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Acta Materialia 66 (2014) 326339
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Characterization and deformation response of orthotropic

bre networks with auxetic out-of-plane behaviour
S. Neelakantan, W. Bosbach, J. Woodhouse, A.E. Markaki
Department of Engineering, University of Cambridge, Trumpington Street, Cambridge CB2 1PZ, UK
Received 9 July 2013; received in revised form 5 November 2013; accepted 5 November 2013
Available online 5 December 2013

Abstract
In the present paper, highly porous bre networks made of 316L bres, with dierent bre volume fractions, are characterized in
terms of network architecture, elastic constants and fracture energies. Elastic constants are measured using quasi-static mechanical
and modal vibration testing, yielding local and globally averaged properties, respectively. Dierences between quasi-static and dynamic
elastic constants are attributed to through-thickness shear eects. Regardless of the method employed, networks show signs of material
inhomogeneity at high bre densities, in agreement with X-ray nanotomography results. Strong auxetic (or negative Poissons ratio)
behaviour is observed in the through-thickness direction, which is attributed to bre kinking induced during processing. Measured fracture energies are compared with model predictions incorporating information about in-plane bre orientation distribution, bre volume
fraction and single bre work of fracture. Experimental values are broadly consistent with model predictions, based on the assumption
that this energy is primarily associated with plastic deformation of individual bres within a process zone of the same order as the interjoint spacing.
2013 Acta Materialia Inc. Published by Elsevier Ltd. All rights reserved.
Keywords: Elastic constants; Mechanical properties; Porosity; X-ray tomography; Fibre networks

1. Introduction
Highly porous materials, particularly those based on
metals, are currently attracting a lot of research interest.
Their high surface-to-mass ratio means that they can be
attractive in terms of transport phenomena characteristics,
leading to applications involving heat transfer, ltration,
catalyst support, acoustic damping and also biomedical
devices. Porous metals are used for hard (e.g. bone) tissue
repair and reconstruction. For instance, titanium bre
coatings are commercially used in total hip prostheses such
as the Zimmer VerSys Epoch Full Coat Hip Prosthesis [1].
The rationale behind this design is that porous implant surfaces favour bone anchoring by providing space for inltration, rst by cells and ultimately by osseous tissue and
vasculature.
Corresponding author. Tel.: +44 1223 766417; fax: +44 1223 332662.

E-mail address: am253@cam.ac.uk (A.E. Markaki).

Some porous materials are divided up into cells of some

sort and are sometimes termed cellular. Those specically designed to be highly porous (>50% porosity) are
often referred as foams, although it should be acknowledged that there is no universally accepted denition of a
foam. It is important to recognize the distinction between
open-cell foams and bre networks. The latter are constructed by assembling a set of slender members such as
bres, wires or rods and bonding them at crossover points.
While both are permeable to uid and abundant in nature
(cancellous bone, sponge, sheeps wool and cotton), bre
networks do not exhibit a distinct cell structure. Fibre
networks are sometimes classied according to whether
they are periodic or stochastic (i.e. exhibiting random variations in bre orientation distribution and spatial location). This can aect certain characteristics, particularly
mechanical properties, since it inuences the incidence of
stress concentration eects. They can be isotropic or they
may be highly oriented (e.g. ropes) and therefore exhibit

1359-6454/$36.00 2013 Acta Materialia Inc. Published by Elsevier Ltd. All rights reserved.
http://dx.doi.org/10.1016/j.actamat.2013.11.020

S. Neelakantan et al. / Acta Materialia 66 (2014) 326339

pronounced anisotropy in both structure and properties.

When characterizing bre networks, the microstructure of
the material constituting the bre is as important as the
network architecture (e.g. bre orientation distribution,
bre segment aspect ratio (inter-joint distance to bre
diameter)). With the advent of digital imaging, the network
architecture is most eectively captured by computed X-ray
tomography [2,3].
There have been several previous experimental studies of
the mechanical response of stochastic metallic bre networks made of Cu [4], Ti [5], 20%Cr80%Ni [6], steel [7
9] and stainless steel [1022] bres (in particular 304
[10,11], 316L [1218] and 446 [1922]). The majority of
these studies focused on the eect of bre size and volume
fraction on tensile [4,6,1014,17,19], compressive
[5,7,13,17,18,2022], torsional [8,17] and impact [9]
responses. Optimization of their performance clearly
requires an understanding of the interplay between processing conditions, network architecture, bre microstructure and mechanical response characteristics under
various types of applied load.
It is important to note that existing studies use small test
specimens, which typically yield only local properties.
However, the response of a structure to imposed loads is
governed by the globally averaged properties. Fibre networks are in many respects intermediate between materials and structures. Furthermore, when measuring
elastic constants, conventional mechanical testing usually
involves much higher applied loads than dynamic methods.
This is potentially important, as it is well known that, in
highly porous materials, local plastic deformation occurs
readily, even at low macroscopic strains (wherein the deformation is expected to be linear).
Auxeticity, i.e. negative Poissons ratio m, has been associated with enhancement of material properties related to
Poissons ratio [23]. Approaches to designing auxetic bre
composites involve the use of auxetic constituents (usually
polymeric bres) or selection of suitable stacking sequences
of highly anisotropic unidirectional bre-reinforced laminate (mostly ceramic bres in a polymeric matrix) [24].
Negative Poissons ratios have been measured experimentally [14,17] and predicted theoretically [25,26] for stochastic metallic bre networks of the type investigated in the
present study.
The present work involves a systematic investigation of
the architecture, deformation and fracture of 316L austenitic stainless steel bre networks with dierent bre volume
fractions. Network architectural characteristics, such as
bre orientation distributions and the mean bre segment
length, were obtained from X-ray tomography. The inplane Youngs moduli of the networks, and also their inand out-of-plane Poissons ratios, were measured using
quasi-static mechanical (tensile and cantilever bend) and
dynamic vibration (plate and beam) testing. Vibration testing automatically provided an estimate of the globally
averaged properties of the networks. A comparison
between the dierent testing methods is presented. Esti-

327

mates of the nominal fracture energy of the networks were

obtained using a simple method based on analysis of tensile
stressdisplacement plots. Experimental values were compared with predictions obtained using an analytical model,
based on the assumption that this energy is primarily associated with plastic deformation of individual bres within a
process zone neighbouring the fracture plane.
2. Materials and methods
2.1. Materials
The present study focuses on AISI 316L austenitic stainless steel in the form of single bres and sintered bre networks (N.V. Bekaert S.A., Belgium).
2.1.1. Single bres
The 316L bres were produced by a bundle-drawing
process [27]. This process involves forming a bundle of
metallic wires, each coated with a sacricial (separation)
layer, encasing the bundle in a tube and drawing the tube
to smaller diameters. Bundle drawn bres exhibit a hexagonal cross-sectional shape. Fig. 1a and b shows optical
micrographs of transverse sections of 316L bres in asreceived and as-heat-treated conditions, respectively. It
can be seen that the diagonal width of the bres is
40 lm (the side length is 20 lm).
2.1.2. Sintered bre networks
Fibre network plates were produced by solid-state sintering at N.V. Bekaert S.A. (Belgium). In particular, loose felts
of bundle-drawn bres were stacked upon one another with
a random planar orientation, and compressed to plates with
three dierent bre volume fractions f; 10, 15 and 20 vol.%.
The plate dimensions were either 297 mm  210 mm 
5 mm or 297 mm  210 mm  2 mm in the longitudinal
(x), transverse (y) and through-thickness (z) directions,
respectively. There were variations within the labelled bre
volume fractions arising from processing. For the 5-mmthick network sheets, the measured bre fraction values were
10.3% (0.003), 14.8% (0.002) and 20.2% (0.39). The
corresponding values for the 2-mm-thick network sheets
were 9.2% (0.36), 14.7% (0.31) and 20.3% (0.36). It is
of note that the 2 mm thick 10 vol.% network sheets had
invariably a slightly lower bre volume fraction (9.2%).
To avoid any edge eects, samples were cut at least 20 mm
in from the edges of the sheets.
2.2. Material characterization
2.2.1. Electrolytic and tint etching for optical microscopy
Cross-sections of as-received and heat-treated bres
were prepared, mounted, ground with a series of SiC
papers and afterwards further polished with 6 and 1 lm
diamond paste. Examination of bre cross sections was

performed using a Leica DMLM microscope. Electrolytic

etching was carried out using a 10% aqueous oxalic acid

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S. Neelakantan et al. / Acta Materialia 66 (2014) 326339

Fig. 1. Optical micrographs showing polished and tint-etched cross-sectional views of (a) as received and (b) heat-treated (sintered) 316L bres. SEM
images of (c) a sintered bond at an inter-bre crossing and (d) a plan view of a 10 vol.% bre network. (e) Optical micrograph showing polished and
electrolytically etched cross sections of heat-treated bres (bres do not lie normal to the plane of the section).

reagent and a voltage of 6 V DC for 35 s. This reagent

strongly attacks the r phase after 6 s, outlines (and dissolves) carbides after 1530 s and reveals grain boundaries
after 4560 s [28].
Tint etching with modied Berahas reagent (100 ml
water, 20 ml HCl, 2.4 g NH4FHF, 0.6 g K2S2O5) was used
to obtain information about the grain size and crystallographic orientation. This reagent deposits a sulde-based
surface lm that creates colour contrast through interference eects in bright-eld imaging mode. Fig. 1a and b
shows the 316L bre microstructure in the as-received
and heat-treated conditions, respectively. It can be seen
that the as-received bre (Fig. 1a) has an average grain size
of 5 lm whereas, after heat treatment (Fig. 1b), substantial grain coarsening (grain size roughly equivalent to bre
diameter) and annealing twins are observed. From the narrowness of the colour range, it can be postulated that the
as-received bres have a more preferred crystallographic
orientation than the sintered ones.
2.2.2. Scanning electron microscopy
Top views and fracture surfaces were investigated by
scanning electron microscopy (SEM), using a Zeiss Evo
MA 15 instrument in secondary mode. Fig. 1c shows a typical surface bre morphology and a sintered bond at a bre
crossing of a network containing 10 vol.% of bres
(f = 10%). It can also be seen that the bres have a coarse
recrystallized grain structure (a bamboo structure) after
sintering. A typical plan view of the network is shown in
Fig. 1d.

2.2.3. X-ray computed tomography

Tomographic data were obtained on specimens cut by
electro-discharge machining (EDM) from the network
plates into 5 mm cubes. In total, six samples (two for each
bre volume fraction) of 316L were analysed.
2.2.3.1. Equipment. Tomography scans were carried out by
a General Electric Phoenix X-ray Nanotom system
equipped with a sub-micron focal spot X-ray source. The
source voltage and current were set at 120 kV and 40 lA
respectively. The voxel size was 7.75 lm. A 0.2 mm copper
lter was used. The scans were recorded at projection
angles between 0 and 360 in steps of 0.25. To increase
the signal-to-noise ratio of the images, 12 frames were captured and averaged for each projection on a 5 megapixel
12-bit detector array.
2.2.3.2. Architecture characterization. For extraction of
architectural parameters, a sub-volume of 4  4  4 mm3
was analysed to avoid edge eects. The process involved
three steps; image reconstruction, segmentation and topological thinning. More details can be found elsewhere [3].
Briey, following X-ray acquisition, the data sets were
lter back-projected (reconstructed) to produce a series of
two-dimensional (2-D) raw greyscale images of the network. Owing to the stochastic nature of the network architecture and the inherent limitations of the ltered backprojection technique, additional ltering was applied to
improve the resolution of the tomographic images. Image
segmentation (separation of the bres from the inter-bre

S. Neelakantan et al. / Acta Materialia 66 (2014) 326339

space (air)) can be carried out by applying a global threshold for the entire image (i.e. ignoring spatial dependence of
phases) or locally by applying dierent thresholds in dierent spatial regions. In this work, a local, spatially adaptive
thresholding algorithm, known as indicator kriging [29],
was employed.
The output of the segmentation procedure is a stack of
binary images featuring only two phases, bres (black) and
air (white). The segmentation algorithm was calibrated
using the bre volume fractions obtained from a simple
volumetric technique (weight and sample dimensions) and
a density value of 7.9 Mg m3 for 316L. It is assumed that
the porosity remains the same for any sub-section within
the original sample volume. Following segmentation, the
binary images were subjected to standard post-segmentation clean-up procedures, such as removal of small blobs
and lling of holes. In the third step, the three-dimensional
(3-D) Medial Axis (3DMA) algorithm (Nihon Visual Science Inc., Japan) [30,31] was employed to reduce the 3-D
reconstructed bres to their medial axes (skeletons), preserving their shape and topology. Once the medial axes
of the bres were obtained, the local bre orientations, size
and other architectural characteristics, such as the number
of inter-bre crossings and bre segment lengths, were
extracted.
2.3. Mechanical testing
2.3.1. Single bre tensile testing
Tensile testing was carried out using a screw-driven
desktop Instron testing machine, tted with a 250 N load
cell. The individual bres were mounted across 14 mm
gauge length paper tabs, using Loctite superglue. After
gripping each tabbed specimen, prior to testing, the tab
edges were cut. The cross-head displacement was measured
using an LVDT. All tests were conducted in displacement
control at a strain rate of 104 s1. Fibres were tested in
the as-received condition and after sintering. The single
bre work of fracture (in joules per metre) was measured
as the area under the loadstrain curve.
2.3.2. Network in-plane tensile testing
In-plane tensile testing of bre networks was conducted
using an Instron testing machine equipped with a 5 kN
load cell. Dog-bone-shaped tensile specimens were electro-discharge machined from the network plates according
to ASTM E8-09 sub-size specimen standards. The gauge
sections were 32 mm long, 6 mm wide and 5 mm thick. In
order to prevent crushing in the grip sections, the ends of
the specimens were impregnated with Loctite superglue.
All tests were conducted in displacement control at a strain
rate of 103 s1. Displacement was measured using a laser
scanning extensometer with a 1 lm resolution. The inplane Youngs moduli (Ex and Ey) were measured from
the tangent slope of the unloading stressstrain curve
(within the elastic regime). Estimation of the fracture energies (in kilojoules per square metre) involved measuring the

329

area under the loaddisplacement curves and then dividing

by the fracture cross section.
Digital image correlation (DIC) was employed [32,33] to
measure in situ the 2-D surface strain elds (xy and xz
planes) in order to evaluate the in-plane and out-ofplane Poissons ratios. For this purpose, two independent
but synchronized high-resolution (2048  1536 pixels)
PixeLink cameras were used to view the front (xy plane)
and side face (xz plane) of the network samples. Consecutive images were taken at a time interval of 500 ms. Tracking of displacements from these series of images with
sub-pixel resolution was performed using a previously
developed code [34]. To acquire and process the data from
these images, Matlab 7 with Optimization and Image Processing toolboxes was used. A region of 1000 (long)  200
(wide) pixels within the gauge section, with a step size of
20 pixels in each direction, was used for the correlation.
2.3.3. Network cantilever bend testing
The in-plane Youngs moduli of the bre networks were
measured by cantilever bend testing using a laser scanning
extensometer to monitor the beam deection d. This
allowed measurement of deections with a resolution of
5 lm. Beams 150 mm(L)  20 mm(b)  2 mm(h), cut
parallel to the longitudinal and transverse (in-plane) directions, were employed. Load was applied using small preweighed masses in the range 0.040.26 g. The response to
unloading was also measured, to ensure that the beams
were still in the elastic regime. A correction to d was
applied by measuring the apparent thickness of the beams,
to account for errors arising from extraneous beam
twisting.
The deection d was measured at a distance x from the
clamped end, while a load P was applied at a distance L
(from the clamped end). The clamping region was impregnated with Loctite superglue to prevent crushing. The
Youngs moduli were calculated from


P Lx2 x3
E

1
Id 2
6
where I is the second moment of area of the beam section
(=bh3/12).
2.4. Vibration testing
2.4.1. Plate vibrations
The dynamic elastic constants were determined by exciting the low-frequency vibration modes of bre network
plates with freefree boundaries. The vibration modes were
located and visualized by Chladni patterns: the natural frequencies correspond to the eigen-frequencies of the plates.
Using classical thin plate bending theory, as described in
detail elsewhere [35], an inverse calculation was performed
to give a best match of the plates elastic constants to the
pattern of measured natural frequencies. Within thin-plate
theory, the potential energy functional U of a thin, at,
orthotropic plate (i.e. with three mutually perpendicular

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S. Neelakantan et al. / Acta Materialia 66 (2014) 326339

planes of symmetry) of thickness h, lying initially in the xy

plane and vibrating with a middle surface transverse (outof-plane) displacement wx; yeixt is given by
U

Z
h3 a
2 0
 2 2
 2 2 #
Z b "  2 2
@ w
@2w @2 w
@ w
@ w
D1

D
dxdy
2
3
4
@x2
@x2 @y 2
@y 2
@x@y
0

where a and b are the in-plane plate dimensions, x is the

angular frequency, and t is the time. Constants D1 and
D3 are associated with bending of the middle surface in
the xz and yz planes, respectively, D2 with Poissons ratio
coupling between the x and y directions, and D4 with
out-of-plane twisting of the middle surface. The four constants D1D4 are related to the in-plane engineering elastic
constants as follows:
Ex
Ey
; D3
121  mxy myx
121  mxy myx
mxy Ey
myx Ex
D2

61  mxy myx 61  mxy myx

D1

D4 Gxy =3
where Ex, Ey are Youngs moduli in the x and y directions,
respectively, Gxy is the shear modulus in the xy plane, and
mxy and myx are the in-plane Poissons ratios.
In brief, the procedure is to obtain rst estimates of the
constants D1, D3 and D4 from the measured resonant frequencies of three particular vibration modes, together with
knowledge of the plate dimensions and density. Next, the
aspect ratio of the plate is adjusted to make it eectively
square, and the frequencies of two modes termed the O
mode (fo) and X mode (fx) are measured. Their frequency
ratio is particularly sensitive to Poissons ratio, and a chartbased method based on this ratio is used to give an estimate
of D2. Finally, these rst estimates of D1, D2, D3 and D4 can
be improved by an iterative process employing numerical
calculations of plate frequencies based on the RayleighRitz
method. A virtue of this plate-based approach is that additional natural frequencies can be measured to provide a
degree of redundancy. If these additional frequencies are
also well predicted by the numerical calculations, the applicability of thin-plate theory is conrmed, and the user can
have more condence in the results.
The experimental setup used to measure the resonant frequencies involves a loudspeaker driven by a sine-wave generator, mounted beneath a large at surface. The plate

specimen is supported over the loudspeaker on small blocks

of soft polymeric foam. These foam supports are adjusted
during testing to lie precisely on nodal lines (i.e. lines where
the amplitude of vibration is zero) of each tested mode. The
frequency of the sine-wave is carefully tuned until the
desired Chladni pattern is observed, and the corresponding
frequency is then read from a frequency counter. The pattern is visualized by sprinkling powder over the surface of
the plate and observing the powder accumulating along
the nodal lines. Sketches of some of the measured mode
shapes are shown in Tables 6 and 7. Network plates were
cut into square and rectangular shapes for these tests: the
plate dimensions are given in Table 1.
2.4.2. Beam vibrations
A second vibration technique was also used to measure
the exural (in-plane) Youngs modulus of the bre network material. The technique involved excitation of
150 mm(L)  20 mm(b)  2 mm(h) beams by means of a
light external mechanical impulse. The beam was supported at the two nodal points of the rst freefree vibration mode, located 25% of the specimen length from
either end. A microphone, connected to an amplier, was
located directly underneath the sample. Following impulsive excitation of the beam between the nodal points, the
response signal was digitized and converted to the frequency domain using Fast Fourier Transform analysis.
The peaks in the frequency spectrum show the locations
of natural frequencies of the specimen. The natural frequencies for dierent vibration modes, along with the beam
dimensions and density, were used to give an estimate of
the Youngs modulus of the networks in the direction parallel to the length of the beam using the following equation
 4
x2n qA L
E
4
I
an
where q is the density, xn is the frequency of the nth mode
(rad s1), and an is the modal constant, equal to 4.73 and
7.85 for modes 1 and 2, respectively [36].
3. Results
3.1. Network architecture
Table 2 summarizes the network architecture characteristics obtained from X-ray tomography. As expected, the

Table 1
Plate dimensions and densities used for vibration testing (Section 2.4.1).
Fibre volume fraction, f (%)

Plate shape

Length, a (mm)

Breadth, b (mm)

Thickness, h (mm)

Density (kg m3)

10

Square
Rectangular

150.02
175.05

150.02
140.04

2.05
2.05

734.6
703.4

15

Square
Rectangular

150.03
175.07

150.03
140.06

2.03
2.03

1185.5
1163.0

20

Square
Rectangular

150.03
175.09

150.03
140.03

2.01
2.01

1600.2
1620.6

S. Neelakantan et al. / Acta Materialia 66 (2014) 326339

331

Table 2
Architectural characteristics extracted from the volumetric reconstructions of 316L bre networks.
Fibre volume
fraction, f (%)

No. of
bres ()

No. of bre
segments ()

Mean segment
length, L (lm)

Average no. of bonds

per bre ()

Fibre
tortuosity ()

Mean bre inclination

angle, h ()

10
15
20

2853 38
4623 297
6269 131

22,851 62
39,264 2,215
59,943 7

237 2
186 5
153 0

8.97 0.07
9.04 0.36
9.17 0.13

1.51 0.02
1.51 0.01
1.85 0.01

82.88 0.31
81.87 0.21
79.62 0.13

average number of bres and bre segments (sections

between joints) and also the average number of bonds
per bre increase with increasing bre volume fraction.
Conversely, the mean segment length decreases with
increasing bre volume fraction. The bre tortuosity,
which is the ratio between its geodesic length and the
Euclidean distance between its two extremities, is higher
for the 20 vol.% networks. Since the bre length is similar
for all bre volume fractions, it can be postulated that, during processing, bres in the 20 vol.% networks bend more
over each other as the sheets are compressed.
Fibre segment orientation distributions are presented in
the form of histograms of the bre segment inclination
angle h to the through-thickness z direction (Fig. 2a) and
stereographic projections on the xy plane (Fig. 2b and c).
The vertical axis of the histograms is giving
P the probability
of the bre segments P hi N hi =Dhi  ni N hi lying at an
angle hi , where N hi is the number of bre segments falling
into a bin of width of Dhi, centred at hi. As expected, the
probability of having segments inclined at low inclination
angles increases with increasing bre volume fraction, as
bres are more likely to come into contact. Stereographic
projections, using the South Pole as the point of projection,
are illustrated in Fig. 2b and c. In Fig. 2b, owing to the
large number of points, each point on the stereogram represents the in-plane orientation of 10 bre segments. High
orientation angles to the z axis would appear as points clustered near the periphery of the stereograms. It can be seen
that there is a clear bias towards the stereogram periphery
and that the number of points near the centre point of the
stereogram (along the z axis) is increasing with bre volume fraction. Fig. 2c shows the stereographic projections
with density contours, produced using the counting grid
approach. A square grid (41  41 cells) is superimposed
on the plot. The points inside each cell are totalled. The
resultant matrix of concentration values is then contoured.
It can be seen that the bre inclination angles are not uniformly distributed between the quadrants. This eect
appears to become more pronounced in the 20 vol.% networks; the right quadrants appear to contain a higher density of points compared with those on the left.
3.2. Single bre testing
Typical tensile stressstrain curves for as-received and
heat-treated 316L bres are shown in Fig. 3. Table 3 summarizes the properties extracted from the curves. (It is

worth noting that the values are comparable with those

obtained for other variants of stainless steels bres
[11,15,19].) It can be seen that, while both bres exhibit
similar work hardening rates (Fig. 3), the sintering heat
treatment induced a signicant reduction in strength and
ductility (Table 3). Consequently, the nominal work of
fracture Us for a single bre, measured as the area under
the loadstrain curve, was appreciably lower for the heattreated bres than that for the as-received bres. The lower
yield strength values may be attributed at least partly to
grain coarsening, which occurred during the sintering process (Fig. 1a and b). Furthermore, the reduction in strength
and ductility may be attributable to precipitation of intermetallic particles at the austenite grain boundaries. Electrolytic etching (Fig. 1e) reveals the presence of r-phase
islands at the austenite grain boundaries after 6 s of etching. It may be possible to reduce the r-phase embrittlement
by annealing; precipitates can be dissolved on annealing
[28].
3.3. Network in-plane tensile testing
3.3.1. Elastic properties (quasi-static)
The measured in-plane Youngs moduli and the Poissons ratios of the network plates are given in Table 4.
The shear moduli Gxy, deduced from the Youngs modulus
and Poissons ratio, are also tabulated. The table shows
that the in-plane Youngs moduli and the out-of-plane
Poissons ratios increase with bre volume fraction,
whereas in-plane Poissons ratios are independent of bre
density. It can be seen that the 10 and 15 vol.% networks
exhibit very similar moduli values in the longitudinal and
transverse directions, whereas a slight deviation in this is
observed for the 20 vol.% networks. However, in-plane
Poissons ratios mxy and myx are almost equal (in the range
0.260.28), which would be expected if the plates were
transversely isotropic. Some dierences, though, are
observed between the out-of-plane Poissons ratios mxz
and myz for the 10 and 20 vol.% networks.
A further point here, shown in Table 4 and also illustrated in Fig. 4, is that the networks exhibit strong auxetic
behaviour in the out-of-plane direction, i.e. negative Poissons ratios. It should be noted that a transversely isotropic
material has no theoretical limit on the value of a negative
Poissons ratio in the out-of-plane direction, in contrast to
the familiar limit of 1 for an isotropic solid. That limit
arises from the relation between Youngs modulus,

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S. Neelakantan et al. / Acta Materialia 66 (2014) 326339

(a)

(b)

(c)

Fig. 2. Fibre segment orientation distributions for the three 316L networks showing (a) the probability distributions of the bre inclination angle h to the z
(through-thickness) direction. Also shown are stereographic projections on the xy plane (b) with points representing the in-plane bre orientations and (c)
density contours.

Poissons ratio and shear modulus, but for a transversely

isotropic material these are independent elastic constants
[37].
Evidently, auxeticity rises with bre density. Similar levels of auxeticity and dependence on bre density have been
theoretically predicted [25] and experimentally measured
[14] for bre networks consisting of ner bres. Since the
bres themselves are not auxetic, the origin of this behaviour is attributed to the processing of these sheets. In cellular solids, it is well established that a non-convex (reentrant) cell shape gives a negative Poissons ratio [38],
and that very high negative values can arise in some geometric congurations. Although bre networks do not
exhibit a cell structure as such, bre kinking is intro-

duced during processing, as layers of randomly laid (loose)

bre felts are compressed to plates with dierent bre volume fractions and subsequently sintered. It is worth noting
that, while the bre tortuosity levels are higher for the
20 vol.% networks, the 10 and 15 vol.% networks exhibit
very similar values (Table 2). It is also of note that the bre
segment lengths (inter-joint distances) are decreasing with
increasing bre volume fraction, whereas the number of
bonds per bre is increasing. DIC images captured in situ
(not shown) suggest that, even at very low strains, weak
inter-bre bonding results in longitudinal cracking/splitting. This is not surprising, as the width of the solid-state
sintered necks can be quite small relative to the bre diameter. Bending of the bre bundle splits, resulting in outward

S. Neelakantan et al. / Acta Materialia 66 (2014) 326339

Fig. 3. Typical tensile stressstrain curves for as-received and heat-treated

316L bres.

Table 3
Tensile properties of as-received and heat-treated single bres, as
measured by single bre testing.
Condition

r0.2%
Yield
strength
(MPa)

Ultimate
tensile
strength
(MPa)

Strain to
failure
(%)

Fracture
energy
(J m1)

As-received
Heat-treated

465 16
252 11

877 11
564 17

30.0 1
14.7 1

0.282 0.015
0.081 0.008

bulging in the through-thickness direction. This can be seen

in the post-fracture images shown in Fig. 5. It can be seen
that the cracks form a tortuous path as they pass through
bundles of bres. Of course, these post-fracture images do
not relate directly to linear-elastic behaviour and Poissons
ratio, but nevertheless the conspicuous cross-direction
expansion is indicative that the bre topology tends to produce strong dilation in all regimes of deformation in
response to uniaxial loading.
3.3.2. Deformation and fracture
Typical loaddisplacement curves obtained from inplane tensile testing of 316L networks with dierent bre
volume fractions are presented in Fig. 6. A similar defor-

333

Fig. 4. Experimental data from in-plane (longitudinal) tensile testing of

316L bre networks with dierent porosities, plotted in the form of
through-thickness expansion as a function of extension in the longitudinal
direction.

mation response was observed in the in-plane directions

for all three networks. All curves show an approximately
linear response followed by a relatively short region of
plastic ow and strain hardening up to a peak load. Thereafter, accumulation of damage at the bres and joints eventually initiates rupture, which is the source of the fall in
load that precedes nal failure. The plastic ow and strain
hardening region is relatively short for low-bre volume
fractions compared with high-bre volume fractions. The
displacement to failure remains approximately the same,
irrespective of bre volume fraction. Average fracture
energy values in the longitudinal and transverse directions
were approximately the same as shown in Table 4. Estimation of the fracture energy in units of kilojoules per square
metre involves obtaining the area under the loaddisplacement curves and then dividing by the fracture cross section.
As illustrated in Fig. 5, fracture is taking place in a tortuous path. A very rough estimate of the fracture area was
obtained by considering the initial gauge length and thickness to nd the diagonal length (equivalent to the hypotenuse of the right angle triangle). Multiplying this length by
the initial gauge width of the samples provided an estimate

Table 4
Elastic constants and fracture energies for 316L bre networks, as measured by in-plane tensile testing.
Elastic constants

Fibre volume fraction, f (%)

10

15

20

Ex (GPa)
Ey (GPa)
mxy ()
myx ()
Gxy (GPa)
mxz ()
myz ()

1.17 0.32
1.13 0.06
0.27 0.01
0.27 0.01
0.46
5.30 0.83
4.45 0.85

2.19 0.11
2.28 0.59
0.28 0.03
0.26 0.02
0.86
7.37 0.32
7.54 0.48

2.51 0.06
3.10 0.86
0.27 0.01
0.26 0.03
0.99
10.67 0.29
11.27 0.66

Fracture energy (kJ m2)

Longitudinal
Transverse

4.27 0.22
3.42 0.67

7.71 0.66
7.24 0.46

11.41 0.94
10.92 1.32

334

S. Neelakantan et al. / Acta Materialia 66 (2014) 326339

Fig. 5. (a) Optical micrographs and (b) DIC images showing side views of 316L bre networks after in-plane tensile testing.



2f sin /
p
Gfr
Ufz
3 3a2

Fig. 6. Typical tensile loaddisplacement curves for 316L bre networks,

of dierent bre volume fractions, measured along the longitudinal (x)
and transverse (y) directions.

of the fracture area. Acknowledging that some gross simplications are being incorporated here, the estimated fracture area was approximately ve times larger than the
cross-sectional area (based on nominal dimensions). Fracture energy values were found to increase with bre volume
fraction in an approximately linear fashion, which is in
agreement with a previously developed analytical model
[16].
The aforementioned model [16] predicts the fracture
energy Gfr for this type of brous material, based on the
work of fracture of a single bre, assuming that all bres
fracture. This model leads to

where a is the side length of the bre hexagonal cross section, z is the deformation zone and / is the in-plane bre
inclination angle to the x axis (Fig. 7). The fraction in
brackets represents the number of bres per unit sectional
area.
From Eq. (5), it can be seen that, by raising the fracture
energy of the bre and controlling the deformation zone
length, this process can absorb large quantities of energy.
In deriving this equation, it is assumed that all bre segments lie at the same in-plane inclination angle /. However, in reality, the in-plane orientation distribution of
the bre segments is more complex than this. To approximate this, an orientation probability distribution P(/) for
a range of / values between 0 and p/2 was introduced in
Eq. (5).
R p=2
2fU f z 0 sin /P /d/
p
Gfr
6
3 3a2
P(/) can be represented using histograms of the type
shown in Fig. 2a, derived using X-ray tomography, with
each measured in-plane angle allocated to a size bin. Discretization of P(/) allows a probability P(/i) to be assigned
to all bres allocated to a bin size of D/i, so Eq. (5) can be
rewritten as
Pn
2fU f z i sin /i P /i D/i
p
Gfr
7
3 3a2
where P(/i) is given by
P /i

Fig. 7. Schematic representation of the geometry used for prediction of

the fracture energy of the bre networks.

N/
1
 Pn i
D/i
i N /i

N hi is the number of bres inclined at an angle /i (i.e. within a bin size of D/i, centred at /i).
A plot of the predicted fracture energies of the networks
against bre volume fraction is shown in Fig. 8. Also
shown are the experimentally estimated values of Gfr in
the longitudinal direction (Table 4). The experimental values are in good agreement with predictions if the deformation zones are taken to have lengths of 80, 110 and 130 lm
for 10, 15 and 20 vol.% networks, respectively. These values are of the same order as the network bre segment

S. Neelakantan et al. / Acta Materialia 66 (2014) 326339

335

Table 5
In-plane elastic moduli for 316L networks, as measured by cantilever bend
testing.
Fibre volume fraction, f (%)

10
15
20

In-plane elastic moduli (GPa)

Ex

Ey

1.10 0.12
1.69 0.03
2.50 0.17

1.09 0.08
1.78 0.02
2.82 0.02

of the same volume fraction. Closed-cell foams are often

very poor, particularly under tensile loading, partly
because of the presence of embrittling constituents in the
cell walls [39,40].
Fig. 8. Predicted dependence of the network fracture energy on the bre
volume fraction. Also shown are the experimental data for bre networks
with dierent bre volume fractions.

lengths, as determined by X-ray tomography (Table 2).

Evidently, the size of the deformation zone is increasing
with increasing bre density.
From images such as those shown in Fig. 9, it can be
seen that failure occurs by failure at the sintered necks followed by plastic deformation of individual bres as they
align along the loading direction. Grain rotations
become very obvious in a bamboo structure of this type,
provided that very large plastic strains have been induced.
In principle, plastic deformation and rupture of the bres
has the potential for greater energy absorption than fracture of joints. There is considerable scope to maximize this
contribution by tailoring the bre microstructure (for
instance by annealing: see Section 3.2) to obtain the desired
combination of strength and toughness.
It is worth noting that, provided both bres and joints
are relatively strong and tough, metallic bre networks
can exhibit good mechanical properties under tensile loading compared with open- or even closed-cell metallic foams

3.4. Network cantilever bend testing

The in-plane Youngs moduli obtained from cantilever
bend testing are listed in Table 5 for dierent bre volume
fractions. Increasing moduli values were observed with
increasing bre volume fraction, similar to in-plane tensile
testing. In addition, similar to in-plane tensile testing, cantilever bending yields dissimilar in-plane moduli values for
the 20 vol.% networks (Table 5).
3.5. Network vibration testing
3.5.1. Plate vibrations
As described in Section 2.4.1, the resonant frequencies
of the rst three mode shapes, shown in Table 6, were initially measured. These frequencies led to rst estimates of
D1, D3 and D4. To estimate D2, the square plate (with
adjusted aspect ratio) was used to observe the O (ring)
and X vibration mode frequencies (mode nos. 2 and 3
in Table 7). The accuracy of these rst estimates of D1,
D2, D3 and D4, was improved using an iterative method,
as described in Section 2.4.1. Since there should be no

Fig. 9. SEM micrographs showing: (a) bre alignment along the loading direction; (b) necking of individual bres prior to fracture; (c) a fractured bre
exhibiting necking; (d) fracture at a sintered brebre joint; and (e) grain rotations at large plastic strains.

336

S. Neelakantan et al. / Acta Materialia 66 (2014) 326339

Table 6
Measured and predicted mode frequencies (in Hz) for rectangular plates made of 316L networks with dierent bre volume fractions.
Mode no.

Mode shapes

Fibre volume fraction, f (%)

Frequency (Hz)
Measured

Predicted

10
15
20

72
70
70

72
70
70

10
15
20

94
88
96

93
88
96

10
15
20

158
146
139

151
146
139

10
15
20

172
157
162

173
168
172

10
15
20

204
185
185

205
198
193

10
15
20

267
241
246

266
254
278

10
15
20

310
288

338
326

10
15
20

319
286
290

344
333
333

preferred direction in any of the bre networks, this iterative process was carried out using an assumption of transverse isotropy. The rst estimates of elastic constants were
consistent with this idea: the empirical values for D1 and D3
were very similar for each network material.
Tables 6 and 7 show the measured natural frequencies
for rectangular and square plates, with dierent bre volume fractions, compared with the predictions using the
nal iterated values of the four elastic constants. Identical
values of the material properties were used for the two
shapes of plate with each tested bre volume fraction: only

the dimensions were changed. This results in considerable

redundancy in the comparison: many more modes are
examined than would be needed simply to t the four values. Irrespective of bre volume fraction, it can be seen
that, for the rst ve or six modes of each plate, there is
good agreement between measured and predicted frequencies. The disparity between measured and predicted frequencies increases as frequencies go up, with predicted
frequencies being systematically higher than measured
ones. This eect seems to be more pronounced for the
20 vol.% networks. This pattern of deviation is exactly

S. Neelakantan et al. / Acta Materialia 66 (2014) 326339

337

Table 7
Measured and predicted mode frequencies (in Hz) for square plates made of 316L networks with dierent bre volume fractions.
Mode no.

Mode shapes

Fibre volume fraction, f (%)

Frequency (Hz)
Measured

Predicted

10
15
20

77
74
73

78
76
76

10
15
20

116
112
112

117
112
112

10
15
20

139
136
135

141
136
142

10
15
20

200
192
183

204
197
193

10
15
20

199
187
182

204
197
204

10
15
20

331
314
304

359
348
328

10
15
20

331
314
302

359
344
378

10
15
20

338
308
300

370
359
361

10
15
20

361
336

409
394

what one would expect from the inuence of throughthickness shear eects, as the theory used for the predictions ignores such shear deformation.
Table 7 also shows that all vibration modes that do not
show symmetry in the diagonal line of the square plate
(modes 4, 5 and 6, 7) occur in pairs with approximately

the same resonant frequencies. The agreement is close for

the 10 and 15 vol.% networks, but less close for the
20 vol.% network. This supports the assumption that the
plates exhibit transverse isotropy. At low-bre volume
fractions, there are no signicant deviations from the theoretical predictions, while at high-bre volume fractions,

338

S. Neelakantan et al. / Acta Materialia 66 (2014) 326339

Table 8
In-plane elastic constants for 316L bre networks, as measured by plate vibrations.
Fibre volume fraction, f (%)

In-plane elastic moduli (GPa)

Poissons ratios ()

Shear modulus (GPa)

Ex

Ey

mxy

myx

Gxy

10
15
20

1.29
1.98
2.55

1.29
2.02
3.40

0.26
0.27
0.24

0.26
0.28
0.32

0.47
0.76
1.07

Table 9
In-plane Youngs moduli for 316L networks, as measured by beam vibrations.
Fibre volume fraction, f (%)

Specimen orientation

Beam density (kg m3)

Mode frequencies (Hz)

Mode 1

Mode 2

10

Longitudinal
Transverse
Longitudinal
Transverse
Longitudinal
Transverse

701.55
746.02
1114.11
1193.32
1569.43
1558.11

117.19 0.00
109.86 4.88
104.17 11.28
100.91 5.04
100.91 5.04
117.19 0.00

332.03 23.28
330.40 32.51
292.97 0.00
277.62 5.22
287.39 13.64
312.50 0.00

15
20

there are some eects of material inhomogeneity, presumably attributable to the manufacturing process. This conclusion is in general agreement with the quasi-static
tensile and bend test results. Even with these eects of inhomogeneity, the general pattern of frequencies ts the predictions well enough that one can have some condence
in the tted elastic constants, interpreted in an averaged
sense over the areas of both plates and over all directions
of wave propagation. The iterated and adjusted D1D4 values are related to the in-plane engineering elastic constants
(Ex, Ey, mxy, myx and Gxy) via Eqs. (3). The values are summarized in Table 8.
3.5.2. Beam vibrations
The beams used for vibration testing gave most accurate
results for the lower modes of vibration (modes 1 and 2).
The corresponding measured frequencies, which are an
average of at least three measurements, and the beam density values are given in Table 9. The obtained in-plane
Youngs moduli of the networks are also listed in Table 9.
Similar to other testing methods, the in-plane moduli values increased with bre volume fraction, and deviations
due to inhomogeneity are also observed for the 20 vol.%
networks. As with the plate vibration test, when higher
modes of the beam samples were examined, eects due to
through-thickness shear were observed.
4. Discussion and conclusions
An experimental investigation was carried out into the
deformation response of bre networks, made by solidstate sintering of 316L austenitic stainless steel bres. Networks with 10, 15 and 20 vol.% bre volume fractions have
been characterized in terms of network architecture and
their response to quasi-static mechanical and dynamic testing. The following conclusions can be drawn from this
work.

In-plane elastic moduli (GPa)

1.08 0.07
1.11 0.10
1.49 0.13
1.39 0.06
1.94 0.18
2.39 0.00

1. Fibre segment lengths were found to decrease with

increasing bre volume fraction. The highest bre tortuosity levels were observed in the 20 vol.% networks,
which may be associated with the way in which the
sheets have been processed; an external pressure is
applied to randomly laid bre felts in order to produce
sheets of specic porosity. As expected, the majority of
the bre segments lie at inclination angles (to the vertical) >75. However, the probability of having bre segments inclined at such inclination angles increases as
bre density falls. Stereographic projections on the xy
plane (in-plane directions) suggest that the 10 and
15 vol.% networks are transversely isotropic, whereas
there is some indication that the 20 vol.% networks are
inhomogeneous in terms of the spatial arrangement of
the bres.
2. A range of quasi-static and dynamic techniques were
employed to determine the elastic constants of the network sheets. The main corollary, in agreement with
the tomography results, is that the 20 vol.% sheets show
signs of material inhomogeneity. This eect is made
most evident in the plate vibration results (Tables 6
and 7). When comparing the in-plane stiness values
obtained from in-plane tension with those measured
by cantilever bending, and plate and beam vibrations,
it can be seen that all techniques yield very similar stiness values for the 10 vol.% networks, but dierences
arise among the dierent methods with increasing bre
density. This may be attributed to the fact that, as the
bre volume fraction increases, there is progressive evidence of shear eects in the cantilever and vibration testing. This could be attributed to the fact that the bre
segment length decreases (Table 2), causing the shear
component arising from the individual struts to have a
more dominant eect on the network deformation,
resulting in lower stiness values. It should also be noted
that bend tests, whether static or dynamic, are inu-

S. Neelakantan et al. / Acta Materialia 66 (2014) 326339

enced mainly by the material in the outer layers of the

network sheet, whereas tensile testing gives equal weight
to the material throughout the thickness.
3. The networks were found to expand in the throughthickness direction when stretched in-plane, resulting
in Poissons ratios lying between 5 and 11. While
the deformation mechanisms that give rise to such
strong auxetic behaviour cannot be easily identied with
this type of testing, this behaviour was attributed to outward bending of kinked bres (kinking was induced during processing, owing to the applied pressure), as the
networks are stretched in-plane. Such a mechanism
would be similar to that studied in detail for 2-D honeycomb structures by Gibson and Ashby [41]. Synchrotron
X-ray tomography experiments are currently being
planned to validate the above observations.
4. Fracture energies of the order of several kilojoules per
square metre were obtained experimentally. These values are consistent with predictions based on the assumption that this energy is primarily associated with plastic
deformation of individual bres within a process zone of
the order of inter-joint spacing. It is worth noting that,
by raising the fracture energy of the bre (e.g. by annealing), this process can make a signicant contribution to
the fracture energy of the networks.

Acknowledgements
This research was supported by the European Research
Council (Grant No. 240446). The authors wish to thank
Miss Erika Oberg, of the Materials Science Department
at Cambridge University, for help with cantilever testing.
Acknowledgement is also due to Mr. Karthikeyan Kandan, of the Engineering Department at Cambridge University, for his help with DIC measurements.
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