Composites Science and Technology 159 (2018) 240e250

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Composites Science and Technology

journal homepage: http://www.elsevier.com/locate/compscitech

Multifunctional BiFeO3 composites: Absorption attenuation

dominated effective electromagnetic interference shielding and
electromagnetic absorption induced by multiple dielectric and
magnetic relaxations
Yong Li a, Ningning Sun a, Jia Liu c, Xihong Hao a, *, Jinhua Du a, Huijing Yang b, ***,
Xiaowei Li a, Maosheng Cao c, **
a
Inner Mongolia Key Laboratory of Ferroelectric-related New Energy Materials and Devices, School of Materials and Metallurgy, Inner Mongolia University
of Science and Technology, Baotou, 014010, China
b
Department of Physics, Tangshan Normal University, Tangshan, 063000, China
c
School of Material Science and Engineering, Beijing Institute of Technology, Beijing, 100081, China

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

Article history: BiFeO3 (BFO) grains prepared by molten salt method were fabricated in paraffin wax based composite
Received 24 November 2017 structure to evaluate electromagnetic interference (EMI) shielding and electromagnetic (EM) absorption
Received in revised form in 2e18 GHz. In the composites, BFO750 paraffin wax composite exhibits excellent EMI shielding and EM
16 January 2018
absorption performance. The EMI shielding effectiveness of BFO750 paraffin wax composite surpasses
Accepted 10 February 2018
10 dB, and its reflection loss shows three absorption peaks which reach
17 dB. The absorption efficiency
Available online 6 March 2018
and attenuation constant are close to 80% and 70, respectively. The results demonstrate that absorption
attenuation is the dominant mechanism of EMI shielding and EM absorption. This is attributed to
Keywords:
BiFeO3
multiple dielectric and magnetic relaxations, where electric and magnetic dipoles coexisting in the
Multifunction composite can respond intensively to electromagnetic wave in the frequency range and thus cause high
Electromagnetic interference shielding electromagnetic loss. The work highlights BFO composites as promising multifunctional materials in
Electromagnetic absorption electromagnetic wave protection fields.
Relaxation © 2018 Elsevier Ltd. All rights reserved.

1. Introduction electromagnetic fields in the radiation. It is thus clear that the

The electromagnetic interference (EMI) shielding and electro-
magnetic (EM) absorption materials have attracted great attention
due to their crucial role in blocking undesirable electromagnetic
wave irradiation from the electronic devices and communication
apparatus [1e12]. Generally, EMI shielding and EM absorption
involve the mechanisms: reflection and absorption attention which
includes absorption and multiple reflection [13e16]. The primary
mechanism of EMI shielding is usually reflection [14,17]. For
reflection of electromagnetic wave irradiation by the shield, the
shield must have mobile charge carriers which interact with the
* Corresponding author.
** Corresponding author.
*** Corresponding author.
E-mail addresses: xhhao@imust.cn (X. Hao), yanghj619@126.com (H. Yang),
caomaosheng@bit.edu.cn (M. Cao).
materials as the shield tend to be electrically conducting [18]. For
example, metals and carbon materials are good materials for EMI
shielding [19e22]. However, the using of conductive materials
based on reflection mechanism may cause potential secondary
pollution of electromagnetic wave [23]. EM absorption is mainly
caused by absorption attention. Impedance matching is a crucial
factor to enhance absorption for electromagnetic wave, which
require a low conductivity for materials. Therefore, the EMI
shielding materials with high electrical conduction are not used in
EM absorption fields due to weak absorption capacity. For complex
dynamic environment and various-field applications, it is desirous
to search for multifunctional materials that possess effective EMI
shielding and EM absorption simultaneously. Unfortunately, the
studies for the field have been rarely reported.
To achieve the multifunctionality, materials should have more
intense absorption attention for electromagnetic wave. Therefore,
the materials should possess electric and/or magnetic dipoles

https://doi.org/10.1016/j.compscitech.2018.02.014
0266-3538/© 2018 Elsevier Ltd. All rights reserved.
 Y. Li et al. / Composites Science and Technology 159 (2018) 240e250 241

which interact with the electromagnetic fields. In addition, it is also
desired for the presence of a large surface area or interface area in
the materials, which cause multiple reflection [15]. Therefore, a
material that meets these conditions may be a candidate as a
multifunctional electromagnetic protection material.
BiFeO3 (BFO) is a classic multiferroic material with electric and
magnetic orderings at room temperature [24,25]. Based on our pre-
vious studies, BFO possesses intrinsic polarization, defect dipole
polarization and ferromagnetic resonance which induce dielectric
loss and magnetic loss, leading to strong attenuation for electro-
magnetic wave at X-band [26,27]. Reshi et al. reported that BFO
nanomaterials with electric and magnetic dipoles can perform as an
EMI shielding material at X-band [28]. These studies reveal that BFO
with peculiar physical characteristics may achieve a balance between
EMI shielding and EM absorption, which is a potential material for
the multifunctional application. However, the combined study and
comprehensive evaluation on EMI shielding and EM absorption of
BFO have not been carried out, particularly in a wider frequency
range (including S, C, X and Ku band). In addition, by material design,
BFO grains as discontiguous medium can be dispersed in the matrix
materials. The strategy can help to form multiple reflection of elec-
tromagnetic wave among BFO grains. Here, BFO paraffin wax com-
posites were fabricated, and their performances of EMI shielding and
EM absorption were investigated at 2e18 GHz. The related mecha-
nisms for EMI shielding and EM absorption based on structure and
electromagnetic properties were discussed.

Fig. 1. (a) XRD patterns of the BFO samples sintered at different temperature and SEM images: (b) the BFO700, (c) BFO750, (d) BFO800 and (e) EDS of the BFO750.
242 Y. Li et al. / Composites Science and Technology 159 (2018) 240e250
2. Experiment
BFO was prepared by molten salt method. Stoichiometric
amount of Bi2O3 (99%) and Fe2O3 (99%) were milled in alcohol for
24 h. The mixture was dried at 80  C for 12 h. The dried powders
and NaCl (1:1 in weight ration) were mixed in a mortar for 30 min.
Then they were sintered at 700  C, 750  C, 800  C and 830  C for
30min, respectively. The resultants were washed by distilled water
until no precipitate was detected by AgNO3 solution. The powders
were dried at 80  C for 24 h. The obtained samples with different
sintering temperature were abbreviated as BFO700, BFO750,
BFO800 and BFO830.
BFO700, BFO750 and BFO800 paraffin wax composites (abbre-
viation: BFO700-PW, BFO750-PW and BFO800-PW) were prepared
by ultrasound mixing method. BFO (80 wt%) and paraffin wax
(20 wt%) were added into pre-heated ether solution at 70  C. BFO
was dispersed in wax by ultrasound. After the ether was completely
evaporated, the mixture was cooled to room temperature. A portion
of the resulting mixture was pressed into toroidal shape
Fig. 2. High-resolution XPS spectra of (a-c) Fe 2p and (d-f) O 1s core levels for the BFO samples.
(Fout ¼ 7.03 mm; Fin ¼ 3.00 mm).
The phase structure of BFO was measured by X-ray diffraction
(XRD, Bruker, D8 Advanced Diffractometer). The morphology of
BFO and the composites were examined by using a field-emission
scanning electron microscopy (FE-SEM, Zeiss, Supra 55). The
oxidation state of elements was confirmed by using a X-ray
photoelectron spectroscopy (XPS, Thermo Scientific, Escalab 250
XI). The relative S parameters, complex permittivity and complex
permeability were measured on vector network analyzer (VNA,
Anritsu 37269D) by the coaxial method.
3. Results and discussion
3.1. Structure and morphology
The XRD patterns of the BFO samples with different sintering
temperature are shown in Fig. 1a. The main peaks of BFO700 are
identified by the structure of BFO (PDF#71-2494), which exhibits
rhombohedral perovskite structure [29]. However, a little impurity
 Y. Li et al. / Composites Science and Technology 159 (2018) 240e250
Fig. 3. (a,b)SEM images and (c,d) element maps of the BFO750-PW.
phase is observed which may be Bi25FeO40. As the sintering tem-
perature increases, the impurity phase disappears. BFO750 shows
single rhombohedral structure. When the sintering temperature is
800  C, a little amount of impurity phase appears in BFO800 again.
The sample sintered at 830  C has an obvious mixed phase struc-
ture which consists of BFO, Bi25FeO40 and Bi2Fe4O9 (Fig. S1), and the
main reason for formation of impurity phase is that a lot of bismuth
volatilizes around the Curie temperature of BFO. Therefore,
BFO700, BFO750 and BFO800 are chosen as the materials investi-
gated in this study. Fig. 1bed shows the SEM images of the BFO
samples. It is observed that the grains of the BFO samples show
random shapes. The size of the grains is in submicron or micro-
meter scale, and it increases with the increase of the sintering
temperature. The EDS of BFO750 demonstrates that it just consists
of Bi, Fe and O elements (Fig. 1e).
The elemental components of BFO750 are identified by XPS
spectrum (Fig. S2). BFO750 is completely composed of Bi, Fe and O
elements. No other elemental signals are detected. The ionic
valence is identified by the high-resolution XPS spectra in Fig. 2.
Fig. 2aec shows the XPS spectra of Fe 2p for the BFO samples. The
dominant Fe 2p peaks are at around 710.6 eV and 724.3 eV binding,
respectively [8]. The splitting of Fe 2p is 13.7 eV, which obviously
arises from Fe3þ. Two high-binding energy shoulders are present at
717.8 eV and 731.6 eV, indicating that Fe2þ exists in these three BFO
samples [30]. The percentage of Fe2þ in BFO750 is significantly
lower than that of the other two BFO samples. The XPS spectra of O
1s are shown in Fig. 2def. Three peaks appear in the spectra. The
main peak at 529.4 eV corresponds to the cation-oxygen bonds. The
higher-energy peaks at 532.4 eV and 531.6 eV are assigned to
243
adsorbed surface H2O as well as the presence of oxygen vacancies,
respectively [31]. Similarly, the concentration of oxygen vacancies
of BFO750 is the lowest among these three BFO samples. It is known
that oxygen vacancies and Fe2þ appear simultaneously for charges
compensation in BFO [32]. The results illustrate a fact that appro-
priate sintering temperature can suppress the forming of anion
vacancies in BFO, which is favorable to decreasing the leakage
current of BFO. The result is confirmed by the current density of the
BFO samples (Fig. S3).
The paraffin wax-based composites were fabricated via com-
pressing at room temperature. Fig. 3a,b show the SEM images of
BFO750-PW. It is found that the BFO grains were dispersed evenly
in paraffin wax. In addition, the element maps of Fe from BFO and C
from paraffin wax are shown in Fig. 3c,d. Fe element and C element
display homogeneous distribution in the measured region, indi-
cating that the BFO grains and wax are mixed uniformly.
3.2. EMI shielding
EMI shielding effectiveness (SETot) refers to the logarithm of the
ratio of the incident wave PI to the transmitted wave PT [33],
SETot ¼ 10 logðPI =PT Þ (1)
The SETot consists of the reflection (SER) and absorption (SEA),
involving the contribution of multiple-reflections. The SER and SEA
can be achieved by the equations [34,35]:
244 Y. Li et al. / Composites Science and Technology 159 (2018) 240e250

Fig. 4. (a) Total EMI SE, (b) reflection, (c) absorption effectiveness and (d) the comparing of the properties of the BFO paraffin wax composites.

SER ¼
10 logð1
RÞ (2) R ¼ jS11 j2 (4)

SEA ¼
10 log½T=ð1
RÞ (3) T ¼ jS21 j2 (5)

where R is reflection coefficient. Fig. 4 shows the EMI ES perfor-
mance of the composites. It is observed that the EMI ES shows
obvious frequency dependence. The SETot of BFO750-PW is bigger
than that of BFO700-PW and BFO800-PW in the entire frequency
range, and the maximum value of the SETot surpasses 10 dB,
exhibiting an efficient EMI shielding. In Fig. 4b, the SER of BFO700-
PW is the highest among these three composites. For the SEA, the
value of BFO750-PW is obviously higher compared with that of
BFO700-PW and BFO800-PW (Fig. 4c). In the measurement fre-
quency range, the proportion of the SEA in the SETot exceeds 50% for
BFO750-PW. The comparison of the EMI ES performance for these
three composites at 10 GHz is shown in Fig. 5d. It can be directly
found that BFO750-PW has the highest SETot, and the SETot is mainly
from the contribution of the SEA.
To verify further contribution of reflection and absorption to the
shielding of the BFO paraffin wax composites, the EMI power data is
analyzed. The EMI power coefficients including reflection coeffi-
cient (R), transmission coefficient (T) and absorption coefficient (A)
are determined by S parameters (S11 and S21), which are calculated
by the equations [33,36,37]:
A¼1
R
T (6)
The R, T and A of the BFO paraffin wax composites in 2e18 GHz
are shown in Fig. 5aec. BFO750-PW has the largest A among these
three composites, and the R and T are smaller compared with the
other composites. Fig. 5d shows the average value of EMI power in
2e18 GHz. For BFO750-PW, the amount of energy blocked by ab-
sorption is higher than that blocked by reflection.
3.3. EM absorption
The EM absorption is another issue for electromagnetic atten-
uation, which is evaluated based on the complex permittivity and
permeability [38]. The reflection loss (RL) of single absorb layer can
be calculated as follow [39e41]:
jZin
1j
RL ¼ 20 log (7)
jZin þ 1j
Here the normalized input impedance Zin of the electromagnetic
 Y. Li et al. / Composites Science and Technology 159 (2018) 240e250
Fig. 5. (a) EMI reflection coefficient, (b) transmission coefficient, (c) absorption coefficient and (d) their average value of BFO paraffin wax composites.
attenuation layer is given by
 
pffiffiffiffiffiffiffiffiffiffiffi 2pfd pffiffiffiffiffiffiffiffiffi
Zin ¼ mr =εr tanh j mr εr
c
Where c is the light velocity, f is the electromagnetic wave fre-
quency, d is the thickness of the absorber, and mr and εr are the
relative permeability and permittivity of the composite medium,
respectively. The RL of these three composites with different
thickness of absorption layer is shown in Fig. 6. Compared with
BFO700-PW and BFO800-PW, BFO750-PW has larger attenuation
capability, and its maximum RL reaches up to
22.5 dB at d ¼ 4 mm,
which is larger than that of other BFO samples prepared by sol-gel
method (
11 dB) and solid solution method (
17 dB) [42,43].
Furthermore, it is observed that the composites have three ab-
sorption peaks located in around 2e8 GHz, 8e13 GHz and
13e18 GHz respectively. Particularly, all the three absorption peaks
of BFO750-PW exceed
17 dB at d ¼ 8 mm, which represents high-
efficiency multiple absorption. In order to understand the multiple
absorption behavior, the mode based on quarter-wavelength
attenuation is presented in Fig. 7. According to electromagnetic
wave theory, the electromagnetic wave absorption occurs in the
neighboring positions of d/lD ¼ 1/4, 3/4, 5/4, 7/4 …, where d is the
thickness of the absorber, lD ¼ l/n is the wavelength in a dielectric,
l is the wavelength in a vacuum and n is the refractive index of
245
materials [44]. In Fig. 7, it is observed that the frequency of these
three absorption peaks is consistent with that of d/lD ¼ 1/4, 3/4, 5/
4. This result demonstrates that the multiple absorption is from the
(8) contribution of quarter-wavelength attenuation.
3.4. Discussion
Generally, the mechanisms of EMI shielding and EM absorption
are reflection and absorption attenuation which includes absorp-
tion and multiple reflection caused by dipoles and interfaces
respectively. For the BFO paraffin wax composites, according to the
results of EMI shielding and EM absorption, it is obvious that part of
the electromagnetic wave is dissipated by absorption attenuation.
Particularly, for BFO750-PW, absorption attenuation is the main
contribution. To investigate the origin of absorption attenuation,
the electromagnetic properties of the composites are measured.
Fig. 8 shows the complex permittivity (ε0 - jε00 ) and complex
permeability (m0 - jm00 ) of the composites in the frequency range of
2e18 GHz. Among these three composites, the BFO750-PW has the
biggest ε0 and ε00 (Fig. 8a,b). Moreover, the polarization contribution
and conductance contribution to dielectric properties can be
explicated by the Debye theory. The ε00 is shown as follow [13]:
246 Y. Li et al. / Composites Science and Technology 159 (2018) 240e250
Fig. 6. The reflection loss of (a) BFO700-PW, (b) BFO750-PW, (c) BFO800-PW and (d) the compare of the reflection loss at d ¼ 8mm.
00 εs
ε∞ s for electromagnetic wave consequently.
ε ¼ ut þ
1 þ u2 t 2 ε0 u
where s is the electrical conductivity, ε0 the vacuum permittivity.
Based on the electrical conductivity, the conduction part (εc00 ) and
the polarization part (εp00 ) of imaginary permittivity are obtained,
as shown in Fig. S4. The εc00 is much smaller than the εp00 . Therefore,
the main contribution to the ε00 of the composites is polarization
rather than conductance. It is found that three dielectric relaxation
peaks exist in the ε00 for the composites, presenting dielectric multi-
relaxation behavior. It is suggested that these three relaxations
should be induced by different polarization modes from various
electric dipoles. Based on frequency response of dipoles, it is pro-
posed that the two relaxations at low frequency may be induced by
intrinsic and defect polarization from the lone pair of Bi ions and
oxygen vacancies respectively, and the relaxations at high fre-
quency may be caused by the polarization from the charges of BFO/
wax interfaces.
Fig. 8c,d shows the m0 and m00 of the composites. For different
composites, the m0 just changes slightly. Compared with the other
two composites, the BFO750-PW has a bigger m00 in the frequency
range. The eddy current coefficients m''(m0 )
2f
1 of the composites
change with the increase of frequency. This indicates that the
magnetic loss is not caused by eddy current loss (Fig. S5) [45],
implying that conductance contribution to magnetic loss is negli-
gible. Interestingly, the m00 possesses similar multi-relaxation
behavior. Three relaxation peaks locate in different frequencies,
which may be caused by domain wall resonance, natural resonance
and exchange resonance. Therefore, various electric dipoles and
magnetic dipoles coexisting in the composites have multiple
responses to electromagnetic wave of 2e18 GHz, which causes loss
(9)
In spite of the existing of electric dipoles and magnetic dipoles, it
does not mean that the composites possess strong attenuation for
electromagnetic wave. The intensity of attenuation depends on
magnitude of loss and electromagnetic matching level. Fig. 9 shows
the dielectric loss (tande) and magnetic loss (tandm) of the BFO
paraffin wax composites. The composites show a relative balance
between the tande and tandm. This indicates that the BFO paraffin
wax composite possesses high level in electromagnetic matching
[46]. However, the values of tande and tandm for BFO750-PW are
higher than those of BFO700-PW and BFO800-PW. This result
represents that electric dipoles and magnetic dipoles of BFO750-
PW have strong response to electromagnetic wave, leading to a
bigger absorption attenuation.
It is known that the attenuation contribution of EMI power and
EM absorption can be expressed by absorption efficiency (AE) and
attenuation constant (a) [47,48]:
AEð%Þ ¼ A=ð1
RÞ (10)
pffiffiffi sffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffi
rffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffi ffi
2pf  
a¼ m00 ε00
m0 ε0 þ m0 2 þ m00 2 ε0 2 þ ε00 2 (11)
c
Based on the AE curves in Fig. 10a, the AE of BFO750-PW is
higher than that of BFO700-PW and BFO800-PW, where the
maximum value is close to 80%. In addition, BFO750-PW has the
largest a among the composites (Fig. 10b). Fig. 10c shows the
reflection and absorption attenuation situation of electromagnetic
wave when it transmits from medium to BFO paraffin wax
 Y. Li et al. / Composites Science and Technology 159 (2018) 240e250
Fig. 7. (a) The reflection loss and (b) the frequency dependence of d/lD for the BFO paraffin wax composites at d ¼ 8mm.
composites. When incident wave arrives at the surface of the
composites, a part of electromagnetic wave will be reflected off the
surface and enter medium again. The other part of electromagnetic
wave will be into the composites. In this part, some can be absorbed
by BFO grains while the others will pass through the composites.
From the results of the AE and a, it is confirmed that a little amount
of electromagnetic wave is reflected for BFO750-PW, indicating that
reflection has less contribution which absorption is the dominant
contribution. This is mainly attributed to the tiny conductance
contribution to the electromagnetic parameters of BFO750-PW,
which leads to most of electromagnetic wave enter the composite.
More crucially, according to the electromagnetic properties, a large
amount of electric dipoles and magnetic dipoles coexist in BFO750-
PW. They intensively interact with electromagnetic wave in the
frequency range and thus cause the strong attenuation (Fig. 10d). In
addition, in the BFO paraffin wax composites, BFO grains are
dispersed in wax matrix uniformity, with the result that part of
247
electromagnetic wave may have multiple reflections behavior,
where electromagnetic wave is reflected multiply among surfaces
of BFO grains and is absorbed gradually. Based on the discussion, it
is demonstrated that absorption attenuation is the dominant
mechanism for BFO750-PW.
4. Conclusion
BFO paraffin wax composites show effective EMI shielding and
EM absorption. The investigation on the EMI shielding and EM
absorption properties indicates that absorption attenuation is the
dominant mechanism. It is attributed to both of multiple dielectric
and magnetic relaxation based on the electromagnetic properties.
Particularly, BFO750-PW exhibits enhanced EMI shielding and EM
absorption properties. Its EMI shielding effectiveness surpasses
10 dB. The reflection loss shows multiple absorptions behavior with
three absorption peaks due to the contribution of quarter-
248 Y. Li et al. / Composites Science and Technology 159 (2018) 240e250

Fig. 8. The complex permittivity and permeability of the BFO paraffin wax composites.

Fig. 9. The dielectric loss and magnetic loss of the BFO paraffin wax composites.
 Y. Li et al. / Composites Science and Technology 159 (2018) 240e250
Fig. 10. (a) Absorption efficiency, (b) attenuation constant of BFO paraffin wax composites, (c) Schematic illustration of reflection, absorption for electromagnetic wave through BFO
paraffin wax composites, (d) the comparing of EMI shielding and EM absorption in the composites.
wavelength attenuation, and all of three absorption peaks
reach
17 dB at d ¼ 8 mm. BFO paraffin wax composites will
[3]
expand the applications of BFO as a multifunctional electromag-
netism materials in communications, imaging, signal and data
protection fields.
[4]
Acknowledgements
[5]
This research was supported by the Innovation Fund of Inner
Mongolia University of Science and Technology (2016QDL-B03, [6]
2016QDL-S01), the Natural Science Foundation of China (51702169,
11604237), the Natural Science Foundation of Inner Mongolia [7]
(2015JQ04, 2017BS0503), Natural Science Foundation of Hebei
Province (E2015105079), the Grassland Talent Plan of Inner
Mongolia Autonomous Region. [8]
Appendix A. Supplementary data
[9]
Supplementary data related to this article can be found at
https://doi.org/10.1016/j.compscitech.2018.02.014.
[10]
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