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CHEMPHYSCHEM
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DOI: 10.1002/cphc.201402088
Growth of Fe3O4 Nanorod Arrays on Graphene Sheets for
Application in Electromagnetic Absorption Fields
Huanming Zhang,[a] Chunling Zhu,*[a] Yujin Chen,*[b] and Hong Gao[c]
A facial strategy is developed to fabricate a three-dimensional
(3D) Fe3O4 nanorod array/graphene architecture, in which
Fe3O4 nanorods with a length and diameter of about 600 and
100 nm, respectively, are grown on both surfaces of the gra-
phene sheets. The measured electromagnetic parameters show
that the 3D architecture exhibits excellent electromagnetic
wave-absorption properties, that is, more than 99 % of electro-
magnetic wave energy can be attenuated by the 3D architec-
1. Introduction
Electromgnetic (EM) wave absorbing materials have attracted
much attention due to expanded EM interference problems to
electronic and communication devices and due to harm to bio-
logical systems. Currently, EM absorbing materials with strong
absorption properties and lightweight characteristics are
highly desired. Traditional absorbers such as ferrite has strong
absorption characteristics, but the large amount that was re-
quired to be added to the insulating matrix and its thickness
have limited its practical application. Therefore, many nano-
structures have recently been investigated for EM absorption
application.[1–3]
Fe3O4 is an important magnetic material, and it has attractive
physical properties such as strong spin polarization at room
temperature and half-metallic character. Its magnetic proper-
ties can be tuned by size, shape, and dimension, and therefore,
Fe3O4 has wide applications in many areas.[4] Recently, Fe3O4
and its nanocomposites have been reported for the attenua-
tion of EM waves.[5] However, the amount of these materials
added to the insulating matrix was usually larger than 40 wt %,
which needs to be further decreased.
[a] H. Zhang, Prof. Dr. C. Zhu
College of Materials Science and Chemical Engineering
Harbin Engineering University
Harbin, Heilongjiang, 150001 (China)
E-mail: zhuchunling@hrbeu.edu.cn
[b] Prof. Dr. Y. Chen
College of Science, Harbin Engineering University
Harbin, Heilongjiang, 150001 (China)
E-mail: chenyujin@hrbeu.edu.cn
[c] Prof. Dr. H. Gao
Key Laboratory for Photonic and Electric Bandgap Materials
Ministry of Education, Harbin Normal University
Harbin, Heilongjiang, 150025 (China)
Supporting Information for this article is available on the WWW under
http://dx.doi.org/10.1002/cphc.201402088.
 2014 Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim
ture if it is added in only 20 wt % of the paraffin matrix, as the
thickness of the absorber is in the range from 2.38 to 5.00 mm.
The analysis of the electromagnetic (EM) absorption mecha-
nism reveals that the excellent EM absorption properties are
related to the special 3D architecture, and therefore, the con-
struction of graphene-based 3D heteronanostructures is effec-
tive in obtaining lightweight EM absorbers with strong absorp-
tion properties.
Recently, graphene (G) and G-based heteronanostructures
showed excellent EM absorption properties.[6–9] Among them,
G/Fe3O4 heteronanostructures have attracted much attention.
Wang et al. fabricated G/Fe3O4 nanohybrids with a minimum
reflection loss of 40.36 dB at a thickness of 5.0 mm.[7a] Guan
et al. assembled nanoparticles on graphene, and they showed
enhanced EM wave loss.[7b] Hu et al. were the first to grow
Fe3O4 nanoparticles on graphene, and they obtained 3D G/
Fe3O4 structures by a freeze-drying process. The minimum re-
flection loss of the 3D structures reached about 27 dB.[7c] Li
et al. reported a single polyol method to fabricate G/Fe3O4 hy-
brids with a minimum reflection loss of 30.1 dB at 1.48 mm
matching thickness and 17.2 GHz matching frequency.[7e] These
above works demonstrated that G/Fe3O4 nanocomposites are
very promising for applications in EM absorbing materials.
However, most of the above nanocomposites are based on
two-dimensional (2D) graphene sheets with anchored or ad-
sorbed zero-dimensional (0D) Fe3O4 nanoparticles. It is believed
that designing and constructing 3D graphene-based heterona-
nostructures will be very interesting to improve their EM ab-
sorption properties further.[9] The experimental fabrication of
such 3D architectures including a 3D polyaniline nanorod
array/graphene architecture and a 3D carbon nanotube/gra-
phene sandwich has been successfully achieved.[9, 10] However,
the growth of magnetic nanorod arrays on the surfaces of gra-
phene sheets is a challenge.
In this paper, we designed a 3D graphene architecture, that
is, Fe3O4 nanorod arrays on the surfaces of graphene sheets by
a simple hydrothermal process and a subsequent heating
treatment. The reflection loss reached 61.5 dB for the 3D
Fe3O4 nanorod array/G (Fe3O4 NRA/G) architecture with a thick-
ness of 2.74 mm. More importantly, the amount of the 3D ar-
chitecture added to the paraffin matrix was only 20 wt %. Thus,
the 3D Fe3O4 NRA/G architecture is very promising for poten-
tial application in the field of EM absorption.
ChemPhysChem 2014, 15, 2261 – 2266 2261
CHEMPHYSCHEM
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2. Results and Discussion
Figure S1a (Supporting Information) shows the X-ray diffraction
(XRD) pattern of the b-FeOOH NRA/G architecture. All the dif-
fraction peaks in the pattern can be indexed to orthorhombic
b-FeOOH, which indicates that that the product consists of b-
FeOOH. Top-view scanning electron microscopy (SEM) images
(Figure 1 a and the inset) show that the average length and di-
Figure 1. Structural characterization of the b-FeOOH NRA/G architecture:
a) Top-view SEM image, b) cross-section SEM image, c) TEM image, and
(d) HRTEM image (inset shows the SAED pattern).
ameter of most of the b-FeOOH nanorods with square tips are
about 600 and 100 nm, respectively. The cross-section SEM
image and low-resolution transmission electron microscopy
(TEM) image (Figure 1 b, c) clearly show that the b-FeOOH
nanorods are grown on both side surfaces of the graphene
sheets with an inclined angle, which results in the formation of
an interesting 3D hierarchical architecture. Lattice fringes in
the high-resolution TEM (HRTEM) image (Figure 1 d) and the
diffraction spots presented in the selected-area electron dif-
fraction (SAED) pattern suggest that the nanorods are of a crys-
tal nature.
To understand the formation process of the b-FeOOH NRA/G
architecture, additional experiments were performed. Sparse b-
FeOOH nanorods with spindle-like tips were grown on the sur-
faces of the graphene sheets at the initial reaction stage
(30 min.), as shown in Figure 2 a. The diameter and length of
these nanorods was about 50 and 200 nm, respectively. With
an increase in the reaction time to 2 h, the density and size of
the b-FeOOH nanorods significantly increased (Figure 2 b), but
the shape of the tips was similar to that obtained at a reaction
time of 30 min. As the reaction time was prolonged to 6 h, the
tips of the b-FeOOH nanorods changed to a square shape (Fig-
ure 2 c) and the diameter and length of the nanorods increased
to about 90 and 500 nm, respectively. If the reaction time was
 2014 Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim
www.chemphyschem.org
Figure 2. SEM images of the products obtained at different reaction times (t)
and temperatures (T): a) t = 30 min, T = 100 8C, scale bar: 100 nm; b) t = 2 h,
T = 100 8C, scale bar: 200 nm; c) t = 6 h, T = 100 8C, scale bar: 250 nm;
d) t = 10 h, T = 100 8C, scale bar: 400 nm; and e) t = 12 h, T = 80 8C, scale bar:
400 nm. f) SEM image of the product without graphene, scale bar: 200 nm.
further prolonged, the density and size of the b-FeOOH nano-
rods on the surfaces of the graphene sheets also increased,
but the shape of the tips did not change any longer (Figure 2 d
and 1 a). In addition, the reaction temperature also had an im-
portant effect on the growth of the b-FeOOH nanorods on the
surfaces of the graphene sheets. For example, relatively sparse
b-FeOOH nanorods with spindle-like tips were anchored on
the graphene sheets at a reaction temperature of 80 8C, but
a red precipitate formed in the solution if the reaction temper-
ature was increased to 120 8C (not shown), which suggests
that overgrowth of the nanorods occurred. The above results
demonstrate that the reaction time and temperature play im-
portant roles in the formation of the 3D b-FeOOH nanorod
array/G architecture. Notably, agglomerated b-FeOOH nano-
rods were obtained without graphene sheets in the reaction
system, as shown in Figure 2 f.
The 3D Fe3O4 NRA/G architecture could be obtained after
the b-FeOOH NRA/G architecture was thermally treated in H2/
Ar flow at 280 8C for 3 h. Figure S1 b shows the XRD pattern of
the product. All the diffraction peaks marked with Miller indi-
ces in the pattern can be indexed to the cubic Fe3O4 phase
(JCPDS no. 19-0629). No diffraction peaks from b-FeOOH were
detected in the product. However, because the patterns of g-
ChemPhysChem 2014, 15, 2261 – 2266 2262
CHEMPHYSCHEM
ARTICLES
Fe2O3 and Fe3O4 are very similar, XRD analysis could not be
used to determine if g-Fe2O3 was present in the product. X-ray
photoelectron spectroscopy (XPS) was therefore used to deter-
mine the difference in the oxidation state of iron. Figure S2
shows the Fe 2p core-level XPS spectrum of the 3D Fe3O4
nanorod array/G architecture. There are two main peaks locat-
ed at 711 and 725 eV that correspond to Fe 2p3/2 and Fe 2p1/2,
respectively. Shakeup satellite peaks as fingerprints of the elec-
tronic structures of the iron oxides such as hematite or maghe-
mite were not identified.[11] This result implies that b-FeOOH
was totally transformed into Fe3O4 after thermal treatment.
The morphology and structure of the 3D Fe3O4 NRA/G archi-
tecture were further investigated by SEM and TEM measure-
ments. The SEM and TEM images (Figure 3 a–c) show that the
Figure 3. Structural characterization of the 3D Fe3O4 NRA/G architecture:
a) Top-view SEM image (inset shows a magnified SEM image), b) cross-sec-
tion SEM image, c) TEM image, and d) HRTEM image (inset shows the corre-
sponding SAED pattern).
3D Fe3O4 NRA/G architecture maintained a morphology that
was similar to that of the 3D b-FeOOH nanorod array/G archi-
tecture; however, a few nanorods lay flat on the surfaces of
the graphene sheets after the thermal treatment. The average
diameter and average length of the Fe3O4 nanorods were close
to those of the b-FeOOH nanorods, as shown in Figure 3 b, c.
Clear lattice fringes are observed in the HRTEM image (Fig-
ure 3 d), which indicates that the Fe3O4 nanorods are of a crystal
nature. The interplanar spacings marked by white lines are
0.488 and 0.298 nm, which correspond to the (111) and (220)
planes of cubic Fe3O4, respectively. The marked diffraction
spots in the SAED pattern (Figure 3 d, inset) correspond to the
(111), (311), and (422) crystalline planes of cubic Fe3O4, and this
reveals the single-crystal nature of the Fe3O4 nanorods. In addi-
tion, even after a long time of strong ultrasonication (30 min.),
the Fe3O4 nanorods were still anchored on the surface of the
 2014 Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim
www.chemphyschem.org
graphene sheets, as shown in Figure S3. This indicates that
there is a strong bond between graphene and the Fe3O4 nano-
rods.
The field dependence of the magnetization for the 3D Fe3O4
NRA/G architecture was measured by using a vibrating sample
magnetometer (VSM) at room temperature, as shown in Fig-
ure S4. Significant hysteresis loops in the M–H curve indicate
the ferromagnetic behavior of the 3D architecture (M = mag-
netization, H = field strength). The saturation magnetization
(Ms), coercivity (Hc), and retentivity (Mr) were 66.5 emu g1,
284.0 Oe, and 21.5 emu g1, respectively. The value of Ms is
smaller than the corresponding bulk value (92 emu g1), which
is attributed to the presence of nonmagnetic graphene in the
3D architecture and the spin disorder on the surface in the
nanomaterials.[12]
The 3D Fe3O4 NRA/G architecture possesses a special struc-
ture and ferromagnetic properties, and this suggests that it
may have good EM absorption properties.[13, 14] The EM absorp-
tion properties were investigated in terms of the relative com-
plex permittivity (er = e’je’’) and the relative complex permea-
bility (mr = m’jm’’), where e’ and e’’ are real part and imaginary
part of the relative complex permittivity, respectively; m’ and
m’’ are real part and imaginary part of the relative complex per-
meability, respectively. The reflection loss (RL) values were cal-
culated by Equations (1) and (2) at a given frequency and
thickness layer according to the transmit line theory:[15]
pffiffiffiffiffiffiffiffiffiffi pffiffiffiffiffiffiffiffi
Zin ¼ Z0 mr =er tanh½jð2pfd=cÞ mr er ð1Þ
RL ½dB ¼ 20 logjðZin  Z0 Þ=ðZin þ Z 0 Þj ð2Þ
in which Z0 is the impedance of free space, Zin is the input im-
pedance of the absorber, c is the velocity of the EM wave in
free space, f is the frequency of the EM wave, and d is the
thickness of the absorber. The calculated values of RL for the
Figure 4. a) The reflection losses of the 3D Fe3O4 NRA/G architecture and
b) top-view of a).
ChemPhysChem 2014, 15, 2261 – 2266 2263
CHEMPHYSCHEM
ARTICLES
3D Fe3O4 NRA/G architecture are shown in Figure 4 and
Table S1. All of the minimum RL values were less than 20 dB
for the 3D Fe3O4 NRA/G architecture with thicknesses and fre-
quencies in the range from 2.36 to 5 mm and from 4.4 to
10.8 GHz, respectively. The absorption bandwidth with a reflec-
tion loss less than 20 dB was up to 6.4 GHz. Importantly, the
minimum RL values were 62, 55, and 53 dB at thicknesses
of 2.74, 3.16, and 3.66 mm, respectively. Because more than
99 % of the EM wave energy can be attenuated by the absorb-
er if its RL value is less than 20 dB, the Fe3O4 NRA/G architec-
ture exhibits excellent EM absorption properties. However, all
of the RL values for the pure Fe3O4 nanorods and the graphene
were larger than 5 (Figure S5) and 11 dB,[8] respectively. In
addition, compared to other Fe3O4 nanostructures, the 3D
NRA/G architecture also has better EM absorption properties.[16]
Moreover, the amount of the 3D architecture added to the
wax matrix was only 20 wt %, which is much less than that
added for other magnetic nanomaterials. Thus, the 3D Fe3O4
NRA/G architecture can be used as a lightweight EM absorbing
material with excellent EM absorption properties.
To understand the possible microwave absorption mecha-
nism, the relative complex permittivity and permeability of the
3D Fe3O4 NRA/G architecture and Fe3O4 nanorods were investi-
gated in the frequency range from 2 to 18 GHz, as shown in
Figures S6 and S7. The real parts of the permittivity for both
the Fe3O4 nanorods and the 3D Fe3O4 NRA/G architecture
show a slight variation at low frequencies ranging from 2 to
10 GHz, but decrease slightly around 12 GHz and remarkably
around 15 GHz. The imaginary parts of the permittivity have
a weak peak at around 12 GHz and a sharp peak at around
15 GHz for both the Fe3O4 nanorods and the 3D Fe3O4 NRA/G
architecture. Because Fe3O4 has a larger electric conductivity
than paraffin, upon mixing together the trapped space charge
in the Fe3O4 grain oscillates in the applied alternating-current
(AC) electric field like a dipole.[17] Such a space charge and clas-
sical orientation polarization results in a dielectric loss peak at
around 12 GHz.[17] Another dielectric loss peak around 15 GHz
is sharper than the former one, which is likely caused by reso-
nance rather than relaxation.[18] The induced interfacial dipoles
between Fe3O4 and paraffin similar to the Stern layer in the
electrical double layer model contribute to the resonance. De-
spite the fact that both the 3D Fe3O4 NRA/G architecture and
the Fe3O4 nanorods have a similar variation trend in the per-
mittivity, the dielectric tangent
loss (tande = e’’/e’) values of the
3D Fe3O4 NRA/G architecture are
in the 0.24–0.34 range, which is
much higher than that of the
pure Fe3O4 nanorods (0.01–0.14,
see Figure S8). Thus, the im-
proved dielectric loss induced by
dipolar polarization, interfacial
polarization, and associated res-
onance phenomena is attributed
Scheme 1. Schematic diagram of the structural effect on the EM absorption of the absorbers: a) 3D architecture
to the enhanced EM absorption
containing a high density of Fe3O4 nanorods, b) 3D architecture containing a relatively low density of Fe3O4 nano-
performance of the 3D architec- rods, and c) the Fe3O4 nanorods without graphene. For simplicity, the reflectance wave between the free space
ture. and the magnetic materials and the transmission wave through graphene are not shown in the scheme.
 2014 Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim
www.chemphyschem.org
Although both the 3D Fe3O4 NRA/G architecture and the
Fe3O4 nanorods have very close m’ values in the frequency
range from 2 to 18 GHz, the m’’ values of the former are much
higher than those of the latter in the low frequency range (2–
8 GHz), as shown in Figure S7. According to this trend,
a strong peak for the sample is expected in the low-frequency
regime (< 2 GHz), which is ascribed to the natural resonance.[19]
This leads to magnetic tangent loss values (tandm = m’’/m’) that
are higher for the 3D Fe3O4 NRA/G architecture than for the
Fe3O4 nanorods in the low frequency range (Figure S9), and
therefore, the improved magnetic loss also contributes to the
enhanced EM absorption performance of the 3D architecture.
The enhanced EM absorption properties of the 3D architec-
ture induced by the improved dielectric and magnetic losses is
related to their special structures, as demonstrated previous-
ly.[8, 13] On the one hand, the magnetic nanorod arrays grown
on both sides of the graphene sheets can decrease the resist-
ance of the absorbers. The decreased resistance will lead to an
increase in the dielectric loss in terms of Equation (3):
e00 / s=2pe0 f ð3Þ
in which s and e0 are the conductivity and the dielectric con-
stant of the absorber at free space, respectively. In this case,
the Fe3O4 NRA/G architecture can consume a greater amount
of heat energy that is produced as the absorber is irradiated
by the EM wave. On the other hand, as described previously,
the graphene sheets exhibited weak EM absorption properties
due to the skin effect, that is, most of incident EM waves are
reflected by graphene.[6d] As shown in Scheme 1 a, the reflec-
tance wave was absorbed by the Fe3O4 nanorod arrays again.
If the graphene sheets were absent, the second absorption
would not occur, as shown in Scheme 1 c. The second absorp-
tion relates to the density of the Fe3O4 nanorod arrays grown
on the graphene sheets. Low density will lead to a decrease in
the EM absorption properties of the 3D architecture, as shown
in Scheme 1 b. To verify this, we prepared a 3D architecture
containing a low density of the Fe3O4 nanorod arrays by the
same process as that shown in the Experimental Section
except the amount of FeCl3·6 H2O added was reduced to 1.0 g.
The SEM image shows that the 3D architecture contains
a lower density of Fe3O4 nanorod arrays (Figure S10). Fig-
ure S10 and the inset show that the average length and diam-
ChemPhysChem 2014, 15, 2261 – 2266 2264
CHEMPHYSCHEM
ARTICLES
eter of the Fe3O4 nanorods are about 600 and 100 nm, respec-
tively. This product exhibits EM absorption properties that are
inferior to those of the 3D architecture with a high density of
Fe3O4 nanorod arrays. However, because the second absorp-
tion still exists (Scheme 1 b), it has better EM absorption prop-
erties than the graphene sheets and the pure Fe3O4 nanorods,
as shown in Figure S11. Due to the similar sizes of the nano-
rods in the two samples, we think that the density of the
Fe3O4 nanorod arrays on the graphene sheets plays the main
role in the EM absorption properties. In addition, the gra-
phene/Fe3O4 nanorod interfaces are advantageous to the im-
provement of the EM absorption properties due to the existing
interfacial polarization. These factors mentioned above reveal
that the excellent EM absorption properties of the 3D Fe3O4
NRA/G architecture are a result of these special structural char-
acteristics.
Notably, a geometrical effect was recently proposed to inter-
pret the EM absorption properties of the absorbers. The geo-
metrical effect occurs as the incident and reflected waves in
the absorbers are out of phase by 1808. It is strongly depen-
dent on the thickness (t) of the absorbers [Eq. (4)],[20]
t ¼ nlm =4ðn ¼ 1; 3; 5; :::Þ ð4Þ
1/2
in which lm = c/[fm(jmrjjerj) ] and j mr j and j er j are the moduli
of mr and er, respectively. According to the data of RL, the
values of fm, mr, and er, n can be obtained, as shown in Table S1.
All the calculated n values were not or close to odd numbers,
and therefore, the geometric effect does not contribute to the
excellent EM absorption properties of the 3D Fe3O4 NRA/G ar-
chitecture.
3. Conclusions
In summary, we developed an efficient strategy to fabricate
a 3D Fe3O4 NRA/G architecture, in which Fe3O4 nanorods with
a length and diameter of about 600 and 100 nm, respectively,
were grown on both surfaces of the graphene sheets. The 3D
Fe3O4 NRA/G architecture with ferromagnetic properties exhib-
its excellent EM absorption properties, including a strong abili-
ty to attenuate the EM wave, and it is also lightweight. The EM
absorption mechanism of 3D Fe3O4 NRA/G, which results from
its special structure, was proposed to explain the excellent EM
absorption properties of the 3D architecture. Our results dem-
onstrate that the design of graphene-based 3D heteronanos-
tructures is effective to obtain lightweight EM absorbers with
strong absorption properties.
Experimental Section
Graphene used in this work was purchased from Nanjing XFNano
Material Tech Co., Ltd. Other analytical reagents were purchased
from Tianjin Kermel Chemical Reagent Co. Ltd. (Tianjin, China).
The b-FeOOH nanorod array/G was prepared by a hydrothermal
method. Simply, FeCl3·6 H2O (1.5 g) was dissolved in distilled water
(40 mL) and then graphene (5 mg) was added to the solution.
After sonication for 5 min, this solution was transferred to a Teflon-
 2014 Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim
www.chemphyschem.org
lined stainless steel autoclave with a capacity of 50 mL. The auto-
clave was sealed, maintained at 100 8C for 12 h, and cooled to
room temperature naturally. The precipitate was washed with dis-
tilled water and absolute ethanol several times and then dried in
vacuum at 40 8C for 12 h. The 3D Fe3O4 NRA/G architecture was ob-
tained by heating the b-FeOOH NRA/G architecture at 280 8C for
3 h under Ar/H2 flow. For comparison, the b-FeOOH nanorods
were also prepared without graphene sheets in the reaction
system under the same conditions as those used for the synthesis
of the b-FeOOH NRA/G architecture. The pure Fe3O4 nanorods
were synthesized after thermal treatment of the b-FeOOH nano-
rods under the same thermal treatment conditions mentioned
above. The morphology and size of the synthesized samples were
characterized by using SEM (JEOL-JSM-6700F) and TEM (JEOL
2010). The crystal structure of the sample was determined by XRD
D/max 2550 V, CuKa radiation. XPS measurements were performed
by using a spectrometer with MgKa radiation (ESCALAB 250, Ther-
mofisher Co.). The EM parameters of the samples (Fe3O4 nanorods,
Fe3O4 NRA/G architecture) were measured with an ANRITSU
37269D vector network analyzer. The measured samples were pre-
pared by uniformly mixing 20 wt % of the sample with a paraffin
matrix. The mixture was then pressed into toroidal shaped samples
(fout = 7.00 mm; fin = 3.04 mm).
Acknowledgements
We thank the National Natural Science Foundation of China
(Grant No. 51272050) and the Open Project Program of the Key
Laboratory for Photonic and Electric Band Gap Materials, Ministry
of Education, Harbin Normal University, China, for the financial
support of this research.
Keywords: electromagnetic wave absorption · graphene · iron
oxide · magnetic properties · nanostructures
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Received: March 4, 2014
Published online on May 14, 2014
ChemPhysChem 2014, 15, 2261 – 2266 2266