Sol Gel

Hindawi
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
pharmaceutical 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
This method is capable of producing two or more types of to 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 methods can be used: (a) dipping coating method and spin
(or metal oxide) precursors in certain proportions [9–11]. coating, (b) spray coating process, (c) flow coating process,
Of course, there are other methods such as plasma method (d) capillary coating process, and (e) the climbing cover
and electrochemical methods that have the ability of process [85–88]. Sol-gel thin films have a wide range of
synthesizing alloy products in one step, but their main applications in the electronics and chemical industries [89].
difference with sol- gel method is the industrial scale of In addition, coatings obtained from the sol-gel process also
sol-gel method [12–15]. In addition, the sol-gel method affect the optical properties of the material. Figure 3 shows
makes it possible to make highly homogeneous composites an overview of the various sol-gel coating processes [90–94].
with very high purity (99.99% purity) [16–20]. Another The sol-gel method can be used in the production of
advantage of this method compared to conventional composite or nanocomposite materials [95–97]. For this
methods is the lower temperature of the process in it, so purpose, continuous porosity at the nanoscale is used as a
that the production of metal and ceramic nanomaterial with place for loading secondary materials [98–100]. Loading
this method is possible in the temperature range between 70 means adding a substance into the cavities. This is done
and 320°C [21–24]. The other methods mentioned produce using methods such as purification in the molten phase or
nanomaterial in the temperature range of 1400–3600°C chemical reactions. Nanoporous materials are classified into
[25–28]. The sol-gel process is a bottom-up synthesis nanocomposites [101–104]. One of the applications of
method. In this process, the final products are formed by nanoporous materials is their use in catalytic industries
performing a number of irreversible chemical reactions [105, 106]. The pores of nanoporous materials are filled
[29–31]. During these reactions, the primary homogeneous with a variety of industrial catalysts, and due to the very
molecules (sol) become an infinite, heavy, three- large active surface area of these materials the catalytic
dimensional molecule called a gel [32–35]. The conversion efficiency increases and the cost of the product decreases
of tuberculosis to gel is done through a process called [107–109]. Figure 4 shows a diagram of the loading of
“compaction process” and leads to the production of wet secondary particles into the nanoporous material [110–
gel [36–38]. Figure 1 shows an overview of the different 114]. In order to produce denser parts, the synthesized or
stages of sol-gel process from precursor to aerogel. For the produced parts are subjected to sintering operations [115].
synthesis of binary or tertiary hybrid systems, a mixture of The high specific surface area increases the rate of
salts with different chemical compositions is used [39–41]. compaction or compaction of the structure, so the
Each of the primary salts has a unique reaction rate [42– nanoporous gels compact better and faster during the
45]. The rate of reaction of salts depends on various factors sintering process [116–119]. On the other hand, it should be
such as pH, concentration, type of solvent, and noted that increasing the temperature during this process
temperature [46, 47]. The polymer gel formed from the causes the growth of grains and creates a microstructure
density of the cell is a three-dimensional structure and is consisting of coarse grains [120–123]. Fig- ure 5 shows an
formed by joining the cavities [48–50]. After drying the overview of the types of processes that can be performed by
gel, due to volumetric shrinkage, a solid and rigid structure the sol-gel method and the products derived from them.
is obtained [51]. It should be noted that, by controlling the
drying conditions of the gel, it is possible to achieve
nanosized porosity [52, 53]. The advantage of nanoporosity
2. Aerogels
is the very large specific surface area compared to normal Aerogels are gels with nanometer pores, low density, po-
porosity [54–56]. For example, nanoporous carbon rosity, and high internal area. Due to these properties,
materials are used to store hydrogen, so that hydrogen is aerogels are widely used in applications that require sound
trapped and stored in the porosity of the carbon material insulation as well as high light transmittance. The aerogel
[57–61]. Figure 2 shows the SEM image of these synthesis process consists of two stages; in the first stage or
nanoporous materials. In the sol-gel process, the conversion the gel-making stage, the solvent penetrates the gel and in
of sol to gel is usually done by changing the pH or the next stage the solvent is removed or dried. In general,
changing the concentration of the solution [62–67]. The the term aerogel refers more to the internal structure of a
main advantages of the sol-gel process are the high purity substance than to its constituent materials; therefore, it is
of the product, the narrow particle size distribution, and the possible to synthesize aerogels by a wide range of raw
achievement of uniform nanostructure at low temperatures. materials with different chemical compositions [ 124–127].
This method is commonly used to synthesize metal The raw materials used to synthesize aerogels include
nanooxides [68–70]. As mentioned, the sol- gel process minerals, organic, and composite. Aerogels were first in-
involves changing the state from sol to gel using a variety of troduced in 1931 by Cuce et al. [76–78]. The chemical
techniques; most of which use gentle drying to remove the composition of the first aerogel introduced was silica. The
solvent [71–74]. Since the drying of the gel is accompanied word “aerogel” is made up of the words air and gel. In
by its shrinkage, providing suitable conditions to prevent general, aerogel is a very light, porous substance derived
the formation of cracks is one of the most important from a gel. In aerogel synthesis, the liquid phase of the gel
issues in this process [75–78]. The produced gel has the is replaced by gas (air), which results in a material with
ability of casting and by molding and drying it is possible low
to produce integrated pieces [79–81]. Products from casting
Advances in Materials Science and 3
Precursors + Solvents Aerogel
Thermal Drying
Xerogel
Sol Formation Connected porous Final Products

(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 convection and conduction in heat transfer [82]. The main
air [77, 78, 128–130]. These gels have a surface area of 250– reason for the elimination of the conduction mechanism is
3000 square meters per gram so that the surface of an the presence of excessive gas porosity in the structure of
aerogel with a volume of one cubic inch is about a football aerogels and the reason for the elimination of the
field [81]. Aerogels usually have amorphous structures and convection mechanism is the inability of air of
lack crystalline order in their microstructure. For this circulating throughout their crystal lattice [131–134].
reason, these nanomaterials are very brittle and have very However, heat transfer by radiation is possible due to the
high transparency [82]. possibility of infrared waves (these waves have the ability of
transferring heat) through the aerogels. Silica aerogels are
used in the manufacture of insulated windows due to
2.1. Properties of Aerogels their low heat transfer. The thermal conductivity of
aerogels is even lower than that of their constituent
2.1.1. Thermal Conductivity Aerogels. Aerogels are known as
gases. This effect occurs when the size of the gas cavities
the best thermal insulation material. The main reason for
is approximately equal to their mean free path [83]. Yang et
the low thermal conductivity of these nanomaterials is their
al. [134] concluded, in an experimental study on the
porous structure, in such a way that the porosity in their
thermal conductivity of aerogel-enhanced insulating
materials under various hygrothermal environments, as
Engineering
Hydrolysis Condensation of the sol particles
polymerisation Gelation
Solution of precursors Sol Gel
Spin-coatingDip-coating
Evaporation
of solvent
Substrate
gelation and
Xerogel film evaporation of solvent Xerogel film
Xerogel
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

NH2(CH2)3Si(OEt)3, Reflux in toluene;
(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 and hygrothermal performance under different moisture
aerogel-
Coating Heating
Xerogel film Dense film
Sintering
Gelation Evaporation
Sphere
Hydrolysis & polycondensation
Xerogel
Rod
Precipitation
Metal Alkoxide Solution Sol
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
thermal conductivity of an aerogel-enhanced HGB, and a of the synthesis steps of hydrophobic silica aerogels.
64% aerogel-enhanced HGB had the optimal thermal per- Aerogels with at least 20% methyl methotrexate remain
formance and density (λ∼0.0465 W/mk, ρ ∼ 233.35 kg/m3 at floating on the water, so they are considered hydrophobic.
20°C) in the dry state; (2) a power function relation was
Figure 7 shows the structural differences between
adopted to fit the thermal conductivity and mass MC of the
hydrophobic and hydrophilic silica aerogels [76–83].
specimens, and with increasing aerogel content the greater
Li et al. [135] concluded that hydrophobic silica
the MC was, the slower the specimens’ thermal
aerogels were produced by the -Si(Me)3 (trimethylsilyl
conductivity increased; (3) the humidity-driven changes in
substituent: TMS) modification of alcogels followed by CO 2
the thermal conductivity of aerogel-enhanced materials are
supercritical drying. The structure of trimethylsilyl modified
significantly greater than temperature-driven changes. For
silica aerogel (TMSA) was the silica matrix produced by
example, as the temperature increased from 20 to 70°C, the
hydrolysis and condensation of only tetramethoxysilane
thermal conductivity increased linearly (high correlation) in
(TMOS). TMS was modified on the surface of the silica
the range of 9.28–13.97%; however, when the RH increased
matrix. TMSA was extremely moisture-resistant. The
from 0% to 98% at 35°C, the increase in the coefficient of
density, size, and transparency of TMSA samples were
thermal conductivity of the 64% aerogel-enhanced HGB
maintained after the moisture-resistance test. The moisture
was the highest (61.54%); (4) the higher the content of
resistance of trimethylsilyl modified silica aerogels
aerogels was, the more sensitive the humidity was to the
(TMSAs) was superior to that of conventional aerogels
thermal conductivity of the materials.
supercritically dried by the ethanol method. Another feature
of TMSA was the small shrinkage during supercritical
2.1.2. Hydrophobicity of Aerogels. In general, aerogels are drying. The shrinkage ratio of TMSA was less than 3% by
composed of particles with a diameter of 2–5 nm. After the comparison with 5% for conventional aerogels. TMSA
aerogel is synthesized, large amounts of hydroxyl groups had the same transparency as conventional aerogels, with a
are formed on its surface. These groups cause the aerogel to transmittance of 90% at a thickness of 1 cm. The existence of
react with water and cause it to dissolve severely in it. One TMS was observed using infrared, 13C nuclear magnetic
way to make hydrophilic aerogels hydrophobic is to replace resonance (NMR) and 29Si NMR.
their hydroxyl (-OH) group with nonpolar (-OR)
groups [76, 80, 135, 136]. Therefore, it can be concluded 2.1.3. Mechanical Properties of Aerogels. One of the main
that aerogels are inherently hydrophilic, but they can be features of aerogels is their lightness and brittleness.
dehydrated by chemical operations. In these groups, R However, they are strong enough to be carried by hand. In
indicates aliphatic compounds. To hydrophobicize silica general, the compressive strength, tensile strength, and
aerogels, these structures are synthesized from elasticity of these materials are very low. The mechanical
methyltrimethox- ysilane and tetraethoxysilane in play properties of aerogels are highly dependent on their
conditions and dried in
Engineering
3 h aging at 50 oC
Gelation
50 oC 4 times gel 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 and 50 oC, 200 oC

MeOH:TMCS:Hexane. 1 : 1 : 1 volume ratio
Surface modification
for 1 h,
Exchange the water with methanol 1 time in 24 h
resy
pectivel
(g) Hydrophobic Silica Aerogel (f) Modified gel (e) Alcogel
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
O Si OH Si O Si R
RO O O
Si
O Si OH Si O Si R
O
R R
HO Si
(a) R OH (b)
OH
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 Bending Test Hg Porosimeter
process. In this way, the gels become more resistant to
capillary pressure [76–83]. Figure 8 shows the techniques
Toughness
for characterizing the mechanical properties of aerogels. Weibull analysis
Feng et al. [136] in a study of mechanical properties Nano Double Cleavage Drilled Uniaxial
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 coe fficient 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
Bradley et al. have well explained the basic chemistry of
on their production by polymerization reactions of various
the 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
temperatures (usually less than 100°C) and in the liquid expensive alkoxide precursors can be substituted by
state. Of course, the final product is solid, and these solids cheaper ones like silicon alkoxide such as TEOS and
are formed as a result of the polymerization process, which TMOS and water-soluble precursor such as Na2SiO3 for
involves the establishment of M-OH-M or M-O-M (where sol-gel processing.
M represents the metal atom) between the metal atoms in
the raw materials. The synthesis of aerogels using the sol-
gel process consists of two steps, which are as follows [140– 3.4. Methods of Converting Wet Gel to Aerogel
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
(ii) The second stage involves colloidal particles in the must be adjusted so that these values are in the critical area
solvent joining together to form a gel. of the liquid trapped in the pores of the gel [80, 82, 144–
147]. As a result, the solvent can be removed from the
Figure 9 shows an overview of the process of synthe- system as gas. Figure 10 shows how to find the critical
sizing silica aerogels using the sol-gel process [76–83]. point using pressure-temperature diagrams, and Figure 11
shows a diagram of an autoclave used for supercritical
3.2. Chemistry of Sol-Gel Process. There are several drying.
parameters which influence the hydrolysis and Supercritical solvents are similar to both liquids and
condensation reactions (sol-gel process), including the gases in that they are dispersed like gases and have the
activity of the metal alkoxide, the water/alkoxide ratio, same density and thermal conductivity as liquids. These
solution pH, temperature, nature of the solvent, and solvents usually have high pressure and heat. Also,
additive used. Another consid- eration is that catalysts are supercritical solvents have less surface tension than liquids,
frequently added to control the rate and the extent of which preserves the porous structure of aerogels and
hydrolysis and condensation reactions. By varying these prevents their structure from collapsing during the
processing parameters, materials with different drying process [76, 83, 148–150]. Figure 12 shows the
microstructures and surface chemistry can be obtained. names and properties of some common supercritical fluids.
Further processing of the “sol” enables the fabrication
ceramic materials in different forms. Thin films can be
produced on a piece of substrate by spin coating or dip- 3.4.2. Drying Methods. It is possible to dry organic gels
coating. When the “sol” is cast into a mold, a wet “gel” will produced in organic solvents by using solvent evaporation
form. With further drying and heat treatment, the “gel” is at ambient pressure (without severe contraction). Also, in
converted into dense ceramic or glass particles. If the liquid these conditions, surfactants can be used to reduce capillary
in a wet “gel” is removed under supercritical conditions, a pressure. Other common drying methods include the fol-
highly porous and extremely low density material called an lowing [76–83]:
“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 process such as glycerol, formaldehyde, oxalic
in many natural systems like opals and agates [18]. The acid, and tetramethylammonium hydroxide;
first 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
regarded as the first “precursor” for glassy materials [19]. (iii) Freeze drying method: the liquid inside the gel is
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
(2) They should be reactive enough to participate in the aerogels and the main difference between them is the
gel forming process[20] number and size of cavities, as the aerogels have more and
larger cavities due to drying by supercritical method [151–
Some salts, oxides, hydroxides, complexes, alkoxides, 153]. Figure 13 shows a flowchart of the synthesis steps of
acrylates, and amines are used as precursors if soluble in aerogels, carbogels, and subgels.
Engineering
H3C
CH 3
O Si Si CH3 O
Sol-gel process O
O
SiCH3
Si CH3
O
O O Si O
CH3 CH OSi
3 O CH3
H C Si CH3
O Si
3
CH3 O Si
Fiber network is impregnated on solution
Silica of silica precursors
composite-gel CH O 3
Drying at
room
-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:
Press
inorganic aerogels including silica aerogels and alumina

solid phase compressible liquid
supercritical fluid aerogels, organic aerogels, carbon aerogels, and hybrid
critical pressure P aerogels [76, 77].
liquid phase critical point
(1) Inorganic Aerogels. Silica gels were the first mineral
gels synthesized under acidic conditions. Of course, natural
triple point gaxous phase
P critical organic gels are more common today. It is possible to
vapour
convert all metals or semiconductor oxides to gels. The
temperature most common mineral aerogels are silica aerogels,
T P
titanium, zirconium, tin, aluminum, vanadium, chromium,
Temperature
iron, tantalum, molybdenum, and niobium-based aerogels.
FIgurE 10: How to find the critical point using pressure-tem- Bi- nary or ternary oxide aerogels can also be synthesized.
perature diagrams [80–82]. Of 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 couple common organic compounds used to synthesize these
aerogels are resorcinol-formaldehyde and melamine-
formaldehyde (resin-formaldehyde). Condensation of the
Vapour outlet mentioned organic compounds in alkaline aqueous so-
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
[80–82]. pyrolysis process at temperatures below 1000 °C increases
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
Hydrogel immersed Ageing 24 hours
in sodium
bicarbonate
Solvent exchange
for 24 hours 50oC, x3
Wet Gel Heat at 70oC,

4 hours
Followed by APD at 150oC
Silica aerogel
Immersion in Ni
Aerogel + EG + NiCl2 ion solution
+ NaOH + N2H4
Ni-SiO2 aerogel Autoclave 110oC
(a)
+NiCl2 +NaOH, N2H4

Aerogel immersed in Ni ion solution In situ reduction 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].
Engineering
H2N
N NH2
H
2 H2O +
N N + 2 O C H H
H NH
NH2 H2N N C O C N N 2
N H2 H2
N N
N N
NH2
NH2
FIgurE 14: Melamine-formaldehyde density reaction for organic aerogel synthesis [82].
process in solution phase
of these aerogels is obtained at a temperature of As600 °C.
the temperature gradually increases, the amount of cavities
decreases and at temperatures above 2100°C the volume of
cavities reaches zero, which indicates the formation of
closed cavities. Carbon aerogels are synthesized in various
forms such as monoliths, powders, films, and granules, the
properties of which are shown in Figure 15
[76, 83, 160, 161].
(4) Hybrid Aerogels. The synthesis of aerogels using

organic-mineral compounds, also known as hybrid
aerogels, significantly increases the applications of aer-
ogels. For example, with the introduction of organic
structures into the silica surface, their hydrophobic and
elastic properties are improved. Hybrid aerogels are
usually synthesized by the sol-gel method. One of the
main advantages of hybrid aerogels over other aerogels is
their lower fragility [149].
4. Advantages of Sol-Gel Method

(i) Simplicity of the process
(ii) Preparation of high purity products;
(iii) Very high production efficiency
(iv) Production of optical components with complex
shapes
(v) Synthesis of uniform compounds in the form of
composite oxides
(vi) bility of designing and controlling chemical
composition and obtaining a homogeneous
composition
(vii) Ability of using the product with special shapes
such as fibers and aerogels
(viii) Surface coverage
(ix) Ability of using this process to synthesize amor-
phous materials in thin layers
(x) Production of materials with modified physical
properties, such as low thermal expansion coeffi-
cient, low UV absorption, and high optical
transparency
(xi) Production of porous and rich materials with
organic and polymeric compounds
(xii) High chemical reactivity of precursors due to
(xiii) Precise control of material structure with the

possibility of adjusting the variables of the early
stages of tuberculosis and network formation
(xiv) Low initial investment while having high quality
products
The sol-gel process is a common and almost old
method [161]. In the mid-nineteenth century, the tendency
to use the sol-gel process to synthesize mineral ceramics
and glass materials began with the efforts of the likes of
Ebelman and Graham and the study of silica gels. In the
1950s, extensive studies began on the synthesis of
ceramics and glass structures using the sol-gel method.
This method has the ability of synthesizing many mineral
oxides such as TiO2, SiO2, and ZrO2. Depending on the
drying conditions of the wet gel, two types of dry gels
are obtained, aerogels and xerogels. By definition, an
aerogel is a dry gel obtained by 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 the gel that results from
the conversion of tuberculosis to gel during the
compaction process. The sol-gel process involves the
transfer from the liquid phase of the “cell” (colloidal
solution) to the “gel” phase. Figure 16 shows the types of
gel processing methods and techniques presented to turn it
into products. As can be seen, the products can be
produced both in powder and thin layers and in porous
or dense materials [76–83].
Inorganic metal salts or organic metal compounds
such as metal alkoxides are commonly used as precursors.
Col- loidal suspension or “cell” is formed after a series of
hydrolysis reactions and condensation of precursors. The
TB particles then condense into a continuous liquid (gel)
phase. With additional drying and heat treatment, the gel
becomes a dense glass or ceramic material. In general,
three reactions are used to describe the sludge process: (1)
hydrolysis, (2) alcohol condensation, and (3) water
condensation. Figure 17 shows the general steps of the sol-
gel process and the types of synthesized materials. Because
water and alkoxides are in- compatible, alcohols are
commonly used as a solvent. Due to the presence of a
solvent, the cellulose and alkoxide precursors mix well
with the water and facilitate the hydrolysis process. Figure
18 shows the hydrolysis and compaction reactions (in both
water and alcohol) in the sol-gel process to produce silica
gel.
During the hydrolysis reaction, by adding water to the
alkoxide groups (OR), these groups replace the hydroxyl
Engineering
Structure
- SEM
- gas adsorption
- Hg-porosimetry backbone
- SAXS/SANS connectivity
- X-ray tomography - thermal solid phase conductivity
- electrical conductivity
Chemical Composition
Surface groups
- EDX Mechanical
Properties
- FTIR
- XPS - ultrasound velocity
- 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
Evaporati
Electro Deposition Dip coating Spin coating

Dense Ceramic
Coating of complex Coating of 3D Ultrathin flat coatings Xerogel

objects objects
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
groups increases, the nanoparticles begin to bridge with glass or ceramics. Figure 19 shows the different gel states
each other to form a silica network. As soon as the wet gel including wet gel, dry gel, and aerogel [76–83].
dries,
Precursor
(usually mixture of metal, bimetallic or
-oxobimetallic alkoxide)
Hydrolysis
S
Condensation
G
Critical Point Melt at lower
Drying temperature
1. Thin films
2. Fibers
3. Spheres
Special Glasses
4. Grains ity
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 + H2 RO Si OH + R-OH
OR O OR
Step 2: condensation
(a) Water condensation
OR OR
OR OR
RO Si OH + OH Si RO Si O Si OR + H2O
OR 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.
Engineering
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
particle size must be small enough that the Brownian
alcohols. For this purpose, first the solvent (usually
motion of the particles overcomes the force of gravity and
containing water, alcohol, organic solvents, or a proportion
prevents them from settling. In this way, the resulting
of them) and the precursor are mixed in a container to
mixture re- mains homogeneous for a long time. If TB has
obtain a homogeneous solution. To achieve a homogeneous
such characteristics, it can be hoped that a homogeneous,
solution, a mixture of two solvents in specific
pure, and high-yield product will be produced [55–60].
concentrations is often used to fully dissolve the precursors.
For example, some metallic organic precursors must first be
dissolved in a water-soluble organic solvent and then the 5.3. Gel Formation. In order to form a gel, it is sufficient to
resulting solution is dissolved in water. However, in cases stimulate the solution in some way, so that the dispersed
where the precursor is metal salt, it is soluble directly in fine particles (each containing several molecular or atomic
water and does not require an organic solvent. Although units of the corresponding precursors) begin to collect [84–
alkoxide precursors are more widely used, the sol-gel 87]. By creating physical and chemical interactions between
process can be performed in other ways, in which, instead sus- pended particles and those dispersed in the
of homogeneous tuberculosis, a “relatively stable colloid” tuberculosis solution, units of tens of thousands of
is used for gel formation. Metal alkoxides, as precursors molecules line up together to form an infinitely large three-
used in the sol-gel method, are a class of organic metal dimensional molecule that occupies the entire volume of
compounds consisting of an organic base attached to a the reaction vessel [61, 65, 88, 89]. Figure 21 shows the
metallic or quasimetallic element. As an interesting example, compression reaction for the synthesis of silica gel from a
consider silicon tetroxide (OC2H5)4. This precursor is also 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 but in the compaction reaction two simple molecules
water to form simpler molecules are called hydrolysis. combine to form a more complex molecule. As the mole-
Figure 20 shows an overview of the steps of the sol-gel cules combine in the compaction reaction, a small molecule
method, including the formation of a homogeneous such as water is released. A compaction reaction is possible
solution, the formation of the sol, the conversion of the sol- when two hydroxides (or one hydroxide + one metal alk-
gel, and the removal of the solvent from the gel (drying). oxide) (M-OR + HO-M) combine to form a metal oxide
The hydrolysis reaction is a simple reaction and to initiate it (M- O-M) [71–73]. Therefore, the gel produced will be
some water is added to the reaction medium. Water is soluble and in order to complete the sol-gel process and
added when a homogeneous solution is prepared in a water- achieve a dry gel the solvent must be separated using some
free solvent. The presence of water causes a hydrolysis methods. The produced gels have different types depending
reaction on the precursor and somehow activates it so that on the solvent used or the drying method and show various
the metal oxide particles come together to form fine and properties and applications [74, 75].
solid particles dispersed in the solvent [40–45]. In a real
solution, the solute is dispersed uniformly in the solvent as
an atom, molecule, or ion, and the particle size does not 6. Application of the Nanomaterials Prepared
exceed 1 nm. If the particle size of the solvent is greater by Sol-Gel Method
than 100 nm, the particles gradually settle to form a (i)Synthesis at low temperature
suspension mixture [46–50]. If the particle size varies
(ii)Preparation of high purity products
between 1 and 100 nanometers, they usually remain
scattered throughout the mixture, which is called colloid. (iii)Very high production efficiency
The sol consists of very fine particles (less than 100 nm) (iv) Production of optical components with complex
dispersed in the solvent phase and are, in fact, a solution or shapes
more precisely a colloidal mixture [51–54]. Thus, (v) Synthesis of uniform compounds in the form of
according to the above explanations, a comprehensive composite oxides
definition of tuberculosis can be given; the
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
Tetraethoxysilane (TEOS) CH2-H3-OH O 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
Vanadium O(Amt)3 -C(CH3) (CH2-CH3)CH3-OH O
Hydrolysis
Polymerization Dip Coat Drying Heat
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
obtaining homogeneous composition optical 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
Engineering
H3CH2CO O
Si O
OCH CH O O HO O O
2 3 Si Si
H 3CH 2CO Si H 3CH 2CO O
O
HO
OCH CH Si OH OCH CH
H CH CO 2 3
O O O O
3 2 2
Si Si Si Si
O O O
HO
O O
Si OH
O
O
pore
O
solid
network
Starting solution Sol

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

Advances in Materials Science and

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

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

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

Precursors + Solvents Aerogel

Sol Formation Connected porous Final Products

Solution of precursors Sol Gel

Dense ﬁlm Dense ﬁlm

Fibers of KCC-1 KCC-1-NH2

Xerogel ﬁlm Dense ﬁlm

Uniform powder Aerogel

(b) Hydrogel (c) Aged hydrogel

(d) Salt free hydrogel

Drying at room temp. for 24 h and 50 oC, 200 oC

(g) Hydrophobic Silica Aerogel (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

Hydrogel aged in EtOH

Hydrogel immersed Ageing 24 hours

Wet Gel Heat at 70oC,

Ni-SiO2 aerogel Autoclave 110oC

+NiCl2 +NaOH, N2H4

(4) Hybrid Aerogels. The synthesis of aerogels using

4. Advantages of Sol-Gel Method

(xiii) Precise control of material structure with the

FIgurE 15: Characteristics of carbon aerogels [68].

Electro Deposition Dip coating Spin coating

Coating of complex Coating of 3D Ultrathin ﬂat coatings Xerogel

(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

[21] B. Li, X. Wang, M. Yan, and L. Li, “Preparation and char-

method in the CO methanation reaction: CO elimination

graphene quantum dots/NiO nanocomposites for antibac-

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