Polymer Testing 32 (2013) 447–454

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Polymer Testing
journal homepage: www.elsevier.com/locate/polytest

Test method

Accelerated creep testing of polymers using the stepped

isothermal method
Frédéric Achereiner*, Kurt Engelsing, Martin Bastian, Peter Heidemeyer
SKZ – Das Kunststoff-Zentrum, Friedrich-Bergius-Ring 22, 97076 Wuerzburg, Germany

a r t i c l e i n f o a b s t r a c t

Article history: The increasing use of polymers in engineering applications requires suitable accelerated
Received 19 December 2012 test methods for predicting their long-term behavior. The stepped isothermal method (SIM),
Accepted 31 January 2013 originally developed for product testing of geosynthetics, was successfully applied in the
presented work to characterize the long-term creep behavior of polypropylene up to
Keywords: approximately 100 years. Based on the time-temperature superposition principle, this
Long-term creep behavior
method can be described as a short-term creep experiment during which the temperature
Stepped isothermal method
is elevated stepwise. It is shown that the temperature steps can be rescaled and shifted to
Accelerated testing
Time-temperature superposition principle
generate a master curve matching the prediction of long-term creep resulting from the
conventional approach of the time-temperature superposition principle (TTSP). This com-
pliance with established test methods and its good reproducibility suggests that SIM might
be a useful tool for accelerated testing of long-term creep behavior, especially for com-
parative purposes such as quick screening of material formulations during the early
development stages, or the at-line assessment of resins as part of quality assurance.
Ó 2013 Elsevier Ltd. All rights reserved.

1. Introduction 50 to 100 years, which is not compatible with tight product

The increasing use of polymers in engineering applica-
tions usually requires a minimum guaranteed service life of
10 to 15 years. In the case of plastic parts relevant to security
or difficult to replace, such as pipes and geomembranes
for landfills, these requirements may reach up to 50 or 100
years. Therefore, the long-term creep behavior of the ma-
terial needs to be considered in the early stages of product
development.
However, polymers are viscoelastic materials. Their
mechanical behavior strongly depends on time and is still
difficult to extrapolate over more than one decade (log
scale). Hence, estimation of the long-term deformation
under static load requires conventional creep experiments
over a long period of 5 to 10 years for product lifetimes of
* Corresponding author. Tel.: þ49 931 4104475; fax: þ49 931 4104717.
E-mail address: f.achereiner@skz.de (F. Achereiner).
development schedules.
Increasing the temperature is a common way to accelerate
the time-dependent creep response [1]. Based on the time-
temperature superposition principle (TTSP) [2,3], short-term
creep experiments at various temperatures are sufficient to
generate a master curve, which describes the long-term
deformation at a reference temperature [4]. This method is
well established for the accelerated creep testing of polymers.
The construction of a master curve involves shifting the
timescale of the measured creep curves to match the creep
behavior at a reference temperature. The corresponding
shift factor aT was described by Williams, Landel and Ferry
[5] as:
 
t
ε0 ðT0 ; tÞ ¼ ε T; (1)
aT
where ε0 is the strain at reference temperature, T0 the ref-
erence temperature, t the time, ε the strain at the elevated
temperature T.

0142-9418/$ – see front matter Ó 2013 Elsevier Ltd. All rights reserved.
http://dx.doi.org/10.1016/j.polymertesting.2013.01.014
448 F. Achereiner et al. / Polymer Testing 32 (2013) 447–454
They also defined the WLF equation, which enables an
empirical description of the shift factor aT for amorphous
polymers above the glass transition temperature Tg:
C1 ðT  T0 Þ
logaT ¼
ðC2 þ T  T0 Þ
where C1 and C2 are empirical constants.
However, the WLF equation is not valid for semi-
crystalline polymers well below their melting points.
Seitz and Balazs [4] showed that in this case the description
of the shift factor aT follows an Arrhenius equation:
 
DH 1 1
logaT ¼  (3)
2:303 R T T0
where DH is the activation energy and R the universal gas
constant.
The present work introduces a further development of
TTSP, the stepped isothermal method (SIM), which was
originally introduced for product testing of geosynthetics.
2. Principle of the stepped isothermal method
In order to predict the long-term creep behavior of
geogrids in soil reinforcement applications, Thornton et al.
[6,7] made some adjustments to the TTSP procedure. SIM
exploits a specificity of geosynthetics, the high surface-to-
thickness ratio of which allows very fast heating. Due to
measurement scatter caused by the use of many specimens,
the conventional implementation of TTSP requires many
experiments to determine a master curve for one load level
(at least 3 short-term creep tests per temperature for sta-
tistical validation), implying long overall duration and high
costs. By contrast, SIM requires only a single test specimen,
which is tested under a constant load, but at a sequence of
stepwise increased temperature levels. This approach
minimizes both scattering effects and testing time, which
makes SIM a very attractive testing method.
TTSP and SIM both involve shifting creep curves using
the temperature-dependent shift factor aT. However, due to
differences in the experimental approach the analysis of
SIM data implies some additional steps prior to this shifting
procedure. Fig. 1 describes schematically these adjustments.
First of all, the temperature changes during the creep
experiment, which means that the measured deformation
does not exclusively account for the creep behavior. Thus,
a vertical shift is required to remove the deformation
caused by thermal expansion while heating the sample
(Fig. 1a).
According to the Boltzmann superposition principle [1]
the creep curves at different temperature steps can be
treated as individual tests starting at the virtual start time
t0 . When the temperature step T2 starts at time t2, some
creep has already taken place at the previous temperature
T1. Therefore, a creep experiment corresponding to the
behavior measured between t2 and t3 would have started at
a time t20 < t2 (Fig. 1b). This virtual start time t0 is empiri-
cally determined; the details of this procedure will be
discussed in section 4. The rescaling of each temperature
step is handled iteratively and the results are all plotted on
the virtual time scale (t-t0 ) (Fig. 1c).
(2)
Fig. 1. Principle of the SIM procedure: (a) correction of measured data due
to thermal expansion, (b) determining virtual start time t0 (c) rescaling, (d)
curve shifting according to TTSP.
The SIM data now correspond to a family of virtually
independent creep tests, which can be shifted to a master
curve the same way as in conventional TTSP (Fig. 1d). The
start temperature is usually employed as the reference
temperature for curve shifting.
The applicability of SIM was investigated for many dif-
ferent geosynthetics [8–10]. Due to the good agreement
with conventional long-term creep tests, SIM meanwhile
becomes a well-established method for the accelerated
product testing of geosynthetics; standards have been
published for both tensile creep (ASTM D 6992) and com-
pressive creep (ASTM D 7361).
Despite the advantages of SIM, only sparse attempts
have been made to extend the scope of this method to
other polymeric products. Alwis and Burgoyne [11] applied
SIM successfully to creep testing of aramid yarns. Like
geosynthetics, high-performance yarns mostly feature
a very small cross-sectional area and can, therefore, be
rapidly heated. More recently, first attempts were made
with thicker samples: Thomas et al. investigated HDPE
under tensile load with respect to plastic pipes [12];
Bozorg-Haddad and Iskander focused on compressive
loading of HDPE [13].
The present study aims at determining whether SIM can
be generalized to material characterization of polymers and
investigated for possible restrictions to the use of SIM.
3. Experiments
Due to its widespread use in engineering applications
susceptible to long-term creep, polypropylene serves in the
present work as an example for the investigation of SIM.
The material used was a commercially available PP homo-
polymer. Tensile specimens were injection-molded and
stored for some months under standard climate conditions
(23  C/50 % relative humidity) before testing. Since not all
samples can be tested simultaneously, this should prevent
 F. Achereiner et al. / Polymer Testing 32 (2013) 447–454 449

the creep behavior from being too much influenced by

differences in physical ageing condition. The geometry of
the dumbbell specimens complies with ISO 527; the
thickness is 4 mm.
In order to assess the applicability of SIM, a reference for
the tensile creep behavior of polypropylene was determined
by means of long-term measurements, and indirectly with
creep master curves, which were generated according to
conventional TTSP. The long-term creep experiments were
performed for up to one year at 23  C using a dead-weight
loading setup.
Short-term creep tests for both conventional TTSP and
SIM were performed on a universal testing machine with
closed-loop load control. The tests were conducted in an
insulated chamber with an external temperature control
unit. Compared to conventional temperature chambers, this Fig. 2. Raw SIM data.
setup not only guarantees a stable temperature (0.5 K) over
many hours but also a quick heating (>5 K min1). Due to
regulating the sample loading dynamically, the thermal
the high air flow, the heating is evenly distributed, so that no
expansion was directly measured by repeating the SIM
temperature gradient occurs in the chamber. Both the
procedure with a controlled load of 0 N, as shown in Fig. 3.
chamber temperature and the temperature at the surface of
This procedure considers the thermal behavior of the
the test samples were recorded. The creep strain was
whole experimental setup.
measured with a clip-on extensometer.
The second analysis step considers the creep behavior
According to conventional TTSP, short-term isothermal
for each temperature step as if the measured deformation
creep tests were performed for up to 10 hours at various
results of an independent creep test at constant tempera-
temperatures. By contrast, SIM experiments lasted up to 3
ture. According to the Boltzmann superposition principle, the
days but the temperature was gradually increased in 10 K
sum of these independent tests would form a creep curve
steps while the sample was still loaded. Between two
corresponding to the raw SIM data. Strictly speaking, the
heating steps the temperature was maintained constant for
Boltzmann superposition principle only applies to small
a dwell time of at least 10000 s. All SIM experiments were
strains since it describes linear viscoelastic behavior.
started at 23  C, which was also chosen as reference tem-
However, investigations on the validity of SIM for geo-
perature for the construction of the master curve according
synthetics [7–10] indicate that an extension of this princi-
to TTSP.
ple to larger strain leads to an approximation, which can be
assumed as appropriate for engineering purposes.
4. Results and discussion
One reason for this may be the empirical procedure
used to determine the virtual starting time t0 of the inde-
Using an appropriate experimental setup, the actual test
pendent tests. The procedure is based on the specificity of
procedure is rather simple and was fully automated. First,
SIM: using a single sample, the physical state at the junc-
the sample is fixed in the setup and the temperature is
tion between two temperature steps is unique. Assuming
regulated. Then, a constant load is applied and the time-
that both steps correspond to independent experiments is,
dependent deformation is recorded. After each dwell time
therefore, only possible when both curves reflect this
the temperature is rapidly elevated to the next level. The
unique physical state. This means that the creep rate at the
raw data of an exemplary SIM test involving a poly-
propylene dumbbell sample loaded with a constant tensile
stress of 10 MPa (i.e. 30 % of the yield stress) are displayed
in Fig. 2.
The specific characteristic of SIM testing lies in the
analysis steps which are required to obtain a smooth
master curve. To illustrate the procedure, the analysis of the
SIM data shown in Fig. 2 will be described in detail.

4.1. Detailed analysis of SIM data

The first analysis step aims at correcting the SIM data in

order to account for thermal expansion. Starting with the
first heating step, the measured deformation of the sample
comprises both creep deformation and thermal expansion.
The latter has to be removed. Thornton [6] determines the
value of this vertical shift empirically; it is also possible to
use the coefficient of thermal expansion (CTE) when
available. However, since the experimental setup allows Fig. 3. Overview of vertical shifting and rescaling.
450 F. Achereiner et al. / Polymer Testing 32 (2013) 447–454

end of a temperature step should be identical to the creep

rate at the beginning of the next step when the two steps
are considered independently.
Since the heating does not take place instantaneously,
there is a small transition region with undefined creep
behavior at the beginning of each temperature step. As
a result, the data from this transition region should be
excluded from the analysis but the time scale is kept in place.
However, if the heating is quick enough, the assumption of
identical creep rates can still be used. Beginning with an
arbitrary value, the starting time t0 is, therefore, iteratively
varied until the slope at the beginning of a temperature step
matches the slope at the end of the previous step in the
logarithmical time scale (t-t0 ), as shown in Fig. 4. This pro-
cedure is repeated iteratively for all temperature steps until
the SIM data rescaled in the virtual time scale (t-t0 ) is
equivalent to a set of independent isothermal creep curves.
These can be used to generate a master curve by means of Fig. 5. Horizontal shifting according to TTSP.
horizontal shifting according to TTSP (Fig. 5).
However, the curves do not overlap since SIM data
correspond to continuous creep deformation. The creep temperature has to be quick enough so that the transition
curve of a temperature step can, therefore, be appended phase with undefined creep behavior can be considered as
directly to the curve of the precedent step, hence building negligible. This is the case for thin products like geo-
a smooth master curve. synthetics. However, heating 4 mm thick tensile specimens
may not be as fast due to the poor thermal conductivity of
4.2. Assessment of the method polymers. Therefore, investigations were performed with
thermocouples in the sample’s bulk as well as at the sam-
The construction of the master curve according to TTSP ple’s surface. The results are shown in Fig. 7 for tempera-
directly provides a tool to evaluate the quality of the creep ture steps of 10 K.
prediction. The empirically determined shift factors just A closer look at the first heating event (Fig. 8) reveals
have to be displayed in an Arrhenius plot as shown in Fig. 6. that the bulk temperature increased more slowly than the
Since Eq. (3) describes the shift factors aT for semi- surface temperature, but the time delay is not very pro-
crystalline polymers, a linear correlation indicates that nounced. More than 80 percent of the required tempera-
the shifting procedure was appropriate; lack of linear cor- ture increase can be achieved in only 150 s; the target
relation suggests false rescaling. If the creep mechanism temperature is reached within 600 s. Hence, compared to
changes within the temperature range used in the SIM the dwell time at constant temperature, the heating of the
experiment, the Arrhenius plot displays two partial linear sample can be considered as stepwise.
correlations with different slopes, which reflects the SIM does not specify how to define the transition
change in the activation energy. This can be used to region. The only requirement is to maintain the specimen
determine the maximal temperature which still leads to temperature within 1 K of the target temperature, which
meaningful results for a given start temperature. is achieved in less than 300 s. This leaves some scope for
Due to the specific analysis approach of SIM, the heating
of the sample requires special attention. The change of

Fig. 4. Determining the virtual start time t0 Fig. 6. Arrhenius plot of the shift factors.
 F. Achereiner et al. / Polymer Testing 32 (2013) 447–454
Fig. 7. Temperature of the sample during a SIM test.
the choice of data which need to be excluded from the
analysis. Other analysis parameters, such as the time range
used to determine the slope at the beginning and the end of
a step, are not clearly defined either, leaving room for
uncertainty.
Lechat and Greenwood [14] pointed out that the manual
analysis of SIM data by different operators can lead to
a significant uncertainty and they emphasize the need for
an automated processing. Therefore, the data presented in
this study were all analyzed using a computer-based rou-
tine. Given this, SIM measurements provide creep master
curves with good reproducibility, as displayed in Fig. 9.
Indeed, master curves resulting from different samples
match nicely. Small differences in the master curve’s form
may still be observed but they can be related to the man-
ufacturing process, in this case the cavity of the injection
mold.
The good reproducibility indicates that SIM is a suitable
comparative method which can be applied as a useful tool,
e.g. for quick screening of material formulations during the
development stage or for at-line quality assessment of
resins.
Since SIM master curves always result from one single
experiment, the specimen variability need to be assessed
Fig. 8. Temperature of the sample during the first heating step.
451
Fig. 9. Repeated SIM measurements with different samples.
separately. Due to the good reproducibility of the master
curve’s form, only the starting strain level needs to be
checked statistically. This can be done with some short-
term creep tests at the starting temperature, as described
in ASTM D 6992 using the term “Ramp and Hold”. The SIM
master curve can then be shifted vertically, like in Fig. 10, to
match the average starting level. This study for the stan-
dard tensile specimen showed that the scattering of the
starting level can be considered negligible when using
a electro-mechanical load unit instead of dead weights.
The SIM testing procedure is fairly straightforward but
three major parameters can influence the construction of
a master curve:
 the dwell time at constant temperature
 the magnitude of the temperature step
 the number of temperature steps
The third parameter affects especially the maximal
range of predictable creep times: the more steps, the longer
the master curve. However, due to the iterative analysis
Fig. 10. Variability of the strain level for short-term creep tests.
452 F. Achereiner et al. / Polymer Testing 32 (2013) 447–454
Fig. 11. Variation of the dwell time at constant temperature while keeping
the magnitude of the temperature step DT constant.
procedure, small errors can add up, leading to incorrect
master curves. The number of steps is also limited by the
temperature range in which the investigated creep mech-
anism is constant.
Thornton claims that poorly chosen testing conditions
lead to master curves with a shorter time range, but the
inadequacy of dwell time or temperature step is conser-
vative [6]. The impact of these two parameters on the
master curves has been reviewed in this study. The dwell
time was varied from 10000 s, which is recommended by
ASTM D 6992, up to 45000 s. The resulting master curves
are displayed in Fig. 11. For times up to one year, the creep
prediction of the three master curves is mainly identical.
More significant differences can be observed in the long-
term behavior. Altogether, shorter dwell times lead to
higher strains. A comparison with conventional test
methods, as done in 4.3, indicates that the master curve for
a dwell time of 45000 s best corresponds to the actual long-
term creep behavior.
Fig. 12. Variation of both the dwell time at constant temperature and the
magnitude of the temperature step DT.
Fig. 13. Raw TTSP data (each curve corresponds to the average of 3 different
creep experiments).
The magnitude of the temperature steps was also var-
ied, showing that larger temperature steps lead to higher
strains. However, Fig. 12 demonstrates that the dwell time
at constant temperature and the magnitude of the tem-
perature step have a combined effect on the master curve:
entirely different test conditions can lead to nearly identi-
cal creep predictions. Optimal test conditions are in the end
a compromise between the quality of creep prediction and
the practicability of the test method; long dwell times and
small temperature steps result in higher accuracy to the
detriment of test duration and costs.
4.3. Comparison with conventional test methods
Creep master curves were also constructed according to
conventional TTSP procedure, hence using many different
isothermal short-term creep tests. The raw data for poly-
propylene under a tensile load of 10 MPa are displayed in
Fig. 13. The creep behavior was measured for 7 different
Fig. 14. Comparison of SIM, conventional TTSP and long-term creep
experiments.
 F. Achereiner et al. / Polymer Testing 32 (2013) 447–454
Fig. 15. Arrhenius plot of the shift factors for both SIM and conventional
TTSP.
temperature levels using 3 specimens for each tempera-
ture. Altogether, 21 single creep experiments, each lasting
at least 10000 s, were necessary to generate a master curve
using conventional TTSP.
As displayed in Fig. 14, the comparison of this master
curve with the SIM master curves presented in Fig. 12
shows a perfect match. The results of both test methods
also correspond to nearly identical activation energy, as
shown in the Arrhenius plot of the shift factors in Fig. 15.
This means that the hypothesis used to split SIM data into
virtual independent creep experiments is indeed appro-
priate. Therefore, SIM can be regarded as a fully functional
alternative to conventional TTSP procedure.
The actual creep data was measured directly in long-term
experiments up to 1 year (Fig. 14). For comparison purposes,
the data was then extrapolated according to Findley’s
equation [15]. Both SIM and TTSP master curves basically
match actual creep data; however, long-term comparison
shows a clear divergence. Physical ageing is presumed to be
responsible for this discrepancy, since the short-term creep
tests offer only a snapshot of the ageing state and do not
reflect that the sample continues ageing while it creeps.
Brinson and Brinson [16] showed that the continued aging
during the application of the load leads to a stiffening of the
material with increasing time. Creep prediction based on
TTSP is, therefore, distorted to shorter times.
A better conformity with the actual long-term creep
behavior should be reached by combining the time-
temperature superposition principle with the time-ageing-
time superposition principle introduced by Struik [17].
Currently the authors are working to modify the SIM pro-
cedure in order to account for physical ageing processes
occurring during long-term creep of amorphous and semi-
crystalline polymers.
5. Conclusions
The stepped isothermal method (SIM), originally devel-
oped for product testing of geosynthetics, was successfully
applied to characterize the long-term creep behavior of
453
polypropylene tensile specimens. Despite their thickness,
the samples could be heated quickly enough to perform
a rescaling of the single temperature steps. Thus, the
measured strain was stripped into a family of virtually
independent isothermal creep curves which were subse-
quently used to generate a master curve according to the
time-temperature superposition principle (TTSP).
SIM proved to have good reproducibility, although the
choice of testing parameters may influence the final results.
Long dwell times and small temperature steps result in
higher accuracy to the detriment of testing duration and
costs, so that a compromise between the quality of creep
prediction and the practicability of the test method needs
to be found.
Compared to the classical TTSP procedure, SIM allows
reducing the experimental effort to a minimum while still
providing the same accuracy of the master curves. The re-
sults suggest that SIM might be a useful tool for accelerated
investigations of long-term creep behavior, especially for
comparative purposes such as quick screening of material
formulations during the early development stages, or the
at-line assessment of resins as part of quality assurance.
However, SIM cannot transcend the limitations for the
prediction of long-term creep due to the snapshot effect of
short-term tests. A more accurate master curve might
require some extra consideration of the physical ageing
phenomenon. Moreover, the presence of some transition
within the testing range of temperature, which causes
changes in the creep mechanism, may prevent the use of
SIM. Instead of varying temperature, it may help in that
case to increase the load stepwise, as recently proposed by
Giannopoulos and Burgoyne [18]. This so-called stepped
isostress method (SSM) is similar to SIM but is based on the
time-stress superposition principle [19].
Acknowledgements
We are grateful to the research association FSKZ e.V. for
its financial support to IGF project 15967 N, which was
provided via the AiF as part of the programme to support
“Industrial Community Research and Development” (IGF),
with funds from the Federal Ministry of Economics and
Technology (BMWi) following a decision of the German
Federal Parliament.
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