The Effect of Carbon Black On The Properties of Magnetic Ferrite Filled Natural Rubber Composites

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The Effect of Carbon Black on the

Properties of Magnetic Ferrite Filled
Natural Rubber Composites
Article in Journal of Reinforced Plastics and Composites November 2008

DOI: 10.1177/0731684407082545
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The Effect of Carbon Black on the Properties of Magnetic Ferrite Filled Natural Rubber
Composites
S.T. Sam, H. Ismail, M.N. Ahmad Fauzi and A. Abu Bakar
Journal of Reinforced Plastics and Composites 2008 27: 1893 originally published online 12
November 2007
DOI: 10.1177/0731684407082545
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The Effect of Carbon Black on the Properties
of Magnetic Ferrite Filled Natural
Rubber Composites
S. T. SAM, H. ISMAIL,* M. N. AHMAD FAUZI AND A. ABU BAKAR

School of Materials and Mineral Resources Engineering
Universiti Sains Malaysia, 14300 Nibong Tebal, Penang, Malaysia
ABSTRACT: The effect of carbon black loading and type on the properties of ferrite filled natural
rubber (NR) composites was investigated. The carbon black loading used was from 0 to 50 phr and
ferrite loading was fixed at 80 phr. Carbon black grades N330 and N660 were used in this work. The
scorch time decreased with the addition of carbon black in ferrite filled NR composites whereas the
cure time increased. The tensile strength and elongation at break of ferrite filled natural rubber
composites were found to decrease with the increase of both types carbon black loading. However,
the stress at 100% elongation (M100) and stress modulus at 300% elongation (M300) exhibit an
increasing trend. The microstructure showed that filler dispersion of ferrite filled natural rubber
composites become poorer with increasing carbon black loading. The thermal stability was found to
enhance with carbon black loading. The swelling test indicated that the swelling percentage reduced
with increasing carbon black loading while at low loading enhanced the magnetic properties of the
composites. The N330 carbon black filled NR composites showed longer scorch and cure times and
better tensile properties, swelling resistance and magnetic properties but lower thermal stability than
N660 carbon black filled NR composites.
KEY WORDS: rubber ferrite composites, nickel zinc ferrite, magnetic filler, carbon black.
INTRODUCTION
materials which are physically dark or black in color, and

F ERRITES ARE MAGNETIC
very hard, brittle and inert to a lot of chemicals. In the form of ceramic, ferrite can be
used in producing magnetic memories, flexible magnets, microwave absorbers, TV yokes,
and some other useful devices. The incorporation of ferrite in natural rubber is important
in producing an easily moldable and flexible composite materials called ferrite rubber
composites (RFCs) or polymer bonded magnets (PBMs). RFCs have wide industrial
applications as they can be tailored in various shapes and properties. According to Malini
et al. [1], RFCs can be applied in wave absorbers and electromagnetic interference (EMI)
shielding material. Several researches [18] have reported the work on RFCs by using
different types of ferrite filler in various rubber matrices.
*Author to whom correspondence should be addressed. Email: hanafi@eng.usm.my
Journal of REINFORCED PLASTICS AND COMPOSITES, Vol. 27, No. 1617/2008 1893
0731-6844/08/1617 189316 $10.00/0 DOI: 10.1177/0731684407082545
SAGE Publications 2008
Los Angeles, London, New Delhi and Singapore

1894 S.T. SAM ET AL.
In this study, the ferrite powder used was waste ferrite with zero economic value. This
type of ferrite was useful in producing many types of electronic devices such as high
frequency transformers and inductors due to their naturally low current loss [9]. Two types
of carbon blacks used in hybrid with ferrite were N330 and N660 grades. The aim of the
study is to investigate the effect of carbon black loading and two different types of carbon
blacks on tensile properties, thermal stability, swelling percentage and magnetic properties
of ferrite filled natural rubber composites.
EXPERIMENTAL
Compounding Ingredient and Mixing Procedure
Natural rubber (SMR L) was obtained from the Rubber Research Institute of Malaysia
(RRIM). The waste ferrite used in this study was Ni-ZnFe2O4, which was obtained from
ACME Ferrite Products Sdn. Bhd. The ferrite powder was a by-product of grinding the
fully sintered Ni-ZnFe2O4. Its specific gravity is 4.90 g/cm3 with mean particle size between
48 mm. The N330 and N660 carbon black were obtained from Cabot Company
(Malaysia) with the mean particle size of 28 and 70 nm respectively. The surface area of
N330 and N660 are 80 and 35 m2/g, respectively. Others chemicals such as sulphur, zinc
oxide, stearic acid, n-cyclohexylbenthiazyl sulpheamide (CBS) and sterically hindred
bisphenol (Vulkanox NKF) were purchased from Bayer (M) Ltd. The carbon black
loadings used in this study were 10, 20, 30 and 50 phr. The formulation used is shown in
Table 1. The ferrite was dried in a vacuum oven at 808C for 24 hours to expel moisture.
Mixing of the raw materials was carried out on a conventional laboratory two roll mill
(160 320 mm). The mixing time was kept below 30 minutes to avoid premature
vulcanization of excess heat. The cure times, t90 were determined using a Monsanto
Rheometer, Model MDR 2000 (moving die rheometer) at 1508C according to ISO 3417.
The rubber compounds were then compression molded at 1508C using t90 and the
vulcanizates were conditioned for 24 hours prior to testing.
Measurement of Tensile Properties
The tensile tests were conducted using an Instron Universal Testing Machine, model
3366 according to ASTM D412 at a 500 mm/min crosshead speed. Parameters obtained
including tensile strength, tensile modulus and elongation at break.
Table 1. A typical formulation of rubber compound.
Ingredient Recipe (phr)
SMR L 100
Ferrite 80
Zinc Oxide 5
Stearic Acid 3
CBS 0.5
NKF 1
Sulfur 2.5
Carbon Black 0, 10, 20, 30 and 50

The Effect of Carbon Black on the Properties of Magnetic Ferrite 1895
Measurement of Thermal Stability
Thermal degradation of RFCs was analyzed using a Perkin Elmer thermal

analyzer. About 10 mg of sample was needed for analyzing. The heating rate of the
system was 108C/min and the test was conducted from 50 to 6008C in a nitrogen
atmosphere.
Swelling Test
The swelling test was carried out according to ISO1817. The dimension of the samples
was 30 mm 5 mm 2 mm. The samples were immersed in toluene for 48 hours in a dark
condition. The excess toluene was removed by using tissue paper. The swollen weight of
the samples was weighted by using an electrical balance. The swelling percentage of the
sample can be calculated with the equation below:
M2 M1
Swelling % 100:
M1
The M1 and M2 refer to original weight and swollen weight respectively.
Scanning Electron Microscopy
The tensile fracture surface of the RFCs was examined using a Scanning Electron
Microscope (SEM), model Leica Cambridge S-200. The micrograph obtained from SEM
was used to observe the filler distribution of the fracture surface and the micro defect of
the samples. All the surfaces were initially sputter coated with gold in order to avoid
electrostatic charging and poor image resolution.
Magnetic Properties
The initial permeability, quality factor and inductance of RFC samples were
determined using a Hewlett Packard impedance/gain phase analyzer model HP-4194 A.
The samples were cut in the form of discs having an inner diameter (ID) of 3.7 mm,
outer diameter (OD) of 20 mm and a thickness of 2 mm. The initial permeability,
quality factor and inductance were measured using 10 Cu wire windings at frequency range
of 1 kHz35 MHz.
RESULTS AND DISCUSSION
Cure Characteristic
Figures 1 and 2 show the scorch time (t2) and cure time (t90) for carbon black filled
RFCs using two types of carbon black, N330 and N660. It can be observed that scorch
time decreased with the increase of carbon black loading for both composites. Geethamma
et al. [10] reported that as the filler loading increased, the incorporation time of the filler
into rubber matrix also increased and consequently generated more heat due to the
additional friction. The decrease of the scorch time indicated that the composites took less
time to reach the onset time of vulcanization as the carbon black loading increased.

5
N330
N660
4.5
Scorch time (min)
3.5
2.5
0 10 20 30 40 50 60
Carbon black loading (phr)
Figure 1. Variation of scorch time with carbon black loading in RFCs.
13
N330
N660
12.5
Cure time (min)
12
11.5
11
10.5
0 10 20 30 40 50 60
Figure 2. Variation of cure time with carbon black loading in RFCs.
Figure 2 shows that the cure time of both RFCs decreased with increasing carbon black
loading. As reported by Ismail et al. [11], the curing rate of rubber composites depends on
presence metal oxide. Thus, the reduction of metal oxide content (ferrite) in rubber
composites with increasing carbon black loading had reduced the curing rate consequently

20 N330
N660
18
16
Torque difference (dNm)
14
12
10
4
0 10 20 30 40 50 60
Figure 3. Relationship between torque difference and carbon black loading in RFCs.
increasing cure time. As can be observed in Figure 2, N330 carbon black displayed longer
cure time than N660. Generally, factors such as low surface area, high moisture content
and high metal oxide content can decrease the cure time of the compounds [12]. The slower
cure time of RFCs with N330 might be due to the high surface area of N330 carbon black.
Variation of torque difference (MH-ML) is shown in Figure 3. The MH-ML of the
composites was found to increase with increasing of carbon black loading. As reported by
Ciesielski [13], the torque difference is an indirect indicator of crosslink density of rubber
composites. The trend indicated that the crosslink density increased with the incorporation
of carbon black in RFCs. Carbon black can act as a crosslink agent in the vulcanization
process, hence the crosslink density increased with the increase of carbon black [14]. It can
be seen in Figure 3 that N330 carbon black exhibits higher MH-ML than N660.
The smaller particle size of a filler with larger surface area normally has greater interaction
with a rubber matrix [12].
Tensile Properties
The effect of carbon black loading on tensile strength in RFCs is shown in Figure 4.
The tensile strength decreased about 10% and 20% with addition of 50 phr N330 and
N660 respectively. The reduction of the tensile strength was due to the agglomeration of
the filler and dilution effect at high filler loading. Thus, the filler was unable to transfer the
stress to polymer matrix since the rubber-filler interaction is weak [5]. The phenomenon is
in agreement with some of our previous work using rice husk ash in natural rubber
composites [15], oil palm wood flour in natural rubber composites [16] and bamboo fibre
in natural rubber composites [17]. Comparing two types of carbon black, tensile strength
of N330 is found to be higher than N660 in RFCs. Again, this must be attributed to the

25
N330
N660
23
21
19
Tensile strength (MPa)
17
15
13
11
5
0 10 20 30 40 50 60
Figure 4. The effect of carbon black loading on elongation at break and tensile strength of RFCs.
better interaction between N330 carbon black and rubber as a result of the smaller particle
size of N330. A similar trend can be observed in the elongation at break as shown in
Figure 5. At a similar filler loading, N330 exhibits higher elongation at break than N660.
The result indicated that the smaller particle size of filler has better interaction with rubber
matrix. Figure 6(a)(c) and Figure 7(a)(c) show the SEM micrograph with different
loading of N330 and N660 in RFCs. As the carbon black loading in RFCs increased, the
fracture surface of the RFCs exhibits more holes or detachment of filler from rubber
matrix. This indicated the rubber-filler interaction becomes poorer with increase of carbon
black loading. It can be seen that, at a similar filler loading, the size of holes is bigger in
N660-filled than N330-filled RFCs. Figures 8 and 9 show the effect of both carbon blacks
loading on stress at 100% elongation (M100) and stress at 300% elongation (M300) of
RFCs. According to our previous report on bamboo filled natural rubber composites [18],
the increase in filler loading would increase the restriction of macromolecular motion of
rubber chains. Another reason might be due to the nature of the fillers. Carbon black is
composed of rigid particles that cause the overall increment of the stiffness of rubber
composites. N330, which has smaller particles size, was found to exhibit higher M100
and M300 than N660. The larger surface area of carbon black N330 has better interaction
with rubber matrix [19].
Thermal Stability
Figure 10 shows the TGA curves of RFCs with different carbon black loading. Since
there was only one type of rubber matrix (i.e. NR) used in the composites, the curves
displayed a singe step degradation process for all RFCs produced. Table 2 shows detailed
summary variation of 5% weight loss (T-5%) and 30% weight loss (T-30%) of RFCs at

1000
N330
N660
900
800
Elongation at break (%)
700
600
500
400
300
0 10 20 30 40 50 60
Figure 5. The effect of carbon black loading on elongation at break and tensile strength of RFCs.
different loading of N330 and N660. T-5% indicates the initial thermal stability whereas
T-30% shows the higher degradation rate of the rubber composites. As shown in Table 2,
the incorporation of the carbon black resulted in overall improvement of thermal stability.
Char residue content increased with higher carbon black loading. According to Ramesan
[20], the higher content of char residue can insulate the undecomposed polymer from the
degradation process. The results show that there is a slightly higher degradation
temperature of RFCs with N660 compared to N330, particularly at the higher filler
loading. The degradation temperature can be related to the volatile material in the filler.
The carbon black N660 which has less volatile matter might enhance the degradation
temperature of RFCs. The enhancement of the thermal stability with increasing filler
loading in polymer matrix have been reported by some researchers using different fillers,
such as TiO2 and Fe2O3 filled poly (methyl methacrylate) [21], ferric oxide in silicone
polymer composites [22] and Al2O3 and ZnO filled silicone rubber [23].
Swelling Percentage
A swelling test is used to observe the filler-matrix interaction. The swelling percentage is
the amount of toluene uptake per weight of the rubber matrix. According to our previous
report [24], the swelling percentage of the rubber composites was influenced by crosslink
type and density, filler loading and type of rubber matrix. Figure 11 shows the effect of
carbon black loading on the swelling percentage of RFCs using two different carbon
blacks. A decreasing trend can be seen as the carbon black loading increased. The results
indicated that the penetration of the toluene into RFCs was reduced with the addition
of carbon black loading. The RFCs with N330 carbon black had less swelling
percentage compared to N660 carbon black. The result is in agreement with our previous

(a)
Holes
(b)
More
holes
(c)
More
and
bigger
holes
Figure 6. SEM micrograph of the tensile fracture surface of RFCs with different N330 loading (a) 10 phr
(b) 30 phr and (c) 50 phr at 500X magnification.
report which indicated that the smaller the particles size of filler, the better the rubber-filler
interaction [12].
Magnetic Properties
The dependence of inductance upon frequency of two different carbon blacks in RFCs is
shown in Figure 12. Generally, the inductance decreased slightly with increase of frequency.
Thus, it can be reported that the RFCs were stable even at high frequency. This indicates
that the RFCs are suitable to be used in high frequency application. The inductance of RFCs

(a)
Holes
(b)
More
holes
(c)
More
and
bigger
holes
Figure 7. SEM micrograph of the tensile fracture surface of RFCs with different N660 loading (a) 10 phr
(b) 30 phr and (c) 50 phr at 500X magnification.
with carbon black N330 displayed higher inductance compared to N660. A similar reason
must be attributed to the better dispersion of the carbon black N330 in rubber matrix to that
discussed in the previous section. Figure 13 shows the variation of the inductance with
different carbon black loading in RFCs. At low and high applied frequency, the inductance
of the RFCs with N330 first increased up to 30 phr, and then decreased with higher loading.
The decreasing trend in high loading was due to the increasing of magnetic interaction
between the ferrite particles as the particles distance reduced [5]. RFCs with N660 carbon
black increased up to 20 phr at a frequency of 100 kHz and thereafter decreased with higher
filler loading. At higher frequency (i.e. 10 MHz) the maximum loading of N660 carbon

4
N330
N660
3.5
2.5
M100 (MPa)
1.5
0.5
0
0 10 20 30 40 50 60
Figure 8. Effect of carbon black loading on stress at 100% elongation (M100).
12
N330
N660
10
8
M300 (MPa)
0
0 10 20 30 40 50 60
Figure 9. Effect of carbon black loading on stress at 300% elongation (M300) of RFCs.
black to achieve optimum inductance was 10 phr. Thus, the ability to store energy in the
form of magnetic field of N330 was better than N660 at low and high frequencies. The plot
of initial permeability as a function of frequency is shown in Figure 14. The trend of the
initial permeability of all samples was the same with the inductance because the initial

110
100
90
Weight loss (%)
80
70
50 phr carbon black N660
60 50 phr carbon black N330

50

40
0 100 200 300 400 500 600 700
Temperature (C)
Figure 10. Thermogravimetric analysis of RFCs with different type and carbon black loading.
Table 2. TGA data for RFCs with different carbon black loading.
Carbon black loading (phr) T-5% (8C) T-30% (8C) Char Residue (%)
N330 N660 N330 N660 N330 N660

0 346 346 397 397 44.9 44.9
10 348 348 406 407 47.4 48.0
30 350 352 412 413 52.4 52.8
50 351 355 414 418 55.6 56.6
permeability depends on the inductance, dimension and number of coil winding of the
samples. It is known that permeability is the measure of the magnetic flux through a core
[25]. Thus, the RFCs with N330 would allow magnetic flux more easily compared to N660.
Figure 15 shows the dependence of quality factor (Q) on frequency at low (10 phr) and high
loading (50 phr) of N330 and N660 carbon black. The resonance frequency of the RFCs
occurred at 30 MHz. The result indicates that the types and loading of the carbon black
would not affect the resonance frequency of Q factor of RFCs but was contributed by the
presence of ferrite in the composites. As can be observed in Figure 15, lower loading (10 phr)
of both types of carbon black exhibit a better quality factor compared to higher loading
(50 phr). This was due to the dilution effect which occurred when the filler loading was
incorporated up to 130 phr, i.e. 80 phr ferrite and 50 phr carbon black. As can be seen in
Figure 16 at a similar carbon black loading, RFCs with N330 exhibited higher Q factor than
N660. This indicates that the larger particles size carbon black (i.e. N660) had caused the
poorer filler distribution and thus reduced the ratio of energy stored to the energy lost in
composites [25].

250
Carbon black N330
Carbon black N660
200
Swelling percentage (%)
150
100
50
0
0 10 20 30 40 50 60
Figure 11. The effect of carbon black loading on swelling percentage of RFCs.
0.35
10 phr of carbon black N330
0.30 50 phr of carbon black N660
0.25
Inductance (H)
0.20
0.15
0.10
0.05
0.00
0.00E+00 5.00E+03 1.00E+04 1.50E+04 2.00E+04 2.50E+04 3.00E+04 3.50E+04 4.00E+04 4.50E+04
Frequency (kHz)
Figure 12. Variation of inductance with frequency for different type and loading of carbon black.

0.35 Carbon black N330 with frequency 100 kHz
Carbon black N330 with frequency 10 MHz
Carbon black N660 with frequency 100 kHz
0.30 Carbon black N660 with frequency 10 MHz
0.25
Inductance (H)
0.20
0.15
0.10
0.05
0.00
0 10 20 30 40 50 60
Figure 13. The effect of carbon black loading on inductance at different frequency of RFCs.
5.00 10 phr carbon black N330

4.00
Initial permeability (Hm1)
3.50
3.00
2.50
2.00
1.50
1.00
0.00E+00 5.00E+03 1.00E+04 1.50E+04 2.00E+04 2.50E+04 3.00E+04 3.50E+04 4.00E+04 4.50E+04
Frequency (kHz)
Figure 14. Variation of initial permeability with frequency for different type and loading of carbon black.


50 phr carboon black N660
100.00
80.00
Q factor
60.00
40.00
20.00
0.00
0.00E+00 5.00E+03 1.00E+04 1.50E+04 2.00E+04 2.50E+04 3.00E+04 3.50E+04 4.00E+04 4.50E+04
Frequency (kHz)
Figure 15. Variation of quality factor (Q) with frequency for different type and loading of carbon black.
80.00 Carbon black N330 with frequency 100 kHz

Carbon black N330 with frequency 10 MHz
Carbon black N660 with frequency 100 kHz
70.00 Carbon black N660 with frequency 10 MHz
60.00
50.00
Q factor
40.00
30.00
20.0
10.00
0.00
0 10 20 30 40 50 60
Figure 16. The effect of carbon black loading on Q factor at two different frequencies of RFCs.

CONCLUSIONS
The incorporation of carbon black in RFCs had decreased the scorch time but increased
the cure time of the composites. RFCs with N330 carbon black exhibit longer cure time
and scorch time compared to N660. On the other hand, the torque difference increased
with increase of both types of carbon black loading whereas the tensile strength and
elongation at break show the opposite trend. At a similar filler loading, RFCs with N330
exhibit higher tensile strength and elongation at break than N660. However, the tensile
modulus (M100 and M300) increased gradually with the increase of both carbon black
loading. The SEM micrographs showed that the dispersion of the ferrite in NR matrix
becomes poorer by incorporation of both carbon blacks but the thermal stability had
improved. The presence of carbon black at low loading enhanced the magnetic
properties of RFCs and carbon black N330 imparts better magnetic properties than
N660 carbon black.
ACKNOWLEDGMENT
The authors acknowledge the materials and testing equipments provided by ACME
Ferrite Products Sdn. Bhd., which has resulted in this article.
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The Effect of Carbon Black On The Properties of Magnetic Ferrite Filled Natural Rubber Composites

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The Effect of Carbon Black on the

Article in Journal of Reinforced Plastics and Composites November 2008

Ahmad Fauzi Mohd Noor

Available from: S.T. Sam

The online version of this article can be found at:

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S. T. SAM, H. ISMAIL,* M. N. AHMAD FAUZI AND A. ABU BAKAR

materials which are physically dark or black in color, and

*Author to whom correspondence should be addressed. Email: hanafi@eng.usm.my

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Compounding Ingredient and Mixing Procedure

Measurement of Tensile Properties

Table 1. A typical formulation of rubber compound.

Ingredient Recipe (phr)

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Measurement of Thermal Stability

Thermal degradation of RFCs was analyzed using a Perkin Elmer thermal

The M1 and M2 refer to original weight and swollen weight respectively.

Scanning Electron Microscopy

RESULTS AND DISCUSSION

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Figure 2. Variation of cure time with carbon black loading in RFCs.

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50 phr carbon black N660

60 50 phr carbon black N330

10 phr carbon black N660

10 phr carbon black N330

N330 N660 N330 N660 N330 N660

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5.00 10 phr carbon black N330

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120.00 10 phr carbon black N330

80.00 Carbon black N330 with frequency 100 kHz

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