phys. stat. sol. (b) 242, No. 3, 509518 (2005) / DOI 10.1002/pssb.

200460371
2005 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim
Original
Paper
How to make auxetic fibre reinforced composites
K. L. Alderson
*, 1
, V. R. Simkins
1
, V. L. Coenen
1
, P. J. Davies
1
, A. Alderson
1
,
and K. E. Evans
2

1
Centre for Materials Research and Innovation, Deane Road, Bolton, BL3 5AB, UK
2
School of Engineering, Computer Science and Mathematics, Harrison Building,
University of Exeter, Exeter EX4 4QF, UK.
Received 15 June 2004, accepted 8 November 2004
Published online 15 February 2005
PACS 81.05.Lg, 81.05.Qk, 81.20.Ev, 81.20.Hy, 81.70.Bt
Auxetic composite materials can be produced either from conventional components via specially designed
configurations or from auxetic components. This paper reviews manufacturing methods for both these
scenarios. It then looks at the possibility of property enhancements in both low velocity impact and fibre
pull out due to the negative Poissons ratio. Tests revealed that auxetic carbon fibre composites made
from commercially available prepreg show evidence of increased resistance to low velocity impact and
static indentation with a smaller area of damage. Also, using auxetic fibres in composite materials is
shown to produce a higher resistance to fibre pullout.
2005 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim
1 Introduction
Developments in structural engineering design and technology over the past three decades in industries
such as aircraft, automobile and sports and leisure equipment have demanded the production of new,
high-performance materials. Within this class of materials are the fibre-reinforced composites. The pos-
sibility of producing composite laminates with Poissons ratios close to 1 was discussed by Milton in
1992 [1]. Advances in auxetic materials production and development have led to the possibility of pro-
ducing auxetic fibre reinforced composites, thus exploiting property enhancements known to arise in
auxetic materials such as energy absorption, improved fracture toughness and better resistance to inden-
tation.
There are a number of ways in which auxetic fibre reinforced composites can be made. The route
closest to conventional manufacture is to use off-the-shelf pre-preg material which, given specific stack-
ing sequences, will produce an overall auxetic effect. Several groups have used this route to auxetic fibre
reinforced composites [27] and have made some inroads into testing the resultant materials for en-
hanced fracture toughness [4] and indentation resistance [5]. Composite laminates can be designed to
have negative in-plane or through-thickness Poissons ratios, . The requirement for an auxetic compos-
ite laminate is that the individual ply materials be highly anisotropic. This means that carbon/epoxy [3] is
a more suitable choice than either Kevlar/epoxy [8] or glass/epoxy [6], though all three material combi-
nations have been investigated. In many cases, the negative Poissons ratios obtained by this route to
date have been small i.e. around = 0.17 [26] although Miki and Morotsu [7] did produce a value of
= 0.37 for an unbalanced, bi-directional laminate. Methods of increasing the value of have
been discussed and these include use of a prepreg with increased anisotropy (i.e. using a stiffer fibre or a


*
Corresponding author: e-mail: k.alderson@bolton.ac.uk
510 K. L. Alderson et al.: How to make auxetic fibre reinforced composites
2005 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim
higher volume fraction) [3]. Another approach would be to investigate different laminate configurations
predicted to give a more negative Poissons ratio [9]. Work towards using specially designed software
[10] to achieve this is ongoing, with prediction of stacking sequences now possible to specifically maxi-
mise the negative Poissons ratio. For example, for a specified set of properties, it has been possible to
predict a value of = 0.25. Clearly this is an area of extreme importance and one in which very inter-
esting results are expected.
The work reported here, however, is concerned with the effect of a negative Poissons ratio on me-
chanical properties of the laminate. In particular, the properties of static indentation and low velocity
impact damage are examined with an emphasis on the energy absorption and damage sustained by
auxetic laminates in comparison with their conventional counterparts.
A further method of manufacturing an auxetic fibre reinforced composite is to use auxetic compo-
nents, for example, an auxetic matrix, auxetic reinforcement or both. This has been achieved using
auxetic foams previously [11] and has been modelled for some considerable time [12]. A simple press-fit
fastener [13]

has been developed based on an auxetic copper foam which demonstrates both theoretically
and experimentally that it is much more difficult to remove than would be a conventional copper foam.
However, it has only very recently been possible to begin work on auxetic fibre reinforced composites of
this type with the advances in the manufacture of auxetic fibres [14] and new methods to produce auxetic
polymers [15, 16].
This paper reports current work to assess the possibility of using auxetic polymeric fibres within a
composite. The fibres used are polypropylene and tests have been carried out to assess their pull-out
performance from a specially designed matrix. The results have shown that it is up to 4 times more diffi-
cult to pull out an auxetic fibre than a similar conventional fibre and these results and their implications
will be discussed.
This paper, then, draws together the work in producing and testing auxetic fibre reinforced compos-
ites.
2 Auxetic fibre reinforced composites made from conventional materials
The work reported here is concerned with looking at manufacturing and testing carbon fibre reinforced
laminates with a negative
13
i.e. through-the-thickness Poissons ratio. The main aim is to compare
auxetic laminates with those of matched through thickness modulus, E
3
, but with a small positive or near
zero Poissons ratio. This is so that any property difference in this direction can be attributed to the Pois-
sons ratio alone. The first stage is, then, to design appropriate laminate configurations and this was
achieved using specially designed software [17, 18], presented by Zhang and Evans. Software packages
generally available for this technique predict the mechanical properties of a specific lay-up orientation,
allowing the designer to try many different lay-ups rapidly. This can be time consuming and may not
result in optimum matched laminate configurations. A number of workers have tried to address this prob-
lem, beginning in the late 1960s by Schmit [19] and Bush [20]. They proposed an analytical approach to
composite laminate design but these were limited by very specific loading conditions and orientation
assumptions. Since then, several different optimisation procedures for the design of laminated plates
subjected to various stiffness and strength constraints have been established. These include work on
optimum design for in-plane loading [2123], maximum stiffness and bending strength [24, 25] and
stability [26, 27]. The optimisation approach of Zhang and Evans, however, is more general. Here, no
symmetry is assumed and all layers can be different to each other. The FORTRAN program developed
enables the design of laminates with required mechanical properties where only the individual lamina
layer properties are known. The program is able to produce an optimised stacking sequence by minimis-
ing the difference between properties calculated from, for example, classical laminate theory and those
properties required by the designer. For this case, where the aim was to study the effect of a negative
Poissons ratio, the stacking sequences predicted are given in Tables 1a and b below. Each panel com-
prised 24 layers.
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2005 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim
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Table 1a Laminate stacking sequences and software predictions of E
1
, E
2
, E
3
and G
12
.
stacking sequences E
1
(GPa) E
2
(GPa) E
3
(GPa) G
12
(GPa)
([0/45/5/40]
s
)
3
75.3 20.1 9.6 19.3
[+/30]
6s
49.6 11.9 9.5 26.5
[35/20/25/40/85/40/25/45/35/15/25/40]
s
49.8 25.0 9.6 20.3

Table 1b Laminate stacking sequences and software predictions of
12
,
21
,
31
and
13
.
stacking sequences
12

21

13

31
([0/45/5/40]
s
)
3
0.721 0.192 0.086 0.011
[+/30]
6s
1.243 0.298 0.156 0.03
[35/20/25/40/85/40/25/45/35/15/25/40]
s
0.554 0.278 0.187 0.036
2.1 Manufacture of auxetic fibre reinforced composites
Specimens with the laminate configurations given in Tables 1a and b were prepared as 80 80 3 mm
square panels from IM7/5882 unidirectional carbon epoxy prepreg. Standard vacuum bagging techniques
were employed. The laminate was prepared in accordance with the required stacking sequence. Each
successive ply was placed directly on top of the other at the desired orientation on a smooth base plate
covered by a PTFE release material to aid removal of the specimen after curing. Once lamination was
complete, a metal top-plate also covered in PTFE release material was placed on the laminate stack. A
layer of breather fabric to allow air to be evacuated efficiently was placed on top with the vacuum valve
attachment taped in a central position. The whole assembly was made airtight using a high temperature
nylon bagging film and vacuum sealant. A vacuum pressure of 0.8 bar was applied over night to consoli-
date the laminate. The lay up was placed in a fan oven and the temperature raised at a rate of 23/min.
until a temperature of 180 C was reached. This was maintained for 130 minutes. The oven and contents
were then slowly cooled to room temperature, the vacuum pressure removed and the bag opened. The
through-the-thickness Poissons ratio values were measured using the technique of video extensometry
and good agreement was found with the predicted values shown in Table 1b [28].
2.2 Static indentation testing
A specially designed flexural indentation test configuration was adapted for this work. The reason for
this was that it was desirable to allow the specimen to flex without the confines of clamping at this stage
and to allow the indentation nose to penetrate through the specimen, giving the full damage capability of
the specimen. This was to build on standard indentation testing of the auxetic carbon fibre laminate
which gave an indication of an enhancement in performance in the elastic region only [5].
Tests were conducted on a Dartec Universal Hydraulic testing facility in compression mode. Four
specimens of each configuration were tested to a penetration depth of 5 mm (i.e. to full specimen dam-
age) at a strain rate of 2 mm/min. The indentor nose, a 12.7 mm diameter hemisphere, was applied at the
centre of the specimen. From the resultant load/displacement plots, the load, displacement and energy
absorbed at first failure and to peak load were obtained.
2.3 Low velocity impact testing
The starting point for the low velocity impact testing was the analysis of the load/displacement curves
from the static indentation tests. An in-house designed and built fully instrumented drop weight impact
machine was used in conjunction with a data capture system with medium range sampling rate per chan-
nel and in-built signal conditioning. Eight channels were available, allowing accelerometer, voltage and
512 K. L. Alderson et al.: How to make auxetic fibre reinforced composites
2005 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim

Fig. 1 Typical static load/displacement curves for the laminates with
13
= 0.156,
13
= +0.187 and

13
= +0.086. The three energy levels selected for impact testing are indicated as 1, 2 and 3.

strain gauge inputs. This system was modified substantially in house and allowed a million samples per
second to be captured. A single bounce mechanism was fitted to ensure clear analysis of the impact
event.
Three energy levels corresponding to specific points in the damage process were selected (see Fig. 1).
These were 2 J, 7 J and 12 J. A fixed mass impactor with an equivalent 12.7 mm hemispherical nose was
used with the same support conditions employed as in the static indentation testing. The impactor
weighed 1.76 kg and, correspondingly, resulted in impact velocities of 2 m/s, 3 m/s and 4 m/s.
Force/time histories were recorded and the same properties were evaluated for comparison with the static
indentation tests.
2.4 Damage observation after testing
The specimens were all sectioned to evaluate the internal damage using fractographic analysis. Images of
the damage were recorded photographically for ease of comparison.
2.5 Experimental results and discussion
2.5.1 Static indentation testing
Typical load/displacement curves for each specimen type are shown in Fig. 1. The extrapolated points
from the curves are given in Table 2a for the first failure point and Table 2b for the peak load data. It can
be seen that the auxetic specimens had the highest properties in each case i.e. a higher load sustained and
more energy absorbed to first failure and to peak load. This points to an enhancement in resistance to
indentation.
The fractographic damage was extremely interesting with this in mind. The laminate with
13
= 0.086
had damage which was dominated by several large delaminations through the thickness. The laminate
with
13
= 0.187 also had several large delaminations but this time towards the back face of the laminate.
However, the damage in the auxetic specimen is characterised by very localised fibre breakage directly
under the indentor with very few delaminations. These findings can be clearly seen in Figs. 2, 3 and 4
below which show the comparison between the laminates with
13
= 0.086,
13
= 0.156 and
13
= 0.187,
respectively. Basically, the auxetic laminate will contract under the indentor as a direct consequence of
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Table 2a Experimental first failure values for the static indentation tests. Poissons ratio refers to
13
.
Poissons ratio displacement
(mm)
load
(kN)
energy absorbed
(J)
initial gradient
(kN/mm)
0.086 1.13 2.42 1.4 2.14
0.156 1.37 3.48 2.4 0.1 2.54
0.187 1.21 3.02 1.8 0.1 2.50

Table 2b Experimental peak load values for the static indentation tests. Poissons ratio refers to
13
.
Poissons ratio displacement
(mm)
load
(kN)
energy absorbed
(J)
0.086 3.3 0.2 6.2 0.6 10 2
0.156 3.6 0.3 7.7 0.7 14 2
0.187 3.6 0.5 6.8 0.1 12 2




Fig. 2 Damage induced in the specimen with
13
= 0.086 by the flexural indentation test.




Fig. 3 Damage induced in the specimen with
13
= 0.156 by the flexural indentation test.




Fig. 4 Damage induced in the specimen with
13
= 0.187 by the flexural indentation test.
514 K. L. Alderson et al.: How to make auxetic fibre reinforced composites
2005 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim
its through-the-thickness (i.e.
13
and
31
) auxetic nature. As the damage is not dissipated over a large
area as in the creation and subsequent growth of delaminations, the majority of the damage created oc-
curs directly under the indentor, where it is more severe but highly localised. This type of response has
been seen in other auxetic materials, and has been studied systematically in foams [29]. Here, the densi-
fication under the indentor was suggested to be due to an enhanced shear modulus for auxetics causing
an improved material response to shear stress and allowing a wider distribution of strain. The suppres-
sion of delaminations observed suggests a similar densification mechanism in the composite laminates
tested here added to a better distribution of strain. In addition, the consistent mismatch between individ-
ual lamina layers in the auxetic laminate which have a stacking sequence of (30)
s
leads to an orderly
progression of damage through the specimen thickness and a greater communication of shear strain,
causing higher resistance to delamination [28]. Thus, there are two effects contributing to this response,
the mismatch and the auxetic effect, and the relative roles of each are currently being examined, as is the
role of the positive in-plane Poissons ratio (
12
).
2.5.2 Low velocity impact testing
The results from the low velocity impact testing of the specimens are presented in Table 3a for results to
first failure (easily isolated from the impact plot) and in Table 3b to the end of the impact event for the 7J
impact. Similar results were obtained for the 12J impact. It should be noted that at the 2J level, no dam-
age was induced in the specimens.
It can be seen that the enhancement at first failure observed in the auxetic samples is found under both
impact and static conditions. It is, however, interesting to note that for the auxetic specimens, the first
failure load is actually the maximum load measured during the impact. This suggests that the first failure
onset is a much more significant event for auxetic specimens. The fractographic examination revealed
that in the specimen with
13
= 0.086, there were several large delaminations in the upper half of the
laminate. The laminates with
13
= 0.187 revealed a number of delaminations in the upper half of the
laminate accompanied by shear cracking under the indentor. The auxetic specimen, however, showed
only a small amount of back face failure (even at such low velocities) but no discernible delaminations at
all. This was very surprising and seems to add weight to the possibility of the localised mechanism de-
scribed above occurring in the auxetic laminates compared to the other two laminates.
In conclusion, static and low velocity indentation resistance of auxetic composite laminates has been
evaluated in comparison with laminates having near zero (
13
= 0.086) and large positive (
13
= 0.187)

Table 3a Experimental first failure values for the low velocity impact tests. Poissons ratio refers to
13
.
Poissons ratio displacement
(mm)
applied load
(kN)
energy absorbed
(J)
initial gradient
(kN/mm)
0.086 1.3 4.1 0.1 2.6 0.2 3.3 0.1
0.156 1.6 4.8 0.1 3.8 0.2 2.9 0.1
0.187 1.3 0.1 4.3 0.3 2.7 0.4 3.2 0.2

Table 3b Experimental end of impact event values for the low velocity impact tests. Poissons ratio re-
fers to
13
.
Poissons ratio max. displacement
(mm)
max. load
(kN)
energy absorbed
(J)
duration
(ms)
0.086 2.3 4.8 0.1 6.2 2.9
0.156 2.3 4.8 0.1 6.1 3.1
0.187 2.3 4.7 0.2 6.1 2.9 0.1
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Poissons ratio values. The auxetic laminates showed higher loads to first failure with enhanced energy
absorption in both cases. The statically tested specimen also sustained higher loads with the onset of
damage and absorbed more energy to catastrophic failure.
The initial damage sustained was found to be much more localised for both static and low velocity
impact testing in the auxetic laminates, with a distinct lack of large delaminations in each case. This
points to a different mechanism operating in response to indentation for auxetic laminates, which is a
combination of the auxetic response and mismatch between layers causing a localised response and sup-
pressing delamination growth.
3 Auxetic fibre reinforced composites made from auxetic components
Though it has been possible to make auxetic foam composites for a number of years [1113],

it is now
possible to make composites using auxetic fibres. Previously, it was suggested [30] that an auxetic fibre
within a composite would resist fibre pullout. This effect is shown schematically in Fig. 5 and would
appear to indicate that as the fibre is pulled, it will expand and lock into the matrix rather than contract-
ing and pulling out easily as a conventional fibre would do. This is also the principle behind the design
of a press-fit fastener using auxetic copper foam reported previously [13]. This section of this paper
reports work to investigate this idea using auxetic PP fibres as the reinforcement to a specially adapted
matrix.
3.1 Manufacture of model single fibre composites with auxetic fibres
In order to assess the single fibre pullout behaviour of composites using auxetic fibres, a model system
must be produced. It is not sensible to produce a fibre reinforced composite with a large volume fraction
of fibres to try to gather this type of data so, in accordance with normal practise, a model system consist-
ing of a single fibre embedded in a matrix has been manufactured. The fibres currently produced [14] are
relatively weak so the matrix material was carefully selected and modified so that the fibre may be re-
moved from the matrix before it necked. Also, in order to rule out thermal effects, the matrix was re-
quired to be a cold-cure resin.
The resin selected was Araldite LY 5052 with hardener HY 5084 and dibutyl phthalate used as the
softener. After an extensive period of experimentation [31], the matrix combination found to be the most
suitable was 40 ml of resin, 9 ml of hardener and 25 ml of dibutyl phthalate. The fibre was embedded in
the resin using a method developed in-house [31] and shown schematically in Fig. 6. A gel time of 6
hours at room temperature (24 2 C) was followed by seven days in the same conditions. The final
specimen was 80 mm long including an embedded fibre length of 20 mm, a free fibre length of 50 mm
and 10 mm spare fibre for handling and gripping. The specimen diameter was 15 mm. For compari-



Fig. 5 Schematic of the predicted response of auxetic reinforcement fibres.
516 K. L. Alderson et al.: How to make auxetic fibre reinforced composites
2005 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim

Fig. 6 Schematic illustrating the manufacture of the fibre pull out samples.

son purposes, both auxetic and carefully matched conventional fibres were prepared for testing. The
matching ensured that the fibres had the same modulus (1.3 GPa) and diameter (227 m) i.e. the main
difference between them was the Poissons ratio. The auxetic fibre had a Poissons ratio of +0.34
whereas the auxetic fibre had a Poissons ratio of 0.60. The Poissons ratio values were determined
using the technique of video extensometry and further details are available in a previous paper [20].
3.2 Fibre pullout tests
The tests were conducted using an Instron 4200 tensile testing machine fitted with a 100 N load cell. The
specimen was inverted and gripped in a collet grip attached to the crosshead of the machine. The free
fibre was clamped in the lower jaw. The distance from the upper end of the inverted resin cylinder down
to the upper edge of the lower jaw was 70 mm, and was set as the grip distance. The free fibre length
(between the lower surface of the inverted resin and the upper edge of the lower jaw) was 50 mm and
this was set as the gauge length. The test was conducted at a loading rate of 5 mm/min.
In order to assess the fibre/matrix interface for any evidence of surface interaction, small samples of
resin of dimensions 10 50 2 mm were cast with fibres of each type laid in. These were allowed to set
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2005 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim
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and cure as above. The samples were then fractured using liquid nitrogen and the broken fragments ex-
amined microscopically. No evidence was found of any surface interaction between the two materials in
either auxetic or conventional specimens.
3.3 Experimental results and discussions
The average curves obtained from performing pull out tests on conventional and auxetic embedded fibres
are shown in Fig. 7. It can clearly be seen that the auxetic fibres have a much higher peak debonding
load (0.96 N as opposed to 0.44 N) which remains higher over a great displacement. This would appear
to indicate a much larger debonding event than the conventional fibre. The energy used to pull out the
fibre is 8.3 mJ for the auxetic fibre which is over three times greater than that required to pull out a con-
ventional fibre i.e. 2.5 mJ. This appears to show that enhanced fibre pullout as has been suggested does
indeed occur. It should be noted that high resistance to fibre pullout is not always beneficial, since en-
ergy dissipation during pullout can confer a toughness on the material. A conceptual model of the fibre
pullout process has been developed and is the subject of a further paper [31]. To complement this de-
scription of the pullout process, existing analytical models for fibre pullout and in particular those focus-
sed on considering auxetic behaviour [13] have been studied.
These are now being adopted to the specific situation of an auxetic fibre in a conventional ma-
trix to further aid analysis of the process. The results, however, do have implications for the use of
auxetic fibres in such applications as fibre reinforced composites and in biomedical applications as su-
tures.
4 Conclusion
This paper has presented two very different ways in which an auxetic composite can be made. The first
uses off-the-shelf prepregs and, by variations of the stacking sequence employed, can be designed to
produce a through thickness or inplane negative Poissons ratio. This has resulted in enhanced mechani-
cal properties with static indentation and low velocity impact testing reported here. The second uses
auxetic constituents in this case, auxetic fibres as part of the composite. Here, fibre pullout is re-
ported to have been resisted due to the auxetic deformation of the fibres.
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obtained from auxetic and non-auxetic single fibre pull-
out.

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