Polymer Testing
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Test method
a r t i c l e i n f o a b s t r a c t
Article history: To predict long term creep of thermoplastics, methods based on the time–temperature
Received 1 December 2013 superposition principle (TTSP) or on the time–stress superposition principle (TSSP) are
Accepted 9 January 2014 commonly used. These methods enable the construction of a creep master curve without a
lengthy experimental program. Recently, a new accelerated creep testing method, termed
Keywords: the stepped isostress method (SSM), was proposed and used to predict long term creep of
Creep
technical yarns. This paper focuses on the processing aspects of the SSM test data and its
Master curve
validity in the creep prediction of thick thermoplastic specimens. Excellent correlation is
Stepped isostress method
Thermoplastic
obtained between the master curves constructed by the classical TSSP method and those
Superposition principle constructed by the SSM method. The variation of the SSM testing parameters has no
significant effect on the obtained master curves, which constitutes proof of the SSM
robustness. Further, the trend of the SSM shift factors in terms of the creep stress obeys the
Eyring equation.
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http://dx.doi.org/10.1016/j.polymertesting.2014.01.003
114 M. Hadid et al. / Polymer Testing 34 (2014) 113–119
creep curve at Tr but with a shift in the origin of the log time non-linear creep of fiber reinforced polyamide by the use of
axis. Mathematically, this idea is expressed by the following an improved empirical creep model [8], on its basis they
equation: constructed a smooth creep master curve [7]. Considering a
nanocomposite with polyamide matrix, Starkova et al. [9]
εðTr ; tÞ ¼ εðT; t:aT Þ (1) were able to build a master curve for time periods more
where Tr and T are the test temperatures while aT is the than 60 times than the test time.
temperature shift factor. Furthermore, it should be mentioned that the stress–
Tobolsky et al. [2] were the pioneers in the use of the time shift factor can be interpreted as the transition from
time–temperature superposition principle in the con- the laboratory testing time to the intrinsic time of the
struction of the master curve representing the creep material. In the construction of the master curve, Hadid
relaxation modulus over a very long time period. Plazek [3] et al. [7] found an exponential relationship between the
analyzed the temperature dependency of creep in term of stress shift factor and the applied creep stress:
free volume. He proposed a relationship of the relaxation
Logðas Þ ¼ b:s (4)
modulus ET at temperature T in term of the relaxation
modulus at the reference temperature Tr, as follows: However, Jazouli et al. [5] and Qaiser et al. [6] proposed
another expression for the stress shift factor using the free
T rr volume approach. The expression assumes an exponential
ET ðt:aT Þ ¼ ETr ðtÞ (2)
Tr r relationship in terms of stress:
The quantity aT is a function of temperature only and,
C1 ðs þ sr Þ
from Eq. (1), is defined as equal to unity at Tr. The quantities Logðas Þ ¼ (5)
ðC2 þ s sr Þ
rr and r are the material densities at Tr and T respectively.
The ratio rr/r allows one to take into account the variation where C1 and C2 material constants
of the density of the polymer due to temperature. However In summary, the works mentioned above [4–9] consti-
the Tr/T ratio, allows an adjustment regarding the kinetic tute examples of the use of the classical time–stress su-
aspect of the creep process. It is assumed that the material perposition principle for different kind of materials; neat
does not change its structure with time, so that the time– polymers, reinforced polymers and nanocomposites. This
temperature superposition (TTS) principle is still valid. confirms the huge interest and the need for the super-
position tool in the prediction of the viscoelastic material
behavior in the very long term.
1.2. Time–stress superposition principle
1.3. The stepped isothermal method SIM
In an analogous manner to time–temperature super-
position, a time–stress superposition principle (TSSP) Stepped Isothermal Method (SIM) is a derivative of the
approach is used to build creep master curves. The TSSP classical TTSP method. The SIM was first established by
assumes that an additional stress provides energy to the Thornton et al. [10] to predict the long-term creep behavior
tested material similar to the heat effect. Mathematically, of geogrids used in soil reinforcement applications. Later,
the TSSP can be expressed as follows: Alwis [11,12] applied this technique to characterize the
creep of Kevlar 49 yarns.
εðs1 ; tÞ ¼ εðs2 ; t:as Þ (3)
In TTSP testing, a single specimen is subjected to a
where s1 and s2 are creep stresses while as is the stress constant load at a certain temperature and a plot of creep
shift factor. strain vs. log (time) is produced. Similar experiments are
The TSSP has been used [4–9] to predict the long term conducted on different specimens at different tempera-
creep of viscoelastic materials. Luo et al. [4] used the TTSP tures. A reference temperature is selected, by applying the
to construct, for a PMMA commercial grade, a smooth principle of superposition, all individual curves are shifted
master creep compliance curve for a period of 290 days along the log time axis. Then, a creep master curve is pro-
from creep curves achieved over 4000 seconds and under duced at the reference temperature. In contrast to TTSP, SIM
various stress levels. The authors verified that the time– involves loading a single specimen subjected to a constant
temperature shift factors are dependent on stresses at load. The test temperature is increased in a series of
which the shifts are applied, and that the time–stress shift controlled steps. At each temperature step, a creep curve is
factors are dependent on temperatures at which the shifts obtained; those curves are processed and transformed in
are applied. Jazouli et al. [5] evaluated the long term non- several independent creep curves for each temperature
linear creep of a polycarbonate at room temperature. level. A creep master curve, at a reference temperature, is
Compliance creep tests, obtained at nine different stress then created in analogous manner to the TTSP method.
levels of one hour duration, were determined and shifted Several authors used the SIM technique to predict the
along the logarithmic time axis to get a master compliance long term creep or the creep rupture time [13–20]. SIM
curve. Qaiser et al. [6] generated a creep curve for an exploits a specificity of technical yarns, the high surface-to
extended time period for an amorphous polycarbonate thickness ratio, which allows very fast heating of the whole
from short-term creep curves obtained at different stress specimen. When dealing with thick specimens concern
levels. Additionally, they checked the effects of physical regarding the rapid heating and the non-uniform temper-
aging on the master curve. Hadid et al. [7] investigated the ature distribution in the specimen needs to be investigated.
M. Hadid et al. / Polymer Testing 34 (2014) 113–119 115
1.4. The stepped isostress method SSM strain was measured with a clip-on extensometer. The
control and data acquisition software of the machine allows
Recently, a few studies [21,22] considered the stepped conducting complex loading sequences, which are well
isostress method (SSM), a derivative technique of the SIM suited for SSM tests.
method. The approach in SSM testing is similar to that of The tests carried out were: i/ Tensile which is absolutely
the SIM method but the acceleration of the creep is ob- necessary to determine the linear section of the tensile
tained by increasing the stress level in steps rather than curve, and to estimate the jaw effects and the true starting
stepping up the temperature. The increase in stress pro- point of the stress/strain curve. ii/ Classical creep tests of
vides energy to the tested material similar to that provided three and six days duration at constant temperature. iii/
by heat in the SIM method. The SSM method is advanta- SSM creep tests with different stepwise increases of stress
geous when compared to the SIM method since there is no (1.5 MPa, 2.5 MPa and 4 MPa) and with different creep
need to use elevated temperatures; chemical properties of dwell time (2 hours and 5 hours). The testing temperature
the tested materials are not affected and the problem was 300 K and the humidity 20%.
concerning the slow and non-uniform heating of thick
polymeric samples is avoided. Indeed, when dealing with 3. Test results
thick specimens, the SIM method confronts the problem of
the poor thermal conductivity of the polymer which re- 3.1. Traction test
quires a heating period at each step to reach a uniform
temperature through the specimen, resulting in a transition Since the polyamide has some slack, the jaws effects
phase with uncontrollable and variable creep conditions. significantly impact the recorded specimen response,
The few previous works dealing with the SSM technique especially in the case of creep deformation. That is why
[21,22] have considered only technical fibers which have a tension tests are needed and performed to determine
relatively lower viscoplastic behavior. In contrast, in the accurately the true initial deformation which allows elim-
present paper more pronounced viscoplastic behavior ination of the initial sliding from the recorded deformation.
related to the nature of the thermoplastic polymer (i.e., Figure 1 illustrates the tensile stress/strain curve of the
polyamide) is expected. Indeed, the stress/strain traction polyamide. It allows determining the initial point, the
curve shown in Fig. 1 shows a small elastic zone followed by linear part of the curve and the stress levels which will be
an extended nonlinear section. considered for creep tests.
The key to produce the creep master curve based on
SSM or SIM methods is the processing steps of the raw test
3.2. Classical creep tests
data [18–22]. The following sections will illustrate the steps
of data handling of the SSM method. Also, its validity for the
Two conventional creep tests of few days duration are
polyamide specimens with thick thickness will be checked.
conducted on the same testing machine. The first test was
The master curve obtained with the SSM method will be
conducted for 6 days under a stress level of 2.5 MPa. The
compared to that obtained with the classical TSSP method.
second test was conducted for 3 days under a stress level of
5 MPa. These two relatively long tests are used to construct
2. Experimental testing the creep master curve according to the conventional TSSP
procedure. This curve is subsequently compared to that
The material in the present work is a polyamide 6, trade obtained with the SSM method. To make up for the jump in
mark TECAMID 6, provided as extruded 7 mm thick sheets. the creep deformation between two consecutive curves,
Specimens were cut from these sheets and stored in an the last part of the creep curve obtained at 2.5 MPa was
atmosphere with 20% of humidity for at least one month. extrapolated with a power law function in order to match it
The experiments were conducted on an Instron 5969 to the beginning of the creep curve obtained at 5 MPa. This
testing machine equipped with a 10 KN cell force. The creep helps to fill the gap in the creep strain between the two
stress levels during the construction of the master curve
and offers a guide for a best fitting of the master curve
based on the actual test data.
Table 1
The different testing parameters for the SSM creep tests.
Fig. 5. Master curves for different SSM testing parameters. Stress ref.
2.5 MPa.
4. Discussion
Fig. 4. The required handling of the tests data of the SSM method.
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