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Textile Research Journal Article

Negative Poisson’s Ratio Polyester Fibers


Naveen Ravirala, Kim L. Alderson,
Abstract Auxetic materials are referred to as Philip J. Davies, Virginia R. Simkins and
those having negative Poisson’s ratio (ν). Initial
work at Bolton successfully fabricated auxetic
Andrew Alderson1
Centre for Materials Research & Innovation, University of
polypropylene fiber using a novel thermal melt-
spinning technique. This paper reports in detail
Bolton, Deane Road, Bolton, BL3 5AB, UK
both the methods and principles involved in
screening polyester powder and also the manufac-
turing method for successful production of auxetic
polyester fibers. Videoextensometry along with
micro-tensile testing were used to measure the
Poisson’s ratio of the fiber. The Poisson’s ratio of
the polyester fiber was found to vary between –0.65
and –0.75.

Key words auxetic, negative Poisson’s ratio,


polyester fiber, videoextensometry

Auxetic materials when stretched axially expand instead of be limitations on the production of auxetic materials in the
contracting laterally. Following Lakes’s [1] successful pro- form of cylinders. In particular, the cylinders (having diame-
duction of auxetic foams, a variety of auxetic products have ters varying between 9 and 15 mm) were found to be unsuit-
been fabricated including honeycombs [2], polymeric and able for application-based research and were restricted to
metallic foams [1] and microporous polymers [3, 4]. An laboratory-based testing. Moreover, the process involved
interesting feature of auxetic materials is that they are pre- was not continuous and problems were envisaged in produc-
dicted [5], and have been found, to have enhanced proper- ing them on a large scale.1 2
ties. For example, it has been shown experimentally that More recently, a novel thermal processing technique-
the indentation resistance [6] of auxetic materials has been involving melt spinning has been employed to produce an
enhanced by up to four times when compared with the con- auxetic product in a more useful and usable form, namely
ventional equivalent. Other enhanced properties include as a fiber [15]. This has led to auxetic polypropylene (PP)
plane strain fracture toughness [7], energy absorption [8], fibers being fabricated in a continuous process. Videoex-
and shear modulus [9]. tensometry analysis was used to show the auxetic nature of
The first synthetic auxetic microporous polymer was a the PP fiber. The processing route developed for auxetic
particular form of polytetrafluoroethylene (PTFE) [10]. It polypropylene fibers is, in principle, flexible enough to be
was found that the auxeticity in this case was solely because adapted to produce other polymeric fibers [15] and films
of its complex microstructure [10]. This consisted of nodules [16] in auxetic form.
interconnected by fibrils that react co-operatively to pro- This paper reports in detail the production of auxetic
duce a negative Poisson’s ratio. Similar microstructures have polyester fiber, including the characterization by videoex-
also been engineered in polymers such as ultra-high-molecu- tensometry.
lar-weight polyethylene (UHMWPE) [3], polypropylene [4]
and nylon [11], which were all produced by a novel thermal
processing route consisting of three distinct stages; compac- 1
Corresponding author: Tel: +44 1204 903513; fax: +44 1204
tion [12], sintering [13] and ram extrusion [14]. The entire 903088; e-mail: a.alderson@bolton.ac.uk
process takes place in a specially designed extrusion rig 2
Part of this paper was presented at Second International
with extrudates produced in the form of cylindrical rods. Conference on Materials for Advanced Technologies & IUMRS –
Although having this special property, there were found to International Conference in Asia, Singapore, 2003.

Textile Research Journal Vol 76(7): 540–546 DOI: 10.1177/0040517506065255 www.trj.sagepub.com © 2006 SAGE Publications
Figures 1, 4–5, 8 appear in color online: http://trj.sagepub.com

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Negative Poisson’s Ratio Polyester Fibers N. Ravirala et al. 541 TRJ

Experimental Methods dried under a partial vacuum oven at 108°C temperature


for 2 days before extrusion.
Scanning electron microscopy (SEM) was employed to
Preliminary Characterization of Polyester characterize the polyester powder derived from grinding.
Granules Typically observations were made at approximately 200×
The polyester resin used in the fabrication of auxetic polyes- magnification. The micrographs of polyester powder were
ter fiber was poly (trimethyleneterephthalate [17] or 3GT) studied in depth not only to analyse the size distributions
supplied by DuPont in the form of granules. In order to but also to understand the surface roughness and shape.
establish the thermal processing window, it was necessary to UTHSCSA Image Tool v3 [19] was employed to analyse
obtain the thermal characteristics of the polyester granules the powder size distribution and the aspect ratio (calcu-
using differential scanning calorimetry (DSC). The DSC was lated as the ratio of the major axis to minor axis) using the
carried out by heating a small amount of polyester sample micrographs of polyester powder obtained from SEM.
(5.5 mg) under flowing nitrogen at 10 mL min–1. The heating
rate was maintained at 10°C/minute and the temperature
profile ranged from ambient (25°C) to 310°C. Figure 1 Extrusion of 3GT Polyester Fibers
shows the DSC curve displaying the onset temperature (the An initial extrusion experiment was carried out with 3GT
temperature at which the polymer just starts melting) at granules to observe the behavior of the polymer during
205°C, and the peak melting point at 229°C. From previous extrusion. The melt spinning process was performed using
results [18] this indicated that the processing window would an Emerson and Renwick Ltd Labline extruder which con-
occur at a particular temperature between the regions of sists of a 25.4 mm screw diameter, 3 : 1 compression ratio,
onset temperature and peak melting point. Therefore, the length/diameter 24 : 1, five temperature zones each having
processing temperature window was defined to be 210 and individual thermostatic controls, and a die slot with 40-fila-
230°C. Following the PP work, a flat profile across all the ment die having each hole size of 550 µm (Figure 2). The
zones of the extruder was employed. processing temperatures investigated were based on ther-
mal analysis studies and were carried out at intervals of
5°C, leading to flat temperature profiles in the range of 230
Polyester Powder Production to 210°C with screw speeds of 0.525 rad/s and take-up
The previously reported auxetic PP fibers were produced speed 0.075 m/s. The extrusion was carried out at higher
from finely divided powder particles. Thus there was a temperature (230°C) profile and gradually decreased the
need to obtain powder particles from the supplied polyes- temperature to 210°C until the viscosity of the powder bulk
ter granules prior to extrusion. The polyester granules was too high to allow free flow through the die-zone. The
were subjected to in-house cryogenic grinding using liquid polyester powder was fed through a hopper into the barrel
nitrogen. Ground polyester particles of less than 150 µm and transferred through the barrel zones to the die zone,
were collected to carry out the extrusion. thereby undergoing sintering due to the maintained tem-
The 3GT granules and powder required pre-drying to peratures along the zones of the extruder. The fibers were
avoid hydrolysis during extrusion. Therefore, 3GT granules extruded from the die head and cooled before winding.
(used during purging) along with 3GT powder were pre-

Characterization of Extruded Fibers


Figure 3 shows the load–elongation data of a typical fiber.
Samples were tested for auxeticity by deforming them to
1% strain, thus not exceeding the elastic limit of the fibers.
Characterization of the extruded fibers was carried out by
using videoextensometry and microtensile testing equip-
ment. Figure 4 shows a schematic of the videoextensometer
and microtensile testing stage. The camera of the videoex-
tensometer was mounted vertically above the microtensile
stage to capture the image of the fiber. The PC1 attached to
the microtensile unit processes the load–extension data
from the microtensile stage fitted with a 77 N load cell. The
PC2 attached to the videoextensometer records the changes
in length and width of the fiber during the test. Polyester
fibers cut to lengths of approximately 10 mm, marked with
Figure 1 DSC curve of polyester powder. two small markers at a distance of approximately 1 mm
apart along the length of the fiber, were mounted between

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TRJ 542 Textile Research Journal 76(7)

Figure 2 Schematic diagram of


melt extruder used to produce
auxetic polyester fiber.

the two clamps of the microtensile tester. Figure 5 shows a


typical sample with the fiducial markers attached. Each of
the tests included mounting the sample between the jaws of
the microtensile stage and cyclically applying and removing
a load (up to four cycles). A strain rate of 0.1 mm/minute
was employed with load applied until a maximum strain of
1% was reached. The videoextensometer operates directly
as a strain meter by tracking the displacement of the edges
of the sample as defined by a contrast change in the video
image at the edges of the attached targets (length) or fiber
edges (width) caused by mechanical strain to the specimen.
During the test, the marked length was divided into ten
regions by the videoextensometer and the individual width
of each was recorded.
Figure 3 Single test load–elongation curve of polyester
fiber.

Figure 4 Videoextensometer set-


up.

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Negative Poisson’s Ratio Polyester Fibers N. Ravirala et al. 543 TRJ

Figure 5 Typical sample with fidu-


cial markers for videoextensome-
tery analysis.

Results extruder set up and was commensurate with the size distri-
bution required to form an optimum network microstruc-
ture.
Polyester Powder Characterization
Figure 6 shows a SEM micrograph of the ground polyester
Measurement of Poisson’s Ratio
powder. The aspect ratio of the powdered particles was
found to vary between 1.5 and 2, with a typical particle Figure 7a shows four cycles of length and width data
dimension of 50 µm in the minor axis and 100 µm in the obtained for a conventional (analogue) polyester fiber pro-
major axis. It was also observed that the particles had a duced at 230°C with screw and take-up speeds at 0.525 rad/
rough surface. Hence, this particular polyester powder second and 0.075 m/second, respectively. It was observed
resembled the powder used in the successful production of that the length and width data were out of phase by 180°,
auxetic PP fibers and cylinders in terms of aspect ratio and clearly showing that the width decreased as the length
morphology. From previous results [20], the size of pow- increased in response to the applied force along the length
der particles was small enough to be processed in the of the fiber. Similarly, the width increased as the length
decreased as the applied tensile load is removed. This
fiber, therefore behaved in a conventional (positive Pois-
son’s ratio) manner.
However, the fibers produced at 225°C with screw speed
0.525 rad/second and take-up 0.075 m/second were found to
have in-phase length–width data (see Figure 7b). It can be
observed that the width increased as the length increases in
response to the applied force along the length of the fiber.
Similarly, the width decreased as the length decreased on
removal of the tensile load. Thus the fiber was confirmed to
be auxetic.
The true axial and lateral strains were calculated from
the length–width data obtained from the videoextensome-
ter. The true axial strain (εx) and true lateral strains (εy) are
given by

 l
ε x = ln  --- (1)
 l 0

 w
Figure 6 SEM micrograph of polyester powder. ε y = ln  ------ (2)
 w 0

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TRJ 544 Textile Research Journal 76(7)

Figure 8 True lateral vs true axial strain data or auxetic


and conventional polyester fibers.

Discussion
Herein the successful extension of the range of polymers
that can be made in auxetic fiber form to include polyester
is reported.
During the course of polyester extrusion, work was car-
ried out with screw speed and take-up values that were pre-
Figure 7 Width–length data for polyester fibers proc- viously employed for the successful production of auxetic
essed with screw speed of 0.525 rad/second, take-up PP fibers. However, the viscosity of the extruded fibers was
speed of 0.075 m/second and flat temperature profiles of too low to wind them with the take-up speed of 0.03 m/sec-
(a) 230°C and (b) 225°C. ond while maintaining the same screw speed of 1.05 rad/
second. The main approach for the production of auxetic
fibers lies in maintaining the minimum draw ratio. The
minimum take-up speed maintained in the course of extru-
where, l0 and w0 are the original length and width of the sion was found to have direct impact on screw speed. It was
fiber, respectively, and l and w are the deformed length found that the optimum processing conditions for extru-
and width of the fiber, respectively. sion could be obtained by reducing the screw speed to
Figure 8 shows the true lateral strain against the true 0.525 rad/second. Further reductions in the screw speed
axial strain from the third extension phase for both the were found to be inappropriate to the production of auxe-
auxetic and conventional polyester fibers. The auxetic pol- tic polyester fibers. By extensive experimentation, it was
yester fibers, produced at 225°C with screw speed 0.525 found that the minimum take-up speed with which the
rad/s and take-up 0.075 m/s, were found to possess Pois- extrusion of fibers would be successful was 0.075 m/second.
son’s ratio = –0.72 ± 0.05. However, the average Poisson’s Table 1 describes the processing conditions of 3GT powder
ratio of the conventional fibers was found to vary between to obtain the processing window for auxetic polyester fib-
+0.18 and +0.25, which is typical for an engineering mate- ers. It can be observed from the table that processing tem-
rial. perature plays a critical role in governing the Poisson’s
ratio of polyester fibers. Although few traces of auxeticity

Table 1 Extrusion matrix for the production of auxetic polyester fiber.


Sample Temperature Extruder speed Take-up speed Auxetic
Die used
no. (°C) (rad/second) (m/second) behavior
1 4-hole mono filament (dia = 1 mm) 230 0.525 0.075 NO
2 40-hole filament (dia = 550 µm) 225 0.525 0.075 YES
3 40-hole filament (dia = 550 µm) 220 0.525 0.075 YES
4 40-hole filament (dia = 550 µm) 215 0.525 0.075 NO
5 40-hole filament (dia = 550 µm) 212 0.525 0.075 NO

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Negative Poisson’s Ratio Polyester Fibers N. Ravirala et al. 545 TRJ

have been detected in the fibers processed at 220°C, the


auxeticity of the polyester fibers is significantly increased in
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TRJ 546 Textile Research Journal 76(7)

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