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Relaxation effects of slip in shear flow of linear

molten polymers
ARTICLE in RHEOLOGICA ACTA JANUARY 2010
Impact Factor: 1.78 DOI: 10.1007/s00397-009-0416-2

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Rheol Acta (2010) 49:267274

DOI 10.1007/s00397-009-0416-2

ORIGINAL CONTRIBUTION

Relaxation effects of slip in shear flow

of linear molten polymers
Igor B. Kazatchkov Savvas G. Hatzikiriakos

Received: 8 July 2009 / Accepted: 30 November 2009 / Published online: 15 December 2009
Springer-Verlag 2009

Abstract The transient shear response of a linear

molten polymer (linear low-density polyethylene) in
the nonlinear domain was studied using a true shear
(sliding plate) rheometer with different gap spacings to
detect slip effects. It was found that nonlinear viscoelasticity is further complicated by wall slip phenomena.
Experimental evidence suggested that static slip models
coupled with Wagners constitutive equation cannot
adequately describe the experimental data at large and
fast shear deformations. A new dynamic slip model
involving multiple slip relaxation times is proposed in
this paper, together with a method to assess the model
parameters. Significant improvement in predicting the
stress response is demonstrated by several examples of
start-up of steady shear and large-amplitude oscillatory
tests of a linear low-density polyethylene.
Keywords Wall slip Polyethylene Oscillatory
shear Wagner model Slip velocity Steady shear

Introduction
Unlike Newtonian fluids, polymer melts slip over metal
surfaces when the wall shear stress exceeds a critical value (de Gennes 1979; Lau and Schowalter 1986;

I. B. Kazatchkov
Schulich School of Engineering, University of Calgary,
Calgary, AB, Canada
S. G. Hatzikiriakos (B)
Department of Chemical and Biological Engineering,
University of British Columbia, Vancouver, BC, Canada
e-mail: hatzikir@interchange.ubc.ca, hatzikir@apsc.ubc.ca

Brochard and de Gennes 1992; Ramamurthy 1986;

Kalika and Denn 1987; Hatzikiriakos and Dealy 1991;
Boukany et al. 2006; Boukany and Wang 2008, 2009).
To determine and understand the true rheological
behavior of these materials at high shear rates, their
interfacial behavior under both steady-state and dynamic conditions should be understood. This could be
extremely useful in evaluating the relative capabilities of molecular or continuum theories in predicting
the rheological behavior of molten polymers (Wagner
1976; Wagner et al. 2005; Wagner and Roln-Garrido
2008).
Most of the previously reported slip velocity models
are static models where the slip velocity depends
on the instantaneous value of the wall shear stress.
However, experimental observations have suggested
that the slip velocity may depend on the past states of
the local wall shear and normal stresses (Hatzikiriakos
and Dealy 1991, 1992). This is similar to the concept
of the viscoelastic fluid memory where the local state
of stress depends on the past deformation history to
which the fluid particles were subjected (Hatzikiriakos
and Kalogerakis 1994; Hatzikiriakos 1995). This time
dependency of slip was referred to by Pearson and
Petrie (1968) as retarded slip due to the presence of
a relaxation slip time.
Although integral constitutive equations coupled
with a static slip velocity models can explain the
steady-state results for linear low-density polyethylenes
in simple shear, they completely fail to describe their
dynamic behavior at high shear rates, i.e., stress growth
during start-up of steady shear as will be shown in
the present work (Hatzikiriakos and Dealy 1991). The
purpose of this work is to develop a multimode slip
model, which would overcome some of the limitations

268

Rheol Acta (2010) 49:267274

of static and single-mode dynamic models and would

offer predictions that are more consistent with experimental results at high strains and strain rates where slip
is present.

Slip models for molten polymers

Static slip models
There are numerous static slip models (no time dependence) proposed in the literature (Archer 2005).
They range from very simple empirical power-law
models (Ramamurthy 1986; Kalika and Denn 1987;
Hatzikiriakos and Dealy 1991, 1992) to elaborate models based on molecular theories which take into account the molecular effects (de Gennes 1979; Lau
and Schowalter 1986; Brochard and de Gennes 1992;
Hatzikiriakos 1993; Stewart 1993). These static models
can be applied only under steady-state conditions or, at
least, they can model the steady-state slip behavior of
molten polymers. They are algebraic equations relating
the slip velocity with shear stress, normal stress, and
various other parameters including molecular characteristics. A general form is as follows:


us = us w , N1,w , Mw , MWD, T

(1)

where us is the slip velocity, w is the wall shear stress,

N1,w is the first normal stress difference at the wall, Mw
is the molecular weight, MWD is the molecular weight
distribution, and T is the temperature. However, they
are not valid under transient flows as slip relaxation
effects might become important, i.e., relaxation of polymer molecules next to solid walls are different compared to those in the bulk and thus delayed slip is
observed (Hatzikiriakos and Dealy 1991; Hatzikiriakos
and Kalogerakis 1994; Hatzikiriakos 1995). Therefore,
there is a need to derive dynamic slip models.
Dynamic slip models
Pearson and Petrie (1968) first proposed a memory
slip velocity model or a retarded slip boundary condition, as they called it, that has the following form:
us + s

dus
= (w )
dt

(2)

where s is the slip relaxation time. The choice of ( w )

depends on the considered static slip model. If s is
set to 0, a static slip model is recovered.

If a power-law slip model is used (Hill et al. 1990;

Hatzikiriakos and Dealy 1991, 1992), Eq. 2 becomes:
us + s

dus
= awm
dt

(3)

where a is a slip coefficient and m is the slip powerlaw exponent of the order of 2 (Ramamurthy 1986) or 3
(Hatzikiriakos and Dealy 1991, 1992) or 6 (Kalika and
Denn 1987; Hill et al. 1990), depending on the molten
polymers molecular structure. In order to examine its
capabilities in predicting the transient behavior of a
molten polymer in start-up of steady shear experiments,
Eq. 3 will be coupled with the Wagner (1976) model,
which in simple shear flow can be written as:
t
(t) =

 
t, t
Gi tt 
e i
dt
i
1 + (t, t )

(4)

where (t) is the stress response as a function of time,

(t,t ) is the shear deformation between times t and t ,
and are the parameters of the damping function, and
Gi and i comprise the relaxation spectrum determined
from linear viscoelastic measurements. In fact, in this
model (Eq. 4), the Soskey and Winter (1984) damping
function is used in place of Zapas (1966) for which
= 1.
A multimode dynamic slip model
Taking a closer look at the single-mode dynamic slip
model, Eq. 3, one may notice its striking resemblance
to the Maxwell mechanical model for viscoelasticity:
+

d
= 0 ,
dt

(5)

which approximates the behavior of a linear viscoelastic

material using a simple mechanical analog. A Maxwell
element consists of a linear spring (Hookean solid) in
series with a dashpot (Newtonian fluid). However, the
actual behavior of polymer melts is more complex and
cannot be represented using a single set of parameters
and 0 . The following generalized Maxwell model was
found to perform better, which is the basis of linear
viscoelasticity:
i + i

di
= 0,i
dt

and =

i .

(6)

The total stress value, , is the sum of individual contributions, i , and its accuracy depends on the number
of the {i , 0,i } pairs.
By analogy to the derivation of the generalized
(or multimode) Maxwell model from its singlemode counterpart, the single-mode dynamic slip model

Rheol Acta (2010) 49:267274

269

(Eq. 3) can be extended to a multimode one, which can

be written as follows:

Results and discussion

Rheological characterization

dus,i
= ai wm
dt

and

us =

us,i .

(7)

One constraint resulting from consideration of the

steady-state slip velocity data is that the sum of all the
slip coefficients ai must equal the static slip coefficient,
a (Eq. 3), so that Eq. 3 can be recovered from Eq. 7
under steady-state flows:


ai = a.

(8)

Experimental
Rheological experiments were carried out with polyethylene Dowlex 2049 (a linear low-density polyethylene resin) at several temperatures using first a
Rheometrics System IV to determine the dynamic
moduli G and G . The data were shifted to produce the
master curves at 200 C where most of the calculations
were performed. The data were subsequently used to
calculate the relaxation spectrum {Gi , i } of the polymer needed for calculations using the Wagners model
(Eq. 4).
An Interlaken true stress sliding plate rheometer was
used to determine the flow curve of Dowlex 2049 at two
different gap spacings at 200 C by performing steady
shear experiments. These two sets of data were needed
to determine the slip behavior of the polymer. Largeamplitude oscillatory shear (LAOS) experiments were
also used to determine the slip relaxation times and to
provide data for a stronger test of the multimode slip
velocity model.
The values of and of the damping function were
determined by measuring the stress relaxation after
imposition of step strains by means of the sliding plate
rheometer. The procedure involved the following steps:
A sudden shear strain, , was imposed on a sample initially at rest and the value of resulting shear stress, (t),
was monitored as a function of time. After allowing the
sample to rest, another step deformation was imposed
using a different value of . This was repeated until the
various values of covered a desired range, i.e., from
0.1 to 20.

The dynamic moduli, G and G , of Dowlex are plotted

in Fig. 1 at 200 C. The relaxation spectrum (Gi , i ) of
the memory function were calculated by using a nonlinear optimization technique from the linear viscoelastic data G and G (Baumgaertel and Winter 1989;
Winter et al. 1993; Winter 1997). The continuous line
represents the predictions of the calculated spectrum
indicating the excellent fit. The values are listed in
Table 1.
Figure 2 shows the relaxation modulus, G( , t), of
Dowlex 2049 at various step strains from 0.1 to 20. The
upper curves, obtained for = 0.1 and 0.2, are considered to represent the linear relaxation modulus, G(t).
These curves agree well with the relaxation modulus
obtained from the relaxation spectrum. Curves for all
other strains are below it, which manifests the dampening of the linear response. The damping function is
determined by finding the coefficient h( ), defined as:
h ( ) =

G ( , t)
G (t)

(9)

that would cause all of the curves, G( , t), to superpose

with the linear G(t), as shown in Fig. 3. The determined
damping function, h( ), is plotted in Fig. 4 together
with two fitted equations. The best fit to the experimental data is attained by using the form proposed by
Soskey and Winter (1984) with = 0.12 and = 1.8.
As seen in Fig. 4, the Zapas damping function cannot
represent the data well.

100

Dowlex 2049

10
Moduli, kPa

us,i + s,i

0.1

150 oC, aT = 2.5

G"

180 oC, aT = 1.45

0.01

0.001

200 oC
210 oC, aT = 0.95
G'
0.01

based on spectra
0.1

10

100

1000

aT, rad/s

Fig. 1 Storage and loss moduli of Dowlex 2049 at Tref = 200 C:

experimental data (symbols) and values calculated from spectra

270

Rheol Acta (2010) 49:267274

Table 1 Parameters used to solve the equations in the multimode

dynamic slip model
i (s)

Others

422.8
137.6
46.78
10.16
1.439
0.155

9.30 104
6.97 103
0.03713
0.1992
1.127
7.527

a = 1.7106 mm kPa3.06
m = 3.06
= 0.12
= 1.80

Dowlex 2049
200 oC
h = 0.45 mm

10
G(,t) / h(), kPa

Gi (kPa)

100

= 0.1

0.1

= 0.2
= 0.5
=1
=2
=5
= 10
= 20

0.01

The flow curve and static slip velocity

0.001

The flow curve of Dowlex 2049 determined from steady

shear experiments is plotted in Fig. 5. The continuous
line represents the Wagner model predictions under
the assumption of no slip. The 95% confidence interval
was calculated to accurately determine the point of
deviation from no-slip conditions. Deviations from the
experimental results were interpreted as the effect of
slip. Based on this difference, the slip velocity was
calculated as a function of shear stress according to the
method explained by Hatzikiriakos and Dealy (1991).
The accuracy of this approach was confirmed by comparing the slip velocity thus obtained with the slip data
resulting from the Mooney (1931) technique using the
flow curves at two different gaps (Hatzikiriakos and
Dealy 1991). The flow curve for the smaller gap used
are not shown in Fig. 5 for the sake of clarity. Figure 6
demonstrates an example of the gap dependence of the
shear stress response from which the slip velocity data
can be calculated. It can also be seen that the stress
response at the smaller shear rate is gap independent.
Figure 7 depicts the slip data calculated from the
two methods which are found to agree well. The slip

0.01

0.1

10

Time, s

Fig. 3 The superposition of the relaxation curves of Fig. 2 to

determine the damping function

velocity was then used to determine the slip coefficient,

a, and the exponent, m, of Eq. 3 (setting s to 0 for the
steady-state conditions). The critical shear stress for the
onset of slip was also determined and was found to be
90 kPa. The fitted parameters are listed in Table 1.
Start-up of steady shear and dynamic slip model
Figure 8 shows the start-up of steady shear of Dowlex
at the nominal shear rates (n ) of 10, 18, and 36 s1
and the model predictions of Wagners model under
the assumption of no slip. Apart from the slight underprediction of the overshoot, the steady shear is well
represented. This was the case for all other start-up
of steady shear experiments for which the steady-state

1
100

Dowlex 2049
200 oC
h = 0.45 mm

Damping factor

Relaxation modulus, kPa

10

= 0.1

0.1

= 0.2
= 0.5
=1
=2
=5
= 10
= 20

0.01

0.001

0.1

Dowlex 2049
T = 200 oC, h = 0.45 mm

experiment
1 / (1 + 0.12 1.8) - Soskey & Winter
2
1 / (1 + 0.12 ) - Zapas

0.01
0.1

0.01

0.1

10

Time, s

Fig. 2 The relaxation modulus of Dowlex 2049 obtained at

different values of step strain

10
Strain

Fig. 4 Damping function of Dowlex 2049 at 200 C. The fits are

to the equation proposed by Zapas (1966) and Soskey and Winter
(1984)

Rheol Acta (2010) 49:267274

271
100

Dowlex 2049
T = 200

T = 200 oC
Slip velocity, mm/s

Wall shear stress, kPa

100

Dowlex 2049

oC

10

experiment
95% confidence
1

10

1
Mooney technique
based on Wagner model

Wagner's model
0.1

10

100

100
-1

Shear rate, s

Fig. 5 Flow curves of Dowlex 2049 at 200 C obtained using

sliding plate rheometer and from the Wagner model

stress was <90 kPa (critical shear stress for the onset of
slip).
Figure 9 shows the start-up of steady shear of
Dowlex at the nominal shear rate of n = 110 s1 and
temperature of 200 C and the Wagners model predictions under no slip, static slip, and single-mode dynamic
slip. The Wagner model under the assumption of no
slip well overpredicts the actual experimental response
since, at this high shear rate, slip becomes significant.
Note that the steady-state stress is well above the critical shear rate of about 90 kPa and slip effects become
noticeable. To improve the prediction of the model,
the steady-state slip should be taken into account. A

300

Fig. 7 Slip velocity of Dowlex 2049 determined using the

Mooney technique and based on deviations of the Wagner model
from the flow curve

power-law static slip model (Eq. 3 with s = 0) was used

coupled with the Wagner model (Eq. 4), which resulted
in an improved shear stress response. As Fig. 9 shows,
the predicted final steady-state value exactly matches
the experimental shear stress. This is to be expected,
since the parameters of the power-law slip model (a
and m, Eq. 3) were determined based on this type of
experiment. However, the model fails to predict the
overshoot that occurs during the start-up. The static
slip model suppresses all the important dynamics of
the flow. Therefore, a dynamic slip velocity model is
needed to preserve the overshoot.

200

100
-1

36 s-1

h = 0.45 mm

110 s

80

150
h = 0.19 mm
100

both gaps, 36 s-1

50
Dowlex 2049
200 oC
0
0.0

0.1

0.2

0.3

0.4

Time, s

Fig. 6 Flow curves of Dowlex 2049 at 200 C obtained using

sliding plate rheometer at two different gaps at shear rates of 36
and 110 s1

Wall shear stress, kPa

Wall shear stress, kPa

200
Wall shear stress, kPa

18 s-1
60

10 s-1
40

20

Dowlex 2049
o
200 C
0.45 mm

0
0.0

0.5

1.0
Time, s

1.5

Fig. 8 Start-up of steady shear experiment at shear rates of

10, 18, and 36 s1 and comparison with the Wagner model
predictions under no-slip conditions

272

Rheol Acta (2010) 49:267274

200

Wall shear stress, kPa

180
160
140

Experiment
Wagner model, no slip
Wagner model, static slip
Wagner model, dynamic slip

120
100
80

Dowlex 2049
o
200 C
0.45 mm
110 s-1

60
40
0.0

0.1
Time, s

0.2

Fig. 9 Start-up of steady shear experiment at a shear rate of

110 s1 and comparison with the Wagner model predictions
under no-slip conditions, Wagner model coupled with a static slip
model, and coupled with a single-mode dynamic slip model

The Wagners model prediction using a single-mode

slip model is also shown in Fig. 9. It can be seen that
the improvement in the prediction over the static model
is dramatic; not only does it yields the correct steadystate value of the shear stress, but it also predicts the
presence of overshoot at small times. However, the
position of the predicted overshoot does not match the
experimental one; if an attempt is made to adjust it by
changing s in Eq. 3, the predicted maximum in the
shear stress would no longer agree with the experimental value.
These findings clearly call for a more versatile slip
model, capable of predicting various nonlinear phenomena under with greater accuracy. The next section
discusses the multimode slip model (Eq. 7) and the
possible methodology to fit experimental results.
Large-amplitude oscillatory shear and multimode
slip model
In using a multimode slip velocity model, a question of
great interest is how one can determine the parameters of Eq. 7., i.e., to determine the parameters of the
multimode slip model ({ai , s,i } pairs) together with the
Wagner model, as the static slip parameters are known
from steady slip experiments.
To do this, one must also choose a nonlinear dynamic
shear experiment for the purpose of comparison with
the dynamic slip model predictions. Such an experiment
should involve large enough deformations and shear
stresses that exceed the critical shear stress for the
onset of slip. Once the experimental data under slip
conditions is available, the next step is to find such a

set of {ai , s,i } parameters that minimizes the difference

between the calculated values and the experimental
data.
LAOS was chosen as a basis for fitting the additional
parameters of the dynamic slip model. The LAOS
experiments allow one to independently control the
frequency, , and the strain amplitude, 0 . By varying
these two parameters, one can obtain a wide range of
different shear stress responses at various time scales,
as well as ensure that the stress exceeds the required
threshold for the onset of slip. The following combinations of frequency and strain amplitude were used
which are listed in Table 2.
Table 3 summarizes the parameters obtained for
the three different slip models, static slip, single-mode
dynamic slip, and two-mode dynamic slip. The slip
exponent, m, is constant for all of the calculations since
it was determined from steady-state experiments. The
steady-state slip model has only two parameters which
are easily obtained by a linear regression between logarithms of the slip velocity and wall shear stress, i.e.,
using the data in Fig. 7.
The single-mode dynamic slip model adds one more
parameter, the slip relaxation time (s ). It is interesting
to note that the determined value of s , 17 ms, is about
2.5 times higher than the characteristic relaxation time
for this resin (7 ms, determined as a reciprocal of the
crossover frequency in Fig. 1). This is to be expected as
the relaxation of polymer molecules next to solid walls
is restricted.
Finally, the multimode dynamic slip model adds two
more parameters to the list. An iterative parameter
estimation procedure was used to find the number of
the {ai , s,i } pairs and their values. It was found that,
for the conditions tested, two pairs were sufficient to
adequately simulate the shear stress response. It can
also be noted that the values of ai satisfy the restriction
imposed by Eq. 8. Furthermore, the values of the slip
relaxation time, s,i , exhibit the following behavior: the
smaller slip relaxation time is s,1 = 11 ms, which is
not far from its single-mode counterpart. This value
corresponds to the strongest slip coefficient a1 . The
other slip relaxation time, s,2 , is much longer; however,

Table 2 LAOS test parameters

Frequency
(Hz)

Strain
amplitude

Shear rate amplitude

(=2 0 )

1
2
4
8
16

16
8
4
2
1

100.5
100.5
100.5
100.5
100.5

Rheol Acta (2010) 49:267274

Table 3 Parameter values for
static, single-mode dynamic
and multimode dynamic slip
models

273
Slip model

Parameters

Steady-state us =

its contribution is significantly lower, as the a2 value

is only 27% of a1 . This is similar to the behavior of
the pairs {Gi , i } where a high Gi value corresponds to
low i .
The predictions of the three slip models, steadystate, single-mode, and multimode (two-mode in this
case), are shown in Fig. 10 for two cases. The steadystate model underestimates the prediction, since it acts

Stress, kPa

Dowlex 2049, T = 200 oC

0 = 8, = 2 Hz

100
50
0

single-model and
two-mode depart

-50
-100
-150

static
single-mode
2-mode
Experiment
1.0

1.2

Time, s

200

Wall shear stress, kPa

Stress, kPa

Frequency sweep,
multiparameter
estimation

180

50
0
-50

-150

Steady shear test,

linear fit
Frequency sweep

1.4

100

-100

kPam ,

instantaneously to reduce the shear stress to its steadystate value. The single-mode model provides a better prediction, but fails when the stress value exceeds
the critical stress for the onset of slip for prolonged
periods of time. For example, in the upper graph in
Fig. 10 ( = 2 Hz, 0 = 8), the predictions of the
single-mode and two-mode models coincide until 0.06 s
(marked with an arrow). At this point, 0.06 s, the shear
stress has already reached 130 kPa, i.e., well above the
critical level (90 kPa). This means that a single-mode
slip model is capable of accurate predictions only at
very short time scales. The addition of a second set of
parameters {ai , s,i } has greatly improved the accuracy
of the prediction. Note that s,2 (which is greater than
s,1 ) is responsible for that improvement and allows
accurate predictions at longer time scales.
Figure 11 shows the prediction of the multimode
dynamic slip model for start-up of steady shear. Comparing it to the prediction of a single-mode dynamic
slip model (see Fig. 9), one can see that a significant
improvement in the accuracy of prediction is achieved.
As a final concluding remark, it is noted that
the procedure described above for the parameter

Dowlex 2049, T = 200 oC

0 = 4, = 4 Hz

150

s1

a = 6.5
mm
m = 2.8
a = 6.5 106 mm s1 kPam ,
s = 0.017 s, m = 2.8
a1 = 5.1 106 mm s1 kPam ,
s,1 = 0.011 s, a2 = 1.4
106 mm s1 kPam ,
s,2 = 0.86 s, m = 2.8

Single-mode dynamic
m
s
us + s du
dt = aw
Multimode dynamic
du
us,i + s,i dts,i = ai wm

150

Methods

106

awm

static
single-mode
2-mode
Experiment

160
140
120
Dynamic multimode slip model
experiment

100
80

Dowlex 2049
o
200 C
0.45 mm
110 s-1

60
40
0.0

0.5

0.6

Time, s

Fig. 10 Comparisons of the multimode, single-mode, and static

(steady-state) slip model predictions with experimental LAOS
data for Dowlex 2049 at 200 C

0.1
Time, s

0.2

Fig. 11 Start-up of steady shear experiment at 200 C and comparison with predictions of the Wagner model coupled with a
multimode dynamic slip model

274

determination of the proposed slip model is only the

first step. Many more experiments are required to
fully comprehend the relationships between these parameters and other properties of polymeric melts, such
as their molecular structure, characteristic relaxation
time, and interfacial behavior. In particular, it would be
desirable to see how the proposed model does in predicting stress response for other deformation histories.

Conclusions
The slip behavior of linear polymers may involve dynamics which are complicated by the viscoelastic nature
of these materials. As discussed above, experimental
evidence indicated that the assumption of a slip relaxation time is necessary to explain the transient response
of linear polymers under slip conditions. Furthermore,
while a single relaxation time can explain the experimental results qualitatively, it may be necessary to
take into account multimode effects for a quantitative
description.
In order to investigate these effects, steady shear experiments were performed for Dowlex 2049 in a sliding
plate rheometer using two different gap spacings. A gap
dependence of the flow curves was obtained. Using the
Mooney technique, the slip velocity was calculated as
a function of shear stress and fitted to a steady-state
slip velocity model. A constitutive equation, Wagners
model, was then used together with the steady-state slip
model and a dynamic slip model to predict the shear
stress response in start-up of steady shear experiments.
Although the steady-state predictions were in good
agreement with the experimental data, both models
failed to accurately describe the dynamic behavior. By
the analogy to the derivation of a generalized Maxwell
model from a simple mechanical two-element model,
a multimode slip velocity model was formulated to
take into account multiple slip relaxation times. A general procedure for the determination of its parameters
based on comparisons with the LAOS data was described. The new multimode dynamic slip model was
found to provide considerably better predictions of the
shear stress in dynamic flow conditions, such as LAOS.

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