International Journal Of Scientific & Engineering Research, Volume 5, Issue 2, February-2014
ISSN 2229-5518
Comparative Study on Titania Nanoparticles
Synthesized by Mechanical, Sonomechanical
and Sol-gel methods
Shamim Ahamad Khan*
a
, Irfan Ali Khan
a
, Mohd. Sajid Khan
b
, Manaal Zahera
b
Abstract- Titania nanoparticles synthesized by three different methods like mechanical method (high energy ball milling or HEBM), sonomechanical
method and sol- gel method. In this work, the high energy ball milling (HEBM) was applied to synthesize nanoparticles (NPs) of TiO2 from its
microcrystalline powder for 10, 20 and 30 hours respectively. The titania NPs also synthesized by sonomechanical and sol-gel method. Eventually, they
were characterized by X- ray diffraction (XRD) and UV-Vis absorption spectroscopy. XRD results stated the complete phase formation of titania
nanoparticles and comparatively correlated the crystal size. UV-Vis absorption spectroscopy determines the energy band gap of titania nanoparticles by
using Tauc Relationship.
Keywords- Titania naoparticles, HEBM, Sonomechanical, XRD, UV-Vis absorption spectroscopySol-gel, Band gap, Optical properties.
1INTRODUCTION
Nanoscale materials have very attractive properties, much
attention due to their unique characteristics, which are not
found in bulk materials. For instance, the reactions of NPs
with other materials become more efficient due to their
high surface-to-volume ratios, in addition to the high
percentage of atoms at the grain boundaries. Some studies
have found that in last three decades, the application of
semiconductor heterogeneous photocatalysts, particularly
titania (TiO2) in the photo decomposition of toxic organic
pollutants has been widely examined [1-3]. Titanium
dioxide (TiO2) has potential applications to remove stain or
pigment. The nano sized titania act as catalytic,
photocatalytic, dye sensitized photovoltaic cells, sensors
and antimicrobial agent. Their use has always expanded for
novel applications such as enhancement of self-sensitizing;
self-cleaning and germ free tiles for hospitals, restaurants,
kitchens etc. Coating of nano sized titania on glass,
decomposes the organic molecules particularly on the glass
i.e. self-cleaning capability [4]. Different methods have been
developed for the synthesis of TiO2 nanoparticles like
chemical precipitation [5], hydrothermal crystallization [6],
vapor phase condensation, sputtering, mechanical
methods, sonomechanical methods and sol-gel methods.
Various studies have beenreported for the synthesis of
nanocrystalline materials by mechanical milling,
mechanical alloying and mechanochemical processing [7].
Not long ago, mechanical milling has proved as a simple
technique which can produce nanocrystalline powders in
————————————————
x
a*
Department of Applied Physics (Nanoscience), Integral University,
Kursi Road, Lucknow-226026, India.
PH-+91-522-2890812, 2890730; Fax: +91-522-2890809
E-mail: khanshamimahamad21@gmail.coms
x
b
Department of Biosciences, Integral University, Kursi Road,
Lucknow-226026, India.
large quantities with modified properties [8-12]. In this
paper we discuss the TiO2 nanoparticles synthesis by
mechanical, sonomechanical and chemical process in order
to illustrate the influence of crystallite size.
2EXPERIMENTAL PROCEDURE
2.1 Synthesis
Commercially available TiO2 powder (Otto 99.9%) was
milled in steel jar of 250 mL by using the hardened balls of
different sizes (05 mm, 10 mm and 20 mm) from 10 to 30
hours. Bulk 150gm of TiO2 is taken in grinding jar and 75
mL methanol is added in bulk titania powder, therefore the
paste of titanium dioxide is formed then 10 mm diameter of
50 balls are added in grinding jar, finally the grinding jar is
clamped in ball mill machine for 10 hrs at 350 rpm with
interval 1 hr and reverse rotation 10 minute. After the
completion of 10 hour, material is placed in oven at 70
0
c for
3 hrs. Further the process repeated by using same material
and condition for 20 hrs and 30 hrs.
Sonomechanical method is more effective because the ultra
sonic waves break down the weak forces and some
chemical bonding present in the material, which cannot be
break down by simple milling. In this process the ultra
sonic waves are provided to the sample by the instrument
ultra sonic processor and bath ultra sonicator. In this new
type of sonomechanical synthesis first of all 50 gm of
titanium dioxide is taken in 250 mL beaker then 30 mL of
methanol is added, therefore liquid suspension is formed.
This liquid suspension is placed for 30 minute for ultra
sonication with amplitude 40%, pulse 0.5- 1.0. After that the
grinding of material takes place by ball milling.
Sol-gel method is a one of the best technique known as
chemical solution deposition. In this synthesis process 7.4
mL of titanium (IV) isopropoxide (alpha acer) was added
drop by drop in 1M HNO3 aqueous solution and then
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