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Materials Today: Proceedings 2 (2015) 3575 – 3579

4th International Conference on Materials Processing and Characterization

Synthesis and Characterization of SiO2 Nanoparticles via Sol-gel

Method for Industrial Applications
R. S. Dubeya*, Y. B. R. D. Rajeshb, M. A. Morec
a
Advanced Research Laboratory for Nanomaterials and Devices, Department of Nanotechnology,
Swarnandhra College of Engineering and Technology, Seetharampuram, Narsapur-534280 (A.P.), India
b
Department of Chemistry, School of Chemical & Biotechnology, SASTRA University, Tirumalaisamudram, Thanjavur-613401 (T. N.) , India
c
Center for Advanced Studies in Materials Science &Condensed Matter Physics, Department of Physics, University of Pune, India, (M.S.), India

Abstract

Silica nanoparticles have received an intensive attention of scientific community due to its broad applications in industry. The
optical properties of silica nanoparticles can be attained with respect to surface defect related to large surface/volume r atio
according to the applications. In this paper, silica nanoparticles were synthesized from tetraethylorthosilicate (TEOS) as a
precursor and PVP as a surfactant by employing sol-gel method. By XRD measurement, a broad peak of pure amorphous nature
is observed while FTIR analysis showed hygroscopic nature of particles. TEM measurement has also confirmed the amorphous
structure of prepared SiO2 nanoparticles with theiraverage diameter~25 nm. The compositional ratio of silicon and oxygen is
analyzed by EDX and found to be satisfactory.
© 2014 The Authors. Elsevier Ltd. All rights reserved.
© 2015 Elsevier Ltd. All rights reserved.
Selection and peer-review under responsibility of the conference committee members of the 4th International conference on
Selection and peer-review under responsibility of the conference committee members of the 4th International conference on Materials
Materials
ProcessingProcessing and Characterization.
and Characterization.

Keywords: SiO2 Nanoparticles; Sol-gel Method; Transmission Electron Microscopy;Amorphous;

1. Introduction

Silica nanoparticles have received an intensive attention of scientific community due to its wide applications in as
electronic devices, insulator, catalysis or pharmaceuticals. The oxide nanoparticles synthesized by several methods
appears more useful because these nanoparticles have good electrical, optical and magnetic properties that are
different from their bulk counterparts [1].

* Corresponding author. Tel.:+91-970-156-8383; fax: +91-881-424-0443.

E-mail address:rag_pcw@yahoo.co.in

2214-7853 © 2015 Elsevier Ltd. All rights reserved.

Selection and peer-review under responsibility of the conference committee members of the 4th International conference on Materials Processing
and Characterization.
doi:10.1016/j.matpr.2015.07.098
3576 R.S. Dubey et al. / Materials Today: Proceedings 2 (2015) 3575 – 3579

Silica nanoparticles have received much interest for applications such as catalysis, pharmaceuticals, drug delivery
and pigments [2]. Amorphous SiO2 nano-particles are used to make electronic substrates, thin film substrates,
electrical insulators, thermal insulators and humidity sensors. The silica particles play a different role in each of
these products. The quality of some of these products is highly dependent on the size and size distribution of the
silica particles [3]. It is essential to have silica particles of a narrow size distribution and a high purity, as high-tech
industries such as biotechnology and photonics provide a tremendous demand for such materials [4]. The optical
properties of silica nanoparticles can be attained with respect to surface defect related to large surface/volume ratio.

For the synthesis of silica nanoparticles various methods are employed such as micro emulsion processing,
chemical vapor deposition, combustion synthesis, hydrothermal techniques, plasma synthesis, solǦgel processing
etc.[5-7]. Irrespective to the method of synthesis, the main focus was to control the particle size,
particle surface reactivity and morphology. The most common process to synthesize silica nanoparticles is a sol-gel
technique which involves the simultaneous hydrolysis and condensation reaction of the metal alkoxide. Among
several methods, SolǦgel method has some advantages such as low temperature synthesis and control of
reaction kinetics by varying the composition of chemicals. By employing sol-gel method, SiO2
particles of 1μm were first reported by Stober et al. [8], however, nanoparticles of
few hundred nanometers to several micrometers size was reported with respected to the
control hydrolysis of TEOS in ethanol [9]. The size and shape of silica nanoparticles are controllable
with electrolytes, surfactants and organic acids etc. In similar manner, silica nanoparticles were reported
by using electrolyte, sodium iodide, whereas control mechanism of particle size was reported by using
ammonium bromide [10,11]. Further, Wang and coworkers have reported preparation of
cubic silica nanoparticles with the use of organic acid (tartaric acid) [12]. Similarly, the preparation of
silica nanoparticles with hexagonally arrayed mesopores has been reported by using binary surfactants method
[13]. The preparation of nanometer sized mesoporous silica particles with the
addition of triethanolamine as base and cationic surfactant as template was reported [14]. Synthesis of
hexagonal shaped mesoporous silica particles have also been been reported
[15]. Synthesized mesoporous silica nanospheres were reported with uniform size and morphology with the use
of polyvinyl pyrrolidine and different types of cationic surfactants [16]. The sol-gel technique provides many
advantages over other methods, mainly owing to facility, versatility, purity, homogeneity and modifications of
material properties by changing synthesis parameters [17,18].

In this paper, the synthesis of silica nanoparticles by using a facile and economic method is presented. In section
2, the details of synthesis of SiO2 nanoparticles have been presented. The structural and optical properties of
synthesized particles are discussed in Section 3. Finally, Section 4 concludes the paper.

2. Experimental

By using sol-gel metod, SiO2 nanoparticles were produced. All the reagents used were of analytical grade without
any further purification. Tetraethylorthosilicate (99.9%, Aldrich), absolute ethanol (EtOH 99.5%, System), acetic
acid (S.D. Fine) and PVP (LOBA) have been used in this work. To a stirred solution of Tetraethylorthosilicate
(TEOS) (2.2 mL), was added acetic acid (2.3 mL) and continued stirring for 10 min. 12 mL of 5 wt % solution of
PVP in ethanol was added slowly to the above solution and the mixture was allowed to stir for 1 h in order to form
sol. After aging for 24 h, the sol was transformed in to gel. In order to get nanoparticles, the gel was dried at 100 0C
for 2 h to evaporate water and organic compounds. Then the dry gel was calcinated at 500 0C for 3 h to obtain a
powder which was grinded to get nanoparticles. The produced silica nanoparticles were characterized for the
structural and optical properties. The XRD pattern of SiO2 was obtained using X-ray diffractometer (Schimadzu
Model: XRD 6000) with CuKα radiation in the range of 20-80o (λ=0.154nm). The surface morphology of particles
was measured by Transmission Electron Microscope (TEM: JEOL-2010) with an accelerating voltage of 100kV.
The infrared spectra were recorded using Fourier-Transformed Infrared Spectrophotometer (FT/IR-610, JASCO) in
transmission mode in the wave number region between 4000 and 400 cm -1. UV-VIS absorption spectra SiO2 was
recorded using a spectrophotometer (Varian Cary 5E) at room temperature in the range of 200-800 nm. In order to
 R.S. Dubey et al. / Materials Today: Proceedings 2 (2015) 3575 – 3579 3577

observe the morphology and acquisition, EDX analysis is done by using scanning electron microscopy (SEM: JEOL
JSM-5800 LV/EDS).

3. Results & Discussion

The prepared silica nanoparticles were studied by x-ray diffraction (XRD) measurement and shown in fig.1. The
XRD pattern shows a typical broad peak which is corresponding to the amorphous phase of prepared silica
nanoparticles.

Fig.1: XRD pattern of SiO2 nanoparticles prepared by sol-gel method.

This broad XRD reflection peak may be due to the small size and incomplete inner structure of the prepared
particles. This demonstrates that a high percentage of these particles are amorphous [19]. No other impurity peak is
present which represents the purity of the silica nanoparticles.

Fig.2 shows high resolution (HR)-TEM images along with selected area electron diffraction (SAED) pattern of
the silica nanoparticles prepared by sol-gel method. TEM images at low and high magnifications are depicted in Fig.
2(a) and (b) which confirms that the morphology consists of almost spherical particle with low aggregation.

(a) (b) (c)

Fig.2. HR-TEM images and diffraction pattern of SiO 2 nanoparticles calcinated at 500 0C.
3578 R.S. Dubey et al. / Materials Today: Proceedings 2 (2015) 3575 – 3579

The nanoparticles have an average diameter of ~25 nm. The small particles due to the increase in the OH group
concentration leads to the reduction in the rate of hydrolysis and condensation reaction which consequently inhibit
the growth of the larger particles. Therefore, by increasing amount of ethanol, the particle size and particle size
distribution of the powder can be controlled. The TEM images illustrate that the crystallites are more in angular
shape and little elongated. Fig.2(c) shows the SAED pattern in which the absence of bright points and rings support
the amorphous nature of the as-prepared silica nanoparticles.

Fig. 3(a) shows FTIR spectra of the resulting silica nanoparticles. The band around ~ 808 cm -1 corresponds to Si-O
[20] bending vibration where the oxygen move at the right angle to the Si-Si lines in the Si-O-Si plane [20, 21]. The
absorption at ~ 964 cm-1 corresponds to Si-OH bending vibration.

Fig. 3. FTIR fig.(a) and EDX fig.(b) spectrum of silica nanoparticles synthesized by sol-gel method.

The band around 1057 cm-1 corresponds to asymmetric stretching vibration of Si-O-Si band which the bridging
oxygen atom moves parallel to the Si-Si lines in the opposite direction to their Si neighbors. The band around 3422
cm-1 corresponds to Si-OH stretching vibration, hydrogen bonded [21]. FTIR analysis shows that the silica particles
are very hygroscopic in nature. There is also another detected peak at 1635cm-1 in the IR spectrum which is
attributed to Si-H2O flexion [22]. For compositional analysis of SiO2 nanoparticles, EDX measurement is done and
shown in fig. 3(b).For SiO2 nanoparticles, the required composition of Si and oxygen was achieved without the
presence of any impurity and atomic % of Si and O2 was that of SiO2 as shown in figure.

4. Conclusions

By employing sol-gel method, amorphous SiO2 particles have been synthesized and characterized. For the
synthesis of silica nanoparticles, tetraethylorthosilicate as a precursor and PVP as a surfactant were used. In XRD
spectra, a single broad peak has confirmed the amorphous structure of prepared particles. In FTIR analysis, various
absorption peaks were observed and found that the nanoparticles are very hygroscopic in nature. EDX of prepared
SiO2 particles has confirmed the required composition of silicon and oxygen without any contaminants.By TEM, the
amorphous structure of the as-prepared particles is confirmed and the average diameter of mono-dispersed
nanosized silica particles was observed to be ~25 nm which is in good agreement with the XRD result. Finally, sol-
gel method is easy and inexpensive for the production of SiO2 nanoparticles for industrial applications.
 R.S. Dubey et al. / Materials Today: Proceedings 2 (2015) 3575 – 3579 3579

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