as metal alkoxides are commonly used as precursors. Col-
composition and obtaining a homogeneous loidal suspension or “cell” is formed after a series of hy-
composition drolysis reactions and condensation of precursors. The TB
particles then condense into a continuous liquid (gel) phase.
(vii) Ability of using the product with special shapes With additional drying and heat treatment, the gel becomes
such as fibers and aerogels a dense glass or ceramic material. In general, three reactions
(viii) Surface coverage are used to describe the sludge process: (1) hydrolysis, (2)
(ix) Ability of using this process to synthesize amor- alcohol condensation, and (3) water condensation. Figure 17
phous materials in thin layers shows the general steps of the sol-gel process and the types of
synthesized materials. Because water and alkoxides are in-
(x) Production of materials with modified physical
compatible, alcohols are commonly used as a solvent. Due to
properties, such as low thermal expansion coeffi-
the presence of a solvent, the cellulose and alkoxide pre-
cient, low UV absorption, and high optical
cursors mix well with the water and facilitate the hydrolysis
transparency
process. Figure 18 shows the hydrolysis and compaction
(xi) Production of porous and rich materials with reactions (in both water and alcohol) in the sol-gel process to
organic and polymeric compounds produce silica gel.
(xii) High chemical reactivity of precursors due to During the hydrolysis reaction, by adding water to the
process in solution phase alkoxide groups (OR), these groups replace the hydroxyl
Structure
- SEM
- gas adsorption
- Hg-porosimetry backbone
- SAXS/SANS connectivity
- X-ray tomography - thermal solid phase conductivity
- electrical conductivity
Chemical Composition
Surface groups Mechanical
- EDX Properties
- FTIR - ultrasound velocity
- XPS - mechanical testing
Pore
Connectivity
- fluid transport
- self diffusion (NMR)
Figure 15: Characteristics of carbon aerogels [68].
Monomers Oligomers Polymers

Hydrolysis Network Solvent
polymerisation formation extraction
Sublimation Porosity
Precursor removal
solutions
Sol formation Gelation Aerogel
Evaporation
Electro Deposition Dip coating Spin coating

Dense Ceramic
Coating of complex objects Coating of 3D objects Ultrathin flat coatings Xerogel
Figure 16: Different methods of gel processing in the sol-gel process [76].
groups (OH). The next condensation reaction involves the the solutes trapped in the network are released. With ad-
silanol (Si-OH) group, which produces siloxane (Si-O-Si) ditional heat treatment at high temperatures, the organic
bonds with by-products including water (condensed water) waste in the structure is removed, destroying the inter-
or alcohol (condensed alcohol). As the number of siloxane connected cavities and eventually forming compressed glass
groups increases, the nanoparticles begin to bridge with each or ceramics. Figure 19 shows the different gel states in-
other to form a silica network. As soon as the wet gel dries, cluding wet gel, dry gel, and aerogel [76–83].
Precursor
(usually mixture of metal, bimetallic or
-oxobimetallic alkoxide)
Hydrolysis
Sol
Condensation
Gel
Critical Point Melt at lower

Drying temperature
1. Thin films
2. Fibers
3. Spheres Speciality Glasses
4. Grains Phase
5. Powder
Fire
Noncrystalline
Crystal ceramic Ceramics
(Xerogel, Aerogels)
Figure 17: An overview of the various stages of the sol-gel process and the types of synthesized products [76].
Step 1: hydrolysis
OR OR
RO Si OR + H2O RO Si OH + R-OH
OR OR
Step 2: condensation
(a) Water condensation
OR OR OR OR
RO Si OH + OH Si OR RO Si O Si OR + H 2O
OR OR OR OR
(b) Alcohol condensation

OR OR OR OR
RO Si OH + RO Si OR RO Si O Si OR + R-OH
OR OR OR OR
Where R is an alkyl chain. For TEOS, R = -CH2CH3
Figure 18: Hydrolysis reactions, condensation with water and alcohol to produce TB, and finally synthesis of silica gel [76].
Springback phenomena
Figure 19: Different states of the gel after the sol-gel process: wet gel, dry gel, and aerogel, respectively.
5. Sol-Gel Process Steps most important thing to say about a good quality TB is that
the resulting TB must be prepared in such a way that it can
5.1. Homogeneous Solution. In the sol-gel process, we seek to be stable for months and not settled. In other words, the
produce a homogeneous solution of precursors and alcohols. particle size must be small enough that the Brownian motion
For this purpose, first the solvent (usually containing water, of the particles overcomes the force of gravity and prevents
alcohol, organic solvents, or a proportion of them) and the them from settling. In this way, the resulting mixture re-
precursor are mixed in a container to obtain a homogeneous mains homogeneous for a long time. If TB has such char-
solution. To achieve a homogeneous solution, a mixture of acteristics, it can be hoped that a homogeneous, pure, and
two solvents in specific concentrations is often used to fully high-yield product will be produced [55–60].
dissolve the precursors. For example, some metallic organic
precursors must first be dissolved in a water-soluble organic
solvent and then the resulting solution is dissolved in water. 5.3. Gel Formation. In order to form a gel, it is sufficient to
However, in cases where the precursor is metal salt, it is stimulate the solution in some way, so that the dispersed fine
soluble directly in water and does not require an organic particles (each containing several molecular or atomic units
solvent. Although alkoxide precursors are more widely used, of the corresponding precursors) begin to collect [84–87]. By
the sol-gel process can be performed in other ways, in which, creating physical and chemical interactions between sus-
instead of homogeneous tuberculosis, a “relatively stable pended particles and those dispersed in the tuberculosis
colloid” is used for gel formation. Metal alkoxides, as pre- solution, units of tens of thousands of molecules line up
cursors used in the sol-gel method, are a class of organic together to form an infinitely large three-dimensional
metal compounds consisting of an organic base attached to a molecule that occupies the entire volume of the reaction
metallic or quasimetallic element. As an interesting example, vessel [61, 65, 88, 89]. Figure 21 shows the compression
consider silicon tetroxide (OC2H5)4. This precursor is also reaction for the synthesis of silica gel from a cell.
known as tetraethoxysilane (TEOS). Table 1 lists some This giant molecule, which has many pores and traps all
common precursors for the synthesis of metal oxides using the solvent inside it, is called wet gel. Figure 22 shows an
the sol-gel method and their functional groups [76–83]. overview of the sol-gel process to produce a uniform, dry gel.
As mentioned, wet gel production requires stimulation
of the tuberculosis solution. This stimulation can be done
5.2. Sol Formation. After forming a homogeneous solution, using a suitable reagent (pure water or water with NaCl and
it should be converted to tuberculosis. This phase is built NaOH). In fact, the cell-to-gel conversion phase, controlled
around the hydrolysis reaction. The word “hydrolysis” is a by reactions called condensation, is an inorganic polymer-
combination of the words “hydro” and “lysis” and means ization reaction whose end product is an oxide network
water decomposition. The term decomposition means that a containing MOM metal oxide clusters [66–70]. The com-
complex compound becomes a simpler compound [37–39]. paction reaction is exactly the opposite of the hydrolysis
In chemistry, water can sometimes break down a molecule reaction. In the hydrolysis reaction, large molecules are
into simpler molecules. In general, reactions in which converted into simpler components by consuming water,
molecules are broken down by chemical reactions with water but in the compaction reaction two simple molecules
to form simpler molecules are called hydrolysis. Figure 20 combine to form a more complex molecule. As the mole-
shows an overview of the steps of the sol-gel method, in- cules combine in the compaction reaction, a small molecule
cluding the formation of a homogeneous solution, the such as water is released. A compaction reaction is possible
formation of the sol, the conversion of the sol-gel, and the when two hydroxides (or one hydroxide + one metal alk-
removal of the solvent from the gel (drying). The hydrolysis oxide) (M-OR + HO-M) combine to form a metal oxide (M-
reaction is a simple reaction and to initiate it some water is O-M) [71–73]. Therefore, the gel produced will be soluble
added to the reaction medium. Water is added when a and in order to complete the sol-gel process and achieve a
homogeneous solution is prepared in a water-free solvent. dry gel the solvent must be separated using some methods.
The presence of water causes a hydrolysis reaction on the The produced gels have different types depending on the
precursor and somehow activates it so that the metal oxide solvent used or the drying method and show various
particles come together to form fine and solid particles properties and applications [74, 75].
dispersed in the solvent [40–45]. In a real solution, the solute
is dispersed uniformly in the solvent as an atom, molecule, 6. Application of the Nanomaterials Prepared
or ion, and the particle size does not exceed 1 nm. If the
particle size of the solvent is greater than 100 nm, the
by Sol-Gel Method
particles gradually settle to form a suspension mixture (i)Synthesis at low temperature
[46–50]. If the particle size varies between 1 and 100 (ii)Preparation of high purity products
nanometers, they usually remain scattered throughout the
(iii)Very high production efficiency
mixture, which is called colloid. The sol consists of very fine
particles (less than 100 nm) dispersed in the solvent phase (iv) Production of optical components with complex
and are, in fact, a solution or more precisely a colloidal shapes
mixture [51–54]. Thus, according to the above explanations, (v) Synthesis of uniform compounds in the form of
a comprehensive definition of tuberculosis can be given; the composite oxides
Table 1: Common precursors for the synthesis of metal oxides using sol-gel method and their functional groups [76–83].
Precursor Leaving group (R-) Structure
O
O
Tetraethoxysilane (TEOS) CH2-H3-OH Si
O O
O
O
Tetramethoxysilane (TMOS) -CH3 Si
O
O
O O
Dibutylphosphate -CH2-CH2-CH2-CH3
O O
O O
Titanium tetraisopropoxide -CH-(CH3)2
O O
O O
O O
Vanadium O(Amt)3 -C(CH3) (CH2-CH3)CH3-OH
Hydrolysis
Dip Coat Drying Heat
Polymerization
Precursors Sol Substrate Coating Xerogel Film Dense Film

Figure 20: Schematic of the steps of the sol-gel method including the formation of a homogeneous solution, the formation of a tuber, the
conversion of a tuber to a gel, and the removal of a solvent from the gel (drying) [45].
Si OH + HO Si Si O Si + H2O
Si OH + RO Si Si O Si + ROH
Figure 21: Gelatinization or compression reaction to form the sol gel.
(vi) Possibility of designing chemical composition and coefficient and low UV absorption and high optical
obtaining homogeneous composition transparency
(vii) Ability of using the product in special forms such (x) Production of porous materials that allow en-
as fibers, aerogels, and surface coatings richment with organic and polymeric compounds
(viii) Ability of using this process to synthesize materials (xi) High chemical reactivity of precursors due to
in an amorphous state and applying them to thin process in solution phase
layers (xii) Precise control of material structure with the
(ix) Production of materials with modified physical possibility of adjusting the variables of the initial
properties such as low thermal expansion stage of tuberculosis and network formation low
H3CH2CO O
Si O
O O
OCH2CH3 O HO O
Si Si
H3CH2CO O
H3CH2CO Si HO
Si
O
OCH2CH3 OH OCH2CH3
H3CH2CO O O O
Si
O
Si
Si Si
HO O O O
O O O
Si OH
O O
pore
solid
network
Starting solution Sol Wet gel Dried monolithic

OH H2
C
OH
gel
OH
CH2 CH2
O O
OH OH CH2 CH2 OH
O OH HO
+ 2H H
HO C
H2
OH
C
OH H2 CH2
CH2OH
O
OH CH2OH CH2
HO OH
C
H2
OH OH
Figure 22: Overview of the compaction reaction and transformation of tuberculosis into wet gel and finally dry and integrated gel.
initial investment and high quality products performing a number of irreversible chemical re-
[134, 135] actions. In this paper, the selection of suitable cat-
alysts, the operating mechanism of the catalysts, and
7. Prospective for the Nanomaterials the drying steps of the wet gel were investigated. It
was said that the reaction rate between water and
Prepared by Sol-Gel Method alkoxides is very low. With the addition of alcohol,
Sol-gel chemistry offers a flexible approach for obtaining a the solution becomes more dilute and the reaction
diverse range of materials. It allows differing chemistries to rate decreases sharply. Therefore, in order to increase
be achieved as well as offering the ability of producing a wide the reaction rate in the sol-gel process, a catalyst is
range of nano-/microstructures. The paper commences with used. It was emphasized that the catalysts used in the
a generalized description of the various sol-gel methods sol-gel process should be selected in such a way that
available and how these chemistries control the bulk it can be easily removed from the environment after
properties of the end products. Following this comes a more the reaction. As a comprehensive example, the
detailed description of the biomedical areas where sol-gel mechanism of action of acidic and alkaline catalysts
materials have been explored and found to hold significant in the silica gel sol-gel process was investigated. It has
potential. One of the interesting fields that has been de- been said that the use of acidic or alkaline catalysts
veloped recently relates to hybrid materials that utilize sol- increases the rate of the hydrolysis reaction and the
gel chemistry to achieve unusual composite properties. amount of sol produced. It was emphasized that
Another intriguing feature of sol-gels is the unusual mor- since the solvent is one of the internal components of
phologies that are achievable at the micro- and nanoscale. the gel and is responsible for forming its network, it
Subsequently, the ability of controlling pore chemistry at a is very difficult to maintain the structure of the
number of different length scales and geometries has proven cavities by removing the solvent. In order to
to be a fruitful area of exploitation that provides excellent maintain the integrity of the gel structure, it is
bioactivity and attracts cellular responses and enables the necessary to allow some time before drying for the
entrapment of biologically active molecules and their con- bonds between the particles to become stronger and
trollable release for therapeutic action. The approaches of stronger. Two methods for solvent separation from
fine-tuning surface chemistry and the combination with gels were introduced. In the first method, the gel is
other nanomaterials have also enabled targeting of specific placed in the atmosphere after production to dry
cell and tissue types for drug delivery with imaging capacity. spontaneously. The gel obtained from this method is
called xerogel. In the second method, called the
supercritical method, the changes in the solid net-
8. Conclusion work are minimized. The material obtained from this
(1) The sol-gel process is a bottom-up synthesis method. method has porous networks and low strength and is
In this process, the final products are formed by “hollow” in correction. This product is called aerogel.
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Nanomaterial by Sol-Gel Method: Synthesis and Application: Advances in Materials Science and Engineering December 2021

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Nanomaterial by Sol-Gel Method: Synthesis and Application

Article in Advances in Materials Science and Engineering · December 2021

Dmitry Bokov Abduladheem Turki Jalil

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Mohammad javed Ansari

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Dmitry Bokov ,1 Abduladheem Turki Jalil ,2,3 Supat Chupradit ,4

Correspondence should be addressed to Ehsan Kianfar; [email protected]

Academic Editor: Zhongchang Wang

1. Introduction the production and synthesis of nanoparticles. Although all

Hydrolysis Condensation of the sol particles

Solution of Sol Gel

Dense ﬁlm Dense ﬁlm

Fibers of KCC-1 KCC-1-NH2

Xerogel ﬁlm Dense ﬁlm

(g) Hydrophobic (f) Modiﬁed gel (e) Alcogel

structural conditions such as the quality of cavity cohesion Dynamical

3.4.3. Types of Aerogels. Aerogels are classiﬁed into four

inorganic aerogels including silica aerogels and alumina

(2) Organic Aerogels. Organic aerogels are synthesized

1 Carbon dioxide 31.3 72.9

2 Ammonia 132.4 112.5

3 Water 374.15 218.3

4 Nitrous oxide 36.5 71.7

5 Xenon 16.6 57.6

6 Krypton -63.8 54.3

7 Methane -82.1 45.8

8 Ethane 32.28 48.1

9 Ethylene 9.21 49.7

10 Propane 96.67 41.9

11 Pentane 196.6 33.3

12 Methanol 240.5 78.9

+NiCl2 +NaOH, N2H4

Figure 15: Characteristics of carbon aerogels [68].

Monomers Oligomers Polymers

Electro Deposition Dip coating Spin coating

Coating of complex objects Coating of 3D objects Ultrathin ﬂat coatings Xerogel

Critical Point Melt at lower

(b) Alcohol condensation

Where R is an alkyl chain. For TEOS, R = -CH2CH3

Precursors Sol Substrate Coating Xerogel Film Dense Film

Figure 21: Gelatinization or compression reaction to form the sol gel.

Starting solution Sol Wet gel Dried monolithic

graphene quantum dots/NiO nanocomposites for antibac-

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