Journal of

Applied
Chemical
Research

Journal of Applied Chemical Research, 6, 3, 22-26 (2012)

w w w. j a c r. k i a u . a c . i r

Synthesis and Characterizations of Silica Nanoparticles by a

New Sol-Gel Method
B. Gorji1*, M.R. Allahgholi Ghasri2, R. Fazaeli1, N. Niksirat1
1Department of Chemistry, Islamic Azad University, South Tehran Branch, Tehran, Iran
2Department of Chemistry, Islamic Azad University, Shahr-e-ray Branch, Tehran, Iran
(Received 14 Dec. 2011; Final version received 23 May. 2012)
Abstract
Silica nanoparticles were synthesized by chemical methods from tetraethylorthosilicate (TEOS),
polyethylene glycol 5% and hydrochloric acid 0.001 N. The sol-gel process was applied for the
preparation of nano silica gel. This method is hydrolysis and condensation reactions of TEOS as
precursor of silica. The optimal synthesis conditions for the preparation of silica nanoparticles were
obtained and the produced silica nanoparticles were characterized by x-ray diffraction (XRD), scanning
electron microscopy (SEM) and transmission electron microscopy (TEM). The results indicated that
the silica nanoparticles were successfully formed. The prepared samples change from amorphous to
-crystallite phase. The XRD analysis indicated the amorphous structure of the synthesized silica
nanoparticles while the SEM and TEM images exhibited monodispersedNano sized silica particles
with a size about 34 nm. In this study, the soft process of sol-gel reaction is favourable from a view
point of energy conservation. Additionally, the advantages of this technique were the purity of products
and ability to control nanometer sized internal structure.
Keywords: Silica nanoparticles, Tetraethylorthosilicate, Sol-Gel process, Characterization.

Introduction
FNanoporous

The sol-gel methods are the most general

materials

have

stimulated method of synthesis silica nanoparticles.

increasing interests due to their extensive Appetence in the sol-gel processing of ceramic
applications in the fields of catalysis, drug and glass materials started in the half of
delivery, chemical sensors, chromatography,

1800s by Ebelman and Grahams researches

microreactor and biological images [1-6].

on silica gels [10]. The sol-gel technique is

Nano silica has been proven to be a very

inexpensive and the silica gels manufactured

promising material due to its low density,

are non-poisonous matters [11-16].

good thermal and mechanical stability, and

Stober supplied monodisperse and nonporous

chemical inertia [7-9].

silica

spheres

with

the

hydrolysis

of

* Corresponding author: Dr. Banafsheh Gorji, Department of Chemistry, Islamic Azad University, South Tehran Branch,
Tehran, Iran. Email: banafsheh_gorji@yahoo.com, Tel: +9821- 88830820, Fax:+9821- 88828956.

B. Gorji et al., J. Appl. Chem. Res., 6, 3, 22-26 (2012)

23

tetraethylorthosilicate (TEOS) in strongly (~ 7.8). Finally, 10 ml HCl 0.1 N was added at

basic medium. Stober and Fink promoted once to pH about 2.
chemical reactions which checked up the The solution was heated to 80 C for forming
growth of spherical silica particles [17]. Bogush a viscous gel. The prepared samples were
and Zukoski procure monodisperesed silica subjected to heat-treatment temperature for 3
particles with controlled hydrolysis of TEOS

hours ranging 200 up to 1000 C.The X-ray

in ethanol [18]. Sung Kyoo Park provided diffraction (XRD) patterns of the prepared
silica nanoparticles from TEOS in ethanol in samples were recorded with Philips model
order that controlled particle properties using PW1800 and the XRD full text were obtained
a semi-batch process [19]. Ryu had prepared with X Pert-Philips X-ray diffractometer
amorphous silica by oxidation of silicon [20].

with monochromatisedCuK radiation of

In the present work, we suggested a novel wavelength 1.5406 A at 55 kV and 40 mA.

method for preparing amorphous silica The surface morphology and nanostructure
nanoparticles through the sol-gel techniques

of the prepared samples was evaluated using

scanning electron microscopy (SEM) (Philips

Experimental

XL30) and transmission electron microscopy

Materials and Methods

(TEM) (Philips CM 200).

Pure

nano

silica

with

hydrolysis

gel
and

was

prepared

condensation

of Results and discussion

tetraethylorthosilicate (TEOS) as precursor The effects of mole ratio of TEOS to water,

material. The procedure is prepared from amount PEG, concentration and speed of
TEOS in the presence of polyethyleneglycol HCladding and reaction temperature on in
5% (PEG) and hydrochloric acid (HCl) situ nano silica formation were investigated.
0.001 N.5g TEOS was dissolved in 80g PEG

These optimal parameters are presented in

(solution 1). Solid silicagel was produced by

experimental section.A typical sol-gel reaction

drop-wise addition (~ 1 ml/10 min) of 30 ml is hydrolysis and condensation of TEOS

HCl 0.001 N to solution 1 with stirring (250 as a precursor of silica. Both reactions are
rpm) at room temperature until a cloudy concurrent and reversible depending on the
solution was formed.Then it was homogenized reaction conditions such as pH, temperature
by homogenizer device model Art-micra D-8 and so on. The overall sol-gel reaction can be
n 11037 (19000 rpm) for about 30 minutes. written as follows:
The obtained solution was stirred (250 rpm)

Si(OC2H5)4 + 4H2O Si(OH)4 + 4C2H5OH

for 4 days. After this period, pH was measured

Si(OH)4 SiO2 + 2H2O

24

B. Gorji et al., J. Appl. Chem. Res., 6, 3, 22-26 (2012)

The characterization of the prepared silica related data and Scherer equation, we can
nanoparticles was carried out by XRD,

predict average size of silica particles. The

XRD full text, SEM and TEM.XRD analysis Scherer equation is as follow:
indicates that a high percentage of particles are

D =0.9 / B cos

amorphous but a few of them are crystalline. where is wave length of x-ray (A), B is
The major phase is SiO2 quarts and the minor

FWHM (radian) and is position (radian).

phase is SiO2 cristobalite. Figure 1 shows the

From the results it can be found out that the

full-text XRD of silica nanoparticles. Using

size of particles are between 8-80 nm.

Figure 1. Full text XRD spectra of synthesized silica nanoparticles.

It is evident from Figure 2 that Nanosized diameter about 34 nm and spherical structures
silica particles with an average particle were formed.

Figure 2. SEM photogragh of synthesized silica nanoparticles.

B. Gorji et al., J. Appl. Chem. Res., 6, 3, 22-26 (2012)

25

Figure3 showsTEM photographs of the

several nanometers. It shows these particles

synthesized nano silica gel. It indicates that

and also the narrow size distribution of these

diameters of the particles are approximately particles.

Figure 3. TEM images of obtained silica nanoparticles.

Conclusions

nanoparticles using TEOS. In order to achieve

In this study, a simple method for the the best conditions for performing silica
preparation of nanoporous silica based on the

nanoparticles, the optimal parameters should

sol-gel process was investigated. Morphous

be considered. This will enhance the use of

silica nanoparticles with regular spherical silica in many applications in many fields such
structure were obtained successfully using

as catalysis.

TEOS as a precursor. The inner diameter of

nanopore size is about 34 nm. It was found Acknowledgements
the following synthesis parameter must be This research has been completedthrough
taken into consideration in synthesis of silica research plan Synthesis of nano-stationary

26

B. Gorji et al., J. Appl. Chem. Res., 6, 3, 22-26 (2012)

phase based on silica and study of its

9, 254 (1997).

physicochemical properties in removal of some [9] J.M. Thomas, B.F.G. Johnson, R. Raja, G.
pollutants under supports and supervision

Sankar, P.A. Midgley, Acc. Chem. Res., 36(1),

of Islamic Azad University, South Tehran

20 (2003).

Branch.The authors acknowledge the supports

[10] L.L. Hench, J.K. West, Chemical Review,

of Islamic Azad University, South Tehran

90, 133 (1991).

Branch and Sharif Industrial University [11] P. Kortesuo, M. Ahola, S. Karlsson,

for the SEM and TEM measurements and

I.Kangasniemi, J. Kiesvaara, A. Yli-Urpo,

KansaranBinalood co. for XRD measurements. Biomaterials, 21, 193 (2000).

[12] R.A.Cunaso, A. Susha, F. Cunaso, Chem.
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