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02014099(95)00009-9

Creep design analysis for a thermoplastic


stress relaxation
measurements
S. K. Reif, K. J. Amberge
~ateria/s

~e~orrna~~e
72309, USA

Received

from

and D. A. ~oo~ord

a~a/ys~s, Inc., 1737 ff~io~ Street, Suite 543, Schenectady,

29 September

7994; accepted

16 February

NY

1995

Innovative designs using thermoplastics


have been limited by available mechanical property
data which often do not span appropriate ranges of stress, time, strain and temperature. In an
effort to improve the design process, a methodology using short-time (less than 24-hour) highprecision stress relaxation tests has been developed to provide comprehensive
design information. This study uses stress relaxation tests to investigate the creep properties of VALOX, a
polybutylene terephthalate, or PBT, developed by General Electric. The approach is extremely
efficient, and the data generated can be presented in several convenient formats. For example,
pseudo-stress-strain
curves may be used to generate strain versus time (at a constant stress) or
stress versus time (at a constant strain). Secant modulus curves as a function of strain, time and
temperature can also be produced. The results are in good agreement with those generated by
traditional test methods. The stress relaxation testing technique thus shows great promise as a
tool to be used in the design of thermoplastic components.
Keywords:

stress

relaxation;

creep; secant

modulus;

Introduction
The assessment of structural performance in plastics, as
in all materials operating at high homologous temperatures, requires property data covering appropriate
ranges of stress, strain, time and temperature1-3. The
traditional approach to generate the data has involved
the testing of many specimens for long times at fixed
values of stress and temperature. This is a costly and
inefficient procedure and is a major obstacle to the
development of new or improved materials. The desire
to avoid long-time creep testing has led to the development of a practical, innovative approach to generating
high-temperature design curves through the use of stress
relaxation tests (SRT)4. The SRT methodology was first
developed for metals and subsequently shown to be
applicable to polymers&.
Short-time (less than 24
hours) SRT are used to generate plots of stress versus
either stress rate or inelastic strain rate. The hightemperature pe~o~an~e
may then be represented in
several ways using these basic plots.
For polymers the scarcity of design-quality creep data
is especially acute because of the great variety of grades
and the batch-to-batch variability. The previous work
on a polycarbonate and polyphenylene oxide showed
great potential in the SRT methodology to provide the
desired acceleration of data generatio#..
The results
were accurate, reproducible and consistent with traditional constant load creep data. Moreover, it was

Correspondence
0261-3069/95/0~001~7

to David

A. Woodford
8 1995 Elsevier

Science

design

analysis

shown that ambiguities


associated with strain on
loading and with the time-dependence
of elastic
modulus could be eliminated using the SRT approach
and total strain analysis.
The present study investigates the mechanical behaviour of VALOX, a polybutylene terephthalate, or PBT,
provided by General Electric, using this approach.

Experimental procedure
Standard flat tensile specimens of VALOX, with a
cross-sectional area of 39 mm2, were stress relaxation
tested in an Instron 4204 testing system with a closedloop control configuration
and an oven capable of
controlling the specimen temperature to within 1C.
Each sample was loaded at a constant displacement rate
of 10 mm/min, using an attached extensometer on a
25.4 mm gauge to measure the strain directly. When the
desired level of total strain was reached, the displacement rate was automatically reduced to 0.5 mm/min for
increased control stability, and the strain then held
constant. By maintaining a constant strain in the specimen, concerns about machine compliance for fixed
crosshead control are eliminated8. Subsequently, a stripchart recorder monitored the reduction of stress with
time over approximately a 24-hour period, as the elastic
strain was continuously
being replaced by inelastic
strain. Time and stress data were taken from the charts
to yield a plot of stress versus time which was subsequently fit with a fourth-order polynomial equation (see
Figure I). These equations were then differentiated to
yield stress rate as a function of stress. In constructing
Materials & Design Volume 16 Number 1 1995

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Creep design analysis for a thermoplastic:

S. U. Reif et al.

14

12

1 .O% strain
1.5% strain
2.0% strain

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Stress relaxation curves from four strain levels at (a) 50C. (b) WC,

Materials & Design Volume 16 Number 1 1995

(set)
(c)

80C

10

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Creep design analysis

for a thermoplastic:

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Materials

& Design Volume

16 Number

1 1995

17

Creep design analysis

for a thermoplastic:

S. K. Reif et al.

these curves (see Figure 2) care was taken to limit the


analyses to times not exceeding the actual test duration.
Relaxation tests were run from total strain levels of
0.5%, l.O%, 1.5% and 2.0% and at temperatures of
50C 65C and 80C. To eliminate the effects of deformation history and ageing, a separate specimen was
tested at each of the desired conditions. Curves of log
stress versus stress rate were used to generate pseudotensile curves at iso-stress rates which in turn were used
to construct creep and secant modulus curves.

Results
Construction

of pseudo-tensile

curves

Using the stress-stress rate curves shown in Figure 2,


families of iso-stress rate pseudo-tensile curves for
VALOX were constructed using a cross-plotting technique. Vertical cuts of constant stress rate were taken
across the stress-stress rate curves. Values of stress were
recorded corresponding to the intersection between the
cuts and the curves. Subsequently, these stresses were
plotted against their respective total strains to yield
pseudo-tensile curves, as shown in Figure 3.

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Generation of creep curves

Using the previously constructed pseudo-tensile plots,


horizontal cuts of constant stress (s) were made and
each intersecting strain value was recorded. The times
(t) to each of these strains were then calculated using
the following formula:
s / (dsldt) = t (seconds)

(1)

After converting time to units of hours, creep curves of


strain versus time were plotted. This procedure was
performed at stress levels of 1.72, 3.45 and 5.2 MPa
(250, 500 and 750 psi, respectively). Figure 4 is an
example of a set of curves at 65C. These generated
creep curves are plotted against effective time with no
extrapolation of actual data, and it should be noted that
the times are much longer than the relaxation test duration. This effective acceleration for creep analysis will
be discussed subsequently.
From the pseudo-stress-strain plots, vertical cuts of
constant strain were made and each intersecting stress
value was recorded. The times to each of these strains
were again calculated using equation (1). These data
were plotted in terms of stress versus time and shown in
Figure 5 for the case of 1% strain.

I . I . I . I
00

& Design

Volume

16 Number

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Because of the strong time-dependence


of elastic
modulus in polymers a secant modulus is often used in
design. This is the slope of the line drawn from the
origin on a stress-strain plot to intersect the curve at a
given strain. It is dependent on strain rate (or stress
rate), temperature and strain. In practice, the secant
modulus is normally plotted against time so that a
pseudo-elastic design may be made for the anticipated
service life of a part, i.e. the appropriate value of the
Materials

0.4

Generation of secant modulus design curves

18

02

1 1995

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Figure 3 Pseudo-tensile
(b) 6SC, (c) 80C

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12

curves

at various

stress rates at (a) 50C

Creep design analysis

12

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for a thermoplastic:

S. K. Reij et al.

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secant modulus may be used in place of Youngs


modulus.
In a procedure similar to the construction of creep
curves, vertical cuts of constant strain were taken across
families of pseudo-tensile curves for a particular
temperature. The stress at which each of the stress rate
curves was intersected was recorded. By dividing these
stress values by strain, secant modulus values were
determined for specific strains and temperatures, A plot
of secant modulus versus time for the three temperatures is shown in Figure 6 for the case of 1% strain. This
indicates up to 50% reduction in effective modulus with
increasing test times to 100 hours.

Discussion
High-temperature
properties are generally evaluated
using either constant stress (in practice, constant load)
or constant strain rate (in practice, constant machine
displacement rate). Much discussion centres on the
conversion of data generated in one test mode to the
other, i.e. the development of a constitutive relationship. This has been extensively pursued in the plastics
literatureg-12, where the viscoelastic behaviour and the
various ageing phenomena common in thermoplastics
create considerable complexities. Nevertheless, design
practice often uses constant load creep data crossplotted to produce isochronous or isostrain curves, as if
Materials & Design Volume 16 Number 1 1995

19

Creep design analysis

for a thermoplastic:

S. K. Reif et al.

TIME (hr)
Figure 6 Time dependence of secant modulus at three temperatures for 1% strain

a simple mechanical equation of state existed. Similarly,


these data, or data generated at constant machine
displacement rate, are used to generate secant moduli
for pseudo-elastic design analysis.
In reality, neither test method provides a unique
mechanical characterization; each relates to a specific
deformation path which may bear little connection to
the deformation path of a part in a device or machine.
In fact, in many cases, stress relaxation and stress redistribution are of major concern, so that an argument
may be made that the stress relaxation test could be
fundamentally more appropriate. Here, we advocate the
SRT test simply because it is more efficient and can be
used in the same way to generate the various design
curves as can the conventional test methods.
In fact, creep curves generated from SRT tests have
been shown to give good agreement with actual
constant load data6p7, so that any discussion of which
test should be used as a fundamental standard becomes
moot. Likewise, Figure 7 shows that creep curves generated using SRT show excellent agreement with experimentally determined data for VALOX.
The attractiveness of the SRT methodology
goes
beyond its ability to generate families of creep curves at
any stress. Because it can predict creep performance to
several hundred hours on the basis of a 24-hour test
without actual data extrapolation,
SRT is far more
economical as a design tool than conventional experimental creep testing. For example, the data of Figure
2(b) show stress rates to about 10 MPa/s. A conventional tensile test (at this constant stress rate) would
reach a stress of 6 MPa (corresponding to the highest
strain point of 2%) in 1667 hours, which should be
compared with the actual SRT test time of 24 hours. In
plotting the data here we have conservatively limited the
analysis to a stress rate of 1O-5 in all cases, but the enormous acceleration potential of the SRT method is
readily apparent. Furthermore,
the SRT analysis is
done in terms of total strain, eliminating the need to
20

Materials & Design Volume 16 Number 1 1995

consider a separate time-dependent elastic contribution.


Nethertheless, if desired, by dividing the stress rate by a
time-independent
Youngs modulus it is possible to
separate elastic and inelastic strain$. Although this is
normally preferred for the analysis of metals and ceramics, the viscoelastic behaviour of polymers makes a total
strain analysis simpler to perform and to apply. The
SRT methodology
could be further improved by
running stress relaxation tests from higher strains,
subsequently enlarging the usable stress range. In addition, longer SRT could be run to expand the predictable
time range, producing families of stress-stress rate
curves which encompass lower stress rates.
To determine the structural integrity of thermoplastics, designers rely heavily on modulus data. The variability of published data available to designers is
perplexing.
For example, modulus data may be
presented as any of the following: creep modulus, [f(t, e,
r)]; relaxation modulus, [f(t, s, ZJ]; complex modulus,
[f(freq, r)]; and secant modulus, [f(e, k, Z)]. Each of
these values varies enough to result in serious consequences in the design process.
In an effort to minimize confusion to designers, the
use of a single effective modulus has been proposed3.
The SRT technique shows great promise as a basis for
producing such effective modulus data. The procedure
is capable of generating secant modulus data for a wide
range of time and temperature. Furthermore, there is no
indication that the usual procedure for calculating
secant modului, based on constant strain rate, is superior to the SRT method which relies on constant stress
rate.
In summary,
the SRT approach is an accurate and
efficient means of producing long-time design information for use in pseudo-elastic design. Despite the apparent success of this methodology,
the SRT does not
model the many time-dependent and deformation pathdependent phenomena seen in polymers at elevated
temperatures. However, it does represent a significant

Creep design analysis

for a thermoplastic:

2.76

Fignre 7 Comparison

S. K. Reij et al.

MPa

experimental and predicted creep curves at 50C for three stress levels

advance in the compilation


engineering data.

of sound thermoplastic

Conclusions
Stress relaxation testing (SRT) can provide an enormous amount of information in a short time, which
can be used to compare projected performance of
different grades of a thermoplastic, and also rapidly
evaluate batch-to-batch variability.
By representing the SRT data for VALOX in the
form of stress versus stress rate plots, a series of
pseudo-tensile curves can be constructed to serve as
the basis of performance analysis and design.
Design creep curves based on strain versus time or
stress versus time were constructed and compare
well with experimental
data generated from
constant load creep tests.
SRT produces effective secant moduli values over a
wide range of time and temperature. This development could significantly aid the pseudo-elastic
design procedure for thermoplastics.

References
1 Trantina, G. G. and Ysseldyke, D. A. An engineering design
database for plastics. Materials Engineering
1987, October, 35-38

Trantina, G. G. and Ysseldyke, D. A. An engineering design


system for thermoplastics. Society of Plastics Engineers, 1989
ANTEC Technical Conference Proceedings, pp. 635639
Turner, S. and Dean, G. Criteria in determining mechanical
properties data for design, Plastics and Rubber Processing and
Applications
1990, 14, 137-144
Woodford, D. A. Test methods for development, design, and life
assessment of high temperature materials. Materials and Design
1993, 14(4), 231-241
Hart, E. W. and Solomon, H. D. Load relaxation studies of
polycrystalline high purity aluminium. Acta Met. 1973, 21,
295-307
Grzywinski, G. G. and Woodford, D. A. Design data for polycarbonate from stress-relaxation tests. Materials
and Design,
1993, U(5), 279-284
Grxywinski, G. G. and Woodford, D. A. Creep analysis of thermoplastics using stress relaxation data. Polymer Engineering and
Science, to be published
Gillis, P. P. and Medrano, R. E. A consistency criterion applicable to strain rate and stress relaxation tests. J. Mater. 1971, 6,
5 14-523

Read, B. E., Dean, G. D. and Tornlins, P. E. A predictive model


for creep in thermoplastics. Plastics and Rubber Processing and
Applications
1990, 14, 153-157
Brueller, 0. S. Predicting the behaviour of nonlinear viscoelastic
materials under spring loading. Poly. Eng. & Sci. 1993, 33 (2),
97-99
Amodeo, J. and Lee, D. Modeling the uniaxial rate and temperature dependent behavior of amorphous and semicrystalline
polymers. Polym. Eng. and Sci. 1992, 32(16), 1055-1065
Rrishnaswamy, P., Tuttle, M. E., Emery, A. F., and Ahmad, J.
Finite element modeling of the time-dependent behavior of
nonlinear ductile polymers. Poly. Eng. and Sci. 1992, 32(16),
1086-1096

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