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Microwave Assisted Iron Oxide Nanoparticles—Structural and Magnetic

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Article  in  IEEE Transactions on Magnetics · August 2014

DOI: 10.1109/TMAG.2014.2313117

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IEEE TRANSACTIONS ON MAGNETICS, VOL. 50, NO. 8, AUGUST 2014 2201504

Microwave Assisted Iron Oxide Nanoparticles—Structural

and Magnetic Properties
Saira Riaz, Robina Ashraf, Aseya Akbar, and Shahzad Naseem
Centre of Excellence in Solid State Physics, University of the Punjab, Lahore 54590, Pakistan

Microwave energy is used as an alternative source of high temperature treatment for synthesis and sintering. Till 1990s, the
main focus was on the thermal effects caused by microwave heating. After 1990s reports began to emerge on the effects called
microwave effects, including changes in material’s structure and so on. We here report the effects of microwave assisted sol-gel
method on structural and magnetic properties of iron oxide nanoparticles (NPs). Microwave power (MP) is varied as 136, 264, 440,
616, and 800 W. The MPs used in this paper are among the lowest for the synthesis of NPs. X-ray diffractometer result of NPs
with 136-W MP shows amorphous behavior with paramagnetic properties. Magnetite NPs are observed with MPs of 264–440 W.
Magnetite phase tends to transform to maghemite phase with the appearance of characteristic (310) peak at MPs of 616–800 W.
Scanning electron microscope results show NPs with diameter ∼20 nm for MPs of 264 and 440 W. Relatively larger diameters
∼50 nm are observed with MPs of 616 and 800 W. Variations in phase and size of iron oxide NPs strongly affect magnetic properties
from superparamagnetic to ferromagnetic. It is observed that microwave assisted synthesis can be fast, low cost, and low energy
consumption method to synthesize NPs with uniform shape and size distribution along with strengthened magnetic properties as
compared with the conventional high-temperature annealing process.
Index Terms— Maghemite, magnetite, microwaves, nanoparticles (NPs).

I. I NTRODUCTION

U NIFORMLY distributed nanoparticles (NPs) are ideal

building blocks for functional materials and nanodevices.
The NPs exhibit shape- and size-dependent magnetic, elec-
tronic, structural, and catalytic properties [1]–[3]. Among the
various magnetic materials, magnetite (Fe3 O4 ) and maghemite
(γ -Fe2 O3 ) are the most promising due to their wide use
in biomedical applications, including magnetic hyperther-
mia, cancer treatment, targeted drug delivery, and magnetic
resonance imaging [4]–[7].
Magnetite (Fe3 O4 or FeO.Fe2 O3 ) crystallizes in inverse
spinel cubic structure in which oxygen ions are set in cubic
close packed arrangement and Fe(II) cations take up the
octahedral sites, whereas Fe(III) cations have an arbitrary
distribution on tetrahedral and octahedral sites [8]. Magnetite
Fe3 O4 or ferrous ferrite exhibits the strongest magnetism as
compared with the entire range of transition metal oxides [9].
Magnetic moment of 4 μB in Fe3 O4 is mainly because of
the occupancy of octahedral sites with Fe2+ ions. It exhibits
a ferrimagnetic behavior, at room temperature, with a Curie
temperature of 850 K [8]–[11].
There are several reports on iron oxide synthesis using
microwaves, especially using hydrothermal method, but very
less attention is given to the use of microwaves in sol-gel
synthesis. In addition, these studies are mostly focused on
maghemite NPs, and synthesis of magnetite NPs are based on
addition of surfactants and/or stabilizers. In addition, very little
consideration is given to study the effect of varying microwave
powers (MPs) on materials’ properties [12]–[15].
In this paper, iron oxide NPs are synthesized without the
use of any surfactant with variation in MPs, i.e., 136, 264,
440, 616, and 800 W, at a fixed frequency of 2.45 GHz.
Manuscript received December 17, 2013; revised March 5, 2014; accepted
March 11, 2014. Date of current version August 15, 2014. Corresponding
author: S. Riaz (e-mail: saira_cssp@yahoo.com).
Color versions of one or more of the figures in this paper are available
online at http://ieeexplore.ieee.org.
Digital Object Identifier 10.1109/TMAG.2014.2313117
0018-9464 © 2014 IEEE. Personal use is permitted, but republication/redistribution requires IEEE permission.
See http://www.ieee.org/publications_standards/publications/rights/index.html for more information.
Fig. 1. Iron oxide NPs. Presenting a good magnetic response synthesized
with MP of (a) 264, (b) 440, (c) 616, and (d) 800 W.
Structural and magnetic properties are correlated with the
variation in MPs.
II. E XPERIMENTAL D ETAILS
Iron nitrate Fe(NO3 )3 .9H2 O, Sigma Aldrich (99.99%), was
dissolved in DI water and stirred at room temperature.
Ethylene glycol was added to the above solution and stirring
continued at room temperature. Solution was subjected to
microwave radiations with variation in power (136, 264, 440,
616, and 800 W) at a fixed frequency of 2.45 GHz. Fig. 1
shows that these nonoparticles exhibited excellent magnetic
properties and can easily be attracted by the magnet. Iron
oxide NPs were synthesized using microwave assisted sol-gel
method without the use of any surfactant or stabilizer.
These NPs were characterized using Bruker D8 Advance
X-ray diffractometer (XRD) with Ni filtered CuKα (1.5406 Å)
radiations. Lakeshore’s 7407 vibrating sample magnetometer
was used to study the magnetic properties. Hitachi S-3400N
scanning electron microscope (SEM) was used to study the
shape and sizes of NPs.
III. R ESULTS AND D ISCUSSION
Fig. 2 shows XRD patterns for iron oxide NPs prepared
using microwave assisted sol-gel method. The NPs synthesized
using MP of 136 W showed amorphous behavior. Indica-
tion of diffraction peaks, corresponding to magnetite phase,
were obtained by increasing the MP to 264 W (JCPDS card
no. 88-0315). Crystallinity of the nanoparticles increased with
the further increase in MPs power to 440 W [Fig. 2(b)]. (220),
(311), and (422) planes appeared at 30.2°, 35.5°, and 53.6°
2201504
Fig. 2. Iron oxide NPs synthesized with variation in microwaves power
(136–800 W) (arrows in figure indicate diffraction peaks, which are present
in maghemite phase only).
correspond to magnetite phase. However, with further increase
in the MP to 616 and 800 W, oxidation of magnetite phase
occured thus converting magnetite to maghemite phase with
the appearance of (310), (311), and (421) characteristic peaks
(JCPDS card no. 39-1346). Main difference in magnetite and
maghemite is only the presence of vacancies on the cationic
sublattice in the case of maghemite [9] so it can be predicted
that at high irradiation power of microwaves, the vacancies are
created on the octahedral site thus leading to transformation
of magnetite to maghemite. Strengthening in maghemite phase
was observed with further increase in MP to 800 W.
Magnetite is extremely difficult to be distinguished from
maghemite phase on the basis of XRD patterns because they
have same crystal structure. However, according to standard
JCPDS cards 39-1346 (magnetite) and 88-0315 (maghemite)
along with the previously published reports [13] and [16],
some extra diffraction peaks appear in the case of maghemite,
which cannot be found in magnetite. Such differentiating
peaks occur in angular range 2θ ° = 20–29°, 31–34°, 44–46°,
48–52°.
IEEE TRANSACTIONS ON MAGNETICS, VOL. 50, NO. 8, AUGUST 2014
TABLE I
E FFECT OF MP ON C RYSTALLITE S IZE AND L ATTICE PARAMETERS
Fig. 3. FTIR spectra for iron oxide NPs.
Appearance of (310) and (421) diffraction peaks [indicated
by arrows in Fig. 2(c)] are indicative of maghemite phase with
MPs of 616 and 800 W. These extra diffraction peaks were
absent in NPs synthesized using MPs of 440 W.
Crystallite size (t) and lattice parameter (a), calculated
using (1) and (2) [17], are listed in Table I
0.9λ
t = (1)
B cos θ
λ2  2 
sin2 θ = 2
h + k2 + l2 (2)
4a
where λ is the wavelength, B is full-width at half-maximum,
and (hkl) are miller indexes.
Crystallite size increases with increase in MP to 800 W.
In general, in wet chemical synthesis methods including
sol-gel, crystallite size strongly depends on the nucleation and
growth stages [18]. Large number of seeds are available as a
result of fast nucleation reaction thus leading to decrease in
number of monomers that are available for particle growth
with reduced crystallite size [18]. Contrary to this, slow
nucleation results in large crystallite size because of the
availability of large number of monomers. Therefore, control
of nucleation speed is extremely crucial in order to avoid
crystallite growth by Ostwald ripening mechanism [18].
In microwave assisted synthesis of NPs, amount of power
dissipated in the sol controls the temperature of reaction.
Power dissipation is given as P = σ (E)2 , where σ is the
conductivity and E is the electric field of the microwaves
used [18]. Above expression shows that reaction tempera-
ture depends on the power of microwaves used. Microwaves
generate dielectric heating, which raises the temperature of
the sol/solvent. In dielectric heating mechanism, energy is
transferred selectively to microwave absorbing material as a
result of which intrinsic temperature around the ion is much
higher as compared with that in conventional heating method
[18]–[20]. Such localized heating of ions controls the nucle-
ation rate and stops Ostwald ripening mechanism [18].
Therefore, MPs control the localized heating rate of ions
and lead to the increased crystallite size as a result of
increased MPs.
RIAZ et al.: MICROWAVE ASSISTED IRON OXIDE NPS
Fig. 4. SEM images of iron oxide NPs prepared with microwaves power
(a) 136, (b) 264, (c) 440, (d) 616, and (e) 800 W.
Lattice parameter of NPs prepared using MP of 440 W
is in close agreement with the standard value of 8.375 Å
(JCPDS card 88-0315). Whereas with increase in MP to 616
and 800 W, the lattice parameter changed to 8.35 and 8.40 Å,
respectively. These values are in good agreement with lattice
parameter of maghemite phase (JCPDS card no. 39-1346).
Bourgeois et al. [21] differentiated between magnetite and
maghemite phases on the basis of difference in lattice
parameters.
Fig. 3 shows FTIR spectra of iron oxide NPs. Appearance
of bands at 474 and 525 cm−1 are attributed to metal oxygen
bonds. These bands correspond to Fe3 O4 indicating stretching
of octahedral and tetrahedral sites in inverse spinel cubic struc-
ture thus indicative of the formation of magnetite phase at MPs
of 264 and 440 W. With the increase in MP to 616 and 800 W,
the infrared peaks shift to slightly higher wave numbers.
This blue shift is attributed to the phase transition from
magnetite to maghemite phase [16], [22]. In addition, NPs
synthesized with MP of 264 and 440 W did not show any IR
bands in the range of 600–700 cm−1 , whereas with increase
in MP to 616 and 800-W small bands in the wavenumber
range of 600–700 cm−1 appear indicating transition from
magnetite to maghemite phase [16], [22]. The infrared band
at 1086 cm−1 is attributed to O–H stretching and/or due to
C–O–C bending vibrations. The bands at 1382 and 1643 cm−1
arise due to symmetric and asymmetric mode of COO−
group [23]. However, reduction in these bands observed with
increased MPs is due to evaporation of residual solvents.
Fig. 4 shows SEM images of iron oxide NPs prepared
using microwaves with powers of 136, 264, 440, 616, and
800 W. The agglomeration of NPs can be seen [Fig. 4(a)]
with MP of 136 W. The NPs, with uniform size and shape
distribution, were observed with the increase in MP to 400 W
(∼20 nm)–616 W (∼30 nm) [Fig. 4(b)–(d)]. However,
agglomerated NPs were again observed by increasing MP to
800 W.
As has been mentioned earlier, the basic principle of
microwave heating involves the agitation of polar ions or mole-
cules because of their random motion [18], [19]. Frequency
of random motion increases with the increase in MP thus
producing sufficient heat required for the coalescence of small
crystallites [18] [Fig. 4(e)].
Al-Gaashani et al. [23] reported that microwaves lead to
localized heating, which generate different regions in the sol.
Such regions, known as hot spots, result in superheating of
the sol that is higher than that estimated with the use of
conventional heating. Thus, reaction temperature inside the sol
increases very fast as compared with the conventional heating
2201504
Fig. 5. Iron oxide NPs synthesized with variation in microwave power
(a) 136–800 W. (b) Ms and μB as a function of MP.
as given by (3). Decrease in viscosity with the increase in
temperature, as given by (4), [23] increases collision of the
particles thus leading to enhanced tendency of iron oxide
nuclei to aggregate. This results in decreased nucleation rate
and increased growth rate thus leading to larger grain size at
high MP as shown in Fig. 4(e)
T Pabs 2πεo εeff
" E2
2πεo εr" tan δ E rms
2
rms
= = = (3)
t ρC p ρC p ρC p
4πηr 3
τ = (4)
kT
where T is the rise in temperature, ρ is the density, t is time,
C p is the specific heat capacity, Pabs is the microwave energy
absorbed per unit volume, εo is the dielectric permittivity of
 is the dielectric loss factor, ε  is the relative
free space, εeff
r
dielectric constant, tan δ is the tangent loss, E rms is the root
mean square of internal electric field, η is the viscosity, τ is
the relaxation time, r is the radius of rotating dipole, and k is
the Boltzmann constant [22].
Fig. 5(a) shows room temperature M–H curves for iron
oxide NPs synthesized with variation in MP. Paramagnetic
behavior was observed for NPs synthesized with MP of
136 W. Paramagnetic behavior is indicative of the incomplete
formation or nonformation of iron oxide at low power of
microwaves. Superparamagnetic behavior, with high saturation
magnetization, was observed with MP of 264 W. High satura-
tion magnetization comparable with that of bulk magnetite [9]
at MP of 264 W is strong indication of the formation of
magnetite phase. Ferromagnetic behavior with very small
value of coercivity and decreased saturation magnetization was
observed for MP of 440 W. Decreasing trend in magnetization
values continued for MPs of 616–800 W. Decrease in satura-
tion magnetization is indicative of the conversion of magnetite
to maghemite phase [9], which is consistent with the changes
observed in the XRD patterns [Fig. 2]. It is worth mentioning
here that these superparamagnetic NPs are obtained at the
lowest ever reported MP without the use of any surfactant.
Jiang et al. [13] prepared iron oxide NPs using microwave
assisted solvothermal method with a power of 400 W.
Manikandan et al. [14] prepared magnetite NPs by microwave
combustion method using a power of 850 W. Pascu et al. [15]
obtained magnetite NPs with MP of 300 W but with the use of
oleic acid and trimethyl ammonium hydroxide as the surfac-
tant. Hu et al. [24] prepared iron oxide NPs with MP of 1 kW.
Magnetic moments in Bohr magneton [9], [25], [26] are
calculated using
Ms × Mol.Wt.
nB = (5)
5585ds
Ms = (1 − P)σs ds (6)
2201504
where n B is the Bohr magneton, Ms is the saturation magne-
tization in emu/cm3, Mol.Wt. is the molecular weight, ds is
the density of specimen, P is porosity, and σs is the saturation
magnetization in emu/g.
Fig. 5(b) shows saturation magnetization and effective
number of Bohr magnetons per formula unit plotted as a
function of MP. Fe3 O4 contains Fe2+ cations present on
the octahedral site, whereas there is an arbitrary distribu-
tion of Fe3+ cations on the octahedral sites. According to
Hund’s rule, the two electrons are paired and rest of the four
electrons remain unpaired thus giving total number of Bohr
magneton value of 4 μ B due to antiparallel arrangement of
cations on the octahedral and tetrahedral sites [9]. On the
other hand, due to presence of vacancies on the cationic
sublattice in case of γ -Fe2 O3 , the effective number of Bohr
magnetons per formula unit (μB /f.u.) reduces to 2.4 μB /f.u.
High saturation magnetization (Ms ) and high value of Bohr
magnetons per formula unit for the NPs synthesized using
MPs of 264 and 440 W are indicative of the formation of
magnetite phase. Increasing the MP to 616 W reduces the
value of Bohr magneton per formula unit to 2.4 μB that is
close to the one reported for bulk maghemite phase [9] thus
indicating the transition from magnetite to maghemite phase
as shown in Fig. 2. Thus, decreased value of magnetization
along with the smaller value of Bohr magneton for 616 and
800 W is indicative of maghemite phase.
IV. C ONCLUSIONS
Iron oxide NPs have been synthesized using microwave
assisted sol-gel method with variation in MP of 136, 264,
440, 616, and 800 W. XRD patterns showed amorphous
behavior for NPs synthesized with MP of 136 W. Increase in
crystallinity with the increased crystallite size was observed
for MPs of 264–800 W. Indication of phase conversion from
magnetite to maghemite was observed with increase in MP
to 616–800 W. Increased Ms (94.38 emu/g) with increased
Bohr magnetons per formula unit (4 μB ) showed formation of
magnetite at MPs of 264–440 W. Whereas decreased value of
Ms (44.45 emu/g) with reduced Bohr magnetons per formula
unit (2.4 μB ) was indicative of maghemite phase at MPs of
616–880 W. The NPs with uniform size (20–30 nm) and shape
distribution were observed for MPs of 264–661 W.
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