POLYMER ENGINEERING AND SCIENCE, NOVEMBER 2002, Vol. 42, No.

11 2107
INTRODUCTION
T
he relationship between rheology and morphology
of emulsions and polymer blends is of impor-
tance, theoretically and experimentally, in order to
understand the evolution of the two-phase morphol-
ogy during mixing, since this morphology governs the
final properties of the end product. By choosing the ad-
equate composing polymers for the blend, it is possible
to obtain a large range of properties. Blend properties
in the liquid/liquid phase are generally influenced by
various factors such as the rheological characteristics
of the components, composition, interfacial tension, do-
main structure etc. (13). For the linear regime of the
viscoelastic behavior, the Palierne model (4) is known
to give rather good results in predicting the blend
properties from the component properties and the
Linear Viscoelastic and Transient Behavior
of Polypropylene and Ethylene Vinyl Acetate Blends:
An Evaluation of the Linear Palierne
and a Nonlinear Viscoelastic Model
for Dispersive Mixtures
SANDEEP TYAGI and ANUP K. GHOSH*
Centre for Polymer Science and Engineering
Indian Institute of Technology, Delhi
Hauz Khas, New Delhi-110016, India
and
P. MONTANARI, G. W. M. PETERS, and H. E. H. MEIJER
Materials Technology
Dutch Polymer Institute
Eindhoven University of Technology
P.O. Box 513, 5600 MB Eindhoven, The Netherlands
Blends of polypropylene/ethylene vinyl acetate (PP/EVA) have been investigated
for linear and transient characteristics. The emulsion model developed by Palierne
in 1990 is used to characterize the linear viscoelastic properties of the blends.
PP/EVA blends with the viscosity ratio of 0.26 and different compositions, such as
90/10, 80/20 and 70/30 wt% PP/EVA have been studied. It was found that the
Palierne Model predicts well the linear behavior of all the compositions studied. At
low frequencies, some deviation in dynamic moduli was found in case of the 70/30
composition. Structural changes are studied during transient shear flow (step-up)
experiments. A nonlinear rheological model for blends, developed by Peters, Hansen
and Meijer (PHM model), is used to describe these transient rheological data. Over-
shoots and undershoots observed in the experimental data are compared to numer-
ical results obtained with PHM model and explained on the basis of the deforma-
tion of the dispersed phase. A modification of the model is proposed in order to get
a better description of the behavior of the viscoelastic blend. Predictions of the mor-
phological evolution of the blends under stepwise increase in shear rate experi-
ments were calculated from the modified model and are found to describe the
break-up phenomenon under moderately high shear flow.
*Corresponding author: Email: akghosh@polymers.iitd.ernet.in
fraction of the dispersed phase. A vast amount of
work has been carried out on immiscible blends sub-
jected to the nonlinear regime shear flow and various
models have been proposed to understand the behav-
ior of the blends during shear flow (512). Consider-
able efforts were made to understand the mechanism
of droplet deformation, break-up and coalescence
(1316). Doi and Ohta (7) proposed a constitutive
model to describe the rheological properties of two-
phase systems with Newtonian constituents, having
equal viscosities, mixed in a nearly equal ratio. In this
model, droplet deformation, coalescence and break-up
were found to be dependent upon the stresses arising
from the interfacial tension. The model was extended,
allowing for a wider range of blend properties, by Lee
and Park (17), and their model was found to describe
the change in morphology of PS/PE blend during dy-
namic oscillatory flow rather well. Vinckier et al. (9,
10) and van Puyvelde (11) carried out extensive work
on the micro-structural analysis and rheology of a
model blend (PIB/PDMS) system. They correlated the
evolution of morphology during start-up of shear and
oscillatory flow, with the first normal stress difference
and dynamic moduli of the blends.
Peters et al. (18) recently proposed an extended ver-
sion of the Lee-Park model, which incorporates the
morphology-rheology relationship of the blends. The
model was developed to study the shear and normal
stresses in liquid-liquid systems using existing models
for the evolution of the deformation of the dispersed
phase, which was incorporated in order to remove the
adjustable parameters of the Lee-Park model. The
model predicts the viscosity and the first normal
stress difference for blends if the size and volume
fraction of the dispersed phase and rheological char-
acteristics of the blend components are known. As the
model was originally developed for Newtonian liquid-liq-
uid systems, the present work includes modifications
to incorporate shear thinning behavior and normal
stresses of the components. In the present study, lin-
ear and nonlinear viscoelastic behavior, with the cor-
responding evolution of morphology in the case of
step-up experiments, have been investigated. The ma-
terial used was a PP/EVA blend with different compo-
sitions. Comparisons have been made with the simu-
lations of both the Palierne Model, for small strain
oscillatory flow, and the PHM Model, for step-up in
shear rate experiments.
RHEOLOGICAL MODELS USED
Paliernes Model
Measurements under small amplitude oscillatory
flow provide useful information for describing the mi-
croscopic state of a blend. Paliernes Model (4) has
been found to be successful in predicting the linear
viscoelastic behavior of blends, under these flow condi-
tions. In this model, viscoelasticity of both phases, the
hydrodynamic interactions, the droplet size and size
distribution and the interfacial tension are included.
Effects of gravity and inertia are neglected. For the
case of an emulsion of two viscoelastic phases Pal-
iernes Model can be written as:
(1)
where,
,

i
is the volume fraction of the dispersed phase with a
radius R; G
m
*, G
d
*, G
b
* stand for the complex shear
moduli of the matrix, the dispersed phase and the
blend respectively, at angular frequency and is the
interfacial tension between the two polymer blend
components. Paliernes Model predicts G
b
*, without
using any adjustable parameter, once the variables
G
m
*, G
d
*, , and R are known. The morphology of the
blend affects the rheological properties to a large ex-
tent and for some concentrated systems Paliernes
Model fails to predict the viscoelastic properties (19).
Peters-Hansen-Meijer Model
A new constitutive model for liquid-liquid systems
was developed by Peters et al. (18). It is based on uni-
fying present phenomenological models and applying
a separate description of the microstructure of the
dispersed phase.
According to Mellema and Willemse (20), who
adopted Batchelors approach, the bulk stress in a
dispersion, T, can be written for Stokes flow as,
(2)
where the angular brackets denote a quantity aver-
aged over the local volume V, having the limitation
that it contains many droplets and that its statistical
properties vary negligibly, T
s
is a structure dependent
stress resulting from interfacial tension,
c
is the vis-
cosity of the continuous phase and T

is referred to as
the viscosity ratio term (17), but it too is structure
dependent.
The viscosity ratio term can be written in terms of a
series of surface integrals as
(3)
in which
d
is the viscosity of the dispersed phase, A
i
is the interfacial area of an individual droplet in V, ds
is a differential element of the droplet interface, n is
the unit normal to the interface directed into the con-
tinuous phase, and u is the local fluid velocity, includ-
ing disturbance terms due to the dispersed phase, of
the flow. The summation indicates that the quantity is
taken over all the droplets, indexed by i, within V.
T

1
d

c
2
1
V
a
A
i
1un nu2 ds
T PI 2
c
D T
s
T

G
m
*12 4 3 16G
m
*12 19G
d
*12 4
3G
m
*12 4 3 16G
m
*12 19G
d
*12 4
H
i
12
41

>
R
2 3 2G
m
*12 5G
d
*12 4 3 G
d
*12
401

>
R
2 3 G
m
*12 G
d
*12 4 3 2G
d
*12
G
b
* 12 G
m
* 12
1 3
i
H
i
12
1 2
i
H
i
12
Sandeep Tyagi et al.
2108 POLYMER ENGINEERING AND SCIENCE, NOVEMBER 2002, Vol. 42, No. 11
The structure dependent stress, T
s
, reflecting the
anisotropy of the disperse phase microstructure, can
be expressed as, (21),
(4)
in which the interfacial tension.
The viscosity ratio term contains two contributions.
An elastic component due to the interfacial tension
and another, pure viscous term, containing the rate of
deformation tensor:
(5)
for high volume fraction, of the dispersed phase.
The elastic forces resulting from interfacial stress
and unequal viscosities are combined through T

ET
s
, with
(6)
T

is determined by
(7)
where Q is the total interfacial area per volume V, T
s
(1)
is the covariant (or lower) convected derivative of T
s
and
4
L is a fourth order tensor given by
(8)
The relaxation time for deformed droplets is given by
(9)
in which Q
0
is the equilibrium area,
0
is the relax-
ation time for a non-dilute dispersion of spherical
droplets, shown by Graebling (22), to be
(10)
and f
struct
is a function of the stretch ratio which
value should approach one for slightly deformed
droplets and was chosen by Peters et al. (18) as
(11)
The final constitutive equation is written in terms of
T

ET
s
, as
(12)
While carrying out the simulations in the final equa-
tion (12) the values of
d
and
c
were not taken as the
zero shear viscosities of the dispersed and continuous
phase but were replaced by shear dependent viscosi-
ties using the Carreau-Yasuda model.
EXPERIMENTAL
In the present study, binary blends of polypropylene
(PP) and ethylene vinylacetate (EVA) were investigated.
PP (Stamylan P13E10, M
w
500 kg/mol, M
w
/M
n
6)
was supplied by DSM, Netherlands and EVA (Pilene
EVA 1802, MFI 2.0 g/min, Vinyl acetate content
18%) was supplied by National Organic Chemical In-
dustries Limited (NOCIL), Mumbai, India. The rheo-
logical properties of the PP and EVA are given in Fig.
1a and 1b.
Sample Preparation
For each type of blend, as well as for the neat poly-
mers, the same blending procedure has been applied
so that the thermo-mechanical history of the blends
and that of neat polymers remain similar. The pellets
were first dried in an air oven at 60C for 3 hrs. Next
the pellets were dry blended and fed in a mini-mixer
(with a conical corotating twin-screw geometry and a
recirculating flow) in a batch of 5 gms. The mixing was
carried out at a temperature of 200C, and rotor speed
of 150 rpm for 200 sec. The samples were taken out
from the mixer in the form of strands and quenched
in air. The strands were chopped into small granules
and compression molded at 200C for 8 min, to obtain
circular discs for the rheological measurements. The
samples were quenched in the cold press of the com-
pression molding machine. Blends with the composi-
tion 90/10, 80/20 and 70/30 wt% PP/EVA were pre-
pared.
Rheological Studies
Rheological measurements were carried out on the
neat polymers and blends, using a Rheometrics Me-
chanical Spectrometer (RMS 800) with a cone and plate
geometry having a cone angle of 0.1004 rad. and a di-
ameter of 25 mm. Linear viscoelastic properties of the
samples were investigated in a frequency range of
0.1100 Hz. The maximum applied total deformation
was kept below 0.5%. Transient shear experiments
were carried out in a range of 0.01 to 0.5 s
1
shear rate.
This shear rate range was restricted to this small value
since at high shear rates edge failure occurred (only in
the case of neat PP we were able to go up to a shear
rate of 0.7 s
1
). All the experiments were carried out at
200C under nitrogen atmosphere. Before the final
tests were carried out, each sample was preconditioned
c 2
101
d

c
2
211 2
d
13 22
c
d
c
D
0
T

T PI
f
struct
1 12
1.5
1
F 1p, 2
119
d
16
c
2 3 211 2
d
13 22
c
4
1011 2
d
110 42
c

3
4Q
F 1p,2 ;

Q
0
Q

0
f
struct
4
L
8QE
15

4
I
2
3
IT

2
EQ
T

T
s
112
c
1

D ln 1Q2
Dt
d T

4
L: D
0
E a
5
c
211 2
d
13 22
c
b
211 2 1
d

c
2
211 2
d
13 22
c
T
s
T

101
d

c
2
211 2
d
13 22
c

c

D
0

T
s

V
a
A
i
a
1
3
I nnb ds
Linear Viscoelastic and Transient Behavior, PP/ EVA Blends
POLYMER ENGINEERING AND SCIENCE, NOVEMBER 2002, Vol. 42, No. 11 2109
Sandeep Tyagi et al.
2110 POLYMER ENGINEERING AND SCIENCE, NOVEMBER 2002, Vol. 42, No. 11
Fig. 1a. Viscosity of Stamylan PP ( ) and EVA 1802 ().
Fig. 1b. Frequency sweep test for Stamylan PP (closed symbols) and EVA 1802 (open symbols) at 200C. (G*, G, G in Pa; * in Pa.s)
by shearing at a low shear rate until a stable mor-
phology was obtained. The minimum time required for
preconditioning has been established during prelimi-
nary tests. With a shear rate of 0.01 s
1
this time was
found to be 800 s. The stable morphology was con-
firmed by scanning electron microscopy for each com-
position. Preconditioning is followed by a step-up
shear rate experiment ( Fig. 2a), which allows probing
the morphology development (i.e. stretching, break-up
and coalescence) during flow ( Fig. 2b). After pre-
shearing of all blends (at 0.01 s
1
for 800 s) step-up of
0.1, 0.3 and 0.5 s
1
was applied in three different ex-
periments. The experiments were repeated several
times, also using different batches of samples.
Morphology
The morphology of the samples was studied using a
Philips Environmental Scanning Electron Microscope
(ESEM-FEG, V-type) in order to investigate the evolu-
tion of morphology generated during transient shear
experiments. For this the RMS 800 Rheometer was
stopped and the sample quenched with liquid nitro-
gen in order to arrest the actual morphology. The
samples were removed from the cone geometry and
were fractured in liquid nitrogen, in specific directions
(Fig. 3) in order to probe the morphology changes that
occur during flow in different directions.
RESULTS AND DISCUSSION
Dynamic Experiments
The dynamic moduli (G, G) and complex moduli
(G*) of the pure components and their viscosities (*)
are shown in Fig. 1b. Paliernes emulsion model was
used to estimate the droplet size of the dispersed
phase, by substituting the values of the complex mod-
uli of the matrix (G
m
* ), the complex moduli of the
dispersed phase (G
d
* ) and the interfacial tension (1.2
mN/m) into Paliernes equation. Lacroix et al. (3, 23)
reported the range of interfacial tension for PP/EVA
blend to be 0.81.2 mN/m and for a similar blend of
polypropylene and a mixture of ethylene vinyl acetate
and ethylene methylacrylate (PP/(EVA-EMA) they re-
ported the value to be 1.2 mN/m. Figures 4 6 show
the G and G for the 90/10, 80/20 and 70/30 wt%
PP/EVA blends along with the prediction of Paliernes
Model. Average droplet sizes of 1.2, 2.5 and 4.5 m
are predicted, which are in good agreement with the
experimental values obtained from microscopy, see
Table 1. The predictions of frequency dependent mod-
uli for the blends using Paliernes model are rather
good, except for the 70/30 blend, where a small devi-
ation can be seen at the lowest frequency (Fig. 6),
which becomes more pronounced at 0.01 rad/sec (not
shown in Fig. 6) (3). Steric interactions, partial misci-
bility as well as the droplet size distribution can be
reasons for this deviation. Interestingly, the droplet
size decreased after a pre-shear (at 0.1 s
1
for 600 sec)
(Table 1) leading to an improved agreement in the low
frequency region.
Transient Experiments
Transient shear rate experiments were carried out
in order to study the first normal stress difference (N
1
)
and the viscosity () of the polypropylene as well as
the PP/EVA blends. The samples were presheared at
0.01 s
1
shear rate for 800 s and then a step-up in
the shear rates to 0.1 s
1
, 0.3 s
1
and 0.5 s
1
was
given.
Figure 7a and b plots vs. time and N
1
vs. time re-
spectively, obtained from the step-up experiments
with pure PP. The final (averaged) values of first nor-
mal stress difference and viscosity are given in Table 2
for different shear rates. To determine the first normal
stress difference N
1
for the blend, the contribution of
the matrix is added by weighting with the volume
fraction. The effect of the dispersed phase on the total
first normal stress difference of the blend is assumed
to be negligible, because the presence of surrounding
drops of the dispersed phase has not been considered
during simulation of the first normal stress difference.
Figure 8i shows the experimental values along with
simulated values obtained using the PHM model, for
N
1
vs. time during the step-up experiments for the
Linear Viscoelastic and Transient Behavior, PP/ EVA Blends
POLYMER ENGINEERING AND SCIENCE, NOVEMBER 2002, Vol. 42, No. 11 2111
Fig. 2a. Schematic representation of a stepwise increase in
shear rate (step-up experiment).
Fig. 2b. Schematic of filament break-up during shear flow.
three different blends. The initial droplet radius was
obtained from micrographs of the blend samples. The
model gives a good prediction of the data at the low
and intermediate step-up in shear rates (i.e., step-up
from 0.01 to 0.1 s
1
and 0.3 s
1
) except for the 70/30
blend (Fig. 8i c) for which N
1
is under predicted.
The differences found can partly be attributed to the
assumption of an initial equilibrium state of (slightly)
deformed droplets with some average size, and the
relaxation behavior. Both the shape and size of the
interface in the blends can be different from that
predicted by the theory using kinetic equations. As ev-
ident from the SEM micrographs of 70/30 composi-
tions (Fig. 9), droplets as well as the stretched fila-
ments are present in the initial sample, leading to the
different relaxation behavior than that compared to
other compositions. In the other blends only droplets
with different dimensions were found in the initial
sample morphology.
In Fig. 8ii , the experimental and predicted (using
PHM model) values of the viscosity vs. time are shown
for the various compositions. The viscosities of the
blends were calculated using two different approaches.
In the first case the model was applied using the zero
shear viscosity (Simulation I). In that case too high
viscosities are found for the blends, as one could ex-
pect, since the PHM model is developed for viscous-
viscous system only.
In the second approach (Simulation II), the shear
dependent viscosity of the matrix material is incorpo-
rated, i.e., the viscosity for the given macroscopic
shear rate. With this modification, the predictions
Sandeep Tyagi et al.
2112 POLYMER ENGINEERING AND SCIENCE, NOVEMBER 2002, Vol. 42, No. 11
Fig. 3. Fractured surface of the
sampl e that was studi ed by
ESEM.
Linear Viscoelastic and Transient Behavior, PP/ EVA Blends
POLYMER ENGINEERING AND SCIENCE, NOVEMBER 2002, Vol. 42, No. 11 2113
Fig. 4. Comparison for experimental and Paliernes Model predictions for 90/ 10 PP/ EVA blend. (G and G in Pa)
Fig. 5. Comparison for experimental and Paliernes Model predictions for 80/ 20 PP/ EVA blend. (G and G in Pa)
were good for every composition and for all the three
step-up in shear rate experiments. Thus it can be con-
cluded that it is possible to describe the rheological
behavior of blends of viscoelastic polymers reasonably
well by the modified PHM model.
For the 70/30 composition, the morphology evolu-
tion with increase in step-up ratio has been analyzed
using microscopy. Increase in step-up ratio leads to
decrease in the droplet size, as evident from Fig. 10.
Figure 10a shows that application of step-up in shear
rate from 0.01 to 0.1 s
1
leads to the formation of
droplets of average size of 3.1 m with size distribu-
tion skewed towards the right. Increase in the step-up
ratio from 0.01 to 0.5 s
1
leads to the decrease in the
average size with the size distribution skewed more
towards left. A summing-up of variation in N
1
, viscos-
ity and average size with the step-up from 0.01 to 0.1,
0.3, 0.5 s
1
is given in Fig. 11.
CONCLUSIONS
Linear viscoelastic properties of PP/EVA blends
were studied. Paliernes model was found to describe
rather well the linear viscoelastic properties of the
blends. The model of Peters, Hansen and Meijer was
able to predict the first normal stress difference of the
blends with some over- and under-predictions. Since
the model is developed for viscous-viscous systems
the predicted viscosities, using the zero shear viscos-
ity of the matrix material, are much higher than the
experimentally obtained values. This problem can be
overcome by taking the shear rate dependent viscosity
of the matrix as measured independently. Moreover,
predictions of the morphological evolution of the
blends under stepwise increase in shear rate were ob-
tained from the modified model and are found to de-
scribe the break-up phenomenon under moderately
high shear flow rather well.
ACKNOWLEDGMENT
One of the authors (S.T.) is thankful to the Dutch
Polymer Institute (DPI) for providing the facility and
support to carry out this work during his stay in The
Netherlands.
Sandeep Tyagi et al.
2114 POLYMER ENGINEERING AND SCIENCE, NOVEMBER 2002, Vol. 42, No. 11
Fig. 6. Comparison for experimental and Paliernes Model predictions before () and after pre-shear () for 70/ 30 PP/ EVA blend.
(G and G in Pa)
Table 1. Predicted and Experimentally Observed
Droplet Size in PP/EVA Blends.
Droplet Size (m)
Blend
Composition Predicted from Experimentally
(PP/EVA) Paliernes Model obtained
90/10 1.20 1.30
80/20 2.50 2.25
70/30 4.50 4.80
70/30 (after preshear) 2.80 3.10
Linear Viscoelastic and Transient Behavior, PP/ EVA Blends
POLYMER ENGINEERING AND SCIENCE, NOVEMBER 2002, Vol. 42, No. 11 2115
Fig. 7. Viscosity and first normal stress difference (N
1
) during step-up experiments for Stamylan PP.
Sandeep Tyagi et al.
2116 POLYMER ENGINEERING AND SCIENCE, NOVEMBER 2002, Vol. 42, No. 11
Table 2. N
1
and for Polypropylene at Different Shear Rates.
Shear rate (s
1
) 0 0.1 0.3 0.5
N
1
(Pa) 0 795 3030 5300
(Pa.s) 20,000 14,900 12,200 10,800
Fig. 8i. First normal difference (N
1
) of the PP/ EVA blends
during step-up experiments (a) 90/ 10 (b) 80/ 20 (c) 70/ 30.
Fig. 8ii. Viscosity () of the PP/ EVA blends during step-up
experiments (a) 90/ 10 (b) 80/ 20 (c) 70/ 30.
Linear Viscoelastic and Transient Behavior, PP/ EVA Blends
POLYMER ENGINEERING AND SCIENCE, NOVEMBER 2002, Vol. 42, No. 11 2117
Fig. 9. Evolution of the structure for of dispersed phase in 70/ 30 PP/ EVA blend with increasing ratio of step change in shear rate
(arrow indicates the direction of flow).
Sandeep Tyagi et al.
2118 POLYMER ENGINEERING AND SCIENCE, NOVEMBER 2002, Vol. 42, No. 11
Fig. 10. Morphology and size distribution of the PP/ EVA 1802 70/ 30 wt% blend, after step-up in shear rate (a) from 0.01 s
1
to
0.1s
1
(b) from 0.01 s
1
to 0.3 s
1
(c) from 0.01 s
1
to 0.5 s
1
.
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Linear Viscoelastic and Transient Behavior, PP/ EVA Blends
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Fig. 11. Variation of first normal stress difference, viscosity and average droplet size with shear rate.