| DOI: 10.3933/APPLRHEOL-26-33503 | WWW.APPLIEDRHEOLOGY.

ORG

Rheological Characterization of Thermoplastic Elastomers (TPE)

Based on PP and Recycled EPDM

Paridokht Mahallati1, Hojjat Mahi Hassanabadi2, Manfred Wilhelm3, Denis Rodrigue1

1Department of Chemical Engineering and CERMA, Université Laval, 1065 Avenue de la Médecine,
Quebec, G1V 0A6, Canada
2CRIQ, 333 rue Franquet, Quebec, G1P 4C7, Canada
3Institute for Chemical Technology and Polymer Chemistry, Karlsruhe Institute of Technology (KIT),

Engesserstrasse 18, Karlsruhe, 76131, Germany

*Corresponding author: denis.rodrigue@gch.ulaval.ca

Received: 12.2.2016, Final version: 28.4.2016

Abstract:
The rheological behavior of thermoplastic elastomers (TPE) based on 50/50 recycled ethylenepropylene-diene monomer
(r-EPDM)/polypropylene (PP) was studied to determine the effect of feeding strategy when preparing these blends using
twin-screw extrusion. In particular, small and large deformation characterizations have been performed to better understand
the relationships between sample preparation and final properties of the blends. It was found that small changes in blend
morphology (particle size and interfacial adhesion) are better distinguished in rheological properties (melt state) under large
deformation (LAOS and step shear) compared to small deformation (SAOS).

Key words:
Polypropylene, recycled EPDM, thermoplastic elastomers, large deformation.

1 INTRODUCTION ods have been developed to modify PP toughness such

Thermoplastic elastomers (TPE) are polymer blends
that can be processed at high temperature like thermo-
plastics (melt processing), but have mechanical prop-
erties similar to elastomers (high elasticity) at low tem-
perature. Depending on the polymers and processing
methods used, different families of TPE can be pro-
duced [1]. TPE prepared by physical melt mixing of a
polyolefin with an elastomer gained considerable at-
tention because their macroscopic mechanical proper-
ties (impact strength, elongation at break) can be mod-
ified over a wide range by simple control of composition
[1 – 3]. Today, polypropylene (PP) is one of the main poly-
mer used as the matrix because of its low density, bal-
anced mechanical properties, and processing behavior.
It is also easy to modify (molecular weight distribution,
branching, tacticity, copolymer, etc.) to meet the re-
quirements for several applications in terms of general
performances [4]. Consequently, PP is widely used in
automobile, household appliance, and construction in-
dustry. Nevertheless, the use of PP alone is restricted
due to its brittleness (low impact strength), especially
at low temperature. In the last decades, several meth-
as blending with elastomers leading to the develop-
ment of TPE based on PP and ethylene-propylene-diene
monomer (EPDM). These blends have been very suc-
cessful due to structural compatibility between both
polymers and several investigations have been pub-
lished dealing with their morphology and mechanical
properties [1, 4 – 10]. Due to the growing importance of
TPE, melt rheology of thermoplastic blends was pro-
posed as a tool to understand the relationships be-
tween structural properties (morphology), processabil-
ity, and mechanical behavior. Therefore, the rheological
properties of TPE have been extensively studied, but
mostly under small deformation in oscillatory shear as
these measurements correlate linear mechanical data
with processing in the non-linear regime [2, 3, 7, 11 – 14].
Over the last decade several attempts to use recy-
cled rubber in TPE formulations were investigated be-
cause of environmental concerns and cost reduction
[15 – 23]. Although the mechanical properties of PP/re-
cycled EPDM (r-EPDM) blends are well-known, very little
attention has been paid to their rheological behavior in
the melt state [24]. This information is highly important
to understand their processing and relate morphology

© Appl. Rheol. 26 (2016) 33503 | DOI: 10.3933/ApplRheol-26-33503 | 1 |

Figure 1: Typical morphology of the samples studied: P-E (left) and E-P (right).

to macroscopic properties. From our previous works on
PP/r-EPDM blends [18, 19], it was found that coupling
agent addition is not necessary for this system due to
good interaction between both phases as confirmed by
mechanical and morphological analyses. This was ob-
tained through optimization of the processing condi-
tions (flow rate, screw speed, temperature profile, screw
design, etc.) and feeding strategy in a twin-screw ex-
truder. It was found that the optimum properties were
obtained when r-EPDM was introduced in zone 1, while
PP was introduced in zone 4 of a twin-screw extruder
having a total of 10 zones. In this case, feeding the r-
EPDM first led to smaller rubber particles (around 200
μm) and higher elongation at break (155 %) compared to
the reverse case of feeding the PP first (300 μm and 86 %
elongation at break).
In order to differentiate between the processing
conditions tested, it is proposed to use rheological mea-
surements in the melt state instead of the usual me-
chanical properties in the solid state (tension, flexion,
impact, etc.). It is expected that the matrix contribution
is less important in the melt state leading to a higher
contribution (higher sensitivity) of the blend morphol-
ogy in terms of the dispersed phase size, dispersion qual-
Sample code Main feed (zone 1) Side feed (zone 4)
PP PP – ties) can be found elsewhere [18, 19].
P-E PP r-EPDM
E-P r-EPDM PP
ity, and interfacial adhesion. To this end, small and large
deformation characterizations were performed to get a
complete understanding of the differences observed in
mechanical properties by other means than morpholog-
ical analysis (optical, scanning electron, and transmis-
sion microscopy) which is very tedious. In particular,
nonlinear oscillatory and large deformation have been
recently used to study the behavior of different materi-
als like silica (SiO2) suspensions [25], bituminous binders
[26] and polypropylene/multiwall carbon nanotube
(MWCNT) composites [27].
2 EXPERIMENTAL
2.1 MATERIALS
Polypropylene (PP) and recycled ethylene-propylene-di-
ene monomer (r-EPDM) rubber were used in this work.
The polypropylene (melt flow rate = 2.80 g/10 min
(230 °C and 2.16 kg), melt temperature = 160 °C and den-
sity = 0.9 g/cm3) was supplied by LyondellBasell (USA)
under the trade name of Montell PF814. The r-EPDM (av-
erage initial particle size = 480 μm and density =
1.29 g/cm3) was supplied by Royal Mat Inc. (Canada).
More information on the materials, methods, and char-
acterizations (morphological and mechanical proper-
2.2 BLEND PREPARATION

Table 1: Sample codes and feeding sequences used for sample PP/r-EPDM (50/50) blends were produced in a co-rotat-
produced via twin-screw extrusion. The blends are 50/50 % wt. ing twin-screw extruder (Leistritz ZSE-27, Germany)
with a screw diameter of 27 mm and a L/D ratio of 40
Tensile Tensile Elongation at Flexural Charpy impact (total of 10 zones). The extruder was operated with a
Sample modulus strength break modulus strength flat temperature profile of 180 °C (all the zones) at 150
(MPa) (MPa) (%) (MPa) (J/m)
PP 412 ± 22 32.3 ± 0.4 792 ± 117 1500 ± 170 38 ± 4 rpm with a flow rate of 6 kg/h and a 3 mm circular die.
P-E 149 ± 9 15.8 ± 0.4 85 ± 12 687 ± 9 76 ± 7
E-P 147 ± 2 14.5 ± 0.5 154 ± 13 559 ± 12 162 ± 13
The main feed hopper was at the beginning of the ex-
truder (zone 1) and a secondary feeder (side-stuffer) was
Table 2: Mechanical properties of the samples presented in placed at zone 4. An injection molding machine (Nissei
Table 1. The blends are 50/50 % wt. PS60E9ASE, Japan) was used with a linear screw tem-

© Appl. Rheol. 26 (2016) 33503 | DOI: 10.3933/ApplRheol-26-33503 | 2 |

Figure 2: Storage G' and loss G" moduli of the samples at
180°C.
perature profile between 180 and 200 °C from the rear
to the injection nozzle with a mold temperature of
30 °C. More details on sample preparation and charac-
terization can be found elsewhere [18]. Two feeding se-
quences were selected as reported in Table 1. In all cases,
25 mm diameter discs were cut from the molded sam-
ples for the rheological characterizations. For a base of
comparison, Figure 1 presents typical micrographs of
the blends, while Table 2 reports on the mechanical
properties.
2.3 RHEOLOGICAL CHARACTERIZATION
Transient rheological tests (step shear) were performed
on a strain-controlled TA Instruments rheometer (ARES)
under a nitrogen atmosphere. All the measurements
were done with a parallel plate geometry (25 mm in di-
ameter) with different shear rates (0.01, 0.03, 0.1, 0.3,
0.6, and 1 s-1) at 180 °C. Strain sweep tests were done at
different temperatures (180, 200, and 220 °C) with a fre-
quency of 1 rad/s between 1 and 200 % strain amplitude.
Small amplitude oscillatory shear (SAOS) were done at
different temperatures (180, 200, and 220 °C) in the fre-
quency range of 0.05 – 400 rad/s at a controlled strain
amplitude of 5 % (linear viscoelastic regime). Large am-
plitude oscillatory shear (LAOS) tests were performed
on a TA Instruments (ARES G2) in a strain-controlled
mode by conducting experiments at different frequen-
cies and 180 °C. The obtained stress was then converted
from a time to a frequency domain using FT-rheology
(Fourier-Transform rheology). More details can be ob-
tained elsewhere [28, 29].
3 RESULTS AND DISCUSSION
First, small amplitude oscillatory data are analyzed to
obtain the cross-over frequency wc where G’ = G”, and
the elastic limit ge which represents the deformation
where the linear behavior ends, for PP and PP/r-EPDM
at different temperatures (180, 200, and 220 °C). Table 3
© Appl. Rheol. 26 (2016) 33503 | DOI: 10.3933/ApplRheol-26-33503
Figure 3: Absolute value of the complex shear viscosity for the
samples at 180°C.
Figure 4: Polypropylene strain sweep tests at different tem-
peratures (w = 1 rad/s).
shows that increasing temperature increases wc indi-
cating shorter relaxation time for all the samples. Ad-
ditionally, wc values for PP samples are higher than PP/r-
EPDM blends at the same temperature. For both blends,
the values of wc (measured at small deformation) are
similar over the temperature range and Table 4 pre-
sents the temperature shift factors aT for a reference
temperature of 180°C [30]. It is clear that the addition
of r-EPDM into PP decreases the aT values indicating
that the blends are more sensitive to temperature than
the neat matrix, but the values are different for both
systems indicating an effect of sample preparation
(morphology difference). Since blend processing is per-
formed in the melt state, both viscosity and elasticity
(moduli) are important parameters to control. Figure 2
shows the shear storage G’ and loss G” moduli of the
different samples at 180 °C under small deformation.
The G’ and G” values for PP/r-EPDM blends are higher
than PP due to the presence of the dispersed phase and
the presence of an interface between both phases. On
the other hand, there is no significant differences be-
tween the G’ and G” curves for both TPE blends. As pre-
| 3 |
Figure 5: Strain sweep tests at 180°C for the different samples
(w = 1 rad/s).
Figure 7: Stress-time curves for P-E at different shear rates
and 180°C.
sented in Figure 3, the absolute value of the complex
viscosity |h*| at 180 °C gives similar trends. It is clear that
|h*| increased with r-EPDM addition since the recycled
rubber particles are partially crosslinked.
Figure 4 (strain sweep tests) shows the shear mod-
uli (G’ and G”) for PP at different temperatures, while
the values at 180 °C for the different samples are shown
in Figure 5. It is observed that G’ and G’’ values for PP/r-
EPDM blends are higher than PP over the whole fre-
quency range because of higher interaction between
both phases. Nevertheless, the values of the elastic lim-
its ge of the blends (Table 3) indicate that a difference
exists between small and large deformation behaviors
as reported by Filipe et al. [31]. Another way to apply dif-
ferent deformation on a sample is via stress-time
curves (shear step) and the results for PP and PP/r-EPDM
samples at different shear rates (180 °C) are presented
in Figures 6 to 8. At low shear rates, the stress curves
did not show any overshoots, while at higher shear
rates (above 0.6 s-1) all the samples had an overshoot
before reaching a steady state. Again, the stress values
for PP/r-EPDM blends are higher than neat PP due to
© Appl. Rheol. 26 (2016) 33503 | DOI: 10.3933/ApplRheol-26-33503
Figure 6: Stress-time curves for PP at different shear rates and
180°C.
Figure 8: Stress-time curves for E-P at different shear rates
and 180°C.
r-EPDM contribution. As reported in our previous study
[18], feeding the r-EPDM before PP in the extruder pro-
duced smaller particle sizes which also improved the
adhesion between the matrix and the dispersed phase
leading to larger interfacial area. Comparing the results
of Figures 7 and 8, different behaviors between both
blends can be seen, especially when the shear rate is
higher than 0.1 s-1: P-E samples (Figure 7) have a behav-
ior similar to neat PP, while E-P samples have a two-step
deformation behavior where the second step occurs on-
ly when the shear rate is above 0.1 s-1. In all cases, the
corresponding critical total deformation (shear rate
multiply by the time) is about 3.5 and constant critical
deformation for the overshoot, independent of the
shear rate applied, has been reported before [32, 33].
These trends point again to large deformation being
more sensitive than small deformation to small differ-
ence in morphology (particle size here) between both
samples.
To better quantify the differences between both
TPE samples at high deformation, LAOS was performed
to detect any increased nonlinearity by the incorpora-
| 4 |
Figure 9: I3/1 as a function of strain amplitude for the sam- Figure 10: I3/1 as a function of strain amplitude for the sam-
ples at 0.5 Hz. ples at 1 Hz.

tion of r-EPDM particles into the PP matrix [29, 34]. The 4 CONCLUSIONS
response was analyzed by FT-rheology which is a very
reliable technique for nonlinear stress data analysis The rheological properties of a polymer blend in the melt
[35]. It has been shown that the relative intensity of the state are controlling the final structure of these blends
third harmonic to its first one I3/1 from FT-rheology and therefore controlling their processability and perfor-
quantifies the transition from the linear to nonlinear mance. Since most polymer processing methods are per-
response [33]. The values of I3/1 can also be used to com- formed at high shear rate/deformation, it is important to
pare different samples and the trends can indicate mor- determine the rheological behavior of the systems under
phological differences in multiphase systems [36, 37]. similar non-linear conditions. Consequently, the rheolog-
For our samples, the values of I3/1 as a function of strain ical behavior must be investigated over a wide range of
amplitude at different excitation frequency (0.5 and deformation, frequency, and temperature. In this work,
1 Hz) are presented in Figures 9 and 10. According to the rheological behavior of PP and PP/r-EPDM blends was
these curves, not only blending PP with recycled rub- studied. Using rheological characterizations under small
bers increased the nonlinearity of the system (higher and large deformation, significant differences were ob-
I3/1 values for P-E and E-P blends), but also different served for TPE blends having similar composition (50/50),
trends in the curves were obtained. For P-E samples, a but processed differently (component feeding order in a
broad peak around g = 1 is usually related to the inter- twinscrew extruder) leading to small changes in their fi-
face deformation created between both phases in a nal morphology. Although their small deformation be-
multicomponent system. This bump seems to increase havior was similar (SAOS), significant differences were
in intensity with increasing frequency (comparison be- observed under large deformation (step shear tests and
tween Figures 9 and 10). As P-E samples have larger par- LAOS combined with FT-rheology in the non-linear
ticle sizes and lower adhesion with the matrix (lower regime). These differences were not only attributed to
mechanical properties) [18], this bump can be associat- small differences in the dispersed phase particle size, but
ed with lower compatibility between the phases in the also to the interaction level (compatibility) between both
blends indicating that LAOS combined with FT-rheolo- phases. Even if small differences were observed in the sol-
gy is a powerful tool to differentiate between samples id state [18], melt rheology was more sensitive to these
having similar rheological behavior at small deforma- differences. This is especially the case under large defor-
tion. As this is a first step, further investigations are mation as LAOS is more sensitive to particle size/geom-
needed in the future. etry, while step shear is more sensitive is more sensitive
to interfacial interactions [31]. Nevertheless, more work
Sample (°C) w c (rad/s) g e (%) needs to be done to completely understand the relation-
PP (180) 12 74 ships between all the parameters involved and the char-
PP (200) 23 76 acterization performed, as well as to get simple models
PP (220) 46 86
P-E (180) 6.3 8.1
for process design, control, and optimization [38].
P-E (200) 9.4 6.1
P-E (220) 36 3.3 Sample aT (200 °C) aT (220 °C)
E-P (180) 5.7 8.4 PP 0.65 0.44
E-P (200) 11 10 P-E 0.50 0.07
E-P (220) 25 11 E-P 0.60 0.27

Table 3: Cross-over frequency wc and elastic limit Table 4: Shift factor aT for the different samples
ge values for the samples at different temperatures. (TREF = 180 °C).

© Appl. Rheol. 26 (2016) 33503 | DOI: 10.3933/ApplRheol-26-33503 | 5 |


ACKNOWLEDGEMENTS
The authors acknowledge the financial support of the Nat-
ural Sciences and Research Council of Canada (NSERC). Al-
so, the technical support of Mr. Yann Giroux for the exper-
iment is appreciated. Finally, many thanks go to the group
of Manfred Wilhelm at the Karlsruhe Institute of Technol-
ogy (KIT) for a student exchange sponsored by FRQNT
(Fonds de recherche du Québec – Nature et Technologies).
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