PRÜFEN UND MESSEN
TESTING AND MEASURING
Fatigue crack growth ⋅ rubber blend ⋅
tearing energy
The present work aims to characterize
fatigue crack growth (FCG) behaviour
for comparative durability prediction of
NR/BR- and NR/SBR- blend based com-
pounds. The influence of strain, tempe-
rature, r-ratio and waveform was stu-
died to simulate realistic service life
condition by using a Tear and Fatigue
Analyser (TFA). Both of these blends
show higher FCG rate at higher tempe-
rature, but the effect is comparatively
higher in the NR/SBR compound. The
influence of r-ratio towards FCG rate
was found to be very less in NR/BR
blend, whereas NR/SBR-blend shows
considerable decrease in FCG rate at po-
sitive initial tension (r-ratio). The higher
FCG rate was observed in pulse mode
compared to sine mode in both the
blends.
Vorhersage der Haltbarkeit von
Reifenlaufflächen-Compounds
auf Basis von NR/BR- und NR/
SBR-Blends durch Einsatz des
„Tear Fatigue Analyser“
Rissausbreitungsgeschwindigkeit ⋅ Elas-
tomer ⋅ Reißenergie
Die Arbeit beschäftigt sich mit der Cha-
rakterisierung des Ermüdungsrisswider-
standes von NR/BR- und NR/SBR-Elas-
tomeren. Der Einfluss von Dehnungs-
amplitude, Temperatur, Vorspannung
und Belastungsfunktion wurden unter-
sucht um die reale Lebensdauer mittels
„Tear and Fatigue Analyzer (TFA)“ zu si-
mulieren. Die beiden Elastomersysteme
weisen eine steigende Rissausbrei-
tungsgeschwindigkeit bei der Belas-
tung in Gegenwart höherer Temperatur
auf. Dieser Effekt ist deutlicher bei dem
NR/SBR-Material. Es wurde ein margi-
naler Einfluss der Vorspannung auf den
Risswiderstand festgestellt. Bei pulsför-
miger Beanspruchung ergibt sich eine
höhere Rissausbreitungsgeschwindig-
keit im Vergleich zur sinusförmigen Be-
anspruchung.
Figures and Tables:
By a kind approval of the authors.
www.kgk-rubberpoint.de
Durability Prediction of NR/BR and
NR/SBR Blend Tread Compounds
using Tear Fatigue Analyser
Tyre in a vehicle is a critical safety compo-
nent as it has to withstand against all
kind of road hazards during service. Tyres
are very much susceptible to get dama-
ged from sharp objects which may lead
to catastrophic failure. Hence durability
assessment should be given proper im-
portance. The fracture mechanical ap-
proach which deals with propagation of
pre-existing cracks is used extensively to
assess durability of elastomeric products.
Over the years researchers [1-3] have
studied fatigue crack growth characteris-
tics of rubbers in great detail. It is also
evident from literature [4] that the Fa-
tigue Crack Growth (FCG) characteristics
of rubber blends are much complex com-
pared to single component based mate-
rials. It is worth mentioning here that
with increasing demand of performance
requirement, usage of blend in tyre tread
is almost inevitable. The blend of Natural
Rubber (NR) either with Polybutadiene
Rubber (BR) or Styrene Butadiene Rubber
(SBR) is widely used in tread compound.
Although previous researchers [5,6] have
reported studies on various blend sys-
tems but systematic investigation consi-
dering realistic service condition is very
limited. In a previous research work [7],
the authors highlighted the influence of
blend composition, curing system and
service conditions on FCG characteristics
over a wide range of tearing energy. The
objective of the present work is to obtain
relative FCG ranking of 60-40 NR/BR and
NR/SBR blend based tyre tread com-
pounds for durability assessment. FCG
measurements are carried out under va-
riable temperature, r-ratio and wave-
form. The relative crack growth rate at
equal tearing energy level is presented as
a measure of durability for the com-
pounds under study.
Materials and experimental details
The compositions of 60-40 NR/BR and
NR/SBR blends are provided in Table 1. A
laboratory Banbury mixture (Make: Ste-
wart Boling, UK) of 1.5 liter capacity was
used for preparing these blends. The mi-
xing was done in three stages. Rubbers
and all chemicals except curatives were
mixed in the first stage of 4 minute dura-
tion. The rotor speed was set at 60 rota-
tions per minute (rpm) and temperature
was at 140°C. The re-milling of the first
stage mixed compound was done at 30
rpm for 3 minutes time at 120°C. In the
final stage, curatives were added and
mixed at 30 rpm for 3 min at 100°C. A
Moving Die Rheometer (Dynesco USA
MDR 2000E) was used for measuring
rheometric properties of these com-
pounds at 141°C for 1 hr. and 0.50 arcs
with 100 CPM frequency. The optimal
cure time (tc90) for NR/BR and NR/SBR
blends were 25.03 min and 29.03 min
respectively. FCG test specimens were
prepared at 141°C for two times of tc90
value in a compression mould and pres-
sure maintained at 14.7 MPa.
FCG properties of these compounds
were measured using a Tear and Fatigue
Analyser (TFA, Coesfeld, Germany) and
the detailed description of this equip-
ment can be found in Eisele et al [8]. The
standard geometry of pure shear speci-
men (length to width ratio of 1:8) having
dimension, length L0 =15 mm, width Q =
120 mm and thickness B =1.5 mm was
used. The initial cut of 21 mm was provi-
ded on both sides of the pure shear test
specimen in accordance to Stocek et al
[9]. In this work, two double sided not-
ched and one un-notched samples were
analysed simultaneously. The crack
growth rate (da/dn) was measured from
the notched samples whereas tearing
energy, T was calculated from the un-
notched sample according to Rivlin et al
Authors
Prasenjit Ghosh, Rabindra
Mukhopadhyay, Kankroli,
Rajasthan, India
Radek Stoček, Zlín, Czech Republic
Corresponding author:
Prasenjit Ghosh, Hari Shankar
Singhania Elastomer and Tyre
Research Institute,
Kankroli, Rajasthan, 313342, India
Tel.: +91 2952 232019
E-Mail: pghosh@jkmail.com
KGK · 06 2016 53
 PRÜFEN UND MESSEN
TESTING AND MEASURING

1 ferent test conditions and provided in

Table 3. In the subsequent sections, dou-
Loading amplitude A

ble logarithmic plot of tearing energy vs

Sine crack growth is presented to show the
influence of various parameters on FCG
behaviours of these blends.
100 ms Time t
1000 ms
Influence of temperature on FCG of NR/
BR and NR/SBR blends
The effect of temperature on FCG charac-
Pulse teristics of NR/BR and NR/SBR blends is
shown in Figure 2. It has been observed
that FCG rate at 70°C is significantly high-
20 ms Time t
1000 ms er compared to 30°C at all tearing energy
levels for both the blends. The increased
crack growth rate at higher temperature
Fig. 1: Schematics of sine and pulse loading.
is associated with the viscoelastic energy
dissipation process at the crack tip as exp-
1 Composition of NR/BR and NR/SBR blends lained by Persson et al [10]. At higher
Ingredients NR/BR NR/SBR temperature of 70°C, polymer molecules
Natural Rubber (phr) 60 60 can move easily because of lowering of
Polybutadiene Rubber (phr) 40 - intermolecular chain friction compared to
Styrene Butadiene Rubber (phr) - 40 room temperature. This leads to decrease
Carbon blacka (phr) 50 50 in viscous dissipation at elevated tempe-
rature as shown by Ghosh et al [11].
Zinc oxide (phr) 2.50 2.50
Hence more elastic energy will be
Stearic acid (phr) 2.50 2.50
available at the crack tip for propagating
Antioxidantb (phr) 2.25 2.25
the crack and thereby decrease in frac-
Sulfur (phr) 1.5 1.8
ture resistance. It has also been observed
Acceleratorc (phr) 0.80 1.0
a
Carbon Black type was N339. b N-(1,3-dimethylbutyl), N‘-phenyl-p-phenylenediamine (6 PPD).
that the influence of temperature is mo-
c
N-Oxydiethylene, 2-benzothiazole sulfenamide. phr – parts per hundred rubber re pronounced in NR/SBR blend. This
may be attributed to the presence of SBR
2 Test condition details for fatigue crack growth measurements as reported by Lake et al [12], where it
Test condition Strain (%) Temperature (°C) r-ratio Waveform also shown very high crack growth rate
Temperature effect 13-25 30 & 70 0 Sine at higher temperature.
r-ratio effect 13-25 30 0 & 0.14 Sine
Influence of r-ratio on FCG of NR/BR
Waveform effect 13-25 30 0 Sine & Pulse
and NR/SBR blends
The influence of r-ratio on FCG characte-
3 FCG parameters of NR/BR and NR/SBR blends
ristics is provided in Figure 3 for NR/BR
FCG Test condition NR/BR NR/SBR
and NR/SBR blends. The significant incre-
b m b m ase in FCG resistance at 0.14 r-ratio is
30°C 3.14 3.70E-07 7.44 1.54E-06 observed in comparison with 0 r-ratio for
70°C 4.33 1.33E-05 2.09 7.25E-05 NR/SBR blend. However in NR/BR blend,
0.14 R-ratio 2.67 2.06E-07 3.49 1.82E-07 FCG resistance is also shown increasing
Pulse Waveform 2.04 1.79E-05 2.89 1.04E-04 trend at higher r-ratio but the extent is
comparatively much less.
[1]. The test condition details are sum- cycles. Then tearing energy, T was obtai- The increase of FCG resistance at hig-
marized in Table 2. The schematics of si- ned using the following equation, her r-ratio is associated with the strain
ne and pulse loadings applied are shown induced crystallization phenomena [13].
in Figure 1. For all sine modes tests, 10 Hz 𝑇𝑇 = 𝑤𝑤 𝐿𝐿0 (1) The formation of crystalline zone in front
frequency was used. For the pulse loa- of the crack tip leads to deviation of the
ding, the pulse duration and the dwell where w is the stored strain energy den- crack path from orthogonal direction of
time was calculated for a tyre of 1.076 m sity and L0 is the length of the not strai- main strain. It is also well known that NR
outer diameter running at 60 kmph ned sample. The variation of crack due to its molecular architecture, it crys-
speed. The pulse duration and dwell time growth rate with tearing energy can be talizes on stretching. At positive r-ratio
was 20 ms and 180 ms respectively. mathematically represented as there will always be some residual strain
which prevents crystallized zone from
𝑑𝑑𝑑𝑑
Results and discussion = 𝑏𝑏𝑇𝑇 𝑚𝑚 (2) melting. Whereas at 0 r-ratio, these crys-
The crack growth rate (da/dn) was calcu- 𝑑𝑑𝑑𝑑 tallites will disappear during every un-
lated from the measured crack length where b and m are material constants. loading cycle as the samples will be to-
over a considerable number of fatigue These parameters are calculated for dif- tally in strain free condition.

54 KGK · 06 2016 www.kgk-rubberpoint.de


2 3
Fig. 2: FCG plots of NR/BR and NR/SBR blends at 30 and 70°C.
Influence of waveforms on FCG of NR/BR
and NR/SBR blends
Figure 4 depicts the effect of waveform
on FCG characteristics. It can be observed
that FCG rate is significantly higher in
pulse mode compared to sine waveform
in both the blends. The previous resear-
chers [14, 15] also made similar observa-
tions for some of the rubbers. However,
the assigned causes as reported for
showing such behaviour are not very
conclusive. The difference in test condi-
tions (strain rate, relaxation time etc.)
between sine and pulse mode may be
taken into consideration to explain this
behaviour. It is very obvious that in pulse
mode, the loading is very fast as the du-
ration is only of 20 milliseconds compa-
red to sine mode which spans 100 mil-
liseconds. This implies five times higher
strain rate in pulse mode than sine which
could lead to instantaneous increase of
crack tip temperature and in turn higher
crack growth rate.
From the results discussed so far, it
has been observed that FCG rates are
higher in NR/SBR blend compared to
NR/BR blend. This is in conformity with
the earlier findings made by Bhowmick
et al [16] where NR/SBR blend showed
much inferior crack growth resistance
compared to NR/BR blend. For the pre-
4 5
Fig. 4: FCG plots of NR/BR and NR/SBR blends at sine and pulse mode.
www.kgk-rubberpoint.de
30°C
70°C
30°C
70°C
Fig. 3: FCG plots of NR/BR and NR/SBR blends at 0 and 0.14 r-ratios.
sent work, crack growth rates are calcu-
lated at equal tearing energy level of 1.5
N/mm for these blends and shown in
Figure 5. It can be seen that in all the
cases NR/BR blend scores much better
with respect to durability compared to
NR/SBR blend.
Conclusion
The influence of temperature, r-ratio
and waveforms on FCG characteristics
of NR/BR and NR/SBR blend based
tread compounds is discussed in detail.
The significant influence of these para-
meters on FCG characteristics was ob-
served in both the blends. However, the
degree of influence is found to be diffe-
rent in these two blends. Overall NR/BR
blend achieved superior crack growth
resistance and hence better durability
in all respect compared to NR/SBR
blend.
Acknowledgement
This work was supported by the Ministry
of Education, Youth and Sports of the
Czech Republic – Program NPU I (LO1504).
The authors thank the Managing Com-
mittee of Hari Shankar Singhania Elasto-
mer & Tyre Research Institute (HASETRI)
for permission to publish this research
work.
Fig. 5: Crack growth rate at 1.5 N/mm tearing energy.
PRÜFEN UND MESSEN
TESTING AND MEASURING
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KGK · 06 2016 55