Polymer Testing 33 (2014) 138–144

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Polymer Testing
journal homepage: www.elsevier.com/locate/polytest

Test method

A novel method for the determination of steady-state torque

of polymer melts by HAAKE MiniLab
Cong Wang, Jing Wang, Chenyang Yu, Bingtian Wu, Ya Wang, Wenguang Li*
State Key Laboratory of Polymer Materials Engineering, Polymer Research Institute of Sichuan University, Chengdu, Sichuan 610065,
People’s Republic of China

a r t i c l e i n f o a b s t r a c t

Article history: HAAKE MiniLab is an apparatus specially designed for compounding polymer material and
Received 25 October 2013 on-line testing of rheological properties. For the first time, it was used to establish a dy-
Accepted 2 December 2013 namic speed test method for the rapid determination of steady-state torque of polymer
melts. The choices of sample feed quantity and screw rotation speed, as well as calibration
Keywords: for real torque, were carefully studied before torque measurements. The repeatability and
HAAKE MiniLab
reliability of torque data were also evaluated. Results showed that the torque could be
Steady-state torque
calibrated by subtracting the torque without samples. Also, a feed quantity of ca. 6 g with a
Dynamic speed test method
Repeatability
dynamic speed test range of 10–105 r/min was suitable for the determination of steady-
Reliability state torque of polyolefin samples. The new method was quick, effective and reliable to
correlate the steady-state torque with rotation speed. Therefore, MiniLab would be a very
useful tool in exploring and characterizing polymer flow behavior through its torque
measurements.
Ó 2013 Elsevier Ltd. All rights reserved.

1. Introduction real processing conditions. Therefore, many researchers

In the polymer field, torque refers to the hindering force
met when polymer resins or compounds are plasticized
and mixed with rotation of screws or rotors. It has been
used as an engineering indicator to learn the polymer
melting process for determining suitable processing con-
ditions, as well as to monitor industrial extrusion produc-
tion for process quality control. Steady-state torque is the
measurement of the torque at equilibrium as the plasti-
cized material is in a stable and homogeneous melt state.
For a pure polymer in a given process, the steady-state
torque is a characteristic of the polymer, which can be
used as a rheological parameter to characterize the poly-
mer flow behavior [1–4].
The torque-rheometer is the most commonly used tool
in polymer processing laboratory for torque measurements.
It can simulate a mixer and the extrusion process in nearly
* Corresponding author. Tel.: þ86 028 85460817; fax: þ86 028
85402465.
E-mail address: wgli2007@126.com (W. Li).
have used it to study the processing properties and mixing
quality of polymers [5–12]. However, as the mixing of
polymer materials with the rotation of rotors generates
heat from viscous dissipation, the pre-set temperature al-
ways changes during the mixing process, dependent upon
material and experimental conditions such as mixing time
and rotation rate. As a result, it is almost impossible to
obtain a consistent torque for a polymer at a given tem-
perature [13,14]. As for measuring the correlation of steady-
state torque with rotation rate at a given temperature, it is
generally required to select several rotation rates and
measure separately the variation of torque with time at
each rotation rate. This is a time-consuming process with
no certainty of reliable data. Only a few researchers have
tried such experiments with no satisfactory results [15–17].
For the above reasons, the application of torque-
rheometers for characterizing the properties of polymer
melts has been greatly restricted.
MiniLab Micro Compounder and Rheometer, devised by
HAAKE Company, Germany, is specially designed for the
compounding of small volume (7 mL only) samples.

0142-9418/$ – see front matter Ó 2013 Elsevier Ltd. All rights reserved.
http://dx.doi.org/10.1016/j.polymertesting.2013.12.001
 C. Wang et al. / Polymer Testing 33 (2014) 138–144
Simultaneously, the rheological properties can be recorded
to document structural changes. Its main features include
integrated torque and viscosity measurements, co- and
counter rotation twin screws and an automatic bypass
operation for circulation/extrusion with pneumatic
feeding. Therefore, MiniLab is considered as a combination
of a batch mixer, a twin-screw extruder and a rheometer.
Based on the unit’s specifications, we found that, in
addition to small usage of samples, there are two distinct
advantages in determining steady-state torque of polymer
melts by MiniLab over other torque-rheometers. First,
MiniLab has a special backflow channel integrated with the
extrusion housing for circulation, which ensures a precise
and stable operating temperature, thus signifying that the
variation of polymer melt state with temperature due to
viscous dissipation can be negligible. Second, MiniLab can
perform dynamic speed measurements in a selected speed
range by a pre-set test program. We will show that in this
way the correlation of steady-state torque with rotation rate
can be quickly obtained through only a single test, making it
possible and convenient to explore the rheological proper-
ties of polymer melts with significant time and cost savings.
Despite the prominent characteristics of MiniLab as stated
above, published research still relates to using it only as a
conventional mixer to prepare experimental samples and to
compound expensive materials such as nano-composites,
bio-polymers and pharmaceuticals [18–27]. No attention
has been paid to its potential powerful function in torque
measurements. The reason may be that the reliability of
rheological measurements by MiniLab has not been evalu-
ated. Moreover, no appropriate method has been established
for the determination of steady-state torque of polymer melts.
This situation was motivation for the current research.
This paper presents a novel method, termed dynamic speed
test method, for the determination of steady-state torque of
polymer melts by means of the MiniLab’s functions. We will
introduce how to obtain repeatable, reliable torque data as
well as the correlation of steady-state torque with rotation
rate in the MiniLab test. The calibration of torque data, sample
loads and screw rotation speeds were carefully investigated
as regards the repeatability of data. The comparison of the
new method with the common fixed speed method for
steady-state torque measurements was also done to
demonstrate the reliability of data. Our results show that the
dynamic speed test is a quick, effective and reliable method
for determining steady-state torque of polymer melts.
2. Experimental
2.1. Materials
All the samples in this study were carefully selected
from commercial resins. These were high-density poly-
ethylene (HDPE), low-density polyethylene (LDPE) and
isotactic polypropylene (iPP). The characteristics of the
materials were shown in Table 1.
2.2. Instrumental details
The HAAKE MiniLab, as illustrated in Fig. 1, is made up of
five functional elements: control system (1 and 4), drive
139
Table 1
Characteristics of materials used.
Material Grade Melt flow index Supplier
(g/10 min)
HDPE 6070EA 7.2 (190  C/2.16 kg) Dushanzi Petrochemical,
China
HDPE 60550 7.0 (190  C/2.16 kg) Lanzhou Petrochemical,
China
LDPE 18D 1.5 (190  C/2.16 kg) Daqing Petrochemical,
China
iPP T30S 2.0 (230  C/2.16 kg) Lanzhou Petrochemical,
China
unit (2), extruder housing (3) and feeding device (5). The
control system includes the manual operating panel (4) and
the application software (1). Both the dynamic speed
measurement and the experimental data documentation
can only be performed through the software. The drive unit
offers motor motion and precisely controls experimental
conditions, such as testing temperature and rotation speed.
It also measures the motor torque from a mixer sensor. The
structure of the extruder housing with co-rotation twin
screws is displayed in Fig. 2 (the co-rotation mode was used
in this study). The filled-in sample can be extruded in a
circulation via an integrated backflow channel. The back-
flow channel is constructed as a rheological slit capillary
with two pressure sensors. While the sample is extruding
through the backflow channel, the rheological information
about the viscosity of the sample can be obtained from the
two pressure sensors. Lastly, the feeding device enables
periodic sample feeding by the piston of a pneumatic
cylinder.
2.3. Dynamic speed test method
There are two stages in the dynamic speed test method.
In the first stage, samples were dynamically plasticized and
melted under a rotation speed range predetermined ac-
cording to the requirement of the experiment and the na-
ture of the material. The number of speed points was set to
5–20 with equal distance logarithmic intervals (rpm)
within the speed range. At each speed, the software pro-
gram measured the torque of the material, and then
Fig. 1. The constitution of HAAKE MiniLab: (1) and (4) control system, (2)
drive unit, (3) extruder housing, (5) feeding device.
140 C. Wang et al. / Polymer Testing 33 (2014) 138–144
Fig. 2. The structure of extruder housing: (1) backflow channel, (2) pressure
sensor, (3) conical twin-screw, (4) bypass valve, (5) temperature sensor, (6)
extrusion channel.
selected 20 data points that met the program’s required
stability criteria. Afterwards, the instrument would auto-
matically switch to the next speed point until the operating
program was over. In the second stage, the same program
ran again in the same way as in the first stage. Then, the
measured data were recorded to correlate steady-state
torque with rotation speed for polymer melts at the test
temperature. Generally speaking, it only took about 15 min
to finish the whole measurement with a speed range of 10–
105 r/min.
2.4. Torque measurements by MiniLab
There were two main steps for the determination of
steady-state torque of the material. In the first step, device
setup was carried out and the measuring procedure was
defined using the software. When the temperature reached
the set point, torque measurements without samples were
performed to obtain a relationship between torque and
rotation speed for calibration purposes. In the second step,
the torque measurements were done after the sample was
fed into the extruder and plasticized. The correlation of
steady-state torque with rotation speed was achieved via
calculating the data exported from the above two-step
measurements.
2.5. Choice of feed quantity
To choose a suitable feed quantity for torque measure-
ments, iPP (T30S) and HDPE (60550) with a dosage of 4–7 g
were used. The test was carried out under a dynamic speed
range of 10–105 r/min and the temperature was fixed at
190  C.
2.6. Choice of rotation speed
HDPE (6070 EA) with 6 g was selected as the sample and
three experiments were conducted as follows. Two samples
were separately plasticized for 5 min under a fixed speed of
50 r/min and 100 r/min, respectively, and another under a
dynamic speed range of 10–105 r/min. All the samples were
measured in the dynamic speed range of 10–105 r/min. The
temperature was set at 150  C for both plasticizing and
measurement.
2.7. Study on repeatability of torque data
Two polyethylenes, HDPE (6070 EA) and LDPE (18D)
with a feed quantity of 6 g, were chosen as test samples.
Plasticizing and measuring were done with a dynamic
speed range of 10–105 r/min. The temperature was set at
190  C for 6070 EA and at 150  C for 18D.
2.8. Study on reliability of torque data
HDPE (6070 EA) was chosen as test material with a
usage of 6 g. The comparison of steady-state torque
determined by the common fixed speed method was made
with that measured by the new dynamic speed test
method. In the fixed speed method, the test samples were
mixed for 8 min at speeds of 30 r/min, 50 r/min, 80 r/min
and 100 r/min. The torque values from 5 min to 8 min were
averaged to obtain the steady-state torques under different
rotation speeds. For the dynamic speed test method, after
being plasticized under a dynamic speed range of 10–105 r/
min, the sample was measured in the same speed range to
acquire the steady-state torques. The experimental tem-
perature in both methods was kept at 150  C.
3. Results and discussion
3.1. Torque calibration without samples
According to the instruction manual for the HAAKE
MiniLab, before beginning the measurement, motor torque
without material but with rotating screws must be cali-
brated to its torque zero point. It was found that the torque
calibration in the manual worked well for a fixed speed but
not for a dynamic speed test. Some torque values were not
always accurate over a wide rotation speed range. Hence in
this paper, we calibrated torque through subtraction on the
basis of the following.
Fig. 3 depicts the torque plotted against rotation speed
without samples in the MiniLab. It can be seen that there
is a linear relationship between torque and rotation speed
within a rather wide range of 5–205 r/min, which can be
expressed as y ¼ 0.0018*x þ 0.019, where x is the rotation
speed, y is the corresponding torque value. It should be
noted that the slope or intercept of the linear line might
vary slightly with the time passed. However, our MiniLab
instrument, after many years of usage, has consistently
demonstrated this linear relationship between torque
and rotation speed. The instrument’s performance
was not subject to atrophy that may apply to other
instruments.
Based on the above finding, we proposed a subtraction
approach to calibrate the torque of polymer melts. That is,
the real torque value was obtained by subtracting the tor-
que value without samples from the torque values with
samples. For any dynamic torque measurement, it was
necessary to preferentially establish the correlation of tor-
que with rotation speed without samples before beginning
the measurement. Thus, the real torque of polymer melts
could be obtained throughout the dynamic speed test
method.
 C. Wang et al. / Polymer Testing 33 (2014) 138–144 141

Fig. 3. Relationship of torque-rotation speed without samples.

3.2. Effects of feed quantity on torque measurements

The torque, by definition, is obviously dependent on the

amount of material used in a measurement. For the Mini-
Lab, the feed quantity needs to be suitable for obtaining a
consistent measuring torque value.
Fig. 4 outlines the effects of feed quantity on the steady-
state torque of T30S (a) and 60550 (b). It can be seen from
Fig. 4(a) that the torque of T30S significantly increased with
feed quantity varying from 4 g to 6 g at given rotation
speeds. When continuing to add up to 7 g, the steady-state
torque leveled off. It should be noted that the torque started
to fall with increased feed quantity from 6 g to 7 g at a
rotation speed of 105 r/min. The most probable explanation
of this trend was that the PP chains degraded with rotation
at such a high speed. Fig. 4. The relationship between steady-state torque and feed quantity to
As shown in Fig. 4(b) for 60550, it was also found that T30S (a) and 60550 (b).
the torque increased with the increased feed quantity from
4 g to 6 g. However, unlike T30S, the steady-state torque of
60550 was constant when the feed quantity was between repeatable and valuable data from torque measurements in
6 g–7 g, even at a high rotation speed of 105 r/min. This the MiniLab be obtained.
may be due to the better chain stability of HDPE than that of
PP. 3.3. Effects of rotation speed on torque measurements
The above results indicated that loads of ca. 6 g were
suitable for obtaining consistent torque values in the Steady-state torque depends, to an extent, on both
MiniLab. This is reasonable if the following calculation is plasticizing and measuring conditions, especially on the
considered. As bulk densities of PP and HDPE are about screw rotation speed. If samples are plasticized or
0.91 g/cm3 and 0.96 g/cm3, respectively, the volume of 6 g measured at a very high rotation speed, polymer chains can
sample could correspond to 6.6 mL for PP and 6.3 mL for be easily broken down, leading to a low torque value. If
HDPE at room temperature. When PP or HDPE is molten, samples are measured at a very low rotation speed, the
the polymer volume will expand somewhat. Since MiniLab torque may be too small to be accurately determined.
has a cavity of 7 mL volume, the feeding quantity of ca. 6 g Hence, there is an optimum rotation speed range for torque
polyolefin samples should completely fill the cavity, which measurements, in which the measured torque can accu-
leads to the maximum torque as expected. Therefore, the rately represent the rheological character of the material.
experimental results are in agreement with the theoretical Fig. 5 gives the steady-state torques of 6070 EA plasti-
calculations. cized under three different plasticizing conditions. It was
It should be mentioned that filling with 4–5.5 g of ma- observed that the torque-rotation speed curve of 6070 EA
terial, as suggested in the operating manual of MiniLab, was plasticized at a dynamic speed range of 10–105 r/min was
not suitable for torque measurements. Since the steady- in accordance with that plasticized at a fixed speed of 50 r/
state torque of polymer melts is strongly related to feed min, revealing that two plasticizing conditions could
quantity, it is important to determine the optimum quan- generate almost identical polymer melts with homoge-
tity for any unknown material. Only by doing that, can neous and stable states. However, for the sample
142 C. Wang et al. / Polymer Testing 33 (2014) 138–144
Fig. 5. The steady-state torque of 6070 EA plasticized under different rota-
tion speed.
plasticized at a fixed speed of 100 r/min, the torque-
rotation speed curve dramatically declined with
increasing speed as compared to that of other two samples.
This trend indicates that polymer chains had been greatly
degraded under that plasticizing condition.
Thus, from the above results, a dynamic speed range of
10–105 r/min was chosen for torque measurements. This
speed range was appropriate enough for the preparation of
samples with identical melt states. Therefore, the true
torque values can be obtained within a relatively wide
speed range.
3.4. Evaluating the repeatability of torque data
Repeatability of measured data must be a primary cri-
terion of how well an instrument works. Fig. 6 shows the
torque-rotation speed curves of 6070 EA measured at
different times (on March 23, May 17 and June 6 of 2012,
respectively). It can be seen that, although there was a
small deviation of data at the speeds of above 80 r/min, the
highest standard deviation was only 2.15% (at a speed of
Fig. 6. Torque-speed curves of 6070 EA measured at different times.
Fig. 7. Torque-speed curves of 18D measured in three consecutives.
105 r/min). Therefore, the data repeatability was very good
for the same samples tested at different times. The results
also indicated that the working state of MiniLab was very
stable.
Fig. 7 shows the relationship between torque and rota-
tion speed of 18D measured on three consecutive tests after
being plasticized at 150  C. The torque curve in the first test
was almost completely overlaid with that in the second
test. In the third test, it started to decline slightly, probably
due to degradation of LDPE chains with time at high tem-
perature. The results demonstrated that the data repeat-
ability was also very good for the sample tested in the first
two replicates after the sample was plasticized.
In general, if test temperature and dynamic speed range
are well set up to minimize the degradation of polymer
chains, we can always get repeatable torque measurements
for any sample by MiniLab.
3.5. Evaluating the reliability of torque data
Data reliability is critical for a measuring method.
Although the measurements were obtained quickly, the
Fig. 8. Torque measurements of 6070 EA under fixed speed.
 C. Wang et al. / Polymer Testing 33 (2014) 138–144
Fig. 9. Torque measurements of 6070 EA under dynamic speed.
reliability of the torque data was not compromised. Fig. 8
exhibits the variation of torque with time for 6070 EA
under the fixed speed test method. It can be seen from
Fig. 8 that, after feeding the sample, the torque values
under each fixed speed from 30 r/min to 100 r/min all
changed with time in the first 5 min. Thereafter, they
reached equilibrium values up to 8 min. As expected, the
steady-state torques increased with increase of rotation
speed. It is important to note that, if the sample is added
into the extruder cavity all at once, the feed path becomes
obstructed. Thus, the sample was divided into two portions,
resulting in two peaks on the graph.
The dynamic speed test method includes plasticizing
and measuring stages. After the plasticizing stage, the
sample becomes a homogeneous and stable melt. Thus, the
torque of a sample quickly reaches an equilibrium value
when the rotation speed changes from one speed to
another. Fig. 9 describes the variation of torque with time in
the measuring stage, by which the steady-state torques
were directly measured with 10 separate rotation speeds.
Please note that only one sample was used in the method
and the steady-state torques could be obtained for 10
different rotation speeds within no more than 15 min.
Fig. 10. Comparison of two methods.
143
Fig. 10 presents the comparison of the steady-state
torques determined by the two methods. It can be seen
that, except at high rotation speed where the torque
measured by the dynamic method was slightly higher than
that determined by the fixed speed method (due to small
degradation of polymer chains), all of other torque data
results were in agreement with each other. This revealed
that these two methods for steady-state torque measure-
ments worked very well in MiniLab. However, the dynamic
speed method had advantages over the common fixed
speed method because of time and cost savings, as well as
achieving accurate data and minimum degradation of
polymer chains.
4. Conclusions
We proposed a novel method for determination of
steady-state torque of polymer melts using the features of
the MiniLab instrument. The torque was calibrated by
subtracting that without material. The optimum feed
quantity of ca. 6 g and a dynamic speed range of 10–105 r/
min were determined for torque measurements of poly-
olefin samples. The data repeatability was evaluated by
measuring the same samples separately at different times
or with sample replicates. The data reliability was
confirmed by comparing the new method with the com-
mon fixed speed method for steady-state torque mea-
surements. The results showed that the dynamic speed test
was a direct, effective and rapid method for the determi-
nation of steady-state torque of polymer melts by MiniLab.
The torque data obtained were repeatable and reliable.
Moreover, the new method had a remarkable time and cost
savings as compared to the conventional method. The
correlation of steady-state torque with rotation speed was
generally considered as a rheological curve for polymer
melts. This promises great potential in academic research
and industrial applications.
References
[1] J.E. Goodrich, R.S. Porter, A rheological interpretation of torque-
rheometer data, Polymer Engineering and Science 7 (1967) 45–51.
[2] L.L. Blyler, J.H. Daane, An analysis of brabender torque rheometer
data, Polymer Engineering and Science 7 (1967) 178–181.
[3] G.C.N. Lee, J.R. Purdon, Brabender viscometry: I. Conversion of
Brabender curves to instron flow curves, Polymer Engineering and
Science 9 (1969) 360–364.
[4] J.G. Mallette, R.R. Soberanis, Evaluation of rheological properties of
non-newtonian fluids in internal mixers: an alternative method
based on the power law model, Polymer Engineering and Science 38
(1998) 1436–1442.
[5] E. Freire, O. Bianchi, E.E.C. Minteiro, et al., Processability of PVDF/
PMMA blends studied by torque rheometry, Materials Science and
Engineering: C 29 (2009) 657–661.
[6] X. Wang, X.Y. Chen, W.C. Yu, et al., Applications of rheological
torque-time curves to the study of thermooxidative degradation of
polypropylene powder, Journal of Applied Polymer Science 105
(2007) 1316–1330.
[7] O. Breuer, H.B. Chen, B. Lin, et al., Simulation and visualization of
flow in a new miniature mixer for multiphase polymer systems,
Journal of Applied Polymer Science 97 (2005) 136–142.
[8] V. Nassehi, M.H.R. Glloreishy, Modeling of mixing in internal mixers
with long blade tips, Advances in Polymer Technology 20 (2001)
132–145.
[9] L. Stradins, T.A. Osswald, Predicting the effect of viscosity ratios on
the mixing of polymer blends using the boundary element method,
Polymer Engineering and Science 36 (1996) 979–984.
144 C. Wang et al. / Polymer Testing 33 (2014) 138–144
[10] T. Avalosse, M.J. Crochet, Finite-element simulation of mixing: 2.
Three-dimensional flow through a kenics mixer, AIChE Journal 43
(1997) 588–597.
[11] H.E. Burch, C.E. Scott, Effect of viscosity ratio on structure evolution
in miscible polymer blends, Polymer Engineering and Science 42
(2001) 7313–7325.
[12] C.H. Yao, Z.I. Manas, R. Regalia, et al., Distributive mixing in variable
intermeshing clearance mixers: simulation and experiments, Rub-
ber Chemistry and Technology 71 (1998) 690–708.
[13] A. Marquez, J. Quijano, M. Gaulin, A calibration technique to eval-
uate the power-law parameters of polymer melts using a torque-
rheometer, Polymer Engineering and Science 36 (1996) 2556–2563.
[14] B.J. Cheng, C.X. Zhou, W. Yu, et al., Evaluation of rheological pa-
rameters of polymer melts in torque rheometers, Polymer Testing
20 (2001) 811–818.
[15] T. Weber, M.G. Oliveira, et al., Processability of revulcanizable SBR
compositions, Polymer Bulletin 61 (2008) 217–224.
[16] S.C. Liu, L.N. Lu, Melt rheological properties of reactive compatibi-
lized HDPE/PET blends, Journal of Applied Polymer Science 108
(2008) 3559–3564.
[17] A.Q. Zhang, L.S. Wang, Y.Y. Zhou, A study on rheological properties
of carbon black extended powdered SBR using a torque rheometer,
Polymer Testing 22 (2003) 133–141.
[18] L. Adragna, F. Couenne, P. Cassagnau, et al., Modeling of the complex
mixing process in internal mixers, Industrial & Engineering Chem-
istry Research 46 (2007) 7328–7339.
[19] W. Yang, Z.Y. Liu, G.F. Shan, et al., Study on the melt flow behavior of
glass bead filled polypropylene, Polymer Testing 24 (2005) 490–
497.
[20] S. Migneault, A. Koubaa, F. Erchiqui, et al., Effect of fiber length on
processing and properties of extruded wood-fiber/HDPE compos-
ites, Journal of Applied Polymer Science 110 (2008) 1085–1092.
[21] Y.J. Xu, W.J. Brittain, C.C. Xue, et al., Effect of clay type on
morphology and thermal stability of PMMA-clay nanocomposites
prepared by heterocoagulation method, Polymer 45 (2004) 3735–
3746.
[22] A. Walther, K. Matussek, A.H.E. Müller, Engineering nanostructured
polymer blends with controlled nanoparticle location using Janus
particles, ACS Nano 2 (2008) 1167–1178.
[23] S.C. Wong, A. Baji, Fracture strength and adhesive strength of
hydroxyapatite-filled polycaprolactone, Journal of Materials Sci-
ence: Materials in Medicine 19 (2008) 929–936.
[24] Y. Sabba, E.L. Thomas, High-concentration dispersion of single-wall
carbon nanotubes, Macromolecules 37 (2004) 4815–4820.
[25] O. Valentino, M. Sarno, N.G. Rainone, et al., Influence of the polymer
structure and nanotube concentration on the conductivity and
rheological properties of polyethylene/CNT composites, Physica E:
Low-dimensional Systems and Nanostructures 40 (2008) 2440–
2445.
[26] A. Loiseau, J.F. Tassin, Model nanocomposites based on laponite and
poly(ethylene oxide): preparation and rheology, Macromolecules 39
(2006) 9185–9191.
[27] W.E. Dondero, R.E. Gorga, Morphological and mechanical properties
of carbon nanotube/polymer composites via melt compounding,
Journal of Polymer Science Part B: Polymer Physics 44 (2006) 864–
878.