Biodegradable Polymers: Wall Slip, Melt Fracture, and

Processing Aids
Norhayani Othman1, 3, a), Nazbanoo Noroozi1, b), Bashar Jazrawi1, c),
Parisa Mehrkhodavandi2, d), Laurel Schafer2, e) and Savvas George Hatzikiriakos1,f)
1

Department of Chemical and Biological Engineering, The University of British Columbia, Vancouver, BC, Canada
2
Department of Chemistry, The University of British Columbia, Vancouver, BC, Canada
3
Faculty of Chemical Engineering, Universiti Teknologi Malaysia, Skudai 81310, Johor Bahru Malaysia
a)

norhayani@cheme.utm.my
nazbanoo.noroozi@gmail.com
c)
bashajs@hotmail.com
d)
mehr@chem.ubc.ca
e)
schaferl@mail.ubc.ca
f)
Corresponding author: savvas.hatzi@ubc.ca
b)

Abstract. The wall slip and melt fracture behaviour of several commercial polylactides (PLAs) and poly(-caprolactone),
(PCLs) have been investigated. PLAs with molecular weights greater than a certain value were found to slip, with the slip
velocity to increase with decrease of molecular weight consistent with wall slip data reported in the literature for other
systems. The onset of melt fracture for the high molecular weight PLAs was found to occur at about 0.2 to 0.3 MPa,
depending on the geometrical characteristics of the dies and independent of temperature. Similarly, sharkskin and gross
melt fracture was observed for the case of PCLs depending on the molecular characteristics of the resins and the
geometrical details of the capillary dies. It was also found that the addition of a small amount of PCL (typically 0.5 wt.%)
into the PLA and vice versa is effective in eliminating and delaying the onset of melt fracture to higher shear rates in the
capillary extrusion of PLA and PCL respectively. This is due to significant interfacial slip that occurs in the presence of
PCL or PLA as well as to the immiscibility of the PLA/PCL blend system at all compositions.

INTRODUCTION
Biodegradable polymers such as polylactide (PLA), and poly(-caprolectone) (PCL) have attracted an increasing
amount of attention over the last decades, due to environmental concerns [1, 2]. Their rheology has been extensively
studied in the literature, i.e. for PLAs see references [3-7] and for PCLs see references [8-12].
While the rheology of PLAs and PCLs has been well documented in the literature, their processing as can be
assessed by melt fracture phenomena [13-16] has not been studied with the exception of a few recent publications
[12, 17, 18]. During extrusion and when the wall shear stress exceeds a certain value, molten polymers exhibit
certain flow instabilities collectively known as melt fracture (surface distortions on extrudates). These can be small
amplitude periodic distortions known as sharkskin melt fracture [13, 14, 16, 19] alternate distorted and relative
smooth portions, known as stick-slip or oscillating melt fracture [15, 20] and gross irregular distortions known as
gross melt fracture [21].
In order to overcome these difficulties and to render the processes economically feasible, polymer processing
aids (PPAs) are frequently used. PPAs can eliminate the flow instabilities known as sharkskin melt fracture and
stick-slip, or postpone them to higher flow rates. The end result is an increase of the productivity as well as an
energy cost reduction, while high product quality is maintained [22-29].

Novel Trends in Rheology VI

AIP Conf. Proc. 1662, 030002-1030002-11; doi: 10.1063/1.4918877
2015 AIP Publishing LLC 978-0-7354-1306-1/$30.00

030002-1

The main objective of this paper is to examine first the wall slip behavior of PLAs and PCLs in capillary flow. A
second objective of this work is to study the melt fracture phenomena occurring in the extrusion of PLAs and PCLs
and finally identify appropriate processing aids that can enhance their processability. The geometric factors of the
dies that play a role in the effectiveness and the time required (induction time) to eliminate melt fracture phenomena
are also examined. Finally, the mechanisms by which the identified processing aids work effectively will also be
discussed.

MATERIALS AND METHODS

Four commercial PLAs studied in this work all obtained from NatureWorks LLC. In addition two commercial
PCLs obtained from Perstorp (Capa technology). These commercial samples have different molecular weights and
about the same polydispersity (Tab. 1).
Table 1. Molecular characteristics and other properties of the PLAs and PCLs used in this work.
Mw/Mn
Tg (C)
Tm (C)
0 (Pa.s) at 160C
Sample
Mw (kg.mol-1)

PLA7001D
PLA2002D
PLA3051D
PLA3251D
PCL6800
PCL6500

110.1
106.9
92.5
55.4
88.4
55.5

1.59
1.82
1.82
1.62
1.22
1.22

57.1
56.5
55.0
58.8
-60
-60

149.0
152.4
150.0
167.9
55
55.4

21,000
17,200
6,372
1,000
3,163
508.4

Samples in the form of pellets were dried overnight using a vacuum oven at around 70oC for use in preparing
samples for capillary rheometry. The processability and shear viscosity at high apparent shear rates were studied by
using a pressure driven Instron capillary rheometer equipped with a barrel having a diameter of 0.9525 cm. A series
of dies having a fixed diameter of 0.76 mm and various length-to-diameter ratios were used to correct for the entry
effects and assess the effect of pressure on viscosity. Two additional series of dies having different diameters of 0.43
mm and 1.22 mm and constant L/D ratios were used to detect slip effects through the Mooney analysis [13-14]. All
dies had an entry angle of 180. These are summarized in Tab. 2 along with their characteristic dimensions. The
Bagley and Rabinowitsch corrections were applied to the data to obtain the true viscosity of the samples in order to
compare them with viscosity data from the parallel plate rheometer. The extrudates from the capillary extrusion
experiments were inspected by Olympus MIC-D microscope to detect any visual defects known as melt fracture
phenomena [13-15].
Table 2. Characteristic dimensions of capillary dies used.
Diameter(mm)
Entry angle (o)
L/D

0.43
0.76
0.76
0.76
0.76
1.22

16
1.8
5.3
16
33
16

180
180
180
180
180
180

Wall Slip
The Mooney technique has been used here to determine the wall slip for all PLAs. Figure 1 shows the Bagleycorrected apparent flow curves of all PLAs for three dies having the same L/D = 16 and different diameters (D =
1.22 mm, 0.76 mm, and 0.43 mm). The dynamic complex modulus is also plotted in Fig. 1 as a function of angular
frequency ( G* G '2 G "2 versus ), which represents the flow curve of the polymers under no slip. The diameter
dependency of the flow curves or deviation of the flow curves from the curve indicated as LVE (failure of the CoxMerz rule) implies wall slip [30]. In fact, such deviations from the LVE curve and diameter dependence has been
obtained for the three PLAs (see Figs. 1a, b and c), whereas for the PLA having the smallest molecular weight, the
no-slip boundary condition seems to apply (Fig. 1d).

030002-2

The slip velocity of all three PLAs are plotted in Fig. 2. First, it is noted that the PLA with the smallest molecular
weight, namely PLA3251D in Tab. 1, does not slip as the flow curves did not exhibited diameter dependence (Fig.
1d) and also the flow curves agreed with the LVE data. PLA 3051D has the highest slip velocity as compared to
PLA7001D and PLA2002D which have higher molecular weights. It appears that the slip velocity increases with
decrease of molecular weight and below a certain molecular weight where the molecular size is comparable to
characteristic size of the asperities it becomes zero. Previous studies have also shown the same molecular weight
dependence of slip velocity for nearly monodisperse or narrow molecular weight distribution polymers. Mehtar and
Archer [31, 32] for the case of nearly monodisperse polybutadiens, and Awati et al. [33] and Mackay and Henson
[34] for nearly monodisperse polystyrenes have shown that slip velocity increases with decrease of molecular
weight. Considering the convective constraint release mechanism for bulk and tethered chains, Joshi et al. [35]
proposed some scaling relationships which are in agreement with these experimental observations.
100

100

PLA 7001
T= 180o C
L/D = 16

10-2

D= 1.22 mm
D= 0.76 mm
D= 0.43 mm
LVE

10-3
10-1

100

Shear Stress (MPa)

10-1

100
101
102
103
Apparent Shear Rate or Frequency (s-1)

D= 1.22 mm
D= 0.76 mm
D= 0.43 mm
LVE

10-2

10-3
10-1

104

10-1

100
101
102
103
104
-1
Apparent Shear Rate or Frequency (s )

PLA 3251D
T= 180oC
L/D = 16

10-2

10-2

10-4
10-2

10-1

100

PLA 3051D
T= 180oC
L/D = 16

10-3

PLA 2002D
T= 180oC
L/D = 16

Shear Stress (MPa)

10-1

Shear Stress (MPa)

Shear Stress (MPa)

PLA 7001D
T= 180oC
L/D = 16

10-3

D= 1.22 mm
D= 0.76 mm
D= 0.43 mm
LVE
10-1
100
101
102
103
Apparent Shear Rate or Frequency (s-1)

10-4

104

10-5
10-1

D= 1.22 mm
D= 0.76 mm
D= 0.43 mm
LVE
100
101
102
103
Apparent Shear Rate or Frequency (s-1)

104

FIGURE 1. Diameter dependence of the flow curve and deviation of these from the LVE curve implies the occurrence of wall
slip. As seen all PLAs slip except PLA3251D having the smallest molecular weight (a) PLA7001, (b) PLA2002D, (c) PLA
3051D and (d) PLA 3251D.

030002-3

103
o

Slip velocity, Vs (mm/s)

T= 180 C
102

101

100

Shear Stress, w (MPa)

10-1
10-2

PLA 2002D
PLA 7001D
PLA 3051D

10-1

100

FIGURE 2. The slip velocity, VS as a function of wall shear stress for 3 PLAs listed in Tab. 1 at 180oC.

Melt Fracture of PLAs

Figure 3 shows images of extrudates of PLA7001D obtained by extrusion through a capillary die having a
diameter of 0.76 mm and L/D of 16 at 180oC, 200oC and 220oC at various shear rates. First at 180oC, the extrudate at
the shear rate of 650 s-1 has a smooth surface (Fig. 3). As the apparent shear rate increases surface irregularities
appear at 1285 s-1, which become gross distortions at 2530 s-1.
Table 3 lists the critical shear stresses and rates for the onset of extrudate disortion at the temperature of 180oC
for PLA 7001D. Similar results were obtained for the other PLAs. It is found that the critical shear rate depends
significantly on the diameter of the die in accordance with the scaling of A,c D 1 , proposed by [36]. However, the
critical conditions for the onset of melt fracture is not sensitive to L/D ratio [37]. The critical stresses are slightly
depended on the diameter and relatively independent of molecular weight, with most of the critical shear stress
values in the range of 0.2 - 0.3 MPa.
TABLE 3. Critical shear stress and critical apparent shear rates for the onset of melt fracture of PLA 7001D at 180oC as a
function of the geometrical characteristics of capillary dies.
Diameter (mm) L/D Shear stress (MPa)
Apparent shear rate (s-1)

0.43
0.76
0.76
0.76
0.76
1.22

16
1.8
5.3
16
33
16

0.33
0.30
0.29
0.29
0.30
0.20

030002-4

914
463
463
463
463
119

FIGURE 3. Im
mages of PLA70
001D extrudates at different appaarent shear rates and various tem
mperatures
ranging frrom 180oC to 2220oC.

Melt Frracture of PCLs

In our capillary
c
experriments we fou
und that the hig
ghest moleculaar weight comm
mercial PCL eexhibits melt frracture
phenomenaa (extrudate distortions) whille the other com
mmercial PCLss always exhibbited smooth annd glossy extruudates.
Figure 4 plots the flow curve
c
of Capa6
6800 at six tem
mperatures, nam
mely 80, 100, 1115, 130, 145 and 160C. Att 80C
which is close
c
to meltin
ng temperaturee of PCL, sheaar induced cryystallization caauses increasee of shear stress and
deviation from
f
Cox-Merrz rule at high shear rates. The
T various in stabilities obseerved on the ssurface of extrrudates
included lo
oss of gloss, sh
harkskin or surfface melt fractture, stick-slip or oscillating m
melt fracture aand finally grosss melt
fracture. Loss of gloss an
nd sharkskin melt
m fracture app
peared at criticcal shear stressses between 0.17 MPa to 0.21 MPa
peratures high
her than 115C. Note that sim
milar critical shhear stresses w
were found for PCLs.
for the extrudates at temp
For measu
urements at 100
0C, sharkskin
n phenomena were
w
surprisinggly obtained att much higher critical stress values
of greater than
t
0.48 MPaa. At the lowestt temperature of
o 80oC the criitical shear streess for the onseet of instabilitiees was
0.41 to 0.4
45 MPa which is comparable to that obtaineed at 100oC. It seems that proocessability off this resin is beetter at
a low temp
perature.

030002-5

w (MPa)

101

100

80C
100C
115C
130C
145C
160C

10-1

Capa6800
L/D=16
D=0.79 mm
10-2
100

101

102

103

104

(s-1)

FIGURE 4. The flow curves of Capa 6800 at 80C 160C. Full symbols represent extrudates free of any distortions.

Figure 5 presents images of extrudates of Capa6800 extruded at 80C, 100C, 130C and 160C. Comparing the
extrudates at various temperatures, it may be easily noted that those extruded at 130oC exhibits clearly periodic
surface instabilities very pronounced even at shear rates as low as 100 s-1. At higher shear rates the amplitude of
distortions increases significantly (Fig. 20). It is also clear the improved processability at the temperature of 100oC.
The origin of this is not known, although similar stable processability temperature windows have been observed in
the extrusion of linear polyethylenes [38, 39].

Processing Aids
In order to overcome extrudate distortions and to render the processes economically feasible, polymer processing
aids (PPAs) are frequently used [23-25, 40, 41]. PPAs can eliminate melt fracture phenomena such as sharkskin or
postpone them to higher shear (flow) rates. The end result is an increase of the productivity as well as an energy cost
reduction, while high product quality is maintained. The additives mostly used are fluoropolymers especially
designed for polyolefin extrusion processes. Achilleos et al. [24] have reviewed the formulation, applications and
performance of various processing aids. As stressed by Rosenbaum et al. [40], a potential polymer to work as a
processing aid for the extrusion of another polymer should first be immiscible and have an interfacial tension with
the polymer under flow smaller than the interfacial tension of the polymer under flow with the wall. Such a
candidate might be a poly(-caprolactone) polymer of similar viscosity, which is immiscible with PLA [42-46].
Extrusion experiments were performed for PLA7001D (more severe melt fracture behaviour) with addition of
0.5wt% of commercial poly(-caprolactone) Capa 6500 (see above for more details). The two polymers were
grinded and mixed in dry form and then loaded into the barrel of the capillary rheometer. Figure 6 depicts a transient
experiment illustrating the process of wall coating by the presence of poly(-caprolactone) (PCL). First, Fig. 6 (left)
shows the pressure transient for the capillary extrusion of pure PLA (PLA7001) by using a die having a diameter
equal to 0.76 cm and L/D ratio of 16. The pressure drop increases slowly and after a certain time assumes a steadystate value. When the blend of PLA+ 0.5% PCL is extruded through a die (Fig. 6 right), the pressure drop passes
through a maximum and as the PCL coats gradually the interface of the die, slip becomes a factor and as a result the
pressure drop starts decreasing. The steady-state value is obtained after filling the reservoir several times (4 times).
The steady-state value of the apparent shear stress in the presence of 0.5 wt% of PCL is significantly lower
compared to that in the absence of PCL. This is clearly due to the occurrence of interfacial slip.

030002-6

FIGURE
E 5. SEM microg
graphs of Capa 6800
6
extrudates at
a various tempeeratures ranging from 80oC to 1660C. The extruddates
were produ
uced by using a capillary
c
die haviing a diameter D = 0.79 mm andd an L/D = 16. T
The apparent shear stress and sheear rate
are listed
d under the imagges.

030002-7

Apparent Shear Stress (Mpa)

0.30

PLA 7001D + 0.5% PCL

T= 180o C
D= 0.76 mm
L/D= 16

Run 1

0.25

Run 2

0.20

Run 3

Run 4

0.15

0.10

Clean surface
0.05

0.00

10

6 8 10 12 14 16 18

20

30

40

50

60

70

Time (min)
FIGURE 6. The effect of the addition of 0.5wt % of a poly(-caprolactone) (PCL) on the transient response in the capillary
extrusion of PLA7001D 4100 at 180oC, A 330 s 1 , L/D = 16 and D = 0.76 mm.

Figure 7 shows the apparent flow curves obtained at 180oC for pure PLA7001D and that of a blend of
PLA7001D with 0.5wt% of the finely dispersed PCL. No end pressure (Bagley) correction was applied in this plot
and this is the reason that the apparent shear stress is plotted. It can be seen that the presence of the PCL
dramatically decreases the shear stress practically over the whole range of apparent shear rates up to 5,000 s-1. The
presence of PCL eliminates completely melt fracture. Thus, the extrudates appear relatively smooth up to the shear
rates of 5000s-1 as can be seen from Fig. 8. The fracture elimination by PCL arises from either interfacial slip which
decreases the effective deformation of the melt significantly particularly at the exit where surface melt fracture
originates [37]. Similar results were obtained in the extrusion of PCLs when a small amount of PLA was used.

Apparent Shear Stress (Mpa)

100

PLA 7001D
o
T= 180 C
D= 0.76 mm
L/D= 16

10-1

10-2
100

Pure PLA
PLA + 0.5%PCL
101

102

103

Apparent Shear Rate (s-1)

104

FIGURE 7. The effect of the addition of 0.5 wt % of a poly(-caprolactone) (PCL) on the flow curve of resin PLA7001D at
180oC using a die with D = 0.76 mm and L/D = 16.

030002-8

FIGURE 8. Images of PL
LA7001D extrud
dates at differentt apparent shear rates extruded w
with and withoutt 0.5 wt% of a pooly(ne) (PCL) at 180
0oC. The addition
n of a poly(-cap
prolactone) (PCL
L) is an effectivee way to eliminaate melt fracture in the
caprolacton
extrrusion of PCL.

CON
NCLUSION
NS
The waall slip and meelt fracture beh
haviour of seveeral commerciaal PLAs and PCLs have beenn investigated. PLAs
with moleccular weights greater
g
than a certain
c
value were
w found to sllip significantlyy, with the slipp velocity to inncrease
with decreease of molecu
ular weight. While
W
this find
ding seems coounterintuitive,, it appears too be consistennt with
findings on
n the slip behaviour of other nearly monodiisperse polymeers such as pollybutadienes annd polystyrenees. The
effect of po
olydispersity on
o the slip behaaviour of this family
f
of polym
mers needs furrther investigattion and at thiss point
it is not known
k
if syneergistic effectss exist on thee combined efffects of moleecular weight and polydisppersity,
particularly
y if stick slip phenomena
p
takee place that sep
parate weak sliip from slip efffects.
The on
nset of melt fraccture for the hiigh molecular weight
w
PLAs aand PCLs was found to occurr at around 0.22 to 0.3
MPa, depeending on the geometrical
g
ch
haracteristics of the dies, andd nearly indepeendent of tempperature. The ccritical
shear rate for the onset of
o melt fracturre was found to
o scale inverseely proportionaal with the diee diameter connsistent
vations on the melt fracture of
o other polymers such as pollyethylenes.
with observ
Finally
y, addition of 0.5wt%
0
polycaaprolactone (PC
CL) was foundd to be effectivve in eliminatiing and delayiing the
onset of melt
m fracture to higher shear rates.
r
Thus, a small amount of PCL may bbe used as a prrocessing aid ffor the
processing
g of PLAs and vice
v versa.

ACKNOW
WLEDGEM
MENTS
The autthors would lik
ke to acknowleedge NSERC fo
or financial asssistance.

030002-9

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