Journal of Magnetism and Magnetic Materials 323 (2011) 897902

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Journal of Magnetism and Magnetic Materials

journal homepage: www.elsevier.com/locate/jmmm

Investigations on structural and magnetic properties of cobalt ferrite/silica

nanocomposites prepared by the coprecipitation method
Sunil Rohilla a,c,n, Sushil Kumar b, P. Aghamkar b, S. Sunder b, A. Agarwal a
a
Materials Science Laboratory, Department of Applied Physics, Guru Jambheshwar University of Science and Technology, Hisar 125001, India
b
Materials Science Laboratory, Department of Physics, Chaudhary Devi Lal University, Sirsa 125055, India
c
The Technological Institute of Textile and Sciences, Bhiwani 127021, India

a r t i c l e in f o abstract

Article history: Magnetic nanocomposites consisting of cobalt ferrite nanoparticles embedded in silica matrix were
Received 13 July 2010 prepared by the coprecipitation method using metallic chlorides as precursors for ferrite. Subsequently
Received in revised form composites were annealed at 100, 200 and 300 1C for 2 h. The samples were structurally characterized by
27 October 2010
X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FTIR) and transmission electron
Available online 7 November 2010
microscopy (TEM). The magnetic properties were measured in the temperature range of 10300 K using
Keywords: vibrating sample magnetometer (VSM). The effects of thermal treatment on structural and magnetic
Magnetic nanocomposite properties of nanocomposites were investigated. When the samples were annealed, CoFe2O4 nanocrys-
Coprecipitation tallites were observed in the SiO2 matrix, whose size increases with increase in annealing temperature.
Cobalt ferrite
The coercivity and saturation magnetization of nanocomposite (annealed at 300 1C for 2 h) are much
Silica matrix
higher than that of bulk cobalt ferrite. The realization of adjustable particle sizes and controllable
Coercivity
magnetic properties makes the applicability of the CoFe2O4 nanocomposite more versatile.
& 2010 Elsevier B.V. All rights reserved.

1. Introduction important method to avoid particle agglomeration and control of

The unique properties of nano-scaled magnetic particles have
generated more interest in the science community because these
nanocrystallites have a high surface to volume ratio leading to magnetic
properties contrary to those of bulk particles and exhibit unique
functional applications in, color imaging, catalysis [1], high density data
storage [2], magnetically guided drug delivery [3], ferro-uids [4] and
magnetic refrigeration systems [5]. Metal oxide nanoparticles are
currently the subject of research interest because of their unusual
optical, electronic and magnetic properties [6,7]. Among them, cobalt
ferrite is a well known hard magnetic material with a strong magnetic
anisotropy, high coercivity, moderate saturation magnetization along
with good mechanical hardness and chemical stability [8]. These
properties make it a promising material for high-density magnetic
recording [9], permanent magnets, magnetic uids, catalysis, photo-
magnetic material [10,11] and in developing new cell thawing agents
[12]. Many synthetic approaches have been employed to prepare
magnetic nanocrystals [1319]. The nanocrystals produced usually
have a strong tendency to aggregate, which makes it very difcult to
exploit the physicochemical properties. The dispersion of nanopar-
ticles in inorganic, polymer, vitreous and amorphous matrices is an
n
Corresponding author at: Materials Science Laboratory, Department of Applied
Physics, Guru Jambheshwar University of Science and Technology, Hisar 125001,
India.
E-mail address: rohillasunil2003@yahoo.co.in (S. Rohilla).
particle size [20]. In addition, such nanocomposites may have many
advantages from a technological point of view, allowing to improve
catalytic [21], magnetic [22], magneto-optic [23] and mechanical
properties [24] of the material. The coprecipitation process has been
proved to be an efcient method to prepare ultra-ne particles
dispersed in different matrices [25]. Using this method, a control over
the surface morphology, structure and chemical composition can be
attained by carefully monitoring the preparation parameters.
In the present work, nanocomposites of cobalt ferrite dispersed
in a silica matrix were prepared by the coprecipitation method
followed by heat treatment. The authors optimized the annealing
temperature and annealing time and made their sincere efforts to
prepare the nanocomposites at low temperatures of 100, 200 and
300 1C for 2 h. XRD, FTIR, TEM and VSM studies of the prepared
samples were carried out. Special attention has been given to the
correlation between structure and magnetic properties of cobalt
ferrite embedded in a silica matrix.
2. Experimental
2.1. Sample preparation
2.1.1. Step-I: Synthesis of CoFe2O4 nanosuspension
The proposed suspension was prepared using the coprecipita-
tion method. High purity reagents like cobalt chloride hexahydrate

0304-8853/$ - see front matter & 2010 Elsevier B.V. All rights reserved.
doi:10.1016/j.jmmm.2010.11.001
898 S. Rohilla et al. / Journal of Magnetism and Magnetic Materials 323 (2011) 897902

(CoCl2  6H2O; Aldrich 99.99%), ferric chloride hexahydrate
(FeCl3  6H2O; Aldrich 99.99%), HCl (37%) and double distilled water
were used. In this method, solution mixture of 0.6 M CoCl2  6H2O in
40 ml of 0.4 M HCl, and 0.7 M FeCl3  6H2O in 70 ml of 0.4 M HCl was
added through piezoelectric nozzle (nozzle size: 0.05 mm, drop
rate: 0.01 ml/s) into 200 ml 1.5 M NaOH aqueous solution, and the
resulting solution was heated at 50 1C for 2 h with constant stirring
at 8000 rpm for homogenization. The pH of the solution was
controlled to 1112, as it was observed that the samples synthe-
sized below a pH value of 10.6 do not show the formation of spinel
ferrite phase and above a pH value of 12, mixed phase was formed
[26]. Finally the solution was allowed to cool and then diluted to
twice its volume. A dark brown precipitate in water suspension was
obtained.
2.1.2. Step-II: Synthesis of SiO2 nanosuspension
In this step, suspension of SiO2 was prepared by adding 0.3 M
SiO2 (AR grade; Aldrich 99.99%) in 50 ml 0.6 M NaOH (Aldrich
99.99%), which gave rise to Na2SiO3; this solution when added
using piezoelectric nozzle (nozzle size: 0.05 mm, drop rate:
0.02 ml/s) with 50 ml 0.6 M HCl gave a white precipitate of SiO2
in the suspension form. The suspension so obtained was stirred at
8000 rpm for 3 h at 50 1C and then washed many times with
distilled water to remove NaCl completely from the suspension.
2.1.3. Step-III: Synthesis of CoFe2O4/SiO2
The resultant suspensions of step-I and step-II were mixed
smoothly by stirring for 6 h at 8000 rpm. The temperature of the
system was kept constant at 60 1C in a water jacketed reaction vessel
using circulating thermostatic bath. The resultant precipitates were
then ltered and washed many times; and then dried at 80 1C in a
vacuum oven at a pressure of 100 mm of Hg for 6 h. The dried sample
was ground to a very ne powder. These ne powdered samples
were then heated at 100, 200 and 300 1C separately for 2 h using a
programmable furnace. In this way the nanocrystallite of cobalt
ferrite embedded in silica matrix was obtained.
2.2. Sample characterization
Complementary methods were used to characterize the struc-
ture and phase of heat treated samples. XRD of samples was
recorded by a Philips X-ray diffractometer PW/1710 comprising the
BraggBrentano geometry with Ni lter, using monochromatic
CuKa radiation of wavelength 1.54056 A at 50 kV and 40 mA, in the
range 2y  10701. The analysis of size, shape and particle dis-
tribution of the samples was carried out using a transmission
electron microscope (Hitachi-H7500) at 100 kV. For this purpose,
dispersions of sample nanoparticles were pipetted onto carbon-
coated copper grids. Infrared spectra were recorded using a Fourier
transform infrared spectrometer (Perkin Elmer 1600) in the range
2500400 cm  1, on the pellets obtained by dispersing the samples
in KBr. Magnetization data were recorded by a vibrating sample
magnetometer VSM, P525 option with PPMS, QD6000, with a
maximum eld of 60 kOe, in a temperature range 10300 K.
relates the direction of propagation of scattered beams (yhkl) to the
interplanar distance (dhkl) in the lattice, hkl is the property of the
material and is related to the lattice constant and Miller indices
[2729].
The plane spacing equation for the cubic crystal is given by
2 2 2 2
1=d h k l =a2 2
Combining Braggs law and plane spacing equation, we have
2 2 2 2
sin2 yhkl l =4a2 h k l 3
Fig.1 shows the X-ray diffraction patterns of as-prepared and
annealed powder samples. The diffractogram of the as-prepared
sample shows that the crystalline phase of cobalt ferrite was not
developed while diffractograms of annealed samples show the
spinel phase of cobalt ferrite with no extra lines corresponding to
any other crystalline phases. All the spectra show a hump around
231, which corresponds to the amorphous matrix of SiO2. Peaks in
diffractograms were indexed by comparing the interplanar dis-
tances with JCPDS data. The powder sample calcined at 100 1C for
2 h, shows diffraction peaks at 2y 30.081 (2 2 0), 35.411 (3 1 1),
43.081 (4 0 0), 56.961 (5 1 1) and 62.51 (4 4 0). These diffraction
peaks may be assigned to spinel face centered cubic cobalt ferrite
(JCPDS File No. 22-1086), which conrms the formation of CoFe2O4
nanocrystallites. When the temperature was increased to 200 1C
for 2 h, no signicant change in the diffraction pattern was
observed. When the diffraction pattern was minutely examined,
it is noticed that intensity and sharpness of the diffraction peak
around 2y  35.061 were increased. Increase in sharpness of the
diffraction peak may be due to the merging of individual nanos-
tructures and as a result the activation energy becomes larger. It is
interesting to note that when the sample was calcined at 300 1C for
2 h some new peaks appeared at 2y  18.281 (1 1 1), 37.051 (2 2 2),
53.441 (4 2 2) (JCPDS File No. 22-1086), which reects the complete
formation of face centered cubic spinel cobalt ferrite. The d-values
(inter planner spacing) and a-values (lattice constant) are calcu-
lated using Eqs. (1)(3) and are in good agreement with the JCPDS
data (Table 2). The strong and sharp diffraction peak around
2y 35.061 was employed to estimate the mean crystallite size
i.e. the diameter of CoFe2O4 nanoparticles using the DebyeScherer
formula [30], Dhkl kl/b cos y (where k is a constant taken as 0.9,
b is the full width at half maximum (in radians), y is the Bragg angle

3. Results and discussion

3.1. XRD analysis

The XRD diffractograms are scanned using BraggBrentano

geometry with a scanning speed of (2y 11/min) and a step
size 0.011 (2y). X-ray diffraction can be pictured as a reection
of the incident beam from the lattice planes. The Braggs law
Fig. 1. XRD of cobalt ferrite/silica nanocomposites: as-prepared, 100, 200 and
2dhkl Sin yhkl nl 1 300 1C for 2 h.
 S. Rohilla et al. / Journal of Magnetism and Magnetic Materials 323 (2011) 897902
Fig. 2. FTIR spectra of cobalt ferrite/silica nanocomposites: as-prepared, 100, 200
and 300 1C (2 h).
and l is the wave length of X-ray radiation used) and found to be
18, 27 and 39 nm for the sample calcined at 100, 200 and 300 1C
for 2 h, respectively. These results show that the crystallite size
increases with increase in calcination temperature because of the
coalescence of nanoparticles, which is in agreement with reported
results [31].
899
3.2. FTIR analysis
FTIR spectra, recorded in wavenumber range 2500400 cm  1,
of as-prepared and heat treated samples are shown in Fig. 2. In the
as-prepared sample, strong absorption bands were observed at
467, 798, 1090 and 1631 cm  1, which may be assigned to SiOSi
symmetric bond stretching vibration, vibration mode of ring
structure of SiO2 tetrahedra [32], to mode of SiOSi asymmetric
bond stretching vibration [33] and bending vibration modes of
HOH absorbed in silica [34], respectively. The characteristic
absorption bands at 1090, 799 and 467 cm  1 indicate the forma-
tion of silica network [35]. The shoulder at 954 cm  1 was probably
due to the contribution from SiOFe vibrations and from SiOH
stretching vibrations. The presence of SiOFe vibrations reected
some interactions between the highly secluded Fe3 + ions and the
adjacent silica network. In addition, a faint band at 590 cm  1 may be
attributed to the presence of cobalt ferrite [36]. The poor develop-
ment of ferrite structure in as-prepared sample is evidenced by the
broadening of ferrite band. This fact is in agreement with XRD
results, which showed poor crystallinity in the as-prepared sample.
In sample a (calcined at 100 1C (2 h)) the enhanced intensity of the
band at 590 cm  1 with increase in annealing temperature shows the
development of cobalt ferrite phase in the sample, which is also
revealed by the XRD data. For sample b (calcined at 200 1C (2 h)),
the absorption bands about the silica network are further broadened.
These data showed that there was a rearrangement process for the
silica matrix network [37]. When the sample was heat treated at
300 1C (2 h) the absorption peak at 1090 cm  1 for SiOSi further
broadened, while that for the SiOSi bending mode at 799 and
467 cm  1 became stronger. In addition, the band at 955 cm  1
drastically disappeared. These results correspond to the production
of well crystallized cobalt ferrite. It is worth mentioning that a
similar phase was developed at higher temperatures (6001000 1C)
as reported by other workers [3842]. Moreover, at 300 1C (2 h), the
elimination of water molecules, SiOH and volatiles in the samples
occurred resulting in the densication of CoFe2O4/SiO2, which is
conrmed by XRD. A denser matrix made matter diffusion more
difcult, justifying the formation of nanocomposites with narrower
particle size distribution as observed in TEM.
3.3. TEM analysis
The morphology and microstructure of the sample calcined at
300 1C (2 h) were investigated by TEM and shown in Fig. 3(a). From
the TEM micrograph, it can be analyzed that homogeneously
distributed, well crystallized and nearly spherical CoFe2O4 nano-
particles are embedded in silica host matrix. The rings in the
Fig. 3(b) are assigned to cobalt ferrite and are well resolved at
(1 1 1), (3 1 1), (4 0 0) and (4 4 0) reections in XRD. The average
particle size estimated by a statistical method is approximately 21,
27 and 36 nm, respectively, which are in accordance with the
values calculated by XRD. The microstructure of uniformly dis-
persed and small grains is desired for high coercivity.
3.4. Magnetization studies
In order to investigate the magnetic properties of the calcined
powder samples, magnetization as a function of the applied eld
was carried out at different measuring temperatures using VSM.
Signicant variation in the hysteresis loops was obtained with the
measuring temperature as well as the annealing temperature of
samples. The hysteresis loops of the samples calcined at 100, 200
and 300 1C for 2 h are shown in Fig. 4(a), (b) and (c), respectively.
From 10 to 300 K, all the samples exhibit hysteresis and display
a large increase in the width of the hysteresis loop as the measuring
900 S. Rohilla et al. / Journal of Magnetism and Magnetic Materials 323 (2011) 897902

20 nm
Direct Mag: 600000x

Fig. 3. TEM micrographs of cobalt ferrite/silica nanocomposites: (a) the morphology micrograph and (b) Selected area electron diffraction pattern of the sample heat treated at
300 1C (2 h).

1.5 10 K 1.5
10 K
50 K
50 K
1.0 100 K
1.0 100 K
200 K
200 K
300 K 300 K
0.5 0.5
M (emu/g)

M (emu/g)

0.0 0.0 o
200 C (2h)
-0.5 o -0.5
100 C (2h)

-1.0 -1.0

-1.5 -1.5

-60 -40 -20 0 20 40 60 -60 -40 -20 0 20 40 60

H (kOe) H (kOe)

1.5
10 K
50 K
1.0 100 K
200 K
0.5
300 K
M (emu/g)

0.0 o
300 C (2h)

-0.5

-1.0

-1.5

-60 -40 -20 0 20 40 60

H (kOe)

Fig. 4. Magnetization curve of cobalt ferrite/silica nanocomposites annealed at (a) 100 1C (2 h), (b) 200 1C (2 h) and (c) 300 1C (2 h) at different measuring temperatures.

temperature of the sample is lowered. The magnetic parameters of coercivity (Hc), which were measured at room temperature (300 K),
different samples are listed in Table 1. It is found that the values of rst increases with increase in annealing temperature which can be
saturation magnetization (Ms), remanent magnetization (Mr) and attributed to the inuence of the average particle size induced by
 S. Rohilla et al. / Journal of Magnetism and Magnetic Materials 323 (2011) 897902 901

Table 1
Magnetic parameters of CoFe2O4 /SiO2 nanocomposites.

Magnetic parameters Sample (annealing Measuring temperature

temperature (1C))
10 K 100 K 200 K 300 K

Hc (kOe) a (1 0 0) 10.28 2.464 1.45 1.18

b (2 0 0) 12.97 8.904 6.32 4.08
c (3 0 0) 17.25 10.99 4.38 2.17

Mr (emu/g) a (1 0 0) 8.663 3.90 3.01 2.33

b (2 0 0) 15.50 11.27 10.18 8.26
c (3 0 0) 16.70 14.79 11.89 8.03

Ms (emu/g) a (1 0 0) 17.81 16.97 15.30 12.94

b (2 0 0) 26.31 25.58 23.70 20.76
c (3 0 0) 20.19 20.10 20.05 18.21

Table 2 authors optimized the annealing temperature and the annealing

Structural parameters of CoFe2O4 /SiO2 nanocomposites (300 1C, 2 h). time and made their sincere efforts to prepare the nanocomposites
at low temperatures 100, 200 and 300 1C for 2 h. The amorphous
Serial 2h (deg.) d (A) exp. dn (A) JCPDS hkl a (A)
number silica network provides an ambient nucleation environment
for cobalt ferrite particles and hence conne them to aggregation
1 18.280 4.8491 4.8470 111 8.39925 and coarsening. The cubic spinel ferrite crystallites with nanometer
2 30.080 2.9684 2.9680 220 8.39612 dimensions were formed. The structure and magnetic properties of
3 35.410 2.5309 2.5310 311 8.39452
4 37.050 2.4244 2.4240 222 8.39862
the resultant particles were investigated by XRD, FTIR, TEM and
5 43.080 2.0979 2.0990 400 8.39219 VSM. By controlling the annealing temperature, particles with an
6 53.440 1.7131 1.7130 422 8.39285 average size from 18 to 39 nm can be prepared. The magnetic
7 56.960 1.6153 1.6150 511 8.39379 particles exhibit a strong dependence on annealing temperature as
8 62.560 1.4835 1.4190 440 8.39233
well as on measuring temperature. The coercivity of nanocompo-
sites is much higher, while the saturation magnetization of nano-
the annealing temperature [43] and then decreases with further composites is much lower than that of bulk cobalt ferrite.
increase in annealing temperature, which may be due to: (i) grain
boundaries interaction and interfaces, as the length of interactions
can span many grains and is critically dependent on the character of Acknowledgement
interface and (ii) strain produced in cobalt ferrite crystallite
because of the difference in thermal coefcient of CoFe2O4 and We would like to thank the DST (FIST), New Delhi for nancial
SiO2 [44]. Interestingly, it is observed that the values of Ms, Mr and assistance and we also thank to Mr. Vivek Kumar Malik of the
Hc increase with decrease in measuring temperature because the Department of Physics, University of Fribourg, Switzerland for
magnetization direction of nanoparticles is frozen to the direction providing VSM facilities.
of applied eld and the anisotropy barrier prevents the magnetiza-
tion direction of each nanoparticle from ipping, which is in
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