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International Journal of Mechanical Engineering and Technology (IJM
Volume 10, Issue 1, January 201
Available online at http://www.iaeme.com/ijmet/issues.asp?JType=IJMET&VType=
ISSN Print: 0976-6340 and ISSN Online: 0976
© IAEME Publication
SYNTHESIS OF
USING
S. Saravanan
Department of Mechanical Engineering,
K. Ramakrishnan
Department of
M.Kumarasamy College of Engineering, Karur.
Department of Automobile Engineering, VELS Institute of Science,
Technology & Advanced Stud
ABSTRACT
The sol-gel route is a simple chemical m
through bonding of atoms at the scale of 10
fabrication of oxides of metals chemically.
chemical & optical are enhanced
that, the relative surface area of the
with the bulk material. Controlling the annealing temperature would result in various
micro structures for the compound being produced.
acid solution was formed by stirring
minutes and subsequently annealed at 400°C.
particles decreased along with
increase of the silica content in the mixture.
Keywords: Nano Particles,
Cite this Article: S. Saravanan, A.Godwin Antony, V.Vijayan, M.Loganathan and S.
Baskar, Synthesis of Sio
Journal of Mechanical Engineering and
http://www.iaeme.com/ijmet/issues.asp?JType=IJMET&VType=
1. INTRODUCTION
Nano technology is helping to revolutionize the technology and
information technology, energy, environmental science, medicine, homeland security, food
safety, transportation and so on.
IJMET/index.asp 785 editor@iaeme.com
International Journal of Mechanical Engineering and Technology (IJMET)
2019, pp. 785–790, Article ID: IJMET_10_01_080
http://www.iaeme.com/ijmet/issues.asp?JType=IJMET&VType=
6340 and ISSN Online: 0976-6359
Scopus Indexed
OF SIO2 NANO PARTICLES
USING SOL-GEL ROUTE
S. 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 (VISTAS), Tamil Nadu, India
l 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,
nhanced at this size range. One of the important factors
that, the relative surface area of the nano materials are increased when compared
Controlling the annealing temperature would result in various
micro structures for the compound being produced. The tetra hydrofuran
solution was formed by stirring at room temperature for a time period of
subsequently annealed at 400°C. The crystallite sizes of prepared nano
along with the increase in surface area monotonically
of the silica content in the mixture.
articles, SiO2, Sol-Gel Process.
S. Saravanan, A.Godwin Antony, V.Vijayan, M.Loganathan and S.
Baskar, Synthesis of Sio2 Nano Particles by Using Sol-Gel Route
Journal of Mechanical Engineering and Technology, 10(1), 2019, pp. 785
http://www.iaeme.com/ijmet/issues.asp?JType=IJMET&VType=10&IType=
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
editor@iaeme.com
http://www.iaeme.com/ijmet/issues.asp?JType=IJMET&VType=10&IType=1
NANO PARTICLES BY
Tamil Nadu, India
Tamilnadu, India
Department of Automobile Engineering, VELS Institute of Science,
ies (VISTAS), Tamil Nadu, India
ethod for fabricating the nano particles
It is most widely used in the
The properties relating to physical,
One of the important factors is
nano materials are increased when compared
Controlling the annealing temperature would result in various
The tetra hydrofuran and silicic
a time period of 60
The crystallite sizes of prepared nano
surface area monotonically owing to
S. Saravanan, A.Godwin Antony, V.Vijayan, M.Loganathan and S.
Gel Route, International
785–790.
&IType=1
industry sectors such as
information technology, energy, environmental science, medicine, homeland security, food
nano materials to differ from larger materials are the
S. Saravanan, A.Godwin Antony, V.Vijayan, M.Loganathan and S. Baskar
http://www.iaeme.com/IJMET/index.asp 786 editor@iaeme.com
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 co-
pillared 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 STS-
100 (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
Synthesis of Sio2 Nano Particles by Using Sol-Gel Route
http://www.iaeme.com/IJMET/index.asp 787 editor@iaeme.com
calcinate the films at 550o
C 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 Values
Density(g/cm3
) 2.2
Thermal conductivity(Wm-1
K-1
) 1.4
Poisson’s ratio 0.165
Modulus of elasticity (GPa) 73
Melting point (ºC) 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 Bottom-
up approach technique the materials are buildup from the bottom, atom-by-atom, molecule-
by-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 self-
assemble 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.
S. Saravanan, A.Godwin Antony, V.Vijayan, M.Loganathan and S. Baskar
http://www.iaeme.com/IJMET/index.asp 788 editor@iaeme.com
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.
Synthesis of Sio2 Nano Particles by Using Sol-Gel Route
http://www.iaeme.com/IJMET/index.asp 789 editor@iaeme.com
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.
REFERENCES
[1] Jiangyao Chen, Xiaolu Liu, Guiying Li, XinNie, Taicheng An, Shanqing Zhang and
Huijun Zhao, (2010), “Synthesis and characterization of novel SiO2 and TiO2 co-pillered
montmorillonite composite for adsorption and photo catalytic degradation of hydrophobic
organic pollutants in water”, Vol. 164, pp. 364-369.
[2] Siti Aida Ibrahim and Srimala Sreekantan, (2010), “Effect of pH on TiO2 nanoparticles
via Sol-gel method”, Proceedings of International Conference on X-Rays & related
Techniques in Research & Industry, pp. 84-89.
[3] Aminreza Noghrehabadi, Mehdi Ghalambaz and Mohammad Ghalambaz, (2011), “A
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isothermal stretching sheet”, International journal of multidisciplinary Sciences and
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[4] Daeyeon Lee., Damali Omolade., Robert E. Cohen. and Michel F. Rubner. (2007), “pH-
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Chemistry of Materials, Vol. 19, pp. 1427-1433.
[5] Kibombo, H.S., Rasalingam, S. and Koodali, R.T. (2013), “Facile template free method
for textural property modulation that enhances adsorption and photocatalytic activity of
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142, No.143, pp.119-128.
[6] Pinho, L. and Mosquera, M.J. (2011), “Titania-Silica Nanocomposite Photocatalysts with
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[7] Rajeev K. Wahi, Yunping Liu, Joshua C. Falkner and Vicki L. Colvin, (2006),
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surface area”, Journal of Colloid and Interface Science, Vol. 302, pp. 530-536.
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[9] Chaochin Su, Kuei-Fen Lin, Ya-Hui Lin and Bor-Hou You (2006), “Preparation and
characterization of high surface-area titanium-dioxide by sol-gel process”, Journal of
Porous materials, Vol. 13, pp. 251-258.
[10] Mahbubul, I.M., Kamyar, A., Saidur, R. and Amalina, M.A. (2013), “Migration Properties
of TiO2 Nanoparticles during the Pool Boiling of Nano refrigerants”, Ind. Eng. Chem.
Res., Vol. 52, pp.6032-6038.
[11] A. Godwin Antony, S. Baskar, V.Vijayan, S. Saravanan and M.Loganathan (2018),
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reinforcement”, IJMET, Volume 9, Issue 12.
[12] R. Venkatesh, V. Vijayan, A. Parthiban, T. Sathish and S. Siva Chandran (2018),
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[13] G. Navaneethakrishnan, V. Selvam, and S. J. Jaisingh, “Development and Mechanical
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[15] P. Parameswaran, A. Godwin Antony, S. Dinesh, and K. Radhakrishnan, “Experimental
study on mechanical and corrosion characteristics of nab alloy with the addition of
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[16] P. Parameswaran, A. M. Rameshbabu, G. Navaneetha Krishnan, R. Yogeshwaran, and R.
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[17] A. M. Rameshbabu, P. Parameswaran, V. Vijayan, and R. Panneer, “Diffraction,
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[18] R. Venkatesh and V. Vijayan, “Performance evaluation of multipurpose solar heating
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[19] K. Pradeep Mohan Kumar, V. Vijayan, B. Suresh Kumar, C. M. Vivek, S. Dinesh, 2018,
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[20] T. Avudaiappan, V. Vijayan, S. Sundara Pandiyan, M. Saravanan, S. Dinesh
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Ijmet 10 01_080

  • 1. http://www.iaeme.com/IJMET/index. International Journal of Mechanical Engineering and Technology (IJM Volume 10, Issue 1, January 201 Available online at http://www.iaeme.com/ijmet/issues.asp?JType=IJMET&VType= ISSN Print: 0976-6340 and ISSN Online: 0976 © IAEME Publication SYNTHESIS OF USING S. Saravanan Department of Mechanical Engineering, K. Ramakrishnan Department of M.Kumarasamy College of Engineering, Karur. Department of Automobile Engineering, VELS Institute of Science, Technology & Advanced Stud ABSTRACT The sol-gel route is a simple chemical m through bonding of atoms at the scale of 10 fabrication of oxides of metals chemically. chemical & optical are enhanced that, the relative surface area of the with the bulk material. Controlling the annealing temperature would result in various micro structures for the compound being produced. acid solution was formed by stirring minutes and subsequently annealed at 400°C. particles decreased along with increase of the silica content in the mixture. Keywords: Nano Particles, Cite this Article: S. Saravanan, A.Godwin Antony, V.Vijayan, M.Loganathan and S. Baskar, Synthesis of Sio Journal of Mechanical Engineering and http://www.iaeme.com/ijmet/issues.asp?JType=IJMET&VType= 1. INTRODUCTION Nano technology is helping to revolutionize the technology and information technology, energy, environmental science, medicine, homeland security, food safety, transportation and so on. IJMET/index.asp 785 editor@iaeme.com International Journal of Mechanical Engineering and Technology (IJMET) 2019, pp. 785–790, Article ID: IJMET_10_01_080 http://www.iaeme.com/ijmet/issues.asp?JType=IJMET&VType= 6340 and ISSN Online: 0976-6359 Scopus Indexed OF SIO2 NANO PARTICLES USING SOL-GEL ROUTE S. 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 (VISTAS), Tamil Nadu, India l 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, nhanced at this size range. One of the important factors that, the relative surface area of the nano materials are increased when compared Controlling the annealing temperature would result in various micro structures for the compound being produced. The tetra hydrofuran solution was formed by stirring at room temperature for a time period of subsequently annealed at 400°C. The crystallite sizes of prepared nano along with the increase in surface area monotonically of the silica content in the mixture. articles, SiO2, Sol-Gel Process. S. Saravanan, A.Godwin Antony, V.Vijayan, M.Loganathan and S. Baskar, Synthesis of Sio2 Nano Particles by Using Sol-Gel Route Journal of Mechanical Engineering and Technology, 10(1), 2019, pp. 785 http://www.iaeme.com/ijmet/issues.asp?JType=IJMET&VType=10&IType= 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 editor@iaeme.com http://www.iaeme.com/ijmet/issues.asp?JType=IJMET&VType=10&IType=1 NANO PARTICLES BY Tamil Nadu, India Tamilnadu, India Department of Automobile Engineering, VELS Institute of Science, ies (VISTAS), Tamil Nadu, India ethod for fabricating the nano particles It is most widely used in the The properties relating to physical, One of the important factors is nano materials are increased when compared Controlling the annealing temperature would result in various The tetra hydrofuran and silicic a time period of 60 The crystallite sizes of prepared nano surface area monotonically owing to S. Saravanan, A.Godwin Antony, V.Vijayan, M.Loganathan and S. Gel Route, International 785–790. &IType=1 industry sectors such as information technology, energy, environmental science, medicine, homeland security, food nano materials to differ from larger materials are the
  • 2. S. Saravanan, A.Godwin Antony, V.Vijayan, M.Loganathan and S. Baskar http://www.iaeme.com/IJMET/index.asp 786 editor@iaeme.com 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 co- pillared 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 STS- 100 (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
  • 3. Synthesis of Sio2 Nano Particles by Using Sol-Gel Route http://www.iaeme.com/IJMET/index.asp 787 editor@iaeme.com calcinate the films at 550o C 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 Values Density(g/cm3 ) 2.2 Thermal conductivity(Wm-1 K-1 ) 1.4 Poisson’s ratio 0.165 Modulus of elasticity (GPa) 73 Melting point (ºC) 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 Bottom- up approach technique the materials are buildup from the bottom, atom-by-atom, molecule- by-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 self- assemble 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.
  • 4. S. Saravanan, A.Godwin Antony, V.Vijayan, M.Loganathan and S. Baskar http://www.iaeme.com/IJMET/index.asp 788 editor@iaeme.com 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.
  • 5. Synthesis of Sio2 Nano Particles by Using Sol-Gel Route http://www.iaeme.com/IJMET/index.asp 789 editor@iaeme.com 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. REFERENCES [1] Jiangyao Chen, Xiaolu Liu, Guiying Li, XinNie, Taicheng An, Shanqing Zhang and Huijun Zhao, (2010), “Synthesis and characterization of novel SiO2 and TiO2 co-pillered montmorillonite composite for adsorption and photo catalytic degradation of hydrophobic organic pollutants in water”, Vol. 164, pp. 364-369. [2] Siti Aida Ibrahim and Srimala Sreekantan, (2010), “Effect of pH on TiO2 nanoparticles via Sol-gel method”, Proceedings of International Conference on X-Rays & related Techniques in Research & Industry, pp. 84-89. [3] Aminreza Noghrehabadi, Mehdi Ghalambaz and Mohammad Ghalambaz, (2011), “A Theoretical investigation of SiO2 water nanofluid heat transfer enhancement over an isothermal stretching sheet”, International journal of multidisciplinary Sciences and Engineering, Vol. 2, pp. 18-21. [4] Daeyeon Lee., Damali Omolade., Robert E. Cohen. and Michel F. Rubner. (2007), “pH- Dependent structure and properties of TiO2/SiO2 Nanoparticle Multilayar thin films”, Chemistry of Materials, Vol. 19, pp. 1427-1433. [5] Kibombo, H.S., Rasalingam, S. and Koodali, R.T. (2013), “Facile template free method for textural property modulation that enhances adsorption and photocatalytic activity of aperiodic titania supported silica materials”, Applied Catalysis B: Environmental, Vol. 142, No.143, pp.119-128. [6] Pinho, L. and Mosquera, M.J. (2011), “Titania-Silica Nanocomposite Photocatalysts with Application in Stone Self-Cleaning”, J. Phys. Chem., Vol. 115, pp. 22851-22862. [7] Rajeev K. Wahi, Yunping Liu, Joshua C. Falkner and Vicki L. Colvin, (2006), “Solvothermal synthesis and characterization of anatase TiO2 nanocrystals with Ultra high surface area”, Journal of Colloid and Interface Science, Vol. 302, pp. 530-536. [8] Sue-min Chang and Ruey-an Doong, (2006), “Characterizations of Zr-Doped TiO2 Nanocrystals prepared by a Nonhydrolytic Sol-Gel metod at High Temperatures”, Journal of Phys. Chem., Vol. 110, pp. 20808–20814.
  • 6. S. Saravanan, A.Godwin Antony, V.Vijayan, M.Loganathan and S. Baskar http://www.iaeme.com/IJMET/index.asp 790 editor@iaeme.com [9] Chaochin Su, Kuei-Fen Lin, Ya-Hui Lin and Bor-Hou You (2006), “Preparation and characterization of high surface-area titanium-dioxide by sol-gel process”, Journal of Porous materials, Vol. 13, pp. 251-258. [10] Mahbubul, I.M., Kamyar, A., Saidur, R. and Amalina, M.A. (2013), “Migration Properties of TiO2 Nanoparticles during the Pool Boiling of Nano refrigerants”, Ind. Eng. Chem. Res., Vol. 52, pp.6032-6038. [11] A. Godwin Antony, S. Baskar, V.Vijayan, S. Saravanan and M.Loganathan (2018), “Analysis of Wear behaviour of Aluminium composite with Silicon Carbide and Titanium reinforcement”, IJMET, Volume 9, Issue 12. [12] R. Venkatesh, V. Vijayan, A. Parthiban, T. Sathish and S. Siva Chandran (2018), “International Journal of Mechanical Engineering and Technology (IJMET), Volume 9, Issue 12, pp. 922-927. [13] G. Navaneethakrishnan, V. Selvam, and S. J. Jaisingh, “Development and Mechanical Studies of Glass / Banana Fiber Hybrid Reinforced Silica Nano Particles with Epoxy Bio- Nanocomposites,” J. Chem. Pharm. Sci., no. 7, pp. 197–199, 2015. [14] S. Dinesh, K. RadhaKrishnan, A. Godwin Antony, K. Rajaguru, “Experimental Investigation on Machining of Aluminium Metal Matrix using Electrical Discharge Machining,” Adv. Nat. Appl. Sci., vol. 11, no. 7, pp. 809–816, 2017. [15] P. Parameswaran, A. Godwin Antony, S. Dinesh, and K. Radhakrishnan, “Experimental study on mechanical and corrosion characteristics of nab alloy with the addition of chromium,” Mater. Today Proc., vol. 5, no. 2, pp. 8089–8094, 2018. [16] P. Parameswaran, A. M. Rameshbabu, G. Navaneetha Krishnan, R. Yogeshwaran, and R. Ramkumar, “Study of the corrosion properties in a hot forged Cu-Al-Ni alloy with added Cr,” J. Mech. Behav. Mater., vol. 27, no. 3–4, pp. 1–6, 2018. [17] A. M. Rameshbabu, P. Parameswaran, V. Vijayan, and R. Panneer, “Diffraction, microstructure and thermal stability analysis in a double phase nanocrystalline Al20Mg20Ni20Cr20Ti20high entropy alloy,” J. Mech. Behav. Mater., vol. 26, no. 3–4, pp. 127–132, 2017. [18] R. Venkatesh and V. Vijayan, “Performance evaluation of multipurpose solar heating system,” Mech. Mech. Eng., vol. 20, no. 4, pp. 359–370, 2016. [19] K. Pradeep Mohan Kumar, V. Vijayan, B. Suresh Kumar, C. M. Vivek, S. Dinesh, 2018, “Computational Analysis and Optimization of Spiral Plate Heat Exchanger” Journal of applied Fluid Mechanics, Vol. 11, special Issue, pp 121-128. [20] T. Avudaiappan, V. Vijayan, S. Sundara Pandiyan, M. Saravanan, S. Dinesh “Potential Flow Simulation through Lagrangian Interpolation Meshless Method Coding” Journal of applied Fluid Mechanics, Vol. 11, special Issue, pp 129-134.