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An apparatus for measuring the thermal conductivity and viscosity of

polymers under shearing strain

Article in Measurement Science and Technology · January 1999

DOI: 10.1088/0957-0233/8/3/011

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Meas. Sci. Technol. 8 (1997) 287–292. Printed in the UK PII: S0957-0233(97)73042-X

An apparatus for measuring the

thermal conductivity and viscosity of
polymers under shearing strain
I H Tavman
Dokuz Eylul University, Mechanical Engineering Department, 35100 Bornova/İzmir,
Turkey

Received 22 March 1996, in final form 11 November 1996, accepted for publication
3 December 1996

Abstract. Due to the difficulty of finding an appropriate method and experimental

set-up to measure thermal conductivity in shear flow, there have been very few
publications about the effect of orientation on thermal conductivity in shear flow in
the literature and viscosity is generally measured separately by using a different
experimental set-up. In order to measure simultaneously the thermal conductivity
and viscosity of polymer melts in shear flow, a concentric cylinder thermal
conductivity cell which is similar in principle to a Couette viscometer has been built.
Thermal conductivity can be measured at temperatures approaching 220 ◦ C and at
strain rates up to 300 s−1 . The outer cylinder may be rotated at the desired speed
of rotation, while the inner cylinder which is stationary has a strain gauge mounted
on its top in order to measure the torque and therefore the viscosity. The gap of
2 mm between the two cylinders is filled with polymer melt. The thermal
conductivity is measured by a transient plane heat source method which consists
of generating heat at a constant rate by using the nickel wire wrapped around the
periphery of the inner cylinder and recording the temperature rise of the nickel wire
as a function of time. The measurement process and the speed of the motor are
controlled by a microcomputer.

1. Introduction
The thermal conductivity and viscosity of polymer melts
are two important properties which depend on temperature,
pressure, shear-rate, chemical composition, molar mass
and additives. During injection and extrusion, polymer
melts are highly oriented and show anisotropic physical
properties due to their macromolecular structure. It has
to be admitted that the transport of thermal energy is more
readily achieved in the direction of the backbone chain than
it is across it, from one molecule to another. It is obvious
that a knowledge of the thermal transport and rheological
behaviours of polymer melts in a shear flow situation is
necessary in order to optimize the injection and extrusion
processes.
The first publications on thermal anisotropy of polymer
melts appeared in 1970. Cocci and Picot [1] constructed
an annular axial flow test cell that utilized a hot-wire probe
technique to measure thermal conductivity under shear. The
hot-wire probe is placed in the centre of the annulus. Later,
an improved version of this axial flow cell was constructed
with the polymer flowing parallel to the wire by Chitrangad
and Picot [2]. Major drawbacks of this cell were found to
be the fragility of the wire in the midst of the flowing
polymer; the requirement for large quantities of specimen
material; the large size of the equipment and cell, making
precise temperature control difficult; and the variation in
the rate of shear along the path of heat conduction. In
order to measure the thermal diffusivity of polymer melts
under shear flow, a rotating concentric-cylinder cell has
been constructed by Tavman [3], a periodic sine heat wave
method is used and the thermal diffusivity is calculated
from the phase difference measured between the outer and
the inner surface of the polymer.
2. The experimental apparatus and the
measurement principle
The experimental apparatus used to measure both thermal
conductivity and viscosity under shear flow is similar in
construction to a Couette viscometer. The measurement
cell is made of two concentric cylinders, see figure 1.
The outer cylinder made of aluminium is painted with a
black heat-absorbing paint on its exterior surface and has an
outer diameter of 40 mm and an inner diameter of 34 mm.
The outer cylinder may be rotated at the desired speed of
rotation by means of an electrical motor which is controlled
by a microcomputer. The inner cylinder, which is made
of a high-temperature thermoplastic polyimide (Vespel), is
stationary and has an outer diameter of 30 mm and an inner

0957-0233/97/030287+06$19.50 c 1997 IOP Publishing Ltd 287

I H Tavman
Figure 1. A sketch of the concentric-cylinder thermal conductivity and viscosity measuring cell.
diameter of 24 mm. A nickel resistance wire 12 m in
length and 0.08 mm in diameter is wrapped around the outer
surface of the inner cylinder; this nickel wire is used both as
a constant flux heat source and as a resistance thermometer.
In order to measure the torque and therefore the viscosity
a strain gauge is mounted on the top of the inner cylinder.
To begin the experiment, a solid cylindrical polymer
sample 34 mm in diameter and 40 mm in height is placed
in the plastification chamber located at the bottom of the
apparatus. The polymer sample is heated and melted
by the temperature-controlled resistance placed around the
plastification chamber; the molten polymer is then injected
into the 2 mm thick, 150 mm high narrow gap between
the two cylinders by means of a piston. When the co-axial
measuring cell has been filled completely, the bar pushing
the piston is drawn back and the piston is fixed to the outer
cylinder by means of a screw preventing leakage of the
molten polymer. The measuring cell is maintained at a
fixed temperature by means of six infrared heating elements
placed symmetrically around the outer cylinder. In order
to avoid heat pulses which may disturb the measurement,
temperature control of the heating elements is achieved by
regulating the voltage of the AC supply current through a
288
rheostat. The temperature of the polymer is measured by
a thermocouple placed on the outer surface of the inner
cylinder in contact with the polymer.
A uniform rate of strain is developed within the fluid
when the outer cell is rotated at the desired speed. When
the viscous heating effects have attained a steady state,
the thermal conductivity is measured by a plane heat
source method which consists of releasing constant heat
from the nickel resistance wire wrapped around the inner
cylinder and measuring the temperature rise at the interface
between the inner cylinder and the polymer. The transient
temperature distribution for a constant heat input at the
interface bounded by two semi-infinite regions, one of
which (Vespel) has known thermal properties, has been
given by Carslaw and Jeager [4]:
t 1/2
1T = 1.1284 Q (1)
(k1 ρ1 cp1 )1/2 + A
1/2
where A = k2 /a2 , 1T is the temperature rise at the
interface during time t, Q is the heat input at the interface
per unit time per unit area, a1 , a2 , k1 and k2 are respectively
the thermal diffusivities and conductivities of the polymer
 Conductivity and viscosity measurement under shear

and Vespel and ρ1 and cp1 are the density and heat capacity Table 1. Measuring cell calibration data.
of the polymer. A plot of 1T against t 1/2 is a straight line
and, if ρ1 and cp1 are known, the thermal conductivity of Silicone oil Ethylene glycol
the polymer, k1 , may be calculated from the slope of this −3
ρ1 (kg m ) 965 1112.5
straight line. cp 1 (J kg−1 ◦ C−1 ) 1630 2460
The electrical resistance Rnw of the nickel wire, k1 (W m−1 ◦ C−1 ) 0.13 0.26
which has the value of Rnw 0
= 195  at the reference (k1 ρ1 cp 1 )1/2 452.2 843.5
◦ Inw (mA) 63.59 63.41
temperature 20 C, changes as a function of temperature
change according to Average 1V (mV) 9.76 9.24
Average m (mV s−1/2 ) 7.691 6.906
3
1Rnw = βRnw
0
1T (2) Inw ξ/(As m ) 769.3 849.5

where β is the temperature resistance coefficient for the

nickel wire. Temperature measurement at the interface is
then made possible by measuring the voltage difference
1(I R)nw across the heating element. Figure 2 shows
the nickel wire heating and the measuring circuit. The
resistances Ra , Rb , Rc and Rd are located outside the
measuring cell and therefore are not affected by temperature
changes in the cell; Rnw is the resistance of the nickel
heating wire wrapped around the inner cylinder. The
variable resistance Rc is used to balance the bridge. A
laboratory DC power supply is used to provide a constant
voltage of 48 V under the varying load conditions. The
relay switch is of the mercury-wetted type in order to
eliminate contact noise. This relay is triggered by the 5 V
output of the microcomputer; the electrical current and thus
the heat pulse is on for 3 s. Within this interval of time the
current Inw stays constant and the bridge is unbalanced due
to the increase in Rnw with the rise in temperature of the
nickel heating wire. The change in 1(I R)nw is recorded
as a function of time by a microcomputer with a 12 bit
analogue-to-digital conversion interface card. The early
(t < 0.5 s) 1T versus time history must be omitted from
the measurements because of the complication caused by
the heating wire’s thermal capacity, which has a negligible
effect at greater time. In addition, 1T values at times
greater than 3 s, for which the depth of penetration of the
heat pulse will be greater than 2 mm, so that the heat
pulse will travel beyond the outer cylinder, will contain
the complicating influence of outer cylinder material and
cannot be adequately analysed. The measurement is fully
controlled by the microcomputer which triggers the heat
pulse of 3 s, acquires 1(I R)nw every 0.1 s, up to 3 s,
draws the line 1(I R)nw as a function of t 1/2 , calculates the
slope m of this line and prints the results, see figure 3.
The temperature rise 1T at the interface due to the heat
pulse is given by
1(I R)nw Ra + Rnw
0
1T = 0 I
(3)
βRnw nw Ra
From equations (1) and (3)
2 in the Wheatstone bridge. The output voltage is connected
1.1284 QInw βRnw Ra 1/2
1(I R)nw = t . (4)
[(k1 ρ1 cp1 ) + A] Ra + Rnw
1/2 0
The slope ‘m’ of 1(I R)nw as function of t 1/2 is given by
0
1.1284 QInw βRnw Ra
m= . (5)
(k1 ρ1 cp1 )1/2 + A Ra + Rnw
0 obtained match the corresponding literature values well.
Using the electrical equivalent of Q, equation (5) becomes
3
Inw ξ (k1 ρ1 cp1 )1/2 A
= + (6)
As m 1.1284 1.1284
where
0
βRnw Ra
ξ = Rnw (7)
Ra + Rnw
0
As is the heating surface of the inner cylinder which is
equal to 5.98 × 10−3 m2 . Therefore equation (6) can be
written as
3
Inw ξ
= C1 (k1 ρ1 cp1 )1/2 + C2 (8)
As m
where C1 and C2 are the constants of the measuring cell
which must be determined by using two different materials
of known properties.
Silicone oil and ethylene glycol were used to calibrate
the measuring cell. The physical properties of these
materials and the results of the measurements are given
in table 1. The values of C1 and C2 calculated from
this table are C1 = 0.205 and C2 = 676.65. The
experiments were performed with the fluid at rest and
at room temperature (20 ◦ C). Five measurements were
performed for each material and the average values are
reported; the reproducibility is better than ±2%.
In order to measure the viscosity of the polymer, the
torque at the inner cylinder must be measured, while the
outer cylinder is rotating with a constant velocity. The
torque caused by the friction through the bearings and the
lower tip of the inner cylinder is taken into consideration
by measuring it at various speeds of rotation when the cell
is empty. The net torque is then calculated by subtracting
the frictional torque at the corresponding speed from the
measured one. The frictional torque is always less than
1% of the measured torque value. The torque measuring
unit supplied by SEDEM has strain gauges belonging to a
Wheatstone bridge which is supplied with 10 V DC. This
unit is mounted on the top of the inner cylinder. The torque
experienced by the inner cylinder causes a disequilibrium
to the 12 bit analogue-to-digital conversion interface card
through an amplifier. Ten values of voltage difference are
recorded by a microcomputer and the average is used to
calculate first the torque and then the viscosity at a given
temperature and shear rate. The values of viscosity thus

289
I H Tavman

Figure 2. The electrical circuitry for thermal conductivity measurements.

Figure 3. A typical plot of the voltage rise, 1(IR )nw , across the probe as a function of the square root of time.

3. Measurements which are thermally anisotropic, he draws an analogy

The thermal conductivity and viscosity of a linear low-
density polyethylene, LLDPE HX 5631, supplied by
Atochem were studied at 160 ◦ C up to a shear rate of
170 s−1 . The thermal conductivity results, which are shown
in figure 4, are expressed in terms of a normalized thermal
conductivity, k/k0 , the ratio of the thermal conductivity
measured perpendicular to the flow direction to that under
zero shear. At low rates of strain, up to a shear rate
of about 70 s−1 , there is a decrease in the thermal
conductivity followed by an increase at higher shear rates.
This is suggestive of two types of flow occuring at low
and high shear rates, respectively. Busse [5] offered an
explanation based on entanglements of macromolecules
with strings of beads of different lengths immersed in a
liquid of the same density. Movements of the beads are
considered representative of normal segmental Brownian
motions of molecular chains. At low shear rates, the flow
is considered laminar and entanglements are formed as the
interpenetrating molecules with different velocities sweep
past each other. If the normal segmental Brownian motion
of the chain segments cannot disentangle the intersecting
chains in some small fraction of a second, the points
of entanglements are pulled apart, causing the molecular
chains to be stretched with a consequent distortion of
the random coils. The thermal conductivity could be
expected to decrease given that the chains are stretched
in the direction of flow. An important implication of

290
 Conductivity and viscosity measurement under shear

Figure 4. The normalized thermal conductivity (k /k0 ) of LLDPE versus the shear rate.

Figure 5. The viscosity of LLDPE versus its shear rate on a logarithmic scale.

the proposed model is that the major initial effect of an
applied shearing stress is to build up elastic energy in the
sample by distorting the polymer random coils. This may
be manifested by the large recoverable elasticity that is
commonly observed when the stress is removed.
The increased thermal conductivity observed at higher
shear rates is due to elastic turbulence and cluster flow.
As the shear rate is increased beyond the slippage rate at
the entanglements in groups of the more tightly snubbed
molecules, these groups will act as temporarily cross linked
clusters. The ends of these molecules that stick out of
the cluster will flow past the surrounding molecules by
normal segmental Brownian motion. These clusters rotate
more or less as a unit, somewhat like small fuzz-covered
soft rubber balls dispersed in a low-viscosity liquid that
is being sheared. This has the effect of increasing the
thermal conductivity. According to Busse’s [5] analysis,
for highly polymeric liquids, the transition from flow with
stretched molecular chains in the direction of flow to flow
with rotating clusters occurs when the elastic energy stored
in the random coils becomes of the same order of magnitude
as the amount of viscous heat generated at the entanglement
junctions. This transition to elastic turbulence occurs when
some critical value of a parameter P is exceeded, such that
P = τ v/L (9)
where v is the velocity of the fluid, L is a characteristic
length and τ is the inherent relaxation time of the molecular

291
 I H Tavman
chains. In the case of shear flow, equation (9) can be written
as
P = τS (10)
where S is the shear rate.
Viscosity is plotted versus shear rate on a logarithmic
scale in figure 5. Two distinct regions may be noticed from
figure 5, for low shear rates (γ < 30 s−1 ), the molten
polymer exhibits Newtonian behaviour, thus the viscosity
is not a function of the shear rate. For higher shear
rates the viscosity decreases with increasing shear rate;
this behaviour is called pseudo-plasticity. It is known that
molten polymers are non-Newtonian fluids; the viscosity
(η) may be expressed by a power law:
η = K(γ ) m−1
(11)
where γ is the shear rate, K is a constant and m is the
pseudo-plasticity index. From figure 5, for γ > 60 s−1 ,
K = 6419 and m = 13 with a correlation coefficient of
0.91.
4. Conclusion
The new apparatus which is similar to a Couette viscometer
in construction has proven itself to be very useful
and practical for measuring simultaneously the thermal
conductivity and viscosity at various shear rates and
292
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temperatures. These two properties are essential in the
simulation of injection-moulding processes. A transient
plane heat source method is used to measure the thermal
conductivity. The thermal conductivity measurements
as well as the speed of the motor are controlled by a
microcomputer. The control of temperatures is achieved
manually by varying the voltage through resistance heaters.
The reason for this is to avoid all heat pulses which may
be generated by automatic control, which would disturb the
acquisition of the voltage difference across the nickel wire.
References
[1] Cocci A A Jr and Picot J J C 1973 Rate of strain effect on
the thermal conductivity of a polymer liquid Polym. Eng.
Sci. 13 337–41
[2] Chitrangad B and Picot J J C 1981 Similarity in orientation
effects on thermal conductivity and flow birefringence for
polymers–polydimethylsiloxane Polym. Eng. Sci. 21
782–6
[3] Tavman I H 1991 Effects of molecular orientation on
thermal diffusivity of polymers under shearing strain
Proc. Second World Conf. on Experimental Heat Transfer,
Fluid Mechanics and Thermodynamics (Amsterdam:
Elsevier) pp 1569–74
[4] Carslaw H S and Jaeger J C 1956 Conduction of Heat in
Solids (London: Oxford University Press) pp 87–8
[5] Busse W F 1967 Mechanical structures in polymer melts. II.
Roles of entanglements in viscosity and elastic turbulence
J. Polym. Sci. A 5 1261–81