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Creep Analysis of Thermoplastics Using Stress

Relaxation Data
G. G. GRZYWINSKI and D. A. WOODFORD*

Materials Research Center


Rensselaer Polytechnic Institute
Troy, New York 12 180-3590
One of the major factors limiting the use of thermoplastics in engineering
applications is the inadequacy of existing design data. Much of the data do not
span appropriate ranges of stress, strain, time, or temperature. This study addresses the need to develop an accelerated method for generating long-time design
data to support the innovative use of engineering thermoplastics. In particular,
stress relaxation tests (SRT) were performed on polycarbonate (PC) and modified
polytphenylene oxide)(PPO), and used to generate time-dependent design data
through the short-time measurement of the materials current state without
dependence on elastic modulus. The test results and analyses reported here
indicate the SRT method to be an efficient means of generating accurate and
repeatable creep and secant modulus data which may be directly used in design.
Therefore, SRT shows great potential both as a design parameter development
tool, and as a quality control instrument for assessing batch-to-batch variability.
INTRODUCTION

uch of the data describing the mechanical behavior of thermoplastics available to designers
today stem from practices standard for conventional
materials which neglect viscoelasticity. While these
single-point data can be used for initial material selection, they are inadequate for assessing the structural performance of a design since time-dependence
may not be properly accounted. In the cases where
necessary engineering data do exist, they most often
do not span a n appropriate range of stress, time,
temperature, or strain rate (1, 2). Thus, the current
data on engineering thermoplastics may be inadequate to fully support the innovative use of these
materials in exacting applications.
To overcome this obstacle, researchers have sought
to expand existing databases by increasing testing
efforts (3) and by developing constitutive models to
predict creep behavior in thermoplastics (4- 11). Because of the many complications associated with both
long time creep testing and detailed mathematical
modeling (12). a n alternative method for generating
high temperature design data which avoids such traditional strategies would undoubtedly be useful to
designers. In an effort to satisfy designers needs for
more complete thermoplastic design data, the authors have previously reported a practical, innovative
approach to generating tensile and creep curves for
polycarbonate through the use of stress relaxation

*Current address: Materials Performance Analysis, Inc.. 1737 Union St.


Schenectady, NY 12309.

testing (SIIT) (12). This testing method has evolved


from ;he stress relaxation analysis of Hart and
Solomon (13), where total strain ( e t ) is divided into
separate components, and a short-time modulus ( E l
is used to get elastic strain ( e e ) . The data are then
plotted in terms of stress vs. inelastic strain rate,
covering up to 5 orders of magnitude in strain rate
from short time tests (I24 h). This approach has
been recently applied successfully to generate design
data for metallic materials (14). Despite favorable results for polycarbonate, the use of a time-independent elastic modulus gave rise to some uncertainty in
the aforementioned analysis (12). To eliminate the
ambiguity, this paper reports further efforts to generate both creep and time-dependent secant modulus
( S ) data for both polycarbonate (PC) and modified
polyphenylene oxide (PPO) through the use of SRT
without specifically isolating the elastic strain compo
nent.
EXPERIMENTAL, PROCEDURE

Standard dogbone-type tensile specimens of General Electric Plastics Lexan polycarbonate and Noryl
modified poly(2.6 dimethyl 1,4 phenylene oxide) (PPO)
were stress relaxation tested in a n Instron 4204 mechanical testing system operating in the closed-loop
control mode. Samples were loaded at a constant
displacement rate of 25 mm/min, with an extensometer attached to record strain in the specimen
gage length. When the desired strain level was
reached, the displacement setting was reduced to .5
mm/min, and a constant strain was maintained in

POLYMER ENGINEERING AND SCIENCE, DECEMBER 1995, Vol. 35, No. 24

1931

G. G. Grzywinski and D. A. Woodford

the specimen. This practice of maintaining constant


strain eliminated concerns associated with machine
compliance encountered in most similar stress relaxation studies (15). The reduction of nominal stress,
u ,with time, t , was then measured for
24 h on a
strip-chart recorder, as the elastic strain was p r e
gressively replaced with inelastic strain, E,. Using
these relaxation data, u vs. In t was plotted, and
polynomial equations were then fit to these data,
which were subsequently differentiated to yield stress
rate, d u / d t . This procedure was performed at total
strain levels of 0.5, 1.0, 1.5, and 2.0% strain, and at
temperatures of 50, 65, and 80C. These curves were
then used in the construction of iso-stress rate
pseudo-tensile ( u- E ) curves, which were subsequently used to generate creep and secant modulus
curves. To eliminate history and aging effects ( 121, a n
individual specimen was used in each separate test.

40
1 5% strain
0
0

1 0% strain
0 5% strain

30

n.

E
E.,
w
F
v)

10

10

12

, . , \
in I ( 5 )

(a)

RESULTS

Representative stress relaxation and stress-stress


rate curves for Noryl and Lexan at 65C are presented
in N s . l a and b and 2a and b, respectively. The
repeatability of these curves was assessed by performing a duplicate test sequence on Noryl at 65C
as was the repeatability of such curves for Lexan in
our previous work (12). As illustrated in Figs 3a to d ,
excellent agreement was observed between the original and repeat test data at each strain level.

Generation of Creep Data


Through the use of another cross-plotting procedure, creep data were obtained from pseudo-tensile
curve families. Horizontal cuts of constant stress were
made across the iso-stress rate pseudo-tensile curves,
and each intersecting strain value was recorded. The
times to each of these strains were then calculated
using the following:
(1)

After converting t into units of hours, creep curves


( E - t ) were generated. For Noryl, this procedure was
performed at stress levels of 1.72, 3.45, and 5.2 MPa
(250, 500, and 750 psi), and the resulting creep data
are presented in Fig. 6. Stresses of 6.9, 13.8, and 20.7
MPa (1000,2000,and 3000 psi) were used for Lexan,
and Fig. 7 displays the resulting creep data for this
1932

to
Lo

u1
-iK

09-

v)

0,

Using the stress-stress rate curves (as in Figs. 1 b


and Zb), families of iso-stress rate pseudo tensile
curves for both Noryl and Lexan were constructed
through a simple cross-plotting procedure. Vertical
cuts of constant stress rate were taken across the
stress rate curves. By recording the values at which
each of the curves was intersected by such a vertical
cut, and subsequently plotting these stresses against
their respective total strains, pseudo-tensile curves
( v - E ) were produced. Resulting curves for Noryl and
Lexan at 65C are presented in Figs. 4 and 5, resp.

11

(3

Construction of Pseudo-Tensile Curves

a / (d u / d t ) = t( S )

00

07-

C .

0.

05

'

0
0

go
0
0

03

'

10-7

'""J

0
' """"

10-6

"'"-'

10-5

' """"

10-4

10.3

"*"'"'

'

10-2
STRESS RATE x - 1 (MPahec)

10-1

loo

(b)
Rg. 1 . ( a ) Stress relaxation curves in N o y l at 65C. ( b )
Stress rate curves in N o y l at 65C.

material. Note that, for comparison, actual creep results for both Noryl and Lexan, taken from the G. E.
Engineering Design Database (EDD), are also presented on Figs. 6 and 7.
Results for Noryl indicate excellent agreement between predicted (from SRT) and experimental creep
data at each stress examined. This agreement is less
impressive for Lexan, but is still reasonable.

Generation of Secant Modulus Data


In addition to tensile and creep data, designers also
rely heavily on modulus data in the context of mechanical performance of thermoplastics. Most published "modulus" values represent Young's Modulus
( E ) , or the slope of a tangent to the u - E curve at the
origin. For thermoplastics, however, this modulus is
not a constant, and is therefore not useful for design
purposes. Since this tangent modulus is often difficult to determine with precision, a secant modulus,

POLYMER ENGINEERINGAND SCIENCE, DECEMBER 1995, Vol. 35, No. 24

Creep Analysis of Thermoplastics Using Stress Relaxation Data


DISCUSSION

40

30

a.

(0

cn

20

Lu

E
in

8
In 1 ( 8 )

10

12

(a)

gEt

***
u)
v)

u1

E
L,
e

@O

o@

00
0

@O

oooo

eo

1 5% strain
1 ou strain
0 5% strain

STRESS RATE x - 1 (MPalsec)

(b)
Fg. 2. ( a ) Stress relaxation curves in Lexan at 65C. ( b )
Stress rate curves in Lexan at 65C.

i,
TI,may be used to incorporate the time/temperature dependence.
Having constructed pseudo-tensile curves through
the use of SRT, these curves were used in the generation of secant modulus (S)values for both Noryl and
Lexan. The procedure for generating these values is
similar to that by which creep curves were determined. Vertical cuts of constant strain were taken
across families of pseudo-tensile curves at a particular T, and the stress at which each of the stress rate
curves was intersected was recorded. By taking these
stress points and dividing by the strain, secant modulus ( S ) was determined at a particular E and T. This
procedure was performed at strains of 0.5, 1.0, 1.5,
and 2.0%, and at temperatures of 50, 65, and 80C.
Plots of S vs. t at these temperatures were then
produced at each strain. For Noryl, these plots are
presented in Figs. 8a to d, and similar plots for
Lexan are presented in Figs. 9a to d.

$6,

POLYMER ENGINEERING AND SCIENCE, DECEMBER

Creep data generated through the use of SRT for


both Noryl and Lexan have shown good correlation
with those generated by experiment. In comparing
experimental and SRT-generated creep data for N e
ryl, exceptionally good correlation is observed. This
correlation is perhaps even better than should be
expected from such a data generation procedure. The
agreement between experimental and SRT-generated
data for Lexan is less impressive in terms of accuracy, but the general trend observed in the predicted
data at all stresses closely matches those seen in the
experimental curves. There are a number of possible
explanations as to why the SRT-generated creep
curves better match data for Noryl than for Lexan.
Batch-to-batch variability is one possibility where, in
this case, essentially no variability exists between
Noryl samples subjected to both creep testing and
SRT, whereas there is some variability between the
Lexan samples tested. Another possible explanation
stems from the creep testing procedure itself. Due to
the loading procedure involved in experimental creep
testing, there is considerable uncertainty in determining the point of zero strain. Such uncertainty
could result in a vertical shift of the entire strain-time
curve to higher (or lower) strains than are actually
present in the test specimen. This may explain why
the strains observed in all points of the experimental
creep curves in Lexan, are, at all times, greater than
those in the SRT-generated curves. It should also be
noted, however, that the degree of variation observed
in Lexan, although considerably greater than that
seen in Noryl, may not be any more severe than that
which would be observed in actual creep tests performed on samples from different batches.
SRT certainly shows promise as a creep data generation tool. This conclusion is based on both the a p
parent accuracy of SRT-generated creep data, and
the obvious advantages this method offers over traditional creep testing. The SRT approach is a far more
economical method than traditional creep testing, a s
this approach is capable of predicting creep data to
several hundred hours from tests lasting 24 h (as
illustrated in Figs. 6 and 7 for a wide range of
stresses. Also, it has been shown that the creep data
generation procedure can be performed in terms of
total strain, without the need to specify a time-dependent elastic modulus. Although the stress for which
the longest time data may be predicted is limited to
the highest stress attained in the lowest stress rate
pseudo-tensile curve, this stress range could be easily increased by running relaxation tests from higher
strains. In addition, the predictable time range itself
may be expanded by allowing longer relaxation times
and thus producing families of stress-stress rate
curves extending into lower stress rates. It must be
stated, however, that broad conclusions regarding
the accuracy of this data generation procedure cannot yet be drawn. Before such generalizations may be
stated, additional testing is needed to assess the
issues of variability and repeatability.

1995, Vol. 35, No. 24

1933

G. G. Grzywinski a n d D. A. Woodford
14
0 5% strain

12

"1

#*
4

0.7

j o t

m
I7

D.
n*

0 ,56 /
o

0.4

0
Q

* *

14

16

1 5% strain (repeat)

0
1.4

l i

r
:
a

.P

1.2

u)

2 0% strain (repeal)
I

P
6

1'
I

1c

I
Q

I-

g@

cn

10

0.E

.*

g*

08
D

nQ*

OE

. . . .....

10-5

,,

,....I

10-4

. . . ..... . , . ,,...

10-3

10-2

10.1

. . . .."
i

STRESS RATE x - 1 (MPalsec)


(C)

&.I

3. Repeatability of stress rate d a t a in N o y l a t 65C. ( a ) 0.5%strain, (b) ~ . W


strain,
O ( c ) 1.5%strain, ( d ) 2.W0 strain.

In addition to creep and tensile data, designers rely


quite heavily upon modulus data, in the broadest
sense of the term, in performing structural performance calculations for thermoplastic components.
There are, however, incompatibilities between many
of the published modulus data, and those which are
actually needed by designers (3).Published data are
traditionally generated by plastics producers, and are
thus geared toward the development and production
of new and improved material grades. These data
thus tend to fall within the framework of chemistry/
chemical engineering. Designers, or data users, on
the other hand, require data applicable to the creation of end-products. These needs, then, lie more
within the framework of mechanical engineering.
These incompatibilities are especially significant in
the case of modulus data, such as: creep modulus
[fct, u ,TI]; relaxation modulus, [f(t, E , T)]; complex
modulus, [$frequency, TI]; and secant modulus
1934

[ fc E , i,
T)]. These variations, while convenient for
plastics producers, serve as a source of confusion to
designers, who probably have little understanding of
the polymer physics defining the various modulus
functions, and simply require appropriate numerical
values for use in design calculations.
This confusion in the communication of modulus
data between data generators and users can have
serious consequences. Modulus values typically
quoted in print [the primary, or reference, modulus
value (3)] are normally generated through constant
strain rate tests, and tend to be higher than most
other moduli generated by alternative test methods
or exhibited by in-service components. Owing to the
combined effects of high strain, long times, and variable molecular alignment, the effective modulus of a
thermoplastic may be as low a s one-tenth the commonly published value (3).Elevated temperatures, of
course, reduce this value even further. I t is therefore,

POLYMER ENGINEERINGAND SCIENCE, DECEMBER 1995, Vol. 35, No. 24

Creep Analysis of Thermoplastics Using Stress Relaxation Data

stress rate = 18stress rate = le-5

0.020

LL

cn

52MPa

Z AO 0.015
O

- I1
A
d

10

s
-c

v)

u1
CT
I-

cn

0.010

0
0

1
STRAIN (X)

TIME (hrs.)

Fig. 4. Iso-stress rate pseudo-tensile curves in N o y l at 65C.

40

30

Flg. 6. Comparison of experimental creep data us. creep


curves generated from SRT in N o y l at 65C.

0015

20

--

0010

E
cn

stress rate = 1e-3


o stress rate = le-2
A stress rate = le-l

0 005

STRAIN (%)

Fg. 5. lso-stress rate pseudo-tensile curves in Lexan at 65C.

.01

.I

10

100

1000

TIME (hrs.)

absolutely critical that downstream users of design


data recognize that the modulus and other mechanical properties of engineering plastics are multi-valued, and highly time- and temperature-dependent.
To clear some of this uncertainty, it has been p r e
posed that the formal distinctions between various
types of moduli be disregarded. Although these data
would thus lose their uniqueness, and even some of
their original precision, the resulting time-dependent
effective moduli would be more consistent and useful
to designers as a whole (3).
The procedure for generating modulus data through
the use of SRT shows enormous potential as a means
of producing effective modulus data, as is currently
needed in the thermoplastics design community ( 3 ,
16).This procedure is efficient-capable of generating
secant modulus values (in MPa) over a wide range.
Furthermore, there is no fundamental reason why
the conventional means of generating secant modu-

Ftg. 7. Comparison of experimental creep data us. creep


curves generated from SRT in Lexan at 65C.

lus data (constant strain rate) should be considered


superior to the SRT method (constant stress rate).
Finally, while these moduli generated through SRT
may be approximations to the values applicable to
any single application, they are nevertheless likely to
be more realistic estimates' than standard, unadjusted reference moduli.
In summary, what has been developed here is a
methodology by which long-time data for use in a
pseudo-elastic design approach may be generated
with reasonable accuracy and greatly improved efficiency. This methodology is not, however, rigorous
under all circumstances. Since the many time-dependent phenomena manifested in polymers exposed to
elevated temperatures, such as physical and thermal
aging, may not be accommodated, this methodology

P O L Y M E R ENGINEERING A N D SCIENCE, D E C E M B E R 1995, Vol. 35, N o . 24

1935

G. G. Grzywinski and D. A. Woodford

"1

3000 I

2400

::I,;\

2200

1800
1600

1400

\o-

600
400
200

or

.01

........' . . . . . . . .' ........' . . .


1

10

100

0
1000

01

10

100

loo0

TIME (hrs )

TIME (hrs.)

(b)

(a)

I-

1400
1400

1000 -

1200

800

400 ;
400 ;
600

200

0
01
TIME (hrs )

O
B\D

\*

\.

*\*

. . . . . . . .'1 . . . . . . . 1.'

- * .
" ' Y

10

100

1000

TIME (hrs )

(C)
(d)
FUJ. 8. ( a ) Time-dependenceof secant modulus in Noryl at 0.5% strain, generatedfrom SRT. ( b ) rime-dependence of secant
strain, generatedfrom SRT. ( c )Tim-dependence of secant modulus in Noryl at 1.5%strain, generated
modulus in Noryl at 1 .WO
from S m . ( d ) Time-dependenceof secant modulus in Noryl at 2.Wo strain, generatedfromSRT.

does not claim to characterize thermoplastics for all


themomechanical histories. I t does, however, provide a significant advance a s a basis for efficient
engineering design with thermoplastics.
CONCLUSIONS

1) Data from Stress Relaxation Testing (SRT) can be


correlated with traditional design data.
2) Constructed iso-stress rate pseudo-tensile curves
may be used as a means of quality control to
assess batch-to-batch variability.
3) Long-time creep curves generated through SRT
show close agreement with creep data, and thus
show potential as a design tool. Additional testing
is necessary to assess accuracy and repeatability.
1936

4) Secant moduli generated though SRT show


promise in providing useful effective modulus data
over a wide range of times and temperatures, and
thus may prove to be a significant aid in the
thermoplastic component design process.
5) The SRT methodology for generating design data is
significantly more time and cost efficient than traditional long-time tensile and creep testing a p
proaches.
ACKNOWLEDGMENTS

The authors wish to acknowledge the continued


experimental support and advice from Donald Van
Steele. The contributions of Dr. Gerald G. Trantina
are also greatly appreciated.

POLYMER ENGINEERING AND SCIENCE, DECEMBER 1995, Vol. 35, No. 24

Creep Analysis of Thermoplastics Using Stress Relaxation Data

TIME (HRS )

(a)

m. 9. ( a ) Time-dependence of secant

modulus in Lexan at 0.5% strain, generated from SRT. ( b ) Time-dependence of secant


modulus in Lexan at 1.0% strain, generatedfrom SRT. ( c ) Time-dependence of secant modulus in Lexan at 1.5% strain, generated
from SRT. ( d )Time-dependence of secant modulus in Lexan at 2.0% strain, generatedfrom SRT.

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Papers, 35,635 (1989).
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7. J. Duxbury a n d I. M. Ward, J. Mater. Sci. 22. 1215
(1987).

8. B. E. Read, G. D. Dean, a n d P. E. Tomlins, Plastics


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Ahmad. Polyrn Eng. Sci., 32, 1086 (1992).
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Design, 14,279 (1993).
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14. D. A. Woodford. Mater. Design, 14,231 (1993).
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POLYMER ENGINEERING AND SCIENCE, DECEMBER 1995, Yo/. 35, No. 24

Revised May 1994

1937

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