Journal of Nanoparticle Research (2007) 9:419–426 Ó Springer 2006

DOI 10.1007/s11051-005-9051-8
Research Paper

Microwave-assisted synthesis and magnetic property of magnetite and hematite

nanoparticles

Wei-Wei Wang1,3, Ying-Jie Zhu1,* and Mei-Ling Ruan2

1
State Key Laboratory of High Performance Ceramics and Superfine Microstructure, Shanghai Institute of
Ceramics, Chinese Academy of Sciences, Shanghai, 200050, P.R. China; 2Analysis & Testing Center for
Inorganic Materials, Shanghai Institute of Ceramics, Chinese Academy of Sciences, Shanghai, 200050, P.R.
China; 3Graduate School of Chinese Academy of Sciences, Beijing, P.R. China; *Author for correspondence
(Tel.: +86-21-52412616; Fax: +86-21-52413122; E-mail: y.j.zhu@mail.sic.ac.cn.)

Received 14 July 2005; accepted in revised form 13 October 2005

Key words: magnetite (Fe3O4), hematite (a-Fe2O3), nanoparticles, microwave heating, synthesis, agglom-
eration

Abstract

Nanoparticles of magnetite (Fe3O4) and hematite (a-Fe2O3) have been prepared by a simple microwave
heating method using FeCl3, polyethylene glycol and N2H4ÆH2O. The amount of N2H4ÆH2O has an effect
on the final phase of Fe3O4. The morphology of a-Fe2O3 was affected by the heating method. Crystalline
a-Fe2O3 agglomerates were formed immediately at room temperature and most of these nanoparticles
within agglomerates show the same orientation along [110] direction. After microwave heating, ellipsoidal
a-Fe2O3 nanoparticles were formed following an oriented attachment mechanism. Both Fe3O4 and a-Fe2O3
nanoparticles exhibit a small hysteresis loop at room temperature.

Introduction gamma-irradiation (Lee & Kang, 2004), sol–gel

Iron oxides including magnetite (Fe3O4) and
hematite (a-Fe2O3) have attracted much interest due
to their interesting properties (Zboril et al., 2002).
For example, a-Fe2O3 is widely utilized as a pig-
ment, as well as a catalyst for oxidation of alcohols
to form aldehydes and ketones. Fe3O4 is used in
information storage (McMichael et al., 1992), in
medical diagnosis (Josephson et al., 1999) and as a
catalyst for various reactions such as ammonia
synthesis (Deshpande et al., 2004). Currently, there
are several methods for synthesis of iron oxide
nanoparticles, for example, pyrolysis (Jana et al.,
2004), coprecipitation (Cheng et al., 2005a),
(Goya et al., 2005) and hydrothermal methods
(Wang et al., 2004; Jing et al., 2005). There are a
few reports about synthesis of a-Fe2O3 by micro-
wave-assisted hydrothermal reactions (Rigneau
et al., 1999; Katsuki & Komarneni, 2001; Caillot
et al., 2002; Katsuki et al., 2004) or by microwave
heating in an open vessel (Li & Wei, 1998; Jia et al.,
2000; Palchik et al., 2000; Liao et al., 2001).
CoFe2O4 nanoparticles have also been prepared by
co-precipitation under microwave heating at
160°C for 60 min (Bensebaa et al., 2004). How-
ever, to the best of our knowledge, there have been
no reports on the synthesis of Fe3O4 nanoparticles
by a simple microwave heating route.
420
Microwave-assisted solution method has become
widely used due to its advantages such as rapid
volumetric heating, higher reaction rate, reducing
reaction time and increasing yield of products
compared with conventional heating methods
(Namboodiri & Varma, 2001). Recently, we have
fast synthesized various nanomaterials with dif-
ferent morphologies using microwave heating
(Wang & Zhu, 2004; Zhu et al., 2004; Jiang & Zhu,
2005; Wang & Zhu, 2005). In this paper, we report
the synthesis of Fe3O4 and a-Fe2O3 nanoparticles
by a fast and simple microwave-assisted solution
method. a-Fe2O3 nanostructures with different
morphologies could be obtained under different
heating methods. The elliptical a-Fe2O3 nanopar-
ticles were formed following the oriented attach-
ment mechanism.
Experimental
Ferric chloride (FeCl3Æ6H2O), polyethylene glycol-
20000 (PEG-20000), hydrazine hydrate (N2H4Æ
H2O) and hydrogen peroxide (H2O2) were pur-
chased and used without further purification.
In the typical synthesis of magnetite, FeCl3Æ
6H2O (76 mg) and PEG-20000 (60 mg) were dis-
solved in distilled water (10 ml). Then hydrazine
(1 ml) was rapidly added into the above solution
at room temperature. The mixture turned to red-
dish brown (the precursor, sample 1). The pre-
cursor suspension was heated by microwave at
100°C for 10 min and black product was obtained
(sample 2).
In the synthesis of hematite (samples 3–6),
FeCl3Æ6H2O (76 mg) and PEG-20000 (60 mg) were
dissolved in distilled water (10 ml). Then hydra-
zine (0.4 ml) and H2O2 (1 ml) were added into the
above solution, respectively. (Caution: the addition
of H2O2 to the solution containing hydrazine was
associated with the release of heat!). Red product
was obtained (the precursor, sample 3). The pre-
cursor suspension was heated by microwave at
100°C for 10 min (sample 4). All products were
separated by centrifugation, washed with distilled
water and absolute ethanol twice, respectively.
Under the same experimental conditions as sample
4 except without using PEG-20000, sample 5 was
obtained. Sample 6 was prepared under the same
experimental conditions as sample 4 but using oil
bath instead of microwave heating.
The microwave oven (2.45 GHz, maximum
power 300 W) used for sample preparation was a
focused single mode microwave synthesis system
(Discover, CEM, USA). The unique, circular sin-
gle-mode cavity ensured the sample was in a highly
dense microwave field. The system was equipped
with a magnetic stirrer and a water-cooled con-
denser. Temperature was controlled by automatic
adjusting of microwave power. X-ray powder dif-
fraction (XRD) patterns were recorded using a
Rigaku D/max 2550 V X-ray diffractometer with
high-intensity Cu Ka radiation (k=1.54178 Å) and
a graphite monochromator. The transmission
electron microscopy (TEM) micrographs, selected-
area electron diffraction (SAED) patterns and
high-resolution transmission electron microscopy
(HRTEM) micrographs were taken with a JEOL
JEM-2100F field emission electron microscope
with an accelerating voltage of 200 kV. A vibrat-
ing sample magnetometer (JDM-13) was used to
evaluate the magnetic properties at room temper-
ature. Fourier transform infrared spectra (FTIR)
between 4000 and 400 cm)1 were carried out on a
Thermo Niocolet Fourier Transform Spectrum,
using a KBr disk method.
Results and discussion
The structure and phase purity of all samples were
investigated by XRD. Figure 1a shows the XRD
pattern of sample 1 prepared at room tempera-
ture. One can see that sample 1 consisted of a
mixture of a-Fe2O3 and a-FeOOH, owing to the
basic property of hydrazine (Patnaik, 2002). No
peaks for Fe3O4 appeared. After microwave
heating at 100°C (sample 2), black product was
synthesized. Figure 1c shows the XRD pattern of
sample 2, indicating it was a single phase of cubic
Fe3O4 (JCPDS file No. 19-629). This shows that
higher reaction temperature was necessary for the
formation of Fe3O4. The amount of hydrazine has
an influence on the phase of the product. When
decreasing the amount of hydrazine from 1 ml
(sample 2) to 0.4 ml, the product remained the
single phase of Fe3O4. However, when 0.2 ml of
hydrazine was used, the product consisted of a
mixture of a-Fe2O3 and Fe3O4 (Figure 1b). In
addition, thermal decomposition of excessive
hydrazine may occur at elevated temperature

Figure 1. XRD patterns of (a) sample 1; (b) the sample
prepared under the same experimental conditions as sample
2 except that the amount of hydrazine was decreased to
0.2 ml; (c) sample 2; (d) sample 3; (e) sample 4. d a-FeOOH;
}a-Fe2O3; * Fe3O4.
according to the following reaction (Patnaik,
2002):
3N2 H4
! 4NH3 þ N2
N2 may protect Fe3O4 from further oxidation by
air. Therefore, the amount of hydrazine played an
important role in the formation of a single phase
of Fe3O4.
Addition of H2O2 immediately resulted in the
formation of well-crystallized a-Fe2O3. The release
of heat by adding H2O2 may favor the formation
of crystalline a-Fe2O3 (sample 3). As shown in
Figure 1d, sample 3 was a single phase of hexag-
onal a-Fe2O3 (JCPDS file No. 33–0664). After
microwave heating, sample 4 remained a single
Figure 2. (a) and (b) TEM micrographs of Fe3O4 nanoparticles (sample 2); (c) HRTEM micrograph of Fe3O4 nanoparticles
(sample 2).
421
phase of a-Fe2O3 with a better crystallinity
(Figure 1e) compared with sample 3.
The morphologies of samples were investigated
with TEM. Figure 2 shows TEM micrographs for
sample 2. One can see Fe3O4 nanoparticles with
sizes less than 20 nm and relatively wide size dis-
tribution. Most of these Fe3O4 nanoparticles have
irregular shapes and a few have the hexagonal shape
with the angles of adjacent edges of 120° as indicated
by an arrow in Figure 2b. It is known that the uni-
formity of the size and shape is controlled by
nucleation (Yin et al., 2004). After hydrazine was
rapidly added at room temperature, the reaction
started. The nucleation and crystal growth contin-
ued during heating, which may result in the wide size
distribution and irregular shape of Fe3O4 nano-
particles. Figure 2c shows the HRTEM micro-
graph of Fe3O4 nanoparticles, which provided
more detailed structural information. It showed
that each Fe3O4 nanoparticle was structurally
single-crystalline. The periodic fringe spacing of
4.80 Å corresponds to the (111) planes of cubic
Fe3O4.
The TEM micrograph of sample 3 (Figure 3a)
shows large agglomerates formed by small
(4–6 nm) nanoparticles. HRTEM micrograph
clearly shows lattice fringes of each of nanoparti-
cles and the interplanar spacing of 2.56 Å agrees
well with the spacing between (110) planes of
a-Fe2O3 (2.52 Å) (Figure 3b). It is very interesting
that the lattice fringes were aligned within
agglomerates and nanoparticles show the same
orientation along [110] direction. After microwave
heating at 100°C, the initial agglomerates were
converted into ellipsoidal nanocrystals (sample 4,
Figure 3c and d). Figure 3d shows a single ellip-
422
Figure 3. (a) TEM micrographs of a-Fe2O3 (sample 3); (b) HRTEM micrograph of a-Fe2O3 (sample 3); (c) and (d) TEM
micrographs of a-Fe2O3 (sample 4); the inset of (d) is the corresponding SAED pattern.
soid-like nanoparticle with a width of 50 nm and
a length of 120 nm and its corresponding SAED
pattern. The SAED pattern can be indexed as the
[1–10] zone axis of a-Fe2O3, indicating single-
crystalline structure. In addition, the growth
direction of the ellipsoidal nanoparticle was along
[110] direction (indicated by an arrow) which was
the same to the aligned orientation of nanoparticles
within agglomerates in sample 3. Other researchers
have also reported the preparation of a-Fe2O3
nanoparticles under microwave heating in the
open vessel (Li & Wei, 1998; Jia et al., 2000; Liao
et al., 2001). For example, amorphous Fe2O3
particles were prepared by microwave heating a
mixture of FeCl3 and urea for 10 min. Crystalline
a-Fe2O3 nanoparticles were obtained after sinter-
ing at 400°C for 2 h (Liao et al., 2001). Similar
ellipsoidal a-Fe2O3 nanoparticles were prepared by
microwave-induced hydrolysis of Fe(NO3)3 for
150 min in the presence of NaH2PO4 (Li & Wei,
1998). However, only spherical a-Fe2O3 nanopar-
ticles were obtained without using NaH2PO4 (Li &
Wei, 1998). In contrast, we have prepared ellip-
soidal a-Fe2O3 nanoparticles at 100°C in a short
period of time (10 min).
Figure 4a and b show TEM micrographs of
sample 5 prepared without using PEG-20000. One
can see ellipsoidal morphology similar to sample 4.
The widths of these ellipsoidal nanocrystals were
up to 100 nm and lengths were about several
hundred nanometers. Compared with sample 4,
more irregular nanoparticles appeared. However,
a mixture of nanoparticles and rods was obtained
using oil bath instead of microwave heating
(sample 6), and no ellipsoidal-like crystals were
observed. The formation of the rods may result

Figure 4. TEM micrographs. (a) and (b) sample 5; (c) and (d) sample 6.
from the PEG assemblage in water (Wang et al.,
2001). Therefore, the heating method plays an
important role in the formation of ellipsoidal
nanocrystals. For microwave heating, the high
polarizability of the solvent makes it an excellent
microwave-absorbing agent, thus leading to a high
heating rate and a significantly shorten reaction
time (Zhu et al., 2004).
In general, when synthesizing nanoparticles from
solution, nucleation was very fast and subsequent
growth occurred by two primary mechanisms:
growth involving oriented attachment (Penn &
Banfield, 1998; Alivisatos, 2000; Adachi, 2004;
Cheng et al., 2005b) and Ostwald ripening (Penn &
Banfield, 1999). With regard to the preparation of
a-Fe2O3, many researchers brought forward dif-
ferent opinions. Schwertmann et al. (1999) pro-
posed the formation of a-Fe2O3 nanocrystals
involved the dissolution of iron oxyhydroxides and
precipitation of a-Fe2O3 nanocrystals, which
resulted in the spherical particles rather than
extended along a specific crystallographic direction.
423
Banfield et al. (2000) reported that iron oxyhy-
droxide particles aggregated in a random manner,
formed parallel orientation through recrystalliza-
tion, and subsequently underwent dehydration to
form a-Fe2O3. However under our experimental
conditions, ellipsoidal a-Fe2O3 nanocrystals were
formed under microwave heating instead of con-
ventional heating. After adding H2O2, a-Fe2O3
nanocrystals were formed immediately and no iron
oxyhydroxide particles were observed. We pro-
posed that the growth of ellipsoidal a-Fe2O3
nanoparticles may follow the oriented attachment
mechanism. The attachment of nanoparticles was
realized by sharing a common crystallographic
orientation (110) and joining at the planar inter-
faces (Ocana et al., 1995; Penn & Banfield, 1998;
Alivisatos, 2000; Adachi et al., 2004; Cheng et al.,
2005b). In addition, Ostwald ripening process
smoothed the morphology of the ellipsoidal-like
crystals after attachment as evidenced by TEM
observation (Schwertmann et al., 1999; Cheng
et al., 2005b).
424

Figure 5. Magnetization curves of (a) sample 2 and (b) sample 4 at room temperature.

Magnetic property of samples 2 and 4 was both samples, which likely contributed to the
measured at room temperature. Both samples lower saturation magnetization of both samples.
exhibit a small hysteresis loop. The saturation
magnetization of Fe3O4 nanoparticles (sample 2)
at room temperature was 62.45 emu/g (Figure 5a), Conclusion
which is smaller than that of bulk Fe3O4 (Shafi
et al., 2002; Mikhaylova et al., 2004) and was Magnetite (Fe3O4) and hematite (a-Fe2O3) nano-
higher than that of Fe3O4 prepared from emul- particles have been prepared by a fast microwave
sions (Zhou et al., 2001). The coercivity is almost heating method. Under our experimental condi-
negligible (Figure 5a). Ellipsoidal a-Fe2O3 nano- tions, hydrazine hydrate acted not only as a
particles (Sample 4) also has the lower saturation reducing reagent but also as an alkali. The
magnetization compared with the spherical amount of hydrazine hydrate affected the final
a-Fe2O3 particles with average diameters 300 nm phase of Fe3O4. Crystalline a-Fe2O3 agglomerates
prepared by aging a solution of FeCl3 and HCl for were formed immediately after adding H2O2 at
14 days at 100°C (Muench et al., 1981). The room temperature. Nanoparticles within agglom-
magnetic behavior of iron oxide nanoparticles is erates showed the same orientation along [110]
very sensitive to the crystallinity and particle sizes direction. The morphology of a-Fe2O3 was
(Lopez-Quintela & Rivas, 1993). The smaller affected by the heating method. Ellipsoidal a-
particle size may result in the decrease of satura- Fe2O3 nanoparticles were prepared by microwave
tion magnetization. Some studies also suggested heating. While a mixture of irregular a-Fe2O3
that the decrease of the saturation magnetization
was likely attributed to the existence of surfactants
on the surface of nanoparticles (Si et al., 2005).
The adsorption of PEG-20000 on samples 2 and 4
was confirmed by FTIR spectra (Figure 6). FTIR
spectra of both samples (Figure 6) revealed the
appearance of some bands among 1050–1150 cm)1
which were assigned to the stretching of ether
groups and the characteristic absorptions of alkyl
(R–CH2) stretching modes (between 2850 and
3000 cm)1) (Mansur et al., 2004; Saravanan &
Subramanian, 2005). Hydroxyl group contribution
was observed with absorption ranging from 3200
to 3600 cm)1 (Mansur et al., 2004; Saravanan &
Subramanian, 2005). FTIR analysis revealed the
presence of PEG on the surface of nanoparticles in Figure 6. FTIR spectra of (a) sample 2 and (b) sample 4.

nanoparticles and rods were prepared by oil bath.
The growth mechanism of ellipsoidal a-Fe2O3
nanoparticles may follow the oriented attachment
mechanism. Both Fe3O4 and a-Fe2O3 nanoparti-
cles exhibit a small hysteresis loop at room tem-
perature due to their nanometer size and the
existence of surfactants on the surface of nano-
particles.
Acknowledgments
Financial support from National Natural Science
Foundation of China (50472014) and Chinese
Academy of Sciences under the Program for
Recruiting Outstanding Overseas Chinese (Hun-
dred Talents Program) is gratefully acknowl-
edged. We thank the Fund for Innovation
Research from Shanghai Institute of Ceramics,
Chinese Academy of Sciences and the Natural
Science Foundation from Science and Technol-
ogy Committee of Shanghai (03ZR14104), P. R.
China.
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