654 Ind. Eng. Chem. Res.

2000, 39, 654-665

An Auxetic Filter: A Tuneable Filter Displaying Enhanced Size

Selectivity or Defouling Properties

Andrew Alderson,*,† John Rasburn,‡ Simon Ameer-Beg,† Peter G. Mullarkey,‡

Walter Perrie,† and Kenneth E. Evans‡

BNFL, Research and Technology, Building 709, Springfields, Preston PR4 0XJ, United Kingdom, and
Department of Engineering, University of Exeter, North Park Road, Exeter EX4 4QF, United Kingdom

Micromachined polymeric honeycomb membranes having conventional and re-entrant cell

geometries have been fabricated using femtosecond laser ablation. Mechanical properties
characterization confirms that the re-entrant membrane is auxetic (possesses negative Poisson’s
ratios: νxy ) -1.82 ( 0.05 and νyx ) -0.51 ( 0.01) whereas the conventional membrane possesses
positive Poisson’s ratios (νxy ) +0.86 ( 0.06 and νyx ) +0.6 ( 0.1). Comparison with honeycomb
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theory confirms that the dominant deformation mechanism is flexure of the honeycomb ribs.
The auxetic membrane has been challenged with single-sized glass chromatography beads such
Downloaded via BOCHUM LIBRARIES on November 8, 2019 at 03:46:23 (UTC).

that the beads were initially resting on the re-entrant cells. Subsequent tensile loading of the
membrane showed the auxetic cells opening during deformation, enabling the beads to pass
through the membrane. We have modeled the pore-opening properties of both types of
membranes, and the observed behavior for the auxetic membrane is consistent with the model.
This is a clear proof-of-concept demonstration of the potential of auxetic materials and structures
in filter defouling or cleaning operations. This paper, therefore, demonstrates the successful
design and fabrication of a micromachined auxetic structure having specifically tailored
mechanical properties that show enhanced functional performance over the conventional filter
structure.

1. Introduction structure have been identified. One is the possibility of

Auxetic materials exhibit a negative Poisson’s ratio;
that is, they expand laterally when stretched and
contract laterally when compressed.1 This unusual,
counterintuitive behavior is very rare in naturally
occurring materials,2 although it has been an accepted
consequence of classical elasticity theory for over 150
years.3 Recent interest in this property resulted from a
number of synthetic auxetic materials being produced.
In nearly all these cases, the auxetic material was
formed by altering the internal microstructure of a
conventional material, for example, foam4 and micro-
porous polymers,5,6 to produce auxetic behavior. In a
rare example of a naturally occurring auxetic material,
the auxetic form (R-cristobalite7) can be thought of as a
geometric rearrangement of the conventional form,
R-quartz. The benefits of having a negative Poisson’s
ratio have been investigated and many improvements
in mechanical properties have been identified including
shear modulus,1 fracture toughness,4 indentation re-
sistance,8 and acoustic response.9
The mechanism for producing a negative Poisson’s
ratio is not scale-dependent, so it is possible to envisage
structures, rather than materials, exhibiting exactly the
same phenomenon. In this situation, other benefits from
having an effective negative Poisson’s ratio across the
* To whom correspondence should be addressed. Current
address: Faculty of Technology, Bolton Institute, Deane Road,
Bolton BL3 5AB, U.K. Tel.: +44 1204 903513. Fax: +44 1204
381107. E-mail: aa1@bolton.ac.uk.
† BNFL.
‡ University of Exeter.
10.1021/ie990572w CCC: $19.00 © 2000 American Chemical Society
Published on Web 01/29/2000
producing synclastic curvatures4 in honeycombs for use
in composite sandwich panels.10 A second, and the
subject of this paper, is the use of auxetic honeycombs
and structures in filtration.4,11
One of the main problems of filter systems is the
reduction in filtration efficiency because of fouling of the
filter itself, by blockage of the barrier pores by particu-
lates. Auxetic materials and structures offer barriers
with the potential for cleaning of the membranes to be
facilitated in a manner not easily achievable in a
conventional barrier material or structure. This entails
opening up the pores of the barrier followed by a back-
flushing (or cross-flow flushing) operation to remove the
entrained particulates blocking the barrier. Pore open-
ing may be effected by the application of an external
tensile uniaxial load (or displacement) which, for an
auxetic material or structure, will cause the pore to open
up along and transverse to the direction of the load. For
a conventional material, however, the pore would only
be extended along the direction of the applied load, the
pore undergoing contraction (closing up) in the trans-
verse direction. This is shown schematically in Figure
1 for re-entrant and conventional hexagonal honeycomb
networks deforming by hinging of the honeycomb ribs.
It has been shown elsewhere that the re-entrant hon-
eycomb structure is auxetic when deformation is due
to rib hinging or flexure.12,13
Alternatively, auxetic materials or structures may be
used in membrane barriers which compensate for cake
fouling in situ. This utilizes a passive pore variation
mechanism due to the synclastic curvature4,10 property
that results from having a negative Poisson’s ratio. In
this scenario, the pressure drop across the barrier

Figure 1. (a) Undeformed re-entrant honeycomb network; (b) re-
entrant honeycomb network under an applied stress in the y
direction; (c) undeformed conventional honeycomb network; (d)
conventional honeycomb network under an applied stress in the
y direction. The re-entrant honeycomb is auxetic and demonstrates
a widening of the pore dimensions along both the x and y directions
under tensile loading. The conventional honeycomb is nonauxetic
and undergoes a pore widening along the direction of an applied
tensile load accompanied by a pore contraction in the transverse
direction.
increases as the cake foulant builds up on the barrier.
The increase in pressure drop may cause the barrier to
bow, which in turn opens up the pores of the barrier.
Thus, an auxetic membrane has an in-built mechanism
to compensate for the reduction in effective pore size
due to fouling, thereby extending the lifetime of the
filter. Such bowing is not possible in conventional
membranes.11
Because the auxetic effect is scale-independent, then
in principle, auxetic materials and structures can offer
enhanced separation barriers for a wide variety of
industrial processes, including solid/liquid separations
(filtration), gas/gas separations (molecular sieves), and
solid/gas separations (air filtration).
Here, we examine the use of honeycomb membranes
in a proof-of-concept demonstration of the defouling and
size-selectivity properties associated with auxetic filters.
To use auxetic honeycombs in practical filtration
systems, it is necessary to construct honeycombs with
cell sizes in the appropriate particulate size range. An
appropriate technology for the production of honeycombs
having cells in the micrometer size range is the use of
laser stereolithography.14 This has been identified as a
method for producing auxetic microstructures for im-
proved sensors15 and for micromachine manipulators.16
However, these applications require stiff materials that
can only withstand very small strains before failure.
Ind. Eng. Chem. Res., Vol. 39, No. 3, 2000 655
Figure 2. Schematic diagram of the Femtosecond laser system.
Low-energy 100-fs laser pulses are produced at 790 nm by a mode-
locked ti-sapphire laser (Coherent Mira 900-F pumped by a
Coherent Innova 300 argon ion laser). After being stretched to 300
ps, selected pulses are amplified in a ti-sapphire regenerative
amplifier pumped by a kilohertz Nd:YLF laser and recompressed
to τp ∼ 170-fs pulselength with pulse energy E ∼ 500 µJ (BMI
Alpha 1000).
The auxetic membrane considered here has a polymer-
based microstructure, fabricated by femtosecond laser
ablation, capable of sufficient distortion for use in
filtration.
2. Membrane Fabrication
UV laser ablation for micromachining and patterning
of polymers using nanosecond excimer lasers is a well-
established technique.17,18 A strong UV absorption coef-
ficient is desirable (>104 cm-1) and, in the case of weak
absorption, significant thermal degradation effects may
be observed.19 Femtosecond pulse laser ablation can
yield precise materials processing resulting from ef-
ficient energy deposition, while simultaneously mini-
mizing heat conduction and thermal damage to the
surrounding material. UV, visible, and near-IR femto-
second pulses may be used to microstructure transpar-
ent polymers at ultrahigh intensity because multiphoton
absorption by chromophores dominates the ablation
mechanism.19-21
Micromachined re-entrant and conventional honey-
comb polymeric membranes were formed by direct
femtosecond laser ablation in air of a sheet of Hewlett-
Packard Color LaserJet Transparency film (part num-
ber: HP C2936A). Figure 2 shows a schematic diagram
of the femtosecond laser system used for polymer
microstructuring. The standard technique of chirped
pulse amplification (CPA)22 was used to amplify the low-
energy (∼1-10 nJ) pulses to the millijoule level compat-
ible with the fluences required for laser ablation (∼1-
10 J cm-2 ). Pulses from the 1-kHz titanium sapphire
regenerative amplifier at 790 nm (170 fs) and frequency-
doubled near-UV pulses at 395 nm (200 fs) were both
used effectively in microstructuring. The laser output
was directed via a pair of temperature-stabilized XY
galvomirrors (General Scanning Inc.) onto a flat field
lens (f ) 160 mm) and focused at the substrate surface
to ≈100-µm spot diameter. Pulses of 100 µJ correspond-
ing to a fluence of 1.3 J cm-2 were used to mark the
cell perimeters at a scan speed of 5 mm s-1. Penetration
through the 128-µm thick polymer substrate was
achieved after ≈5 overscans/cell (∼100 pulses/spot
diameter) corresponding to an ablation rate of ≈1.3 µm/
pulse. In terms of the linear response, the polymer
membrane is highly transparent at both wavelengths
and absorbs strongly only below 350 nm.
Photographs of re-entrant and conventional honey-
comb membranes ablated at 790 nm are shown in
Figure 3.
656 Ind. Eng. Chem. Res., Vol. 39, No. 3, 2000
Figure 3. (a) Polymeric re-entrant honeycomb membrane; (b)
polymeric conventional honeycomb membrane. Pores are ap-
proximately 1 mm in width (along the x direction). The membranes
were fabricated by direct femtosecond laser ablation in air, with
pulses at 790 nm (170 fs).
The resulting cell dimensions measured from optical
micrographs were h ) 0.78 ((0.03) mm, l ) 0.54 ((0.02)
mm, t ) 0.086 ((0.006) mm, w ) 0.128 ((0.005) mm,
and R ) -23((2)° for the re-entrant membrane and h
) 0.69 ((0.07) mm, l ) 0.56 ((0.02) mm, t ) 0.14
((0.03) mm, w ) 0.128 ((0.005) mm, R ) +23((2)° for
the conventional membrane (see Figure 1 for definition
of geometrical parameters).
3. Membrane Characterization
Mechanical testing of the honeycomb materials was
carried out on a Shimadzu AGS-D 10 kN universal
testing machine, using both 10 kN and 500 N load cells.
Load data were synchronously logged with displacement
data obtained both parallel and transverse to the
loading direction using a videoextensometer (Mess-
physik VideoExtensometer package, Messphysik, La-
borgeräte Ges.M.B.H., Fürstenfeld, Austria). The video-
extensometer used differential contrast on a digitized
image of the specimen obtained from a CCD (charge
coupled detection) video camera (Mintron OS-65D),
giving image data of 480 × 640 pixels, to measure
displacements. The magnification (ratio of a given
distance on the acquired digital image divided by the
known actual value of this distance) was 19, giving a
resolution of (2 µm corresponding to a strain of
(10-4.
Four sets of output were recorded with each test,
these being the instantaneous run time of the data
points, the load developed on stretching the specimen,
and the length and width of the specimen. For the
overall deformation of the honeycomb specimens, the
latter were measured by an “indirect” means, namely,
the movement of thin, bright, adhesive markers placed
on the specimen, as detected by the videoextensometry
software that is capable of automatically measuring
images by changes in contrast. These markers were
placed toward the periphery of the honeycomb so
that the average deformation behavior of a large num-
ber of cells (>20) could be determined. From the raw
data, the stress and longitudinal and lateral strains
were calculated.
A simple demonstration of the feasibility of employing
auxetic membranes in filter defouling operations was
performed by challenging the re-entrant membrane with
glass chromatography beads of diameter 0.42 ((0.02)
mm. The beads were on average slightly larger than the
“size” of the pores of the membrane so that there was
little transmission of the beads from one side of the
membrane to the other in the undeformed state. A series
of tensile tests were performed and the subsequent bead
transmission with strain measured for the re-entrant
membrane. This was achieved by counting the number
of blocked (or vacant) pores in the field of view at regular
time/strain intervals from a video recording of a con-
tinuously strained membrane.
In total eight particle transmission tests were per-
formed for loading in the x direction and five were
performed for loading in the y direction. This number
of tests was carried out to determine a representa-
tive average of the strain-dependent defouling proper-
ties with an acceptable level of experimental uncer-
tainty.
In the case of the conventional membrane it was not
possible to observe particle transmission for the range
of bead sizes available. For beads of diameter 0.68
((0.05) mm all the beads passed through the conven-
tional membrane in the undeformed state, whereas for
beads of diameter 1.03 ((0.03) mm no particle trans-
mission was observed in either the undeformed state
or in a strained state up to a tensile strain of ∼1.5%.
4. Results
4.1. Mechanical Properties. Typical longitudinal
versus transverse extension data are presented in
Figure 4a,b for the re-entrant and conventional (hex-
agonal) cases, respectively. It is clear, from the width/
extension curves of Figure 4a,b, that the re-entrant
honeycomb expands laterally when stretched while the
conventional honeycomb contracts laterally.
This is also illustrated in Figure 5a,b where the
transverse true strain x is plotted versus the longitu-
dinal true strain y applied in the y direction. The slope
of this plot gives Poisson’s ratio -νyx (see for example
ref 23). An analogous set of data was obtained for the
orthogonal direction, giving -νxy. Young’s modulus in
each case was determined from the initial slope of the
stress-strain curves (Figure 6a,b). The overall results
are summarized in Table 1. In all cases the honeycombs
remained linear elastic up to strains of about 0.01.
The mechanical properties for honeycomb networks
for deformation due to rib hinging or flexure have been
 Ind. Eng. Chem. Res., Vol. 39, No. 3, 2000 657

Figure 5. (a) Longitudinal vs transverse true strain data for re-

entrant honeycomb membrane; (b) longitudinal vs transverse true
strain data for conventional honeycomb membrane. Deformation
Figure 4. (a) Longitudinal vs transverse extension data for re- is due to an applied load in the y direction in both cases.
entrant honeycomb membrane; (b) longitudinal vs transverse
extension data for conventional honeycomb membrane. Deforma-
tion is due to an applied load in the y direction in both cases.
shown that24

(tl)
3
derived elsewhere12,13,24 and are simply quoted here: Kf ) Esw (4)
cos2 R
νxy ) νyx-1 ) (1) where Es is the intrinsic Young’s modulus of the rib
(hl + sin R) sin R material and t is the rib thickness defined in Figure 1.
Similarly, if hinging is considered to be due to shearing
K cos R of the material at the cell wall junction, Kh has been
Ex ) (2) shown to take the form24
h
( )
w + sin R sin2 R
l
h
Kh ) Gsw (tl) (5)

Ey )
l (
K + sin R ) (3)
w cos3 R
where Ex and Ey are Young’s moduli due to loading in
the x and y directions, respectively, h, l, and R are the
geometrical parameters defined in Figure 1, w is the
depth of the honeycomb ribs, and K is the force con-
stant for the hinging (Kh) or flexure (Kf) deformation
mechanism. From standard beam theory it has been
where Gs is the shear modulus of the cell wall material.
The shear mechanism for hinging is expected to be
important for cells where the rib aspect ratio l/t is small.
Note that Poisson’s ratios for honeycomb networks are
identical when deformation is due to hinging or flexure,
depending only on the geometrical parameters of the
network (eq 1). The expressions for Young’s moduli
associated with the hinging and flexure mechanisms
differ only by the form of the respective force constants.
658 Ind. Eng. Chem. Res., Vol. 39, No. 3, 2000

Table 1. Values for ν and E for Conventional and Auxetic HoneycombssTheory and Experiment
νxy νyx Ex, GPa Ey, GPa
Conventional Membrane
experimental 0.86 ( 0.06 0.6 ( 0.1 0.23 ( 0.04 0.130 ( 0.001
theory (flexure)12 1.4 ( 0.3 0.7 ( 0.1 0.2 ( 0.2 0.12 ( 0.08
theory (concurrent)13,24 1.0 ( 0.2 0.6 ( 0.1 0.15 ( 0.08 0.09 ( 0.05
Re-entrant Membrane
experimental -1.82 ( 0.05 -0.51 ( 0.01 0.127 ( 0.006 0.032 ( 0.006
theory (flexure)12 -2.0 ( 0.2 -0.49 ( 0.05 0.10 ( 0.03 0.024 ( 0.006
theory (concurrent)13,24 -1.8 ( 0.1 -0.44 ( 0.04 0.08 ( 0.02 0.021 ( 0.005

membrane, variation between the two sets of data is

Figure 6. (a) Stress-strain data for re-entrant honeycomb
membrane; (b) stress-strain data for conventional honeycomb
membrane. Deformation is due to an applied load in the y direction
in both cases.
The theoretical mechanical properties for the mem-
branes studied here are also presented in Table 1,
calculated using eqs 1-4 and assuming deformation is
due to rib flexure when Young’s moduli are calculated.
The value of Es, the stiffness of the polymer material,
was obtained by testing a piece of the unablated polymer
material, yielding a value of the intrinsic material
modulus Es ) 4.4 ((0.6) GPa.
The agreement between experiment and theory for
Poisson’s ratio and Young’s modulus data is generally
good. With the exception of νxy for the conventional
within the calculated uncertainties.
4.2. Particle Transmission. Figure 7 shows stills
from a video recording of the particle transmission
experiments for loading of the re-entrant membrane in
the x direction. The stills cover a strain range of 0 e x
e 0.01, which is indiscernible by the eye in Figure 7.
The glass beads, which were initially resting on the re-
entrant cells, began to fall through the membrane pores
as tensile strain is applied. It should be noted that in
the particle transmission experiments the negative
values of Poisson’s ratios were smaller in magnitude
than those originally measured (νxy ∼ -1.4 and νyx ∼
-0.18, cf. -1.82 and -0.51, respectively) due to the
advent of three broken ribs in the membrane at this
stage of the experiment. These imperfections and other
small variations in geometrical parameters (of the
membrane and the beads) probably account for the fact
that not all beads were transmitted at the same instant.
The normalized fraction of blocked pores, averaged
over all tests, is plotted versus the loading strain in
Figure 8 for loading in the x and y directions. The data
are normalized to account for different levels of fouling
at the start of each test (i.e., n/n0 ) 1 initially for the
best fit line to each set of loading data, where n is the
number of blocked pores in the field of view and n0 is
the initial number of blocked pores in the field of view).
The principle of mechanical control of the sieving or
filtering action of the membrane is clear from Figures
7 and 8. Furthermore, Figure 8 shows the rate of
defouling is dependent in some manner on the value of
Poisson’s ratio, as indicated by the different slopes of
the data for loading in the x and y directions (slopes )
-30.00 and -9.46, respectively).
It was not possible to observe similar particulate
defouling behavior with the conventional honeycomb
membrane, because of the beads available for testing
purposes being either too small (and therefore passing
through the membrane in the undeformed state) or too
large for significant pore variation to be achieved
without the membrane yielding plastically. The case of
using a conventional membrane in this scenario is,
however, discussed below.
5. Discussion and Conclusions
The requirement of a quadratic strain energy function
and hence of a symmetric stiffness matrix for an
orthotropic linear elastic material implies the following
relationship should be satisfied:25
νxyEy
)1 (6)
νyxEx
From the experimental data in Table 1, we find (νxyEy)/
(νyxEx) ) 0.8 ((0.2) and 0.9 ((0.2) for the conventional

Figure 7. Video stills of re-entrant membrane defouling when challenged by glass chromatography beads: (a) ∼60% bead coverage on
an undeformed membrane; (b) ∼50% bead coverage at a strain of 0.5% in the x direction; (c) ∼40% coverage at a strain of 0.75% in the
x direction; (d) ∼30% coverage at a strain of 1% in the x direction.
Figure 8. Averaged normalized fraction of blocked pores vs
loading strain for the re-entrant membrane challenged by glass
beads. Data for loading in the x and y directions are shown.
and re-entrant honeycomb membranes, respectively.
Hence, the experimental data are consistent, within
experimental error, with classical anisotropic elasticity
theory.
Similarly, the requirement that the strain energy of
an orthotropic material be positive definite for static
equilibrium leads to25
()
Ex 1/2
|νxy| e
Ey
which is also satisfied by the experimental data in Table
1 for both membranes.
The excellent agreement between theory and experi-
ment clearly demonstrates that honeycomb structures
can be designed and fabricated using femtosecond laser
ablation with specifically tailored mechanical properties.
Auxetic and nonauxetic structures can be made from
the same material by modifying the geometry of the
structure, for example, by changing R or h/l.
5.1. Deformation Mechanisms and Force Con-
stants. In a comparison of the experimental mechanical
properties with theory, it was assumed that deformation
of the micromachined structures was via flexure of the
honeycomb ribs. This is vindicated by comparing the
force constants for rib flexure and hinging given in eqs
4 and 5, which leads to
Kf Es t 2 t2
)
K h Gs l ()
) 2(1 + νs)
l ()
where νs is Poisson’s ratio of the rib material which we
Ind. Eng. Chem. Res., Vol. 39, No. 3, 2000 659
assume to be isotropic, allowing us to use the standard
relation from classical elasticity theory of isotropic
materials: Es ) 2Gs(1 + νs). Experimentally, we deter-
mined νs ) 0.56 ((0.10), which is consistent with the
maximum positive value of +1/2 allowed by classical
elasticity theory for isotropic materials, or may be
indicative of some degree of anisotropy in the film due
to the drawing process during manufacture. Hence,
employing the values of t/l established above, we find
for the conventional honeycomb structure Kf/Kh ) 0.18
((0.08), and for the re-entrant honeycomb structure Kf/
Kh ) 0.08 ((0.01). The lower the value of the force
constant for a given deformation mechanism, the more
significant that mechanism becomes,13,24 and so we see
that flexure dominates over hinging for both types of
membranes in this case.
A third possible deformation mechanism exists for
these membranes, corresponding to stretching of the
ribs in response to an applied load. In this case the force
constant is given by13,24
Ks ) Esw (tl) (9)
leading to Kf/Ks) 0.06 ((0.02) and 0.026 ((0.003) for
the conventional and re-entrant honeycomb membranes,
respectively. Hence, flexure again dominates.
A model has been developed where all three deforma-
tion mechanisms act concurrently.13,24 An example of
the concurrent model expression is given here for νxy:
(7)
sin R cos2 R
[1
+
1
-
Kf Kh Ks
1
]
( )[( ]
νxy ) (10)
h
l
+ sin R
1
+
1
Kf Kh )
sin2 R +
cos2 R
Ks
To check the validity of the force constant expressions
(eqs 4, 5, and 9), the concurrent model calculations for
the membranes considered here are also presented in
Table 1. Again, good agreement is achieved with experi-
ment, as expected because flexure dominates and we
have already seen that the experimental data are in
good agreement with the flexure model. The concurrent
model predictions are slightly different from those of the
flexure model (because of the influence of the hinging
and stretching mechanisms), but the experimental
errors are too large to enable a definitive statement as
to which model best represents the experimental data.
(8) Note, though, that the experimental νxy value for the
conventional membrane agrees within error with the
concurrent model predictions. This was found not to be
true using the flexure model alone.
660 Ind. Eng. Chem. Res., Vol. 39, No. 3, 2000

5.2. Strain-Dependent Deformation. The strain-

dependent deformation and particle transmission of the
membranes considered here have also been investigated;
see Figures 5-8. We have also developed simple ana-
lytical expressions for the maximum inscribed sphere
for the pores of both membranes. It is, therefore,
possible to model the particle transmission with strain
for both membranes, assuming deformation is due to
rib hinging (i.e., R varying); see below. However, it has
been noted above that rib flexure appears to dominate
the deformation of the membranes. Hence, in the
following we consider the strains in the x and y direc-
tions for deformation to be due to rib flexure and hinging
to (i) facilitate comparison with the experimental strain
data (Figure 5a and 5b) and (ii) compare the strain data
for rib flexure and rib hinging to assess the viability of
subsequently using the hinging model to model the
experimental strain-dependent particle transmission
data.
True strains are evaluated from

x ) ln ( )
X
X0
) ln(1 + ex) (11)

where X and X0 are the deformed and undeformed unit-

cell lengths in the x direction, respectively, and ex is the
engineering strain in the x direction. Similar expres-
sions exist for strain in the y direction.
For example, in the case of the flexure model, ex is
given by12

δ
ex ) tan R (12)
l
where δ is the deflection of the rib undergoing flexure.
In the flexure model, therefore, strains are calculated
by varying δ, while maintaining l and R constant. This
is applicable to low strains where beam theory26 is valid,
as is the case for the experimental data presented in
Figures 5 and 6.
In the case of the hinging model x is given by

( )
cos R
x ) ln (13)
cos R0
where R and R0 are the deformed and undeformed
honeycomb angle, respectively. In the hinging model
strains are therefore calculated by varying R while
maintaining all other geometrical parameters constant.
In Figure 9a we show the comparison of the experi-
mental x versus y data with the flexure and hinging
models for the re-entrant membrane. The two models
are almost coincidental throughout the entire strain
range (0 e y e 0.010). Furthermore, the agreement
with the experimental data is also good, with the models
having only a slightly lower gradient than that shown
by the experimental data. This is of course reflected in
the excellent agreement between the theoretical and
experimental values of νyx for the re-entrant honeycomb
membrane (see Table 1).
The experimental and theoretical (flexure and hinging
models) x versus y data for the conventional membrane
are shown in Figure 9b. Again, the hinging and flexure
models give almost identical results throughout the
strain range considered in Figure 9b. The experimental
trends are also reasonably well reproduced, although
there is slightly more discrepancy in the model and
experimental slopes for the conventional membrane
Figure 9. (a) Theoretical (hinging and flexure models) and
experimental x vs y data for the re-entrant honeycomb mem-
brane; (b) theoretical (hinging and flexure models) and experi-
mental x vs y data for the conventional honeycomb membrane.
Hinging model ) solid line; flexure model ) dashed line.
than for the re-entrant membrane (Figure 9a). However,
we note that the calculated uncertainties in the slope
of the model curves are of the order of 15-20% (see
flexure model νxy and νyx data in Table 1).
Hence, the experimental strain data agree within the
calculated uncertainties with the flexure model data.
It also appears reasonable to use the rib hinging model
as a first approximation to model other strain-depend-
ent properties (e.g., particle transmission) for these
membranes.
5.3. Strain-Dependent Particle Transmission. In
the simple particle transmission tests performed here
we have demonstrated the potential of auxetic materials
or structures in filtration applications, specifically in the
cleaning of fouled membranes. This has been achieved
by the application of a uniaxial load or displacement to
open up the pores in a manner unique to auxetic
materials or structures, thereby allowing the passage
of glass beads from one side of the re-entrant membrane
to the other. This was not observed in the comparative
tests on the conventional membrane. This may be due
to the fact that the conventional honeycomb cells simply

Figure 10. The maximum radius of a sphere capable of passing
through the pores of the re-entrant and conventional honeycombs
studied here plotted as a function of loading strain in the y
direction. The values are normalized to the radius of the inscribed
sphere at the undeformed geometry (y ) 0). Geometrical values
determined experimentally (see text) were used in the calculations.
The pore walls constraining the maximum sphere size are shown
schematically in the figure.
contract in the lateral dimension when stretched lon-
gitudinally (see Figure 1), thus reducing the size of the
sphere able to pass through the membrane. Alterna-
tively, it may be due to the beads employed in the test
not having a diameter with a close enough match to the
conventional pore size in this case.
To clarify this issue further, we have modeled various
situations involving the admission of a uniform sphere
through six-sided re-entrant and conventional cells.
Although we have ascertained that rib flexure is the
dominant mechanism, we have seen that the strain and
Poisson’s ratio calculations are almost identical between
the flexure and hinging models and so the maximum
bead size analysis assumes deformation is due to rib
hinging for simplicity.
In this analysis, the maximum inscribed sphere
radius R when the vertical pore ribs constrain the
sphere (see Figure 10) is given by
t the bead size, and so the angle corresponding to the
R ) l cos R - (14)
2
Equation 14 is valid for both the conventional and re-
entrant honeycomb geometry.
In the case where the diagonal ribs constrain the
bead, for the conventional membrane we have
h t
R) cos R + l sin R cos R - (15)
2 2
and for the re-entrant membrane
h π R t
R)
2 (
tan + -
4 2 2 ) (16)
Figure 10 shows the variation in the radius of the sphere
able to pass through the pores of conventional and re-
entrant membranes having the geometrical parameters
established above for the membranes considered in this
paper. The radius is plotted versus the applied strain
Ind. Eng. Chem. Res., Vol. 39, No. 3, 2000 661
in the y direction and has been normalized to the radius
of the sphere able to pass through the pore in the
undeformed membrane in each case. In effect, the
normalization enables a comparison between re-entrant
and conventional membranes having the same initial
effective pore size. In the calculations we have assumed
deformation to be due to rib hinging.
For the re-entrant membrane, it is clear that the size
of the particle that can pass through the membrane can
be increased significantly by applying a tensile load or
strain in the y direction. The size of the particle is in
this case constrained by the diagonal ribs (length l). The
case where the particle is constrained by the vertical
ribs (length h) is possible but requires h/l > 2.
From eq 16 the geometrical parameters measured for
the re-entrant membrane (see above) yield a maximum
bead diameter ()2R) for transmission through the
membrane of 0.43 ( 0.03 mm. This corresponds well
with the known value of 0.42 ((0.02) mm for the beads
employed in the test, enabling this simple bead and
membrane system to demonstrate proof of principle for
auxetic materials or structures in filter defouling or size
selectivity operations.
For the conventional membrane the size of particle
that the pore can accommodate is at a maximum (within
error) when the membrane is in the undeformed state
for the membrane geometry considered here. Equation
15 yields a value for the maximum inscribed bead
diameter for the pores of the conventional membrane
of 0.89 ( 0.05 mm, which explains why the beads of
diameter 0.68 ((0.05) mm passed through the unde-
formed membrane whereas those of diameter 1.03
((0.03) mm did not. Application of a tensile or compres-
sive load or strain in either direction for the conven-
tional membrane only leads to a decrease in the size of
bead able to pass through the membrane, which ex-
plains why the 1.03-mm diameter beads were not
transmitted when the conventional membrane was
deformed. The conventional membrane is, therefore,
unsuitable for the type of defouling operation afforded
by the auxetic membrane.
The maximum particle size a conventional honeycomb
membrane (with h/l < 2) can accommodate occurs at
the geometry at which the ribs constraining the particle
change from being the diagonal ones to the vertical ones
(see Figure 10). (For a conventional honeycomb mem-
brane with h/l g 2 the vertical ribs always constrain
maximum particle size occurs at R ) 0°.) Clearly, it is
possible to design conventional honeycombs (with h/l <
2) with an undeformed pore “size” away from the
maximum, which would allow some potential defouling
operation due to increasing the pore size. However,
away from the “regular hexagon” geometry other effects
due to, for example, pressure drop and particle flux
through the membrane may need to be taken into
account.
The rate of particulate defouling with loading strain
has been found to be related in some manner to
Poisson’s ratio for the particular direction of loading (see
Figure 8). Consider the case of loading in the y direction.
Here, the rate of defouling with respect to the loading
strain (y) is related to the rate of defouling with respect
to the transverse strain (x) by
(d(n/n0)
dy ) (
σy
)-
dx )
d(n/n0)
νyx
σy
(17)
662 Ind. Eng. Chem. Res., Vol. 39, No. 3, 2000

where the subscript σy indicates that the strain-depend-

ent rates of defouling are due to an applied load in the
y direction, and we have used the definition for Poisson’s
ratio of

dx
νyx ) - (18)
dy

which is applicable to nonlinear as well as linear

deformation.23,27 If we assume that the rate of defouling
with strain in a given direction is independent of the
direction of loading, for example,

(d(n/n0)
dx ) (
σx
)
d(n/n0)
dx )
σy
(19)

then, from eqs 17 and 19, the ratio of the slopes of the Figure 11. Averaged normalized fraction of blocked pores vs
strain in the x direction for the re-entrant membrane challenged
two curves in Figure 8 is given by by glass beads. Data for loading in the x (crosses) and y (circles)

( )
directions are shown. Also shown is the calculated curve assuming
d(n/n0) a normal cumulative distribution of glass bead sizes having a mean
value of R/l ) 0.415 and a standard deviation of 0.019. All
dx σx 1 membrane geometrical parameters were as observed experimen-

( )
)- (20) tally.
d(n/n0) νyx
dy σy where [d(n/n0)/dx)]σx is the gradient of the straight line
()-30.00 in Figure 8). Similarly, for loading in the y
Similarly, it can also be shown that the ratio of the direction

( )
slopes is related to νxy by
d(n/n0)

( )
n
d(n/n0) ) y + 1 (23)
n0 dy σy
dx σx

( )
) -νxy (21)
d(n/n0)
dy σy
In the case of the flexure or hinging models, eq 1 is valid
and eqs 20 and 21 are equivalent. However, for models
or structures where νxy * νyx-1, the assumption that the
rate of defouling with strain in a given direction is
independent of the direction of loading may not be valid.
This is the case for the concurrent model and mem-
branes discussed in this paper. Furthermore, the mem-
brane used in the particle-transmission experiment
contained a small number of damaged ribs, further
invalidating the assumption in eq 19. In such cases, eqs
20 and 21 give different values, which we take to be
the limiting cases.
Taking the average of eqs 20 and 21 for Poisson’s
ratios associated with the membrane during the particle
transmission experiment (νxy ) -1.4 and νyx ) -0.18)
gives a predicted ratio of the slopes for Figure 8 of 3.5,
which is in good agreement with the observed value of
3.2. Hence, the magnitude of Poisson’s ratio is a
measure of the sensitivity of the membrane to changes
in the pore size.
To check for consistency in the particle transmission
data for loading in the x and y directions, plotted versus
the loading strain (i.e., x and y, respectively) in Figure
8, it is instructive to plot the data versus the strain in
one direction only. To a first approximation each set of
data in Figure 8 can be fitted by a straight line which
in the case of the x-loaded data is given by
n
n0
) (
d(n/n0)
dx )σx
x + 1 (22)
Equations 20 and 21 provide conversion between the
gradients of the straight lines in Figure 8, defined by
eqs 22 and 23. Taking the average of the rate of
defouling with respect to strain for loading in the x
direction given by eqs 20 and 21 (due to the assumption
that the rate of defouling with strain in a given direction
is independent of the direction of loading being invalid
in this case; see above), we have
1
( )
〈( ) 〉 ( )
+ νxy
d(n/n0) νyx d(n/n0)
)- (24)
dx σx 2 dy
σy
Rearranging eq 22 and substituting eqs 23 and 24 yields
2y
x ) -
( )
(25)
1
+ νxy
νyx
Equation 25 provides the necessary conversion factor
to enable the particle transmission data due to loading
in the y direction to be plotted versus the same strain
as the data due to loading in the x direction. (Note that
if the assumption of the rate of defouling being inde-
pendent of the loading direction was valid, then νxy )
νyx-1 and so eq 25 would simplify to x ) -νyxy.)
This is illustrated in Figure 11 where the experimen-
tal normalized fraction of blockages (n/n0) are plotted
versus x for uniaxial loading along both the x and y
directions. In Figure 11, the data due to loading along
the x axis (crosses) are as given in Figure 8. The data
due to loading along the y axis (circles) have also been
included by using eq 25 to convert the strain data. Using

this method, it is readily seen that the data for loading
along the x and y directions are consistent, because they
now overlap once the effects of Poisson’s ratios and
loading direction have been taken into account.
For a bead/membrane system consisting of beads of
exactly identical shape and size, and a membrane
having exactly identical pore structure and rib geometry
throughout the membrane, it might be expected that
complete defouling would occur at the instant the pore
size exceeds the bead diameter. In reality, of course, the
beads will have a distribution of sizes, and there will
be some variation in the pore geometry across the
membrane, leading to particle transmission occurring
across a range of strains, as observed in Figure 8.
Therefore, we have modeled the particle transmission
through the re-entrant membrane assuming a normal
distribution of particle sizes going through pores of a
particular size governed by eq 16 for the membrane
geometry considered in this paper. In the calculations,
therefore, those particles in the distribution having a
radius less than that determined from eq 16 are
considered to be transmitted through the membrane.
Particle transmission was calculated for varying R (i.e.,
assuming membrane deformation is due to rib hinging).
The normalized fraction of blockages calculated in this
way are also plotted in Figure 11 (solid curve), using
eq 13 to convert the variations in R to x.
The model curve is normalized to n/n0 ) 1 at the
undeformed geometry to ensure consistency with the
experimental data. A normal cumulative distribution of
particles having a mean value of R/l ) 0.415 and a
standard deviation of 0.019, with all other membrane
geometrical parameters as observed experimentally,
gives the best fit to the experimental data in Figure 11.
The mean value of R/l employed in the calculations is,
therefore, in excellent agreement with the value of R/l
) 0.40 ( 0.04 calculated using eq 16 from the experi-
mentally determined geometrical parameters for the
undeformed membrane, which we have already seen
possesses a pore size which corresponds well with the
size of beads used in the test.
In this paper the potential of employing auxetic
materials in filter defouling operations has been con-
sidered under uniaxial loading conditions. Of course,
biaxial loading operations may be possible in certain
filtration applications. Tensile loading in either the x
or y direction leads to an increase in pore dimensions
of an auxetic membrane, and so the effects are additive
in the biaxial loading case, leading to further enhanced
pore-opening possibilities. However, for a conventional
membrane the effects due to tensile loading in each
direction oppose each other from a pore-opening point
of view (i.e., one tends to open the pore in the y direction
while closing the pore in the x direction and vice versa).
This is demonstrated by considering eq 20 or 21 where
positive Poisson’s ratio values lead to a negative ratio
of the slopes of the defouling with strain curves for
loading in the x and y directions, indicating that
defouling may be possible by loading in one direction
but not the other. Hence, once again we expect auxetic
materials or structures to offer improvements in filter
defouling operations.
An alternative mechanism for effecting pore variation
may be as a result of the passive response of a
membrane subject to a pressure-drop build-up across
the membrane as a result of membrane fouling. This
may be considered equivalent to the application of
Ind. Eng. Chem. Res., Vol. 39, No. 3, 2000 663
bending moments leading to curvature (“bowing”) of the
membrane in the direction of flow. It is known that
materials and structures possessing a negative in-plane
Poisson’s ratio undergo synclastic curvature when sub-
ject to a bending moment, whereas those possessing a
positive in-plane Poisson’s ratio undergo anticlastic
curvature.4,10 In other words, auxetic materials and
structures can be deformed into a doubly curved “dome”
shape more easily than nonauxetic materials and struc-
tures. Such deformation will lead to an increase in pore
size which, as we have demonstrated in this paper, may
be used for membrane defouling or for reducing a
pressure increase during fouling.
However, it should be noted that the bowing action
due to pressure build-up could also introduce detrimen-
tal effects such as the release of initially trapped
particulates into the downstream. The transmission of
particles through the filter due to bowing may also
hinder the establishment of the more effective filtration
phase where the initial deposit acts as part of the
filtering media to trap finer particles.
In the case of thick filtering media then the bowing
mechanism may not be applicable. In this case the
pressure build-up across the filter would tend to close
the pores which would oppose the effect of tensile lateral
forces that may be applied to open up the pores for
defouling purposes. Clearly, the anticipated forces due
to pressure build-up need to be considered in the design
and selection of the appropriate filter material and
control system to ensure satisfactory defouling occurs
in reality.
The pore-opening properties characteristic of auxetic
materials and structures may also be of benefit in
applications where, for example, tuneable pore size
variations or oscillations are required, or where dynamic
alterations of pore size are needed.
Auxetic materials and structures have potential in
smart filtration applications requiring both active and
passive control of the pore size. Future work will involve
the use of alternative fabrication techniques to enable
auxetic structures having smaller pore sizes to be
fabricated and tested. For example, the LIGA (Lithog-
raphie, Galvanoformung, Abformung) micromachining
technique, which employs lithography, electroplating,
and moulding processes to manufacture finely defined
microstructures for use in microelectronic and micro-
filtration components, for example, has been used to
fabricate conventional honeycomb structures having
pores up to 2 orders of magnitude smaller than the
membranes fabricated and tested here. Hence, this
technique enables the possibility of auxetic membranes
for use in practical air filtration systems to be consid-
ered. Scaled-down auxetic honeycombs may also find
use in biomedical applications such as ultrafiltration
and drug-release membranes where the filtering or
release of a clearly defined dose of similarly sized cells/
molecules is required.
The fabrication, characterization, and testing of aux-
etic forms of more realistic filter materials than the
membrane studied here for the proof-of-concept dem-
onstration are also now required. Auxetic forms of
polymeric foams used in air filtration are known,4 which
are obvious choices for study in this respect. Auxetic
foams could also be used to support auxetic membranes,
similar to the one studied here, for large-scale filtration
operations. In this case the support would be required
to be highly deformable and have a larger effective pore
664 Ind. Eng. Chem. Res., Vol. 39, No. 3, 2000
size and matching in-plane Poisson’s ratios with respect
to the membrane for the auxetic membrane to exhibit
the full benefits in filter defouling and size selectivity
demonstrated here. Auxetic metallic foams4 should also
be useful in this respect, particularly in applications
where increased support stiffness is required. Alterna-
tively, deeper honeycomb monoliths having larger ef-
fective pore sizes could be used to support honeycomb
membranes. Because of the scale-independent nature
of the auxetic effect, the analytical models described in
this paper would enable a close match of the in-plane
mechanical properties of the membrane and the mono-
lith to be achieved in this scenario.
6. Summary
In summary, we have used femtosecond laser ablation
to fabricate micromachined auxetic and nonauxetic
polymeric membrane structures. The structures have
mechanical properties in good agreement with the
flexure model for the deformation of honeycombs, and
also in good agreement with a more detailed model in
which deformation due to rib hinging and stretching are
also incorporated. The experimental data are consistent
with both models because of flexure being the dominant
mechanism in the real structures. Simple tests have
been performed, demonstrating that auxetic membranes
have beneficial properties over conventional membranes
in filter defouling and controlled pore size applications.
The strain-dependent defouling is seen to be dependent
on the value of Poisson’s ratios of the membrane.
Acknowledgment
This work has been funded by BNFL and the Engi-
neering and Physical Sciences Research Council of the
United Kingdom.
Nomenclature
ex ) engineering strain along the x direction
Es ) intrinsic Young’s modulus of honeycomb rib material,
GPa
Ex ) Young’s modulus in the x direction, GPa
Ey ) Young’s modulus in the y direction, GPa
f ) flat field lens focal length, mm
Gs ) intrinsic shear modulus of honeycomb rib material,
GPa
h ) vertical honeycomb rib length, mm
Kf ) flexure force constant, N/m
Kh ) hinging force constant, N/m
Ks ) stretching force constant, N/m
l ) diagonal honeycomb rib length, mm
n ) number of blocked pores in the field of view
n0 ) initial number of blocked pores in the field of view
R ) radius of inscribed sphere, mm
t ) honeycomb rib thickness, mm
w ) honeycomb rib depth, mm
X ) deformed unit-cell length along the x direction, mm
X0 ) undeformed unit-cell length along the x direction, mm
R ) honeycomb angle, deg
R0 ) undeformed honeycomb angle, deg
δ ) deflection of honeycomb rib due to flexure, mm
x ) true strain along the x direction
y ) true strain along the y direction
νs ) intrinsic Poisson’s ratio of honeycomb rib material
νxy ) Poisson’s ratio for uniaxial loading along the x
direction
νyx ) Poisson’s ratio for uniaxial loading along the y
direction
σx ) applied stress along the x direction
σy ) applied stress along the y direction
τp ) laser pulse length, fs
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Received for review August 2, 1999
Revised manuscript received November 23, 1999
Accepted November 24, 1999
IE990572W