COMPOSITES

SCIENCE AND
TECHNOLOGY
Composites Science and Technology 66 (2006) 20032008
www.elsevier.com/locate/compscitech

Synthesis, magnetic and microwave absorbing properties

of core-shell structured MnFe2O4/TiO2 nanocomposites
a,b a,b a,*
Hong-Mei Xiao , Xian-Ming Liu , Shao-Yun Fu
a
Technical Institute of Physics and Chemistry, Chinese Academy of Sciences, Beijing 100080, PR China
b
Graduate School, Chinese Academy of Sciences, Beijing 100039, PR China

Received 23 August 2005; received in revised form 27 December 2005; accepted 10 January 2006
Available online 17 February 2006

Abstract

The core-shell MnFe2O4TiO2 nano-composites were prepared by hydrolysis of titanium butoxide precursor in the presence of
MnFe2O4 nanoparticles that were synthesized via the pyrolysis of polyacrylate salt precursor prepared by in situ polymerization of
the metal salts and acrylate acid. The magnetic properties of the MnFe2O4 and MnFe2O4TiO2 composites measured at the maximum
magnetic eld of 10 kOe and room temperature exhibited a super-paramagnetic behavior. The complex permittivity and permeability of
MnFe2O4 and MnFe2O4TiO2 composites measured in the microwave frequency range of 210 GHz showed that the microwave absorp-
tion properties of the MnFe2O4TiO2 composites were higher than that of MnFe2O4.
2006 Elsevier Ltd. All rights reserved.

Keywords: Manganese ferrite; Titanium dioxide; Nanocomposites; Microwave absorbing property; Magnetic property

1. Introduction that magnetic nano-composites are useful as microwave

Much attention has been paid to microwave absorption
materials due to their unique absorbing microwave energy
and promising applications in the stealth technology of air-
craft, television image interference of high-rise buildings,
and microwave dark-room and protection [13]. Extensive
study has been carried out to develop new microwave
absorbing materials with a high magnetic and electric loss
[49]. To our knowledge, ferrites might be a candidate as
the microwave absorbing materials because of their high
specic resistance, remarkable exibility in tailoring the
magnetic properties and ease of preparation [2]. In the past
decades, the spinel ferrites have been utilized as the most
frequent absorbing materials in various forms [3]. Manga-
nese ferrite (MnFe2O4) is a common spinel ferrite material
and has been widely used in microwave and magnetic
recording applications [10]. Recently, it has been shown
*
Corresponding author. Tel.: +86 10 62626152; fax: +86 10 62569040.
E-mail addresses: syfu@cl.cryo.ac.cn, syfu@mail.ipc.ac.cn (S.-Y. Fu).
absorbing materials due to their advantages in respect to
light weight, low cost, design exibility, and microwave
properties over pure ferrites [8,11].
On the other hand, titanium dioxide (TiO2) is an impor-
tant inorganic semiconductor and has temperature and
environmentally stable dielectric properties [12]. A series
of papers dealing with application for the magnetic com-
posites containing TiO2 nanoparticles have been reported
[1329]. Nonetheless, up to now, most research work has
only been focused on the TiO2-based composites applica-
tion for magnetic photo-catalysts [1323]. There are few
articles concerning the microwave absorbing properties of
TiO2-based composites. Soitoh et al. and Ueda et al.
reported the mixture of carbonyl iron (FeOH) and TiO2
in hypolan (chlorosulfonated polyethylene) as the micro-
wave absorber [28,29]. To our best knowledge, the core-
shell structured electro-magnetic functional composites
are promising as new microwave absorbing materials.
However, as we know, no work has been reported on the
microwave absorbing properties of core-shell structured
TiO2-based magnetic composites.

0266-3538/$ - see front matter 2006 Elsevier Ltd. All rights reserved.
doi:10.1016/j.compscitech.2006.01.001
2004 H.-M. Xiao et al. / Composites Science and Technology 66 (2006) 20032008
Recently, syntheses of ferrite nanoparticles by the ther-
mal decomposition reaction are of great interest in the
study and tailoring of specic magnetic properties. Gabal
and Ata-Allah [30] synthesized manganese ferrites through
the thermal decomposition reaction taking place between
the solid-state oxalate mixture of MnC2O4 2H2O
FeC2O4 2H2O in air. However, when the annealing tem-
perature was lower than 1100 C, there existed impurities
such as a-Fe2O3 and Mn2O3. Compared to the reported
methods, there are two advantages of the thermal decom-
position of the polyacrylate precursors [31]. It can provide
high product yield and highly homogeneous nanocrystal-
line spinel ferrites at medium calcination temperature.
In this article, the core-shell structured MnFe2O4TiO2
nano-composites were prepared by hydrolysis of titanium
butoxide precursor in the presence of MnFe2O4 nanoparti-
cles in a mixed organic solvent, where MnFe2O4 was syn-
thesized via the pyrolysis of polyacrylate salt precursors
prepared by in situ polymerization of the metal salts and
acrylate acid. The crystal structure, magnetic properties
of the composites were measured and compared with
that of the MnFe2O4 nanoparticles. The eect of the
content of the TiO2 on the complex permittivity and per-
meability of the nano-composites at 210 GHz frequency
have been investigated.
2. Experimental
The chemical reagents, including Mn(CH3COO)2
4H2O, Fe(NO3)3 9H2O, acrylic acid, (NH4)2S2O8, cetylt-
rimethylammonium bromide (CTAB), titanium tetrabutyl-
oxide, n-butanol and ethanol are of analytical grade and
were used without further purication.
2.1. Preparation of MnFe2O4 nanoparticles
Nanocrystalline MnFe2O4 powders were prepared by a
polymer-pyrolysis method using polyacrylates of Mn and
Fe as precursor compounds. Measured amounts of
Mn(CH3COO)2 4H2O and Fe(NO3)3 9H2O (molar ratio
of Mn:Fe = 1:2) were dissolved in 10 g of acrylic acid aque-
ous solution (acrylic acid:H2O = 70:30 wt%) under stirring.
Then, a small amount (0.5 g) of 5% (NH4)2S2O8 aqueous
solution as the initiator was added to the mixed acrylic acid
solution to promote the polymerization. Under heating at
7090 C for 2 h, the mixed solution was dried to form
the well-distributed polyacrylates of Mn and Fe. After
the resulting polyacrylates were dried at 100 C for 24 h,
and calcined at 500 C for 2 h in air, the MnFe2O4 nano-
particles were obtained after being slowly cooled to room
temperature.
2.2. Preparation of MnFe2O4TiO2 nano-composites
The whole experiment was operated in an ultrasonic
pool (100 W, 50 Hz). Titania was coated on MnFe2O4
nanoparticles by hydrolysis of titanium butoxide precursor.
In one experiment, 0.15 g of as-synthesized MnFe2O4
nanoparticles and 0.15 g of cetyltrimethylammonium bro-
mide (CTAB) were dispersed into 135 mL of n-butanol
and anhydrous ethanol (8:1 in volume) solution. After son-
ication for 30 min, a few of drops of nitric acidwater solu-
tion (2 wt%) were added to the mixture. Then, 0.12 M
titanium tetrabutyloxide in anhydrous ethanol was added
by drop-wise into the mixture at room temperature with
controlled rhythm. The weight contents of TiO2 in the
composites were 10%, 20%, 50% and 100%, respectively.
After the drop-wise addition was over, the reaction mixture
was irradiated with ultrasound and the temperature of the
reaction mixture rose to 75 C. This experiment went along
for 4 h. The resulting nanoparticles were separated centrif-
ugally. The supernatant was discarded, and the precipitate
was washed repeatedly with anhydrous ethanol. Then the
precipitate was dried at 100 C for 24 h in air. The tita-
nia-coated MnFe2O4 nano-composites were obtained after
being calcined at 500 C for 2 h in air.
2.3. Characterization
The dried samples (i.e. MnFe2O4 and MnFe2O4TiO2
composites) were analyzed for their composition, micro-
structure, magnetic and microwave properties.
The scanning electron microscopy (SEM) images and
EDX were obtained using a HITACHI S-4300 microscope
and EMAX Horiba, respectively. XRD analysis was car-
ried out on a Rigaku D/max2500 diractometer at a volt-
age of 40 kV and a current of 200 mA with Cu Ka
radiation (k = 1.5406 A), employing a scanning rate of
0.02 s1 in the 2h ranging from 5 to 70 C. TEM images
and the electron diraction (ED) patterns were recorded
on a Hitachi-600 transmission electron microscope
(TEM) at an accelerating voltage of 20 kV. Magnetic mea-
surements were carried out at room temperature using a
vibrating sample magnetometer (VSM, Lakeshore 7307,
USA) with a maximum magnetic eld of 10 kOe.
The samples for measuring microwave properties were
prepared by dispersing the MnFe2O4 and MnFe2O4TiO2
composites powders in paran wax, respectively. The vol-
ume fraction of the powders is 60%. The powder-wax com-
posites were die-pressed to form cylindrical toroidal
specimens with 7.0 mm outer diameter, 3.0 mm inner diam-
eter, and 2 mm thickness. The measurements of complex
permittivity, e, and permeability, l, for the specimens were
carried out using an Agilent E8363B vector network ana-
lyzer in the 210 GHz ranges.
3. Results and discussion
3.1. Morphology and crystal structures
The panoramic morphology of the representative
MnFe2O4TiO2 nano-composite (20%TiO2) was obtained
by SEM as shown in Fig. 1(a), in which the solid sample
was mounted on conductive resin with dispersion
 H.-M. Xiao et al. / Composites Science and Technology 66 (2006) 20032008
Fig. 1. SEM images (a) and SEMEDS element analysis (b) of represen-
tative TiO2MnFe2O4 (20%TiO2) nano-composites.
treatment. Fig. 1(a) displays that the composite nanoparti-
cles have homogeneous structures with a diameter of
1525 nm. The corresponding SEMEDS spectra are pre-
sented in Fig. 1(b). It conrms the presence of Fe, Mn,
Ti, and O atoms. Fig. 2 shows the X-ray diraction
(XRD) patterns of MnFe2O4 nanoparticles and the repre-
sentative MnFe2O4TiO2 composites (20%TiO2). Fig. 2(a)
shows XRD patterns of the MnFe2O4 powders, presenting
the characteristic peaks of cubic spinel structure. The peaks
appear at 2h = 18.5, 30.2, 35.6, 43.0, 53.4, 57.1, and
62.5 which are well indexed to the crystal plane of spinel
ferrite (1 1 1), (2 2 0), (3 1 1), (4 0 0), (4 2 2), (5 1 1), and
(4 4 0), respectively. The average crystallite diameter
(ACD) of the Mn ferrite particles was determined from
the major diraction peak (3 1 1) using the well-known
Scherrers formula [32]:
ACD 0:9k=Dw  cos h;
where k is the X-ray wavelength, h the angle of Bragg dif-
fraction, and Dw the dierence between the full-width at
half-maximum (FWHM) and the instrumental broadening.
The calculated ACD value of nanocrystalline MnFe2O4 is
found to be about 12 nm that is in agreement with TEM
results shown in Fig. 3(a). The TiO2 as a shell has an ana-
tase structure for the annealed titania-coated Mn ferrite
sample, determined from XRD pattern in Fig. 2(b) where
2005
(101)
. MnFe2O4
*
. * Anatase TiO2
. .. .
. .
(004)
. *
(200)
*
(105)
*
b
(311)
.
(220)
. . . (440)
.
(111)
(400)
.
(511)
(422) a
10 20 30 40 50 60 70
2 theta(degree)
Fig. 2. XRD patterns of MnFe2O4 nanoparticles (a) and the representa-
tive MnFe2O4TiO2 nano-composites (b).
the peaks of (1 0 1), (1 0 4), (2 0 0) and (1 0 5) are the charac-
teristic peaks of anatase structural TiO2 [33]. In particular,
a weak peak at 2h = 33.16 in Fig. 2(b) shows the evidence
of small content of titanate in the MnFe2O4TiO2 nano-
composite [34,35].
TEM images for the obtained nano-sized MnFe2O4
powders and the MnFe2O4TiO2 composites are shown
in Fig. 3(ad). The average size of MnFe2O4 particles is
estimated to be between 10 and 20 nm. It is clearly seen
that the composite particles show a good coating when
the weight ratio of TiO2 is 20%. With the increase of the
weight ratio of TiO2, the product is complicated. For the
MnFe2O4 nanoparticles, a typical ED ring pattern of spinel
structure is also shown in Fig. 3(e). Fig. 3(f) gives ED pat-
tern of the representative TiO2 coated MnFe2O4 nanopar-
ticles. In contrast, the characteristic diraction rings of
anatase TiO2 appear in the coated MnFe2O4TiO2 com-
posites (20%TiO2) attributing to (1 0 1), (0 0 4) and (2 0 0)
lattice faces of anatase TiO2.
3.2. Magnetic properties, complex permittivity and
permeability at 210 GHz
The magnetic properties of the as-synthesized MnFe2O4
and the representative MnFe2O4TiO2 nano-composite
(20%TiO2) were measured using a vibrating sample magne-
tometer (VSM) at room temperature with an applied eld
10 kOe 6 H 6 10 kOe, as shown in Fig. 4. In case of
MnFe2O4 nanoparticles, saturated magnetization (Ms),
1
remnant magnetization (Mr) and coercive force (Hc) were
estimated to be Ms = 48.6 emu/g, Mr = 0 and Hc = 0,
respectively. No hysteresis loop (i.e. Mr = 0 and Hc = 0)
was observed, indicating a super-paramagnetic behavior.
A similar behavior for the MnFe2O4TiO2 composites
was observed. In contrast, Ms of the TiO2 coated MnFe2O4
decreases to 25.15 emu/g, mainly attributing to the volume
of the non-magnetic coating layer to the total sample
volume.
2006 H.-M. Xiao et al. / Composites Science and Technology 66 (2006) 20032008

Fig. 3. TEM micrographs of MnFe2O4 nanoparticles (a) MnFe2O4TiO2 nano-composites the weight content of TiO2 = (b) 10%, (c) 20% and (d) 50%,
ED ring pattern of MnFe2O4 nanoparticles (e) and representative MnFe2O4TiO2 nano-composites (20%TiO2) (f).

Fig. 5 shows the real and imaginary parts of permittivity
(e 0 , e00 ) and permeability (l 0 , l00 ) spectra of pure MnFe2O4
wax composites and MnFe2O4TiO2 (weight ratio of
TiO2 = 10%, 20%, 50%, 100%)wax composites. As shown
in Fig. 5(a) and (b), the real and imaginary parts of the per-
mittivity of the specimens remained almost constant in the
whole frequency range, where the e 0 increased slightly with
the increase of the weight ratio of TiO2 and the e00 values
were around zero and independent of the weight ratio of
TiO2. The change in the e 0 and e00 with frequency for
MnFe2O4TiO2 (weight ratio of TiO2 = 10%, 20%, 50%,
100%)wax composites obeys the Lichiteneckers mixed
law [36]. Compared with the pure MnFe2O4, TiO2 has high
e 0 and equivalent e00 . So the existence of TiO2 will result in
the slight increase of e 0 but cannot inuence e00 of the
MnFe2O4TiO2wax composites. The real and imaginary
parts of the complex permeability are shown in Fig. 5(c)
and (d). We can nd that l00 of the MnFe2O4TiO2wax
composites are higher than that of pure MnFe2O4wax
composites in the whole frequency range. This result can
be explained by the magnetic dissipation. According to
Van Der Zaags suggestion [37], the magnetic dissipation
of classied ferrite includes: hysteresis loss, eddy current
loss, residual loss, ferromagnetic resonance loss and
 H.-M. Xiao et al. / Composites Science and Technology 66 (2006) 20032008 2007

TiO2 being a semiconductor with band gap energy of

40
3.2 eV [38,39]. Especially, when the weight ratio of TiO2
a
is 20%, both l 0 and l00 of the MnFe2O4TiO2wax compos-
ites show the maximum value. The TEM images (Fig. 3c)
Magnetization(emu/g)

20 b showed the best coating with the 20%TiO2. When the

MnFe2O4 was coated with the TiO2 completely, the com-
0 posites have good compatible dielectric and magnetic prop-
erties and hence the microwave absorbing properties show
-20 the maximum value.

-40
4. Conclusions

The TiO2 coated MnFe2O4 nano-composites have been

-10000
Fig. 4. Dependence of magnetization on the applied magnetic eld at
room temperature for MnFe2O4 nanoparticles (a) and representative
MnFe2O4TiO2 nano-composites (20%TiO2) (b).
intragranular domain wall loss. In this study, however, the
enhancement of eddy loss might be contributed to higher
l00 of the MnFe2O4TiO2wax composites because of
-5000 0 5000
Applied field(Oe)
10000 successfully prepared by the hydrolysis of titanium
butoxide precursor under ultrasonic conditions. The repre-
sentative MnFe2O4TiO2 nano-composites exhibited
super-paramagnetic behavior resulting from MnFe2O4
nanoparticles. Compared with MnFe2O4 nanoparticles,
the enhancement of the imaginary parts of permeability
(l00 ) of the MnFe2O4TiO2 nano-composites was due to
the eddy loss resulting from semiconductor TiO2 nanopar-
ticles. When the weight ratio of TiO2 was 20%, both l 0 and

4.8
4.7 pure MnFe2O4
0.28 pure MnFe2O 4
4.6 10% TiO2 0.24 10% TiO 2
4.5 20% TiO2 20% TiO 2
Imaginary Permittivity ('')

50% TiO2 0.20 50% TiO 2

4.4
Real Permittivity (')

4.3 100% TiO2 0.16 100% TiO2

4.2
0.12
4.1
4.0 0.08
3.9 0.04
3.8
3.7 0.00
3.6 -0.04
3.5
3.4 -0.08
3.3 -0.12
3.2
-0.16
3.1
3.0 -0.20
2 4 6 8 10 2 4 6 8 10
a Frequency (GHz) b Frequency (GHz)

1.5
pure MnFe2O4 0.20 pure MnFe2O4
10% TiO2 10% TiO2
1.4 0.18
Imaginary Permeability ('')

20% TiO2 20% TiO2

50% TiO2 0.16 50% TiO2
1.3
Real Permeability (')

0.14
1.2 0.12
0.10
1.1
0.08
1.0
0.06

0.9 0.04
0.02
0.8
0.00
0.7 -0.02
2 4 6 8 10 2 4 6 8 10
c Frequency (GHz) d Frequency (GHz)

Fig. 5. The complex permittivity and complex permeability of pure MnFe2O4wax composites and MnFe2O4TiO2 (weight ratio of TiO2 = 10%, 20%,
50%, 100%)wax composites. (a) real part of permittivity; (b) imaginary part of permittivity; (c) real part of permeability; (d) imaginary part of
permeability.
2008 H.-M. Xiao et al. / Composites Science and Technology 66 (2006) 20032008
l00 of the MnFe2O4TiO2wax composites showed the
maximum value.
Acknowledgment
We appreciate the nancial support of the National
High Technical Research and Development Program of
China (No. 2003AA305890).
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