Journal of Elastomers

and Plastics
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Comparison of microwave absorbing properties of chloroprene rubber

composites containing carbon black and nickel/cobalt powder
Omar A Al-Hartomy, Ahmed Al-Ghamdi, Nikolay Dishovsky, Rossitsa Shtarkova, Vladimir
Iliev and Farid El-Tantawy
Journal of Elastomers and Plastics 2013 45: 471 originally published online 10 October
2012
DOI: 10.1177/0095244312457801
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Article

Comparison of
microwave absorbing
properties of
chloroprene rubber
composites containing
carbon black and
nickel/cobalt powder

Journal of Elastomers & Plastics

45(5) 471485
The Author(s) 2012
Reprints and permissions:
sagepub.co.uk/journalsPermissions.nav
DOI: 10.1177/0095244312457801
jep.sagepub.com

Omar A Al-Hartomy1,2, Ahmed Al-Ghamdi1,

Nikolay Dishovsky3, Rossitsa Shtarkova4,
Vladimir Iliev5 and Farid El-Tantawy6

Abstract
In this study, the influence of hybrid combination of fillers (carbon black in concentrations
from 0 to 100 phr and conducting nickel (Ni) or cobalt particles in concentration 10 phr
on the dielectric (dielectric permittivity and dielectric loss angle tangent)) and microwave (reflection coefficient, attenuation coefficient, and shielding effectiveness) properties of chloroprene rubber composites has been investigated in the wide frequency
range (112 GHz). The results achieved showed that the hybrid combination of Ni
powder and active furnace carbon black gives an opportunity of considerable increase in
the dielectric permittivity and also a possibility for its adjustment varying carbon black
content. The comparison in the behavior of prepared composites can be explained by
the differences in some characteristics of two metals and influence of these differences
on the real and imaginary parts of the complex dielectric permittivity and magnetic
permeability.
1

Department of Physics, Faculty of Science, King Abdulaziz University, Jeddah, Saudi Arabia
Department of Physics, Faculty of Science, University of Tabuk, Tabuk, Saudi Arabia
3
Department of Polymer Engineering, University of Chemical Technology and Metallurgy, Sofia, Bulgaria
4
Department of Chemistry, Technical University, Sofia, Bulgaria
5
Department of Wireless communications and broadcasting, College of Telecommunications and Posts, Sofia,
Bulgaria
6
Department of Physics, Faculty of Science, Suez Canal University, Ismailia, Egypt
2

Corresponding author:
Nikolay Dishovsky, Department of Polymer Engineering, University of Chemical Technology and Metallurgy,
8 Kl. Ohridski blvd., 1756 Sofia, Bulgaria.
Email: dishov@uctm.edu

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Journal of Elastomers & Plastics 45(5)

Keywords
Chloroprene rubber composites, carbon black, nickel/cobalt filler, dielectric properties,
microwave properties

Introduction
Rubbers as electrical insulators are transparent to electromagnetic radiation and thus do
not provide microwave absorption and electromagnetic interference shielding effectiveness (SE). Both microwave absorption and SE can be improved by the incorporation
of conductive fillers in a rubber matrix.1 Different rubber composites for electromagnetic
interference shielding and microwave applications have been reported and include nitrile
rubber,2 polychloroprene,3,4 silicone,57 polyurethane,8 butyl rubber,9,10 polysulfide
polymer,11 ethylene vinyl acetate (EVA),1215 EVA blended with natural rubber,15 and
EVA/ethylenepropyleneethylidenenorbornene blend.14 Depending on microwave
absorption and SE at different frequency ranges, these composites are considered as
absorbing materials in different microelectronic devices and microwave applications. The
most often used conductive fillers with high dielectric losses include carbon black,2,10,1216
short carbon fiber,24,1215 graphite particles,5,11 and boron carbide.9,16 On the other hand,
rubber composites containing fillers with high magnetic losses are also important for many
applications such as microwave absorbers or materials for electromagnetic wave shielding,
magnetic data storage media, magnetic field sensors, and so on.1719
Nickel (Ni) and cobalt (Co) are two of four elements that are ferromagnetic around the
room temperature (the other two being iron and gadolinium). Some metal oxides and ferrites
(FeOFe2O3, NiOFe2O3, CuOFe2O3, MgOFe2O3, barium, and strontium hexaferrites) are
also ferromagnetic. The necessity for developing absorbing composites with improved
effectiveness and wider frequency band is the reason for introduction of both fillers with
high dielectric and high magnetic losses in the rubber matrix. The development of chloroprene rubber (CR)-based composites containing combination of reinforcing active carbon
black and Ni or Co ferromagnetic powder is expected to broaden the application of this type
of composites. The aim of such a study is to prove that a hybrid combination of fillers (active
carbon black and highly conductive ferromagnetic metal powder) incorporated in a strongly
polar rubber matrix will preserve the good mechanical properties of the vulcanizates filled
with carbon black and at the same time will improve their microwave properties and SE.
This article presents the results obtained and the comparison of dielectric and microwave
properties and electromagnetic interference SE at higher frequencies (112 GHz) of CRbased composites filled with carbon black and Ni or Co particles.

Experimental
Materials
Baypren 226 (most suitable for high loadings of fillers/plasticizers, Mooney viscosity
ML(1 4) 100 C-75, produced by Lanxess) was used as CR matrix. Furnace carbon
black, namely Corax N-220 (produced by Evonik), of primary particle size about

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473

20 nm was used as a reinforcing filler with high dielectric losses. Ni and Co powders
supplied by Wako Chemical Company with particle size of 100300 nm were used as conductive ferromagnetic fillers with high magnetic losses. Other ingredients such as zinc
oxide (ZnO), magnesium oxide (MgO), stearic acid (SA), N-(1,3 dimethylbuthyl)-N0 phenyl-p-phenylenediamine (Vulkanox 4020, produced by Lanxess), tetramethyl thiuram
disulfide (TMTD, Vulkacit Thiuram/C, produced by Lanxess), and sulfur (S) were commercial grades and were used without further purification.
Preparation of rubber composites. Compositions of rubber compounds (in phr) consisted
of chloroprene rubber (CR) 100, stearic acid 2, ZnO 5, Dioctyl phthalate (DOP) 15,
Ni or Co powder 10, carbon black 0, 20 40, 60, 80, 100, TMTD 2.5, Vulkanox 1.5
and MgO 5.
One of the samples contained only Ni or Co powder as filler. A composite comprising
only 100 phr carbon black N220 as filler (without Ni or Co powder) was also prepared
for comparison and to prove our thesis.
First, mixtures of carbon black with conducting Ni or Co particles were prepared by
grinding them together in a grinding machine for 1 h. The filler mixing with rubber was
accomplished in an open two-roll mill under identical conditions of time, temperature,
and nip gap, with same sequence of mixing of all compounding ingredients to avoid the
effect of processing on the properties. The vulcanization of the rubber compounds was
carried out in an electrically heated hydraulic press using a special homemade mold at a
temperature of 153 C and under a pressure of 150 KN/m2. The optimal curing time was
determined by the vulcanization isotherms, taken on an oscillating disc vulcameter MDR
2000 (Alpha Technologies) according to ISO 3417:2002.

Characterization and measurements

Microwave properties.
Reflection and attenuation. Measurements of reflection and
attenuation were carried out using the measurement of output (adopted) power Pa in the
output of a measuring line without losses, where samples of materials may be included.
Because of the wide frequency measurement, a coaxial line was used. Samples of
materials were shaped like discs with an external diameter D 20.6 mm, equal to the
outer diameter of the coaxial line and thickness
 2 mm. The internal diameter is
depending on the relative dielectric permittivity of the material.
Part of the incident electromagnetic wave with power Pin on the sample was reflected
from it. The rest of the wave with power Pp penetrates the material so that the attenuation L
depends on the coefficient of reflection ||. His module is determined by a reflect meter.
So attenuation is determined by
Pa
; dB
Pp

Pp Pin: 1  jGj2

L 10 log
where

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Journal of Elastomers & Plastics 45(5)

Figure 1. Schematic representation of the equipment for measuring the microwave properties.
(1) A set of generators for the whole range: HP686A and G4-79 to -82; (2) Coaxial section of the
deck E2 M Orion, with samples of material; (3) Power meter HP432A; (4) Scalar reflectance meter
HP416A; (R) Reflect meter, including: two directional couplers Narda 4222.16 and two crystal
detectors Narda 4503-N.

Figure 2. Schematic representation of the equipment for measuring the dielectric properties. (1)
Generators for the whole range: HP686A and G4-79 to -82; (2) Frequency meters: H 532A; FS-54;
(3) Cavity resonator; (4) Sample; (5) Oscilloscope EO 213.

The following scheme shown in Figure 1 was used for testing both the parameters.
Shielding effectiveness. This parameter is defined as the sum of the reflection losses
R; dB and attenuation L; dB in the material.20 It can be directly measured or calculated
from the measured reflectance and attenuation in the material. In the first case, as
measured, incident power on the sample Pin and adopted after the sample Pa (Figure 2),
SE is determined by
SE 10 log

P0
; dB
Pa

In the second, if reflection and absorption in the material is known, SE is determined, by

definition, as
SE R; dB L; dB
where R, dB is the attenuation due to the reflection of power at the interfaces.

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475

Dielectric Properties
Complex permittivity. The determination of complex permittivity is carried out by the
resonance method, based on the cavity perturbation technique.21
Measuring resonance frequency of empty cavity resonator fr and then measuring the
shift in resonance frequency with the sample material f . Then the dielectric constant "r is
calculated from the shift in resonance frequency, cavity and the sample cross sections Sr
and S" , respectively
"r 1

Sr fr  f"
:
2S"
fr

The sample is in the form of a disc with a diameter of 10 mm and thickness about 2 mm.
It is placed at the maximum electric field location of the cavity. Because the thickness of
the sample is not equal to the height of the resonator, in the place of its inclusion obtains
a dielectric with an equivalent permittivity, "e , which is determined by equation (5) and
instead "r be saved "e . Then "r is determined by
"r  "e k 1  k;
<< l

where k l=
and l is the distance from the disc to the top of the resonator.
Loss factor tan. The loss factor tan  is calculated from quality factor of the cavity
with Q" and without sample Qr


1 Sr 1
1
tan 

7
4"r S" Q" Qr
The measurement setup uses several cavity resonators for the whole range, generators for
the whole range, frequency meter, and oscilloscope. Schematic representation of Figure
2 was used for measuring the dielectric properties.

Results and discussion

Dielectric properties
Complex relative permittivity. Real part (relative dielectric permittivity). The relative
dielectric permittivity of composites containing Ni or Co powder (10 phr) and different
amounts (0100 phr) of conventional furnace carbon black depending on frequency and
fillers content are shown in Figures 3 and 4.
For Ni containing composites (Figure 3), the relative dielectric permittivity "r varies
in the investigated frequency range more than twice (2.56.2). Different amounts of
carbon black has considerable effect on r and its growing results in an increase in "r .
This is most clearly seen in the middle of the range 410 GHz. At frequencies higher than
4 GHz, the degree of loading has less influence. On the other hand, this slight effect of
the frequency on "r is a positive characteristic of the material in certain areas of
application (the desired value can be reached by varying the concentration of carbon
black). In the frequency range above 10 GHz, the relative dielectric permittivity starts to

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Journal of Elastomers & Plastics 45(5)

Figure 3. Frequency dependence of relative dielectric permittivity er at various carbon black

contents (n 0100 phr) and at 10 phr Ni powder.

Figure 4. Frequency dependence of relative dielectric permittivity er at various carbon black

contents (n 0100 phr) and at 10 phr Co powder.

increase noticeably, especially for n > 60. As with other composites on the same basis,
60 phr filler content plays the role of a boundary regarding the materials behavior. For
n < 60, almost all parameters change relatively slowly, their values are unsatisfactory,
and for n > 60, or sometimes even for n  60, the same material transforms. It becomes
more adaptable for different applications, and its parameters are significantly better
(Figure 3). It is also obvious that the composite containing only Ni powder as a filler
(n 0) has the lowest dielectric permittivity. The hybrid combination of Ni powder and
active furnace carbon black gives an opportunity of considerable increasing dielectric
permittivity and also a possibility for its adjustment varying carbon black content. With
composites containing Co instead of Ni (Figure 4), the values of the relative dielectric

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477

Figure 5. Frequency dependence of dielectric loss tan de at various carbon black contents
(n 0100 phr) and at 10 phr Ni powder.

permittivity are generally lower (2.55.25). The tendency toward growth in the dielectric
permittivity with the increase in frequency and the amount of carbon black is kept, but
the nature of the dependences is different: primarily the difference in values between the
dielectric permittivity of the low-filled composites (n 0 and 20) and the rest (n 40,
60, 80, and 100) is very large. With the first, almost no change in frequency is observed
throughout the whole range studied, whereas with the latter, which are well formed in a
group, with the increase in frequency above 8 GHz, the relative dielectric permittivity
begins to grow rapidly.
The polarization mechanism operating in the gigahertz frequency is purely electronic
or orientational with relaxation times smaller than the time period of the applied signals.22 Interfacial polarization, which is the basic reason for the dispersion in dielectric
permittivity at radio frequency regime, has no role to play in microwave frequencies as it
does not produce dispersion in r because of its much smaller relaxation time. But r was
found to increase with the increase in carbon black loading in the composite, as it is
evident from Figures 3 and 4. This phenomenon of increase in dielectric permittivity
with the increase in carbon black concentration can be attributed to the enhancement of
electrical conductivity of the composites, but the differences are due to the incorporation
of metal particles as the second filler and first of all to the differences in the resistivity/
conductivity of Ni and Co.
Complex relative permittivity. Imaginary part (dielectric loss). The dielectric losses of
composites containing Ni or Co powder (10 phr) and different amounts (0100 phr) of
conventional furnace carbon black depending on frequency and fillers content are shown
in Figures 5 and 6.
Dielectric losses gradually increase with the increase in the carbon black amount and
the frequency. The lowest values were measured for the composites, containing Ni or Co
powder only (n 0). For Ni containing composites, the dielectric loss tan  changes

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Journal of Elastomers & Plastics 45(5)

Figure 6. Frequency dependence of dielectric loss tan de at various carbon black contents
(n 0100 phr) and at 10 phr Co powder.

slightly to about 8.5 GHz. Above this frequency, there is a tendency for rapid increase in
the dielectric losses, especially for the composites, containing 80 and 100 phr of carbon
black (Figure 5). In case of Co-containing composites, with a higher carbon black
amount (n 60, 80, and 100), the increase in tan  values with frequency starts at a
lower frequency (3 GHz). Overall, the dielectric loss values of Co-containing composites
are higher (from 3.103 to 12.103) than those containing Ni (from 2.103 to 9.2.103).
At low carbon black content, the dielectric loss is not sensitive to the frequency. At a low
frequency, tan  is less sensitive to the carbon black content than at higher frequency.
The dielectric losses increase toward the higher frequency side and the sharply increase
at higher loading fractions can be attributed to the conductance loss due to the presence of
Ni or Co inclusions in the rubber matrix. The difference in the Ni and Co conductance loss
is the reason for the difference in the dielectric loss of Ni- or Co-containing composites.

Microwave properties
Coefficient of reflection. The coefficients of reflection of composites containing Ni or
Co powder (10 phr) and different amounts (0100 phr) of conventional furnace carbon
black depending on frequency and fillers content are shown in Figures 7 and 8.
Overall, the differences in the coefficients of reflection of both composites are
noticeable but the values for Ni containing composites are slightly higher. On the whole,
the reflection coefficients increase with the increase in the frequency and the amount of
the filler, but the variation is different. With the frequency increase, the variation is
faster, and with the filler loading increase, the variation is slower, under other similar
conditions (Figures 7 and 8).
Attenuation coefficient. Attenuation coefficient of composites containing Ni or Co
powder (10 phr) and different amounts (0100 phr) of conventional furnace carbon black
depending on frequency and fillers content are shown in Figures 9 and 10.

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479

Figure 7. Frequency dependence of reflection || at various carbon black contents (n 0100 phr)
and at 10 phr Ni powder.

Figure 8. Frequency dependence of reflection || at various carbon black contents (n 0100 phr)
and at 10 phr Co powder.

For Ni containing composites in the absence of carbon black (n 0) and in the

presence of 10 phr Ni powder only at 1.8 GHz, a  (12) dB/cm, whereas at
n 100, a  40 dB/cm. This is an extremely important feature of these composites
in view of their application. Over 8 GHz, this parameter increases by approximately
the same gradient but with a different absolute value, depending on the amount of
filler. Thus, for a frequency of 12 GHz and n 0, a  26 dB/cm, and for n 100,
a 58.5 dB/cm. The curves corresponding to low values of loading (040 phr) are
grouped and have small differences in attenuation coefficient. As the degree of
loading increases, the differences in attenuation increase for any of the frequencies,
so the curve n 60 can be characterized as a borderline between low and high

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Journal of Elastomers & Plastics 45(5)

Figure 9. Frequency dependence of attenuation coefficient of electromagnetic waves a at various

carbon black contents (n 0100 phr) and at 10 phr Ni powder.

Figure 10. Frequency dependence of attenuation coefficient of electromagnetic waves a at

various carbon black contents (n 0100 phr) and at 10 phr Co powder.

degrees of loading. It could be said that Ni-containing composites have a higher

attenuation coefficient than Co-containing composites. This is confirmed by the fact
that composites containing only Ni (without carbon black) have a higher attenuation
coefficient than composites containing only Co (without carbon black). With Co
containing composites, the differences between the curves characterizing different
degrees of loading are better defined. Obviously, the combination of Ni with carbon
black is more effective regarding the attenuation of the electromagnetic waves in
comparison with the combination of Co with carbon black. With the latter, there
is not a synergetic effect.

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481

Table 1. Comparison of attenuation coefficient a (dB/cm) of composites containing single fillers

and their synergetic combination.
Frequency (GHz)
CB, 100 phr
Ni powder, 10 phr
CB, 100 phr Ni, 10 phr
Co powder, 10 phr
CB, 100 phr Co, 10 phr

1.8

3.96

5.6

8.5

10.5

12

32.00
0.90
39.75
0.50
25.40

38.00
1.05
43.30
1.21
26.70

40.00
2.84
43.80
1.08
30.59

40.00
5.56
45.00
2.66
37.20

45.00
14.50
47.29
4.53
36.93

65.00
26.34
58.53
8.92
39.50

Figure 11. Frequency dependence of shielding effectiveness at various carbon black content
(n 0100 phr) and at 10 phr Ni powder.

The values of microwave absorption for the composites containing Ni or Co powder

(10 phr) only, carbon black (100 phr) only, that is, single fillers, and hybrid combinations
between them are compared in Table 1.
It is obvious from the table that the composite containing the hybrid combination of
carbon blackNi powder has the best microwave absorption in the frequency range
110 GHz. In the range 18 GHz, the same hybrid combination investigated shows a
synergetic effect also.
Electromagnetic interference SE. The electromagnetic interference SE of composites
containing Ni or Co powder (10 phr) and different amounts (0100 phr) of conventional
furnace carbon black depending on frequency and filler contents are shown in Figures 11
and 12.
The study of the SE of the elastomeric material is performed indirectly by the data
obtained for reflection coefficient || and attenuation coefficient a. For comparability of
results, all the data have been brought to the same thickness (
2 mm). The results
make us conclude that the composites filled with more than 40 phr of carbon black

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Journal of Elastomers & Plastics 45(5)

Figure 12. Frequency dependence of shielding effectiveness at various carbon black contents
(n 0100 phr) and at 10 phr Co powder.

exhibit exceptional broadband properties (practically throughout the entire investigated

range) in terms of the effectiveness of electromagnetic shielding; the degree of carbon
black filling and the nature of the second filler (Ni or Co) have little effect on
the effectiveness, which remains within 1213 dB range (Figures 11 and 12). Obviously,
the higher attenuation of Ni-containing composites is due to higher reflection, and on the
whole, the results are almost identical to those of Co-containing composites, where the
attenuation is lower, but reflection is lower as well.
Microwave absorbing material is a kind of functional material that can absorb
electromagnetic wave effectively and convert electromagnetic energy into heat or
make electromagnetic wave disappear by interference.23 Generally, the electromagnetic absorbing performance of any microwave absorbing material is linked to its
intrinsic electromagnetic properties (i.e. conductivity, complex permittivity, and
permeability) as well as to extrinsic properties such as the thickness and working
frequencies.
When the electromagnetic radiation is incident on the surfaces of conductor/insulator
composites, the electric field induces two different electrical currents within the material, that is, the conduction and displacement currents.24 The former arises from free
electrons in conducting inclusions (Ni and Co particles) and will give rise to electric loss
(imaginary permittivity). The latter comes from the bound charges, that is, polarization
of dielectric matrix (real permittivity).25
It is evident when all the other conditions are equal, the observed differences in
dielectric and microwave properties of composites are due to difference in the chemical
nature of Ni and Co (both metals belong to the ferromagnetic elements) and the influence
of this difference on the investigated properties.
Magnetic properties of these materials are often expressed in terms of the magnetic
field strength H, magnetic flux density B, and the magnetic polarization J. The available
data in the literature indicate that their magnetic properties are different (Table 2).

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483

Table 2. Comparison of magnetic properties and resistivity of Ni and Co powders.26,27

Material

1000

5000

Magnetic
HcB
Curie
moment
Resistivity,
Js (T) (A m1) point ( C) Bohr magneton 108 Om (273 K)

Ni
Co

0.45
0.21

0.55
0.70

0.615
1.76

B/T for H/(A m1)

400
950

358
1115

0,61
1,61,7

6,16
5,60

B: Magnetic flux density; H: magnetic field strength; HcB: induction coercive force, coercivity; Js (B  0H)s:
saturation polarization.

Ni and Co are ferromagnetic metals and retain this property to Curie Point (358 and
1115 C, respectively). As our previous investigations indicated, introducing a ferromagnetic component in the magnetic absorber probably leads to the improvement of the
long-range order in the arrangement of the absorbing fillers in the polymer matrix and, as
a result, the hysteresis losses in the substance increase.19 The magnetic properties of
fillers strongly affect the dielectric response of the composite. High value of magnetic
permeability and dielectric constant can be obtained in the composites containing ferromagnetic particles (Ni and Co). They possess a good electromagnetic microwave absorption property due to the large values of saturation magnetization. The results were
attributed to the reduction in eddy current loss (increase of permeability) and enhancement of space-charge polarization (increase of permittivity).
On the basis of mentioned differences, it can be expected that the influence of these
metals on the dielectric and especially on the magnetic properties of the investigated
composites will be different. On the other hand, the microwave properties and especially the attenuation of the electromagnetic waves are determined by both the
dielectric and magnetic losses of the composite.28 Evidently, it is the different magnetic losses due to the different magnetic properties of Ni and Co that determine the
observed differences. It is obvious that the suitability of these composites as microwave absorbers is dependent on the real and imaginary parts of the complex dielectric
permittivity and magnetic permeability. The same conclusion is made in the study by
Muhammad Abdul Jamal et al.22

Conclusions
1.

The dielectric and microwave properties of CR-based composites containing

0100 phr furnace carbon black and Ni or Co powder 10 phr have been compared
in the frequency range 112 GHz. It has been found out that:
 in terms of dielectric properties with composites containing hybrid combination
of carbon black and Ni powder, the values of the real part of the complex
dielectric permittivity (relative dielectric permittivity) under the same other
conditions are higher than the values for composites containing Co, and the
values of the imaginary part (dielectric losses) are lower;

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2.

Journal of Elastomers & Plastics 45(5)

 in terms of magnetic properties with composites containing a combination of

carbon blackNi powder, the coefficients of reflection and attenuation are higher
that those of Co-containing composites.
 the electromagnetic SE of two types of composites is virtually identical when the
carbon black amount in them is more than 40 phr.
The observed differences in behavior can be explained by the differences in some
characteristics of two metals, especially in terms of the values of magnetic moment,
magnetic flux density, induction coercive force, saturation polarization, volume
resistivity, and so on, and influence of these differences on the real and imaginary
parts of the complex dielectric permittivity and magnetic permeability.

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