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Materials and Design 31 (2010) 23972405

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Materials and Design

journal homepage: www.elsevier.com/locate/matdes

Mechanical and thermal characterization of epoxy composites reinforced with

random and quasi-unidirectional untreated Phormium tenax leaf bers
Igor Maria De Rosa a, Carlo Santulli b,*, Fabrizio Sarasini a
a
Sapienza, Universit di Roma, Department of Chemical Engineering Materials Environment, Via Eudossiana 18, 00184 Rome, Italy
b
Sapienza-Universit di Roma, Universit di Roma, Department of Electrical Engineering, Via Eudossiana 18, 00184 Rome, Italy

a r t i c l e i n f o a b s t r a c t

Article history: The present work investigates tensile and exural behavior of untreated New Zealand ax (Phormium
Received 5 October 2009 tenax) ber reinforced epoxy composites. Two series of laminates were produced using the same rein-
Accepted 26 November 2009 forcement content (20 wt.%), arranged either as short bers or quasi-unidirectional ones. Composites
Available online 3 December 2009
reinforced using quasi-unidirectional bers showed higher modulus and strength both in tensile and ex-
ural loading, when compared to neat epoxy resin. Short ber composites, although still superior to epoxy
Keywords: resin both for tensile and exural moduli, proved inferior in strength, especially as concerns tensile
A. Natural materials
strength. These results have been supported by scanning electron microscopy (SEM), which allowed char-
E. Mechanical
G. Non-destructive testing (NDT)
acterizing bermatrix interface, and by acoustic emission (AE) analysis, which enabled investigating
failure mechanisms. In addition, thermal behavior of both untreated phormium bers and composites
has been studied by thermogravimetric analysis (TGA), revealing the thermal stability of composites to
be higher than for phormium bers and epoxy matrix alone.
2009 Elsevier Ltd. All rights reserved.

1. Introduction choice of manufacturing technique and type of matrix to be used

In recent years, the use of natural (ligno-)cellulosic bers, e.g.,
ax, hemp, sisal, kenaf, banana and jute, has been gaining a note-
worthy attention in polymer composites, as an alternative to tradi-
tional bers such as glass, carbon, and aramid. The increasing
interest in these materials is due to the inherently environmentally
friendly nature of natural bers, leading to carbon dioxide mitiga-
tion, their low cost and low density. Other advantages include bio-
degradability, recyclability and signicant processing advantages.
In particular, equipment abrasion, energy consumption, pollutant
emission, dermal and respiratory irritation are all reduced.
However, signicant drawbacks in the use of plant bers are in
the variability and non-uniformity of the dimensions of the bers
and of their mechanical properties, their high moisture absorption,
low microbial resistance and poor wettability. The use of plant -
bers as a reinforcement of polymer matrices is also limited by their
polarity, mainly due to hydroxyl groups, and their hydrophilic nat-
ure. These characteristics result in plant bers incompatibility with
oil-derived thermoplastic matrices (e.g., polyolens), having a non-
polar and hydrophobic character, and in a consequent poor interfa-
cial bermatrix bonding and non-uniform dispersion of the bers
within the matrix. Another serious drawback is the low thermal
stability of lignocellulosic bers above 200 C, which limits the
* Corresponding author. Tel.: +390644585539.
E-mail address: carlo.santulli@uniroma1.it (C. Santulli).
for composite production [14].
In particular, Phormium tenax, commonly known as harakeke or
New Zealand ax, belongs to Agave family, and is a monocotyle-
donous endemic to New Zealand and Norfolk Island. The leaves
are stiff and can grow up to 3 m long and 125 mm wide. The hara-
keke ber aggregates, referred to as muka, lie along the leaves and
are extracted from their upper and lower side. The muka consists
of aggregates of ultimate sclerenchyma bers (individual elon-
gated hollow cells) arranged as overlapping bundles in a spiral
geometry [5]. The traditional use of phormium stripped leaves in
the Maori culture was making plaiting mats and containers, whilst
extracted bers have been used for weaving tissues and making
ropes [6]. However, phormium industry appeared to be declining
in New Zealand during last decades.
A recent study indicated that the exural strength of epoxy re-
sin reinforced by NaOH-pulped phormium leaf reinforced compos-
ites is about 30% lower than that of chopped E-glass strand mat
with the same ber volume, whilst the exural modulus of the
two composites is comparable [7]. In [7] phormium bers were ar-
ranged after pulping to form a hand-prepared mat, a geometry
which has been suggested to reduce the micro-compressive de-
fects, also referred to as kink bands, which are a common cause
for mechanical weakness of plant bers [8]. It is also suggested
elsewhere that alkali treatment is benecial on reducing water
uptake in phormium bers by removing acetylate groups from
the bers, hence improving ber adhesion with epoxy matrices [9].

0261-3069/$ - see front matter 2009 Elsevier Ltd. All rights reserved.
doi:10.1016/j.matdes.2009.11.059
 Author's personal copy
2398 I.M. De Rosa et al. / Materials and Design 31 (2010) 23972405
The purpose of this study is trying to compare two possible phor-
mium ber arrangements in epoxy composites, using untreated -
bers, extracted by pure combing and washing from the central
section of the leaves. This would allow appreciating which are the
inherent possibilities of this ber as for composite reinforcement,
initially without the application of any chemical surface treatment
which may considerably hinder their eco-compatibility prole.
2. Materials and methods
2.1. Fibers and resin
Phormium tenax bers were collected from New Zealand. Leaves
were stripped and the hanks of ber were washed and then pad-
docked and scutched [9] (Fig. 1). Fibers of 20 mm in length were
chopped in order to manufacture the short ber reinforced compos-
ites. The scattering in ber diameters was assessed through optical
microscopy and an average diameter was obtained from three
apparent diameter measurements taken at different positions along
the bers. Each ber was considered as perfectly round to simplify
the analysis. The average diameter and standard deviation of the -
bers tested (50 bers were tested) was 151.3 45.65 lm.
The matrix used was a low viscosity epoxy system (SP Systems
Ampreg 26) with a slow hardener (mixing ratio 100:33.3 by
weight).
2.2. Composite fabrication
The composites were manufactured in an aluminum mould
(250 mm  250 mm). The mould was coated with a thin layer of a
release agent (polyvinyl alcohol) and then the short bers, ran-
domly arranged like a mat, were placed in the mould. The resin
and hardener mixture was poured into the mould and was left to
soak into the ber mat, following the procedure described in [10].
Fig. 1. Dry Phormium tenax bers.
Fig. 2. Typical samples of Phormium tenax reinforced epoxy composites.
The mould was then closed with another aluminum mould and
the resin was left to cure for 24 h at room temperature followed
by 24 h-post curing at 70 C. The quasi-unidirectional composites
were manufactured in the same way, except that the continuous -
bers were aligned by hand before being soaked in the resin. The -
ber weight fraction was controlled by using known weights of ber
and matrix. The nal weight fraction was 0.20 0.02 for both types
of composite materials. For comparison purposes, a neat resin panel
was also manufactured.
Upon completion of the curing cycle, the composite laminate
panel was removed from the mould and ready for being cut into
test specimens (Fig. 2).
2.3. Tensile and exural testing
The dimensions of the specimens were 200  30  5 mm and
130  30  5 mm for tensile and exural tests, respectively. The
mechanical characterization was carried out by longitudinal ten-
sion test (ASTM D-3039) and three-point bending test (ASTM D-
790) using an Instron 5584. Crosshead speeds of 1 mm/min and
2.5 mm/min were used for tension and bending tests, respectively.
The span-to-depth ratio was 20:1, while the gauge length was
120 mm for tensile tests. All the specimens tested were equipped
with strain gauges (HBM GmbH, type 1LY113/350) in order to
measure the tensile and exural moduli. All the results were taken
as the average value of ve samples.
2.4. Acoustic emission monitoring (AE)
An AMSY-5 acoustic emission system by Vallen Systeme GmbH
was used to monitor and record the AE signals during the mechan-
ical tests. The threshold setting was 35 dB and the total gain was
set at 34 dB. Four PZT (lead zirconate titanate) sensors resonant
at 150 kHz (Deci, type SE150-M) were used for AE detection. Two
sensors were placed on the surface of the specimens at a distance
of 120 mm and 90 mm (for exural and tensile tests, respectively)
to allow linear localization and other two sensors were used as
guard sensors.
2.5. Scanning electron microscopy (SEM)
A scanning electron microscope Hitachi S-2500 was used to
investigate the ber morphology and the fracture surfaces of
composites.
2.6. Thermal analysis (TGA/DTG)
Thermogravimetry (TGA) and differential thermogravimetry
(DTG) techniques were used to analyze the thermal stability of -
bers and composites. Thermogravimetric analysis was carried out
to analyze the thermal stability of bers and composites. All the
measurements were performed using a TA Instruments High Reso-
lution 2950 TGA thermogravimetric analyzer. Samples weighing
between 10 and 20 mg were placed in a platinum pan and tests
were carried out in a programmed temperature range of 20
700 C at a heating rate of 5 C/min under nitrogen atmosphere
at ow rate of 50 ml/min.
3. Results and discussion
3.1. Chemical composition and ber morphology
It is worth noting that chemical composition as well as the struc-
ture of plant or vegetable bers is fairly complicated. Plant bers can
be considered as a natural composite material wherein rigid crystal-
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I.M. De Rosa et al. / Materials and Design 31 (2010) 23972405 2399

Table 1
Chemical composition, moisture content, and microbrillar angle of some plant bers.

Type of ber Cellulose (wt%) Hemicellulose (wt%) Lignin (wt%) Pectin (wt%) Moisture content (wt%) Wax (wt%) Microbrillar angle () Ref.
Bast ber
Flax 64.171.9 16.720.6 2.02.2 1.82.3 812 1.7 510 [11,15,16]
Hemp 70.274.4 17.922.4 3.75.7 0.9 6.212 0.8 26.2 [11,15,16]
Jute 6171.5 12.020.4 11.813 0.2 12.513.7 0.5 8 [11,15,16]
Kenaf 3157 21.5 819 35 [11,16]
Ramie 68.676.2 13.116.7 0.60.7 1.9 7.517 0.3 7.5 [11,15,16]
Leaf ber
Sisal 65.878 814 1014 0.810 1022 2 1022 [11,15,16]
Phormium T. 45.172.0 30.1 11.2 0.7 10.0 0.7 [1719]
Henequen 77.6 48 13.1 [11,16]
Pineapple 7082 512.7 11.8 14 [11,16]
Banana 6364 1019 5 1012 11 [11,20]
Seed ber
Cotton 82.790 5.7 01 7.858.5 0.6 [11,15,16]
Fruit ber
Coir 3243 0.150.25 4045 34 8 3049 [11,15,16]

line cellulose microbrils are embedded in an amorphous lignin and/
or hemicellulose matrix in a given orientation [11].
Generally, plant bers may be classied into the following main
categories, depending on the part from which they are extracted:
bast or stem, leaf, seed, fruit, stalk and grass. The basic constituents
of all these bers, with the exception of cotton, are cellulose, hemi-
cellulose and lignin; they also contain some pectin, waxes and
water-soluble compounds [1214].
The chemical compositions and structural parameters of several
important plant bers are represented in Table 1. As reported in
Table 1, the chemical composition of a specic plant ber may vary
considerably. Such variation, as well as the difference in structure
of plant bers, may be inuenced by area of growth, climatic con-
ditions, age of the plant and the mode of extraction process of the
ber from source adopted. In particular, Phormium tenax ber is a
multicellular lignocellulosic leaf ber having a relatively low
cellulose and high hemicellulose content compared to other com-
mercial plant bers [18]. This plays an important role in the tough-
ness of the plant bers as the toughness increases with growing of
the hemicellulose and lignin [21].
Microscopic examinations of the longitudinal and cross section
surface of Phormium tenax bers are depicted in Figs. 35. The mor-
phological structure of the ultimate bers of Phormium tenax, also
called technical bers, comprises a thick wall with a central lumen
(Fig. 3a), both of irregular shapes and different diameter as can be
seen in Fig. 3b. In particular, in Fig. 4a a number of lumens appear
to be completely lled with protoplasm [22]. The thick wall is built
up of several layers of microbrillar structure consisting of micro-
brils linked together by hemicellulose and lignin matrix of varying
composition. Typically, the ultimate ber diameter in Phormium te-
nax bers is in the range of 525 lm [12,18,19,23,24]. This scatter-
ing has a considerable inuence over the mechanical properties of
both bers and composites.
Microscopic examination of the cross section of Phormium tenax
bers reveals aggregate bundles of ultimate bers having different
cross sectional shapes, which can be categorised in a few number
of geometries, as will be specied below. In particular, scanning
electron micrographs of cross sections of typical Phormium tenax
technical bers are shown in Fig. 4. The transverse sectional shape
of the ber aggregate bundles is highly variable and depends on
the location within the leaf, where the bundles were extracted
(upper or lower) [5,6].
In particular, ber cross-section is seldom circular. Common
geometries are usually referred to as horseshoes shape or key-
hole-like shape, as shown in Fig. 4a and b, respectively. Whilst the
horseshoes shape bundles are situated in the lower part of the leaf,
the keyhole-like bundles are in the upper one [5,6,9,23,24].
It is also worth noting that the horseshoe shape is similar to that
of the bers of sisal leaf [25]. Furthermore, in the centre of the leaf
the cells between the upper bers and lower ones are relatively

Fig. 3. Micrographs of cross sections of Phormium tenax bers: (a) ultimate ber and (b) technical ber.
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2400 I.M. De Rosa et al. / Materials and Design 31 (2010) 23972405
Fig. 4. Micrographs of cross sections of two typical bers of Phormium tenax: (a) horseshoe shape and (b) keyhole-like shape.
Fig. 5. Micrographs of longitudinal (a) and cross section (b) of Phormium tenax bers.
large and with a thin wall, and are characterized by helical brils,
as indicated by the arrows in Fig. 5a and b. These cells are known as
vascular bundles [5,24,26] and are considered to be pathways for
uids in the plant bers.
In longitudinal and cross section surface of Phormium tenax rep-
resented in Fig. 5a and b, respectively, it can be appreciated on the
external surface of the cell wall the presence of ligninaceous mate-
rial, hydrophobic non-cellulose compounds (such as waxes or fats)
and surface impurities. These compounds constitute a protective
and smooth layer on the surface of the bers and bond the bers
together. As a consequence, this surface forms weak bonds at the
interface between the ber bundles and the polymeric matrix of
the composite.
3.2. Thermal degradation by TGA
As thermal stability is considered one of the limiting factors in
the use of natural bers as reinforcement for composites in com-
parison with synthetic ones, the thermal stability of Phormium te-
nax bers was investigated. In particular, TG and DTG curves were
used to study the high temperature degradation behavior of neat
resin, Phormium tenax bers, and epoxy resin composite containing
20 wt% ber, as shown in Fig. 6a and b, respectively.
In Phormium tenax bers, the decomposition occurs in two main
stage process, as shown in TG curve of Fig. 6a. This is in agreement
with other studies on lignocellulosic bers [2731].
According to Wielage et al. [32], the TG curve shows that the on-
set of thermal degradation for Phormium tenax bers does not occur
before 200 C, whilst the initial weight loss (8%) between 37 and
130 C corresponds to the vaporization of water from the bers.
Above this temperature, thermal stability is gradually decreasing
and decomposition of bers occurs (Fig. 6a). The rst stage process
TI (200305 C) is the thermal depolymerisation of hemicellulose,
pectin and the cleavage of glycosidic linkages of cellulose (weight
loss 20.0%) [28,33,34], the second one TII (305370 C) is attributed
to the decomposition of the a-cellulose (weight loss 45.2%) [35,36],
whilst the decomposition of lignin takes place in a wide tempera-
ture range (200900 C) [3234,37]. Among these components, lig-
nin was the most difcult one to decompose. Its decomposition
occurred slowly within the whole temperature range. It is due to
the complex structure of lignin, having an aromatic structure with
various branches [37].
The residual weight of Phormium tenax bers has also been
measured: this is equal to 15.7 wt% at 700 C (Fig. 6a).
Table 2 shows the weight losses and also the peak temperatures
for the Phormium tenax bers at the different stages. These results
are also conrmed by DTG curves (Fig. 6b). In DTG curve of Phormi-
um tenax it can be appreciated that most cellulose decomposition
occurs at the temperature of 337 C. Neat resin decomposes at a
temperature of 335 C, which is slightly lower than that of the ber
whilst the composite decomposition occurs later at 347 C. There-
fore, the system bermatrix degrades later than the neat resin. As
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I.M. De Rosa et al. / Materials and Design 31 (2010) 23972405 2401

Fig. 6. (a) TG and (b) DTG curves of neat resin, Phormium tenax bers, and Phormium tenax reinforced composites.

Table 2
Thermal degradation data of Phormium tenax bers at 5 C/min in nitrogen atmosphere.

Weight loss (%) below 130 C First degradation stage Second degradation stage Residual char (wt%)
TI (C) Weight loss (%) Tpeak (C) TII (C) Weight loss (%) Tpeak (C)
Phormium T. Fibers 8.1 200305 20.0 270 305370 45.2 337 15.7

a consequence, the thermal stability of the composite is higher
than those of ber and matrix. It can be due to improved berma-
trix interaction [38].
3.3. Mechanical properties
The use of untreated leaf-extracted bers in composites can be
considered as the rst step for a possible use of the bers as an
effective reinforcement. Further studies would need to evaluate
the degree of improvement in ber quality obtained by the differ-
ent chemical treatments, aimed at removing non-structural mat-
ter, such as pectin and wax. In addition, hand lay-up of plant
bers, adding to the effect of variable ber diameters and section
geometries, is recognized introducing mismatches in the orienta-
tion of bers, when introduced in the resin. The signicant effect
of disruption in reinforcement orientation on mechanical results
has been analyzed already on composites reinforced using leaf-ex-
tracted bers, such as, e.g., palm leaves [39]. It was therefore con-
sidered whether it was more reasonable, for a rst approach to this
type of reinforcement ber, to use longer bers in a quasi-unidirec-
tional arrangement or rather try a random short ber arrangement.
The tensile and exural properties of composites with different
ber arrangement were compared to neat epoxy. Figs. 7 and 8
show the mechanical properties of the tested materials. As a gen-
eral result, the addition of phormium bers increased the modulus
in all composites, regardless of the ber arrangement and type of
loading. On the other hand, the different ber arrangement af-
fected both the tensile and exural strength. In particular, the qua-
si-unidirectional bers improved both the tensile and exural
strength of the neat resin by 25% and 32%, respectively. The addi-
tion of short phormium bers had a negligible effect on the exural
strength but caused tensile strength to decrease by approximately
40%. This outcome is not totally unexpected. From previous studies
[4044], it has been demonstrated that mechanical properties of
short ber reinforced composites are strongly inuenced not only
by ber content but also by ber length and orientation. In a dis-
continuous ber composite, the stress along the ber is not uni-
form. A critical ber length is needed for effective transfer of
stress between ber and matrix, which depends in turn on the

Fig. 7. Average tensile strength (a) and Youngs modulus (b) of phormium/epoxy laminates compared to the pure resin.
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2402 I.M. De Rosa et al. / Materials and Design 31 (2010) 23972405

Fig. 8. Average exural strength (a) and modulus (b) of phormium/epoxy laminates compared to the pure resin.

Fig. 9. SEM micrographs showing typical fracture surfaces of (a) short and (b) continuous phormium ber reinforced composites failed in exure.

Fig. 10. SEM micrograph showing the interface in short phormium ber reinforced composite failed in tension.
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I.M. De Rosa et al. / Materials and Design 31 (2010) 23972405 2403

characteristics of the specic bermatrix system, hence on the

quality of the bermatrix interface. In this case, the length used
(20 mm) could not represent the optimum ber length for this type
of composite. This is a key aspect requiring further investigation.
The decrease in tensile strength could also be ascribed to the fact
that only a small part of bers is oriented in the direction of load-
ing in these laminates thus acting as potential defects. This can be a
consequence of the manufacturing process leading to non-uniform
distribution of the bers in the composite, resulting therefore in re-
sin-rich areas and ber entanglements, both detrimental for com-
posite strength.
Figs. 9 and 10 show a detailed view of the fractured surfaces of
phormium ber reinforced composites. A feature that is common
to all fractured surfaces is the occurrence of ber pull-out and
debonding, which appear to be the dominant failure mechanisms
with a lower number of ber breakages. The relative absence of
epoxy particles sticking to the ber surface is a further indication
of poor adhesion between ber and matrix which affected to a Fig. 11. AE localized events at different load levels during tensile tests on
phormium/epoxy composites.
greater extent the mechanical strength of short ber composites.

3.4. Acoustic emission monitoring

The analysis of acoustic emission data during tensile and exural

tests monitoring concentrated on the number of localized AE events
detected during loading. For this purpose, four load levels were iden-
tied, namely I = 025% Fmax, II = 2550% Fmax, III = 5075% Fmax,
IV = 75100% Fmax, following the analysis carried out in [4547].
This analysis, whose results are presented in Figs. 11 and 12,
suggested that acoustic emission activity takes place only at a later
stage in both exural and tensile tests and for both ber congura-
tions. As a general result, more AE events were recorded during
exural loading compared to tensile one. This can be due to the
complex state of stress that is present during a exural test with
tensile, compression and interlaminar stresses. During tensile
loading, most AE events have been detected during the third stage
instead of during the fourth. These signals are not related to ber
breakages, as these signals are concentrated in the amplitude range
Fig. 12. AE localized events at different load levels during exural tests on
5070 dB (as can be seen in Fig. 13) which are generally ascribed to phormium/epoxy composites.
failure mechanisms occurring in the matrix and at the interface,
whilst signals coming from ber breakages are characterized by
higher amplitudes. Quasi-unidirectional composites show a more directional ones with the occurrence of a higher number of high
uniform distribution of signals over the four loading intervals with amplitude AE signals (Fig. 14). This allows suggesting that ber
a larger number of higher amplitude signals during the fourth orientation plays a minor role in exure also in virtue of the more
stage, originating from ber breakages. complex stress state. This can explain the negligible effect of the
During exural loading, it is to be noted that short ber rein- short bers on exural strength compared to the signicant de-
forced composites showed a behavior similar to that of quasi-uni- crease reported for tensile strength.

Fig. 13. Relative distribution (%) of amplitude in short (a) and long (b) phormium ber reinforced epoxy composites during tensile loading (I: 00.25Fmax; II: 0.250.5Fmax;
III: 0.500.75Fmax; IV: 0.751Fmax).
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2404 I.M. De Rosa et al. / Materials and Design 31 (2010) 23972405
Fig. 14. Relative distribution (%) of amplitude in short (a) and long (b) phormium ber reinforced epoxy composites during exural loading (I: 00.25Fmax; II: 0.250.5Fmax;
III: 0.500.75Fmax; IV: 0.751Fmax).
The weakness of interface appears to be conrmed from AE
activity during exural tests, where short ber reinforced lami-
nates show a much larger number of events (especially low and
medium amplitude ones) at all stages, whilst long ber reinforced
ones only present signicant acoustic activity in the nal loading
stage (Figs. 12 and 14).
4. Conclusions
The aim of this study was investigating the use of phormium -
bers as potential reinforcement for epoxy composites. The addition
of bers (arranged in a quasi-unidirectional way) was found to in-
crease both strength and modulus for tensile and exural loading.
The short ber reinforced composites exhibited higher exural and
tensile moduli if compared to the neat resin but lower strength,
especially in tensile loading. The introduction of a limited amount
(20 wt%) of untreated phormium bers in an epoxy resin was dem-
onstrated to have also a positive effect on the thermal stability of
the composites.
Areas of weakness appear to be in the non-optimal control of -
ber orientation achieved with the manufacturing technique
adopted (hand lay-up) and the quality of the bermatrix inter-
face, which was found to affect the mechanical properties of the
resulting composites, as conrmed by SEM and AE analysis. The
next step would be, retaining for the moment the use of thermo-
setting matrices, the improvement of interface through chemical
treatments. However, in the long run, passing to biodegradable
thermoplastic matrices would be recommended. This would assure
both the environmental signicance of these materials and the full
structural exploitation of phormium bers as a reinforcement for
composite materials.
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