"Development of Extrusion Instabilities and Surface

Irregularities of Extrudates of Polymer Melts and Filled

Polymers"

Dilhan M. Kalyon, Elvan Birinci and Halil Gevgilili

Highly Filled Materials Institute

Stevens Institute of Technology

Castle Point Station, Hoboken, NJ 07030

* dkalyon@stevens-tech.edu, 201 216 8225

Synopsis
This study is a continuation of an earlier study [Kalyon and Gevgilili (2003)] and aims at

probing the effects of the flow boundary condition at the wall on the development of flow

instabilities and extrudate surface irregularities upon the extrusion of polymer melts and

polymeric suspensions. The wall slip and flow instability behavior of two polymers, i.e.,

a poly (dimethyl siloxane), PDMS and an oxetane based alternating block thermo plastic

elastomer BAMO/AMMO-TPE were studied along with the wall slip and flow instability

behavior of PDMS filled with 10, 20, 40% by volume of hollow glass spheres and 60%

by volume of KC1 Filled BAMO/AMMO- TPE. Steady torsional flow was used in

conjunction with the straight-line marker technique to analyze wall slip in steady

torsional flow. Thermal imaging and high-speed cinematography were used with

capillary flow to characterize the surface features of extrudates emerging from capillary

dies. The effects of the convergence angle from the reservoir into the capillary die were

also investigated (15, 45 and 75 °) for pure PDMS and 10% glass filled PDMS. The angle

of convergence had no effect on the development of surface irregularities. The

incorporation of the glass filler into the PDMS binder gave rise to a reduction of the shear

rate range over which gross surface irregularities are observed. Furthermore, the

extrudates of PDMS with 40% glass filler were largely free from surface irregularities.

On the other hand, BAMO/AMMO elastomer melt, which exhibits stable stick over

relatively high strains and shear rates in steady torsional flow does not exhibit surface

irregularities in the same shear rate range in capillary flow [Kalyon and Gevgilili (2003)].

However, the incorporation of rigid particles into the BAMO/AMMO elastomer gives
rise to flow instabilities and surface irregularities during extrusion. These results suggest

that the mechanisms for the development of surface irregularities of the extrudates of

polymeric suspensions differ from those of the binder phase. Depending on the binder of

the suspension and with the appropriate type and concentration of the rigid filler phase,

the incorporation of the rigid fillers can prevent or induce the formation of surface

irregularities in extrudates of polymeric suspensions.

Key words" flow instabilities, wall slip, extrudate, and surface irregularities
INTRODUCTION

The development of surface distortions in the extrudates of polymer melts emerging from

extrusion dies (described as melt fracture, shark skin, gross surface irregularities) is an

important industrial problem. The initiation on extrudate distortions presents an upper

limit to the manufacturing rate in extrusion based processing of polymers and polymeric

suspensions. Consistent with its industrial importance it has received significant

academic and industrial attention [Benbow and Lamb (1963); Petrie and Denn (1976);

Larson (1992); Denn (2001); Kalyon and Gevgilili (2003)].

Various polymer melts, especially linear polymers, exhibit wall slip [Awati et al. (2000);

Hatzikiriakos and Dealy (1991); Gevgilili and Kalyon (2001); Rielly and Price (1961);

Kalika and Denn (1987); Ramamurthy (1986); Chen et al. (1993); Migler et al. (1993);

Mi.instedt et al. (2000)] and wall slip is considered to be one of the major factors which

can affect the formation of extrudate distortions. Kissi and Piau (1990) carried out flow

visualization experiments with PDMS using transparent dies with tracer particles and

were able to document wall slip in the 0.05-0.07 MPa shear stress range. Benbow and

Lamb (1963) used a similar experimental technique and determined a critical shear stress

of 0.07 MPa for the onset of wall slip for PDMS.

The data presented in the literature indicate that there may be multiple mechanisms for

the wall slip of polymers to allow the differentiation of two regimes in the wall slip

velocity versus the shear stress (or shear rate) behavior. For example, with PDMS Migler
et al (1993) have determined a sharp transition between a regime of weak slip and one of

strong slip as the shear rate is increased during simple shear in which the velocity

distribution is directly measured within the 100 nm of the wall. The transition from weak

to strong slip in simple shear is considered to occur at a material-dependent wall shear

stress, value of which depends on the surface density of surface-anchored chains (Leger,

Hervet and Massey, 1997). Here in this paper wall slip is taken to be synonymous with

slip which can be detected with macroscopic means, i.e., through the dependence of the

flow curves on the surface to volume ratio of the rheometer (Mooney method) [Mooney

(1931); Yilmazer and Kalyon (1989); Kalyon et al. (1999)] or through the detection of

mm-scale discontinuities at the free surface of the melt and the edges of the fixtures used

in steady torsional flow upon following a marker line [Kalyon et al. (1993); Aral and

Kalyon (1994)].

Recently, Kalyon and Gevgilili (2003) have focused on the wall slip and flow instability

behavior of three polymers, two of which exhibit easily detectable wall slip in simple

shear flow and one that does not. The polymers included a high density polyethylene

(Exxon-Mobil HAD 601, a PDMS (GE Silicones-SE-30) and an oxetane-based

alternating block copolymer, BAMO/AMMO, with hard blocks consisting of [3, 3-bis

(azidomethyl) oxetane, BAMO] and with soft blocks of (3-azidometyl-3-metyloxetane,

AMMO) from ATK Thiokol of Promontory, Utah. The same PDMS and the

BAMO/AMMO are used in this study also. However, in this study these polymers were

filled with rigid fillers to allow the investigation of the effect of the incorporation of rigid

filler particles to the development of extrudate surface irregularities. For PDMS the filler
consisted of spherical hollow glass particles with a specific gravity of 1.09 and an

arithmetic mean particle diameter of 12 ~tm (Potters Industry). For BAMO/AMMO a KC1

filler with approximately cubical particle shape was used.

Experimental Apparati and Procedures

An Advanced Rheometric Expansion System (ARES) rheometer, from Rheometric

Scientific, Inc., Piscataway, NJ, was utilized in conjunction with steady torsional flow

using cone-and-plate and parallel-disk configurations. The environmental chamber was

equipped with an imaging window and auxiliary optics for continuous monitoring of the

free surface of the specimen [Aral and Kalyon (1994); Gevgilili and Kalyon (2001)] A

high-speed camera, capable of recording at filming speeds as high as 2,000 frames per

second, was part of the set-up shown in Figure 1.

During steady torsional flow a straight-line marker was placed on the edges of the

cone/plate and the free surface of the polymer melt to enable the characterization of the

wall slip velocity and the true deformation rate [Kalyon et al. (1993), Aral and Kalyon

(1994); Gevgilili and Kalyon (2001)]. The discontinuities that develop between the

surface of the plates of the rheometer and the bulk of the melt suggest the initiation of

wall slip (Figure 2). The steady wall slip velocity values determined using the straight-

line marker technique agree well with the steady wall slip velocity values determined

upon the analysis of the dependence of the shear stress on the surface to volume ratio of

the rheometer, i.e., the conventional Mooney technique [Kalyon et al. (1993)]. The steady

torsional flow behavior of the three resins was characterized at various shear rates and
temperatures to determine the conditions under which the catastrophic failure of the no-

slip condition became apparent.

An Instron capillary rheometer was employed to collect additional shear viscosity data

and to study the development of extrudate distortions upon exit from the die. The

diameters, length over the diameter ratios and the converging angle of the taper

connecting the reservoir of the barrel of the rheometer to the straight land section of the

capillary die (Figure 3) were changed systematically. The shapes of the extruded samples,

immediately upon extrusion from the die, were captured using a high-speed camera

(Figure 4) to allow the immediate characterization of the surfaces of the extrudates

(Figure 5). The temperature distributions of the extrudates emerging from the die were

also monitored using a ThermaCam thermal imaging camera. A typical image showing

the temperature distribution on an extrudate upon emerging from the die is shown in

Figure 4 to reflect the temperature of the material at the die wall. The temperature of the

material immediately upon exit provided data on the effect of viscous energy dissipation

and allowed the determination of the true temperature of the melt (Figure 6).

RESULTS AND DISCUSSION

U n f i l l e d p o ly m ers :

The steady torsional flow behavior of poly(dimethylsiloxane) (PDMS) was characterized

at 10, 30 and 50°C. Fig. 7 shows the results of shear stress growth experiments performed

at various shear rates at 30°C using the cone-and-plate fixtures. At relatively small shear

rates, i.e., less than 1 S-1, the shear stress grows monotonically as a function of time until
steady state values are reached. In this relatively small shear rate range the shear stress

curves are approximately parallel to each other and do not exhibit overshoots. The typical

results of the straight-line marker technique corresponding to this set of experiments are

shown in Fig. 7. At relatively small shear rates the straight-line marker remains

continuous and connects the moving and stationary walls. On the other hand, at the

higher shear rates, for example, at 40 s -1 the continuity of the straight-line marker is lost

during steady torsional flow. The formation of the mm-scale discontinuity at the wall is

indicative of the loss of the wall stick condition at the wall "macroscopic wall slip". On

the other hand, at greater shear rates the occurrence of wall slip and the eventual ejection

of the specimen from the gap force the shear stress to decrease upon reaching maxima.

For PDMS the shear stress maximum at which wall slip is initiated occurs around 0.07

MPa at 30°C at a shear rate of 40 s -~. This critical shear stress value was determined to be

the same at 10 and 50 °C also [Kalyon and Gevgilili (2003)].

The capillary flow curve of PDMS at 30°C is shown in Figure 8. At apparent shear rates

of 19 s -~ and lower, the extrudates of PDMS did not exhibit any type of surface or bulk

distortions. As the shear rate is increased to 25 s -1 distortions of the extrudate surface in

the form of fine sharkskin were observed (Fig. 8). At 38 s -1, thread-like sharkskin forms

at a wall shear stress of 0.067 MPa. At 50 s -~ and the corresponding wall shear stress of

0.08 MPa, the sharkskin loses its uniformly repeating thread-like structure and becomes

more non-uniform. Thus, one observes a dramatic change in the surface topology of the

extrudate in approximately the same mean wall shear stress range at which wall slip

becomes apparent in steady torsional flow. Is this behavior dependent on the surface to
volume ratio of the capillary die? Data collected at three different capillary die diameters

are shown in Figure 9. The flow curves and the surface topologies of the extrudates are

found not to be affected by the surface to volume ratio of the die. Thus, regardless of the

diameter of the die, the wall shear stress at which the transition to the unstable region (at

which the extrudate surface is no longer smooth) coincides with the critical shear stress

range at which wall slip is onset under steady torsional flow.

Is the flow instability behavior of the polymer melt affected by the convergence angle of

the capillary die entrance? The effect of the convergence angle for PDMS is shown in

Figure 10. This typical behavior indicates that the flow curves and the development of the

surface irregularities are not affected by the convergence angle.

The steady torsional flow behavior of the TPE (over a very broad range of shear rates up

to 200 s~) was very different than PDMS. Even at the highest shear rates investigated the

samples of TPE stayed intact within the gap, without any sign of wall slip, edge distortion

and outward ejection for strains as high as 50. For TPE the straight-line marker was

observed to retain its continuity even after one whole revolution of the moving surface

[Kalyon and Gevgilili (2003)]. The thermoplastic elastomer thus appears to exhibit little

affinity to slip at the wall and behaves very differently than PDMS. This significant

difference can possibly be attributed to the strong electrostatic interaction between the

azido groups of the thermoplastic elastomer and the metal surface as revealed using

force-field calculations (U. Olgun, private communication, 2002). During capillary flow
the extrudates of the TPE were relatively smooth and exhibited only non-periodic minor

surface blemishes regardless of the shear rate.

The general trend in the development of flow instabilities during extrusion of polymer

melts involves the absence of extrudate surface distortions at relatively low shear

rate/stress values (at which presumably the wall slip velocity is negligible) on one hand

and at relatively very high shear rate/stress values at which correspondingly high (and

presumably stable) wall slip velocities exist. This suggests that extrudate distortions are

less likely to occur under conditions in which a stable flow boundary condition exists at

the wall; whether it is either a stable wall stick or stable wall slip condition.

Filled Polymers:

PDMS and TPE were compounded with glass spheres and KC1, respectively. From earlier

studies it is known that in the presence of the particles an apparent slip layer (the Vand

layer) forms at the wall during both steady torsional and capillary flows [Yilmazer and

Kalyon (1989); Kalyon et al. (1993)]. The formation of the apparent slip layer is the

dominant mechanism for wall slip of suspensions with rigid particles [Aral and Kalyon

(1994)].

The incorporation of the KC1 particles into BAMO/AMMO TPE gives rise to the

development of flow instabilities at shear stress values, which surpass 0.3 Mpa (Figure

11). This is an interesting finding and suggests that the presence of particles can render

the flow unstable for a polymeric binder, which only exhibits stable flow over the same

10
apparent shear rate range. Since the BAMA/AMMO TPE is energetic it was not possible

to make additional supporting measurements, so our attention was turned to PDMS

compounded with differing concentrations of spherical glass particles. How will the

behavior of PDMS be affected by the presence of rigid particles in the 10 to 40% by

volume range?

The typical flow curves of PDMS incorporated with 10% by volume glass collected with

three capillaries with the same length over diameter ratio of 40 but with differing

diameters are shown in Figure 12. The images pertain to extrudates extruded at

approximately the same apparent shear rate of about 30 to 50 s -~. Thus, at the same

apparent shear rate all of the extrudates extruded with capillary dies with differing

diameters exhibit a similar type of surface irregularities.

Figure 13 shows all of the points on the flow curves at which extrudate surface

irregularities were observed (as indicated by the presence of arrows here.) Thus, the

points marked with arrows indicate that surface irregularities occur at those points of the

flow curves and the absence of an arrow for a point indicates that there were no extrudate

surface irregularities evident at that shear rate.

The data indicate that extrudates free of surface or bulk distortions could be obtained

either at the low apparent shear rates (less than 10 S-1) or at the relatively high shear rates

(over 1000 s-~). In the wall shear stress range of 0.07 to 0.1 MPa the extrudates exhibited

surface irregularities. In the relatively high shear rate regime, smaller shear stress values

11
are generated for the capillaries with smaller diameters at constant length over the

diameter ratio, suggesting that the suspension is slipping strongly. The flattening of the

flow curves at the highest apparent shear rates at which wall slip is clearly observed is

also interesting. Such flattening is generally associated with plug flow of the suspension

[Kalyon et al. (1993); Yaras et al. (1994)].

The wall slip behavior of the suspensions of PDMS with 10, 20 and 40% by volume glass

particles were investigated using steady torsional flow. Generally, there was widespread

wall slip of the suspension samples. Earlier experimental evidence suggests that the flow

instabilities and extrudate distortions occur under conditions in which the stability of the

flow boundary condition at the wall is perturbed [Atwood and Schowalter (1989)].

Distortion-free extrudates are obtained when a stable wall slip condition, for example

through the generation of an apparent slip layer at the wall by coating of the wall surfaces

with fluoroelastomers, is introduced [Kissi and Piau (1997) and Wang and Drda (1997)].

One can surmise that an apparent wall slip mechanism is also introduced upon the

incorporation of the rigid particles into PDMS, to be superimposed on the wall slip of the

PDMS itself. The incorporation of the particles broadens the shear rate range over which

flow stabilities occur but at the same time generates smooth extrudates at the highest

apparent shear rates.

The effect of the convergence angle of the entry region of the flow geometry to the

development of the surface irregularities of the extrudates of suspensions of PDMS with

10% rigid glass filler particles is shown in Figure 14. Similar to the behavior of pure

12
PDMS the angle of convergence values between 15 to 75 ° do not affect the development

of the extrudate distortions, suggesting that the source of the observed flow instabilities

for both the pure PDMS and filled PDMS is not likely to be related to the dynamics of the

entry flow.

The flow curves obtained for the suspension of PDMS with 20% by volume glass are

shown in Figure 15. The arrows are used again to indicate that distorted extrudates are

extruded under that particular condition and the absence of an arrow over a given point

suggests that the extrudate was smooth and free of distortions. In comparison to 10%

suspension the range of shear rates over which flow instabilities are observed is

considerably reduced at 20% by volume glass (between 100 to 1000 s-1) with no

extrudate distortions observed below an apparent shear rate of 100 s-~, regardless of the

diameter of the capillary die.

The flow curves of the 40% by volume glass spheres incorporated PDMS are shown in

Figure 16. Except for one flow condition involving an apparent shear rate of 72 s -~

collected at the highest capillary diameter of 0.1378" (3.5 mm), all of the extrudates were

smooth and were free of distortions. The elimination of the surface irregularities over the

same apparent shear rate upon increasing the concentration of the particles from 20 to 40

is counter to conventional thinking. The incorporation of the particles increases the

apparent shear viscosity of the material thus increasing the shear stress at the wall and

hence is expected to give rise to conditions at which extrudate distortions would occur

more readily. However, the opposite occurs here with the extent of extrudate distortions

13
decreasing or being eliminated completely with increasing concentration of rigid

particles.

The occurrence of wall slip is clearly surmised by comparing the data collected at

different diameters (at constant length over the diameter ratio). As the diameter increases

(hence a decrease of the surface to volume ratio) the wall shear stress increases

suggesting that there is significant wall slip, with the slip velocity increasing with

increasing wall shear stress. This is consistent with our findings from steady torsional

flow that suggest that wall slip prevails over a broader range of shear rates as the particle

concentration increases. Again the flattening of the flow curves is a precursor of plug

flow, which renders the application of Mooney's approach for the determination of the

wall slip velocities irrelevant [Mooney (1939); Yaras et al. (1994); Kalyon (2003)].

The comparisons of the behavior of the effects of incorporation of the rigid particles into

the polymer matrix are more clearly seen in Figures 17-19, which show the flow curves

of the 10, 20 and 40 % by volume particle incorporated suspensions at each capillary

diameter. The arrows again indicate that extrudate distortions occur at that point. The

data suggest that although the wall shear stress increases with increasing particle

concentration the range of apparent shear rates, over which flow instabilities and

extrudate distortions prevail, decrease with increasing particle concentration.

Conclusions: This study suggests that the flow instabilities observed with a polymeric

binder can be eliminated upon the incorporation of particles (with the fight concentration

14
and characteristics) into the binder phase. This is an important finding and can be

exploited to our industrial advantage. Conversely, if the extrudates of the binder phase

are smooth and distortion flee, the incorporation of rigid particles can introduce extrudate

distortions. This is another important finding and should be kept in mind especially when

polymeric compounds are formulated to include various solid ingredients. These results

attest to the intimate relationship between the wall slip of polymers and polymeric

suspensions and the development of surface irregularities in their extrudates.

Understanding of the factors that control the stability of the flow boundary condition at

the wall can provide a better understanding to the underlying mechanisms of the

development of extrudate distortions.

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17
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18
 Computer interface for rheometer
and high speed Camera
Force Rebalance +
Transducer

Environmental High Speed Camera

controller 500-2000 fps

Actuator
Motor

Figure 1
A discontinuity in the straight-line marker indicates loss of no-slip
boundary condition at the polymer melt-metal interface
Figure 2
 "- D=0.375"

•,--
.- 4 5 O a n g 1e
................ i" - ' -

r D
L

" i

.... ~ ......... iI

The angle of convergence was varied between 15, 45 and 75 degrees.

Figure 3
Thermal Imaging
Camera .

High Speed Camera

Figure 4
 PDMS
45deg d-0.096 L/D-40 Crosshead Speed: 2in/min

0.375 in

F igure 5
190

Tbarrel= 180oC
180 er=0.03" L/D=66

170
Discharge of the die - ~
160 -

150 -

140

130

120 Cross-Head speed:0.5"/min,

7=467.3 s -1, Tmax: 182.5°C
110 -

100 I I I I I

5 10 15 20 25 30

Position (Pixels)

Figure 6
 100000
=40
"-3.0 S "1 = 1 0 s -1 -- '~' - - 5 S -1
: ' ~ = 2 s -1

10000

r~
r~

1000

100

10
0.01 0.1 10

Time, s

F igure 7
100,000

0 Capillary Rheometer

A Steady Torsional Flow

/o/ 0 0
0

"X'•Wavy
racture
<)

0
/ Sharkskin

0
10,000

1,000
0.1 1 10 100 1000

Shear Rate, S-I

PDMS in capillary flow, development of surface irregularities

F igure 8
 1000000
A D=0.0984" L/D=40
X D=0.0591" L/D=40
* D=0.0328" L/D=40

~a=0.078 MPa

100000 - X
r,~ i>

= -- Ir

A
<
I

, ;tli~'~ #

10000 1 i i I I i l I I i I I I I I I t I I i I I I l t I I

1 10 100 1000 10000

Apparent Shear Rate, s

PDMS" development of extrudate surface irregularities
Figure 9
As a function of capillary surface/volume ratio
 1.E+06

• D-0.0591 15 degrees
(~- 45 °
LxD=0.0591 45 degrees 7 = 45S'1
x D=0.0591 75 degrees

4P~

raO
raO

A
3
1.E+05

0~- 75 °
.4,,,a
g 7 = 45S'1
0~- 15 ° A
~D
7 = 45S'1

<

1 .E+04 ! | i i i i i i I = i i ! ~ i I | ! t i J

10 100 1000

-1
Apparent Shear Rate, s
Pure PDMS :Apparent Shear Stress vs. Apparent Shear Rate Behavior:
Comparison of Different Converging Entry Angles
Figure 10
 1,000,000

o,,
Ih
0

0
<
100,000

I I I I I I l I I I I I I I I I I I I I I
10,000
0.01 0.10 1.00 10.00

-1
C O R R E C T E D S H E A R RATE, s

KCI filled BAMO/AMMO TPE Figure 11

 D=0.0591
1 .E+06
4 5 s -~

O
.,i,-a
D=0.098
? - 40s-~
O X •
1 .E+05 x~) • •
c~ .
O •
O xo
O
O O D=0.0328
t::
o 7- 53 s -1
• D=0.0328 L/D=40

x D=0.05 91 L/D=40

O D=0.0984 L/D=40

1 .E+04 , | , i i , , , I v i i , , i i | i

10 100 1000 10000

Apparent Shear Rate, s -1

PDMS + Hallow Sphere Glass Particles

Figure 12
( 10% by vol.) Mixture
 1 .E+06

I D = 0 . 0 3 2 8 L/D-=40

X D=0.0591 L/D=40

¢ D=0.0984 L/D=40 D-0.0591in

r.~
D=0.09841in At 45, 90, 1-81 s-1
At 10, 19, 39, 98 s-1

1 .E+05 x • •
I I
rae~

.4,.,a
¢ D=0.0328in
~D
t:z
O
At 27, 53, 106, 265, 531 s-1

1 .E+04
1 10 100 1000 10000

Apparent Shear Rate, s-

PDMS + Glass Sphere(10% by vol.) Mixture

Corrected Shear Stress vs. Apparent Shear Rate Behavior
Comparison of Different Diameters Figure 13
 1.E+06

• D=0.0591 15 degree (~- 75 °

ix D=0.0591 45 degree
x D=0.0591 75 degree

tt 0~- 15 °
(D
xZ 1.E+05 i t
r~
];

o
I:: = 45 °
O

1 .E+04
10 100 1000

Apparent Shear Rate, s

PDMS + Glass Sphere(10% by vol.) Mixture
Apparent Shear Stress vs. Apparent Shear Rate Behavior
Comparison of Different Convergence Angles
Figure 14
 1 .E+06

• D=0.0328 L/D=40
x D=0.0591 L/D=40
LxD=0.0984 L/D=40
rae~
D - 0.0591 in
.4-a
c~ 90, 181,454 s-1
D= 0.0984 in
No irregularity
1 .E+05
o

A
)lftX
• T
D - 0.0328 in
A
265,531, 1062 s-1
O

1 .E+04 , | , , , i i i I i i i i i i i ; I , i i i i i ! , J i | , i i i i

1 10 1 O0 1000 10000

-1
Apparent Shear Rate ,S
PDMS + Glass Sphere(20% by vol.) Mixture
Corrected Shear Stress vs. Apparent Shear Rate Behavior
Comparison of Different Diameters
Figure 15
 1 .E+06 . . . . . . . .

• D-0.0328 L/D=40
o D-0.0591 L/D=40
- D=0.0984 L/D=40
x D = 0 . 1 3 78 L / D = 4 0 D - 0.1378in
At 72 s-1

.4-a
X
x
x~ • ~ o •
~D 1.E+05 - "-El
X 131. -- •
O
oe]

O
~D
tZ
O

1 .E+04

0 1 10 100 1000

Apparent Shear Rate, s-

PDMS + Glass Sphere(40% by vol.) Mixture

Corrected Shear Stress vs. Apparent Shear Rate Behavior
Comparison of Different Diameters Figure 16
 1 .E+06

x 10% D=0.0328 L/D=40

o 40% D=0.0328 L/D=40
o 20% D=0.0328 L/D=40
r/l
ra0

At 40% there is no irregularity

rae~
0
0
0 0 0
1.E+05

At 20% D= 0.0328in
o 10% D=0.0328in At 2 6 5 , 5 3 1 , 1062 s-1
At 26, 5 3 , 1 0 6 , 265, 531 s-1
O

1 .E+04 i l l i i l i 1 | , , , , l l i i , , I
,
i i i i | i i i i , , l | ,

10 1O0 1000 10000

Apparent Shear Rate, s-

PDMS + Glass Sphere Mixture
Corrected Shear Stress vs. Apparent Shear Rate Behavior
Comparison of Different Loaded Material Figure 17
1.E+06 . . . .

x 10% D-0.0591 L/D-40

o 20% D=0.0591 L/D=40
n 40% D-0.0591 L/D=40

At 40% there is no irregularity

o
0
0 0
0

/
1 .E+05
0
0 X
X
D=0.0591 in
20% At 90, 181,454 s-1
D-0.0591in
10% At 45, 90, 181 s-1

1. E + 0 4 t i i l l l i i I i i i i , i , , I i ,

1 10 100 1000

Apparent Shear Rate, s-1

PDMS + Glass Sphere Mixture
Apparent Shear Stress vs. Apparent Shear Rate Behavior
Comparison of Different Loaded Material
Figure 18
 1 .E+06

:,: 10% D-0.0984 L/D-40

zx 20% D=0.0984 L/D=40
D 40% D=0.0984 L/D=40

D= 0.0984 in
40% no irregularity
D D

D O D
1 .E+05
A
E! A X
A
D
A
e,..) X
~D A D= 0.0984 in
t:z
O D - 0.09 84 in
20% no irregularity
10% At 10, 19, 39, 98 s-1

1 .E+04 i i s ~ i i i i I i i | ! , , , , I i | | l l , i i

10 100 1000

Apparent Shear Rate, s-

PDMS + Glass Sphere Mixture
Apparent Shear Stress vs. Apparent Shear Rate Behavior
Comparison of Different Loaded Material
Figure 19