Accepted Manuscript

Recent advances on fatigue of rubber after the literature survey by Mars and
Fatemi in 2002 and 2004

Yun Lu Tee, Mei Sze Loo, Andri Andriyana

PII: S0142-1123(18)30008-2
DOI: https://doi.org/10.1016/j.ijfatigue.2018.01.007
Reference: JIJF 4536

To appear in: International Journal of Fatigue

Received Date: 29 August 2017

Accepted Date: 8 January 2018

Please cite this article as: Tee, Y.L., Loo, M.S., Andriyana, A., Recent advances on fatigue of rubber after the
literature survey by Mars and Fatemi in 2002 and 2004, International Journal of Fatigue (2018), doi: https://doi.org/
10.1016/j.ijfatigue.2018.01.007

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Recent advances on fatigue of rubber after the literature survey by
Mars and Fatemi in 2002 and 2004
Yun Lu Teea , Mei Sze Loob , Andri Andriyanab,∗
a
Department of Civil Engineering, Faculty of Engineering, University of Malaya, 50603 Kuala Lumpur -
Malaysia
b
Centre of Advanced Materials, Department of Mechanical Engineering, Faculty of Engineering, University
of Malaya, 50603 Kuala Lumpur - Malaysia

Abstract
Subjected to multiaxial mechanical loading and hostile environment, rubber experiences
degradation over a period of time. Therefore, it is of utmost importance to prevent failure
of rubber components during the service. As highlighted in Mars and Fatemi [Mars, W.V,
Fatemi, A., 2002. A literature survey on fatigue analysis approaches of rubbers. Int. J.
Fatigue 24, 949-961; Mars, W.V, Fatemi, A., 2004. Factors that affect the fatigue life of
rubber: A literature survey. Rubber Chem. Technol. 77, 391-412], a large number of works
focused on the durability of rubber. Furthermore, it has been expanding rapidly until today.
For this reason, the present work focuses on collecting and analyzing the vast amount of
works on fatigue of rubber conducted in the last 15 years since the review of Mars and
Fatemi in 2002 and 2004. To this end, three bibliographic databases are consulted: Google
Scholar, Scopus and Web of Science. The collected works are analyzed with the objective
to identify the current and future trends and needs in the study of rubber fatigue.
Keywords: Rubber; fatigue; fracture; crack; life prediction

∗
Corresponding author. Fax: +60 3 79 67 53 17
Email address: andri.andriyana@um.edu.my (Andri Andriyana)
Preprint submitted to International Journal of Fatigue January 5, 2018
1. Introduction
Rubber is widely used in many applications due to its excellent mechanical properties.
Some of the common applications are tyre, gaskets, hoses and vibration isolators. During
its service, majority of rubber components undergo fluctuating loading which could lead to
fatigue failure. Hence, the study of fatigue in rubber becomes highly essential. In general,
rubber fatigue involves a period during which cracks initiate due to fluctuating loading in
regions that were initially free of observable flaws, followed by a period during which nucle-
ated cracks grow to the point of failure. Along this line, two distinct approaches in fatigue
analysis of rubber are available [1]: crack nucleation and crack propagation approaches. In
the crack nucleation approach, the end-of-life is experimentally defined as a loss of mechan-
ical stiffness, the occurrence of small cracks or complete rupture [2, 3, 4, 5, 6]. It is based
on quantities defined at each material point in the sense of Continuum Mechanics and the
crack initiation location is part of the fatigue life estimation process. The crack propagation
approach is used when the initial crack shape and position are known. The crack growth
is estimated through the calculation of the tearing energy. This approach is suitable to the
case where rubber components should be able to sustain crack propagation before failure
[7].
Due to the importance of preventing fatigue failure of rubber components in service,
works focusing on durability of rubber has been significantly increasing in the past few
decades. Focusing on the past fifteen years since the literature survey conducted by [1],
almost 200 papers related to rubber fatigue have been published as can be consulted in Figure
1. In this figure, the data are obtained from three bibliographic databases: Google Scholar,
Scopus and Web of Science using fatigue, lifetime, rubber, predictor and swelling as the
main keywords in the searching tool. The finding clearly shows the current needs for better
understanding and prediction of the fatigue failure in rubber materials. Motivated by this
finding, the present work focuses on analyzing the vast amount of works on fatigue of rubber
since 2002 with the main objective to identify the current and future needs and trends in the
world of rubber fatigue. To this end, the paper is organized as follows. In Section 2, different
types of specimens used for fatigue analysis in rubber are recalled. Fatigue life predictions
found in the literature is explored in Section 3. It covers two approaches: crack nucleation
and crack propagation approaches. The application of respective predictor are discussed.
Section 4 is devoted to fractography studies. Crack nucleation and crack propagation regimes
are reviewed. Factors affecting fatigue lifetime are presented in Section 5. Mechanical
loading conditions, chemical compositions and environmental conditions which contribute
to the lifetime of rubber are discussed. Section 6 highlights the perspective and future trend
of this field. Finally, Section 7 closes the paper.

2. Fatigue specimens and tests

From the experimental point of view, the guidelines for the fatigue test procedure and
sample geometry are established in ASTM D4482 and ISO standards. Nevertheless, these
standards are frequently not sufficient to test rubber components under real service condition

2
 Figure 1: Publications on rubber fatigue from 2002-2017.

such as under multiaxial loading. In fact, the existing standards confined the dumbbell
specimen as the only geometry of sample for fatigue test. Hence, most of the proposed
experimental fatigue works do not adopt the available standards. Researchers have proposed
a number of geometry specimens to be used in fatigue tests. These specimens are designed
with the objective to meet the complexity of various testing conditions. Indeed, the specimen
geometry is crucial and needs to be customized for an accurate result interpretation.
Following the classification of approaches in fatigue analysis, two types of specimen ge-
ometry used for fatigue test are available: crack nucleation and crack propagation specimens.
The corresponding summary of specimens is shown in Figure 2. In this figure, specimens
employed in the study of crack nucleation are diabolo, dumbbell, circular cylinder, hollow
cylinder and disk specimen. Dumbbell and diabolo are often used to describe the specimen
with cylindrical shape having larger radius at both ends while smaller radius at the center
[8]. Some researchers also named it as hourglass specimen or dumbbell cylindrical specimen
[9, 10, 11]. To avoid confusion, this type of geometry will be referred to as diabolo specimen
in the present paper. The precise dimension for diabolo specimen is unclear as none of the
available standards use it for fatigue test. Cadwell and his team [12] studied the fatigue
of rubber in 1940 using diabolo specimen. Beatty [13] extended the work by Cadwell and
his co-worker [12] and named the specimen as dumbbell of revolution to perform tensile-
compression fatigue testing. This geometry gives the advantage of controlling the crack to
appear at the center of the specimen. The thinner central section is able to prevent high
thermal gradient between the surface and the core of the specimen [14]. Flamm et al [15]
mentioned that the diabolo specimen had similar manufacturing process and comparable
3
Figure 2: Geometry of fatigue test specimens.

4
volume with the industrial rubber component. In most of experimental works, both ends of
the specimen are attached to the metallic plates for experimental assembly purpose. Con-
sequently, the applicable load is limited. Failure of the material near the bonding zone
with the metal plates instead of the center are commonly found, especially at high loadings.
Le Cam et al [16] explained that the occurrence of cracks below the metal plates highly
depends on the mean load. In a high level of loading, with the loading ratio R between
0 and 1, small cracks appeared at the specimen feet below the metal plates. This is due
to the large number of crystallites induced crack branching at the median section or below
the metal plates. Takeyuchi et al [17] proposed another diabolo specimen with an elliptical
cross-section instead of circular cross-section. Disk samples were used in the bubble inflation
test in the work by Zhou et al [18], Hanley [19] and Jerrams [20]. This type of specimen
allows high reversible stretch ratios in equi-biaxial extension loading condition.
In crack propagation approach, a crack with specific length is first introduced in the
specimen before the specimen is subjected to fatigue test. Some of the commonly found
geometry specimens used in this approach are shown in Figure 2. Gdoutos et al [21] have
conducted an experiment using trousers specimen with shims to determine the critical tearing
energy of rubbers. The thin metal shims were boned at the opposite side of the specimen
legs to prevent crack path deviation and unstable crack growth. This method was originated
in the work of Gent and Herry [22]. Semicircular bend specimens were used by Mull et al
[23]. The specimens were obtained by slicing a cylindrical standard gyratory compacted core
into four equal sections. The four sliced specimens originated from one single core produces
a less scattered results. Other specimens used in crack propagation test are flexing specimen
with semicircular groove [24], angle test piece [25], and peeling specimen [26]. No artificially
initiated tear was created on these specimens, but the geometries introduced a region for
crack appearance.
As mentioned in the Introduction, the total fatigue life of a component can be analyzed
through crack nucleation and crack propagation approaches. Based on these two approaches,
the end-of-life of material needs to be defined. Yet, no universal criteria are established to
define the lifetime of material. Indeed, the fatigue data obtained in different experimental
work is dependent on the criteria used to determine the end-of-life of the specimen. In
general, three ways were commonly found in literature to define the end-of-life. Firstly,
complete rupture is used to define the end-of-life of material for both crack nucleation and
propagation approaches. It was observed that time to crack nucleation occurrence is around
90-95% of the total test time, which is close to the time for complete fracture. Therefore it
can be seen that in some occasion, complete fracture is taken as the end-of-life [8, 11, 27].
A specimen with small volume is more suitable in such condition for the sake of feasibility
[12, 28]. Secondly, the end-of-life is considered as the occurence of crack with a certain size.
Mars [29] defined the crack size as the material failure by observing a drop of 15% load from
the stabilized stress response at the 128th cycle [29, 1]. Meanwhile, other researchers adapted
the load drop criteria as their end-of-life definition [30, 31, 32]. Lastly, the end-of-life defined
by effective stiffness was introduced by Ostoja-Kuczynski and Charrier [33]. The definition
is applicable for both displacement and load-controlled experiments. It is defined as the
ratio of maximum force to maximum displacement measured during a cycle. This criterion
5
was used by Le Cam et al [16] to observe the crack nucleation and complete fracture of a
diabolo specimen. Seichter et al [34], analyzed all of the three criteria in their work and
finally chose the effective stiffness as the end-of-life criterion. They justified their choice as
the simplest and most reliable.
Data obtained from the fatigue test may be represented differently. S-N curve, Wöhler
curve and Haigh diagram are the common representation of fatigue data. S-N curve is
typically plotted on a log-log scale of stress vs fatigue life, Nf . Fatigue life of rubber is often
presented in the form of Wöhler curve, where maximum stretch or strain energy is plotted
against fatigue life, Nf . Each curve represents the evolution of the lifetime under a specific
loading condition. One of the earliest work which presented the fatigue life of rubber using
Wöhler curve was found in the work of Roelig and Fromandi [35]. Haigh diagram is initially
a plot of stress amplitude vs mean stress which can be seen in the work of André and his co-
worker [2]. The curve shows the influence of the parameters on a specific lifetime. Fatigue life
predictions can be estimated with the curves obtained from the fatigue experimental data.
Recently, Haigh diagram is also plotted using other mechanical variables such as strain [16].

3. Fatigue life predictions

Fatigue life prediction of rubber is important to ensure the safety and reliability of rubber
during service. Motivated by the interest, researchers estimate the fatigue life of rubber using
different mechanical quantities, commonly known as the predictor in literature. Numerous
amount of works related to the fatigue prediction have been reported which can also be
categorized into crack nucleation and crack growth approaches.

3.1. Crack nucleation

The crack nucleation approach follows the work of Wöhler [36]. It was first applied to
rubber by Cadwell et al [12]. It considers that fatigue life of rubbers can be determined from
the history of strain and stress at each material point in the body. The most widely used
predictors for fatigue crack nucleation in rubber are presented in the following.

3.1.1. Strain-based predictor

Strain is often used as a variable in rubber fatigue experiments as it can be directly
determined from the imposed displacement which can be measured easily [1]. Cadwell et
al [12] studied fatigue life of NR and found the lifetime improved with increasing minimum
strain under constant strain amplitude. Fielding [37] had a similar conclusion with Cadwell
et al [12]. Suryatal et al [38] used maximum principal strain to predict the lifetime of
elastomeric pad made from chloroprene rubber under compressive loading. They found that
as the compressive load increases, the maximum principal strain increases while fatigue life
decreases. It has been mentioned by Mars [1] that compressive loading along one direction is
often associated with simultaneous shear and or tensile loading in different directions. It is
worth to note that maximum principal strain and strain energy density may not be accurate
for compressive loading predictions as crack closure was not included [1]. Li et al [32] applied
Mooney-Rivlin model in the analysis with maximum principal strain as the predictor. The
6
prediction is in good agreement with the fatigue test results. While the above mentioned
experimental works showed positive results, Ro [39] concluded that maximum principal
strain is not suitable for unifying multiaxial fatigue data for NR. Ayoub et al [40] subjected
styrene-butadiene-rubber (SBR) to tension, torsion and combined tension-torsion loadings.
They revealed that maximum principal strain was unable to produce accurate estimation of
lifetime. Similar conclusion was made by Alshuth and co-workers [41].
The Green-Lagrange strain was used to predict fatigue life of NR diabolo specimen by
Kim et al [42] and Woo et al [43]. Comparing with the strain energy density approach, the
Green-Lagrange strain was able to show better correlation of the prediction. This good cor-
relation was further validated by Woo and his team who investigated the rubber performance
under different temperature conditions.

3.1.2. Stress-based predictor

Continuum Damage Mechanics (CDM) is considered as an effective stress-based damage
evolution rule [44]. Wang et al [45] and Miehe et al [46] showed that CDM approach is
suitable for predicting lifetime of elastomeric materials. Ayoub et al [47] developed a CDM
combined with the Cracking Energy Density (CED) model of Mars [48] for multiaxial loading
under both constant and variable amplitudes. It was further investigated by considering
the effect of load ratio [49] and verified by Ayoub et al [40]. Brunac et al [50] proposed
Dang-Van-like approach which took into account variables related to stress. The work was
presented to overcome the limitation of strain-based and energy-based predictors. André
et al [2] showed that this approach is able to describe multiaxial fatigue damage which is
dependant on the largest principal stress. On the contrary, Abraham et al [51] stated that
stress criterion is not sufficient to predict the lifetime of elastomer as the fatigue life of
non strain-crystallizing rubber decreases when the minimum stress is zero but with varying
maximum stress. Similarly, Alshuth et al [41] found that the lifetime of rubber decreases with
zero minimum stress and varying stress amplitude. However, longer lifetime was observed
at higher stress value with increasing minimum stress and constant stress amplitude. Due
to the ambiguity, Alshuth et al [41] concluded that stress criterion should not be used to
predict fatigue life of elastomers. Saintier and his team [6] predicted fatigue life of NR
using Cauchy stress tensor but found that it is not accurate. Instead, it was found that
critical plane approach was able to predict the fatigue life, locate the crack initiation site
and orientation. The main drawback of this approach is its inability to include the size or
gradient effect.

3.1.3. Energy-based predictor

Strain energy density (SED) is chosen as a predictor when the energy release rate is
proportional to the strain energy density and crack size [52]. It is an approach to predict
the fatigue crack nucleation under simple loading condition [48, 52, 53, 54]. Being a scalar
quantity, it does not provide information on the orientation of nucleated crack. It is a
common approach used by researchers to predict fatigue crack nucleation life due to its
simplicity. Zine et al [27] showed that this approach predicted the response of rubber under
uniaxial tensile and pure shear loading conditions. However, Ayoub et al [40] reported that
7
this approach could not unify the multiaxial fatigue data of SBR. Moon et al [31] utilized
maximum principal strain and strain energy density obtained from FEA to predict the
lifetime of diabolo specimens. They found that the predicted lifetime is underestimated,
probably due to shear deformation. They suggested that normal strain and shear strain
should be included for better accuracy. Meanwhile, Kim et al [42] found that SED approach
predicted longer lifetime than experimental result. They explained the overestimation of
SED approach may due to the variation of material property during manufacturing process
and underestimation of local strain in their finite element analysis.
Mars [48] proposed a new predictor, referred to as the Cracking Energy Density (CED).
It is the stored elastic energy density that is available to a crack on a given material plane,
and can be calculated for an arbitrarily complex strain history. His proposal emphasized
two important features: critical plane and energy release rate. The author showed that this
predictor is capable to unify multiaxial fatigue data. Along this line, a number of works in
the literature adopted this proposal. Indeed, Harbour et al [55] applied this approach and
found that it was effective in predicting fatigue life of NR and SBR under constant amplitude
loading. Zine et al[8] further confirmed the superiority of CED criterion over SED.
In an attempt to improve the theoretical foundation of CED using a well-established
theoretical framework, Verron and Andriyana [53] adopted the Configurational Mechanics
theory. More precisely, authors related the energy released during defects growth to the
properties of the configurational stress tensor. Some progress was made in pursuing it [56].
The proposed predictors appeared to be able to unify multiaxial fatigue data [57] and to
predict the well-known fatigue life improvement observed in natural rubber under positive
minimum stress [58]. Previati and Kaliske [59] utilized different predictors in the study
of multiaxial loading in pneumatic tires, and reported that the configurational mechanics
approach is able to distinguish between different load cycles. This was advantageous when
a particular load cycles was needed for detail examination. However, Ayoub et al [47]
reported that the predictor was unable to unify the experimental data for tensile and torsion
experiments. As strain energy density was unable to show good agreement, configurational
mechanics which consists of SED effect showed similar trend as well.
The use of dynamic stored energy was also explored in the literature [41, 60]. This
predictor appears to be promising for fatigue life prediction of EPDM materials [41]. This
approach was also used in the prediction of magnetorheological rubber under equi-biaxial
loading [61].

3.1.4. Damage rule

Miner’s linear damage rule proposed by Miner [62] is a cumulative damage model to
calculate the total damage caused by a series of applied cycles. Failure is predicted when
the sum of number of cycles applied, Ni , divided by number of cycles to failure Nf equals
to 1. It is suitable to predict fatigue lifetime of rubber subjected to various amplitude
loading condition. Harbour et al [55] showed that the predicted fatigue life from Miner’s
linear damage rule with combination of maximum normal strain and cracking energy density
exhibited good correlation with the experimental result for NR but weaker for SBR. They
accounted the difference due to crack development of the materials where NR produced a
8
large number of crack compared to SBR. In line with Harbour [55], Zarrin-Ghalami and
Fatemi [63] proved that Miner’s rule worked effectively in the prediction of NR specimens
under variable amplitude loading condition. A modification of Miner’s linear damage rule
commonly used for the fatigue of metals was proposed by Jardin et al [64] for elastomers
based on continuum damage mechanics. This modification allows the change of sign when
there is a reversal in loading sequence.

3.2. Crack growth

In most of fatigue analysis, crack propagation approach is used by performing either one
of the followings:

• Pre-cracks are introduced in rubber samples before fatigue tests.

• Crack growth from initial defects in rubber are considered with information on defects
localization or size.

The crack growth approach can be used as a total life approach, where the total fatigue life
consists of the growth of pre-existing flaws to fracture. Mars and Fatemi [4] explained that
the advantage of crack growth approach over the crack nucleation comes from its ability
to avoid unintentional and uncontrolled flaws during the tests. In fact, the entire range
of fatigue behaviour can be characterized using a small number of specimens with crack
growth approaches when compared to the numerous amount of individual tests needed for
crack nucleation.
Fracture mechanics have been the basis of crack growth approach and the energy re-
lease rate is one of the essential component to predict fatigue lifetime. Mars and Fatemi [1]
have provided an extensive review on the energy release rate, detailing from its origin until
its application by other researchers. They later noted that the fatigue crack growth rate
da/dN (a is crack tip position; N is the number of cycles) in strain crystallizing rubbers
depends not only on the maximum energy release rate experienced during a loading cycle,
but also on the minimum. This in fact placed the loading ratio, R, as a highly influential
factor towards the fatigue lifetime. Therefore, Mars and Fatemi [65] proposed a simple phe-
nomenological model to capture the effect of R ratio on fatigue behavior based on several
characteristic features exhibited by the data from strain crystallizing rubbers. Asare and
Busfield [66] validated the fracture mechanics approach when they successfully predicted
the fatigue crack growth behaviour at both room and high temperature. In fact, the cyclic
stress softening associated with fatigue of filled rubber was quantitatively accounted, for
the first time. Meanwhile, Papadopoulos et al. [67] used strain energy release rate as the
variable to characterize the rate transitions of fatigue crack growth behavior in NR and
SBR. Later, they proposed an efficient mathematical equation to predict the propagation
rate even though the rate fluctuates. Aı̈t-Bachir [68] derived the energy release rate of a
center-cracked region, specifically under arbitrary far-field homogeneous multiaxial loading
conditions with Configurational Mechanics. Their work focused on the steady-state crack
growth with the condition that the damage zone does not reach the boundary of the domain.
The relevance of their approach was demonstrated through its ability to frame and prove
9
the widely held view that the energy release rate of a small crack is proportional to the size
of the crack, irrespective of the state of loading or the orientation of the crack. Fukahori
et al. [69] explained the transition in the relationship between critical strain energy release
rate and critical crack growth rate in terms of elasticviscous transition phenomenon. The
new introduced elasticviscous transition diagram consists of three zones; elasticbrittle frac-
ture zone, a viscousductile fracture zone and an intermediate transition zone between the
elastic and viscous zones. The transition zone characterized by stickslip motion is caused
in mechanics as results from unstable fluctuations of crack growth rate due to the energy
dissipation near the glass transition temperature. At the same time, Netzker et al. [70]
analyzed the fracture behavior of rubber materials based on a global energy balance. They
revealed that the energy losses are due to the increase of a dissipative zone rather than the
limited stable crack propagation zone. Saintier et al. [71] suggested that crack nucleation is
a better approach for multiaxial loading conditions especially when the crack locations are
unknown. Besides that, the condition is more complex when strain crystallization induces
reinforcement in rubbers. They showed that if large strain conditions are correctly taken
into account, cracks are found to propagate systematically in the direction given by the
maximal first principal stress reached during a cycle, even under non-proportional loading.
A very recent work by Marco et al. [72] related the fatigue lifetime to the dissipation and
the defects population for carbon black filled NR. The fatigue criterion was built, assuming
that the ratio between the global energy dissipated and the energy related to the fatigue
mechanisms to be driven by the crack surface density.

3.2.1. Engineering applications

This approach was later adapted by researchers to analyse the fatigue in tires [21, 59,
73, 74, 75, 76, 77]. Schubel et al. [73] provided a detailed method to characterize the fatigue
behaviour in tire rubber subjected to tension-tension loading. They estimated the fatigue
life to be 8.1 million cycles after determining the critical tearing energy value of 34.8 N/mm.
At the same time, Gdoutos et al. [21] reported a similar critical tearing energy value (35
N/mm) for the same rubber blend. Chou and Huang [78] have investigated the effects of
the heat aging, temperature and belt stiffness on the fatigue lifetime of tire. They have
shown that the temperature has a greater effect on the tearing energy instead of the belt
stiffness. Therefore, it was suggested that the fatigue life of tire can be improved if the critical
tearing energy has an immunity towards temperature. Apart from tires, researchers have
also applied fracture mechanics for other real life engineering components such as disk [79],
sprung railway wheels [80], V-ribbed belts [81], shock absorbers [82] and circular bearings
[78].
The application of J-integral in fatigue analysis still remain as a worthy field of study
among researchers. Sundararaman et al. [81] modelled a fatigue crack growth based on J-
integral representation of the tearing energy to establish limits on growth size of initial small
flaws in V-ribbed automotive belts. Zhu et al., Nait-Abdelaziz et al., Previati and Kaliske
[76, 83, 59] have used J-integral as the lifetime predictor. Previati and Kaliske [59] related
the integral to material forces and compared it to other continuum mechanics predictors,
which is maximum stretch, maximum stress, strain energy density and configurational stress.
10
Among all the predictors, the configurational stress stood out for its ability to distinguish
between different load cycles with the same maximum load. Nait-Abdelaziz et al. [83]
assumed that the fracture is induced by the intrinsic defect and is controlled by the critical
value of J. A fracture criterion was derived based upon this assumption to predict the
failure of rubber parts under biaxial monotonic loading. Dong et al. [84] have predicted the
fatigue properties of silica/CB/NR composites using critical J-value.
A very recent work by Xiang et al. [85] utilized a back-propagation artificial neural
network (BP-ANN) model to predict fatigue property of natural rubber (NR) composites.
Their model consists of fatigue life, three mechanical properties (stress at 100%, tensile
strength, elongation at break),and hysteresis (tan at 7% strain) was established to predict
the tensile fatigue life of the NR composites which showed an average prediction accuracy of
97.3%. Demassieux et al. [86] improved further the work of Gent and his co-workers [79, 87]
by limiting the abrasion of cracked surfaces under small mode I opening of the crack. They
have demonstrated that crack growth laws under mode I and mode III coincide for high
fracture energies.

3.2.2. Recent advance test method

The two most commonly used specimens in rubber fatigue crack growth studies are the
single edge cut planar tension specimen and single edge cut simple tension specimen [1].
South et al. [88] revealed that these common geometries produced a condition of plane
stress. The plane stress geometry creates a difficulty during the interpretation of plane
stress data if the test has to be stopped and a new starter crack needs to introduced into the
sample. This difficulty arises because of the unfavoured crack propagation direction during
the fatigue test. Therefore, they have compared the crack propagation of natural rubber
using a double cantilever beam (DCB) specimen and the traditional single edge notch test
specimen. The DCB rubber is adhered in between two aluminium adherends and the critical
strain energy release rate values were calculated. The fatigue crack growth rate was found
to be approximately two orders of magnitude faster than those obtained from the traditional
single edge notch test specimen. They inferred from the data that cracks grow faster under
a state of plane strain rather than plane stress. Later, Hamdi et al. [89] developed a new
failure criterion for three kinds of rubber under plane stress conditions, without introducing
any crack in the initial state.
The usual automatic operating fatigue testing systems utilizes the crack length shadow
images of rubber specimens to evaluate the crack growth. However, this system is only
accurate if there are no deviations of the crack path. Recently, researchers have been re-
fining their experimental set ups to overcome such limitation. Kaang et al. [90] developed
an advanced test methodology by using a high speed CCD color camera in a temperature-
controlled chamber. The newly designed machine was able to measure the in-situ length
of crack and provided plots the crack length as a function of number of cycles. Stadl-
bauer et al. [91] focused their measurement set up for two different geometries subjected to
tension-compression loading conditions. The deviations in crack shape and path under such
conditions motivated the team to extend a measurement set up by capturing images from
the front and back side of the sample, with additional fully illuminated images. A com-
11
plementary thermal imaging system was also used to determine the heat build-up. They
deduced that specimen with pure shear geometries were preferred rather than faint waist
pure shear for accurate tearing energy values.
Brüning et al. [92] measured the local degree of crystallinity around a crack tip in
natural rubber under dynamic load by time-resolved scanning wide-angle X-ray diffraction
(WAXD). They demonstrated that under dynamic conditions, the crystallinity around the
crack tip is reduced as compared to static conditions. Around the same time, Rublon
et al. [93] built a home-made mechanical fatigue machine coupled with wide-angle X-ray
scattering to measure the crystallinity distribution around a fatigue crack tip. This set up
was later extended to measure principal strain directions and change in thickness around
fatigue cracks in natural rubber [94]. Their result discussion emphasized the influence of
crystallinity on crack growth in filled elastomers leading to the remarkable fatigue crack
growth resistance in natural rubber. The authors’ work gained creditability after validating
their results with the conventional digital image correlation method. They were the first
to establish a simple relationship between the tearing energy and the crystallized volume
in the vicinity of the crack tip. Meanwhile, Weng et al. [95] adapted X-ray scattering in
small angles to investigate the effect of silica nanoparticles on the crack growth mechanism
of styrene-butadiene rubber. They found that the damage nucleation is the key factor for
the crack growth in large tear energy range, while the growth feature of damage structure
dominates the crack growth in smaller tear energy range.

3.2.3. Crack growth in viscoelastic solids

Mars and Fatemi [1] highlighted that the J-integral does not uniquely characterize lo-
cal crack tip conditions considering that the stress-strain behavior of rubber is strongly
viscoelastic. Indeed, the viscoelastic behaviour of rubber imposed a major challenge for
researchers to characterize its complex behaviour. The time-dependent path-integral ap-
proach developed by Schapery [96, 97] have yet been applied to rubbers. However, Persson
et al. [98] studied the energy released rate, G, of the crack propagation from the viscoelastic
deformations of rubber-like materials. The G was shown to be dependent on the crack tip
velocity, v, and on the temperature, T, by Gent and Schultz [99]; Maugis and Barquins [100];
Gent [101]; Greenwood [102]; Persson et al. [98]; Carbone and Persson [103] as
G(ν, T ) = G0 [1 + f (ν, T )] (1)
where f → 0 as ν → 0. G0 is a threshold value below which fracture does not occur.
Persson et al. [98] presented a qualitative discussion on the contribution of viscoelastic
energy dissipation at crack tip front and the bond-breaking processes at the crack tip to
crack propagation energy in Equation 1. In this equation, the velocity is highly dependent
on the derivation from factor f (v, T ), where the Gmay be enhanced by a factor 103 or more
during high crack tip velocities. The crack propagation energy G will generally depend on
the exact nature of the processes occurring in the crack-tip process zone. The standard model
used to describe the crack-tip process zone was founded by Barenblatt [104]. He assumed
that the bond breaking at the crack tip occurs by stretching the bonds orthogonal to the
crack surfaces until they break at some characteristic stress level. Persson and Carbone
12
[105, 103] compared their work with Barber et al. [106] who adopted the Barenblatt model
for crack propagation in viscoelastic solids. They found Barenblatt model consisted of
complex equations and proposed a simpler approach based on energy conservation. Later,
they proved that the two models gave similar results in spite of the different treatment
of the crack-tip process zone leading to the assumption that the exact nature or shape of
the crack-tip process zone is not important for the velocity dependence of G(v). Damico
et al.[107] recently proposed a novel set up to measure G with a square sample tear test,
instead of the tensile or pure shear specimen test. This proposition was to overcome the
limitations of the two aforementioned tests by guaranteeing a precise measurement of the
energy release rate G and, at the same time, to allow the full development of the annular
viscoelastic dissipative region around the crack tip. On the other hand, Heinrich et al.
[108] simulated the tear fatigue analyzer (TFA) tests on rubber with a mesoscopic model
combined of self-similar crack propagation and a complex viscoelastic rubber model (flow-
enhanced linear standard solid). This combination consisted three physical concepts: (i)
self-affine crack propagation, (ii) stress intensity factor (crack tip opening displacement),
and (iii) Eyring-like flow-enhanced neo-Hookean standard solid as a representative of the
rubber solid.

4. Fractographic studies
The general fractographic study can be done by observing the appearance of the fatigue
fracture surface on the specimen. Figure 3 is the proposed schematic view of three different
regions at macroscale which can be observed on the fracture surface of rubber. In this figure,

Figure 3: Schematic view of three different regions on fracture surface of rubber. A: Crack initiation, B:
Crack propagation, C: Final failure.

the crack initiation point and corresponding morphologies can be identified at the region
labelled as A. As the crack grows, the crack pattern can be distinguished from initiation at
region B. Finally, the final failure damage characteristics is studied at region C. However,
the study of the fracture surface morphology alone is not sufficient to identify the exact
13
phenomena involved in crack propagation or to explain fracture chronology. Thus, the frac-
tographic studies appears to be more complete when the study includes pattern recognition
at microscales. The microstructure of fatigue damage depends on three basic mechanisms:
chemical (composition, crystallization), environmental (oxygen) and mechanical (stretching,
triaxial stresses) [109]. Some of the common encountered morphologies for filled vulcanized
rubbers are cracks, striations [15, 110, 111, 112, 113], dimples [114, 115, 116, 117], tongues
[15, 109, 118], stick-slip [21, 88] and rubber balling [114, 119].

4.1. Crack initiation regime

Cracks occurring at the initiation stage are usually due to intrinsic flaws which existed
in the un-deformed material. These flaws can only be characterised by microscopic methods
such Scanning Electron Microscope (SEM) or FESEM. Hainsworth [120] identified crack
nucleates at the sample surface while other researchers found flaws at sub-surfaces [109, 121,
122]. Some of the common identified flaws are discussed in detail in the following subsections.
Besides flaws, locations which generate high stress concentrations could also be the crack
initiation point. Le Cam et al. [122] demonstrated crack initiated from overvulcanised
zones contain more sulphur than the rest of the material. Hainsworth [120] found edges
of their samples are points of high stress concentrations. Yet, some researchers did not
observe any specific features indicating the origin point of failure at the crack initiation site
[88, 119, 120, 123].

4.1.1. Voids
Voids are regions with large number of atoms missing from the lattice [124]. Depending
on the strength of the link between the inclusion (impurity atoms cluster together to form
small regions of a different phase) and the matrix, the voids will be created at the interface
(decohesion) or in the matrix (cavitation) [125].
Le Saux et al. [121] reported that voids have a higher tendency to appear in isolated
inclusions, regardless of the type or nature of particles involved. The formation of void was
illustrated by Weng and his co-workers in their work [126]. They have shown that the densely
packed ZnS nano-particle aggregations begin to detach after the rubber was subjected high
temperature fatigue, leading to the formation of void. The identified void later evolved to
cracks and are primarily initiated when the rubber is stretched at 70% strain and above.
Wang et al. [45] have previously observed that the size of microvoids varies according to
the applied nominal strain amplitudes in rubber. The largest microvoids were found in
the broken rubber after subjected to 100% nominal strain amplitude and almost no visible
microvoids were present when subjected to 300% nominal strain amplitude. Grandcoin et
al. [127] recently observed that a void remains at the poles of the agglomerate when the load
is released, even though it was left for a long time to eliminate the viscous effects in rubber.
Besides inclusions, Le Cam et al. [128] have proposed that the curing process duration has
an effect on rubber matrix. Voids are formed at these highly cured regions in the matrix
which has a higher local modulus and an inclusion-like behaviour.

14
4.1.2. Cavities
Cavities are distinguished from voids in regions where particles are removed from the
rubber matrix and this region becomes a flaw in the material. Legorju-Jago and Bathias
[109] noticed that the first cavity formed in both NR and SBR rubber when it is stretched
up to 20% strain under tension-torsion loading. They found that cavitation have different
tendencies to occur when the rubber was subjected to static tension, cyclic tension and
static tension-torsion loadings. Le Saux et al. [121] revealed that cavitation happens at
the very early stage of the test. After only five cycles, the final defect density is almost
reached under a low displacement loading. The amount of defects increased greatly, within
a number of cycles lower than 10% of the initiation lifetime. This rise of the number of
cavities is strongly related to the global displacement and to the maximum local strain. At
the same time, no significant of volume increase in the defect was observed, except when
the rubber was submitted to high elongations.
Le Cam et al. [5] determined the microstructural damage surrounding the crack tip in
NR by using SEM beam microcutting technique. Their observations revealed that most of
the cavities at the crack tip are due to decohesion between oxides and rubber matrix. Le
Saux et al. [121] found that the oxides could exist as in the forms of inclusions (ZnO and
carbon black) or agglomerates (SiO2 ). The fatigue loading conditions and the stress state
at the crack tip were accounted for the growth of these cavities. Yet, cavitation from ZnO
particles at crack tip where not accountable in un-crystallized SBR rubber [122]. This is
especially true when the size of cavities are not greater than ZnO particles.
Unlike voids, the shape of cavities changes from a spheroidal shape to an elliptical under
loadings. The mechanism behind these observations was later described in detailed by Le
Cam et al. [5]. The spherical cavities are found at the relaxed zones while and ellipsoidal
cavities (due to the stretching level) are located at behind the crack tip. Weng et al. [126]
observed that nanoscaled cracks evolved into large elliptical and spherical cavities under
high temperature fatigue loading.
A very recent work by Ding et al. [129] investigated the effect of functionalized carbon
nanotubes on the crack growth behavior of natural rubber. They found that cavitation pro-
cess was resisted by carbon nanotubes during cyclic loading. This resistance was contributed
by rougher surface at the crack tip with thinner and densely distributed ligaments.

4.1.3. Agglomerates
One of the origin of cracks was due to the failure of carbon black agglomerates with a
reported size of less than 400 mm by [5] and 100 µm by [130] in NR. Grandcoin et al. [127]
noticed that silica agglomerate (20 µm) was present inside the matrix of a virgin sample.
The sample was then subjected to fatigue loading and the same region was observed again.
This time, they observed a decohesion of the filler-matrix interface and it was accounted
as the principal micro-mechanism leading to the formation of micro-cracks. Meanwhile,
Hainsworth [120] reported a agglomerate size of 30 µm in Si rubber.

15
4.1.4. Ligaments
Le Cam et al. [5] shown that the crack tip was composed of elliptical zones separated
by ligaments forming a flat but rough crack tip. For the case filled NR rubber, crystallized
ligaments are generated from highly stretched zones between elliptical zones and resist crack
propagation. The highly stretched ligaments represent the most crystallized zones of the
crack tip. As the microcrack grew, ligaments break and shrinked to form wrenchings at the
fracture surface. The same crystallized ligaments was observed in Si and CR rubbers in the
work by Hainsworth [120] and Le Saux et al. [121].
Le Cam and his team later investigated the behavior of ligaments in non-crystallized
filled SBR [122] . They deduced that the nature and origin of ligaments are not the same in
NR and SBR rubbers. In SBR, non-crystallized ligaments originates from a tearing line and
do not resist crack propagation. In fact, the ligaments failed (less than seconds) without any
resistance for the same energy brought by the electron beam. This observation is significantly
different in NR where crystallized ligaments do not break even if they are exposed to the
beam for very long time. They suggested that the microstructure of ligaments in SBR is
the same and homogeneous regardless of the deformation state. The team carried further
investigations for NR subjected to severe loading and did not observed the regeneration
of ligaments similar to moderate loading [110]. The detailed crack growth mechanism is
provided in Section 4.2. Meanwhile, Yao et al. [117] reported the crack tip is composed of a
number of dimple zones separated by ligaments in a silica filled NR. The pattern of ligaments
and dimple zones can be described as multiscaled. This meant that the large dimple zones
confined by large ligaments are made up of smaller zones confined by smaller ligaments. They
revealed that the thickness of ligaments did not increase in proportion with the amount of
silane coupling agent. However, thin ligaments with homogeneous distribution on the crack
tip contributed to the fatigue lifetime by effectively increasing the surface energy of cracking.

4.2. Crack propagation regime

A detailed fracture chronology includes studying the crack propagation pattern. The
crack propagates after it is initiated at crack tip where microscale flaws described in the
previous Section 4.1 existed in the virgin material. These microcracks will eventually grow
into macrocrack (visible to naked eye) causing the material to fail or rupture. Thus, it is
necessary to study crack propagation at two scales; microscale and macroscale for a complete
understanding of fracture chronology.

4.2.1. Microscale
The general crack propagation mechanisms shown in Figure 4 at the crack tip of NR
and Si rubber is described by Le Cam et al. [5] and Hainsworth [120]. Le Cam et al. [5]
successfully portrayed the crack growth mechanism due to cavities from front and side views
of the crack tip in NR in their work. As the crack tip was stretched, elliptical areas took
place with ligaments on both sides and wrenchings at the top and bottom. More cavities
were revealed after breaking through the thin wall that separates them from crack tip. The
corresponding microcracks propagated perpendicularly to the crack growth direction and
eventually coalesce until the destruction of the elliptical areas. Ligaments broke and relaxed
16
 Figure 4: The mechanism of fatigue crack propagation.

to form wrenchings at the top and bottom of these elliptical zones. These cracks were
considered to participate the opening of existing cavities until they break without creating
any new defects [121, 131]. Eventually, the broken crack tip grow into cracks and the process
repeats itself again. Hainsworth [120] noticed almost similar mechanism as Le Cam and his
team for Si rubber but no elliptical zones, wrenchings and striations were observed.
Le Cam and Toussaint [110] later showed that the mechanism strongly differs between
NR under moderate and severe loading. Under severe fatigue loading, the crack propagated
by generating only striations and no ligament was regenerated. This was due to the high
crystallinity at the crack tip prevents cracks to propagate through it, leading bifurcation
to occur at the microscopic scale. They distinguished the crack tip under moderate from
severe loading by using Digital Image Correlation (DIC) method. The crack tip was reported
to be flat and rough under moderate loading while flat and smooth under severe loading.
Meanwhile, in a less crystallizable rubber, CR, no conical shaped cracks due to strain induced
crystallization were observed [121].
Horst and Heinrich [132] calculated the crack tip fields at various crack tip velocities
using the linear viscoelastic theory. A transition from rubbery to glassy material behavior
in the vicinity of the crack tip can be observed. The Shear behavior was ascribed to the
increase of tearing energy at higher crack tip velocities, bulk behavior influences the fracture
mechanism. They explained that material separation at low crack tip velocities was the result
of formation, growth, and coalescence of cavities. At high crack tip velocities, cavitation was

17
suppressed and fracture was driven by a rather brittle mechanism resulting in a decreased
amount of energy to propagate the fracture process zone.
Saintier et al.[130] investigated crack propagation pattern for NR under relaxing and
non-relaxing conditions. They identified strong multi-cracking and crack deviation patterns
under non-relaxing conditions. In this particular case, at least 7 different crack tips were
identified with typical crack length of 100µm. Moreover, these microcracks appeared to
be present in additional to the secondary cracking (length in ranges between 2-10µm) at
larger magnification. The crack deviation was related to the contribution of the fatigue life
reinforcement. The authors justified that the crack growth rate was significantly reduced
due to the higher dissipation of energy during secondary crack formation. Yao et al. [117]
listed two factors which affected the surface energy dissipation at the crack tip in their study.
The first factor was attributed to the energy necessary to break the bonds at crack tip, and
the second factor to the cracking surface area [133, 134].

4.2.2. Macroscale
At this scale, the cracks are evident at the fracture surface and can be seen by the naked
eye. Le Cam et al. [16, 112] successfully presented the ’cartography of damage’ in NR
by using Haigh-like diagram. The diagram is split into three zones with different loading
conditions to fully represent the five elementary fatigue damages modes. Both crack pattern
and location were clearly captured on the diabolo shaped rubber for each damage modes.
Le Cam et al. [112] observed significant different type of fatigue damage under relaxing
tension-torsion in opposite phases compared to other loading conditions. They clarified that
this type of fatigue test can be considered as a relevant test to characterize fatigue damage
predictors. Saintier et al. [130] described that crack branching occurred under non-relaxing
conditions was due to highly heterogeneous and anisotropic zone at the crack tip induced
by strain crystallization. Ding et al. [129] proved that carbon nanotubes increased the
energy consumption of NR during cyclic loading by crack branching. They concluded their
work with carbon nanotubes improved the crack resistance of NR in two ways; cavitation
resistance and increase of energy consumption for crack propagation.
In SBR, Le Cam et al. [122] identified stable and unstable crack propagation on the frac-
ture surface under fully relaxing uniaxial loading conditions. The unstable crack propagation
surrounded the stable zone and its surface was relatively smooth with slight bifurcations of
the crack. Unlike in NR, no fatigue striations are observed for every loading conditions con-
sidered in this study. Ayoub et al. [40] performed different fatigue loadings to characterize
the fatigue crack damage for cylindrical hourglass and diabolo cylindrical hourglass-shaped
SBR. They captured and categorized the different crack propagation pattern under tension,
torsion and compression loadings.
Hainsworth [120] showed three different regions of crack growth pattern on the fracture
surface of a Si rubber. The first region was the crack initiation point which grew to the
second region as fast ductile fracture. The final fracture region appeared with ’concertina’
features. This feature were related to the typical final crack growing in mode III with an
element of tearing in the failure [135]. The cracks were found to initially grow along the
surface rather than through the thickness of the specimen.
18
5. Factors affecting fatigue lifetime
In order to prevent failure of material, it is highly important to understand the factors
which governs the fatigue lifetime. Factors affecting lifetime of rubber has been a subject of
interest over the years since 1964 [13, 136, 137]. An extensive review on the factors affecting
the lifetime of rubber was completed by Mars [138] in year 2004.
In this section, experimental works on factors affecting fatigue lifetime of rubber are
summarized into three categories: mechanical loading, chemical composition of rubber and
environmental conditions. Majority of the experimental works studied the effect of mechan-
ical loading, which involved the imposed level of stress and strain, frequency, and type of
loading conditions. Apart from the types of rubbers used, a number of works are related
to the chemical composition of rubber depending on its content. Environmental conditions
including the temperature, oxygen, ozone, air and water are also discussed in this section.

5.1. Mechanical loading conditions

Failure of rubber component is closely related to its mechanical loading condition. Rub-
ber components are often subjected to fluctuating or combination loading such as tension-
tension [33, 112], tension-compression [6, 16, 112], tension-torsion [137, 139], compression-
torsion [109, 140] and compression-compression [109].
In the fatigue testing, the effect of loading can be investigated by applying constant
amplitude or variable amplitude (stress or strain). Abraham et al [51] investigated the
effect of maximum and minimum stress amplitude for non-crystallizing rubber. They found
that increasing minimum stress with constant strain amplitude greatly increases the service
life of the filled rubber materials. While researchers generally focused on constant amplitude
loading conditions [141, 142, 71], Harbour et al [143] proposed the study of fatigue behaviour
of rubber under variable amplitude and multiaxial loading conditions as it represented actual
applications during service. Comparing NR and SBR, crack appearance in NR is more than
SBR. The increase of fatigue life is related to the rubber fillers system. On the contrary,
strain crystallizing is the common contribution to fatigue life in strain crystallizing rubbers.
Besides displacement control, some researchers have conducted tests under stress control
loading conditions. Legorju-Jago and Bathias [109] examined the effects of load ratio on
the lifetime of different rubbers. The load ratio is defined as the maximum load over the
minimum load. The compression loading, where R = −1, caused damage to NR because
reinforcement due to crystallization did not occur. Similarly, Ghosh et al [144] showed that
positive R ratio resulted significant decrease in crack growth rate for the NR specimens. El
and Altstädt [145] investigated fatigue behaviour of thermoplastic and silicone rubber under
stress controlled loading condition the material exhibited great fatigue lifetime compared to
silicone rubber due to its higher dynamic modulus.
In fatigue testing, the rubber material tend to self-heat due to its low thermal conductiv-
ity. Consequently, increasing the frequency should be avoided when it increases the surface
temperature of rubber. Indeed, it was reported that the lifetime of NR was shortened when
crystallization was hindered due to high temperature [146]. Self-heating of rubber NR has
been explored in the work by Stadlbauer et al [147]. Moreover, Stadlbauer and her team
19
[147] found that the frequency range between 1-5Hz is not important unless self-heating
exceeded the temperature limit.

5.2. Chemical compositions

5.2.1. Type of rubbers
Fatigue property of rubber has been a great interest among researchers and different
rubbers have been used in the studies. Lifetime of rubber is directly related to its nature
and the type of loading. As a result, it exhibits constitutive behaviour such as Mullins
effect, strain-crystallization, hysteresis and viscoelasticity [138]. NR is the most popular
choice due to its inherent strength, ability to withstand large deformations and resistance
to crack propagation. The effect of crystallization of NR on the fatigue life was investigated
by many researchers [16, 94, 109, 130, 136, 148, 149, 150, 151, 152, 153]. Le Cam [16]
described the different levels of strain experienced by natural rubber led to different type
of fatigue damage. Under non-relaxing uniaxial tension, small surface crack at sample feet
and crack branching due to the presence of crystallites were observed. This contributes to
the improvement of the rubber fatigue life. SBR is the most popular synthetic rubber used
by researchers. Wu et al [24], Ayoub et al [10] and Zine et al [8] have proposed experimental
works on filled SBR. Rublon et al [93] on the other hand, studied the effect of antioxidant
on fatigue crack growth behavior of SBR. Le Cam (2014) studied the crack initiation and
propagation patterns on the fracture surface of SBR.
Polychloroprene rubber (CR) has been used by Berton et al [154], Poisson et al [118],
Suryatal et al [38], and Marco et al[9]. Berton et al [154] observed that the stiffness of the
rubber decreases when subjected to increasing phase of force ratio. During the decreasing
phase, strain-induced-crystallization occur at the cracked site thus increases. Berton and
his team concluded the evolution of hysteresis and stiffness indicated the effect of strain-
induced-crystallization of polychloroprene. Magnetorheological elastomer (MRE) is a new
branch of material based from magnetorheological materials which consist of magnetically
permeable particles suspended in a non-magnetic rubber matrix. It has gained attraction
from researchers such as Zhang et al [155] and Zhou et al [18]. Magnetorheological elastomers
can be made from various rubber as matrices with different properties. MRE used in Zhang
et al’s experimental works is made up from polybutadiene rubber (BR) while Zhou et al
fabricated silicone-based MRE. Both of the authors presented the mechanical behaviour of
the respected MREs.
Self-healing of the silicon based rubber (RTV 360, Slygard 184) was investigated by
Keller et al [156] under fatigue torsion loading. Under torsion fatigue testing, the rubber
exhibited self-healing property and inhibited fatigue crack growth. Fatigue behaviour of
tire rubber was investigated by Schubel et al [73] using natural rubber and polybutadiene
blend. Characterization and crack growth investigation of NR and BR blend was proposed
by Ghosh et al [144]. An extended work [141] involving NR/BR blend and NR/SBR blend
was presented. They found that NR/BR has superior crack growth resistance resulting
better durability. Recent work by Seichter et al [34] investigated the influences on fatigue
behaviour of industrial rubber (SBR/BR/NR blends).

20
 Finally, it is to note that a proper quantitative comparison on the effect of rubber type
on the lifetime is challenging due to lack of detail information on rubber formulation in the
literature.

5.2.2. Type of fillers

The effect of filler in rubber compound on the fatigue life was studied since 1945 [157, 158,
159]. Carbon black as the most widely used reinforcing filler was popular in the past because
it improves rubber strength significantly and it is conventionally available. Strengthening of
carbon black in a component is governed by the hydrodynamic theory [160]. However even
until today, researchers are still investigating the optimum amount of the different type of
carbon black used in rubber compound [11, 161, 139, 149, 162, 163, 164, 165].
In the recent years, the term ’filler’ is not constrained only to carbon black. A number
of works reported different materials were added as fillers into rubber compound. Nanoclay
offers high reinforcing efficiency due to its high aspect ratio and good barrier property. SBR
filled with a mixture of carbon black and nanoclay was prepared by Wu et al [24]. It was
found that the material had improved hysteresis and tearing energy. In terms of fatigue
life, the SBR nanocomposite showed improvement with increasing of nanoclay content. Liu
et al [25] claimed that rubber containing hybrid carbon black and nanoclay have superior
mechanical properties and better fatigue resistance. Woo and Park [166] verified that the
hybrid material is more durable. Rooj et al [167] introduced a high degree of filler-filler
networking carbon black filled NR-nanoclay composite. The crack growth rate was reduced
with the presence of nanoparticles. Tian et al [168] studied the mechanical properties of
ethylene-propylene-diene monomer (EPDM) filled with silicate nanofibers and short PA-66
microfibers. With the same filler content, nanofibers filled EPDM has better dynamic prop-
erties than PA-66 microfibers. This showed that nanofibers exhibit excellent reinforcement
effect.
The study of graphene (GE) as a filler in polymeric material had gained much atten-
tion because it provides remarkable properties to the material. Apart from its excellent
thermal, electrical, mechanical and optical properties, it is also observed that strong in-
teraction between rubber and graphene improves the fatigue resistance of the material
[169, 170, 171, 172, 173]. Yan et al [174] studied the fatigue crack growth of NR and
graphene filled-NR. They found that graphene was able to restrain further the crack growth
due to crystallization at higher strain. Dong et al [175] fabricated graphene oxide filled-NR
composite and subjected it to multiaxial fatigue loading. They revealed that the composite
performed better at lower filler content. Ismail et al [176] investigated the fatigue life of
rattan powder-filled NR and the effect of silane coupling agent. The fatigue life material
decreases with increasing rattan powder content in thermal aging test. Their results showed
that there was a decrease in tensile strength and elongation at break, while increase in tensile
modulus and stress. With the addition of silane coupling agent, it was proven that there is
better adhesion between the rubber matrix and rattan filler, thus improving the fatigue life
and the aging properties.
In the work of Klüppel [177], the fatigue crack propagation behaviour was compared
between two types of fillers, silica and carbon black in SBR. It was observed that the filler-
21
filler bond increased with carbon black content. Compared to carbon black, silica formed
less stable filler cluster which results in lower hysteresis and tensile strength. Dong et al [84]
studied the fracture and fatigue of NR filled with varied silica and carbon black content. It
was found that the addition of silica improved the crack initiation and propagation resistance,
resulting in longer lifetime. Ismail et al [176] investigated fatigue life of rattan powder-filled
NR. The fatigue life of the material decreases with increasing rattan powder content in
thermal aging test. They showed that there was decrease in tensile strength and elongation
at break, while increase in tensile modulus and stress.

5.3. Environmental conditions

Apart from mechanical loading and chemical compositions, environmental issue is an-
other factor that contributes to the lifetime of rubber component [138]. Exposure of rubber
in different environments may result in alteration of mechanical properties which affect its
service life in the long run.
Fatigue of rubber in air has been extensively studied, and oxygen played an important
role. Le Gorju and Bathias [109] found that NR experienced chemical damage due to the
presence of oxygen in the air. The condition is extended to high temperature and oxidation
reaction occurred rapidly. This situation differs when NR is exposed to nitrogen and water.
Temperature effect on the lifetime of rubber is a concern as deterioration may occur when
the material is used above its optimum temperature. Le Gorju and Bathias [109] found that
crack growth rate of NR increased when the temperature was higher. The crystallisation of
NR was greatly affected when the temperature was increased. Rey et al [178] investigated
the effect of temperature on filled and unfilled silicone rubber. Stiffness of unfilled silicone
rubber increases with increasing temperature as the microstructure was stabilised. For
filled silicone rubber, the hysteresis, stress relaxation and stress softening decrease with
increasing temperature. Ismail et al [176] showed that mechanical property of rubber was
improved after thermal aging. On the contrary, experimental works based solely on EPDM
by Chou et al [179] found that the fatigue life of the rubber of both with and without carbon
black filled was dramatically reduced after six months of thermal aging. Increase in aging
temperature and aging time caused significant decrease in fatigue [180]. Ngolemasango et al
[180] explained that strain crystallization characteristic of NR is inhibited when exposed to
high temperature, resulting the increase in fatigue crack growth rate. Moreover, during aging
process, antioxidants added in the rubber compound are depleted. This allows oxidative
aging to occur, causing hardening at the rubber surface. While undergoing fatigue loading,
cracks can be easily formed leading to failure in short duration.
While it is well-known that temperature affects the lifetime of rubber, the condition
is worsen with the presence of oxygen as chemical-aging takes place [181]. Several works
[182, 181, 183] elucidate the characterization of thermo-oxidative aging characterization.
Neuhaus et al [184] conducted an experimental work to identify the aging effect with the
combination of elevated temperature and oxygen. They found that thermo-oxidative aging
increases the temperature sensitivity of rubber. In addition, the temperature sensitivity
increases linearly with aging time.

22
 Meanwhile, ozone is known to deteriorate rubber [137]. Vinod et al [185] found that
ozone resistance of NR is improved with the addition of aluminum powder. Although cracks
are observed on the specimen under the exposure of ozone, aluminum filled NR specimens
have smaller and discontinuous crack compared to unfilled NR specimens. Saharako et al
[186] studied the effect of ozone on NR/BR/EPDM blend. It was shown that the presence of
EPDM in the rubber compound improves the ozone resistance compared to NR/BR blend
compound. Similarly, Sae et al [187] investigated the properties CR/NR blend. It was
found that higher CR content in the blend improves both the mechanical properties and
environmental resistance. Double bonds in the structure of NR made it susceptible to ozone
attack. However, when suitable compound is added into NR formulation, it will greatly
improve its ozone resistance property [185].
Experimental works have been conducted to understand further the lifetime of rubber
component in marine environment. Le Gac et al [188] studied the fatigue behaviour of
NR rubber in marine environment. They concluded that there was no difference in the
mechanical response of rubber in marine and air under relaxing loading condition. However,
decreasing lifetime was observed when the specimens underwent non-relaxing loading. This
phenomenon was related to the reduced effectiveness of strain induced crystallization of
the rubber which contributed to the lifetime. Effect of load ratio of rubber in marine
environment was further studied by Ulu et al [189]. Although it showed similar trend under
relaxing loading condition by Le Gac et al [188], there was a contradiction of results for
rubber under non-relaxing loading condition. They observed that the lifetime of rubber
improved when load ratio increased and was supported by other studies [12, 6, 130].
Bouklas and Huang [190] defined swelling as a kinetic process coupling mass transport
and mechanical deformation, which depends on the interaction between the polymer network
and the solvent. Later, Andriyana et al. [191] found that degradation takes place with
swelling when biodiesel creates a hostile environment for elastomeric components.
One of the earliest research work on fatigue resistance of swollen rubber was reported by
Gul et al. [192]. About almost half a century later, Cho et al. [193] predicted the fatigue
life of swollen rubber using crack growth approach. They found that the crack growth
rates of swollen rubbers did not increase linearly with the tearing energy. Besides that,
the fatigue behaviour in different rubbers varies despite of the similar swelling ratio used.
The importance of comparing the swollen rubbers at similar degrees of swelling was further
highlighted in the work of Loo et al. [119]. They have shown that different immersion
durations of the different solvents were needed to achieve the same swelling level for the
same rubber. Meanwhile, their FESEM analysis revealed that similar locations of crack
initiation and crack propagation patterns were identified in both dry and swollen rubbers
in biodiesel, for different loading conditions. Similar results were also found at different
swelling levels [123].
All of the aforementioned studies were carried out under uniaxial loading conditions. Two
other research works have reported for multiaxial loading conditions [19, 20]. Both studies
have conducted fatigue tests for swollen EPDM rubber in reference oil IRM 903 using bubble
inflation method and proposed complex modulus energy as the predictor for fatigue lifetime.
They attributed the reduced fatigue lifetime of the swollen rubbers to physical and chemical
23
factors. These two types of factors have also been considered to describe the degradation of
mechanical properties and acceleration of damage in rubber [119, 123].

6. Future trends
In light of the literature study presented in the previous sections, future trends for
investigating fatigue life of rubber are summarized in this section from various perspectives.
First, a statistics on types of rubbers studied by researchers in the literature is shown in
Figure 5.

Figure 5: Types of rubbers.

In this figure, natural rubber appears to be a popular option in the research works
while SBR is the most widely studied synthetic rubber. There is a trend that researchers
are working on the variety of rubbers which are cost effective and excellent in mechanical
properties. The ability of hydrogenated nitrile butadiene rubber (HNBR) to withstand
hostile environment, including oil and heat resistance makes it a good material in automotive
industry [194, 195]. The property of this material can be enhanced with suitable rubber
compound [196]. Magnetorheological elastomer (MRE) has high potential in engineering
applications such as vibration absorber, base isolator and sensing device [197]. Addition
of iron particles into the rubber compound makes MRE differ from conventional rubber
materials. Further study of the material properties and complex loading conditions is needed
to expand the usage of this material in the industry.
Carbon black has been widely used as reinforcing filler. A number of works have been
done to investigate the optimum type and amount of carbon black in rubber compound
24
however this issue remained unsolved. Apart from using carbon black, researchers are look-
ing for alternative fillers which provide better bonding between rubber matrix and filler.
There is an emerging trend in using nanofillers to achieve better reinforcement that led to
improvement in fatigue lifetime [24]. Carbon nanotubes (CNTs) provides excellent thermal,
mechanical and electrical properties [194].
Exposure to long term cyclic loading could generate significant increase in temperature
which potentially could lead to further degradation in rubber [137]. Two criteria are needed
to take into consideration: environmental temperature and self-heating temperature. A
number of researchers studied the role of environmental temperature on rubber component
[109, 166, 176, 178]. As there is no standard procedure in the study of heat on rubber
specimen, the experimental approach varies from each researcher. Additional works need to
be done before the results are comparable. In addition, rubber material tend to self-heat
when subjected to fatigue loading [147]. Le Saux and his team [14] investigated fatigue
of different rubber compounds based on self-heating temperature. However, there is no
clear description on the relationship between frequency and self-heating temperature on the
fatigue lifetime of rubber. In practical application, rubber experiences simultaneous effect of
both environmental and self-heating temperature. Thus, a complete data of different rubber
types and temperature will be useful in rapid estimation of its fatigue lifetime.
Aging changes the properties of rubber physically and chemically, affecting the lifetime
of rubber component. While rubbers are used in various applications, the components are
exposed to different environmental conditions. One of the most common phenomena is
thermo-oxidative aging [198]. Elevated temperature and oxygen are the causes of rubber
failure. Thus there is an urgent need for quantitative models of the effects of aging on the
fatigue life of rubbers.
Various geometry of test specimens are used to investigate fatigue of rubber. As shown
in Figure 2, it can be seen that dumbbell and diabolo specimens were commonly used.
Dumbbell samples are well established in ASTM and ISO standards. However, there is
no standard describing the geometry of diabolo specimen, resulting various sizes of diabolo
specimen used in research works. The study of fatigue of rubber by different researchers
can be standardised following an acceptable guideline and geometry sample used for fatigue
testing.
Presentation of actual fatigue lifetime by researchers varies according to the experimental
setup and several factors that affect the lifetime [138], including mechanical loading, rubber
formulation, environmental conditions and specimen geometry. Complete information are
needed for the results to be comparable.

7. Conclusions
The present paper attempted to collect and analyze recent works on fatigue of rubber in
the literature in the past 15 years. To this end, three bibliographic databases were consulted:
Google Scholar, Scopus and Web of Science. Almost 200 papers were found which highlight
the important of the topic in rubber industry.

25
 Two different approaches are adopted in the evaluation of fatigue failure in rubber: crack
nucleation and crack propagation approaches. In crack nucleation approach, a number of
predictors were used to represent multiaxial fatigue data. However, none appears to be
robustly successful so far especially in unifying multiaxial data. Meanwhile, in the crack
propagation approach, the main challenge remains on the computation of the energy release
rate associated with the crack in question.
Potential future trends in the study of rubber fatigue were identified. It appeared that
there has been a significant amount of works on exploring alternative fillers which provide
better bonding between rubber matrix and filler through the use of nanofillers such as carbon
nanotube that could lead to the improvement of lifetime. Moreover, there is a more general
understanding that the study of rubber fatigue should also include the self-heating analysis
of rubber during cyclic loading. Thus, the coupling termo-mechanical analysis becomes
pre-requisite for a robust durability analysis of rubbers.

Acknowledgement
This work was supported by the Ministry of Higher Education Malaysia through High
Impact Research grant MOHE-HIR D000008-16001, by the University of Malaya through
University of Malaya Research grant UMRG RP022B-13AET, by the University of Malaya
Institute of Research Grant and Consultancy under the IPPP Fund Project PG100-2014A,
and by the Embassy of France in Malaysia.

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Highlights

Highlights
 Review of important aspects of rubber fatigue from the year 2002-2017.
 Fatigue life predictions via crack nucleation and crack growth are presented.
 Researchers are exploring alternative filler to improve the lifetime of rubber.
 Potential future trends in the study of rubber fatigue are identified.