Polymer 82 (2016) 181e189

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Polymer
journal homepage: www.elsevier.com/locate/polymer

Strain sensing, electrical and mechanical properties of polycarbonate/

multiwall carbon nanotube monofilament fibers fabricated by melt
spinning
€tschke a, *, Harald Brünig a, Gert Heinrich a, b

Roberto Bautista-Quijano a, b, Petra Po
Jose
a
Leibniz-Institut für Polymerforschung Dresden e.V. (IPF), Hohe Str. 6, 01069 Dresden, Germany
b
Technische Universita €t Dresden, Institut für Werkstoffwissenschaft, 01062 Dresden, Germany

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

Article history: Polycarbonate (PC)/multiwall carbon nanotube (MWCNT)/composites were prepared by melt mixing and
Received 18 August 2015 subsequently melt spun to monofilament fibers. Electrical, mechanical and piezoresistive (strain sensing)
Received in revised form properties of the fibers were evaluated as a function of the MWCNT weight concentration, which was
9 November 2015
varied up to 6 wt%. After the incorporation of MWCNTs, a decrease in electrical resistivity of the fibers
Accepted 13 November 2015
Available online 1 December 2015
was found for MWCNT concentrations as low as 2 wt%. Furthermore, an important effect of the draw
down ratio (DDR) on the electrical properties of the fibers was observed. While the electrical percolation
threshold (4c) for the bulk material was <1 wt% and ~1 wt% for the undrawn-extruded rods, for the melt-
Keywords:
Carbon nanotubes
spun fibers 4c was found to be highly dependent on the DDR. Stiffness and offset yield stress of the
Polymer fibers MWCNT/PC fibers were increased starting with the addition of 1 wt% of MWCNTs. However, decreased
Piezoresistivity spinnability was observed for fibers with MWCNT concentrations above 4 wt%. The coefficient that re-
Strain sensing lates the electrical resistance changes to the mechanical strain (strain gage factor SGF) was estimated for
Melt spinning fibers with MWCNTs amounts that range from 3.5 to 6 wt%. The highest SGF ~16 was found at 3.5 wt% and
the lowest SGF ~2.5 at 6 wt% MWCNT. Smart multifunctional textiles, made from such conductive fibers,
have wide applications such as structural health monitoring, detection of gases and liquids, sensor arrays
and flexible sensors.
© 2015 Elsevier Ltd. All rights reserved.

1. Introduction 1.1. Current strain sensing technology

The fast growth of technological needs has led to the develop-
ment of new functional materials with enhanced properties such as
sensing capabilities. It is well known that the addition of multiwall
carbon nanotubes (MWCNTs) improves electrical and mechanical
properties of polymeric materials [1e3]. For this reason CNTs have
been extensively studied for the fabrication of nanocomposites
with several potential applications [4e6]. Furthermore, the addi-
tion of MWCNTs has been proven to provide polymers with sensing
capabilities [7,8]. The versatility of CNT/polymer composite sensors
has been reflected recently by its multiple uses for sensing liquids
[9], gases [10], chemicals [11], pressure [12], force [13], strain as
well as for structural health monitoring [14].
* Corresponding author.
€tschke).
E-mail address: poe@ipfdd.de (P. Po
Specifically in the case of strain sensing and structural health
monitoring there are already some commercial technologies
available. A short summary of some of them will be given next.
Metallic/semi-conductive strain-gauges (MSGs) are probably the
most widely used sensors. However, due to their morphology and
shape, placing the sensor is a key factor which in complex struc-
tures would require a lot of interconnected MSG arrays with a
tendency for experimental results to be misinterpreted. Other types
of mechanical strain measuring devices are extensometers. They
are very accurate and reliable, although mounting them in complex
structures is impossible in practice; this technology is more suitable
for laboratory conditions. Using strain sensors made of magnetic
film deposited on copper wires (MFCW) is a good approach because
it can be easily placed onto nearly any structure. However, it re-
quires a secure and direct electrical connection to provide a mag-
netic excitation. Fiber optic sensors have the same advantages as
MFCW. Most of them work using the fiber Bragg grating principle

http://dx.doi.org/10.1016/j.polymer.2015.11.030
0032-3861/© 2015 Elsevier Ltd. All rights reserved.
182 J.R. Bautista-Quijano et al. / Polymer 82 (2016) 181e189
which is very accurate. This kind of sensor however, has the same
limitation as MFCW and also is highly sensitive to transverse strains
and temperature. Another type of strain sensor available is the
piezoelectric transducer embedded in miniaturized integrated cir-
cuits. Even when placing them in complex structures they are
reliable and robust. Unfortunately, this type of sensor demands
expensive and complex manufacturing processes, as well as so-
phisticated instrumentation and data acquisition to interpret the
electrical signals. In addition to all these drawbacks, the cost of all
the above described devices is high, and their performance is still
not optimal.
1.2. Polymer based strain sensors
An interesting approach for strain sensing applications is the use
of composite materials filled with carbon fillers. Due to the excel-
lent viscoelastic properties of polymers and their processing
versatility, carbon particle filled polymers have been widely studied
for their use as strain sensors. It is possible to know the strain
sensitivity of composite materials by quantifying the changes in
their electrical resistance upon a mechanical stimulus (e.g. tension
or compression), a phenomenon known as piezoresistivity. The
sensitivity magnitude is commonly referred as the gauge factor
(SGF) and it is the quotient between the relative resistance change
(DRrel ¼ (RactualRinitial)/Rinitial in %) and the applied mechanical
strain (Dε in %). Murugaraj et al. reported a maximum SGF of ~7 on
polyimide films filled with 1.5e8 vol% carbon nanoparticles upon
tensile stress [15]. Luheng et al. found a direct relationship between
the carbon black (CB) weight concentration and the piezoresistivity
of silicon rubber composites which is related to the number of
effective conductive paths [16]. Kim et al. evaluated piezoresistivity
on epoxy/graphene composites finding SGF as high as 11.4 within
the range of 1000 micro-strain (i.e. the strain producing a defor-
mation of 1000 parts per million) [17]. Polymer/MWCNT compos-
ites have been also widely evaluated as strain sensors showing to be
a very promising alternative for future commercial applications
[18]. Nevertheless, the kind of polymer, shape, morphology and
design of the CNT composite play also a very important role in
strain sensing and structural health monitoring materials devel-
opment. Dog-bone samples made from CNT reinforced thermosets
like vinyl ester resins have proven to provide very accurate sensing
and detection of the elastic and plastic regimes upon compression
[19]. However, the electrical response shows a nonlinear and non-
monotonic behavior which makes it difficult to transfer it to prac-
tical applications. Rein et al. proposed a sensor made from MWCNT
buckypaper (BP) for measuring strain onto an epoxy dog-bone
sample [20]. The BP sensor was shown to be very accurate and
sensitive, yet high amount of nanotubes are needed to fabricate a
BP. A multilayer polyelectrolyte/carbon nanotube composite of
single-walled CNTs (SWCNT) prepared by a layer-by-layer assembly
method onto a polyvinyl alcohol substrate has been evaluated by
Loh et al. [21]. They found that increasing the CNT concentration
used to form each layer as well as increasing the number of layers
improves the sensing properties of the composite. On the other
hand, elastomer polyurethane/MWCNT films have the advantage to
withstand and sense strains as large as 400% [22,23]. Subramani
et al. proposed the use of a flexible strain sensor made of poly-
chloroprene rubber with an ionic liquid (IL)-modified MWCNTs
that combines the advantages of high stretchability of the rubber
with high conductivity of the IL-MWCNTs [24]. More recently,
Tadakaluru et al. proposed a strain sensor made of MWCNT/
graphite powder deposited onto the surface of a pre-stretched
natural rubber film [25]. They achieved very accurate reproduc-
ibility. Over 400 loading cycles for a strain range of 150%e500% and
a maximum strain measurement capacity of 620% limited by the
natural rubber substrate. These polymer composite based sensors
seem to be very favorable for measuring strain, similar to some of
the commercial strain sensors which have the disadvantage of not
being able to be freely placed in complex assemblies or in long
structures such as beams, pipes, columns, etc.
1.3. Non-polymer fibers and their composites for strain sensing
Even when the previously described composites seem to be a
good alternative for strain sensor fabrication, fibers have the
advantage of being more flexible than bulk materials, as well as
they can be woven together with other fibers for smart textile
fabrication. Additionally, they can be fabricated as very long fibers.
Thanks to these advantages the fibers are easier to place in any kind
of structure with all kind of shapes and lengths. Hence, fibers with
piezoresistive properties offer a very promising approach for sensor
fabrication. Nevertheless, as is the case for bulk materials the
processing technique and conditions are key factors for the final
properties of the fiber sensor. Several studies have reported the
performance of fibers as strain sensors, though the majority of
published work is based on non-polymer fibers.
By using carbon filaments (0.15 mm of diameter and length
>100 mm) embedded into polyether sulfone, Shui et al. were able to
accurately measure strain below 1% under cyclic loadings [26].
Embedded fiber optic sensors into concrete beams subjected to
tension and flexure has been reported by Belarbi et al. finding that
the sensor can keep working even beyond the beam break [27]. For
a hybrid material made from carbon fiber (CF)/CNT/epoxy com-
posite Lee et al. found that the composite had a better sensing
performance when adding CNTs than when using CF alone [28].
More recently Boehle et al. made a strain sensor for structural
health monitoring by using glass fiber (GF) with CNTs and carbon
nanofibers grown on the GF surface finding that the fiber can follow
the true mechanical strain and has a SGF similar to that of
commercially available MSGs [29]. Similar findings were obtained
by Gao et al. for GF coated with MWCNT by dip-coating [30].
1.4. Polymer fibers for strain sensing
All the previously described works show the great effort to
achieve accurate and reliable sensor materials consisting either of
glass or carbon fibers or polymer composites made there from.
However, polymeric fibers can be regarded are much more versatile
as their properties can be fine-tuned by the choice of conductive
fillers, amounts and filler combinations and their geometries. The
published work on the use of polymer fibers as strain sensors is
rare. In a study by Denis-Lutard et al., MWCNT/polyvinyl alcohol
wet-spun fibers exhibited an approximate strain sensitivity of 1.5
Ucm/% of strain [31]. This illustrates that polymer/MWCNT fibers
are good candidates for strain sensing applications. In studies by
Mattmann et al. filament fibers made from styreneeethylene/
butyleneestyrene (SEBS)/CB could be used to successfully measure
in-situ the deformation of a textile [32]. However, 50 wt% of filler
was needed to achieve suitably high conductivity values in the
SEBS/CB filaments for accurate sensing. These filaments were
fabricated using a capillary rheometer and had thicknesses in the
range of 300e315 mm. Interestingly, Melnykowycz et al. found that
the performance of self-prepared SEBS/CB monofilaments is better
than that of a commercial filament Merlin® made of carbon
impregnated rubber. They found that melt-spinning the polymer
together with CB enables higher sensing capability achieving SGF up
to 19 for fibers with 50 wt% of CB as compared to the SGF of com-
mercial strain gauges which is around 2 [33,34].
At present, commercially available strain sensor fibers are very
limited and commercial melt-spun fibers as strain sensors are not
 J.R. Bautista-Quijano et al. / Polymer 82 (2016) 181e189 183

yet in the market. On the other hand, melt spinning has been
shown to be efficient suitable technique for the fabrication of
conductive fibers made from polymers filled with MWCNTs
[35e39]. It is also known that a lower amount of MWCNT is needed
to achieve the same or higher conductivities as compared to other
traditional conductive fillers, like CB. Having polymer/MWCNT fi-
bers with sensing capabilities enables the fabrication of smart
multifunctional textiles. Through their versatility, smart multi-
functional textiles have wide applications such as strain sensing,
structural health monitoring, detection of gases and liquids, flexible
sensors and many more. However, the properties (e.g. strain
sensing, electrical resistivity, etc.) and behavior of MWCNT/poly-
mer composite fibers are not completely understood and further
research is needed.
In this work, commercially available MWCNTs were incorpo-
rated into polycarbonate (PC) by melt mixing, and subsequently,
MWCNT/PC fibers were fabricated by melt-spinning in a piston-
type spinning device by varying the spinning conditions, espe-
cially the draw down ratio. Electrical, mechanical, and strain
sensing (piezoresistivity) properties of these fibers were evaluated
as a function of the MWCNT concentration (1e6 wt%) and spinning
conditions.

2. Experimental

2.1. Materials and fiber fabrication

Fig. 1. Schema of the piston type spinning device, constructed at IPF.

Commercially available MWCNTs (Nanocyl™ NC7000; Nanocyl
S.A., Belgium) as powder and polycarbonate (Makrolon® 2205;
Bayer MaterialScience AG, Germany) were melt-mixed in a DSM
microcompounder at 280  C for 5 min using a screw speed of
250 rpm. Dried PC pellets (100  C, 8 h) and MWCNT powder were
manually mixed and then added to the running compounder. The
MWCNT weight concentration was varied from 1 to 6 wt%. Prior to
spinning, the pelletized composite material obtained from
microcompounding was dried again in the vacuum oven at 100  C
for 8 h. Melt-spinning was carried on a piston-type spinning de-
vice (Fig. 1) constructed at IPF with a spinneret die hole diameter
of 0.6 mm.
A melt temperature of 280  C was used and the pellets were pre-
heated for 5 min in the barrel before spinning. Different through-
puts (0.47e1.17 cm3/min) and take-up velocities (20e800 m/min)
were used and selected according to the homogeneity obtained on
the fibers [36]. By varying the throughput and take-up velocity
different draw dawn ratios were obtained. The draw dawn ratio
(DDR) can be defined as [40],
2.2. Characterization of the state of nanotube dispersion
Light microscopy photographs were taken in transmission mode
using a BH2 microscope combined with a DP71 camera (Olympus
Deutschland GmbH, Germany) of the melt-mixed MWCNT/PC
extruded strands for investigating the state of nanotube dispersion
before melt-spinning. For this, thin cuts with a thickness of 10 mm
were prepared using a glass knife perpendicular to the extrusion
direction. From each of the images, the agglomerate area ratio (A/
A0) was determined. This is the ratio of the cumulative area of the
projected MWCNT agglomerates (A) to the total area of the
micrograph (A0) and was calculated using the digital image pro-
cessing software ImageJ on Analyze Particles mode. A minimum of
10 thin cuts per sample was used for this dispersion analysis.
2.3. Resistivity measurements

DDR ¼ vL =v0
(where vL ¼ velocity of the fiber at the winder and v0 ¼ velocity at
the die).
According to the law of conservation of mass and the continuity
equation the throughput can be expressed as,

.  a Weber hot press (Model PW EH, Paul Otto Weber GmbH, Ger-
Throughput ¼ p 4D20 *v0
(where D0 ¼ diameter of the die hole).
Thus, the DDR can be calculated by using the following equation,
DDR ¼ ðtake  up speed=throughputÞ*Ac
(where Ac ¼ cross sectional area).
For further discussions only the DDR will be referred hereafter.
(1) In order to evaluate the effect of the processing conditions
during spinning on electrical resistivity (r) of the MWCNT/PC
composites, r was measured on melt-mixed compression molded
samples and on melt-spun fibers. The pelletized extruded strands
from melt-mixing were compression molded at 280  C for 2 min
into circular plates of 60 mm diameter and 0.5 mm thickness using
(2) many). Electrical resistivity was measured using a Keithley elec-
trometer 6517A combined with a Keithley 8009 test fixture for
resistances higher than 107 U on disc shaped samples (triangles in
Fig. 4). For resistances lower than 107 U strips with the dimensions
30  3  0.5 mm3 were measured using a four-point probe (squares
(3) in Fig. 4) [41].
In order to have a first approach on the r of the fibers, in a first
set the electrical resistivity was measured on composites contain-
ing 1 wt% of MWCNT with DDRs varying between 30 and 480 and
184 J.R. Bautista-Quijano et al. / Polymer 82 (2016) 181e189
Fig. 2. Schema of the measuring set-up for piezoresistive testing of fibers.
compared to undrawn fibers and the compression molded samples.
Based on these results, a second set of fibers with more suitable
electrical properties and good spinnability produced at much lower
DDRs was fabricated and used for further characterizations; these
DDRs were 4.83, 6.02, 8.08 and 12.03. Electrical resistivity mea-
surements of the fibers were carried out on single PC/MWCNT fil-
aments with diameters ranging from ~15 mm (DDR ¼ 480) to
~250 mm (DDR ¼ 4.83). Electrical resistivity of the fibers was
measured using a Keithley 8002A test fixture for 60 mm long fibers
(circles in Fig. 4).
2.4. Mechanical and piezoresistive characterization of melt spun
fibers
Tensile tests on the fibers were carried out with a Zwick-Roell
universal testing machine and at least 5 specimens were evalu-
ated for each set of samples. The load cell, the test speed and
sample's length were 20 N, 5 mm/min and 95 mm, respectively. The
Fig. 3. Light microscopy of PC/MWCNT composites after melt-mixing (compression molded plates) for three different MWCNT weight concentrations together with the calculated
agglomerate area ratio A/A0.
free sample length was 35 mm (See Fig. 2). The offset yield stress
(soff) at 0.8% (namely, the stress at a strain offset of 0.8% in the
stressestrain curve) was obtained to evaluate the effect of the
addition of MWCNTs on the plastic yielding of the fibers.
Piezoresistivity tests were carried by measuring the change in
electrical resistance DRrel in-situ during tensile tests until sample
break. The same test conditions and specimen dimensions were
employed as for the mechanical characterization testing. The
changes in electrical resistance were measured using a Keithley
DMM 2001 electrometer applying software for data acquisition
with a sampling rate of 1s developed at IPF. The fibers were con-
tacted using electrically conducting silver paint and connected to
the measuring instrument with copper wires, as illustrated in Fig. 2.
3. Results and discussion
3.1. State of nanotube dispersion in the composites
The spinnability of composites is dependent on the homoge-
neity of the material, as agglomerates above a certain size may
cause breakage during the spinning process. Thus, the state of
dispersion of the melt-mixed composites was analyzed before
spinning using transmission light microscopy, as shown in Fig. 3.
For the 1 wt% MWCNT composite no larger agglomerates are seen.
The larger agglomerates start from 3.5 wt% MWCNT and become
larger as the wt% of CNTs increases. In order to quantify the quality
of dispersion in the MWCNT/PC composites, the agglomerate area
ratio (A/A0) was determined. All composites with amounts lower
than 3.5 wt% (also 2 and 3 wt%, not shown here) have similar
dispersion state as 1 wt%. The composite with 1 wt% shows a value
of A/A0 of 0.24% which increases to 0.75% for 3.5 wt% and 3.28% for
composites with 6 wt% of MWCNTs.
This shows that good dispersion was successfully achieved for
composites with low wt%. However, for composites with higher
 J.R. Bautista-Quijano et al. / Polymer 82 (2016) 181e189
MWCNT/PC (disc)
18
MWCNT/PC (strip)
16 MWCNT/PC as extruded (DDR = 1)
Log(ρ) (ρ in Ω cm)
MWCNT/PC fiber (DDR = 30)
14 MWCNT/PC fiber (DDR = 120)
12
MWCNT/PC fiber (DDR = 480)
10
8
6 bers with 6 wt% of MWCNTs and higher DDR than 4.83 could not be
4 continuous fibers. This may be related to the size of the
2
0
0.00 0.25 0.50 0.75 1.00 1.25
MWCNT concentration (wt%)
Fig. 4. Electrical resistivity of PC/MWCNT composites as a function of the MWCNT
concentration, sample set 1.
nanotube amounts there are still primary agglomerates remaining
after melt-mixing. This indicates that melt-spinning of composites
with higher MWCNT amounts may be more difficult, due to the
existence of agglomerates. It is expected that the melt-spinning
shaping step does not contribute to further nanotube dispersion
and that such agglomerates are also existent within the melt-spun
fibers.
3.2. Electrical resistivity of pressed plates and melt-spun fibers
When studying the strain sensing performance of conductive
composites, a certain low resistivity value r (about 50 MU cm) has
to be given in the sample before stretching. During stretching, in-
crease in resistance is expected which needs to be followed with
the electrometers applied. Thus, the electrical resistivity of the
initial samples was investigated in their different shapes, as shown
in Fig. 4 for the PC/MWCNT samples from set 1.
In the case of compression molded samples, a significant
decrease in r was found after the addition of 0.25 wt% MWCNT and
percolation occurs below 0.5 wt%. At the addition of 0.5 wt%, r
decreases by 13 orders of magnitude. On the other hand, melt-spun
fibers have significantly higher r depending on the DDR, as shown
for the 1 wt% samples. Even the extrudate taken from the spinning
device without winding (DDR ¼ 1) has higher r than the
compression molded sample. This suggests that the shaping pro-
cess of the composite material significantly influences the
morphology of the conducting MWCNT network and by that the
measured resistivity and the percolation threshold 4c of the
structures.
Consequently, 4c of the melt-mixed and compression molded
samples is below 0.5. For melt-spun fibers, 4c shows a dependency
on the DDR, as different MWCNT network structures are formed
depending on DDR. The main effect is an expected and confirmed
orientation of individualized MWCNTs and smaller agglomerates
while the composite is pushed through the spinneret hole. As
shown in TEM images of PC-MWCNT fibers, also prepared at
different take-up velocities [35], this is likely to happen along the
fiber axis on melt-spun fibers. Interestingly, the difference in r of
melt-spun fibers at DDR ¼ 30 and at DDR ¼ 480 is of only 2 orders
of magnitude while the difference in r of fibers at DDR ¼ 30 and
DDR ¼ 1 is of approximately 6 orders of magnitude. Additionally,
the r of fibers is already at the DDR of 30 higher than 109 U cm and
therefore not suitable for strain sensing applications. For this
185
reason, a second set of fibers with MWCNT contents varying from 1
to 6 wt% and DDRs lower than 30 was fabricated to identify DDRs
with suitable electrical resistivity for piezoresistive measurements
(Fig. 5).
As shown in Fig. 5, even for DDRs as low as 4.83 and 12.03 there
is an evident difference between the r of the corresponding fibers.
For instance, r of fibers with 2 wt% MWCNTs is 4 orders of
magnitude lower for DDR ¼ 4.83 than for DDR ¼ 12.03. After
increasing the amount of MWCNTs the difference in r decreases
though it is still visible until 5 wt%. It is worth mentioning that fi-
produced, as fiber breakage occurred preventing the generation of
agglomerates.
1.50
12
11
10
DDR = 12.03
Log (ρ) (ρ in Ω cm)
9 DDR = 8.08
8 DDR = 6.02
DDR = 4.83
7
6
5
4
3 ρ suitable for sensing
2
1
0 1 2 3 4 5 6
MWCNTconcentration (wt%)
Fig. 5. Electrical resistivity of MWCNT/PC fibers at different DDRs as a function of
MWCNT concentration, sample set 2.
3.3. Mechanical properties of melt spun fibers
The characteristic stressestrain curves of the PC/MWCNT fibers
for the evaluated DDRs are shown in Fig. 6. For easier comparison,
the scales are the same for all the graphs shown. Table 1 lists the
tensile properties of PC/MWCNT fibers with a DDR of 4.83. It should
be mentioned that the other DDRs evaluated (not shown in Table 1)
exhibited very similar trends to those shown in Table 1 for
DDR ¼ 4.83. It is evident from Fig. 6 and Table 1 that the addition of
MWCNTs has a strengthening effect on the polymer fibers. An in-
crease in the tensile strength (smax) is visible from the addition of
2 wt% of MWCNTs reaching a maximum of ~30% increase in fibers
with 6 wt%. Similarly, as seen from the magnitudes of the elastic
modulus (E) a stiffening effect was achieved as from the addition of
1 wt% reaching a reinforcement of ~50% for 6 wt% MWCNT/PC fi-
bers. However, it is also seen that the addition of MWCNTs reduces
the strain at break (εmax) of the fibers which is known to be typical
for particle filled polymers. Ductility of the fibers was decreased
upon increased MWCNT content as well as for lower DDRs. The
decrease in ductility with DDR was visible even for the neat PC fiber
where εmax was reduced from ~80% (DDR ¼ 12.03) to <40%. This
reduction in εmax was more pronounced after the addition of
MWCNTs. Interestingly, when comparing the tensile properties of
the fibers with different DDRs at the same amount of MWCNTs,
186 J.R. Bautista-Quijano et al. / Polymer 82 (2016) 181e189

80 DDR = 4.83 (ø = 260 ± 8 μm) DDR = 6.02 (ø = 234 ± 7 μm)

70
60

Stress (MPa)
50
PC neat PC neat
40 1% MWCNT/PC 1% MWCNT/PC
2% MWCNT/PC 2% MWCNT/PC
30
3% MWCNT/PC 3% MWCNT/PC
20 4% MWCNT/PC 4% MWCNT/PC
10 5% MWCNT/PC 5% MWCNT/PC
6% MWCNT/PC 6% Not spinnable
0
80 DDR = 8.08 (ø = 200 ± 5 μm) DDR = 12.03 (ø = 164 ± 7 μm)
70
60
Stress (MPa)

50
PC neat PC neat
40 1% MWCNT/PC 1% MWCNT/PC
30 2% MWCNT/PC 2% MWCNT/PC
3% MWCNT/PC 3% MWCNT/PC
20 4% MWCNT/PC 4% MWCNT/PC
10 5% Not spinnable 5% Not spinnable
6% Not spinnable 6% Not spinnable
0
0 10 20 30 40 50 60 70 80 90 0 10 20 30 40 50 60 70 80 90
Strain (%) Strain (%)

Fig. 6. Stress-strain curves of the PC/MWCNT fibers prepared at different DDRs; average diameter (ø) of the fibers are also shown.

Table 1
Tensile properties of PC/MWCNT fibers prepared at DDR ¼ 4.83.

MWCNT concentration (wt%)

0 1 2 3 4 5 6

E (GPa) 2.25 ± 0.02 2.35 ± 0.08 2.56 ± 0.04 2.58 ± 0.05 2.72 ± 0.04 2.98 ± 0.14 3.33 ± 0.17
smax (MPa) 60.3 ± 0.54 60.0 ± 1.48 64.8 ± 0.77 66.3 ± 1.07 69.4 ± 1.46 73.9 ± 6.31 77.2 ± 6.27
soff (MPa) 47.0 ± 0.69 50.3 ± 0.84 53.4 ± 1.27 53.6 ± 1.79 53.4 ± 1.24 57.6 ± 3.04 59.1 ± 2.64
εmax (%) 32.7 ± 11.0 24.1 ± 2.81 19.6 ± 4.25 28.7 ± 7.67 19.0 ± 2.69 6.88 ± 1.47 8.30 ± 0.84

mechanical reinforcement was more significant for fibers made
with lower DDR.
As can be seen from Table 1, an increase in soff of the fibers is
visible for all the wt% evaluated where a maximum of ~25% increase
was achieved for fibers with DDR ¼ 4.83 at 6 wt% MWCNTs. This
implies that the addition of MWCNTs has an important effect on
increasing the stress required to reach plastic deformation of the
fibers. These results are in accordance with Zetina-Herna
ndez et al.
who also found an effect on the polymer yielding after the addition
of 4e10 wt% of MWCNTs in compression molded polypropylene
dog-bone samples [42]. This phenomenon can be explained by the
wrapping of polymer chains around MWCNTs. These polymer-
MWCNT entanglements restrict the movement of the polymer
chains while they are subjected to tensile loading. Similarly, when
the MWCNT amount increases, the energy needed to overcome the
physical interactions (mainly van der Waals forces) between a
larger amount of MWCNT and polymer chains to reach the plastic
deformation during tensile test also increases. Likewise, the strain
at break is also affected since after the addition of MWCNTs the
strain at which breakage occurs is significantly decreased as a result
of the reduced mobility of the polymer chains.
It is also seen in Fig. 6 that reduced spinnability was found with
increasing MWCNT amount which also may be a consequence of
the reduced mobility of the polymer chains upon addition of
MWCNTs. In addition, the higher number of remaining primary
nanotube agglomerates seen after melt-mixing (Fig. 1) may also
contribute to breakage at lower strains. The fiber breakage was
more pronounced at larger DDRs where the size of the primary
agglomerates becomes more significant due to the reduced cross-
section of the fibers. At 6 wt% MWCNT loading, the largest ag-
glomerates seen in Fig. 1 are in the same size as the fiber diameters
of 164e260 mm. Thus, above DDR ¼ 6.02 the composite was not
spinnable anymore, which starts for samples with 5 wt% loading at
DDR ¼ 8.08. This indicates that improving dispersion could be a
major need to get better performing fibers. These findings are in
accordance with studies by Po €tschke et al. who found that the
addition of MWCNT into polylactid acid (PLA) in amounts above
percolation threshold leads to a significant reduction of flow
properties of the melt due to increased fillerefiller interaction [36].
They also found that the addition of 5 wt% of MWCNT into PLA
resulted in inhomogeneous fiber diameters which led to fiber
breakage.
3.4. Piezoresistive properties of melt spun fibers
Piezoresistive properties of MWCNT/PC fibers with r suitable for
sensing applications are presented in Fig. 7. The electrical response
of the piezoresistive samples during tensile tests is shown for PC/
MWNCT fibers produced at 4 different DDRs with MWCNT loadings
ranging from 3 to 6 wt%. The tests were carried out until sample
break.
As discussed in Section 3.2, not all the fibers were suitable for
the measurements of resistance changes. Additionally as discussed
in Sections 3.1 and 3.3, fibers could not be produced at high wt%
 J.R. Bautista-Quijano et al. / Polymer 82 (2016) 181e189 187

DDR = 4.83 DDR = 6.02

80
3% MWCNT/PC
60 3.5% MWCNT/PC 3% ρ was too high
ΔR/R 4% MWCNT/PC 3.5% MWCNT/PC
(%)
5% MWCNT/PC 4% MWCNT/PC
40 6% MWCNT/PC 5% MWCNT/PC
6% Not spinnable

20

0
DDR = 8.08 DDR = 12.03
80
3% ρ was too high
3.5% ρ was too high
60
3% ρ was too high 4% MWCNT/PC
ΔR/R0
3.5% MWCNT/PC 5% Not spinnable
(%) 6% Not spinnable
40 4% MWCNT/PC
5% Not spinnable
6% Not spinnable
20

0
0 2 4 6 8 0 2 4 6 8
Strain (%) Strain (%)

Fig. 7. Electrical response of PC/MWCNT fibers of sample set 2 during tensile testing for different DDRs. The vertical line in the plot of DDR ¼ 4.83 illustrates the strain limit of 1.8%
used for the calculation of SGF.

due to reduced spinnability resulting from remaining MWCNTs
primary agglomerates. Therefore, depending on their spinnability
and the achieved resistivity values, the piezoresistivity was only
characterized for fibers with 3 wt% and higher. In the case of the
highest DDR (12.03) only one weight concentration (4 wt%) could
be measured. In order to compare the strain sensing capabilities at
low wt%, a composite with a MWCNT amount of 3.5 wt% was
additionally prepared and studied.
From Fig. 7 it is visible that the electrical response increases
upon increasing strain. For instance, in average for fibers with
3.5 wt% MWCNTs and DDR ¼ 4.83 the electrical response continues
increasing until the samples break at about ~5.5% of strain. For fi-
bers with 4 wt% and 5 wt% (excepting DDR ¼ 8.08) the electrical
response reaches a maximum and then decreases slightly until
sample break which occurs between 4 and 5% strain depending on
the DDR. This behavior is due to the necking effect in the fibers
during stretching. Nevertheless, for fibers with 3.5 wt% of MWCNT
and DDR ¼ 6.02 the change in electrical resistance is as high as 80%
at 6% of strain, which is indicative of high sensitivity. Furthermore,
the difference in the strain sensitivity of fibers at DDR ¼ 4.83 with
composite films is less sensitive to the internal density and size of
CNT agglomerates than the electrical conductivity [47].
In order to quantify the strain sensitivity of the different
MWCNT/PC fibers, the gage factor (SGF) was calculated and is
shown in Fig. 8. The SGF was estimated as the slope in the range
from 0 to 1.8% strain from the characteristic DR/R0 vs. strain curves
(see vertical line on Fig. 7, DDR ¼ 4.83). As shown in Fig. 8, fibers
with higher DDRs have higher SGF and sensitivity shows a larger
decrease with the nanotube amount; while the fibers with the
lowest DDR have significantly lower SGF values which show a much
smaller decrease with nanotube amount. For instance, fibers with
3.5 wt% of MWCNT that were melt-spun at a DDR ¼ 8.08 have a SGF
three times larger (~16) than fibers with 4 wt% at the same DDR
18
16
DDR = 12.03
14 DDR = 8.08
DDR = 6.02
Gage Factor SGF(-)

3 wt% and 3.5 wt% is significant. There are several theories for the 12
working mechanisms in the piezoresistive nanocomposite strain DDR = 4.83
sensors. Among these, the most accepted are: (a) significant 10
changes in the conductive network structure formed by CNTs [43],
8
(b) changes in tunneling resistance between neighboring CNTs due
to distance change [44] and (c) piezoresistivity of CNTs themselves 6
due to their deformation [45]. For our case the first two are the
most relevant and likely to happen. This can be concluded from the 4
findings that melt-spinning promotes MWCNT orientation along
the fiber axis [35] and that it has been stated that the CNT
2
piezoresistive sensitivity has as a very small contribution (~5%) of 0
the whole piezoresistive effect of the composite [46]. It may be also 3 4 5 6
assumed that the internal density and size of the CNT agglomerates MWCNT concentration ( wt%)
have an effect on the piezoresistive properties of the fibers. How-
ever, Gong et al. found that the piezoresistivity of the CNT polymer Fig. 8. Gage factors SGF of the PC/MWCNT fibers at different DDRs as a function of the
MWCNT concentration.
188 J.R. Bautista-Quijano et al. / Polymer 82 (2016) 181e189
(~5). This indicates that the SGF is highly sensitive to the weight
concentration of the MWCNT and to the DDR employed to produce
the fibers.
This sensitivity of SGF on MWCNT wt% and DDR can be explained
when considering the MWCNT network structure within the fibers.
The change in electrical resistance upon elongation gets higher as
the nanotube concentration is closer to the electrical percolation
threshold concentration. The change is much lower if the MWCNT
amount is well above 4c. This is due to the fact that a less dense but
already existing conducting network inside the polymer is
deformed easily and some of the nanotubes are more easily
disconnected upon external stimuli and therefore the change in
electrical resistance is much larger as compared to composites with
higher density of conductive elements. In the latter, external
stimuli do not have a considerable effect on the density of
conductive pathways and, thus, on the electrical resistance. Similar
behavior was also found by Villmow et al. who studied liquid
sensing sensitivity on polycarbonate/MWCNT compression molded
composites and found higher sensitivity in conductive composites
with lower MWCNT amounts [48].
When drawing fibers the used DDR also modifies the perco-
lating network structure inside the polymer. As the DDR increases,
the nanotube orientation along the fiber increases leading to a less
dense network with more interrupted pathways as compared to a
nondrawn sample. Thus, 4c increases with DDR. At an actual CNT
concentration, the difference to 4c gets smaller with increasing
DDR.
Therefore, there is compromise between the strain sensitivity,
the MWCNT wt% and the DDR. The compromise is that the re-
sistivity has to be in a stable measurable range, and at the same
time high resistive samples always result in larger sensitivity.
It is worth mentioning that even the lowest SGF found in this
work (~2.5 for 6 wt% and DDR ¼ 4.83) is above the SGF of conven-
tional MSGs which generally is close to 2 [34]. The SGF's found in
this work are also higher than the ones found in literature for dog-
bone shaped thermoset samples and compression molded or so-
lution cast thermoplastic films [49e51]. For other polymer fibers,
similar SGF were only found after filling with ~50 wt% of CB [32,33]
which is much higher than the MWCNT contents used in this study.
4. Conclusions
Fibers made of PC with different MWCNT weight concentrations
were fabricated by melt-mixing and subsequent melt-spinning. It
was found that MWCNT are dispersed well in PC for composites
with low wt%. Higher amounts than 3 wt% resulted in the existence
of residual MWCNT agglomerates. MWCNT/PC fibers were suc-
cessfully melt-spun by varying the draw down ratio DDR by
changing throughput and take-up velocity. However, the presence
of agglomerates in the composite material starting at 3 wt%
MWCNTs significantly reduced the capability of the composites to
be melt-spun. As a consequence, it was not possible to produce
fibers with loadings of MWCNT higher than 5 wt% and DDR values
higher than 4.83. In mechanical testing, an increase in the stiffness
of the fibers was seen for all the wt% evaluated, as well as a
reduction in the strain at break. A relationship between the offset
yield stress of the fibers and the amount of MWCNTs was found
suggesting an effect on the polymer yielding due to the addition of
the MWCNTs. Mechanical reinforcement was more significant for
fibers made with the lower DDR evaluated (4.83).
Electrical percolation of melt-mixed PC/MWCNT compression
molded composites occurred below 0.5 wt% while for PC/MWCNT
fibers 4c was shifted to higher values dependent on the DDR used to
produce the fibers. There is a compromise between spinnability
(depending on state of nanotube dispersion) and suitable electrical
resistivity of the fibers. Piezoresistivity effects could be character-
ized only for fibers with MWCNT amounts of 3 wt% or higher. In the
case of the highest DDR (12.03) only one weight concentration
(4 wt%) could be evaluated. SGF was found to be very sensitive to the
amount of MWCNTs and to the DDR. Lower MWCNT wt% and
higher DDR led to higher SGF. The highest SGF found in this study
was ~16 for fibers with 3.5 wt% MWCNT prepared at a DDR of 8.08.
This value is promisingly high compared to commercial available
MSG having values in the range of 2.
For this kind of polymer based fiber strain sensors there is a
wide list of potential applications ranging from health monitoring
to robotics.
Acknowledgments
Author Bautista-Quijano wants to thank to The National Council
of Science and Technology of Mexico (CONACYT) and The National

n State
Council of Science, Innovation and Technology of the Yucata
(CONCIYTEY) for the financial support.
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