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Materials Today: Proceedings 2 (2015) 1051 – 1055

5th International Conference on Perspectives in Vibrational Spectroscopy

Synthesis and characterization of iron oxide nanoparticles using

DMSO as a stabilizer
S. Veena Gopala, R. Minib, V. Bena Jothyb, I. Hubert Joea*
a
Centre for Molecular and Biophysics research, Department of Physics, Mar Ivanios College, Thiruvananthapuram-629 015, Kerala, India
b
Department of Physics, Women’s Christian College, Nagercoil-629 001, Tamil Nadu, India

Abstract

Magnetite (Fe3O4) nanoparticles were prepared by the reverse co-precipitation method from the solution of ferrous/ferric
mixed salt. The variation in morphology and size has been studied by coating the particle with an organic solvent like
DMSO (Dimethyl sulphoxide) at its different concentration. Meanwhile, Fe3O4 nanoparticles without coating are also
synthesized under the same condition for comparison. The particle size and the nature of the nano crystals are characterized
by X-Ray Diffraction (XRD). UV visible spectrum of the synthesized nanoparticles has been taken. The surface
morphology of the sample is studied by scanning electron microscopy (SEM). The SEM image indicates that the particles
are uniformly distributed and shape of the particles is semi-spherical in nature. The crystalline size of the particles ranges
from12-4nm with the increasing concentration of DMSO (Dimethyl Sulphoxide) SEM studies shows that the
agglomeration of the particle is found sensitive to DMSO concentration. Fourier transform infrared microscopy result
indicates the interaction of DMSO with Fe3O4 nanopartices.

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Spectroscopy.

Keywords: DMSO; FTIR; XRD; SEM;

*Corresponding author. Tel.: +91-471-2531053; fax: +91-471-2530023.

E-mail address: hubertjoe@gmail.com

2214-7853 © 2015 Elsevier Ltd. All rights reserved.

Selection and Peer-review under responsibility of the Conference Committee Members of the 5th International Conference on
Perspectives in Vibrational Spectroscopy.
doi:10.1016/j.matpr.2015.06.036
1052 S. Veena Gopal et al. / Materials Today: Proceedings 2 (2015) 1051 – 1055

1. Introduction

The synthesis of nanoparticle with uniform particle size is a subject of intensive research in recent times because
of their fundamental scientific interest as well as for the technological importance. With a reduction of their size,
nanoparticles reveal unique properties. The nanoparticles materials often exhibit very interesting electrical, optical,
magnetic, and chemical properties, which cannot be achieved by their bulk counterparts [1, 3]. Especially, iron
oxide and ferrite attract a great deal of interest due to their technological importance in the nanotechnologies of
information storage, magnetic resonance imaging contrast agent, and ferrofluids[4]. They have a significant role in
magnetic devices, catalysts, and drug delivery than any other material. It can be used for gene therapy, insertion of
genes into living cells for treatment of disease [5-9]. An attempt has been made to prepare Fe3O4 nanoparticles
using chemical co precipitation method and is coated with an organic solvent DMSO just as EDTA [10].
Size of the synthesized nanoparticles was characterized using UV visible absorption techniques, X-ray diffraction
techniques and Scanning Electron microscopy. FTIR has also done to verify the interaction of DMSO with the
synthesized nanoparticles. An attempt has been made to understand the effect of DMSO concentration on
nanoparticles formation.

2 Experimental details

2.1Materials

Anhydrous FeCl3, Anhydrous FeCl2, Stabilizers Dimethyl Sulfoxide (DMSO), N2 gas and reducing agents
NaOH.

2.2 Synthesis

4ml of 2M Fecl3 and 2ml of 1M Fecl2 solution was mixed to a 200ml flask. Add 50ml 1M NaOH solution to the
above solution and stirrer well, 50ºC heated for 5 minutes in a deoxygenized atmosphere. A black precipitate was
formed immediately. The experimental results have shown that flowing N2 gas not only protects critical oxidation
but also reduces the particle size when compared with methods without removing the oxygen [11]. The iron oxide
Fe3O4 nanoparticles are produced by the following solid state reaction:

FeCl2 4H2O(s) + 2FeCl3 6H2O(s) ĺ 8NaCl + Fe3O4 + 14H2O

The Fe3O4 nanoparticles are synthesized with the varying concentration of DMSO.

3. Results and discussion

3.1 X-Ray Diffraction studies

The crystallographic analysis of iron oxide samples were performed by powder X-ray diffraction (XRD).
Diffraction patterns (vs2‫ )ڧ‬were recorded using (XPERT-PRO). A continuous scan mode was used to collect 2‫ڧ‬
ranging from 10 to 70°. Fig. 1 (s1), (s2), (s3) and (s4) represents the XRD pattern of Fe3O4 nanoparticles prepared
with varied DMSO concentrations. Six characteristics peaks at 32.26º, 35.79º, 44.49º, 53.71º, 58.11º, 62.15º were
corresponding to the [220], [311], [400], [422], [511] and [400] crystal planes of pure Fe3O4 with a spinel structure
according to JCPDS Card no: 65-3107 [12]. The interplanar distance, d is found to be 2.5ǖ [13], which is identified
as the separation between [220] planes in magnetite. The spot marked as [220] in Fe3O4 are exclusive to magnetite
and cannot be assigned to Fe [12]. The size of particles are calculated using Debye-Sherrer’s equation

D = 0.89λ β cosθ (1)

 S. Veena Gopal et al. / Materials Today: Proceedings 2 (2015) 1051 – 1055 1053

Where D is the particle size, Ȝ is the wavelength of the X-ray used. ȕ and ș are the half width of X-ray diffraction
lines and half diffraction angle of 2ș respectively. Table 1 shows the variation of grain size with DMSO
concentration. The crystallite size of the particles formed without DMSO is found to be 12 nm. By the addition of
2.5ml, 5ml and 7ml, DMSO the crystallite size is found to be 10,7,4 nm respectively.

Table 1. Variation of grain size with DMSO Concentration

Concentration of DMSO(ml) 2‫(ڧ‬degrees) FWHM Grain Size (nm)
0 35.79 0.012 12
2.5 36.88 0.014 10
5 36.91 0.020 7
7 37.12 0.037 4

[311]
[200]

[511][440]
[400]
[422]
Intensity in (au)
(s1)

(s2)

(s3)

(s4)

0 20 40 60 80 100
Angle 2 Theta

Fig. 1(s1) Uncoated Fe3O4 nanoparticl(s2),(S3),(s4) Fig. 2. The variation in particle size with concentration of DMSO
Fe3O4 nanoparticle coated with DMSO at 2.5, 5 and 7(ml)

The particle size was observed to be decreased with increase in DMSO concentration. The variation in particle
size with concentration of DMSO is shown in figure 2

Table 2. Inter planar Spacing and Lattice Parameter corresponding to maximum intensity peak [311]
Sample Interplanar spacing dhklǖ Lattice parameter ‘a’(ǖ) Crystal size estimated from XRD(nm)
Fe3O4 2.50 8.29 12

The lattice parameter ‘a’ and inter planar spacing dhkl are determined by

d (hkl) = λ (2)
2 sin θ
a
d (hkl ) = (3)
h + k2 + l2
2

The lattice parameter and inter planar spacing for the prepared sample is lower than the values reported for the
bulk magnetite JCPDS Code No. 79-0417 (a=8.394 and d311=2.531) [15].
The information regarding lattice strain is calculated from the full width at half maximum of diffraction peaks.
The relation between particle size and strain is estimated using the following equation:
1054 S. Veena Gopal et al. / Materials Today: Proceedings 2 (2015) 1051 – 1055

β cos θ 1 η sin θ
= + (4)
λ ε λ
Where ȕ is a measurement of FWHM in radians, ‫ ڧ‬is Bragg angle of the diffraction peaks, Ȝ is the wavelength of
the X- rays used, İis the effective particle size and Ș is the the amount of strain[16].

3.2 FTIR studies

Figure 3 shows FTIR spectra of the Fe3O4 magnetic nanoparticles as well as DMSO coated Fe3O4 nanoparticles.
The absorption peaks at 540-535 cm-1 corresponds to the Fe-O vibration related to the magnetite phase [17]. Two
absorption bands at 2924 and 2853 cm-1 were attributed to the asymmetric CH2 stretching which emphasize the
presence of methyl group of DMSO get incorporated with sample[R]. The absorption band in the figure 3 at 980 cm-
1
which corresponds to the S=O stretching [18] is shifted to 880 cm-1 due to the hydrogen bonding.

Fig. 3. FTIR spectra of uncoated Fe3O4 nanoparticles and of 7 ml DMSO coated Fe3O4 nanoparticles

3.3SEM studies

The surface morphology of the magnetite without any coating is shown in figures 4. It is seen that the particles
shows a rough spherical structure and were agglomerated. The DMSO coated Fe3O4 shows agglomeration but self-
assembled lamellar structures. The DMSO coated Fe3O4 are found to be monodispersed in size which is very
important because the properties of nano crystal strongly depend up on the dimension of nanoparticles. The figures 4
also shows Fe3O4 nanoparticles are embedded in DMSO coating.

Fig. :4. SEM photograph of Uncoated Fe3O4 nanoparticles and modified Fe3O4 nanoparticles at magnification .

4. Conclusion

In the present study Fe3O4 nanoparticles were synthesized by chemical co-precipitation. Magnetite nanoparticles
show a broad absorption band in the UV-Vis region. From the X-ray diffraction studies it was found that the size of
the magnetite particle decreases with increase in concentration of DMSO, showing the action of the DMSO as a
good surfactant. The grain size is found to be 4-12 nm. The nanoparticles are suitable for the medical application.

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