Synthesis and Studies of PANI/Cerium Dioxide Nanocomposites: E. Kumar, P. Selvarajan
Synthesis and Studies of PANI/Cerium Dioxide Nanocomposites: E. Kumar, P. Selvarajan
Synthesis and Studies of PANI/Cerium Dioxide Nanocomposites: E. Kumar, P. Selvarajan
Department of Physics, Infant Jesus College of Engineering and Technology, Keela vallanadu, Tuticorin- 628851, Tamilnadu, India; 2Department of Physics, Aditanar College of Arts and Science,
Tiruchendur-628216, Tamil Nadu, India; 3PRIST University, Thanjavur, - 613 403, Tamil Nadu, India
Abstract
Introduction
Experimental
Materials
The aniline (AR grade MERCK) was distilled twice under reduced
pressure. Ammonium persulphate[(NH4)2S2O8] (Analytical regant,
RANBAXY fine chemicals Limited, india), Hydrochloric acid (AR
grade MERCK) and ammounium Ce(IV) nitrate, [(NH4)2Ce(NO3)6]
(AR grade MERCK) and Sodium hydroxide [NaOH] (AR grade
MERCK) were used to prepare the nanocomposites of this work.
Water used in this investigation was de-ionized water.
Synthesis
Initially, Ceria (CeO2) nanoparticles was prepared as follows: the
precursors like ammounium Ce(IV) nitrate ((NH4)2Ce(NO3)6) and
Sodium hydroxide (NaOH) were taken in 1:4 molar ratio and
dissolved completely in de-ionized water. Here the pH value of the
solution was adjusted to be 12. The mixture solution was stirred well
using a magnetic stirrer for about 1 hour with a stirring rate of 1000
rpm. Then the prepared mixture solution was kept in the microwave
oven (900 W, 2450 MHz., Onida, India) at a temperature of 500C for
about for 30 minutes. When ammounium ceric nitrate is treated
with sodium hydroxide, the hydrolysis process takes place and the
products like sodium nitrate, ammonium hydroxide and cerium
hydroxide are formed. During the reaction, one proton(H+) is
removed from cerium hydroxide due to polar nature of water and
this leads to the formation of hydrated cerium dioxide. Synthesized
pale-yellow precipitate was filtered and washed with de-ionized
water twice. Annealing of the synthesized powder at 130 oC in air
for 2 hours results in the formation of CeO2 nanoparticles. The
following chemical reaction takes place in the formation of ceria
nanoparticles.
y ((NH4)2Ce(NO3)6) + x (NaOH) x (NaOH) + y (NH4OH) + CeO2
nH2O + H3O+
Polyaniline / CeO2 nanocomposite was prepared as follows: 4.5 ml
aniline was injected to 70 ml of 2 M HCl containing 2 g of CeO2
nanoparticles under ultrasonic action to reduce the aggregation of
nanoparticles. After 12 h, 4.5 g Ammonium Persulphate(APS) (
dissolved in 20 ml de-ionized water) was dropped into solution with
constant stirring for about 10 minutes. The polymerization was
allowed to proceed for 3 h at 300 C. Reaction mixture was filtered
under gravity, and washed with 2 M HCL and de-ionized water,
afterwards dried at 900 C for 12 h in vacuum to obtain a fine tint
green powder.
Instrumentation
Powder X-ray diffraction pattern of the nanoparticles was obtained
using a powder X-ray diffractometer (PANalytical Model, Nickel
filtered Cu K radiations with = 1.54056 at 35 KV, 10 mA). The
sample was scanned over the required range for 2 values(1070o). The powder XRD pattern of the sample was recorded at RRL,
Trivandrum. The FTIR spectrum of the sample was recorded at
M.K.University, Madurai using a Shimadzu 8400S spectrometer by
the KBr pellet technique in the range 400-4500 cm-1. The optical
spectra of nanocomposites
have been recorded in the region
190-1100 nm using a Perkin Elmer (Model:Lambda 35) UV-vis-NIR
spectrometer at M.K.University, Madurai. The SEM image of the
synthesized cerium dioxide nanoparticles was recorded using a
Hitachi Scanning Electron Microscope at IIT, Chennai. The size and
shape of nanoparticles were obtained by transmission electron
microscopy (TEM). TEM measurements were carried out on a
HITACHI H-7500 TEM. Sample for TEM was prepared on 300 mesh
JES
ISSN: 2218-1768
where
is
the
Conclusion
Acknowledgement
The help and supports extended in the research by IIT, Chennai,
RRL (Trivandrum), CECRI(Karaikudi), M.K.University(Madurai) are
gratefully acknowledged. Also we thank authorities of Management
of Aditanar College of Arts and Science, Tiruchendur, Infant Jesus
References
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