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Journal of Magnetism and Magnetic Materials 321 (2009) 3093–3098

Contents lists available at ScienceDirect

Journal of Magnetism and Magnetic Materials

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

Studies of magnetite nanoparticles synthesized by thermal decomposition of

iron (III) acetylacetonate in tri(ethylene glycol)
Dipak Maity a,, S.N. Kale b, Ruchika Kaul-Ghanekar c, Jun-Min Xue a, Jun Ding a
a
Department of Materials Science and Engineering, National University of Singapore, Singapore 117574, Singapore
b
Department of Electronic-Science, Fergusson College, Pune 411004, India
c
Interactive Research School for Health Affairs, Bharati Vidyapeeth University, Pune 411008, India

a r t i c l e in fo abstract

Article history: In this paper, water-soluble magnetite nanoparticles have been directly synthesized by thermal
Received 10 February 2009 decomposition of iron (III) acetylacetonate, Fe(acac)3 in tri(ethyleneglycol). Size and morphology of the
Received in revised form nanoparticles are determined by transmission electron microscopy (TEM) and dynamic light scattering
6 April 2009
(DLS) measurements while the crystal structure is identified using X-ray diffraction (XRD). Surface
Available online 18 May 2009
charge and surface coating of the nanoparticles are recognized using Fourier transform infrared
PACS: spectroscopy (FTIR), X-ray photoelectron spectra (XPS) and zeta potential measurements. Magnetic
75.75.+a properties are determined using vibrating sample magnetometer (VSM) and superconducting quantum
81.07.b interference device (SQUID) measurements. The results show that as-prepared magnetite nanoparticles
81.16.c
are relatively monodisperse, single crystalline and superparamagnetic in nature with the blocking
87.85.Qr
temperature at around 100 K. The magnetite nanoparticles are found to be highly soluble in water due to
87.85.Rs
steric and electrostatic interactions between the particles arising by the surface adsorbed
Keywords: tri(ethyleneglycol) molecules and associated positive charges, respectively. Cytotoxicity studies on
Nanoparticle human cervical (SiHa), mouse melanoma (B16F10) and mouse primary fibroblast cells demonstrate that
Magnetite up to a dose of 80 mg/ml, the magnetic nanoparticles are nontoxic to the cells. Specific absorption rate
Thermal decomposition (SAR) value has been calculated to be 885 and 539 W/gm for samples with the iron concentration of 1
Superparamagnetic and 0.5 mg/ml, respectively. The high SAR value upon exposure to 20 MHz radiofrequency signifies the
Hyperthermia applicability of as-prepared magnetite nanoparticles for a feasible magnetic hyperthermia treatment.
& 2009 Elsevier B.V. All rights reserved.

1. Introduction synthesize water-soluble magnetic nanoparticles [10,11]. Recently,

Superparamagnetic (SPM) iron oxide (particularly Fe2O3 and
Fe3O4) nanoparticles have been attracted a great attention in the
bio-medical field such as magnetic separation, drug delivery,
cancer hyperthermia and magnetic resonance imaging (MRI)
contrast enhancement [1–6]. The single-step synthesis of highly
water-soluble, superparamagnetic and biocompatible magnetite
nanoparticles with controlled size and distribution is extremely
important to realize the full potential of these materials in
biomedicine. To date, the thermal decomposition method is very
promising technique to fabricate high-quality superparamagnetic
and monodisperse magnetite nanoparticles [7–9]. Typically, this
method involves decomposition of Fe(acac)3 in a high-boiling
temperature solvent in presence of stabilizing surfactants such as
oleic acid and oleylamine. However, the obtained magnetite
nanoparticles are organic soluble which makes them inappropri-
ate for bio-medical applications. Therefore, many groups have
further developed the thermal decomposition method to directly
 Corresponding author. Tel.: +65 6516 7779; fax: +65 6874 2081.
E-mail address: dmaity@nus.edu.sg (D. Maity).
Cai et al. [12] have synthesized water-soluble magnetite nano-
particles by high-temperature decomposition of Fe(acac)3 in
triethylene glycol (TREG). An obvious advantage of this approach
is that no further reducing agent and surfactants are required,
which made this process easy to scale-up for mass. The TREG has
been used for a triple role as high-boiling solvent, reducing agent
and stabilizer to efficiently control the particle growth and
prevent interparticle aggregation. Here, we have extended this
work and proposed a mechanism for solubility of the as-prepared
magnetite nanoparticles in aqueous suspension by exploring
surface charge and surface coating of the nanoparticles. Cytotoxi-
city and hyperthermia studies of the nanoparticles have also been
performed to evaluate their potentiality in biomedicine.
2. Experimental section
Absolute ethanol and ethyl acetate were used without
purification. Tri(ethylene glycol) (TREG, 99%) and Iron(III) acet-
ylacetonate (Fe(acac)3, 97%) were purchased from Sigma-Aldrich.
Water-soluble Fe3O4 nanoparticles were prepared by the thermal
decomposition of Fe(acac)3 in TREG at elevated temperature with out

0304-8853/$ - see front matter & 2009 Elsevier B.V. All rights reserved.
doi:10.1016/j.jmmm.2009.05.020
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using any surfactants [12]. Typically, 2 mmol of Fe(acac)3 was 3. Results and discussions
dissolved in a 20 ml of hydrophilic TREG media and then magnetically
stirred under a flow of argon. The solution was dehydrated at 120 1C 3.1. Crystal structure
for 1 h, and then quickly heated to 280 1C and kept at this temperature
for 2 h. The black solution was cooled to room temperature by Fig. 1 shows the XRD patterns which match well with the
removing the heat source. The nanoparticles were precipitated by standard XRD patterns for bulk magnetite (JCPDS File no. 19-0629)
addition of 20 ml of ethyl acetate and then isolated by centrifugation. indicating that the particles are consisting of Fe3O4 phase. The
The obtained precipitate was re-dispersed in ethanol and further average crystallite size is measured using Scherrer’s equation [15]
precipitated by ethyl acetate, followed by centrifugation. This washing as 10.7 nm.
procedure was repeated many times and then, one-half of the washed
particles were dispersed in water to get a stable aqueous ferrofluid
suspension and the other half was dried overnight in oven to obtain 3.2. Size and morphology
dry particles.
Size and morphology of the nanoparticles were deter- The TEM image in Fig. 2 indicates that the magnetite
mined using transmission electron microscopy (TEM, JEOL 2010) nanoparticles are well dispersed in water. The average size of
and dynamic light scattering (DLS) (Zetasizer Nano-ZS, Malvern the particle is about 11 nm which is very close to the crystallite
Instruments) while crystal structure was identified by X-ray size obtained from XRD. Inset of Fig. 7 is showing the HRTEM
diffraction (XRD, Bruker D8 Advance). Surface charge and surface image of a single Fe3O4 nanocrystal.
coating of the nanoparticles were recognized by Fourier transform
infrared spectroscopy (FTIR, Varian 3100), X-ray photoelectron
spectra (XPS, Kratos AXIS Ultra DLD) and laser Doppler anemo-
metry (Zetasizer Nano-ZS, Malvern Instruments). Magnetic prop-
erties of the nanoparticles were studied by the supercon-
ducting quantum interference device (SQUID, Quantum Design,
MPMS XL) and vibrating sample magnetometer (VSM, Lakeshore,
Model 665).
Cell viability studies were performed by MTT assay on SiHa
(human cervical), B16F10 (mouse melanoma) cell lines as well as
on mouse primary fibroblasts cells that were isolated from skin
epithelium of Swiss albino mice. The cells were seeded at density
of 1 105 cells/ml in 96-well plates. The cells were grown in
Dulbecco’s modified Eagle’s medium (DMEM) supplemented with
10% fetal bovine serum, 2 mM L-glutamine, 100 m/ml of penicillin/
streptomycin followed by incubation at 37 1C in 5% CO2 overnight.
Next day, cells were treated with fresh medium containing
the magnetite nanoparticles at concentrations ranging from
2.5–160 mg Fe/ml in each well in triplicates and the plates were
further incubated for 24 h. After 48 h, medium was removed and Fig. 1. XRD patterns of the magnetite nanoparticles.
5 mg/ml MTT solution was added and the cells were incubated
for 4 h at 37 1C in 5% CO2 incubator. The intensity of colored
formazan derivative was determined by measuring the absor-
bance at 570 nm in ELISA microplate reader (BioRad, Hercules,
CA). The mean optical density (OD) value of three wells (for
each concentration of nanoparticles dosed to the cells) was used
for assessing the cell viability that was expressed as per-
centage of control [% cell viability ¼ nanoparticle-treated cells/
control cells  100].
Heating ability of the as-prepared nanoparticles was meas-
ured from the time-dependent calorimetric measurements.
Four milliliters of the aqueous ferrofluid with the Fe con-
centration of 0.5–1 mg/ml are subjected to radiofrequency (RF)
radiation (generator: 20 MHz, 100 W, capacitatively coupled
into a small 5 ml glass bottle) for different times, and the
temperature rise was monitored. The temperature increase
was compared to that for pure deionized water. The specific
absorption rate (SAR) was calculated using the following
equation:

DT 1
SAR ¼ C (1)
Dt mFe

where C is the specific heat of solvent (here Cwater ¼ 4.18 J/g 1C),
DT/Dt is the initial slope of the time-dependent temperature curve
and mFe is weight fraction of magnetic element (i.e. Fe) in the Fig. 2. TEM image of the magnetite nanoparticles in an aqueous suspension. Inset
sample [13,14]. is the HRTEM image of individual magnetite nanocrystals.
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Fig. 3 is showing DLS size distribution plot of the magnetite
nanoparticles in an aqueous suspension. The DLS measurement
indicates that the nanoparticles are relatively monodisperse in
aqueous media. The obtained average hydrodynamic size of
the nanoparticles is about 13 nm which is slightly larger than
the size measured by TEM (11 nm). This difference is due to the
coordination of TREG molecules, which effectively increase the
particle size.
3.3. Surface charge and surface coating
Fig. 4 shows flow of the aqueous suspension of as-prepared
Fe3O4 nanoparticles when exposed to a very strong permanent
magnet. This indicates that the particles are highly soluble in
water to form a stable ferrofluid suspension. FTIR, XPS and zeta
potential measurements are carried out to identify the surface
charge and surface coating which are responsible for the water
solubility of the Fe3O4 nanoparticles.
Fig. 5 depicts the FTIR spectra for the particles. The peaks at
about 2962–2809, 1632, 1455, 1350, 1251 and 1063 cm1 are due
to C–H stretching, O–H stretching, C–H bending, C–O bending and
O–H bending vibration, respectively, attributed for adsorbed TREG
molecules to the particle surface [16,17]. The broad band between
3600 and 3000 cm–1 centered at about 3400 cm–1 are due to the
Fig. 3. DLS size distribution plot of the magnetite nanoparticles in an aqueous
suspension.
Fig. 4. Stable aqueous magnetite suspension (ferrofluid) exposed to a strong
permanent magnet.
3095
Fig. 5. FTIR spectra of the magnetite nanoparticles.
O–H stretching vibration attributed for water and TREG molecules
adsorbed to the particle surface [11]. In addition, the strong
absorption band at about 580 cm–1 is due to Fe–O stretching
vibration for the Fe3O4 nanoparticles [18].
Fig. 6(a) shows wide scan XPS spectra while Fig. 6(b) and (c)
are the deconvoluted O(1 s) and C(1 s) spectra of the Fe3O4
nanoparticles, respectively. The O(1 s) peaks at 531.6 and 533.3 eV
are due to O–H and C–O bond which arise from the adsorbed
water and TREG molecules, respectively [19,20]. The C(1 s) peaks
at 285.5 and 288 eV are due to C–C/C–H and C–O–C bond,
respectively, arise from the chemically adsorbed TREG molecules
to the particle surface [21,22]. In addition, the Fe(3p3/2), O(1 s),
Fe(2p3/2) and Fe(2p1/2) peaks of Fig. 6(a) at about 55, 530.3, 710
and 724 eV are due to Fe–O bond of the Fe3O4 nanoparticles [18].
Fig. 7 shows the zeta potential distribution plot of the
magnetite nanoparticles. The maximum of the plot is at about
+40 mV which indicates that surface of nanoparticles is positively
charged. The TREG molecules polarizes into R–O and H+ ions at
elevated reaction temperature (ROH3RO+H+, where
R(CH2–CH2–O)3–H)). The R–O part of TREG molecules
coordinates with Fe2+/Fe3+ of the Fe3O4 nanoparticle (which is
confirmed by FTIR and XPS) while the H+ ions associates with the
particles along with the R–O and as a consequence surface of the
nanoparticles become positively charged. Thus, the adsorbed
R–O and the associated H+ ions cause the steric and electrostatic
interactions between the nanoparticles (as shown in Fig. 8) and
this could be the reason of higher water solubility of the as-
prepared Fe3O4 nanoparticles.
3.4. Magnetic properties
Fig. 9 shows the hysteretic M–H curve of the magnetite
nanoparticles at room temperature. The saturation magnetization
(MS) of the magnetite nanoparticles are found to be 65 emu/g
which is smaller than that of bulk magnetite (92 emu/g). The
decrease in MS compared to bulk magnetite could be due to the
surface effect of the smaller size (11 nm by TEM) magnetite
nanoparticles [23–27] and the presence of nonmagnetic TREG
molecules adsorbed to the surface of the nanoparticles [16]. Zero
coercivity and zero remanance on the magnetization curves
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Fig. 6. XPS spectra of the magnetite nanoparticles: (a) wide scan, (b) O(1 s) and (c) C(1 s) spectra.

Fig. 7. Zeta potential distribution plot of the magnetite nanoparticles in an

aqueous suspension.
Fig. 9. M–H curves of the magnetite nanoparticles.

Fig. 8. Steric and electrostatic interactions between the magnetite nanoparticles in

an aqueous suspension.

indicates superparamagnetic behavior of the magnetite nano-

particles [26,28].
Fig. 10 shows the temperature dependence of the zero-field-
cooled/field-cooled (ZFC–FC) magnetization of the magnetite
nanoparticles measured by SQUID under an applied field of Fig. 10. ZFC and FC magnetization curves of magnetite nanoparticles under an
100 Oe. The feature of the ZFC–FC curves is indicating that the applied field of 100 Oe.
nanoparticles are of superparamagnetic in nature [29]. The ZFC
curve reached the maximum at about 100 K, which corresponded
to the blocking temperature (TB) of the sample. Above TB the 3.5. Cytotoxicity studies
sample is superparamagnetic and below is ferromagnetic. Thus,
the as-prepared magnetic nanoparticles are SPM in nature with The cytotoxicity results on the cell lines SiHa, B16F10 and
the blocking temperature at around 100 K. mouse primary fibroblast cells have been shown in Fig. 11 that are
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Fig. 11. Cytotoxicity profile of the magnetite nanoparticles on SiHa (human
cervical), B16F10 (mouse melanoma) and mouse primary fibroblasts cells.
compared with control cells, which is not treated with the
magnetite nanoparticles. The observation revealed that cells do
not show any cytotoxicity with the magnetite nanoparticles in the
range 2.5–80 mg/ml dose. However, at 160 mg/ml concentration,
the cell viability is decreased slightly for B16F10 cell lines (80%
viability as compared to control), which could be due to mild
cytotoxic effect at higher concentrations in this cell line. But, other
two cell lines do not show any cytotoxicity even at 160 mg/ml
concentration. Thus, it is evident from the cytotoxicity study that
the as-prepared magnetite nanoparticles are biocompatible up to
the iron concentration of 80 mg/ml with SiHa, B16F10 and mouse
primary fibroblast cells.
3.6. Hyperthermia studies
We now show that the magnetite nanoparticles can also
absorb radiofrequency radiation causing heat generation, a
property of great interest to hyperthermia applications. We also
briefly discuss the possible mechanism of heat generation. It may
be noted that generally speaking RF radiation in the frequency
range 100–500 kHz is used for hyperthermia. Here we used
20 MHz because the corresponding generator is available to us,
just to demonstrate the electromagnetic radiation absorption
property of our nanoparticles. Given the fact that there are no
resonances in absorption for this material over the range
100 kHz–30 MHz, we expect similar (but quantitatively somewhat
different) heating effects at lower frequencies as well. It is useful
to mention here that in one of our previous papers on a different
material system, we have addressed the safety concern related to
the radiofrequency at 20 MHz, and have shown based on
experiments in different body tissues and blood that use of this
(20 MHz) high radiofrequency is also safe [30].
Fig. 12 shows a significant temperature rise for sample loaded
with the magnetite nanoparticles as compared to that of pure
deionized water. A systematic increase in the heat generation with
increase in the quantity of the dispersed nanoparticles is observed
for RF irradiation as a function of time. This confirms the potential
applicability of the as-synthesized Fe3O4 nanoparticles for
magnetic hyperthermia application. Fine control on the final
achievable temperature with a judicious combination of
concentration of the nanoparticles and the time of RF irradiation
is definitely possible, which is underway. The heating effects in
magnetic nanoparticles in alternating fields are due to several
types of loss mechanisms such as hysteresis loss, Neel loss and
3097
Fig. 12. Time-dependent temperature rise of 4 ml sample with different iron
concentration on exposure to RF radiation with 20 MHz frequency and 100 W
power. The inset shows the RF response of water (without nanoparticles)
indicating that there is no increase in temperature with radiofrequency exposure.
Brownian loss, all being strongly dependent upon the particle size.
For SPM particles above the blocking temperature, the process of
hysteresis loss is ruled out. However the other two mechanisms,
Brownian loss due to the magnetically driven physical rotation of
the particle and Neel loss due to the rotation of magnetization
vector can still contribute. In addition to the nanoparticle size, the
anisotropy energy of the magnetic material and the viscosity of
the dispersion medium control the relaxation times of the Neel
and Brownian mechanisms, respectively, and thereby their
relative dominance in the heating phenomenon.
SAR value has been calculated to be 885 and 539 W/gm of Fe
for the sample with iron concentration of 1 and 0.5 mg/ml,
respectively, which indicating a higher SAR value as compared to
the reported values in the literature [31,32]. Clearly, the use of
much higher RF power in our case generates the high SAR value,
suggesting that as-prepared magnetite nanoparticles are useful
for a feasible hyperthermia treatment.
4. Conclusions
As-prepared magnetite nanoparticles are relatively monodis-
perse, single crystalline and superparamagnetic in nature. The
nanoparticles are highly soluble in water because of the steric and
electrostatic interactions between the particles arise from the
surface adsorbed tri(ethyleneglycol) molecules and the associated
positive charges, respectively. Cytotoxicity studies show that as-
prepared magnetite nanoparticles are biocompatible up to the
iron concentration of 80 mg/ml. The significant temperature rise of
the magnetite nanoparticles upon exposure to 20 MHz radio-
frequency confirms their potential applicability for magnetic
hyperthermia application.
Acknowledgments
The authors gratefully acknowledge the help of Dr. S.D. Dhole,
Department of Physics, University of Pune, for the hyperthermia
heating measurement.
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