You are on page 1of 10

A study on the material properties and fatigue life of natural

rubber with different carbon blacks


J.-H. Kim
a
, H.-Y. Jeong
b,
*
a
Korea Railroad Research Institute, 360-1, Woulam-Dong, Uiwang-City, Kyounggi-Do 437-050, South Korea
b
Department of Mechanical Engineering, Sogang University, 1 Shinsoo-Dong, Mapo-Gu, Seoul 121-742, South Korea
Received 14 November 2003; received in revised form 6 April 2004; accepted 9 July 2004
Abstract
Natural rubber compounds lled with N330, N650 or N990 were experimentally investigated in order to examine the effects of carbon
black on the fatigue life, the hysteresis, the fracture surface morphology and the critical J-value. The fatigue life was obtained by conducting
a displacement-controlled fatigue test on an hourglass-shaped specimen, and the hysteresis was calculated from the loading and unloading
curves obtained during the fatigue test. The fracture surface obtained after the fracture test was examined by a microscope, and its roughness
was calculated for the surface prole obtained by using a stylus-type roughness tester. In addition, the critical J-value was obtained by
conducting a tensile test for pre-cracked dumbbell specimens. Based on the test data, it was noticed that the fatigue life, the hysteresis, the
small-scale roughness and the critical J-value were ranked in the following order for the NR compound lled with N330, N990 or N650. It
was also noticed that the logarithmic value of the fatigue life was linearly proportional to the square root of the product of the critical J-value
and the hysteresis.
q 2004 Elsevier Ltd. All rights reserved.
Keywords: Carbon black; Natural rubber; Fatigue life; Critical J-value; Hysteresis; Fracture surface morphology; Roughness
1. Introduction
Carbon black is used as a reinforcement to increase the
structural and thermal properties of NR (natural rubber).
When a rubber component lled with carbon black is under
loading, the rubber matrix around carbon black is strained
more than the rest. If a large or repeated force is applied,
carbon black is separated from the matrix nucleating
microcracks. There are other sources of microcracks in
rubber including contaminants or voids in the matrix,
imperfectly dispersed compounding ingredients, mold
lubricants and surface aws [1,2]. Upon further loading,
the microcracks coalesce resulting in a noticeable crack that
may lead to failure [3]. On the torn surface of stronger
elastomers vertical steps are more frequent and larger, and
each step is associated with a carbon black particle [4].
Therefore, it is important to gure out the characteristics
and effects of carbon black in order to understand the
material behavior of NR.
For this purpose, many researchers have studied the
characteristics and effects of carbon black using diverse
methods. Greensmith [5] investigated the effect of carbon
black on the tearing behavior of NR and SBR (styrene
butadiene rubber, then called GR-S), and he discovered
that the reinforcement of carbon black was effective only
in a limited range of temperature and rate of crack
propagation. Hess and Ford [6] reviewed microscopy of
lled rubbers, and they showed evidence that a micro-
crack nucleated from a carbon black, and a crack followed
a path through reagglomeration areas. Lake and Lindley
[1] investigated the effects of deformation, testing
environment, protective agents and llers on the fatigue
life and the crack growth rate, and they noticed that the
crack growth rate decreased by addition of carbon black
especially small carbon black particles such as HAF (high
abrasion furnace), and the fatigue life of NR decreased
0142-1123/$ - see front matter q 2004 Elsevier Ltd. All rights reserved.
doi:10.1016/j.ijfatigue.2004.07.002
International Journal of Fatigue 27 (2005) 263272
www.elsevier.com/locate/ijfatigue
* Corresponding author. Fax: C82 2 712 0799.
E-mail address: jeonghy@sogang.ac.kr (H.-Y. Jeong).
less than that of SBR as temperature increased. Goldberg
et al. [7] investigated the effect of carbon black loading on
stretching, tearing and failure of NR and SBR, and they
noted that knotty tearing was more frequently observed in
NR than in SBR, and the tearing energy increased as the
loading increased from 0 to 35 phr. Chung et al. [8]
measured the tearing energies of SBR, HNBR (hydrogen-
ated nitrile rubber) and NR with different loading of
carbon black, and they noticed that the tearing energy
became maximized around the loading of 40 phr in SBR
and NR, but the effect of carbon black on the tearing
energy was not considerable in NR because of crystal-
lization occurring in front of a crack. Wang [9]
thoroughly reviewed the effect of carbon black on
dynamic properties of lled vulcanizates such as the
elastic modulus, the viscous modulus and the loss tangent,
and he noted that the loss tangent was dependent on the
temperature, the strain amplitude and the loading of
carbon black. Legorju-jago and Bathias [10] investigated
the effects of the load ratio, the temperature, the thickness
and the stress state on the fatigue life and the crack
growth rate of NR, CR (polychloroprene rubber) and
SBR, and they noticed that for the high load ratio or
thickness, the fatigue life of NR increased because of
crystallization.
However, no research was conducted on the change of
the material property and the failure behavior of lled NR
due to different types of carbon black. Thus, in this paper
the material properties (the critical J-value and the
hysteretic loss), the fatigue life and the fracture mor-
phology of NR compounds lled with three types of
carbon black, N330, N650 and N990, were experimentally
obtained. The fatigue life was measured for an hourglass-
type specimen under a displacement control with three
different amplitudes. The fracture morphology was
examined not only by photos but also by fracture surface
roughness. In addition, the roughness was classied into a
large-scale roughness and a small-scale roughness. By
reviewing the experimental data, several interesting points
could be noted. First, the material properties, the fatigue
life and the fracture morphology became different due to
variant types of carbon black. Secondly, the trend of the
large-scale roughness was opposite to that of the small-
scale roughness, and the critical J-value increased as the
small-scale roughness increased. Thirdly, the logarithmic
value of the fatigue life for each of the displacement
amplitude was linearly proportional to the square root of
the product of the critical J-value and the hysteretic loss.
Thus, the logarithmic value of the fatigue life could be
represented as a function of the displacement amplitude,
the critical J-value and the hysteretic loss. This implies
that the fatigue life of a rubber component can be
predicted from the displacement amplitude and the
material properties such as the critical J-value and the
hysteretic loss.
2. Experimental results
2.1. NR lled with three types of carbon black
In this research, NR compounds lled with three kinds of
carbon black, N330, N650 and N990, were investigated.
Table 1 shows the characteristics of the NR compounds
along with carbon black. Carbon black can be classied into
the small, medium and large size according to ASTM
D1765 [11], and a representative carbon black for each size
was selected. When a rubber component is under develop-
ment in industry, the static stiffness of a rubber component
is usually specied. Since there is a relationship between
Youngs modulus and the hardness of rubber, the hardness
can be determined from the required static stiffness [12,13].
For this study, the amount of carbon black in each
compound was determined in a way that the hardness of
the rubber compound remained the same at 62. In addition,
the hardness was measured using durometer type A on a
compression specimen of diameter of 28.8 mm and height
of 12.5 mm [14,15].
2.2. Fatigue life
The hourglass-shaped specimen designed by Takeychi
et al. [16] was used to measure the fatigue life of the lled
NR compounds, and it is shown in Fig. 1. It has an elliptical
cross section, and the seam line is located on the surface of
the minor axis. Since the stress on the surface of the major
axis is higher than that on the surface of the minor axis, a
crack usually starts at the major axis, and the seam line
hardly affects the fatigue life of the specimen. The fatigue
test was conducted at room temperature, 23 8C, and it was
displacement-controlled using MTS810. The displacement
was prescribed as a sinusoidal pulse at the frequency of 1 Hz
with the maximum displacement of 16, 19 or 22 mm and the
minimum displacement of 0 mm. Thus, the maximum
displacement was equal to the double displacement
amplitude, and the load ratio, which is dened to be the
ratio of the minimum load (or displacement) to the
maximum load (or displacement), was equal to 0. During
the test, the specimen was air-cooled to keep the
temperature around 23 8C. The fatigue life was dened to
Table 1
Characteristics of NR compounds lled with N330, N650 and N990
N330 N650 N990
CB particle
diameter (nm)
30 61 285
Specic weight 1.1245 1.1485 1.2270
CB phr 46 54 90
Volume fraction (%) 16.8 18.4 28.0
Total phr 171.26 183.00 219.26
Curing time (s) 420 420 420
Curing temperature (8C) 173 173 173
Hardness 62 62 62
J.-H. Kim, H.-Y. Jeong / International Journal of Fatigue 27 (2005) 263272 264
be the cycle at which the load became half the load
measured at 10,000 cycles.
Three fatigue tests were conducted at three different
double displacement amplitudes for each type of carbon
black. Table 2 shows the average and the standard deviation
of the fatigue life of the NR compounds. As expected, the
fatigue life reduced as the amplitude increased. Regardless
of the amplitude, the NR lled with N650 resulted in the
shortest fatigue life, but the NR lled with N330 resulted in
the longest fatigue life. However, there were comparatively
small deviations among tests showing the repeatability of
the test. Previous research showed that the fatigue life of NR
is dependent on testing environment [1], the load ratio [10]
and additives [17]. In addition, this study showed that the
fatigue life is also dependent on the type of carbon black.
2.3. Measurement of the hysteresis
Rubber has a characteristic of viscoelasticity resulting in
an energy loss during a cyclic loading. The energy loss is
called the hysteresis (or hysteretic loss), and it eventually is
converted to heat causing temperature increase [18]. Since
the temperature increase gradually degrades rubber, it
is important to understand the mechanism and effects of
the hysteretic loss. The specimen shown in Fig. 1 was also
used to measure the amount of hysteresis, and the conditions
were the same as that for the fatigue test. It is well known
that the material properties of NR change during the rst set
of loadings due to so-called Mullins effect [19]. Thus, the
hysteresis was measured after several thousands of loadings.
For example, when the double displacement amplitude was
22 mm, the specimen was loaded up to 10,000, 15,000, and
20,000 cycles, and the force vs. displacement curve was
measured for the next 100 cycles. Then, the hysteresis was
obtained from the average of the energy loss occurring for
the 100 cycles. The number of cycles for the rst
measurement, 10,000 cycles, was chosen at about a quarter
of the minimum fatigue life which occurred for the rubber
compound with N650 at the fatigue test with the amplitude
of 22 mm. When the amplitude was 16 or 19 mm, the cycles
for which the hysteresis was measured were higher than
those for the amplitude of 22 mm.
Three sets of tests were conducted for each test
condition, and the averages and the standard deviations of
the hysteresis for three rubber compounds are shown in
Table 3. As expected, the hysteresis increased as the
amplitude increased. Note that the hysteresis was ranked in
the following order for the rubber compound lled with
N330, N990 or N650, and there were negligible deviations
showing the repeatability of the test.
Carbon black particles are rmly fused together in
rubber, and the smallest discrete entity existing in rubber is
always the aggregate [20]. By virtue of their irregular
morphology, the aggregates are bulky, and occupy an
effective volume considerably larger than that of carbon
black itself. The bulkiness of the aggregate is the property
commonly called structure. It is adequate to describe carbon
black morphology by two parametersone related to the
structure and the other to the mean particle size.
The most commonly used techniques for measuring
carbon black structure have been based on internal void
volume using absorptive measurements or volumetric
measurements under pressure [20]. Dibutylphthalate
(DBP) is continuously added using a constant rate buret to
dry carbon black in an internal mixer tted with a device
measuring the torque on the mixer blades. When the
interstices between carbon black particles are lled with
DBP, an appreciable torque level is developed, and the
absorptometer and buret will shut off automatically. The
volume of DBP per unit mass of carbon black is the DBP
Fig. 1. Hourglass-shaped fatigue test specimen (all dimensions in mm).
Table 2
Fatigue life test data (cycle)
N330 N650 N990
Double amplitude
of 16 mm
Ave. 625,800 213,940 457,310
Std. 7860 34,150 6720
Double amplitude
of 19 mm
Ave. 480,650 98,930 323,860
Std. 10,530 7200 5550
Double amplitude
of 22 mm
Ave. 382,210 41,110 214,340
Std. 6140 1040 14,000
Table 3
Hysteresis test data (N mm)
N330 N650 N990
Double amplitude
of 16 mm
Ave. 355.3 44.5 205.3
Std. 7.8 1.6 3.3
Double amplitude
of 19 mm
Ave. 465.5 47.4 276.3
Std. 0.9 0.4 0.8
Double amplitude
of 22 mm
Ave. 487.1 49.3 359.3
Std. 5.4 1.3 3.3
J.-H. Kim, H.-Y. Jeong / International Journal of Fatigue 27 (2005) 263272 265
absorption (DBPA) number. The test method for DBPA
number determination is described in ASTM2414-00 [21].
The traditional particle size count of electron micro-
graphs is difcult and inherently imprecise. Thus, the
specic surface area is determined instead. The absorption
of cetyltrimethyl ammonium bromide (CTAB) by carbon
black in an aqueous solution is a method for surface area
determination. This method covers the measurement of the
specic surface area of carbon black exclusive of area
contained in micropores too small to admit CTAB
molecules, and it is described in ASTM 3765-99 [22].
The amount of hysteresis depends on both the structure
and the surface area per unit volume of carbon black
aggregate [23]. In Table 4, the DBPA number and the
CTAB surface area are shown for the three types of carbon
black. If the structure of carbon black aggregate develops
well, the carbon black aggregate is more likely to be cut off
by a blade in the mixing process, and new surface is more
likely to be created. This causes stronger cohesion and
smaller friction between rubber and carbon black, sub-
sequently resulting in less hysteresis. When the specic
surface area of carbon black is high, there occurs more
friction between rubber and carbon black, subsequently
resulting in more hysteresis. Therefore, the hysteresis
increases as the DBPA number decreases or the CTAB
surface area increases. Data in Table 4 indicate that the
structure of N650 was well developed, and the surface area
of the carbon black was comparatively small. Therefore, the
hysteresis of the NR lled with N650 turned out to be the
smallest. The opposite situation happened to N330, and
the hysteresis of the NR lled with N330 turned out to be
the largest.
Hysteresis of an elastomer can be approximately
obtained from the loss tangent multiplied by input energy
[24]. In addition, the loss tangent is a function of the strain
amplitude, temperature as well as the type of carbon black.
As an example, the loss tangent of lled SBR has a critical
temperature around 0 8C below which it decreases but over
which it increases as the CTAB surface area increases [9].
Therefore, the ranking of hysteresis of the three lled NR
compounds could change at different temperatures, and the
hysteresis obtained from this study should be accepted with
caution.
2.4. Measurement of the critical J-value
Since the fatigue life depends on the growth of a crack,
which is related to the critical J-value, it is important to
investigate the effect of carbon black on the critical J-value.
Thus, the critical J-value of the NR compounds was
measured. Based on the method of Begley and Landes
[25], the critical J-value was measured using the dumbbell
specimen shown in Fig. 2 [26]. For each type of the NR
compound, a set of ve specimens were pre-cracked, the
crack length ranging from 1 to 3 mm, every 0.5 mm apart.
The specimen was stretched under the standard speed of
500 mm/min using UTM (Universal Test Machine).
The J-value can be calculated from the following
equation:
J ZK
1
B
vU
va

D
(1)
Here, B is the thickness of the specimen, U is the strain
energy, a is the crack length, and D is the displacement. The
J-value is the amount of decrease of the strain energy per
unit area of new crack surface with the displacement xed.
While the specimen was being loaded, it was video-
recorded by a digital motion camera. The moment when
the geometry around the crack became asymmetric with
respect to the crack line was regarded as the moment of the
crack growth [7], and the J-value at the moment was
assumed to be the critical J-value. Thus, the critical J-value
is the same physical quantity as the tearing energy [27].
The critical J-value remained almost the same regardless
of the pre-crack length, and the test showed a good
repeatability. Thus, only the average and the standard
deviation of the critical J-values for the NR compounds
obtained for three sets of ve specimens are shown in
Table 5. Note that the critical J-value is ranked in the
following order for the compound lled with N330, N990 or
N650, which is in the same order for the fatigue life and the
hysteretic loss. The critical J-value of the NR lled
with N330 is smaller by a factor of about 3 than that of
gum NR and lled NR measured by Chung et al. [8].
This difference stemmed from different denitions on
Table 4
DBPA number and CTAB surface area of N330, N650 and N990
N330 N650 N990
DBPA
a
(cm
3
/100 g) 100 129 35
CTAB
a
(m
2
/g) 84 38 9
a
Carbon black science and expanded. Marcel Dekker; 1993. p. 113.
Fig. 2. Dumbbell specimen used to measure the critical J-value (all
dimensions in mm).
Table 5
Critical J-value of NR compounds lled with N330, N650 or N990 (N/mm)
N330 N650 N990
Ave. 1.416 0.379 1.167
Std. 0.012 0.019 0.030
J.-H. Kim, H.-Y. Jeong / International Journal of Fatigue 27 (2005) 263272 266
the moment of the crack growth. The process of crack
growth can be described by two steps [8]. First, the crack
starts at one or two spots on the inside surface of the tip, then
it propagates across the thickness of the specimen to form a
full initial crack before it propagates along the width of the
specimen. In this study, the moment of the crack growth was
dened to be the time when the crack surface lost its
symmetry, but Chung et al. dened the moment to be the
time when a full crack through the thickness started to grow.
Thus, the crack growth dened in this study happened
earlier, and the critical J-values measured turned out to be
smaller.
2.5. Measurement of the fracture surface morphology
In general, fracture surface morphologies give infor-
mation about failure process and mechanisms [3]. As shown
in Fig. 3, the (large-scale) fracture surface morphologies of
the three types of the NR compounds look quite rough.
Thus, the stereo optical microscope that had a poor depth of
focus could not be used for the analysis of the fracture
surfaces. Instead, LG DSP color camera, a microscope for
the inspection of semiconductor, which had a good depth of
focus, was used and its magnication was from !100 to !
1000. The large-scale and the small-scale fracture surface
morphologies of the NR compounds are shown in Figs. 3
and 4, respectively. Figs. 3 and 4 show that the NR
compound lled with N330 or N990 has many small humps,
but the NR compound lled with N650 has a small number
of large humps. In other words, the NR compound lled
with N330 or N990 has a smoother surface in the large-scale
but a rougher surface in the small-scale than the NR
compound lled with N650.
To quantify the roughness of the fracture surfaces, the
prole of the fracture surfaces was obtained by using a
stylus type roughness tester, and the root-mean-square
(RMS) roughness was employed. Moreover, the RMS
roughness was calculated in two different scales. The
prole along the major axis of 14 mm long was obtained,
and the RMS roughness was calculated for the prole. This
roughness was named the large-scale roughness in this
paper. The prole of four 1 mm long segments along the
major axis was obtained, and the average of the roughness
of the four segments was assumed to be the RMS roughness
for the prole. This roughness was named the small-scale
roughness. The large and small-scale RMS roughness data
are shown in Tables 6 and 7, respectively. It is striking to
notice that the order of magnitude of roughness is opposite
to each other; the order of large-scale roughness is N650O
N990ON330, but the order of small-scale roughness is
N330ON990ON650.
Fukahori and Andrews [28] found out that the hyteresis
of highly deformable polymers decreased as the fracture
surface roughness increased. As shown in Fig. 5, the
hysteresis of the NR compounds studied in this paper
decreased as the large-scale roughness increased. However,
as shown in Fig. 6, the hysteresis increased as the small-
scale roughness increased. Therefore, when the roughness
of a NR compound is examined, the scale should be taken
into account, otherwise the conclusion would be opposite.
Fig. 3. Large-scale fracture surface.
Fig. 4. Small-scale fracture surface.
J.-H. Kim, H.-Y. Jeong / International Journal of Fatigue 27 (2005) 263272 267
Note also that the test data are located near the regression
line in Fig. 5, but they are located off the regression line in
Fig. 6. The poor linearity of the test data shown in Fig. 6
stemmed from the fact that the small-scale roughness was
obtained for four short proles, and it in itself had a high
variance relative to the average value (refer to Table 7). In
other words, the small-scale roughness is quantitatively less
reliable than the large-scale roughness. However, the trend
of the small-scale roughness is correct in that the small-scale
roughness increases as the critical J-value increases (refer to
Fig. 8). As Gent and Pulford [4] noted, vertical steps are
more frequent, higher and less spaced on the torn surfaces of
tougher elastomers, and the spacing is in the order of 10 mm.
Therefore, the small-scale roughness should be higher for
tougher elastomers.
2.6. Analysis of the carbon black distribution
The fracture surface was sliced to a thin sheet using a
glass knife in liquid nitrogen. Three locations on the thin
sheet were randomly selected to examine the carbon black
distribution using an optical microscope. Each location was
a square of 1 mm!1 mm, and it was divided into 10,000
cells. The dispersion of carbon black agglomerates was
examined, and Table 8 shows the percentage of cells in
which carbon black agglomerates were observed, proving
that they were well distributed in all three NR compounds.
Then, the number of cells in which an agglomerate of
carbon black larger than 50 mm
2
existed was counted, and
the diameters of those large agglomerates were also
measured. In Fig. 7, the number of cells is shown as a
function of the diameter of the agglomerates. In the rubber
compound lled with N330, an agglomerate with diameter
of 9 or 10 mm was observed in one or two cells. In the
rubber compound lled with N990, an agglomerate with
diameter of 9 or 10 mm was observed in seven or three cells,
Table 6
Large-scale RMS roughness data (mm)
N330 N650 N990
Ave. 0.311 0.771 0.425
Std. 0.012 0.027 0.066
Table 7
Small-scale RMS roughness data (mm)
N330 N650 N990
Ave. 0.095 0.028 0.045
Std. 0.040 0.008 0.017
Fig. 5. Hysteresis as a function of the large-scale roughness.
Fig. 6. Hysteresis as a function of the small-scale roughness.
Table 8
Carbon black dispersion data
N330 (%) N650 (%) N990 (%)
1 99.90 98.10 98.40
2 99.70 96.90 97.80
3 99.70 97.20 97.70
Avg. 99.77 97.40 97.40
Fig. 7. Diameter and frequency of carbon black agglomerates.
J.-H. Kim, H.-Y. Jeong / International Journal of Fatigue 27 (2005) 263272 268
and an agglomerate with diameter of 12 mm at highest was
observed. However, in the rubber compound lled with
N650, an agglomerate with diameter of 9 mm was observed
in ten cells, and even an agglomerate with diameter of about
15 mm was observed. This observation on the distribution is
compatible with the DBPA numbers shown in Table 4. In
the case of the NR compound lled with N650, for example,
the DBPA number is high. This means that the carbon black
is well developed, and the agglomerate of the carbon black
is big.
Knotty tearing is an important aspect of the reinforcing
mechanism of carbon black, and it results in a rough torn
surface and a high critical J-value [5]. For the NR
compounds studied in this paper, the critical J-value was
also high when the small-scale roughness was high, as
shown in Fig. 8. The rubber compound lled with N330 had
a rough surface in the small-scale, and its critical J-value
turned out to be high. This means that the carbon black,
N330, formed small agglomerates, which acted as a local
stress raiser. The small agglomerates deected the direction
of a crack growth causing the knotty tearing [29]. However,
the rubber compound lled with N650 had a clean surface in
the small-scale, and its critical J-value turned out to be low.
This means that the carbon black, N650, formed large
agglomerates, which were easily separated from the rubber
matrix. Thus, a crack propagated rapidly creating a cleaner
surface in the small-scale.
3. Function of the fatigue life
NR has good mechanical characteristics of large elastic
deformation and damping. In addition, it can be readily
manufactured at a comparatively low cost. Because of
these characteristics, rubber is widely used in numerous
products such as automobiles, locomotives and commod-
ities [30]. However, a rubber component is susceptible to
fatigue failure, and its durability is one of the major
concerns. Thus, when a rubber component is under
development using various compositions, the fatigue life
of the component is to be measured from a fatigue test,
which usually takes a long period of time. If the fatigue
life of a rubber component can be predicted from material
properties which can be obtained from simple exper-
iments, it can save time and efforts to select a composition
which results in the best durability.
By reviewing the experimental data obtained from this
study, it was easily noticed that the fatigue life increased
as the critical J-value or the hysteresis increased. After
trying many different functional forms, it was nally
noticed that the logarithmic value of the fatigue life was
linearly proportional to the square root of the product of
the critical J-value and the hysteresis. In Fig. 9, the
logarithmic value of the fatigue life is shown with respect
to the square root of the product of the critical J-value and
the hysteresis. For the case of N650 for which the value
of the square root was low, the fatigue life was also low.
In contrast, for the case of N330 for which the value of
the square root was high, the fatigue life was also high.
As mentioned previously, the fatigue life increased as the
displacement amplitude decreased. The regression lines
for the test data are also shown in Fig. 9, and it is
noteworthy that they t the test data well for all three
displacement amplitudes. Thus, the regression lines can be
expressed as the following Eq. (2)
logN
f
ZA
J
C
EL

Hysteresis
EV
1
2
CB (2)
Here, N
f
is the number of cycles at failure, J
C
is the
critical J-value, and A and B are proportionality constants
which are different for a different displacement amplitude.
Since the fatigue life is given in cycles, i.e. it is
dimensionless, the right-hand side of Eq. (2) should be
made dimensionless by dividing the critical J-value and
the hysteresis by some representative values, E, L and V,
Fig. 8. Critical J-value as a function of the small-scale roughness.
Fig. 9. Logarithmic value of the fatigue life as a function of
[(J
C
/EL)(hysteresis/EV)]
1/2
.
J.-H. Kim, H.-Y. Jeong / International Journal of Fatigue 27 (2005) 263272 269
of the rubber specimen. E is the representative Youngs
modulus of the rubber compounds, and it is given as a
function of IRHD (International Rubber Hardness Degree)
as long as the hardness of the rubber is between 30 and 85
IRHD [12,13]. In addition, hardness measured by
durometer type A is compatible with that in IRHD [12].
Since the NR compounds studied in this paper had the
same hardness, 62, the representative Youngs modulus
turned out to be 3.87 MPa. L was selected to be the radius
of the minor axis, i.e. LZ5 mm. In addition, V was
assumed to be the volume of the most deformable part of
the specimen, i.e. between K2.5 and C2.5 mm from the
middle plane of the specimen, and it turned out to be
549.78 mm
3
. However, note that as long as the same
specimen is used to evaluate the fatigue life, any
representative value can be used. Even if a different
representative value is used, the constant A will be
adjusted accordingly.
The constants A and B are shown with respect to the
double displacement amplitude D in Figs. 10 and 11,
respectively. Note that there is a linear relationship of A or B
to the double displacement amplitude. Thus, A and B can be
expressed as a function of D as shown in the following Eqs.
(3) and (4)
A Za CD
b
L
(3)
B Zc CD
d
L
(4)
Plugging Eqs. (3) and (4) into (2), the logarithmic value
of the fatigue life can be expressed as a function of the
critical J-value, the hysteresis, and the double displacement
amplitude as in the following Eq. (5)
logN
f
Z a CD
b
L

J
C
EL

hysteresis
EV
1
2
C a CD
d
L

Z0:623
J
C
EL

hysteresis
EV
1
2
d
L

K0:135
J
C
EL

hysteresis
EV
1
2
K4:878
D
L

C7:4 (5)
In order to evaluate the adequacy of the nal equation,
the equation is shown graphically along with the test data
for the amplitude of 16 mm (shown in Fig. 12), 19 mm
(shown in Fig. 13) and 22 mm (shown in Fig. 14). Note that
the equation is in good agreement with the test data for all
three amplitudes. In other words, the fatigue life can be
Fig. 10. Coefcient A as a function of the double displacement amplitude
(R
2
Z0.9777).
Fig. 12. Comparison of the fatigue life equation with test data for the double
displacement amplitude of 16 mm (R
2
Z0.9621).
Fig. 11. Coefcient B as a function of the double displacement amplitude
(R
2
Z0.9956).
J.-H. Kim, H.-Y. Jeong / International Journal of Fatigue 27 (2005) 263272 270
predicted from the displacement amplitude and the material
properties, the critical J-value and the hysteresis, which can
be obtained from simple tests. Therefore, it may be said that
when a rubber component is under development using
various compositions, a composition for which the product
of the critical J-value and the hysteresis is the highest will
result in the best durability.
In this study, the hysteresis was measured from the same
specimen and at the same deformation mode as the fatigue
life was evaluated. If hysteresis had been measured from a
different specimen or at a different deformation mode, the
fatigue life prediction equation (5) would not be in good
agreement with the test data mainly because hysteresis is
dependent on the strain amplitude and the load ratio [9,10].
Therefore, in order to predict the fatigue life based on the
critical J-value and the hysteresis, more reliable prediction
will be obtained if the hysteresis is measured at the same
deformation mode and for the same rubber component for
which the fatigue life is to be predicted.
4. Conclusion
In this paper, NR compounds lled with three types of
carbon black, N330, N650 and N990 were experimentally
investigated in order to evaluate the effects of carbon black
on the fatigue life, the hysteresis, the critical J-value and the
fracture morphology. By reviewing all the test data, the
following conclusions could be reached.
(1) The fatigue life, the hysteresis and the critical J-value
were ranked in the following order for the NR
compound lled with N330, N990 or N650.
(2) The small-scale roughness showed a trend opposite to
that of the large-scale roughness. The hysteresis or the
critical J-value increased as the small-scale roughness
increased.
(3) In the NR compound lled with N650, there existed
large carbon black agglomerates, which separated from
the rubber matrix comparatively easily. Thus, the
fatigue life of the NR compound lled with N650 was
shorter, and its fracture surface was cleaner in the small-
scale than that of the NR compound lled with N330 or
N990.
(4) The logarithmic value of the fatigue life of the NR
compounds was linearly proportional to the square root
of the product of the critical J-value and the hysteresis.
In addition, the proportionality constants were linearly
proportional to the double displacement amplitude.
Thus, the logarithmic value of the fatigue life could be
expressed as a function of the double displacement
amplitude, the critical J-value and the hysteresis.
Acknowledgements
The specimens were provided by Pyoung Hwa Industrial
Company, and some experiments were conducted at
Hankook Tire R&D Center. All of these supports are highly
appreciated.
References
[1] Lake GJ, Lindley PB. Ozone cracking, ex cracking and fatigue of
rubber. Rubber J 1964;146:309.
[2] Mars WV, Fatemi A. A literature survey on fatigue analysis
approaches for rubber. Int J Fatigue 2002;24:94961.
[3] Sawyer LC, Grubb DT. Polymer microscopy, 2nd ed. London:
Chapman & Hall; 1996.
[4] Gent AN, Pulford CTR. Micromechanics of fracture in elastomers.
J Mater Sci 1984;19:36129.
[5] Greensmith HW. Tear properties of vulcanizates containing carbon
black. J Polym Sci 1956;21:17587.
[6] Hess FM, Ford FP. Microcopy of pigmentelastomer systems. Rubber
Chem Technol 1963;36:1175228.
[7] Goldberg A, Lesuer DR, Patt J. Observations made during stretching,
tearing, and failure of NR and SBR loaded with various amounts of
carbon black. Rubber Chem Technol 1988;62:288304.
Fig. 14. Comparison of the fatigue life equation with test data for the double
displacement amplitude of 22 mm (R
2
Z0.9983).
Fig. 13. Comparison of the fatigue life equation with test data for the double
displacement amplitude of 19 mm (R
2
Z0.9825).
J.-H. Kim, H.-Y. Jeong / International Journal of Fatigue 27 (2005) 263272 271
[8] Chung B, Funt JM, Ouyang GB. Effect of carbon black on elastomer
ultimate propertiesIR compounds. Rubber World 1991;204:4651.
[9] Wang MJ. Effect of polymerller and llerller interactions on
dynamic properties of lled vulcanizates. Rubber Chem Technol
1998;71:52089.
[10] Legorju-jago K, Bathias C. Fatigue initiation and propagation in
natural and synthetic rubbers. Int J Fatigue 2002;24:8592.
[11] ASTM D1765. Standard classication system for carbon blacks used
in rubber products.
[12] ASTM D1415-88. Standard test method for rubber property
international hardness.
[13] Hawley SW. Anomalies in ISO 48, hardness of rubber. Polym Test
1997;16:32733.
[14] ASTM D2240-97. Standard test method for rubber property
durometer hardness.
[15] ASTM D575-91. Standard test methods for rubber properties in
compression.
[16] Takeychi K, Nakagawa M, Yamaguchi H, Okumoto T. Fatigue test
technique of rubber materials for vibration insulators and their
evaluation. Int Polym Sci Technol 1993;20(10).
[17] Mathew NM, Bhowmick AK, De SK. Chemical and scanning electron
microscopy studies on fatigue failure of natural rubber. Rubber Chem
Technol 1982;55:5161.
[18] Young RJ, Lovell PA. Introduction to polymers. London: Chapman &
Hall; 1991.
[19] Mullins L. Softening of rubber by deformation. Rubber Chem
Technol 1969;42(1):33962.
[20] Mark JE, Erman B, Eirich FR. Science and technology of rubber.
New York: Academic Press; 1994. p. 387418.
[21] ASTM D2414-00. Standard test method for carbon black-n-dibutyl
phthalate absorption number.
[22] ASTM D3765-99. Standard test method for carbon black-CTAB
(cetyltrimethylammonium bromide) surface area.
[23] Lee BC. Effect of carbon black on the reinforcement and vibration
damping of rubber vulcanization. Korea: Chungbuk National
University; 1997 p. 703.
[24] Wei YT, Tian ZH, Du XW. A nite element model for the rolling loss
prediction and fracture analysis of radial tires. Tire Sci Technol,
TSTCA 1999;27(4):25076.
[25] Begley JA, Landes JD. The J-integral as a fracture criterion. ASTM
STP 514. Philadelphia: American Chemical Society for Testing and
Materials; 1972 p. 120.
[26] ASTM D412-98a. Standard test method for vulcanized rubber and
thermoplastic elastomers-tension.
[27] Rivlin RS, Thomas AG. Characteristic energy for tearing. J Polym Sci
1953;10:291318.
[28] Fukahori Y, Andrews EH. Fracture surface roughness in highly
deformable polymers. J Mater Sci 1978;13:77785.
[29] Lee DJ. Fracture, aging and microstructural changes in carbon
black lled natural rubber.: University of Massachusetts; 1987.
p. 10820.
[30] Treloar LRG. The physics of rubber elasticity. Oxford: Clarendon
Press; 1975.
J.-H. Kim, H.-Y. Jeong / International Journal of Fatigue 27 (2005) 263272 272

You might also like