Comparing The Effect of Corona Treatment and Block Copolymer Addition On Rheological Properties of Polystyrene

Comparing the effect of corona treatment and block copolymer addition on
rheological properties of polystyrene/polyethylene blends

M. Bousmina, P. Bataille, S. Sapieha, and H. P. Schreiber
Citation: J. Rheol. 39, 499 (1995); doi: 10.1122/1.550709

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Comparing the effect of corona treatment and block
copolymer addition on rheological properties of
polystyrene/polyethylene blends
M. Bousmina, a) P. Bataille, S. Sapieha, and H. P. Schreiber
Department of Chemical Engineering, Ecole Polytechnique, P.0. Box

6079, Station "A" Montreal H3C 3A7, Quebec, Canada
(Received 26 April 1994; accepted 14 December 1994)
Synopsis
The effect of corona treatment and copolymer modification on linear viscoelastic properties of
PSIPE blends in the molten state has been investigated. The results show that corona treatment has
little effect on rheological properties of the blends. On the other hand, SEBS addition results in an
appreciable decrease of the elastic modulus in the low-frequency region and in a more evident
secondary plateau. The data have been analyzed quantitatively by Palierne's emulsion model, which
takes into account the presence of an emulsifier agent. The model has been used to estimate the
interfacial tension in PSIPE blends as modified by corona treatment and by SEBS copolymer
modification. Addition of as little as I wt % copolymer resulted in a fivefold decrease of interfacial
tension, whereas only a little change was observed in the case of corona modified blends. Further,
corona treatment did not affect the size of the dispersed particles, whereas I wt % SEBS addition
reduced the particle size of the dispersed phase by a factor of 5. Experiments as well as simulations
also have been carried out to examine the individual effects of viscosity ratio, particle size
distribution, and interfacial tension on dynamic moduli of the blends. © 1995 Society ofRheology.
I. INTRODUCTION
When two or more immiscible polymers are blended, phase separation occurs. Coarse,
unstable morphologies are observed, leading to weak mechanical properties. These bulk
properties of the blend are essentially controlled by the nature and the properties of the
interface and the interphase.
Compatibilization and modifications of the interface are then needed to enhance ad-
hesion between the phases. To achieve this enhancement, a number of strategies may be
used. The common approach consists of adding a third component, which is totally or
partially miscible (or at least compatible) with both phases. The additive may be a
homopolymer, like polymethyl methacrylate (PMMA), added to immiscible blends of
poly(styrene-co-acrylonitrile) (SAN) with polytstyrene-co-maleic anhydride) (SMA) or
with poly(vinylidene fluoride) (PVF2) (Machado and Lee, 1994; Kwei et al., 1977) or a
suitable block or graft copolymer, such as styrene-co-ethylene-butene random copolymer
(SEBS), added to polystyrene/polyethylene (PElPS) (Locke and Paul, 1973); Barentsen
etal., 1974; Fayt etal., 1981; Lindsey et al., 1981; Schwarz etal., 1988). Compatibili-
zation may also be achieved in situ during melt-blending of two immiscible polymers
a)Corresponding author. Present address: Departement de Genie Chimique, Faculte des Sciences et de Genie,
Universite Laval, Quebec, QC.. Canada G IK 7P4.
© 1995 by The Society of Rheology, Inc.

l Rheo!. 39(3), May/June 1995 0148-6055/95/39(3)/499/19/$7.00 499
500 BOUSMINA ET AL.
contammg chemically interacting groups (Baker and Saleem, 1987; Teh and Rudin,
1991). Ionomers also have been used to provide enhancement of the adhesion at the
interface (Bazuin et al., 1993).
The above methods represent chemical routes toward compatibilization. Physical strat-
egies are also applicable and are of growing interest in adhesion technology. Among
these, we note particularly the surface activation methods, such as cold plasma treatment
at atmospheric pressure and low or high current-density discharges, such as corona or arc
plasmas (Blais et al., 1971). Usually these treatments have been used to surface modify
films. promoting printability, or in multilayer systems to improve adhesion between me-
tallic substrate and polymers. Surprisingly, only little effort has been made to extend this
procedure to the area of polymer blends.
Initial studies performed in our laboratory (Schreiber et al., 1990; Dong et al.• 1993)
have shown that corona treatment improves the mechanical properties of polyolefin com-
posites, in which CaC0 3 or cellulose fibers were the reinforcing agents. Air-corona treat-
ment has been shown to modify surface properties of the composite components and to
improve adhesion between the phases. Corona treatment may also be applied to improve
adhesion between two thermoplastic polymers. In a previous paper (Bousmina et al.,
1994a) we have shown the applicability of this method to enhance adhesion in blends of
PE and PS. We have also compared the emulsification effect of corona treatment and of
SEBS copolymer addition on morphological and mechanical properties of the PSIPE
polymer blends. The results obtained revealed that SEBS addition is more effective than
corona treatment in stabilizing the morphology of the blends, and in enhancing their
mechanical properties. Nevertheless, relative increases of tensile strength and elongation
at break were obtained on samples prepared by the simple melt-blending of corona
treated PE and PS components.
The processing/morphology/property relationships in immiscible polymer blends are
influenced by the rheological properties of their molten components. Conversely, the flow
properties of the blends depend on their morphology and, hence, also on the modification
of blend morphology, such as size reduction and stabilization of dispersed particles, due
the compatibilization of the blend. Rheological methods are powerful tools to elucidate
such modifications and give information permitting one to optimize processing condi-
tions. In this paper, we focus on the effects of surface/interface controls, obtained by
corona treatment and SEBS addition, on melt rheological properties of PSIPE blends.
1\vo important criteria can be used to evaluate the effectiveness of a compatibilization
strategy to emulsify the interface in polymer blends: (i) decrease of interfacial tension
and thus a decrease in the particle size of the dispersed phase to dimensions permitting
the blend to be considered macroscopically "homogeneous;" (ii) enhancement of adhe-
sion between the components, allowing for better stress transfer in the material. In this
study, we will use the interfacial tension as a pertinent parameter to evaluate the effec-
tiveness of blend modification procedures. Accordingly, we will compare the decrease of
interfacial tension in PSIPE blends modified by corona treatment and by SEBS copoly-
mer addition. In fact, when two thermodynamically immiscible polymers are chemically
or physically forced toward compatibilization, the interfacial tension between the blend
components decreases (Wu, 1982; Elmendorp and de Vos, 1986).
In this work, we have used melt rheological measurements to determine the interfacial
tension in PSIPE blends. A rheological emulsion model was used. This leads to an
interpretation of blend properties based on the interfacial tension and on the deformability
of the minor dispersed phase.
COMPATIBILIZED BLENDS 501
TABLE I. Description of the blends. T indicates that the polymer was treated by corona discharge.
System Series Description
PSIPE (70/30) Al Control blend

PSIPE (30170) A2 Blend with the inverse composition of
that of blend Al
TPSrrPE (70130) B Both components corona treated
before melt blending
PSIPE (70/30) C PSIPE blends modified by I wt %
+1 wt% SEBS SEBS copolymer
II. EXPERIMENT
A. Materials
PS, PE, and SEBS triblock copolymer used in this study were commercial polymers.
The linear low-density polyethylene (LLDPE GI5026; MI = 50 g110 min) was supplied
by Novacor in powder form. The polystyrene, in the form of spherical beads, approxi-
mately 0.5 mm in diameter, was obtained from Polymers Scott Ltd. SEBS triblock co-
polymer (KRATON 01650), from Shell Chemical Co., was used as interfacial modifier.
It contained 30% by weight of end-block polystyrene (S) and 70% by weight of hydro-
genated polybutadiene midblock (EB), which has a structure similar to ethylene-
(butene-I) random copolymer. EB blocks are miscible with PE, and S blocks are chemi-
cally identical to the PS phase. This structure is expected, therefore, to penetrate both
blend components.
B. Corona treatment
Corona treatment was performed with a system developed in our laboratory. It consists
of two flat aluminum electrodes separated by a quartz-dielectric plate. Teflon rings were
fixed to the bottom electrode, forming a cylindrical cell. The sample was placed in the
cell and covered by the dielectric electrode, and then by the other aluminium electrode.
This geometry provided uniform corona treatment for the polymers used in this work.
The corona cell volume was 5 cnr', For each treatment 4 g of polymer was used. Treat-
ment conditions were 20 rnA, 60 s, at a frequency of 3.5 kHz, and a voltage of 10-15 kYo
The experiments were performed in an air-conditioned room with a relative humidity of
50% and a temperature of 23°C. Corona treated polymers were melt blended within 30
min of treatment. XPS analysis performed on PS and PE revealed the incorporation of
new chemical species, namely C-O (ether), C = 0, or O-C-O (carbonyl or double
ether), 0 = C-OH or 0 = C = O-C (carboxyl), and C-N or C = N (amine or imine),
due to air-corona treatment. The quantitative analysis of the relative concentrations of
these various functionalities also revealed a decrease in C-C bond concentration
(Bousmina et al., 1994b). These chemical modifications may be expected to have an
important effect on rheological properties of the polymers.
C. Blend preparation
PSIPE blends with weight compositions of 30nO and 70/30 were used. The blends are
described in Table I. All the blends studied were prepared in the same conditions by first
dry blending and then fusing and mixing for 5 min in a Brabender batch mixer at 180°C,
and a rotor speed of 50 rpm. The time of mixing was defined by the attainment of
constant torque values, and this occurred generally in about 3-4 min.
502 BOUSMINA ET AL.
TABLE II. The thermal shift factors for PS, PE, blend AI, and blend A2
with respect to the 200 DC reference.
PS PE Blend Al BlendA2
150 2.08 0.58 2.12 0.51

170 1.13 0.32 1.23 0.28
ISO 0.76 0.17 0.63 0.16
220 -0.52 -0.26 -0.59 -0.23
235 -0.84 -0.41 -1.01 -0.37
The blends may be divided into three series: control untreated blends, corona modified
blends, and copolymer modified blends. They are identified in Table I by the code letters
(A), (B), and (C), respectively. Series B was obtained by mixing components which were
treated by corona discharge, as reported below. Series e was obtained by premixing all
the components together (PS, PE, and SEBS) before blending in the batch mixer. The
effect of copolymer was investigated at a concentration of I wt %. The melt-blended
compounds were compression moulded at 200°C and 3.5 bars for 5 min. This gave
specimens in the form of 25 mm diameter disks, suited for rheological measurements.
D. Scanning electron microscopy
Blend morphologies were examined by scanning electron microscopy using the Jeol
model JSM-820 apparatus. The samples were fractured in liquid nitrogen and then coated
with gold/palladium (50150), to avoid charging.
E. Rheological tests
Small-amplitude oscillatory shear measurements were carried out on a Bohlin eSM
constant stress rheometer in the parallel-plate geometry, with 25 mm diameter platens.
Prior to testing, the specimens were dried under vacuum at 70°C for at least 48 h. The
tests were made under a continuous purge of dry nitrogen. The temperature was varied in
the range 140-230 oe. No thermal degradation occurred during the measurements as
verified by repeated measurements and by comparisons of dynamic moduli with those
obtained initially. Morphological analyses were made before and after dynamic measure-
ments. These showed that the morphology was stable during the measurements. The
frequency sweeps were from 0.01 to 100 rad/s. Depending on frequency and temperature,
the stress was adjusted to ensure that the rheological behavior was in the linear viscoelas-
tic range.
III. RESULTS
The curves for storage shear modulus G I and loss shear modulus Gil at various
temperatures, as a function of frequency, were superimposed onto master curves at
200 "C, using the time-temperature superposition principle. The thermal shift factors at
various temperatures, with respect to the 200°C reference, for both components and for
blends Al and A2 are listed in Table II. Rigorously, the time-temperature superposition
principle was established only for pure homopolymers. Nevertheless, experimentally the
superposition was found to be valid for the PSIPE blends, in the range of the temperatures
tested. The blend shift factors are close to those of the corresponding matrix polymers.
The master curves for G I and Gil are shown in Figs. I and 2. Rheological character-
istics of the components in the terminal zone and those of blend A 1 are given in Table III.
.4
t: 3
.51
C,
" 2
J • Q'
a-
PS
PS
o (J' PB
0 lL a- PB
aeneralised Maxwell
-j
-3 -2 -j o 2 3 .4 5
Log(ro In radiI)
FIG. 1. Dynamic shear moduli G', Gil vs frequency for PS and PE at 200 "C.
The zero-shear viscosities and terminal relaxation times are 2.2X 102 Pa s and 0.002 s for
PE, and 1.3X 104 Pa sand 0.740 s for PS, respectively. The zero-shear viscosity ratio
k = 'TJI/'TJM (/: inclusions; M: matrix) is 0.017 for blend Al and 59 for blend A2.
Roughly speaking, the terminal relaxation time can be defined as the inverse of the
critical frequency, below which the terminal zone appears. Figure 2 shows that the elastic
modulus of blend Al is lower than that of the matrix at high frequencies, whereas the
opposite behavior is noticed in the low-frequency range. In the latter frequency region,
the rheological behavior of the blend is very different from that of the components. The
blend is characterized by an increase in the elastic modulus and by a substantial shift of
the terminal zone to lower frequencies, corresponding to a long relaxation time process.
..
a.
.51
.4
3
C.
2 tI>'" 0
! "
" ' " 00
0
e:P
0
G',G"
C',C'
PS
PE
0
0
.
a
C'
C"
G'
Ble-ndAl
Blend A.I
lSIead A:1
C' BIe_dILl
-1
-4 -3 -2 -1 0 2 3 4 5 6
Log(ro lD radls)
FIG. 2. Comparison between dynamic shear moduli G', G" vs frequency of blends Al and A2 and their
corresponding matrixes PS and PE at 200 -c. Blend AI: PS/PE (70/30); blend A2: PSIPE (30170),
504 BOUSMINA ET AL.
TABLE III. Rheological characteristics of the samples in the terminal

zone at 200 'c.
Zero-shear viscosity Terminal relaxation time

Sample (Pa s) at 200 °C (s) at 200 °C
PS 1.3 X 104 7.4XIO- 2

PE 2.2X 102 2.0XlO- 3
Blend AI S.4X 104 40
The end-relaxation time of the blend is of the order of 40 s, much higher than the
relaxation times of the individual components (0.002 s for PE and 0.740 s for PS), as
reported in Table III. On the other hand, no secondary plateau is observed in the low-
frequency range for blend A2, which has the inverse composition.
Figure 3 shows the effect of corona treatment and SEBS modification on dynamic
moduli of the blends. Corona treatment produces only small effects, with a slight de-
crease of the dynamic moduli of the blends. This seems to be essentially due to a decrease
in polystyrene viscosity, induced by corona treatment, as shown in Fig. 4. In contrast,
copolymer addition results in an appreciable decrease of the dynamic moduli at low
frequencies (between 0.01 and I rad/s) when compared to those of the unmodified blend.
The width of the plateau and the terminal relaxation time have been increased. The
morphologies of these blends are shown in Fig. 5, where a comparison is made of
scanning electron micrographs taken from fracture surfaces of the unmodified and the
modified PSIPE blends. The histograms of particle size distributions are given in Fig. 6.
Clearly, corona treatment has no effect on particle size, whereas a substantial reduction in
particle size and a relative reduction of particle size distribution were produced by I wt %
copolymer addition.
The effect of copolymer addition on mechanical properties of immiscible polymer
blends is well described in the literature. In contrast, the effect on rheological properties
remains poorly documented. Different results have been reported and variously refer to
8
7
6
...:
+ 5
l 4
.!l
b, 3
~
J2 ..o G'
G'
BInd AI
BInd AI
G'
..... -
0 ....-+- G"
G'
G"
BInd-
_c
..... c
-1
-4 -3 -2 -1 0 2 3 4 5
Loa(Ol III ndls)
FIG. 3. Effect of blend modification on dynamic shear moduli G', Gil of PSIPE (70130) blend at 200 "C.
Corona treated blend (blend B): A = 0; I wt % SEBS modified blend (blend C): A = 2.
COMPATIBILtZED BLENDS 505
5
... 1'8
• '1'I'B
4 -e- l'B
• '1'1'11
... 3
t.
.! . . . . .11 Iii
2
'!
o.......~.......~......................................~........~....................
-2 -1 o 2 3 4 5
Log(ro ID radls)
FIG. 4. Effect of corona treatment on dynamic shear viscosity of PS and PE components at 200 "C.
no effect, to an increase as well as to a decrease of melt viscosity of the blends, when a

copolymer is added. For example, Utracki and Sammut (1988) studied the effect of SBS
copolymer on the rheological behavior of PEIPS blends under steady-shear flow. No
significant effect of copolymer addition was observed either on morphological or on
rheological properties of the blend. On the other hand, several authors reported substan-
tial effects of copolymer addition on the rheological properties of polymer blends. For
instance, it was reported that the addition of copolymer increases the dynamic viscosity
of polypropylene/polyamide 6 (PPIPA6) blends (Germain and Genelot, 1991). Similar
results were also reported by Nishio et at. (1994) for PPIPA6 blends and by Matsuo and
Takahashi (1994) for polyethylene terephthalate (PET)IPA6 blends. Other studies con-
ducted on PSIPA6 revealed that copolymer addition resulted in a decrease of the viscosity
at high shear rates and an increase at low shear rates (Chang and Hwu, 1991). Brahimi
et al. (1991) found that the effect was very sensitive to the concentration and to the
structure of the added copolymer. Thus 1 wt % addition of tapered diblock styrene-
butadiene copolymer decreased the viscosity of high-density polyethylenelhigh impact
polystyrene blend (HDPElHIPS), whereas the opposite behavior was observed when the
blend was modified by 5 wt % addition of the copolymer. The authors stated that, when
added in large amounts, a portion of the copolymer was localized between the two
phases, saturating the available interlace, the rest dispersing preferentially in one or other
of the phases, forming micelles. Recently, Macosko (1994) showed that the formation of
micelles in PSIPMMA blends occurs when the concentration of PS-co-PMMA diblock
copolymer is larger than 1-2 wt %. The critical concentration, at which the formation of
micelles is favored, depends both on the structure and the molecular weight of the
copolymer.
In our investigation the copolymer was added at a concentration of 1 wt % by weight
so as to avoid the possible aggregation of the copolymer.
IV. DISCUSSION
This section contains additional comments and discussions of our findings. An effort is
made, by application of a theoretical model, to rationalize the results. The melt rheology
506 BOUSMINA /Z-AL.
(4
FIG. 5. SEM micrographs of (a) umnodilied PSIPE (70130) blend, (b) corona treated PS/PE (70/30) blend, and
(c) 1 wt % SEBS copolymer modified PS/PE (70/30) blend.
45
40
S5
SO
25
20
15
10
5
0
6 8 10 12 14- 18
"
(a)
--
~
"--"
45
40
35
>. SO
o 25
~
OJ 20
;:1 15
o- 10
~
OJ
~
5
0
6
n 8 10 12
n n'n
14 18
r.1
20 22
" '8
(b)
45
40
35
30
25
20
'5
10
5
0
1.0 1.2 '.4 1.6 1.8 2.0 2.2 2.4 2.6 2.8 3.0
(c)
Radius
FIG. 6. Histograms of particle size distributions of (a) unmodified PSIPE (70/30) blend, (b) corona treated
PSIPE (70/30) blend, and (c) 1 wt % SEBS copolymer modified PSIPE (70/30) blend.
508 BOUSMI NA ET AL.
of polymer blends is generally characterized by pronounced elastic properties and a long

relaxation-time process. This phenomenon, common in multiphase systems (Han and
Huang, 1985; Scholz et al., 1989), has been discussed by several authors. For instance,
Frohlich and Sack (1946), Oldroyd (1953, 1955), and then Choi and Schowalter (1975)
attributed this to the deformability of suspended droplets under a macroscopic strain. The
mechanism was described by theory which considers a balance between hydrodynamic
forces, which deform the particles, and interfacial forces, which try to maintain the
particles in their spherical, equilibrium shape. However, among the explanations about
the origins of blend elasticity, only Oldroyd's and Choi-Schowalter's constitutive equa-
tions include the interfacial parameter explicitly. Their models, however, were restricted
to dilute and semidilute emulsions of two Newtonian liquids, with monodisperse particle
sizes of the dispersed phase.
Recently, Palieme (19901199 I) proposed an emulsion-type model including the vis-
coelasticity of the phases, hydrodynamic interactions, and the effect of interfacial tension.
It is applicable to concentrated systems, taking into account the polydispersity of both the
nature and the particle sizes of the dispersed phases. Graebling et at. (1993) have found
the Palieme model to predict accurately the experimental behavior of PSIPMMA and
polydimethylsiloxanelpolyoxyethylene (PDMSIPOE) blends. Germain and Genelot
(1991) found good agreement between the predictions of the model and experimental
data for PPIPA6. Lacroix et al. (1994) showed that the model well describes the linear
viscoelastic properties of polyethylene terephthalate glycol/polyethylene vinyl acetate
(PETGIEVA) blends at different temperatures and compositions. Further support comes
from Brahimi et at. (1991), who found that the model well predicts the rheological
behavior of HDPElHIPS, but failed when the blend was modified by copolymer addition.
Some discrepancies between predictions of the model and experiment also were reported
by Kim and Denn (1992) for polymer blends containing a liquid-crystalline phase. Ad-
ditionally, Bousmina and Muller (1992, 1993), Bousmina and Carreau (1993), Carreau
et at. (1993, 1994), and Carreau and Bousmina (1994) have shown that the model works
well for blends of two viscoelastic polymers (PSIPMMA, PAlPP), but fails for concen-
trated multiphase systems in which the dispersed phase is nondeformable (PMMN
rubber, PS/rubber, PNrubber). The discrepancies between the model predictions and
experimental data were attributed to particle-particle interactions, neglected in the
model. Interestingly, the Palierne emulsion model also takes into account the presence of
a modifier agent. This makes the model well suited for considerations of the degree of
miscibility or immiscibility in multiphase systems. In this study, we have used the
Palieme model to make quantitative comparisons of the effect on the linear viscoelastic
properties of PSIPE blends due to corona treatment and copolymer addition. The com-
parison is based on estimated variations of interfacial tension in modified blends, as
discussed further in the following section.
A. Emulsion model
For a two phase system constituting a dispersion of viscoelastic incompressible inclu-
sions in a viscoelastic incompressible matrix, the model expresses the complex shear
modulus of the blend CGt) as a function of the complex shear moduli of the individual
phases (G!t: matrix; Gj: inclusions) and the ratio of interfacial tension and droplets
size CaIR i)' That is,
1+3"'J:,·¢H{w)
G*() G* ( ) , I I (I)
b W = M W 1-2"'J:,i¢#i(W)'
where
4(alR j)[2G,t(w) + 5Gj(w)]+[Gj(w)-G,t(w)][16G,t(w)+ 19Gj(w)]

Hlw) = 40(alR i)[G,t(w)+Gj(w)]+[2Gj(w) + 3G,t(w)][ 16GZ,(w)+ 19Gj(w)]" (2)
The summation is carried out over the distribution of droplets sizes (¢>i is the volume
fraction of droplets with radius R j). For systems with monodisperse particle size distri-
bution, Palierne's constitutive equation reduces to an expression similar to that of Old-
royd's model. For narrow distributions, good agreement between model predictions and
experimental data is obtained, if the summation over the distribution of particle sizes and
the volume fractions are replaced by the volume-average particle radius and the total
volume fraction of the dispersed phase, respectively (Bousmina and Muller, 1993). In this
paper, we compared the predictions obtained with particle size distributions to those
obtained by considering only volume-average values.
We note that in his approach Palierne took into account the deformation of the inter-
face through two frequency dependent parameters p' (w) and {i'(w), which represent the
dilatation and the shear moduli of the interface, respectively. These two parameters may
play a role for blends modified by addition of an interfacial agent. However, these pa-
rameters are difficult to determine experimentally. If we set P'(w) and {i'(w) equal to
zero, which amounts to take a constant interfacial tension, Eqs. (1) and (2) follow, and
satisfactory agreement between experiment and model predictions is obtained for a blend
of two thermoplastic polymers (Bousmina and Muller, 1993). In present experiments, we
assumed that the interfacial tension does not vary with the deformation (but does with
copolymer addition), and we used Eqs. (1) and (2) to estimate the interfacial tension in
both unmodified and modified PS/PE blends.
If the dynamic moduli G' and Gil of the phases, the particle size, and the interfacial
tension are known, the dynamic shear moduli of the blend (G~ and G~), with uniform
particle size distribution, can be easily calculated from the above equations (1) and (2).
The real and imaginary components of the complex shear modulus of the blend are given
by
G~ = llD[G~(BIB2+B3B4)-G~(B4BI-B2B3)],
(3)
G~ = l/D(G~(BIB4-B2B3)+G~(BIB2+B3B4)]'
where
B I = C I-2¢>C3'
B2 = C I + 3¢>C3 ,
(4)
B 4 = C Z+3¢>C4.
D = (Cz-2¢>C4)Z+(CI-2¢C3)2.
The constants C j are given by the following expressions:
CI = 40alR(G~+G;)+38(G;Z-c'?)+48(Gj-G';J)+89(G~G;-G~G7),
Cz = 40alR(G~+G7)+96G~c'~+76G;G7+89(G~G;+G~G7),
(5)
510 BOUSMINA ET AL.
C3 = 4a/R(2G'M +5G')-16(G,2_
I M G,,2)+
M
19(G,2_
I G"2)-3(G'
I MI
G' -c;MI'
Gil)
C4 = 4a/R(2d,'M +5G")-32G'
I MMG" +38G'G"-3(G"
II MIG'+G'MI'
Gil)
Equations (3)-(5) can be summarized by the following expression:
G~ ,G~ = f( G~ ,G~ ,G; ,G; ,R,a,f/J). (6)
All the parameters appearing in this equation are experimentally accessible. The knowl-
edge of the dynamic moduli of the phases, the particles size, the volume fraction, and the
interfacial tension allows the use of the emulsion model to predict the dynamic moduli of
the blend, without any fitting parameter. When the interfacial tension is unknown, the
model can be used to determine its value by fitting theoretical curves to experimental
data. The value of a giving the best fit represents an evaluation of the interfacial tension
parameter.
The low-frequency plateau on G', generally observed for immiscible polymer blends,
is a manifestation of the interfacial tension effects. This leads to a shift of the terminal
zone to lower frequencies. For an emulsion of two Newtonian liquids (G,t = i WT/M,
Gj = iWT/I; I: inclusions, M: matrix), Eqs. (1) and (2) amount to Oldroyd's result. In
this case, the time corresponding to the frequency, separating the plateau on G' and the
terminal zone (G I IX w 2 , G" IX w) is determined by the differentiation of G' f W by fre-
quency W [at W = VAw, d(G' Iw)ldw = 0]:
A = (R"IM) (19k+16)[2k+3-2f/J(k-1)]
(7)
w 4a lO(k+ 1)-2f/J(5k+2) ,
where k = "Ill T/M is the zero-shear viscosity ratio. This expression for the relaxation
time of the emulsion is related to the deformability of the dispersed droplets.
B. Influence of particle size and interfacial tension on dynamic moduli of

the blend
Here we report model simulations of some emulsion parameters. We examine, essen-
tially, the effect of particle size and interfacial tension on dynamic moduli of the blend.
These two parameters are the more affected, when a blend is compatibilized. In the
model, these parameters, expressed as the ratio alR, are manipulated as though they were
independent variables. In fact, of course, changes in a must trigger corresponding varia-
tions in R, as will be noted later in this discussion. In order to illustrate this, theoretical
curves were constructed for a two phase system. The end viscosities of the Maxwell-like
phases were arbitrarily set constant and equal to 105 Pa s. The volume fraction of the
minor phase has been set at 20%. The effect of particle size on dynamic moduli of the
blend is shown in Fig. 7 (at constant interfacial tension a = 5 mN/m). It follows from the
curves in the figure that the magnitude of the low-frequency plateau decreases with
increasing particle size, whereas the opposite effect is noticed with regard to the width of
the plateau. The greater the particle size, the more extended is the plateau, and thus the
longer is the relaxation time of blend elasticity, as reflected by the shift of the terminal
zone to lower frequencies. For the smallest particle radius, no evidence of a secondary
plateau is seen. This gives useful insight into the effect of compatibilization on dynamic
moduli of the blend. In fact, a blend with small enough particle sizes can be considered
macroscopically as a "homogenous" system, for which no secondary plateau is expected.
However, varying the interfacial tension has the opposite effect. The actual behavior of
6
5
4
3
... 2
"".$
"~. 0
-1
G' ,
t
-2
-3
-4
Of 0.1
.oo
matrix
R = 10
R =
R =
5
2
pm
pm
pm
••
R = 1 pm
R 0.1 pm
-5
-6 -5 -4 -3 -2 -1 o 2
Log(ro In radii)
FIG. 7. Theoretical curves illustrating the effect of particle size (R) on dynamic shear moduli G'. G" for a
viscoelastic immiscible blend. The end viscosities of the two Maxwell-like phases were set arbitrarily at 105
Pa s. The interfacial tension was fixed at 5 mN/m.
the blend then is a result of the two effects, since, as noted, the constitutive equation
involves the ratio of the two parameters (aiR).
C. Comparison with experimental data

In this section, we examine the linear viscoelastic properties of unmodified and modi-
fied PSIPE blends, with reference to the preceding discussion. The calculation of G' and
G" of the blend from Eq. (3)-(5) requires knowledge of Grand G" of both phases at the
same frequencies. This can be obtained by fitting the dynamic moduli with the general-
ized Maxwell model:
G·"A~w2
I I
G'(w) =~
I +>-..fw2
and
GiAjW
G"(w) =L (8)
I +"Afw2'
where G, and Ai are the modulus and the relaxation time of the ith mode of the model.
The generalized Maxwell fits allow us also to extrapolate the dynamic moduli of the
homopolymers to low frequencies, as shown in Fig. 1.
Figure 8 compares the experimental G' and G" with predictions of the emulsion
model for PS/PE (70/30) at 200 "C. The blend morphology was characterized by scan-
ning electron microscopy (see Fig. 5), and the particle size distribution, given in Fig. 6,
was used for the calculations. The theoretical curves shown in Fig. 8(a) were obtained by
adjusting the value of a, so as to obtain the best agreement between experimental and
512 BOUSMINA ET AL.
4
.. 3
..
II.
.!!
~ 2
! 0 .
lJ G'
G"
.......,
BlndA.l G',G'· ... ... p.rtkle stze dlslrlhu1J1MI
G',G" rs G"G" witlll voI__ ."er......u••
G',G" E••"I•• mlMlel
2 345
Log(co In rid/I) LOI(ro In rlldll)
(II) (b)
FIG. 8. Comparison between the experimental data and the model predictions for PSIPE (70130) at 200 QC.
a = 5.2±O.2 rnN/m. (a) Model predictions using particle size distribution, given by the histogram of Fig. 6. (b)
Comparison between the effect of particle size distribution and that of volume-average radius (R = 10 1Jffi) on
dynamic shear moduli of blend A1, No effect of particle size distribution is noticed.
theoretical curves. The adjustment was particularly realized in the low-frequency range,
surrounding the secondary plateau, where the effect of interfacial tension is more sensi-
tive. Using this procedure, we obtained a value of 5.2:!::0.2 mN/m for the interfacial
tension. This is consistent with the value 4.7 mN/m given in the literature (Wu, 1982;
Elemans et al., 1990). The difference is due essentially to the error made when estimating
particle sizes from micrographs, required for the calculation of the interfacial tension. In
Fig, 8(b), we compare the predictions of the model obtained by using the particle size
distribution to that obtained by replacing the distribution by the volume-average radius,
which is about 10 JLm. Figure 8(b) clearly shows that there is no influence of particle size
distribution on the model predictions, over the whole frequency range, Figure 8 shows
the good agreement between model predictions and the dynamic moduli data. The model
predicts correctly the increase of blend elasticity, The low-frequency plateau in G' is
characteristic of a lengthy relaxation-time processes of about 40 s, much longer than the
terminal relaxation times of the individual phases (see Table 11). The long relaxation time
in the blend may be estimated from the relaxation-time spectrum, which is related to
experimental values of G' and G" by
+OO w2X2
G'(w) =
f-00
H("A) 22dln("A)
l+"Aw
(9)
and
+OO WA
G"(w) =
f-00
H("A) 2 2 d In("A).
I+Aw
H('A) can be calculated by several methods (Weese and Honerkamp, 1992; Baumgaertel
and Winter, 1989; Ninomiya and Ferry, 1959; Tschoegl, 1989). In this paper the relax-
ation spectra were calculated using the Ninomiya and Ferry approximations.
A more appropriate way to make evident the long relaxation-time process of the blend
is to plot the weighted relaxation spectrum 'l\H(X) as a function of log ("A) (Gramespacher
•.. PS matrix
Blend Al
6000
III
4500
III
Po
....t: 3000
r<
:z:
r< 1500
0
-5 -3 -j 1 3
Log(),. in s)
FIG. 9. Weighted relaxation-time spectrum for PS (matrix) and PSIPE (70/30) blend at 200 "C. The arrow
denotes the position of the relaxation time of the blend elasticity as calculated by the Palieme emulsion model,
Eq. (7).
and Meissner, 1992). This plot is given in Fig. 9 for the PS matrix and the PSIPE (70/30)
blend. As in the Cole-Cole plot for a two phase system, the weighted relaxation spectrum
for the blend exhibits two maxima, corresponding to short and long relaxation times. It is
worth noting that the short relaxation time coincides with that of the matrix, suggesting
that the rheological behavior of the blend in the high-frequency region is dominated by
the behavior of the matrix. In contrast, the peak corresponding to the long relaxation time
denotes the defonnability of particles under macroscopic strain and gives an experimental
estimation of the relaxation time of the blend elasticity. The estimate is about 40 s, which
is consistent with the value calculated from Eq. (7) of Palierne's emulsion model, and
represented in the figure by an arrow.
Figure 10 compares experimental data and theoretical predictions for blend A2, in
which the matrix is less viscous than the dispersed phase (k = TJlTJM = 59). As pre-
dicted, the secondary plateau does not appear, confirming that the pronounced elasticity
of the blend in the low-frequency region is linked to the defonnability of the suspended
droplets.
As mentioned before, the effect of blend modification on the rheological properties is
more evident for SEBS addition than for corona treatment. As shown in Fig. 11, 1 wt %
copolymer addition decreases the magnitude and increases the width of the elastic modu-
lus of the blend, in the frequency range of 0.0 I-I rad/s. The full lines in Fig. 11 are the
theoretical curves calculated from Eqs. (3)-(5), using the experimental G I and G" of the
phases. As noted for the unmodified blend, the particle size distribution has no effect on
the model predictions, both for SEBS and corona modified blends. From the histogram of
particle size distribution, a volume-average particle radius of 2 ~m was estimated for the
blend modified by 1 wt % SEBS addition. The interfacial tension was obtained from the
best fit of the theoretical curves to experimental data. This was found to be 1±O.3 mN/m,
thus 5 X smaller than the interfacial tension of the unmodified blend, 5.2± 0.2 mN/m. It is
interesting to point out that copolymer addition resulted in important variations of CI' and
R, but had no effect on the ratio a/ R (interfacial forces). This is about 5 X 102 N/m 2 for
both unmodified and copolymer modified PSIPE blends.
514 BOUSMINA ET AL.
6
0 G' IlleDd .u
5 l> G" Blnd.u

G',G" PE
G',G" E••••lo. ..odel
.
,.
4 , ,
,.
:oS 3
,,
, , ,
c. 2
.
,,
,,
,
~
r
, ,,
..l
, ,,
, ,,
0 , ,,
, ,,
-1
-3 -2 -1 0 2 3 4
Log(oo In raells)
FIG. 10. Comparison between the experimental data and the model predictions for PSIPE (30170) at 200 "C,
No secondary plateau is observed when the matrix is less viscous than the dispersed phase (7Jrl7JM = 59),
The same procedure has been used to estimate the interfacial tension for corona
modified blends (Fig. II). By fitting the model to the experimental data, a value of
3.5 :±:O.3 mN/m was obtained, slightly smaller than that of the unmodified blend, but
clearly much higher than that obtained for SEBS modified compounds. The difference
between the interfacial tension of the unmodified blend and that of the corona modified
blend is about 1.5 mN/m. This difference is small in absolute terms, but represents a
relative change of about 30%, which is significant on the scale of interfacial tensions for
immiscible polymer blends (typically 1-10 mN/m at 200 QC). The above results demon-
strate that SEBS addition is a more effective modifier of PSIPE blends than corona
treatment, and confirms statements made in our previous paper (Bousmina et al., 1994a).
7 •.
6
..
-< 5
...
llo
oS 4
b 3
C
-
J2 •
0
G'
G'
G" --_c_c
0
-4 -3 -2 -1 0
Log(m In nells)
l>
2
G"
C,G"
3
-
Eo......
4 5
FlG. 11, Comparison between the experimental data and the model predictions for PSIPE (70/30) modified by
corona treatment at 200 °C (blend B); by I wt % SEES addition (blend C),
The results of this work show that SEBS addition decreases both particle size and
interfacial tension. In contrast, corona treatment slightly decreases the interfacial tension
but has no effect on particle size. This result is in contradiction with the discussion in
Sec. III concerning the effect of particle size and that of interfacial tension on dynamic
moduli of the blend. The difficulty may be rationalized by analysis of the capillary
number, Ca = TJMyRla. This is applicable to the melt blending of multiphase systems,
and expresses an equilibrium between the viscous forces (TJMY) and interfacial forces
(aIR). Under identical conditions of mixing (constant Ca, which is the case in our
experiments), at constant viscosity (TJM) of the matrix, and at constant shear rate (y), a
decrease or rise in a should result in a similar change in R. However, this was not
observed in blends made from corona treated PS and PE. As mentioned previously (Sec.
Il B), XPS analysis revealed significant modifications on the surface of PS and PE, due to
corona treatment. These involved particularly a decrease in the concentration of C-C
bonds, due to polymer chain scission, leading to a decrease of blend components viscosi-
ties. This may be seen in Fig. 4. The decrease of viscosity is more evident for PS than for
PE. In terms of the capillary number, the decrease of PS (matrix) viscosity leads to a
decrease in interfacial tension, without requiring a decrease in the particle size (R).
V. CONCLUDING REMARKS
Linear viscoelastic properties of molten immiscible polymer blends are characterized
by an increase in the low-frequency elastic modulus and by a long relaxation-time pro-
cess. Oscillatory shear measurements on molten PS/PE blends. at two viscosity ratios
(k = 0.017 and k = 59), revealed that the increase in blend elasticity and the longer
relaxation time observed in the low-frequency range arise from the defonnability of the
suspended droplets. The increase of elastic modulus, at low frequencies, was observed
only when the dispersed phase was less viscous than the matrix. This behavior was
analyzed quantitatively by using the Palieme emulsion model.
The low-frequency plateau characteristics were used to compare the compatibilization
effect of corona treatment and SEBS copolymer modification. The emulsion model was
used to determine the interfacial tension in unmodified and modified PS/PE blends. A 1
wt % SEBS addition resulted in an important decrease of both interfacial tension (a) and
particle size (R), whereas corona treatment slightly decreased the interfacial tension. but
had no effect on particle size. This unexpected result could be rationalized in terms of the
equilibrium capillary number, which calls for a direct variation of R and a. In the case of
corona treated PS/PE blends, however, the decrease of a was not accompanied by a
decrease of R. This was attributed to a decrease of the matrix viscosity ( TJ M), as a result
of polymer chain scission. as confirmed by XPS analysis.
We conclude by noting a particularly interesting aspect of the corona route to surface
modification: it appears unique in its ability to affect the interfacial tension without
necessitating an accompagning modification in the particle size of the dispersed phase. It
is therefore possible to discriminate between the effect of interfacial tension and particle
size on the rheological properties of immiscible polymer blends.
ACKNOWLEDGMENTS
Portions of this work were supported by Strategic and Operating grants received from
the N.S.E.R.C. Additional funding was received from the Fonds pour la Formation de
Chercheurs et l' Aide a la Recherche (Quebec Ministry of Education).
516 BOUSMINA ET AL.
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Comparing The Effect of Corona Treatment and Block Copolymer Addition On Rheological Properties of Polystyrene

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Comparing The Effect of Corona Treatment and Block Copolymer Addition On Rheological Properties of Polystyrene

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Comparing the effect of corona treatment and block copolymer addition on

rheological properties of polystyrene/polyethylene blends

Citation: J. Rheol. 39, 499 (1995); doi: 10.1122/1.550709

Additional information on J. Rheol.

M. Bousmina, a) P. Bataille, S. Sapieha, and H. P. Schreiber

Department of Chemical Engineering, Ecole Polytechnique, P.0. Box

(Received 26 April 1994; accepted 14 December 1994)

© 1995 by The Society of Rheology, Inc.

System Series Description

PSIPE (70/30) Al Control blend

150 2.08 0.58 2.12 0.51

TABLE III. Rheological characteristics of the samples in the terminal

Zero-shear viscosity Terminal relaxation time

PS 1.3 X 104 7.4XIO- 2

no effect, to an increase as well as to a decrease of melt viscosity of the blends, when a

of polymer blends is generally characterized by pronounced elastic properties and a long

4(alR j)[2G,t(w) + 5Gj(w)]+[Gj(w)-G,t(w)][16G,t(w)+ 19Gj(w)]

The constants C j are given by the following expressions:

Equations (3)-(5) can be summarized by the following expression:

G~ ,G~ = f( G~ ,G~ ,G; ,G; ,R,a,f/J). (6)

B. Influence of particle size and interfacial tension on dynamic moduli of

C. Comparison with experimental data

5 l> G" Blnd.u

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