Journal of Alloys and Compounds 575 (2013) 123–127

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Journal of Alloys and Compounds

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

The microwave absorbing properties of SmCo attached single wall

carbon nanotube/epoxy composites
Liming Yu ⇑, Bo Li, Leimei Sheng, Kang An, Xinluo Zhao ⇑
Department of Physics, Institute of Low-dimensional Carbons and Device Physics, Shanghai University, Shanghai 200444, China

a r t i c l e i n f o a b s t r a c t

Article history: The SmCo nanoparticles attached single wall carbon nanotubes (SmCo attached SWCNTs) were prepared
Received 25 January 2013 by hydrogen dc arc discharge method using 2:17 type SmCo permanent powder as catalyst. The SmCo
Received in revised form 26 March 2013 attached SWCNT/epoxy composites with different doping ratios were investigated in the frequency
Accepted 31 March 2013
region of 2–18 GHz. The complex permittivity and permeability of the SmCo attached SWCNT/epoxy
Available online 18 April 2013
composites were calculated. The reflection loss properties were simulated by transmission line theory
and the microwave absorptive mechanisms were discussed. The results indicate that, due to the better
Keywords:
interfacial polarization absorption mechanism of SmCo attached SWCNTs and the electromagnetic
Carbon nanotube
Microwave absorbing
(EM) matching of magnetic loss and dielectric loss, the microwave absorption properties of SmCo
Composite attached SWCNT/epoxy are evidently improved. When the SmCo attached SWCNTs is doped by 1 wt%,
Sm2Co17 the composite display a larger and wider absorption peak, and the bandwidth of the reflection loss below
20 dB is larger than 6 GHz with the thickness of 3.3 mm. It is expected that the new SmCo attached
SWCNT/epoxy composites will be a good microwave absorbing material for the applications in X band,
Ku band, or even K band.
Ó 2013 Elsevier B.V. All rights reserved.

1. Introduction
Currently the nano-composite material is one of the developing
trends of microwave absorbing materials that play an important
role in modern civil and military applications. Since the discovery
of carbon nanotube (CNT) by Iijima [1] in 1991, CNT has attracted
much attention for its special structure and intriguing properties
[2]. The CNT can be categorized into the single wall carbon nano-
tube (SWCNT) and the multiwall carbon nanotube (MWCNT).
Due to its high aspect ratio, one-dimensional nanostructure and
quantum effects, CNT exhibit a good prospect application, espe-
cially in microwave absorbing materials. Until now, there have
been many research papers on the permittivity characteristic and
the microwave characterization of CNT composites [3–10]. In order
to improve the absorption properties of CNT, many methods are
adopted to adjust the electromagnetic parameters of CNT, such
as mixing, doping and filling magnetic nanoparticles in CNT [11–
18]. It has been proved that the magnetic nanoparticles such as
Co, Fe and ferrites attached or coated on CNTs can improve the
EM matching properties of the composites.
The arc discharge method is a common technique to fabricate
high crystallinity SWCNTs. One of the advantages of this method
⇑ Corresponding authors. Tel.: +86 21 66132416/66136916; fax: +86 21
66134208.
E-mail addresses: lmyu@shu.edu.cn (L. Yu), xlzhao@shu.edu.cn (X. Zhao).
is that the needed metal particles can be directly attached to the
SWCNTs during the preparation. This approach opens up a new
avenue to fabricate the metals/SWCNT composites. Recently Tsai
et al. using permanent magnet samarium–cobalt (Sm–Co) chlo-
ride as a catalyst, successfully synthesized SWCNTs by arc dis-
charge method [19]. As we know, Sm is a kind of rare earth
elements whose unpaired 4f electrons are screened by the outer
layer electrons and the interaction between 4f electrons and the
surrounding environment is an indirect exchange interaction.
Unlike Fe, Co, Ni and other transition metals, rare earth elements
have very large structure anisotropy, good chemical activity, and
rich absorption spectrum characteristics. When they are com-
bined with Fe, Co, Ni, etc. elements, they would form binary
compounds or ternary compounds and exhibit a very good ferro-
magnetism, large saturation magnetization, magnetic anisotropy
and magnetostriction. These characteristics of rare earth ele-
ments can be used to adjust and optimize the electromagnetic
parameters of the materials, so as to improve the material
absorbing properties.
To our best of knowledge, though it has been reported that add-
ing a small amount of rare earth elements in ferrite can improve
the composites’ microwave absorbing properties [20–24], the
microwave absorbing properties of SWCNTs attached with rare
earth elements have rarely been studied. In this paper, we utilized
the commercial Sm2Co17 powder as a catalyst to directly synthe-
size SmCo attached SWCNTs by hydrogen arc discharge method,

0925-8388/$ - see front matter Ó 2013 Elsevier B.V. All rights reserved.
http://dx.doi.org/10.1016/j.jallcom.2013.03.286
124 L. Yu et al. / Journal of Alloys and Compounds 575 (2013) 123–127

and investigated the electromagnetic properties of the composites

in the frequency range of 2–18 GHz.

2. Experimental procedures

2.1. Sample manufacturing

SmCo attached SWCNTs were prepared by hydrogen dc arc discharge method

[25] using commercial 2:17 type SmCo permanent powder (Shanghai Jieling mag-
netic device Co., Ltd. and the grain size is about 1 lm) as catalyst. Briefly, a cathode
and an anode were horizontally installed in the center of a homemade water-cooled
stainless steel chamber. The cathode was a pure carbon rod (10 mm in diameter,
30 mm long), and the catalyst-doped carbon anodes were prepared as follows.
The mixture of graphite powder with homogenously doped Sm2Co17 catalyst
(1 wt%, 2 wt% and 4 wt%) was ball milled about 24 h, then the mixture were shaped
into a rod by isostatic pressing (10 mm in diameter, 60 mm long). Afterwards, the
rods were heated to 1100 °C in N2 atmosphere for 3 h to remove tar oil and other
impurities and then cooled down naturally. A dc arc discharge was generated by
applying 120 A current in hybrid H2–Ar atmosphere (2:3/v:v) at a total pressure
of 400 Torr. During arc discharge, the distance between two electrodes was main-
tained constant (about 1–2 mm) by a step motor. The typical synthesis time was
9 min, and the as-grown SmCo attached SWCNTs were collected with tweezers
after arc evaporation. Three SmCo attached SWCNTs powder samples were synthe-
sized and labeled Y1, Y2, and Y3 corresponding to the different catalyst loadings of
1 wt%, 2 wt% and 4 wt%, respectively.
A commercially available epoxy resin (1601 type, Shanghai Sinopharm Group
Co., Ltd.) and the curing agent (593 type, Shanghai Sinopharm Group Co., Ltd.) were
mixed with resin/curing agent mass ratio of 3:1. Then the mixture was poured into
a suitable mold to form ring samples (£3.05 mm (inner), and £7.00 mm (outer)).
Then the prepared samples were labeled S0, S1, S2 and S3 corresponding to doping
0.5 wt%, 1 wt %, 2 wt% and 3 wt% SmCo attached SWCNTs, respectively.

2.2. Characterization and measurement

The raw 2:17 type SmCo permanent powder was characterized by X-ray
diffraction (XRD) pattern (Rigaku Corporation DLMAX-2200), vibrating sample
magnetometer (VSM, LakeShore 7407) and energy dispersive spectroscopy ana-
lyzer. The structures of as-grown SmCo attached SWCNTs powder were examined
by Raman analysis with an excitation power of 10 mW at 633 nm (Renishaw, Invia
plus). Morphological observations of the samples were performed using a field
emission scanning electron microscope (FE-SEM, JEOL JSM-6700F) equipped with
an energy dispersive spectroscopy analyzer (EDS, Oxford Inca) and high-resolution
transmission electron microscopy (HRTEM, JEOL JEM-2010F).
The electromagnetic parameter and the microwave absorbing properties of all
samples were calculated by the S parameters measured by the HPE8363B vector
network analyzer using the coaxial method in the frequency range of 2–18 GHz.
The reflection loss (RL) was simulated by computer based on Nicolson Ross Weir
(NRW) algorithm [26,27] with the following formula:
 
Z in  1
RL ¼ 20 lg   ð1Þ
Z in þ 1
rffiffiffiffiffi  
lr 2pfd pffiffiffiffiffiffiffiffiffi
Z in ¼ tan h j lr er ð2Þ
er c
where the RL denotes the reflection loss in decibel unit, f is the electromagnetic wave
frequency, d is the thickness of an absorber and c is the velocity of light.
3. Results and discussion
3.1. Raw Sm2Co17 material characterization
Fig. 1a shows the XRD pattern of the raw Sm2Co17 material,
according to the reference JCPDS Card No. 19-0359, the diffraction
peaks of 2h = 28.7°, 30.7°, 31.9°, 33.4°, 37°, 38.8°, 43.1°, 43.5°, 44.3°
and 44.7° are corresponding to Sm2Co17 crystal indexes of [2 0 2],
[1 1 3], [1 0 4], [2 1 1], [3 0 0], [0 1 5], [2 2 0], [3 0 3], [2 1 4] and [2 0 5]
respectively. The lattice structure of the raw material is a rhombo-
hedral Th2Zn17-type (2:17 R) crystal structure and is basically con-
sistent with the literatures [28–31]. The EDS analysis indicates
that, as a commercial powder, there is also some Fe, Zr, Cu ele-
ments exist, but the amounts are so small and hard to characterize.
Fig. 1b is the hysteresis loop of Sm2Co17 at room temperature un-
der the magnetic field of 20,000 Oe. The coercive force (Hc), the
saturation magnetization (Bs) and the residual magnetization
Fig. 1. Characterizations of 2:17 type Sm–Co permanent magnet: (a) XRD pattern;
(b) hysteresis loop.
(Br) are 1253.4 Oe, 84.9 emu/g and 23.9 emu/g, respectively. This
is a typical hysteresis loop of the permanent magnetic powder.
3.2. The structure and magnetism characterization
Fig. 2 is the Raman spectra and hysteresis loop of the as-grown
SmCo attached SWCNTs powder. In Fig. 2a, the peaks in the range
of 100–400 cm1 are generally called RBM peaks and the next two
peaks are D band, G band respectively. The Raman spectrum has
been normalized to the intensity of the G band. The RBM peak in
the Raman spectra is a unique feature of SWCNTs which provides
information when the carbon atoms in SWCNTs vibrate in the ra-
dial direction [32]. Using the relation between the diameter d
(nm) and the RBM peak frequency x (cm1): d = 224/(x  10),
the calculated results indicate that the diameters of the SWCNTs
are in the range 1.3–2.1 nm. The ratio of D band and G band inten-
sity (ID/IG) represents the defects or crystallinity of the SWCNTs.
The smaller the ratio of ID to IG, the better the cryallinity of the
SWCNTs is. In Fig. 2a, the ratios of the peak intensity ID/IG of the
as-grown sample Y1, Y2 and Y3 are about 0.17, 0.20 and 0.06
respectively, which demonstrates that the SWCNTs in the experi-
ment have good crystallinity and purity.
Fig. 2b shows the hysteresis loop of the as-grown SmCo at-
tached SWCNTs powder prepared with 4 wt% catalyst (Y3) at room
temperature. The coercive force, remanence, and saturation mag-
netization are 112.5 Oe, 2.2 emu/g and 16.1 emu/g, respectively.
As we know that the hysteresis loop area indicates the magnitude
of the magnetic hysteresis loss. From Fig. 2b, it can be seen that the
hysteresis loop area is comparatively large compared with refer-
ence papers [33], which indicates that the SmCo attached SWCNTs
powder has a larger magnetic hysteresis loss.
 L. Yu et al. / Journal of Alloys and Compounds 575 (2013) 123–127 125

Fig. 2. Characterization of as-grown SmCo attached SWCNTs: (a) Raman spectra for Fig. 3. Morphology and microstructure of as-grown sample Y3: (a) TEM image; (b)
sample Y1, Y2, Y3; (b) Hysteresis loop of for sample Y3. SEM image.

3.3. Morphology analysis

The TEM and SEM images of the as-grown SmCo attached

SWCNTs sample prepared with 4 wt% catalyst are shown in
Fig. 3. It can be seen that due to the van de Waals interaction,
SWCNTs are entangled into bundles in Fig. 3a. And from Fig. 3b,
we can clearly see that the SmCo nanoparticles are uniformly at-
tached on the SWCNTs surface. According to the EDS analysis, it
can be inferred that the particles attached on SWCNTs are SmCo
and SmFe compound.
The Fig. 4 is the HRTEM image of the SmCo attached SWCNT/
epoxy composite (sample S1). The picture shows that the diameter
of SWCNT is about 2 nm, the size of the particle is about 10 nm and
the SmCo attached SWCNTs are dispersed homogeneously in
epoxy. It proved that the SmCo attached SWCNTs doped in the
composite have formed a network structure.

3.4. Electromagnetic parameter analysis Fig. 4. HRTEM image of the SmCo attached SWCNT/epoxy composite (S1 sample).

Fig. 5 shows the frequency dependence of two basic electro-

magnetic parameters e and l of SmCo attached SWCNT/epoxy
composites measured in the frequency range of 2–18 GHz. As it
is known, the permittivity and permeability can be expressed as:
e = e0  je00 and l = l0  jl00 . the real part of complex permittivity
(e0 ) stands for the electric field energy storage capacity of compos-
ites and the imaginary part of complex permittivity (e00 ) represents
the ability of dielectric loss, while the real part (l0 ) and the imag-
inary part (l00 ) of the complex permeability signify the magnetic
field energy storage and magnetic loss ability of the composites,
respectively.
It can be seen that the values of real parts of (shown in Fig. 5a)
the complex permittivity of all samples are in the range from 1 to
4.5 and decrease when the frequency increase. The imaginary parts
of permittivity (shown in Fig. 5b) of different samples increased
with the frequency. The real part of the complex permittivity of
sample S3 shows a peak around 17 GHz, while the imaginary part
of S3 also has a resonance phenomenon at nearly the same fre-
quency. The imaginary part of permittivity of the S3 sample is neg-
ative in the beginning frequency which means the sample have no
dielectric loss. The real parts of the magnetic permeability of all the
126 L. Yu et al. / Journal of Alloys and Compounds 575 (2013) 123–127

Fig. 5. Electromagnetic parameters of the composites in the frequency range of 2–18 GHz: (a) real part of the complex permittivity, (b) imaginary part of the complex
permittivity, (c) real part of the complex permeability and (d) imaginary part of the complex permeability.

samples (shown in Fig. 5c) show obvious differences in the high

frequencies (8–18 GHz), nevertheless have not much differences
in the low frequencies (2–8 GHz). The values of the imaginary parts
of the magnetic permeability (shown in Fig. 5d) of all the samples
change from 0.1 to 1.3 with the frequency increase. The influence
of doping content is clear. When the doping content is 2 wt%, the
imaginary parts of the magnetic permeability has a maximum va-
lue. According to the electromagnetic wave theory, in order to
achieve the maximum large absorption, two requirements must
be satisfied by microwave absorbing materials [14]. The first one
is the impedance matching performance on the surface of the
materials. The second is the EM matching conditions of the mate-
rials. Generally, the electromagnetic parameter matching is diffi-
cult in practice. Comparing the real parts and imaginary parts of
the e and l of all composites changing with frequencies, we can
find that the values of two electromagnetic parameters (l, e) of
sample S1 are very close in the frequency range of 12–18 GHz. It
reveals that there will be a wideband matching condition in the
frequency range of 12–18 GHz (There e0  l0 , e00  l00 ). This indi-
cates that the S1 sample will have a good electromagnetic match-
ing performance in the frequency range of 12–18 GHz

3.5. Microwave absorbing property

Fig. 6 shows the frequency dependence of the reflection losses
for SmCo attached SWCNT/epoxy composites. As it can be seen
from Fig. 6a, the four composite samples all have very good reflec-
tion loss. There are two absorption peaks for S1. One is at 13.4 GHz
with a peak value 23.5 dB and the other is at 16.9 GHz with a
peak value 23.7 dB. The reflection loss peak of S2 shifted to the
lower frequency (10.5 GHz) and increased slightly (23.4 dB) com-
pared to sample S1, while the absorption peak of S3 (24.5 dB)
moved to 12.8 GHz. The bandwidths of S0, S1, S2 and S3 decline
with increasing doping content. S2 has the widest bandwidth
Fig. 6. Frequency dependence of the reflection losses for SmCo attached SWCNT/
epoxy composites: (a) for S0, S1, S2, S3 at 3.3 mm thickness and (b) for different
thickness of S1.
(11.2 GHz) at the reflection loss below 10 dB (90% absorption).
The bandwidths where the reflection loss is below 15 dB for S0,
S1, S2 and S3 are 5.4, 7.6, 5.8 and 3.6 GHz, respectively. The band-
widths where the reflection loss is less than 20 dB for S0, S1, S2
and S3 are 1.3, 6.2, 2.7 and 2 GHz, respectively. Therefore, we can
 L. Yu et al. / Journal of Alloys and Compounds 575 (2013) 123–127
conclude that adding more SmCo attached SWCNTs in epoxy can
strengthen reflection loss, but the bandwidth would become nar-
rower. The optimal adding amount of SmCo attached SWCNTs in
epoxy is 1 wt%. The bandwidths where the reflection loss is less
than 20 dB can reach more than 6 GHz. This fact is consistent
with the above electromagnetic parameter analysis results.
The relations between the reflection loss and the thickness of
sample S1 are shown in Fig. 6b. There are two microwave absorp-
tion peaks for different thickness of sample S1. When the thickness
is at 3.1 mm, the relative high frequency absorption peak is small;
when the thickness increasing from 3.1 to 3.5 mm, the relative low
frequency absorption peak is obviously increased, and shifted to
lower frequency. That is to say, the microwave absorbing proper-
ties of SmCo attached SWCNT/epoxy composites are sensitive to
the sample thickness; only 0.2 mm changes in thickness will have
a great impact on the microwave absorbing properties of the
material.
3.6. Microwave absorbing mechanism
As discussed above, the excellent microwave absorption prop-
erty of SmCo attached SWCNT/epoxy composites can be ascribed
to the following reasons: (1) Samarium has electron configuration
of 4f66s2 and has good chemical activity. It is easy to combine with
other metal or non-metal elements forming alloy or intermetallic
compounds. (2) Samarium combined with the metal cobalt to form
samarium–cobalt alloy. SmCo alloy has large anisotropy and is
among the strongest magnets known. When SmCo nano-magnetic
particles attached on SWCNTs, not only does it introduce a suitable
magnetic hysteresis loss, natural resonance and exchange reso-
nance, but it also greatly improves dielectric and magnetic param-
eter matching of the composites so as to enhance the microwave
absorption performance of the composites. (3) Many suspending
bonds on the SWCNTs, and many defects on SmCo attached
SWCNTs can cause interfacial electric polarization. The metallic
SWCNTs can generate an inductive current in the electromagnetic
field, and then cause a lossy current and energy dissipation [11].
(4) According to the Kubo theory, the quantum confine effect
makes the energy levels in the SmCo attached SWCNTs discontin-
uous and if one energy level is in the range of microwave energy
band, the electron will absorb a photon to hop from a low energy
level to a higher one [12], which means the nano-SmCo particles
will increase the microwave absorption [33]. (5) The efficient com-
bination of epoxy matrix and SmCo attached SWCNTs (suitable
doping quantities and composites’ thickness) will form a multiple
scattering network, which improves the microwave absorption
properties. Therefore, combining all the effects together, the result-
ing microwave absorption properties of the composites are
excellent.
4. Conclusion
In summary, the SmCo attached SWCNTs can be prepared in one
step via arc discharge method using 2:17 type SmCo permanent
powder as catalyst. The SmCo attached SWCNT/epoxy composites
manufacturing is quite simple and speedy. The results of the elec-
tromagnetic parameters analysis and the reflection loss simulation
indicate that the SmCo attached SWCNTs is a good dopant, the
microwave absorbing properties of SmCo attached SWCNT/epoxy
composites are sensitive to the sample thickness. There is a wide-
band matching condition in the frequency range of 12–18 GHz
(There e0  l0 , e00  l00 ) for S1 sample. With a small amount of SmCo
attached SWCNTs (1 wt%) doping, through adjusting the thickness
127
of the composites (3.3 mm), the S1 sample has a reflection loss
peak value 23.7 dB, and the bandwidths less than 20 dB can
reach more than 6 GHz. The unique microwave absorbing proper-
ties of the composites can be mainly ascribed to the wideband
electromagnetic matching, the interfacial electric polarization
and the multiple scattering network structure. It is expected that
the new SmCo attached SWCNT/epoxy composites will be a good
candidate for the microwave absorbing materials in X band
(8–12 GHz), Ku band (12–18 GHz), or even K band (18–27 GHz).
Acknowledgments
This work is supported by the National Natural Science Founda-
tion of China (Nos. 51202137 and 61240054). Acknowledgments
are also made to the Instrumental Analysis and Research Center
of Shanghai University. Special thanks are given to Professor Jian-
chao Peng and Professor Yuliang Chu for their help in HRTEM
and SEM testing.
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