Original Article

Journal of Reinforced Plastics

and Composites

Impregnated fibre bundle test for natural 0(0) 1–16

! The Author(s) 2017
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DOI: 10.1177/0731684417695461
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F Bensadoun1, I Verpoest1, J Baets1, J Müssig2, N Graupner2,

P Davies3, M Gomina4, A Kervoelen5 and C Baley5

Abstract
In this study, the impregnated fibre bundle test, a common method used by carbon and glass fibre manufacturers to
determine the properties of fibres used in composites, was adapted for natural fibres and validated by a round robin test
on one type of natural fibres, namely flax fibres. Five European laboratories have carried out in parallel the impregnated
fibre bundle test, on the same batch of hackled flax (long fibres), to check the applicability and reliability of this modified
method on natural fibres. The results were compared to the more traditional single fibre test on elementary fibres.
The back-calculated fibre stiffness shows a very low scatter between the five laboratories of less than 5%
(59.8  2.4 GPa, as measured between 0 and 0.1% strain). The fibre ultimate tensile strength of 527  138 MPa has a
higher scatter, compared to stiffness values, as this property is highly sensitive to imperfections and flaws.

Keywords
IFBT, flax fibre, hemp fibre, mechanical properties, single fibre test

Introduction data sheets to report the fibre properties.4 There are

Natural fibres play an increasing role as reinforcement
in polymer composites not only because they are
‘natural’ but also because they have interesting proper-
ties, which makes them competitive with or complemen-
tary to glass and carbon fibres. When designers have to
decide which reinforcement to use in their composite
products, they first look at the mechanical performance
of the fibre-reinforced composite. Basic mechanical
properties, like strength and stiffness, are dominated by
the fibre properties; hence, it is important to characterize
the fibre properties and measure them in a reliable way.
As of today, there are three distinct ways to characterize
the fibre properties. Either, the fibres are tested as such,
using single fibre tensile tests (SFT)1 or dry fibre bundle
tests.2 Alternatively, the fibre properties are back-calcu-
lated from the results of the impregnated fibre bundle
test (IFBT).3 In this last method, a unidirectional com-
posite is loaded in the fibre direction, and the fibre stiff-
ness and strength are back-calculated from the measured
composite properties, using straightforward microme-
chanical equations such as the rule of mixture.
The IFBT is well established for carbon and glass
fibres and many companies refer to it in their technical
two intrinsic advantages of this method. The first is
that a large number of fibres is tested simultaneously,
resulting in a rather direct measurement of the average
‘‘effective’’ back-calculated fibre stiffness and strength.
Second, the test is less complicated than a single fibre
test (SFT), where a delicate preparation of the fibres is
required. Moreover, a very large number of individual
fibres have to be tested to provide statistically reliable
results.1,5
1
Department of Materials Engineering, KU Leuven, Leuven, Belgium
2
HSB – University of Applied Sciences Bremen, Faculty 5 – Biomimetics/
Biological Materials, Bremen, Germany
3
Centre de Bretagne, Marine Structures Group, IFREMER, Plouzané,
France
4
Laboratoire CRISMAT, UMR 6508 CNRS/ENSICAEN, Université de
Caen Basse-Normandie, Caen Cedex, France
5
Université de Bretagne Sud, Lorient, France
Corresponding author:
I Verpoest, Department of Materials Engineering, KU Leuven,
Kasteelpark, Arenberg 44, 3001 Leuven, Belgium.
Email: ignaas.verpoest@kuleuven.be
2 Journal of Reinforced Plastics and Composites 0(0)
A possible drawback of the IFBT is that the back-
calculated properties depend on the validity of the
micromechanical equations used. This is not a problem
for the stiffness where the influence of matrix and inter-
face is negligible, at least when continuous fibres, or dis-
continuous fibres with a very high aspect ratio, are used.
However, for strength, the influence of the matrix,
the possible (local) fibre misorientations, the fibre
volume fraction and the fibre-matrix adhesion have to
be considered. The matrix and interface properties and
fibre volume fraction will influence the mutual inter-
action of fibre failures; hence, in order to provide
detailed stochastic information on the fibre strength,
more elaborate data reduction schemes should be
used.6,7 In this paper, however, the simple ‘rule of mix-
ture’ will be used; it can be argued that the fibre
strength values, back-calculated from the IFBT, can
be considered as reliable values, when the fibre strength
data are used for predicting the properties of composite
where matrices with similar properties and similar
interface strengths are used. Extrapolations to com-
pletely different matrix materials have to be handled
with care. For instance, if the matrix would have a
very low yield stress or interfacial strength, then the
rule of mixture would not apply directly and another
micromechanics calculation method (certainly for the
strength) needs to be used.
The particularities of natural fibres and their
potential effects on the IFBT results
Natural fibres, because of their complex morphology
and microstructure, distinguish themselves from glass
and carbon fibres which have continuous filaments with
a constant cross-section. The heterogeneity of the glass
and carbon fibre microstructure happens at the nano-
scale (for instance, orientation of graphitic layers in
carbon fibres), and hence the mechanical properties
can be considered as homogeneous on the micro or
fibre scale. Various types of defects will, however,
create a scatter in the strength values, leading to the
well-known stochastic nature of the strength of
carbon and glass fibres. On the other hand, natural
fibres are not homogeneous as they have a complex,
multiscale morphology as seen in Figure 1.8,9
In composite applications, the technical plant fibres
are mostly used to create continuous preforms. These
technical fibres are composed of several elementary
fibres bonded together by a middle lamella mainly com-
posed of pectin.10,11 These elementary fibres have an
average length of 25–30 mm and an average diameter
of 19 mm.12 Furthermore, they are composed of differ-
ent layers made of crystalline cellulose microfibrils with
different orientations and embedded in an amorphous
matrix. The technical fibres consist of 10 to 40
elementary fibres. As the number of elementary fibres
varies over the length of a technical fibre, the diameter
of a technical fibre will also vary over its length.13 This
cross-section variation renders the determination
of stresses, strength, and Young’s modulus problematic
when one technical fibre is tested in an SFT.14 Different
methods have been proposed to measure the cross-
section variation, but the procedure is tedious and the
variation has a bigger effect on strength (sensitive to
the weakest cross-section) than on modulus (a property
averaged over the tested fibre length) of technical fibres.
On the contrary, elementary fibres can be tested indi-
vidually and have the advantage of a limited diameter
variation over their length.
The main difference between glass and carbon fibres
on one hand and flax fibres on the other hand is the fact
that the latter are not continuous. Whereas an elemen-
tary flax fibre can be considered as a continuous
filament with limited length, the technical flax fibres
are composed of several elementary fibres assembled
together to create a discontinuous long fibre. When
these technical fibres are subjected to tensile testing, it
has been found that they have a lower ‘apparent’ stiff-
ness than elementary fibres.15 This is caused by the
elementary fibres sliding over each other because of
the weak shear resistance of the pectin-rich layer
(‘middle lamella’, see Figure 1).14 These shear stresses
are highest at the elementary fibre ends, which will
be present if the technical fibre length tested is longer
than the maximum elementary fibre length, which is
normally the case. This adds an amount of strain to
the intrinsic strain in the elementary fibres, which will
be dependent on the rigidity of the pectin-rich layer and
on the number of elementary fibres in the technical
fibre. This sliding effect can be minimised by embedding
the technical fibres into a resin, like in the IFBT.
The outer elementary fibres will be adhered to the
matrix,9,16,17 and hence their sliding relative to the
other (outer and inner) elementary fibres will be limited.
In this way, this in situ behaviour of the technical fibre
is much more realistic and relevant for composite appli-
cations than its behaviour when tested as an individual
technical fibre (without resin impregnation), as
described above.
As another alternative to the SFT, sometimes the
‘‘dry fibre bundle test’’ or ‘‘unimpregnated’’ fibre
bundle test is proposed. The pertinence of using IFBT
testing instead of ‘‘dry fibre bundle test’’ for natural
fibre arises considering the facts that:
. It is practically impossible to carry out a ‘dry fibre
bundle test’ on elementary fibres, as they have dif-
ferent lengths (<3 cm) and diameters. Moreover,
they are difficult to extract and to bring together
into a bundle.
Bensadoun et al.
Figure 1. The multi-scale structure of the flax fibre: (a) cross-section of the stem of a flax plant and of the position of the bundles of
elementary fibres, forming the technical fibres after extraction8 and (b) ESEM Image of a ‘‘technical fibre’’ and its constituting
elementary fibres.9
. Technical fibres are discontinuous, and as such, test-
ing a bundle of dry fibres would inevitably mean that
some fibres (an unknown number) are not loaded,
because they have their fibre end somewhere within
the tested bundle length.
Hence, the use of the impregnated fibre bundle
method on technical fibres becomes more interesting as
all the fibre ends inside the bundle length will be loaded
thanks to the interfacial shear stresses with the matrix.
The IFBT method for natural fibres
The aim of this paper is to show that there are many
advantages in using the IFBT, from which the fibre stiff-
ness and strength are back-calculated. It should represent
correctly the behaviour of flax fibres and, by extension, of
other natural fibres in a composite (because they are also
3
discontinuous fibres with a multi-scale microstructure, as
described above). It generates effective and average prop-
erties, as in each sample hundreds to thousands of rein-
forcing fibres are tested. Furthermore, the manufacturing
of the specimens and the tensile testing are common prac-
tice in composite labs.
A well-established standard is followed, enhancing
in this way the confidence the composites industry has
in the reliability of technical data provided by the flax
fibre producers. Finally, the IFBT can also be used to
assess flax fibres at different stages of the refinement
process (scutching, hackling, carding, combing, etc.)
for long fibres as well as tows and yarns.
Motivation of the study
In 2013, the European Scientific Committee of the
Technical Section of the European Confederation on
4 Journal of Reinforced Plastics and Composites 0(0)
Linen and Hemp (CELC)18 started the elaboration of
technical data sheet templates for flax and hemp fibre
preforms (weaves, non-crimp fabrics, random mats,
yarn/roving, etc.).19 These technical data sheets follow
a similar structure as the well-established ones for glass
and carbon fibre preforms. When coming to fibre prop-
erties, or to properties of unidirectional tapes or rov-
ings, the question arose which standardized method
could be used, either the SFT (on elementary fibres) or
the IFBT (on technical fibres). For the scientific reasons
presented above, it was decided to investigate the possi-
bility of adapting the IFBT methodology standardized
for continuous carbon filaments (ISO 10618:2004) to the
specificities of natural fibres, and in this particular case
to flax fibres.3,20
A working group of five European laboratories sup-
ported by CELC’s European Scientific Committee
studied the existing ISO standard3 and proposed some
modifications to the specimen-manufacturing proced-
ures, whereas the testing and data reduction were left
unchanged. Then, a limited round-robin experiment
was set up, in which five European laboratories parti-
cipated. One batch of hackled long fibres type Aramis
was chosen. This is a recent variety of spring flax, which
was sowed for the first time in 2011 and has a good
fibre yield and good disease resistance.21,22 In 2013, the
Aramis variety represented 4.9% of the cultivated area
of 58.500 hectares of flax in France.22 The choice of
only one batch of fibres is justified, because the aim
of this round-robin experiment was to verify that
the method works independently of the operator.
Such comparison cannot be made if different varieties
are used.
Five laboratories manufactured the specimens and
performed the tests and data reduction following as
much as possible the ISO-standard with its proposed
modifications. The results of these tests are presented in
this paper and critically assessed taking into account
the differences in matrix resins and testing parameters.
Finally, they are compared to tensile tests on elemen-
tary fibres, carried out on the same batch of hackled
long fibres.
Experimental
The flax fibres
In this study, hackled flax fibres type Aramis from the
Terre de Lin company (France) were used. The flax
plants were harvested mature in 2013 in Normandy
and then field retted (dew-retting). The dew-retted
flax was selected by the producer for its good quality,
i.e. optimal retting, as it is known that the retting influ-
ences the mechanical properties of the fibres.23 The
retted flax subsequently underwent scutching, which
separates the bast fibres from the shives, and hackling.
After these two steps, hackled tapes of long flax fibres
and tows were obtained; all fibres are parallel to each
other, and no twist is induced (as would be the case
during spinning flax yarns used for weaving). It has
to be noted that the sampling area of fibres in the
plant height is a parameter that influences their mech-
anical properties and that, if the fibres from only one
area are tested, a reduction in the variability of strength
and stiffness has been observed.24,25 In this research,
however, the hackled tape contains fibres from all pos-
itions along the plant height, and hence homogenised
or averaged properties with somewhat higher scatter
can be expected. A batch of 20 kg of tapes of hackled
fibres was randomly split up into tapes of 10 meters.
These hackled flax tapes were sent to each of the five
research institutes.
The matrices
The IFBT was performed by several research institutes,
thus, several polymer matrix resins were used. Their
compositions, curing cycles and mechanical properties
are shown in Table 1. All resins have been chosen
according to a number of criteria: a low viscosity to
allow a good impregnation of the fibres and a good
fibre/matrix adhesion, which is an important parameter
to obtain a good fibre-matrix stress transfer in the
composite.26–28
To stay close to the fibre performance in ‘‘real’’ com-
posites, where the matrix and interface are optimised
towards optimum composite performance, the ISO
standard advises to use a matrix (preferably epoxy)
with a good adhesion to the fibre, and with a sufficiently
high failure strain.3 This means that the strain to failure
of the polymer matrix should be at least twice that of
the fibre, preferably three times. All resins chosen had
Young’s moduli between 2.5-3.5 GPa with a failure
strain of at least 4% (beside HSB) and a low curing
temperature (<150 C) to avoid degradation of the
fibres. In the Ensicaen laboratory, a vinyl ester was
used. Including another type of resin, but still fulfilling
the requirements on stiffness and failure strain as stipu-
lated in the ISO-standard, allowed the influence of the
matrix type on the back-calculated fibre properties to
be assessed.
Manufacturing of the IFBT samples
The IFBT on technical flax fibres has been performed
based on the ISO 10618:2004 standard for carbon
fibres. In this research, bundles of unidirectional,
hackled fibres are used instead of rovings (untwisted
yarns) and the manufacturing method has been slightly
modified following the parameters below.
Bensadoun et al. 5

Table 1. Thermoset matrix characteristics.

Tensile Tensile Hardener
Matrix Commercial modulus strength Strain at Density Hardener ratio in
Institute type name (GPa) (MPa) failure (%) (g/cm3) type resin (phr) Cure cycle Supplier


KU LEUVEN Epoxy Epikote 828 LVEL 2.7 70 4 1.16 Dytek DCH-99 15.2 2 h at 150 C Resolution
(amine) performance
products
UBS Epolam 2020 3 69 4.2 1.17 Epolam 2020 34 24 h at room Axson
hardener temperature +
3 h at 40 C + 2 h
at 60 C + 2 h at
80 C + 5 h at 100 C
IFREMER SR 1500/2505 3.1 71 5.4 1.13 SD2505 (amine) 33 4 h at 50 C Sicomin
HSB RIM 135 3 53 1.8 1.15 RIMH 137i 30 48 h at room Lange+Ritter
temperature GmbH
ENSICAEN Vinyester Atlac 580 3.5 83 4.2 1.11 MEKP Butanox 2 10 h at 40 C DSM
Urethane M50

First, the fibres were pre-dried for 24 h at 60 C, cut
into a length of 25 cm and weighed in order to calculate
the fibre volume fraction. In method I, the fibres are
placed in the mould cavity where a vacuum film was
previously laid (see Figure 2(a) to (c)) to create a uni-
directional composite. The resin is then degassed and
poured on top of the fibres. The vacuum film is then
folded and the counter-mould is placed on top. The
whole set-up is then positioned inside a heated press
for consolidation. Once the curing is completed, the
samples are demoulded and conditioned for testing at
21 C  2 C and 50  2% relative humidity. The set-up
in Figure 2 is a modified version of the one studied by
Coroller et al. and Trujillo et al.26,29 and the samples
are comparable in geometry.
Because the mass of the fibres placed in the mould
is precisely controlled, the fibre volume fraction can be
controlled by imposing a precise specimen thickness,
using spacers as displayed in Figure 2(c). The speci-
men width is determined by the mould width. In this
way unidirectional composite samples with small cross
sections have been manufactured, which normally
leads to a limited number of defects and a good con-
trol of the orientation of the fibres. They are moreover
distributed evenly throughout the composite, as shown
in the cross-sections (Figure 3) obtained by scanning
electron microscopy (SEM) and micro-tomography.
All manufacturing parameters such as curing
conditions and resin/hardener ratio are described
in Table 1.
A second method, manual ‘‘pultrusion’’ was used
by HSB to manufacture the samples (see Figure 2(d)).
In this method, the long flax fibres, assembled together
at one end by a nylon cord, were impregnated by
immersion in a bath, containing the epoxy resin, for
at least 10 minutes. The impregnated bundle was then
drawn through a pultrusion die with a dog-bone shape
using the nylon cord. The pultrusion die was then
closed on one side and was mounted vertically.
Within 10 minutes, additional epoxy matrix was
filled into the mould using a syringe. After 10 minutes,
the mould was fully closed, inverted and re-opened on
the other side. More resin was injected for the next 10
minutes. Thereafter, the mould was closed and laid
horizontally. The fibre volume fraction of the sample
was set to 31.4%. The fibres have a nearly unidirec-
tional orientation in the parallel section of the pul-
truded test specimens. No further compression
consolidation was applied using this technique. After
48 hours at room temperature, the sample was cured
and demoulded.
It has to be noted that all samples should have a
resin volume content of at least 35%,3 a good orienta-
tion of the fibres in the unidirectional direction (0 ) and
a limited porosity.
This was indeed realised by the first method, where
a wet impregnation was followed by compression to
consolidate the composite resulting in the required
volume fraction, a good fibre orientation and an
acceptable porosity (&1.7% for UBS and <1% for
KU Leuven (KUL – University of Leuven)). The
void content in the IFREMER samples was limited
to values below 0.1%. The void content of the
Ensicaen samples was not measured, but because
they used a processing method and a resin which
were very similar to the one used by KUL and
UBS, it is believed that their porosity level will be
similar as well. In the second, pultrusion-like method
however, the lack of consolidation pressure could have
caused a misorientation of the fibres (due to the dog-
bone shape obtained through pultrusion) and led to a
slightly higher porosity content (2.9%). It has to be
noted that the porosity levels were calculated by either
SEM, Micro-CT or density measurements.
6 Journal of Reinforced Plastics and Composites 0(0)

Figure 2. Impregnated fibre bundle test method I, (a) top view of six mould cavities and (b) Front view of one cavity of the mould
(spacer not included, the vacuum film surrounds all the flax fibre bundle), (c) longitudinal cross section view of the counter-mould with
the spacers and (d) side and top view of the pultrusion mould.
Bensadoun et al.
Figure 3. UD/epoxy IFBT sample cross-section (a) SEM cross-section from UBS and (b) micro-CT image of the KU Leuven
specimen.
Single fibre testing – Elementary fibres
Single fibre tensile (SFT) tests on elementary fibres
were carried out and the results will be compared to
the back-calculated properties obtained through the
IFBT test. The elementary fibres were manually
selected and the testing was done according to the
AFNOR NF T 25-501-1,30 AFNOR NF T 25-501-
231 and AFNOR NF T 25-501-332 standards. They
were adhesively bonded onto a paper frame with a
gauge length of 10 mm. The average apparent diam-
eter was determined under a microscope from 6 meas-
urements. The frame, as described in Trujillo De Los
Rı́os,33 was clamped on a universal MTS-type tensile-
testing machine equipped with a 2 N capacity load cell
and a span length of 10 mm. The load was applied at a
constant crosshead-displacement rate of 1 mm/min up
to failure, in a controlled environment with a tempera-
ture of 23 C and relative humidity of 48%. The deter-
mination of the tensile properties was carried out in
accordance with the NF T 25-501-2 (flax fibres) and
the NF EN 1007-4 (advanced technical ceramics)
standards which take into account the compliance of
the loading frame. Fifty valid tensile tests were per-
formed to ensure reliable results. In addition to the
stiffness defined according to standard NF T 25-501-
2, the stress-strain curves were studied to understand
the evolution of tangent modulus with increasing
strain, as seen in Figure 4.
7
IFBT sample testing – Technical fibres
The tensile tests were performed in the longitudinal
direction of the IFBT samples. A gauge length of
150 mm was used. The samples were rectangular with
2 mm thickness, 10 mm width and 200 mm length. At
least 6 samples were tested by each laboratory in order
to ensure reproducibility and reliable standard devi-
ations. Only the HSB laboratory used 35 mm gauge
length because of the dog-bone shape of 2 mm
x2.8 mm x60 mm of the sample manufactured accord-
ing to the DIN EN ISO 527-2 standard. All samples in
all labs were conditioned for at least 24 h at a controlled
temperature of 23 C  1 C and a relative humidity of
50%  2% (RH ¼ 48% for UBS).
Abrasive paper was placed without any glue in-
between the testing clamps and the samples to avoid
slippage. However, in the tests carried out by UBS,
glass fibre composite end tabs were used. These were
bonded and cured for 24 h at room temperature followed
by 14 h at 50 C. Finally, the HSB laboratory did not use
either end tabs or abrasive paper, because the samples
had a dog-bone shape. The porosity content in the
samples (and the volume fraction) was calculated by
image analysis from the picture shown in Figure 3.
All remaining parameters are described in Table 2.
The calculations of the composite properties were
made according to the standards ISO 527, DIN EN
ISO 527-2 and ASTM D3039, which are standards
8 Journal of Reinforced Plastics and Composites 0(0)

Figure 4. Example of a tensile test on an elementary flax fibre. The dotted line is the behaviour (stress/strain curve), and the full line
is the tangent modulus. The red dot represents the yield point.

Table 2. Tensile testing parameters.

Specimen shape
and dimensions Strain Extensometer
thickness  width rate Load type and gage
Institute  length (mm) Standard Equipment (% min1) cell (kN) length (mm)

KU Leuven Rectangular ASTM D3039 Instron 4505 4 30 Clip-on 50

2  10  200
UBS Rectangular ISO 527 MTS Synergie 4 10 (preload 25
2  10  200 RT 1000 80 N)
IFREMER Rectangular ASTM D3039 Instron 5566 4 10 Clip-on, 50
2  10  200
HSB Dog-bone DIN EN Zwick Z020 2 20 (preload 50
4  10  15 ISO 527-2 10 N)
ENSICAEN Rectangular ASTM D3039 Instron 3366 4 10 25
2  10  200

for tensile testing of unidirectional and symmetric and
balanced laminate composites. The main difference
between these standards and the present characterisa-
tion method is that two stiffnesses are calculated from
the stress-strain data:
. Ef,1: the stiffness is calculated between 0% and 0.1%
strain
. Ef,2: the stiffness is calculated between 0.3% and
0.5% strain
The reason for calculating two values for the stiff-
ness is that it has been observed that, in flax fibre com-
posites, a decrease in stiffness can occur at strains
higher than 0.2%,34 this was also observed in our
experiments (see Figure 5, IFBT results for technical
fibres section). It is important to provide both values
as they can be relevant for design purposes. The
strength was calculated at the maximum strain and
only the samples which failed between the grips were
deemed valid.
Bensadoun et al. 9

Figure 5. Stress–strain curve of flax-epoxy IFBT specimens from KU Leuven (Vf ¼ 52–62%), UBS (Vf ¼ 35–55%) and IFREMER
(Vf ¼ 25–29%). The zones were the moduli E1 and E2 are calculated are indicated.

(ISO 10618:20043). From the measured composite

Fibre volume fraction calculation properties on this impregnated fibre bundle, the fibre
The calculation of the fibre volume fraction (Vf) was properties can be back-calculated using the following
performed in the following way and according to the formulae, which are in fact the inverted formulae of the
ISO 14127:2008 standard:35 well-known ‘‘rule of mixture’’:36

mf EC  Em ð1  Vf Þ
f Ef ¼ ð3Þ
vf ¼ ð1Þ Vf
Vc
where mf is the mass of the fibres (mf ¼ vf  Vc  f Þ, VC  C   0 m ð1  Vf Þ
 u, f ¼ ð4Þ
is the volume of composite and rf the density of the Vf
fibres. A density of flax of 1.4 g/cm3 was used for the
calculations. This method was used by KUL, Ensicaen where Ef is the longitudinal modulus of the fibre, Em is
and UBS. A second method, used by HSB and the modulus of the matrix and Vf is the fibre volume
IFREMER, determines the Vf using the mass of the fraction, sf is the longitudinal strength of the fibre and
fibre and the mass of the composite with the hypothesis s’m the stress in the matrix at the failure strain, which
that there is no porosity (equation (2) can be calculated assuming linear elastic deformation of
the matrix up to the moment of fibre (and hence com-
mf posite) failure: s’m ¼ Em * "u, c. Equation (4) is valid
 only when the fibres fail first, meaning that they have a
Vf ð%Þ ¼ m mf  m  100 ð2Þ
f c f lower failure strain than the matrix. For this reason, the
þ
f res matrix needs to have a sufficiently high ductility.

Statistical analysis – One way ANOVA

Back-calculation of the fibre properties
From the strength and stiffness of the impregnated fibre
bundles, the properties of the flax fibres, as they are
present and behave in a composite, can be determined,
using the methodology developed for carbon fibres
To evaluate in a ‘quantitative’ way whether the results
for each measured property were significantly different
or not, the data generated by the 5 labs, (i.e. stiffness
Ef,1 and Ef,2,and strength su,f) were statistically evalu-
ated using a a one-way analysis of variance statistical
10
technique, ANOVA, with a confidential interval of
95% (a ¼ 5%). The post hoc single-step multiple com-
parisons (grouping) were done using the Tukey
method. The calculations were performed using the
JMP 11 statistical software.37
Results and discussion
Elementary single fibre testing
As the unidirectional flax composite in the IFBT is con-
stituted of flax technical fibres and within them elemen-
tary fibres, tensile tests were carried out in order to
assess the behaviour of both constituents. The technical
fibre properties, back-calculated from the IFBT results,
are compared with the results from the SFT on elemen-
tary fibres. The tensile tests on elementary fibres are
delicate, due to their small diameter and their modest
length. It is not straightforward to keep the elementary
fibres perfectly straight and aligned with great precision,
once clamped in the tensile machine. A misalignment
could lead to an inaccuracy in the measurement of the
strain at small deformations.
Table 3 shows the average diameter and average ten-
sile mechanical properties of the elementary fibres,
while Figure 4 shows the full stress-strain curve of an
elementary fibre. A non-linear behaviour was observed,
thus confirming the need to calculate two stiffnesses
according to the strain region. The moduli (Ef,1 and
Ef,2) of the elementary fibres are calculated, using the
stress-strain curves and the modulus-strain curves pre-
sented in Figure 4.
The yield point corresponds to the point coinciding
with a drop in tangent modulus, i.e. the deviation from
linear-elastic behaviour. It is represented by the red dot in
Figure 4. The tangent modulus is calculated as the ratio
of the stress increment to the strain increment for succes-
sive readings of the stress and strain. This tangent modu-
lus (Etan) technique is also used to calculate the initial
composite modulus, from which Ef,1 is back-calculated.
The tangent modulus (Etan) value is not constant and
there is a maximum value for low deformations. Hence,
the value of Ef,1 mentioned in Table 3 is the average of
the maximum values of Etan, measured in the initial strain
interval (< 0.3%). For the calculation of Ef,2, the NF
T25-501-2 standard31 was used.
IFBT results for technical fibres
A set of typical stress-strain curves for the IFBT speci-
mens with technical fibres, tested in tension, is pre-
sented in Figure 5. also here, the non-linearity can be
clearly observed, and the slope changes at a strain of
about 0.25%. It has to be noted that the scatter in
properties is caused by the variation in fibre volume
Journal of Reinforced Plastics and Composites 0(0)
Table 3. Tensile tests on elementary flax fibres.
Ef1 Strength
Diameter (GPa) Ef2 s f,u
(mm) (Etan) (GPa) (Mpa) " (%)
Average 19 57 44.5 791 1.8
Standard 3 12.8 13.6 319 0.5
deviation
Note: The average fibre diameter and average mechanical properties are
listed. Etan max is the maximal tangent modulus for low strain represent-
ing Ef1. Ef2 is the tangent modulus for the second part of the curve
(strains > 0.5%) according to the standard NF T25-502.
varying from 52% to 62% depending on the sample.
In order to determine the back-calculated fibre proper-
ties, individually obtained by each of the participating
laboratories, equations (3) and (4) have been applied
separately to the data sets of each of the laboratories,
while taking into account the fibre volume fractions of
each of the specimens individually.
Figure 6 presents all the individual data on stiffness
and strength of technical fibres as a function of the
measured fibre volume fraction. It can be observed
that these data follow a trend, as predicted by the
rule of mixture for stiffness and strength, taking into
account an average modulus and stress at fibre failure
for the matrix of Eavg ¼ 3 GPa and s’m ¼ 35 MPa
respectively. When these equations are fitted through
all the experimental data, the following average values
are found for the fibre stiffnesses and strength: E1,f ¼
59.8 GPa, E2,f ¼ 40.8 GPa and su,f ¼ 527 MPa. These
values can be considered as an overall average for the
back-calculated properties, and are represented in
Figure 7 by the dotted horizontal lines.
The results, presented in the diagrams in Figure 7(a)
and (b), clearly show that the difference between the
data of the five laboratories for the back-calculated
fibre stiffnesses E1,f and E2,f is limited, as the average
values fall within a scatter band of  5% around the
overall average. This was expected as the modulus
is known to be less sensitive to imperfections in the
fibre-matrix interface, in the fibres and in the compos-
ites than the strength. As expected, the average value
for the stiffness at higher strains (> 0.3%) E2, f is about
31% lower than for the stiffness at very low strains
(<0.1%) E1, f, which is in fact the ‘real’ Young’s modu-
lus according to its strict definition. The reason for this
non-linearity, which starts at strains between 0.2 and
0.3%, has been related to several possible phenomena.
When all elementary fibres in a technical fibre are well
bonded to the matrix, the non-linearity should be
linked to the intrinsic non-linearity of the elementary
fibres, which is mostly explained by the start of visco-
plastic deformation of the amorphous materials inside
the different lamellar layers or S-walls38 (see flax fibre
Bensadoun et al. 11

Figure 6. Composite properties vs. fibre volume fraction: (a) modulus and (b) strength.

internal wall structure in Célino et al.39), and which was
also observed in the elementary fibre test (see Figure 4).
At much higher deformations (> 0.3%) this could grad-
ually lead to a rotation of the crystalline cellulose
microfibrils towards the loading (longitudinal) axis,
resulting in a gradual increase of the stiffness, and
hence of the slope of the stress-strain-curve.
However, not all elementary fibres are well bonded
to the matrix. When a technical fibre contains a large
number of elementary fibres, the interior ones are not in
12 Journal of Reinforced Plastics and Composites 0(0)

Figure 7. Back-calculated properties of the technical flax fibre: (a) modulus and (b) strength. Dotted horizontal lines (E1 - - - and E2
) represent the average values, as calculated by fitting the rule-of-mixture equation through all the experimental data.

contact with the matrix. Then a second mechanism can
lead to the decrease in stiffness and hence to the observed
‘‘yield point’’ (as seen in Figure 5): when some ‘interior’
elementary fibres are bonded to their neighbours by only
a weak pectin-rich layer, shear deformation in these
layers could occur. This will reduce the contribution of
these weakly bonded elementary fibres to the resistance
of the embedded technical fibre against deformation,
and hence to the measured and back-calculated stiffness
of the embedded technical fibre. This is not an artefact,
but a fundamental characteristic of the behaviour of the
technical fibre inside a composite. Hence, the measured
E2,f is a correct representation of the behaviour of tech-
nical flax fibres in composites at higher strain levels.
Thus, it can be stated that the IFBT will provide a reli-
able, albeit average, fibre stiffness for both E1,f and E2,f.
The variation in strength is higher than the stiffness
variations, as shown in Figures 6(b) and 7(b)). This is
not unexpected; it is also the case for traditional com-
posites, because the strength depends on the
Bensadoun et al.
distribution of defect sizes and types. The reasons for
the systematic difference between the results of some of
the laboratories are discussed in the next section.
Flax fibre properties - Statistical analysis
In this study, it was observed that some of the fibre
properties, obtained by back calculation from the
IFBT data, presented a certain variation between
the five participating laboratories, as shown again in
Figure 7. The question however remains whether this
scatter is acceptable and whether there was a significant
difference between the results of the different labora-
tories. In order to quantify this in a reliable way, a
statistical ANOVA study was performed using
Tukey’s grouping method (see section 2.8). Table 4
summarises the results obtained for the moduli (E1,f
and E2,f) and the strength su,f. It was confirmed, as
was mentioned before in a qualitative way, that there
were no significant differences in modulus values (95%
confidence level) for all laboratories, as they all share
the letter A (Tukey’s grouping method, see Table 4).
As for the strength significant differences were found
between the laboratories: only KUL and Ensicaen seem
to be similar (sharing letter A), with UBS having a
slight but significantly lower strength value. Usually,
a large variation in flax fibre strength is attributed to
the flax fibre extracting conditions and refining, the
crop quality, the environmental conditions during
growing, etc. . . In this study however, all the fibres
came from the same batch, and hence these explan-
ations are unlikely. The low value for the IFREMER
tests is probably related to the manufacturing method
as a mechanical clamping system rather than a press
was used to apply pressure, and this may encourage
heterogeneous fibre distribution and lower strength.
The lack of consolidation pressure in the HBS sample
could also have caused a misorientation of the fibres
(due to the dog-bone shape obtained through
Table 4. Statistical analysis of tensile properties of flax back-
calculated properties.
E1 E2
KU Leuven A A
UBS A A
IFREMER A A
HSB A A
ENSICAEN A A
Note: All the grouping was obtained from the Tukey’s method. A, B and C
are just names given to the three groups which have been distinguished
when applying Tukey’s method.
13
pultrusion as described in section 2.3) and a higher por-
osity level (2.9%), which may cause a further reduction
of the longitudinal strength. Hence, the variation in
strength, observed between the different laboratories,
could be related to a difference in composite manufac-
turing, leading to a different quality of the test samples.
For instance, a small misorientation of the fibres during
composite manufacturing could lead to a locally
increased stress, and hence to a decrease of the longi-
tudinal strength, which in turn leads to a reduction of
the back-calculated fibre strength.40
There may also have been small variations in retting
and defects related to the hackling, although these
effects are expected to be minimal as the retting was
carefully controlled and the scutching and hackling
were performed under optimum conditions. Finally,
also the manipulation of the fibres by the operator
and the way the fibres are stored before the composite
manufacturing will play a role.
Because strength is a defect sensitive property, the
larger variation in strength suggests that even more
attention should be paid to a fully randomised fibre
selection and a defect free specimen preparation.
Comparison with results on elementary fibres
Two points need to be considered if the correlation is to
be made between the elementary fibre properties and
the back-calculated properties of the technical fibres
from the IFBT. First, the span length of the elementary
fibre tests was 10 mm and it is known that this length
influences the mechanical properties and in particular
the tensile strength.26,33 Secondly, the technical fibres
in the IFBT tests are a combination of several
elementary fibres.
Comparing the back-calculated technical fibre prop-
erties obtained with the IFBT method to the elementary
fibre properties measured by the SFT (see Table 5),
some interesting observations can be made. First, the
scatter in the back-calculated data from the IFBT is
much smaller than the elementary fibre test data
Strength Table 5. Elementary flax fibre properties vs back-calculated
technical fibre properties.
A
B Strength
C Ef1 (GPa) Ef2 (GPa) s f,u (Mpa)
BC Elementary 57.0  13 44.5  14 791  319
A fibre test
Back-calculated 59.8  2.4 40.8  3.5 527  138
from IFBT
IFBT: impregnated fibre bundle test.
Note: Mean values and standard deviations are indicated.
14
(+/- 4% vs. +/- 23% for E1,f). This is logical as the
IFBT sample contains a few tens of technical fibres, and
hence a few hundreds of elementary fibres and each
measured composite data point provides an average
value in itself. Even for strength, the scatter in the
IFBT-derived values is about half of that of the elem-
entary fibre test (+/- 26% vs. +/- 40%).
Second, the average values of fibre stiffness follow
the same trend in both the IFBT and the SFT results,
Ef,2 being about 30% lower than Ef,1. It is interesting to
observe that Ef,1is almost identical for both test meth-
ods, suggesting that, at these low strains and hence low
loads, the elementary fibres in the technical fibres,
embedded in the IFBT-samples, do not yet slip over
each other. This seems however to be different for the
stiffness Ef,2 measured at higher strains. In this case the
IFBT results in about 10% lower values than the elem-
entary fibre test. This is consistent with the assumption
that, at higher strains, the elementary fibres inside the
technical fibres, embedded in the IFBT-samples, can
indeed slip over each other, leading to a lower back-
calculated stiffness as previously mentioned in section
3.2.
Third, despite the large scatter, it can be stated that
the average strength of the elementary fibres is higher
than that of the technical fibres. This was not unex-
pected, because the technical fibres are composed of
shorter elementary fibres, and hence fracture can be
induced by debonding of the elementary fibres, starting
at their fibre ends. On the contrary, elementary fibres
can be considered as short but continuous filaments,
and hence fracture has to be introduced by all kinds
of defects (for instance at kink bands), leading to a
higher average strength but also a larger scatter.
Conclusions
In this study, the applicability and the reliability of the
IFBT technique to determine the flax fibre properties
by back-calculation from the composites properties was
investigated. The results show a very low scatter
between the five laboratories for the two stiffness
values Ef,1 and Ef,2, back-calculated from the IFBT-
results, typically less than  5%. These values are
comparable with the stiffness values measured on elem-
entary fibres in the two strain regions. At low strains
(>0.1%), Ef,1 values are very similar for both SFT and
IFBT meaning that the elementary fibres in the tech-
nical fibres (embedded in the IFBT-samples) do not yet
slip over each other. The larger difference observed for
Ef,2 can be explained by the fact that in the IFBT-sam-
ples not all elementary fibres (in particular the ones at
the interior of the technical fibre) might be well bonded
to the matrix, and hence the stress transfer to them is
less efficient, especially at higher strains.
Journal of Reinforced Plastics and Composites 0(0)
However, the back-calculated strength data from the
five laboratories show larger differences. The two
laboratories presenting lower strength values used a
different manufacturing process, potentially resulting
in a lower specimen quality in terms of fibre orientation
and fibre distribution. This highlights on one hand the
necessity to prepare the samples with great care,
according to the proposed method. On the other
hand, it confirms that measurement of strength
always leads to a higher scatter, compared to stiffness
as it depends on critical defects, whereas stiffness is an
average property where small defects are averaged out
and have much less impact. Once the data are com-
pared to the elementary fibre properties, the average
strength of the technical fibres is lower, although the
scatter in the SFT results for the elementary fibres was
higher.
The IFBT-method is well suited for assessing in a
quantitative way the influence of the different extrac-
tion and refining steps on the effective stiffness and
strength of flax and hemp fibres, and of other natural
fibres in composites. Finally, this method could be used
in the future for the characterization of the properties
of twisted yarns in order to study the effect of twist on
the yarn properties. These data can also be used as
input to model woven flax composites and predict
their performance according to the quality of the
yarns as proposed by Straumit et al.41
Acknowledgments
Special Thanks to the remaining members of the European
Scientific Committee of the Technical Section of CELC: Hans
Lilholt, Joris Van Acker, Mark Hughes and Gerhard
Ziegmann, for their valuable input in the development of
this new standard, as well as to Julie Pariset (CELC) for the
efficient coordination of this study. Many thanks to members
of the natural fibre team within the Composite Materials
Group at KU Leuven, Eduardo Trujillo, Dieter Perremans,
Aart W. van Vuure and others, for valuable discussions
during the development of the IFBT method. The authors
also acknowledge Birgit Uhrlaub, Fabian Uhrlaub and
Tim Dunter for the sample preparation and the tensile testing
of the composites. Special mention to Jean-Paul Trouvé from
Terre de Lin for providing the flax fibres samples.
Declaration of Conflicting Interests
The authors declared no potential conflicts of interest with
respect to the research, authorship, and/or publication of this
article.
Funding
The authors disclosed receipt of the following financial
support for the research, authorship, and/or publication of
this article: This research is sponsored by the European
Confederation of Linen and Hemp (CELC).
Bensadoun et al.
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