Materials Chemistry and Physics 113 (2009) 933–936
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Materials Chemistry and Physics
journal homepage: www.elsevier.com/locate/matchemphys
Synthesis and characterization of a mesoporous silica microsphere
from polystyrene
N. Venkatathri
∗
, S. Nanjundan
Department of Chemistry, Anna University, Chennai 600 025, Tamil Nadu, India
article info
Article history:
Received 31 January 2008
Received in revised form 16 August 2008
Accepted 19 August 2008
Keywords:
Polystyrene
Mesoporous
Silica nanosphere
abstract
Even though there are several methods available in literature to synthesis mesoporous silica nanosphere,
the method suitable for cosmetic applications is none. There are two different methods are known for
possible encapsulation of ultraviolet ray absorber (2,2
′
,4,4
′
-tetrahydroxy benzophenone). They are pre-
and post-synthesis modification. In this report, we have succeeded by pre synthesis modification. Further,
we have used polystyrene and cetyltrimethylammonium chloride as template for the first time to synthesis
mesoporous silica nanosphere. The synthesized material was characterized by several physicochemical
techniques. The results show that the synthesized material is mesoporous, which can hold good number
for ultraviolet ray absorber.
© 2008 Elsevier B.V. All rights reserved.
1. Introduction
Nanometer to micrometer-sized materials is widely used in
different areas of process industries. There are several research
focused on the preparation of nanospheres. This is an important
class of materials science having applications in the field of deliv-
ery of encapsulated products for cosmetic and medical purposes
to their use as lightweight composite materials and as fillers with
low dielectric constant in electronic components [1]. Applications
for silica nanospheres also cover areas such as catalysis, acoustic
insulation, piezoelectric transducers and manufacture of advanced
materials [2]. Various materials have been used for the prepara-
tion of nanospheres, for example, polymers, glasses, metals and
ceramics [1]. The methods currently used to fabricate a wide range
of stable spheres include nozzle reactor processes, emulsion/phase
separation, sol–gel processing and sacrificial core techniques [1].
The latter involves the use of cores that are coated with the mate-
rial interest. The core is subsequently dissolved or volatilized by
heating, leaving the shell of the desired hollow microsphere.
The fabrication of hollow spheres has been greatly impacted
by the layer by layer (LbL) self-assembly technique. This method
allows the construction of composite multilayer assemblies based
on the electrostatic attraction between nanoparticles and oppo-
sitely charged polyions [3–9]. An important extension of the
method is the preparation of multilayers of colloids on three-
dimensional substrates. For example, polystyrene beads were
∗
Corresponding author. Tel.: +91 9486565702.
E-mail address: venkatathrin@yahoo.com (N. Venkatathri).
coated with homogeneous layers of colloidal silica particles [10,11].
LbL-coated colloidal spheres of 640 nm comprising layers of titania
or silica were used for the preparation of macroporous structures
[12].
In the present study, the polystyrene and cetyltrimethylammo-
nium chloride were employed as template for the preparation of
mesoporous silica nano structures. The material synthesized by this
method was used for cosmetic applications by pre synthesis mod-
ification. Further the material was also characterized by various
physicochemical techniques.
2. Experimental
Mesoporous silica nanospheres were synthesized by the following method.
The reaction mixture was prepared by mixing 34.4ml tetraethyl orthosilicate (98%,
Aldrich, USA), cetyltrimethylammonium chloride (3.96 ml, CTACl, 25%, Aldrich, USA)
and polystyrene suspension (90 ml, 4.8%) in the polyethylene bottle at 298 K and
stirred vigorously for 24h. The resulting solids were collected by centrifugation,
washed with ethanol–water (1:1, v/v) mixture solution and dried at 333K for 12h.
Surfactant micelles were partly removed by washing with 0.1 M HCl–EtOH, filtering
and drying in an oven. The rest of surfactant and polystyrene spheres were com-
pletely removed by subsequent calcination in air at 823 K for 8 h at a heating rate of
1.5 K min
-1
to obtain hollow core silica capsules.
The polystyrene spheres used in the above synthesis were prepared by follow-
ing method. It was prepared by dispersion polymerization of styrene in water with
potassium per sulfate as initiator. A 250-ml three-necked round bottomed flask,
equipped with a mechanical stirrer, a condenser and connection with a nitrogen
reservoir was used. The monomer solution was prepared by mixing 20 ml of styrene
with 78 ml of water in the flask at 343 K. Potassium per sulfate (2 g) was dissolved in
the above monomer solution. Polymerization was carried out under nitrogen atmo-
sphere by stirring (350 rpm) the mixture solution at the temperature 343 K for 4 h.
The resulting polystyrene suspension was centrifuged and the residue was collected
(spherical shape, 300 nm diameter) and used for mesoporous silica nanosphere
synthesis.
0254-0584/$ – see front matter © 2008 Elsevier B.V. All rights reserved.
doi:10.1016/j.matchemphys.2008.08.072