International Journal of Mechanical Engineering and Technology (IJMET)
(IJM
Volume 10, Issue 1, January 2019,
201 pp. 785–790, Article ID: IJMET_10_01_080
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ISSN Print: 0976-6340
6340 and ISSN Online: 0976-6359
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SYNTHESIS OF SIO2 NANO PARTICLES BY
USING SOL-GEL ROUTE
S. Saravanan,
Saravanan A.Godwin Antony, V.Vijayan
Department of Mechanical Engineering,
K. Ramakrishnan College of Technology, Trichy, Tamil Nadu, India
M.Loganathan
Department of Mechanical Engineering,
M.Kumarasamy College of Engineering, Karur. Tamilnadu, India
S. Baskar
Department of Automobile Engineering, VELS Institute of Science,
Technology & Advanced Studies
Studies (VISTAS), Tamil Nadu, India
ABSTRACT
The sol-gell route is a simple chemical m ethod for fabricating the nano particles
through bonding of atoms at the scale of 10-9 m. It is most widely used in the
fabrication of oxides of metals chemically. The properties relating to physical,
chemical & optical are enhanced
nhanced at this size range. One of the important factors is
that, the relative surface area of the nano materials are increased when compared
with the bulk material. Controlling the annealing temperature would result in various
micro structures for the compound being produced. The tetra hydrofuran and silicic
acid solution was formed by stirring at room temperature for a time period of 60
minutes and subsequently annealed at 400°C. The crystallite sizes of prepared nano
particles decreased along with the increase in surface area monotonically owing to
increase of the silica content in the mixture.
Keywords: Nano Particles,
articles, SiO2, Sol-Gel Process.
Cite this Article: S. Saravanan, A.Godwin Antony, V.Vijayan, M.Loganathan and S.
Baskar, Synthesis of Sio2 Nano Particles by Using Sol-Gel
Gel Route,
Route International
Journal of Mechanical Engineering and Technology, 10(1), 2019, pp. 785–790.
785
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1. INTRODUCTION
Nano technology is helping to revolutionize the technology and industry sectors such as
information technology, energy, environmental science, medicine, homeland security, food
safety, transportation and so on. Cause nano materials to differ from larger materials are the
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S. Saravanan, A.Godwin Antony, V.Vijayan, M.Loganathan and S. Baskar
increased relative surface area. When a particle gets smaller, the surface-to-volume ratio
gradually increases, leading to an increasing proportion of atoms on the surface of the
particles. Another factor that shapes the nano scale behaviour is the predominance of quantum
effects that takes place as the electrons are confined by the dimensions of the nanostructure.
The quantum effect starts to dominate the properties of matter like optical, electrical and
magnetic behavior of materials, when the size is reduced to a few tens of nano meters. The
chemical and physical properties exhibited by these materials depend on both the composition
and the degree of homogeneity.
2. REVIEW OF LITERATURE
Jiangyao Chen et al. (2010) studied the synthesis and characterization of SiO2 and TiO2 copillared montmorillonite composite for adsorption and photo catalytic degradation of
hydrophobic organic pollutants in water. A series of SiO2 and TiO2 co-pillared
montmorillonite photo catalyst with excellent adsorption capacity and high photo catalytic
activity were synthesized via sol-gel method by pillaring both SiO2 and TiO2 mixed sol into
sodium montmorillonate. Various material characterization techniques such as powder X-ray
diffraction, Nitrogen adsorption/desorption isotherms and Scanning Electron Microscopy
were used to examine the pillar montmorillonite. 2, 4, 6 trichlorophenol, a typical
hydrophobic organic pollutant was used as a model pollutant to evaluate the adsorption
capacity and photo catalytic activity of the prepared co-pillared montmorillonates. The
experimental results indicate that the adsorption capacity of the pillered montmorillonates
increased with the increase of the molar ratio of SiO2 to TiO2. Siti Aida Ibrahim & Srimala
Sreekantan (2010) studied the effect of pH on TiO2 nano particles via sol-gel method. Their
XRD results showed the existence of nano crystalline anatase phases with crystallite size
ranging from 7-14 nm. It was noticed that pH affects particles size and degree of crystallinity.
The most efficient photo catalyst is the TiO2 made at pH=9 with following characteristic as
anatase and crystallite size of 8.4 nm. Aminreza Noghrehabadi et al. (2011) studied the heat
transfer enhancement of water in the presence of SiO2 nano particles over an isothermal
stretching sheet. In order to make investigations the boundary layer governing differential
equations were transformed to a set of ordinary differential equations using similarity
transformations. The effect of SiO2 nano particles on the heat transfer characteristics was
studied. Heat transfer characteristics of the boundary layer over a continuous stretching sheet
were investigated. The results revealed that increase of nano particle volume fraction
increases the non-dimensional heat flux, reduced Nusselt number are approximately linear.
Also it was observed that any increase of nano particle volume fraction increase the
magnitude of temperature profiles. Daeyeon Lee et al. (2007) demonstrated the structure and
properties of layer-by-layer assembled multilayer thin films comprising positively charged
TiO2 and negatively charged SiO2 particles. Anatase titanium-dioxide nano particles STS100 (18wt% TiO2 suspension in water, average particle size 7 nm, silica nano particles Ludox
(40wt% SiO2 suspension in water average particle size 22 nm and specific surface area 140
m2/g) were purchased. Sequential adsorption of TiO2 and SiO2 nano particles on to glass
substance was performed using an automated dipping machine. The concentration of each
nano particle suspension was adjusted to 0.03 wt%. The pH of each nano particles suspension
was adjusted using 1.0 M HCl or NaOH. Glass substrates were decreased with 2 vol. %
detergent solution and then cleaned with 1.0 M NaOH solution under sonication for 15 min.
Deionized water was used to make the nano particle suspensions. The dipping time in each
nano particle solution was 10 min followed by three rinse steps (2, 1 and 1min) in Deionized
water. The pH of the nano particles suspension was readjusted after deposition of every three
by layers corresponding to approximately 1.5 hr. A Barnstead thermolyne furnace was used to
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Synthesis of Sio2 Nano Particles by Using Sol-Gel Route
calcinate the films at 550oC for 2 hr. Changes in the Zeta-potential of TiO2-SiO2 multi layers
assembled on polystyrene microsphere at different conditions were indicated.
3. SYNTHESIS OF SIO2 NANO PARTICLES
Silicon dioxide also known as silica is a chemical compound it is an oxide of silicon with the
chemical formula SiO2. It is most commonly found in nature as sand or quartz as well as in
the cell walls of diatoms. Silica is manufactured in several forms including fused quartz,
crystal, fused silica, colloidal silica, silica gel and aero gel. Silica is one of the most abundant
oxide materials in the earth’s crust. It can exist either amorphous form or crystalline form.
Often it occurs as a non-crystalline oxidation product on the surface of silicon or silicon
compounds. There are three crystalline forms of silica namely quartz, tridymite and
cristobalite (Kibombo et al. 2013). It is used primarily in the production of glass for windows,
drinking glasses, beverage bottles and many other uses. The majority of the optical fibers used
for telecommunication are also made from silica. It is a primary raw material for ceramics
such as earthenware, stoneware and porcelain (Pinho & Mosquera 2011). Silica is a common
additive in food production, where it is primarily used as a flow agent in powdered foods or to
absorb water in hygroscopic applications. It is also a primary component of rice husk, ash and
cement manufacturing. The Si atom shows tetrahedral coordination with 4 oxygen atoms
surrounding with a central Si atom. In most thermodynamically stable crystalline forms of
silica, all the four vertices of the SiO4 tetrahedra are shared with others, yielding a net
chemical formula SiO2. It is noted that, fourth oxygen atom is bonded with each silicon atom;
either behind the plane of the screen or in front of it and these atoms is omitted for clarity.
The properties of SiO2 are given in Tables 1.
Table 1 Properties of SiO2
Properties
Density(g/cm3)
Thermal conductivity(Wm-1K-1)
Poisson’s ratio
Modulus of elasticity (GPa)
Melting point (ºC)
Values
2.2
1.4
0.165
73
1830
The uniqueness of structural characteristics, energetic and chemical properties of
nanostructures constitutes the basis of nano science. Manipulated control of the properties and
response of nanostructures can lead to new devices and technologies. For the synthesis of
nano materials and nanostructures, two approaches are mainly used namely top-down and
bottom-up. Top-down approach implies the breaking down of the bulk material into nano
sized structures or particles. Top down is realized by breaking, cutting or etching techniques,
which is achieved by bulk or film machining, surface machining and mold machining
occupying lithography. Bulk machining makes use of photolithography, which applies the
etching process while mold machining uses soft lithography. There are four types of top down
approach such as Ball milling, Laser ablation, Electro deposition and Sputtering. In Bottomup approach technique the materials are buildup from the bottom, atom-by-atom, moleculeby-molecule or cluster-by-cluster. In this technique synthesis of nano materials first forms the
nano structured building blocks (nano particles) and then collects these into the final material.
The building blocks may be manipulated through controlled chemical reactions to selfassemble and make nanostructures such as nanotubes and quantum dots (Rajeev et al., 2006).
There are four types of bottom-up approach such as Sol-Gel method, Hydrothermal Method,
Chemical Vapor Deposition and Templating.
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S. Saravanan, A.Godwin Antony, V.Vijayan, M.Loganathan and S. Baskar
The Sol-Gel method is a versatile process used for synthesizing various oxide materials.
This method generally allows control of the texture, the chemical and morphological
properties of the solid. This method also has several advantages over other methods, such as
allowing impregnation or co-precipitation, which can be used to introduce dopants (Sue-min
Chang & Ruey-an Doong, 2006). The major advantages of the sol-gel technique includes
molecular scale mixing, high purity of the precursors and homogeneity of the Sol-Gel
products with good physical, morphological and chemical properties (Siti Aida Ibrahim &
Srimala Sreekantan 2010). In a typical sol-gel process, a colloidal suspension or a sol is
formed from the hydrolysis and polymerization reactions of the precursors, which are usually
inorganic metal salts or metal organic compounds such as metal alkoxides (Chaochinsu et al.
2006). Complete polymerization and loss of solvent leads to the liquid sol transforming into a
solid gel phase. A wet gel will form when the sol is cast into a mould and the wet gel is
converted into a dense ceramic upon further drying and heat treatment. This method involves
hydrolysis of the metal alk oxide with water and catalyst i.e., an acid or a base, condensation
into macromolecules, forming a colloidal sol and subsequently, three dimensional network,
solvent exchange to remove water by alcohol, then drying the wet gel using a super critical
fluid to produce the aero gel (Mahbubul et al. 2013). Aero gels can be used for advanced
applications including electrochemical devices, thin coatings, composite biomaterials,
catalysts, ceramics, heat and electric insulation devices due to the aero gels having unique
morphological and chemical properties. Schematic representation of Sol-Gel process
synthesis is shown in Figures 1.
Figure 1 Schematic representation of Sol-Gel process.
However, the property of the sol-gel product depends upon the precursor, processing
temperature, catalyst, solvents and solvent removal process. The sol-gel route demonstrated a
high potential for controlling the bulk and surface properties of the oxides. Depending on the
drying conditions the binary oxide could be obtained. The silica particles were prepared by
adding tetra hydrofuran (C4H8O) with silicic acid (SiO2 x H2O) and this mixture was stirred
at room temperature for 60 minutes. Thus formed gel was dried under 50ºC in vacuum to
remove water and organic impurities. Then the moisture-free dried gel was annealed at 400ºC
for 60 minutes and then crushed using portable ball miller to make fine powders. The
synthesis of SiO2 nano particles is shown in Figure 2.
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Synthesis of Sio2 Nano Particles by Using Sol-Gel Route
Figure 2 Synthesis of SiO2 nano particles
4. CONCLUSIONS
In this work the SiO2 nano powders was prepared by sol-gel route at room temperature. The
silica particles were prepared by adding tetra hydrofuran with silicic acid and this mixture was
stirred at room temperature for 60 minutes and subsequently annealed at 400°C. By
controlling the conditions properly, nano-SiO2 powders of anatase form with the grain size of
~ 6 nm could be obtained. The mole ratio of starting materials and calcinations temperatures
was highly predominating among the factors which affect the grain size of nano particles. The
crystallite sizes of prepared nano particles were decreased and the surface area monotonically
increased with an increase of the silica content.
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