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Synthesis and characterization of iron oxide nanoparticles by solvothermal

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Article  in  Protection of Metals and Physical Chemistry of Surfaces · September 2014

DOI: 10.1134/S2070205114050128

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ISSN 20702051, Protection of Metals and Physical Chemistry of Surfaces, 2014, Vol. 50, No. 5 pp. 628–631. © Pleiades Publishing, Ltd., 2014.

NANOSCALE AND NANOSTRUCTURED

MATERIALS AND COATINGS

Synthesis and Characterization of Iron Oxide Nanoparticles

by Solvothermal Method1
Deepti Mishra, Ruma Arora, Swati Lahiri,
Sudhir Sitaram Amritphale, and Navin Chandra
Council of Scientific and Industrial Research Advanced Materials and Processes Research Institute,
Hoshangabad Road, Bhopal (M.P.) 462 064, India
email: ssamritphalerrl@yahoo.co.in
Received August 23, 2013

Abstract—In the present work iron oxide nanoparticles have been synthesized by alkaline solvo thermal
method using anhydrous ferric chloride, sodium hydroxide, polyethylene glycol and cetyl trimethyl ammo
nium bromide and characterized by Xray diffraction (XRD), Fourier Transform Infrared Spectroscopy
(FTIR), Field Emission Scanning Electron Microscopy (FESEM), Energydispersive Xray Spectroscopy
(EDX) and Thermal Gravimetric Analysis (TGA). XRD indicated that the product is a mixture of different
phases of iron oxide viz. gammaFe2O3 (maghemite, tetragonal), Fe2O3 (maghemite, cubic), Fe3O4 (magne
tite, cubic) and εFe2O3(epsilon iron oxide). FESEM studies indicated that size of the particles is observed in
the range of about 19.8 nm to 48 nm. EDX spectral analysis reveals the presence of carbon, oxygen, iron in
the synthesized nanoparticles. The FTIR spectra indicated absorption bands due to O–H stretching, C–O
bending, N–H stretching and bending, C–H stretching and Fe–O stretching vibrations. TGA curve repre
sented weight loss of around 3.0446 % in the sample at temperature of about 180°C due to the elimination of
the water molecules absorbed by the nanoparticles from the atmosphere.

DOI: 10.1134/S2070205114050128

1
1. INTRODUCTION
Iron oxide nanoparticles have been widely studied
in recent years due to their magnetic, optical and cat
alytic properties and applications in diverse areas such
as magnetic resonance imaging [1], drug delivery [2],
ferrofluids [3], catalysis[4] and magnetic nanodevices
[5]. Many techniques have been developed for their
synthesis including coprecipitation, solgel method,
microemulsion technique and hydrothermal tech
nique [6]. Their characteristics depend significantly
on particle size and shape. However, the control of size
is very important as it plays a major role in determining
their properties. In the present work iron oxide nano
particles have been synthesized by alkaline solvo ther
mal method using anhydrous ferric chloride, sodium
hydroxide, polyethylene glycol and cetyl trimethyl
ammonium bromide as surfactant and characterized
by Xray diffraction (XRD), Fourier Transform Infra
red Spectroscopy (FTIR), Field Emission Scanning
Electron Microscopy (FESEM), Energydispersive
Xray Spectroscopy (EDX) and Thermal Gravimetric
Analysis (TGA).
1 The article is published in the original.
2. EXPERIMENTAL
Anhydrous ferric chloride, sodium hydroxide and
cetyl trimethyl ammonium bromide (CTAB) (all of
analytical grade) were procured from Rankem, poly
ethylene glycol was procured from Merck and used as
such without further purification.
For synthesis of iron oxide nano particles, an aqueous
solution of anhydrous ferric chloride (25 g in 250 mL
water), polyethylene glycol (62.5 g), sodium hydroxide
(1.5 M in 250 mL water) and CTAB (2.5 g in 10 mL
water) were mixed together and refluxed at tempera
ture around 198 to 200°C for a period of around 8 h.
After reflux, the system was allowed to cool at ambient
temperature. The product in the form of reddish
coloured gel was collected at the bottom of flask. It was
washed extensively with double distilled water and
finally with acetone and dried at room temperature.
Xray diffraction pattern was obtained using CuKα
radiation on D8 advance Xray diffractometer. The
Xray diffraction intensity was recorded as a function
of Bragg’s 2θ in the angular range of 5°–70°. IR spec
tra was recorded between 500–4000 cm–1 using
Bruker alpha Fourier Transform Infra Red Spectrom
eter. FESEM images and EDX spectra were taken on
Field Emission Scanning Electron Microscope
(FESEM), model NOVA NANOSEM430 of COM

628
 SYNTHESIS AND CHARACTERIZATION OF IRON OXIDE NANOPARTICLES 629

Intensity, cps
10000

8000

6000

4000

2.510
2.691

2.201
2000

2.083

1.692

1.451
1.838
3.664

1.484

1.257
1.311

1.212
2.724
2.992

2.383

1.226
3.221

20 40 60 80
2θ, deg

Fig. 1. XRD pattern of synthesized iron oxide nano particles.

FEI and Energydispersive Xray spectroscopy compared with JCPDS data [File Number 251402,
(EDX), Model XMAX of Oxford. Thermal Gravi 2481, 19629, 16895] [7]. No other phase due to
metric Analysis (TGA) was performed by heating impurity was detected in the sample.
sample at a heating rate of 10°C from 30°C to 800°C FESEM image of synthesized nanoparticles is
on Tolendo TGA/DSC1 of Mettler company. shown in Fig. 2 and EDX spectra is shown in Fig. 3.
Several particles were investigated to determine parti
cle size. It can be seen that sample consist of the parti
3. RESULTS AND DISCUSSION cles which are well dispersed and almost spherical in
shape. The size of the particles varies in the range of
Xray diffraction pattern of synthesized nanoparti about 19.8 nm to 48 nm. EDX spectral analysis reveals
cles is shown in Fig. 1. The pattern showed diffraction
peaks at 3.664, 3.221, 2.992, 2.724, 2.691, 2.510,
2.383, 2.201, 2.083, 1.838, 1.692, 1.484, 1.451, 1.311,
(а)
1.257, 1.226, 1.212 which can be indexed to the mix
Spectrum 1
ture of iron oxides viz. gammaFe2O3 (maghemite,
tetragonal), Fe2O3 (maghemite,cubic), Fe3O4 (mag
netite, cubic) and εFe2O3(epsilon iron oxide) when

nm 40 μm
.8
19
(b)
nm

Spectrum 1
.7

C
48.0 nm O
23

Fe

0 1 2 3 4 5 6 7
500 nm keV

Fig. 2. FESEM Image of synthesized iron oxide nano par Fig. 3. EDX spectra of synthesized iron oxide nano parti
ticles. cles. (a) Selected area, (b) EDX outcomes.

PROTECTION OF METALS AND PHYSICAL CHEMISTRY OF SURFACES Vol. 50 No. 5 2014

630 DEEPTI MISHRA et al.

100
TGA curve of iron oxide nano particles is shown in
BRUKER
Fig. 5. The TGA curve represented weight loss of
80
Transmittance, %

around 3.0446 % in the sample at temperature of

60 about 180°C. This weight loss can be due to the elimi
40 nation of the water molecules absorbed by the nano
20 particles from the atmosphere after that sample weight
is almost constant [13] which indicates the thermal
stability of the sample.
3354.47

2359.49

1621.25

1033.57

3500 3000 2500 2000 1500
Wave number, cm–1
Fig. 4. FTIR spectra of synthesized iron oxide nano particles.
the presence of carbon, oxygen and iron in synthesized
nanoparticles. The appearance of peak of carbon in
EDX spectra is due to presence of organic linkages of
ethylene glycol and CTAB.
The FTIR spectrum of synthesised nanoparticles
shown in Fig. 4 indicated presence of absoption
bands at 3354, 2359, 1621, 1033, 920 and 602 cm–1.
These observed bands may be due to O–H stretching
(3354 cm–1), C–O bending (2359 cm–1), N–H
stretching and bending (1621 cm–1), C–H stretch
ing (1033 cm–1), vibrations [8, 9] and vibrations of Fe–
O bond (602 cm–1) which is in agreement with the lit
erature values [10, 11].
The absorption band at 3354 cm–1 appeared due to
absorption of moisture by nanoparticles from the envi
ronment [12]. This was further supported by the
weight loss observed in thermogravimetric analysis.
602.26
920.83
1000 500 4. CONCLUSION
Iron oxide nano particle were synthesized successfully
by a alkaline solvo thermal technique and characterised
using various sophisticated complementary techniques.
XRD studies confirmed that the product is a mixture of
different phases of iron oxide viz. gammaFe2O3
(maghemite, tetragonal), Fe2O3 (maghemite,cubic),
Fe3O4 (magnetite, cubic) and εFe2O3(epsilon iron
oxide). FESEM studies indicated that size of the particles
is in the range of about 19.8 nm to 48 nm. EDX spectral
analysis reveals the presence of carbon, oxygen, iron in
the synthesized nanoparticles. Further studies on tailor
ing of shape and size of nanoparticles for application in
radiation shielding are under way.
5. ACKNOWLEDGMENTS
Authors are grateful to Director CSIRAMPRI
Bhopal for providing necessary institutional facilities and
encouragement. We acknowledge thanks to Mr. Anup
Khare and Mr. Mohd. Shafique, CSIRAMPRI, Bho
pal (M.P.) India for analysis of samples on FESEM
and EDX and providing data of thermal analysis and

mg

66.5 Step: 3.0446%

2.0285 mg

66.0

65.5 Sample weight: 66.6270 mg

65.0

64.5

64.0 50 100 150 200 250 300 350 400 450 500 550 600 650 700 750

0 5 10 15 20 25 30 35 40 45 50 55 60 65 70

Fig. 5. TGA curve of synthesized iron oxide nano particles.

PROTECTION OF METALS AND PHYSICAL CHEMISTRY OF SURFACES Vol. 50 No. 5 2014

 SYNTHESIS AND CHARACTERIZATION OF IRON OXIDE NANOPARTICLES
Xray diffraction pattern of sample. Thanks are also
due to Dr. Neelesh Jain, SIRT, Bhopal (M.P.) India
for providing IR spectra of sample.
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PROTECTION OF METALS AND PHYSICAL CHEMISTRY OF SURFACES Vol. 50 No. 5 2014
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