Capillary Rheometery

Report
Karim Habbas
B122608
Loughborough University
Department of Materials
Polymer Engineering - Processing and
Manufacture
14MPC012
Word Count: 1500
Abstract: 164
Introduction: 212
Results and Discussion: 968
Conclusion: 156

24/03/15

Capillary Rheometery

Karim Habbas, B122608

Abstract
Using capillary rheometery the true shear stress, apparent strain rate, shear viscosity, swell
ratio, and melt fracture of Borealis High Density Polyethylene, BS2581, resin were
investigated. Dies with a 2mm diameter with length/radius ratios of 20, 10, and 5; a
temperature of 190C and ram velocities of 8, 15, 30, 60, 120 mm/min were used. A Bagley
end-correction plot was used to mitigate the effects of pressure drop, due to convergent flow,
across the die. After calculating both the true shear stress and apparent shear rate a shear
flow curve was used to derive an approximation for the Power Law Index (n) and
Consistently Index (K), 0.348 and 29648 respectively. With n < 1, the polymer melt was
confirmed to be pseudoplastic and experiencing shear thinning at the aforementioned
boundary conditions. Therefore, the apparent viscosity of the material decreases with
increasing shear rate. Die swell was found to reduce with increasing L/R ratios, whereas
melt fracture shear rate decreased with decreasing L/R ratios.

Capillary Rheometery

Karim Habbas, B122608

Contents
1.0 Introduction ..................................................................................................................................... 1
2.0 Results and Discussion ................................................................................................................ 2
2.1 Bagley End-Correction .............................................................................................................. 2
2.2 Shear Flow and Shear Viscosity ............................................................................................. 4
2.3 Die Swell.. ....................................................................................................................... 7
2.4 Melt Fracture .............................................................................................................................. 9
3.0 Conclusion .................................................................................................................................... 10
4.0 References ................................................................................................................................... 11
5.0 Appendix ....................................................................................................................................... 12

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Capillary Rheometery

Karim Habbas, B122608

1.0 Introduction
Capillary rheometry is the controlled extrusion of a test material used to determine the melt
viscosity at shear rates relevant at an assumed constant temperature. Shear viscosity is
derived from the controlled experimental parameters of capillary die dimensions, ram
velocity and pressure.
Capillary rheometry can be used to evaluate other rheological and process characteristics,
including die swell, melt fracture, wall slip, flow/no-flow stress, melt strength, haul off and
pVT relationships (1). Since the shear rate and shear stress vary with radial position within
the capillary, the wall of the capillary is chosen as a point where both of these variables are
determined (2).
Predominantly associated with polymer melt processing, capillary rheometry is directly
relevant to other processes. From high speed coating, printing applications and pressure
nozzle design, capillary rheometry ensures test conditions are representative of
manufacturing processing conditions (3).
In industry the output data and analysis of capillary rheometry experiments can greatly
influence the manufacturing of parts by optimising process parameters. The characterisation
of the swell ratio and melt fracture shear rate compared to ram velocity are examples of
variable parameters that need to be considered.
Borealis High Density Polyethylene, BS2581 is intended for blow moulding products with
high stiffness and very good environmental stress crack resistance (5).

Capillary Rheometery

Karim Habbas, B122608

2.0 Results and Discussion

2.1 Bagley End-Correction
The convergence of the wide barrel to narrow capillary dimensions, causes acceleration of
melt flow, resulting in elongation deformation and shear stress which causes an abrupt drop
in pressure. The Bagley end-correction factor compensates for this pressure drop by
extended the length of the die to an effective length (Leffective). Bagley end-correction factor
must be included to ensure the shear stress is not overestimated by correcting for the
assumption that the flow exhibits Newtonian behaviour (4). Figure 1 is a plot of the variation
of pressure along the flow length, where the increasing gradient denotes an increasing shear
rate.

Figure 1: Pressure vs L/R with Bagley end-correction estimations.

The Bagley end correction factor, e, can be calculated by averaging the values at which the
best fit lines cross the x axis (where y = 0). Example calculation of e for 120mm/min flow
rate:
= 0.4113 + 2.255
=

2.255

0.4113

= 5.48
Repeating the aforementioned calculation for each flow rate and averaging the results gives
the average Bagley end-correction factor, e:
(5.48 + 4.66 + 3.99 + 3.84 + 3.17) = 21.17

=
2

21.17
= 4.23
5

Capillary Rheometery

Karim Habbas, B122608

N.B. the Bagley correction factor is treated as an absolute value hence finally calculated as a
positive length. The effective length is defined by the equation below:
= +

Calculation for shear stress at the wall, , for ram velocity 8.0mm/min and L/R = 20:
=

2( + )

(4 106 )(0.001)

20.02 + (4.23 103 0.001)

= 101.73

Repeating the above calculations for all ram velocities, Table 1 shows the true shear stress
values for L/R = 20. As expected the true shear stress increases with increasing ram
velocities. This is because the increasing relative motion within the polymer melt intensifies
shear stress between the melt layers causing the molecular chains to slip.

Capillary Rheometery

Karim Habbas, B122608

2.2 Shear Flow and Shear Viscosity

In order to calculate the apparent shear rate, at the wall, where it is assumed there is zero
slip, average velocity of the melt needs to be derived from the ram velocity and dimensions
of the die. Example calculation for average velocity, :
=

2 = ( )2
( )2
= 2

=
= 0.001

= 0.008

0.008
0.0082

0.0012
60

= 8.53 103 1
4
= 3

=
=

4(8.53 103 )

0.001

= 34.13 1

Repeating this calculation for all ram velocities yielded the results found in Table 2. As the
ram velocity increases, the apparent shear rate also increases.

With both the true shear stress and apparent shear rate positively correlating with increasing
ram velocities, further investigation can be found in Figure 2.

Capillary Rheometery

Karim Habbas, B122608

The shear flow curve provides a graphical representation of true shear stress over apparent
shear rate. By plotting the variables on a logarithmic scale, a linear line of regression can be
plotted and used to derive an approximation of the Power Law Index (n) and Consistency
Index (K).

Figure 2: Log shear stress vs log apparent shear rate to obtain the shear flow curve.
=

log10 = log10 + log10

= +

= 0.348 log10 + 4.472 ( 4)

log10 = 4.472
= 29648
= 0.348

Since the Power Law Index, n < 1 the polymer melt is pseudoplastic and experiencing shear
thinning. The apparent viscosity of the material decreases with increasing shear rate (5).
From this the shear viscosity, , and the zero-shear viscosity, 0 , can be calculated:

Capillary Rheometery

Karim Habbas, B122608

To further confirm the pseudoplastic, or non-Newtonian nature, of the HDPE at 190C,

plotting the shear stress vs shear rate, for the L/R = 20 is illustrated in Figure 3. For a
Newtonian fluid, with a Power Law Index of 1, shear stress is proportional to the shear rate
and hence the viscosity remains constant throughout (6).

Figure 3: Shear stress against shear rate

Figure 4 illustrates the reduction in apparent viscosity as a function of an increasing shear
rate. Ultimately, viscosity of a fluid is a measure of its resistance to gradual deformation by
shear stress, and like all rheological properties the viscosity depends on the chemical
composition of the material and flow conditions (7).

Figure 4: Apparent shear viscosity vs shear strain rate

Capillary Rheometery

Karim Habbas, B122608

2.3 Die Swell

Die swell is associated with elastic recovery or memory, and is the ratio of the extrudate
diameter to the diameter of the capillary. Along the direction of melt flow, elongation stress
results in stretching out of the polymer molecules as they enter the die. Shear stress at the
walls influences the orientation of the molecules, where die swell causes elastic recovery as
the polymer exits the die. Consequently, the molecules relax to random formations which
result in the expansion or contractions of the extrudate (8).
For shorter die lengths, greater pressure is required and therefore, in general the extruded
part experiences greater die swell (9). This is due to polymer memory, whereby the
molecular arrangement wishes to return to its original shape, after only being in contact with
the die mould over a short time (10). Similarly, increasing ram velocities results in more die
swell. Table 3 details measurement results obtained and calculated swell ratio for all 15
extruded parisons.

Example swell ratio, B, calculation for extrude with a L/R of 20 and Ram Velocity of
8mm/min:
=

= 2.743 103
= 0.002

2.743 103
0.002

= 1.372
7

Capillary Rheometery

Karim Habbas, B122608

Figure 5: Swell Ratio vs Die Ratio L/R for maximum and minimum apparent shear rates,
512s-1 and 34s-1 respectively.
Figure 5 illustrates that as the L/R increases the swell ratio decreases at a linear rate. If the
plot was extended to a high L/R ratio the swell ratio would consequently decrease further
and tend towards zero. Due to the polymer melt having more time to relax inside the die
channel, this minimises elongation stresses, resulting in reduced compressional forces on
the melt and reductions in spring back as the polymer exits the die (11). The die swell cannot
be totally eliminated due to the presence of shear stress at the wall across the polymer melt.

Capillary Rheometery

Karim Habbas, B122608

2.4 Melt Fracture

Melt fracture is a form of flow instability that initiates in the flow channel and further develops
down the extrude (12). As the polymer exits the die its deformed thus negatively affecting
surface quality and critical mechanical properties. A pattern of rough conical spirals was
observed along the length of the extruded polymer. For decreasing melt fracture pressures
the melt fracture observed decreased in size until the point where no fracture was present.
Melt fracture occurred at different melt pressures for different dies, as the die ratio
decreased, so did the melt fracture shear rate.
By calculating the melt fracture shear rate, the maximum production rate can be obtained to
achieve acceptable part quality. For a manufacturer of polymer sheet extrusions, individual
experimentation should be conducted to optimise their specific processes.
See Table 4 for the different fracture melt pressures, ram velocities, and shear rates for the
three die ratios. Example calculation, for melt fracture shear rate, , for Die Ratio 20/2:
=

2
= 2

Vr = 200 /1000 / 60 = 3.33x103 ms 1

2 = 0.0082 = 6.4x105 m
2 = 0.0012 = 1x106 m

= 3.33x103

6.4x105

1x106

= 0.213 ms1
=

4 0.213
0.001

= 853.33 1

Capillary Rheometery

Karim Habbas, B122608

3.0 Conclusion

To ensure the shear stress is not overestimated Bagley end-correction is required to

compensate for the pressure drop created by the convergence of the capillary.

There is a positive correlation between both ram velocity and true shear stress, as
well as ram velocity and apparent shear rate. As ram velocity increases, so does the
shear stress and apparent shear rate.

As obtained from the shear flow curve, High Density Polyethylene can be categorised
as a non-Newtonian due to the fact it has a Power Law Index, n, value < 1.

Due to the pseudoplastic nature of HDPE BS2581 at 190C, the apparent viscosity
decreases with increasing shear rate.

By increasing the L/R ratio, die swell, B, decreases. With high L/R ratios the
elongation stresses tend towards zero and the shear stress at the wall becomes the
predominant cause of die swell.

Melt fracture pressure and melt fracture shear rate decrease as the L/R die ratio
decreases.

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Capillary Rheometery

Karim Habbas, B122608

4.0 References

1. Malvern. Rheometry - capillary . Malvern. [Online] Malvern. [Cited: 13 March 2015.]

http://www.malvern.com/en/products/technology/rheometry-capillary/.
2. Capillary rheometry of polymer melts Simulation and experiment. Aho, Seppo Syrjl
and Johanna. 3, Tampere, Finland and Hillerd, Denmark : Korea-Australia Rheology
Journal, 2012, Vol. 24, pp. 241-247.
3. INSTRON. Capillary Rheometer. INSTRON. [Online] INSTRON. [Cited: 13 March 2015.]
http://www.instron.com/en-gb/our-company/library/glossary/c/capillaryrheometer?region=United%20Kingdom.
4. Polymer Processing: Capillary Rheometry. Thomas, Noreen. Loughborough :
Loughborough University, 2015.
5. Polymer Processing: Geometry of Flow. Thomas, Noreen. Loughborough :
Loughborough University, 2015.
6. Birley, A.W., Haworth,B. and Batchelor,J. 1992. Munich : Hanser Publishers, Physics of
plastics: processing, properties, and materials engineering.
7. John M Dealy, Jian Wang. Melt Rheology and its Applications in the Plastics Industry.
Dordrecht : Springer, 2013.
8. Melt elasticity and extrudate characteristics of polystyrene/polybutadiene blends. Susan
Jospeh, Zachariah Oommen, Sabu Thomas. 4-5, Kerala, India : Material Letters, 2002,
Vol. 53, pp. 268-276.
9. Kealy, Tim. Explanation and Evaluation of Die Swell. Victoria, Australia : Rheology
Soloutions, 2006.
10. Deng, Eason. 14MPC012 Lab Classes. Capillary Rheometry. Lougborough :
Loughborough University, 24 Febuary 2015.
11. RHEOLOGICAL AND DIE SWELL MEASUREMENTS OF THERMOPLASTIC STARCH/
ACRYLONITRILE- BUTADIENE- STYRENE BLENDS. Mosab Kaseem, Kotiba Hamad,
Fawaz Deri. 1, Damascus, Syria : Malaysian Poylmer Journal, 2012, Vol. 7, pp. 22-27.
12. Catherine, Olivier. Looking into Photovoltaic Film? Here Are Material & Die-Design
Insights. Plastics Technology. [Online] Plastics Technology, Febuary 2012. [Cited: 11 March
2015.] http://www.ptonline.com/articles/looking-into-photovoltaic-film-here-are-material-diedesign-insights.
13. Subramanian, R. Shankar. Non-Newtonian Flows. Potsdam, New York : Department of
Chemical and Biomolecular Engineering, Clarkson University.
14. Borealis. Polyethylene BS2581 Data Sheet. Vienna, Austria : Borealis, 2008.

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Capillary Rheometery

Karim Habbas, B122608

5.0 Appendix
Appendix A Physical properties for Borealis High Density Polyethylene, BS2581.

http://www.borealisgroup.com/en/polyolefins/products/Others/BS2581/
Appendix B Schematic of Capillary Rheometer

http://www.atsrheosystems.com/PDF%20files/CapillaryRheometers.pdf

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