phys. stat. sol. (b) 244, No. 3, 828 841 (2007) / DOI 10.1002/pssb.

200572702

Microstructural evolution in the processing

of auxetic microporous polymers
K. L. Alderson*, 1, R. S. Webber2, and K. E. Evans3
1
2
3

Centre for Materials Research and Innovation, University of Bolton, Bolton, BL3 5AB, UK
Department of Materials Science, University of Liverpool, Liverpool, L69 3BX, UK
Department of Engineering, University of Exeter, EX4 4QF, UK

Received 2 November 2005, accepted 31 August 2006

Published online 12 January 2007
PACS 61.41.+e, 62.20.+e, 81.05.Lg, 81.05.Zx
Microstructural formation in auxetic microporous UHMWPE has been studied in detail using extensive
mapping of the microstructure during its processing. To ease sectioning for microstructural examination, a
sintering and extrusion route was used. The fibrillar microstructure was found to occur in both the radial
and longitudinal directions. Fibril generation was also seen to occur prior to extrusion with enough fibrils
of sufficient size to lead to auxetic behaviour. A mechanism for fibril generation is proposed which is based on surface melting of the particles and drawing out of the interparticle contact points by particle movement, which is not necessarily the result of extrusion through a die. These findings will aid in the
understanding of processing of auxetic microporous polymers and in the drive to extending the range
available to include other polymeric materials and different processing routes.
2007 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim

Introduction

Auxetic materials are those which show an expansion both transversely to and along the direction of an
applied tensile load [1]. Since the first synthetic auxetic material (a polymeric foam) was produced in
1987 by Lakes [2], a variety of other auxetic materials have been produced. These include polymeric and
metallic foams [25], honeycombs [6, 7], polymer gels [8] and angle ply laminate composites [915].
The auxetic effect was first observed in microporous polymeric material in 1989 [16, 17]. In this case,
an expanded form of polytetrafluoroethylene (PTFE) was found to exhibit a highly anisotropic negative
Poissons ratio, , as low as = 12. This was due to its complex microstructure which consists of nodules interconnected by fibrils and is shown in the micrograph of Fig. 1. Both the nodule and fibril dimensions and their interconnectivity were found to be behind the causal mechanism, which is illustrated
schematically in Fig. 2.
The observation of the auxetic effect in PTFE revealed that there was no underlying reasons why other
polymers should not be processed in such a manner as to produce this particular microstructure. So, a
batch process consisting of three distinct stages of compaction [18], sintering [19] and extrusion [20] was
developed and used to produce auxetic microporous samples of ultra high molecular weight polyethylene
(UHMWPE) [21], polypropylene (PP) [22] and nylon [23]. An example of the microstructure of auxetic
UHMWPE produced by this three stage route is shown in Fig. 3.

Corresponding author: e-mail: k.alderson@bolton.ac.uk

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Fig. 1

829

Micrograph of the microstructure of microporous auxetic PTFE.

A very detailed study of the three stage processing route has been carried out [1820] and this indicated that the role of the compaction stage was to impart structural integrity to the extrudate. So, the
compaction stage was omitted systematically. The results of this were that without a separate extrusion
stage, the extrudate produced was highly fibrillar and very auxetic but had low mechanical properties and
low density [24, 25]. Equally, the detailed study indicated that the extrusion stage may also be omitted
and more recent work has shown that this is indeed the case. If the specimens are compacted and then,
rather than undergoing sintering and extrusion, they are subjected to a multiple sintering regime, then the
result is a material which retains some of its auxeticity, but has excellent structural integrity [26]. Thus,
the effects of processing on structural integrity and overall auxeticity have been explored and are well
understood and documented. The flexural properties, density and density packing factor are included
here in the Table 1, for completeness. Similarly, as mentioned above, the causal mechanisms behind the
auxetic response are also well understood for auxetic microporous polymers. What has not been studied
in depth to date, however, is the process by which the microstructure actually forms.
In conventional die drawing of HMWPE, performed to increase mechanical properties [27], microstructural examination has been studied and is well documented. Peterlin has suggested that the process
is divided into three stages: the plastic deformation of spherulites, the transformation from spherulite to
microfibril and the plastic deformation of the fibril [2830]. Hendra, William and Taylor [31] suggested
that this model could be further developed to include local melting and recrystallisation. Lee and Li did a
detailed microstructural examination and found broad agreement with previous work, though they state
that rather than plastic deformation of the spherulites, they found alignment at low draw rates and local
melting and strain-induced recrystallisation at draw rates of about 7 [32].

Fig. 2 Schematic of the microstructure of a typical auxetic

polymer. (a) represents the polymer before application of a
tensile load and (b) after application of a tensile load. a and b
represent the nodule dimensions, l1 is the fibril length and 0
is the angle between the fibril and the r-axis.

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K. L. Alderson et al.: Microstructural evolution in the processing of auxetic microporous polymers

Fig. 3 Micrograph of the microstructure of auxetic microporous UHMWPE.

As regards auxetic polymers, previous work has suggested that in the three stage processing route, the
fibrils appear to be formed by the initial drawing out of transition material formed during sintering,
which links the nodules. This is followed by elastic stretching and then plastic deformation to failure of
the fibrils [23]. It is not clear at which stage during the processing route that each of these stages occur,
however. The aim of this paper is, then, to use detailed experimental maps to trace how the polymer
microstructure actually forms in auxetic UHMWPE. This will help in the drive to producing homogeneous samples and in understanding and developing future processing routes and a more diverse range of
auxetic polymers. In order to facilitate the process of detailed microscopy, the samples were produced by
the two stage processing route of sintering and extrusion, ensuring an auxetic material which can be
readily sectioned and observed.

Experimental methods

2.1 Fabrication route for sample production

Specimens were manufactured for testing using the two stage processing route of sintering and extrusion.
This takes place within a specially designed processing rig (see Fig. 4a). The powder is poured into the
barrel which has been pre-heated to 160 C. (It should be noted that the die is lightly plugged with paper
to hold the powder in the barrel). The powder is then sintered at 160 C for 20 minutes and then immediately extruded at 500 mm/min through a die with entry diameter 15 mm (to match the barrel of the extrusion rig), exit diameter 9.5 mm, cone semi-angle 45 and zero capillary (see Fig. 4b). The die was in two
pieces for ease of removal from the specimen.
In order to map the microstructure, the extrusion process was stopped at pre-defined displacements.
The displacements selected were 0 (i.e. the control specimen), 25, 50, 75, 100, 125, 150 and 175 mm.
Between 2 and 10 samples were produced at each condition to get consistent maps. It was obviously
Table 1 Mechanical properties and density of the forms of microporous auxetic UHMWPE.

specimen type

density
(kg/m3)

flexural modulus
(MPa)

density packing factor

(%)

3 stage
no compaction
no extrusion

858
730
920

360 10
53 6
106 2

90
79
96

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a)

b)
Fig. 4 (a) Schematic of the processing rig used for the production of auxetic polymers; (b) schematic of
a typical extrusion die.

necessary to dismantle the processing rig after each extrusion to release the specimen and this was done
with the utmost care. It is for this reason that up to 10 samples were required for each condition. The
position of the die in each case is shown clearly in Fig. 5 for reference. It can be seen that the powder
does not start to flow through the die until between 75 and 100 mm of displacement has been applied.
2.2 Microscopic examination of the extrudate
For ease of understanding, Fig. 6 shows the terminology to be employed as the microstructural evaluation is traced and discussed in the remainder of this paper.
Fracture surfaces were obtained in both the radial and axial directions. For the pre-extrudate material,
fracture surfaces were obtained in both orientations at the plunger end (i.e. that closest to the plunger),
mid-span and die end (i.e. that closest to the die). After 100 mm of displacement, when the extrudate has
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K. L. Alderson et al.: Microstructural evolution in the processing of auxetic microporous polymers

Fig. 5

Schematic showing the position of the die at each selected extrusion.

begun to form, fracture surfaces were also obtained from the rapid expansion zone and the zone of maximum attainable expansion. In addition, fracture surfaces at the edge and central regions of the samples
were taken. This very detailed examination was achieved to the required accuracy by freezing the specimens in liquid nitrogen, notching carefully at the required location and then fracturing the sample. The
required surfaces were mounted on aluminium stubs, gold coated using an Edwards S150 sputter coater
and observed at magnification of up to 1500 in a Philips 501 scanning electron microscope. Photographs of the images were obtained and these were transposed into schematic maps of the microstructure.

Fig. 6 (online colour at: www.pss-b.com)

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Schematic of the terminology employed.

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a)

b)

c)

Fig. 7 (a) Map showing microstructural features in the r, radial, and z, longitudinal, directions after 0 mm displacement; (b) micrograph of the microstructure at the midspan in the radial orientation after 0 mm displacement; (c)
micrograph of the microstructure at the midspan in the longitudinal orientation after 0 mm displacement.

Results

The results of this investigation are presented as schematics, together with selected micrographs for
comparison and to demonstrate the accuracy of the transposed maps. It should be noted at this stage that
the micrographs shown are examples of the regions and do not correspond directly with the maps shown
since the latter were obtained by observing up to 10 samples and not just the single examples shown in
the micrographs.
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K. L. Alderson et al.: Microstructural evolution in the processing of auxetic microporous polymers

a)

b)
Fig. 8 (a) Map showing microstructural features in the r, radial, and z, longitudinal, directions after
25 mm displacement; (b) micrograph of the microstructure at the plunger end in the radial orientation after 25 mm displacement.

At 0 mm, i.e. at the control condition of no extrusion and just sintering, no fibrillation is observed.
This can clearly be seen in Fig. 7ac which do show, however, that some interparticle necks have begun
to form as would be expected due to the sintering process. This can most clearly be seen in the micrograph Fig. 7c, which shows the midspan of the sample in the longitudinal direction.
At 25 mm, it was expected that further thick necks could be observed. However, Fig. 8 shows that, in
addition to necks at the midspan and die areas, there is some evidence of fibrillation. Fibrils were seen at
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Fig. 9 Map showing microstructural features

in the r, radial, and z, longitudinal, directions
after 50 mm displacement.

835

Fig. 10 Map showing microstructural features in

the r, radial, and z, longitudinal, directions after
75 mm displacement.

the plunger end with lengths of up to 810 m and this is shown in Fig. 8b. Clearly, the formation of
fibrils prior to extrusion is a major finding in so far as understanding how the microstructure forms.
This finding is further underlined by Fig. 9, which shows the microstructural map after 50 mm displacement. There has still been no material passing through the die so this is still a complete preextrudate. Fibrillation is now observed in both the plunger and midspan areas. The die area remained
unfibrillated.
At 75 mm displacement, the final example where no extrusion had occurred, fibrillation was found to
occur in all pre-extruded material. This is shown in Fig. 10. The fibrils are short, of the order of 56 m
in length only. A further observation was that the microstructure in the plunger end in particular was seen
to be closing up due to increased pressure from the plunger.
Figure 11ae show the microstructure as the material begins to flow through the die. There is fibrillation throughout, but there are marked differences which are clearly shown in particular in the micrographs. After extrusion, the fibrils formed are longer than any observed in the pre-extrudate material (i.e.
up to 35 m in length) and consequently, the microstructure is more open.
This trend is observed to continue as more material is pushed through the die. Figures 12, 13 and 14
show the microstructural maps for displacements of 125, 150 and 175 mm respectively. There is fibrillation throughout, with longer, more profuse fibrils formed on exit from the die.
To summarise, there are two main findings to arise from the results of this very detailed examination.
Firstly, fibrils are formed in both the radial and longitudinal directions. The techniques used in this work
have allowed this to be stated categorically for the first time. Secondly, fibrils are formed before extrusion. The importance of this are discussed below.
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K. L. Alderson et al.: Microstructural evolution in the processing of auxetic microporous polymers

a)

b)

c)

d)

e)

Fig. 11 (a) Map showing microstructural features in the r, radial, and z, longitudinal, directions after 100 mm
displacement; (b) micrograph of the microstructure at the die end in the radial orientation after 100 mm displacement.; (c) micrograph of the microstructure at the die end in the longitudinal orientation after 100 mm displacement;
(d) micrograph of the microstructure just beyond the region of rapid expansion in the radial orientation after 100 mm
displacement; (e) micrograph of the microstructure just beyond the region of rapid expansion in the longitudinal
orientation after 100 mm displacement.

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Fig. 12 Map showing microstructural features in the r,

radial, and z, longitudinal, directions after 125 mm displacement.

Discussion

4.1 Mechanisms of fibril generation

Prior to the examination of how the microstructure is formed in this case, it is worthwhile revisiting fibril
formation previously proposed for auxetic microporous polymers and conventional die-drawn polymers.
The idea of local or surface melting and plastic drawing out of material is central to the mechanisms
involved in microstructural formation for die-drawn polymers [2732] and has a key role in the formation of the nodule-fibril microstructure in auxetic polymers. Fibrils are thought to be produced in the
compaction, sintering and extrusion route for auxetic UHMWPE [23, 26] by a process based on drawing,
stretching and necking of the fibrils on a very small scale. This begins with the drawing out of transition
material formed during sintering, which links the nodules, into fibrils. The fibrils then viscoelastically
stretch prior to plastic deformation to failure. It was initially believed that this entire process all occurred
during the extrusion stage as the material is pushed through the die. A further mechanism of fibril formation was required to interpret how the fibrils were formed during the process of compaction followed by
multiple sintering i.e. without extrusion. This is charted in a previous publication [26], but will be summarised here. Once again, the basis of microstructural formation is local surface melting, leading to a
partially fixed structure at favoured contact points, after the initial compaction and single sintering stages. With subsequent sintering treatments, the interparticle links are then drawn out by particle movement during the heating and cooling cycles of the multiple sintering routes.
In this case, though, there is no extrusion and no multiple sintering at the initiation of fibrillation, but
the central theme is comparable with previous work and, indeed, for the first time studies from experimental evidence have shown the process of microstructural formation. The mechanism begins with particles being brought into close contact by being poured into the processing rig barrel. Carrying out a sepawww.pss-b.com

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K. L. Alderson et al.: Microstructural evolution in the processing of auxetic microporous polymers

Fig. 13 Map showing microstructural features in the

r, radial, and z, longitudinal, directions after 150 mm
displacement.

Fig. 14 Map showing microstructural features in

the r, radial, and z, longitudinal, directions after
175 mm displacement.

rate compaction stage as in the three stage processing route and the compaction and multiple sintering
route is an extreme version of this stage whereby the particles are forced into very close contact. As the
polymer powder is then sintered, interparticle necks develop at contact points, leading to the exchange of
nodular material between neighbouring nodules across interparticle boundaries. This is now known to
occur in both the longitudinal and radial directions. The shared nodular material is then drawn into fibrils
as the contact points of the neighbouring nodules become displaced from one another. This displacement
could be due to a number of possible scenarios including die extrusion and movement of particles either
before die extrusion occurs or during multiple sintering. However, die extrusion does have a significant
role in the formation of the microstructure even if it is not required in the initiation stage. This is because
fibril numbers are found to increase dramatically within the die. This is clearly illustrated as the most
significant increase occurs as the material rapidly expands on escaping the die constraints. Also, the fibril
length depends on how much the nodules have been compressed and interlocked. This indicates that the
key to producing a very auxetic microporous polymer is still extrusion of the polymer as this is what
generates a highly fibrillar, open microstructure.
4.2 Modelling the microstructure to study the Poissons ratio
This study has shown that the microstructure required to produce auxetic polymers can be formed before
extrusion occurs. However, the question remains is the pre-extrudate material which has a small number
of small fibrils auxetic? The samples produced here have been specially designed to be easy to section

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whilst retaining their microstructure. The three stage processing route produces a good structural integrity which causes problems in sectioning to obtain detailed and positional microstructures. For this particular examination, it is imperative to be able to observe the microstructure at all positions along and
across each of the specimens. If the more dense, higher modulus samples had been used (see Table 1),
pinpointing the microstructure with the required accuracy would be extremely difficult. However, performing tests to get the value of the Poissons ratio then becomes very difficult due to the weak nature of
the samples designed specifically to to be easy to section. There does exist, however, a very successful
technique for the interpretation of the strain dependent Poissons ratio in auxetic polymers. This is the
nodule-fibril model which employs simple geometric models based on the microstructural parameters to
present an excellent first approximation to experimental behaviour [17, 33, 34]. The model is shown
schematically in Fig. 2 and it requires knowledge of the nodule dimensions, a and b, the major and minor
lengths of the nodules respectively, l1, the fibril length and 0, the angle between the fibril and the r-axis,
all as indicated in Fig. 2. The model utilizes a space-filling unit cell that, from Fig. 2, can be defined as
having sides of:
r = 2a + 2l1 cos 0 ,

(1)

z = 2b 2l1 sin 0 .

(2)

As a compressive strain is applied, the angle between the fibril and the r-axis varies, the angular variation being characterized by . Thus, the compressive engineering strain applied in the radial direction, r,
is given by:
r =

r ( ) - r ( 0 )
,
r ( 0 )

= l1

(cos - cos 0 )
.
a + l1 cos 0

(3)

(4)

Fig. 15 (online colour at: www.pss-b.com) Graph of the radial Poissons ratio, rz, against strain, r for
specimens produced to displacements of 75 mm at the plunger (a), mid span (b) and die ends (c) and at the
die end for a displacement of 100 mm (d).

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K. L. Alderson et al.: Microstructural evolution in the processing of auxetic microporous polymers

Now,
rz = -

=-

z z/z0
,
=
r r/r0

(5)

(sin 0 - sin ) (a + l1 cos 0 )

,
(cos - cos 0 ) (b - l1 sin 0 )

(6)

where z = z - z0 is a small, but not infinitesimal change and similarly for r.

Microstructural dimensions measured during this examination were inputted into Eqs. (4) and (6) and
the theoretical curves obtained are shown in Fig. 15. It can be seen that behaviour is predicted to be auxetic for these samples, with the largest values being obtained at the die end for 75 mm displacement.
This is the area of the four considered with the most open microstructure and thus the results are as
expected. The plunger pressure causes the microstructure to close up, allowing less space for nodule
translation, and so reducing the opportunity for auxetic behaviour to occur. Nevertheless, in all four
cases, auxetic behaviour is predicted to occur without the need for extrusion.

Conclusion

Detailed microscopy has revealed how the microstructure which generates auxetic behaviour is formed
in UHMWPE. Using a sintering and extrusion route combined with extensive microstructural mapping
has revealed that fibrils are formed in both the radial and longitudinal directions, though not to the same
extent, as is indicated by the anisotropy of the material. If the microstructure were isotropic, it would be
expected that the material would also be isotropic overall. More importantly, the mapping has also revealed that fibrils are formed before extrusion. Though these are short and few in number, simple geometric models do predict that auxetic behaviour would occur. The fibrils increase in both number and
length as the material is forced through the extrusion die.
The main aim of this work was to study the mechanisms of microstructural formation and this has
been achieved. The microstructure is now known to be produced by surface melting of the material leading to the formation of thick necks. These are drawn into fibrils which is not necessarily the result of
extrusion as had previously been assumed, but could also be the result of particle movement prior to
extrusion as the plunger forces the material into close contact.
Understanding how microstructural formation occurs in auxetic microporous polymers will allow
further studies to attempt more homogeneous fabrication of samples and help in the drive towards producing new polymers in auxetic forms using a variety of processing techniques.
Acknowledgements RSW would like to acknowledge the support of the EPSRC through the provision of a studentship and Prof. Wesley Cantwell for his assistance with this project.

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