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Composites: Part A 37 (2006) 1473–1479

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Tensile mechanical properties, morphological aspects and


chemical characterization of piassava (Attalea funifera) fibers
a,*
J.R.M. dÕAlmeida , R.C.M.P. Aquino b, S.N. Monteiro b

a
Materials Science and Metallurgy Department, Pontifı́cia Universidade Católica do Rio de Janeiro, Rua Marquês de São Vicente,
225, Gávea – 22453-900, Rio de Janeiro, RJ, Brazil
b
Science and Technology Center, Universidade Estadual do Norte Fluminense, Av. Alberto Lamego, 2000, Horto – 28015-820,
Campos, RJ, Brazil

Received 5 August 2004; received in revised form 15 March 2005; accepted 16 March 2005

Abstract

The tensile mechanical properties of piassava fibers, as well as their chemical composition and morphological aspects, are reported.
The values obtained showed that piassava has a mechanical behavior and chemical composition comparable to that of coir fibers. The
difficulties related with a reliable way of measuring the true elastic modulus of these slender fibers are discussed and a simple correction of
the experimental data is presented. As main characteristic surface features piassava fibers present a well arranged pattern of silicon rich
star-like protrusions. Its chemical composition reveals that piassava are lignin rich fibers, 48.4 wt%. X-ray diffraction showed that cel-
lulose I is their main crystalline constituent. Their thermal degradation begins at 225 °C, and the whole thermal degradation behavior of
piassava fibers has many aspects, like the initial water loss and the content of residues, close to that shown by pure lignin.
Ó 2005 Elsevier Ltd. All rights reserved.

Keywords: A. Piassava fibers; B. Mechanical properties; C. Elastic properties; D. Scanning electron microscopy

1. Introduction composites has the benefit of less wear and deterioration


of machine member parts.
Natural fiber reinforced composites have yet many chal- Flax and hemp are the natural cellulosic fibers that at-
lenges to overcome in order to become largely used as reli- tract the most attention in Europe [3]. On the other hand,
able engineering materials for structural elements. jute, sisal, and to a lesser extent coir, are more extensively
However, their use is steadily increasing and many large reported in the literature; see for example [4–9]. There are,
industrial corporations are planning to use, or have yet however, many other less studied cellulosic fibers that are
commencing to use, these materials in their products [1]. attractive, whether by their morphology, by their intrinsic
One of the great advantages of these composites is the large properties or by their cost. Luffa cylindrica is one fine
quantity of natural fibers available worldwide. Further- example of such fibers. Its fibersÕ natural mat like spatial
more, as highlighted on many texts, e.g. [2], natural fibers arrangement provides a detouring path for cracks, and pro-
are a biodegradable and renewable resource. Their softness duces tougher composites [10]. Another of such less studied
is also an advantage in relationship to the common syn- fibers is piassava (Attalea funifera).
thetic fibers, like glass fiber. Natural fibers are much less An earlier study from our group has shown that it is a
abrasive and, therefore, the manufacture of natural fiber promising candidate as fiber reinforcement for resin matrix
composites [11]. Therefore, in this work, the chemical com-
position, structural characteristics and tensile mechanical
*
properties of piassava fibers are presented and its main fea-
Corresponding author. Tel.: +55 021 31141234; fax: +55 021 3114
1236.
tures are highlighted and discussed. One has to point here,
E-mail address: dalmeida@dcmm.puc-rio.br (J.R.M. dÕAlmeida). that although piassava has some characteristics common to

1359-835X/$ - see front matter Ó 2005 Elsevier Ltd. All rights reserved.
doi:10.1016/j.compositesa.2005.03.035
1474 J.R.M. d’Almeida et al. / Composites: Part A 37 (2006) 1473–1479

other lignocellulosic fibers, their properties have not yet 100000


been fully described. And, in order to enable their reliable
use in composites, the basic aspects of their structure and
80000
morphology, such as the lignin content and surface topo-
graphic features, and aspects related to their thermal

production, ton.
behavior, such as the onset of thermal degradation, must 60000

be analyzed. This work aims to fulfill this gap of informa-


tion about these traditional fibers. 40000

2. Piassava (A. funifera)


20000

Piassava is a stiff fiber extracted from the leaves of a


palm tree of natural occurrence at the Brazilian Atlantic 0
rain forest. The natural incidence range of the piassava 1990 1991 1992 1993 1994 1995 1996 1997 1998 1999

palm tree is close to the coastal zone (up to 60 km inland) year

and it is mainly concentrated between 13°S and 17°S lati- Fig. 2. Annual production of piassava fibers.
tudes. Its grow is favored at regions with hot average tem-
perature (24 °C) and high relative humidity (>80%). The
fibers, up to 4 m long with an average width of 1.1 mm, enough to be used as reinforcement in fiber composites
are harvested once by year. The palm leaf is cut, and the [11].
fibers are mechanically separated from the petiole. Each
palm tree can yield 8–10 kg of fibers. Fig. 1 shows typical 3. Experimental methods and materials
cross-sections of piassava fibers, where one can see the
usual variability of form and size common to all naturally Piassava fibers disregarded by a broom industry were
occurring cellulosic fibers. used in this work. Their tensile properties were evaluated
The production of piassava fibers is steadily increasing following the procedures recommended by the ASTM stan-
over the past years and, nowadays, it amounts to about dard D-2101. Since it is not possible to attach mechanically
100,000 metric tons per year, as shown in Fig. 2 [12]. The gripped extensometers to the single fibers under test, sev-
main use of these fibers is for industrial and domestic eral gage lengths were used in order to measure the elastic
brooms, industrial brushes, ropes and baskets, carpets compliance of the test apparatus and to correct for the true
and roofs. It is estimated that around 20% of the fiber pro- modulus of elasticity. The correction procedure used is out-
duction is disregarded by the transformation industries. lined in Appendix A. The gage lengths used were: 150, 120,
These leftover fibers, that do not meet the requisites for 80, 50, 25 and 15 mm. The tests were performed on a
the uses cited above, are, however, undamaged and long mechanically driven machine with 10 kN of capacity and
equipped with pneumatic action grips. An optimum hold
pressure of 0.3 MPa was experimentally found to give reli-
able test data. With this clamping pressure neither fiber
slippage during tests nor fiber crushing at the grips were
found to occur. The test speed used was 1 mm/min and
15 specimens were tested per gage length.
The morphological characterization of the fibers was
done by scanning electron microscopy (SEM). The analysis
was performed on gold sputtered samples using secondary
electrons, and with a beam voltage of 15–20 kV. The com-
position of topographic features identified at the surface of
the fibers was determined by energy dispersive X-rays spec-
trometry (EDS).
The thermal stability of the fibers was evaluated by
thermogravimetric analysis (TGA). This experiment was
conducted under nitrogen atmosphere, from ambient
temperature (25 °C) to 400 °C at a heating rate of 10 °C/
min.
The crystalline character and the chemical composition
of the fibers were determined by X-rays diffraction and
by the van Soest method, respectively. To perform the X-
Fig. 1. Transversal cross-section of piassava fibers. Observe the variability rays analysis a sample was calcinated at 400 °C by 2 h. This
of shape and size. sample was then scanned from 2h = 5° to 2h = 125°, with
J.R.M. d’Almeida et al. / Composites: Part A 37 (2006) 1473–1479 1475

increments of 0.05°, using the Cuja radiation. The equip- palm tree, since many areas appear clean, and there one
ment was set at 35 kV and 40 mA. The van Soest method can observe the common parenchyma cells seen at the out-
is one of the several acid-detergent fiber methods used to er surface of lignocellulosic fibers [15,16], Fig. 4. Fig. 4 also
evaluate lignin and cellulose content of plant materials. It shows, besides parenchyma cells (!), an array of pro-
involves the hydrolysis of the cellulose component with truded features. These protrusions are shown in detail in
72% w/v sulphuric acid solution with deionised water. A Fig. 5 and were identified by EDS as Si rich particles
complete description of this method, as well as a descrip- (Fig. 6). Similar features were also reported for coir fibers
tion of its precision in relationship to other acid-detergent [8,17].
fiber methods, can be found elsewhere [13,14]. A typical stress–strain curve of piassava fibers is shown
in Fig. 7. One can see a non-linear region following the ini-
4. Experimental results and discussion tial linear portion of the graph. Similar behavior was also
reported for other lignocellulosic fibers like sabai [16], coir
The surface morphology of the piassava fibers is shown
in Fig. 3(a). As observed at higher magnification, Fig. 3(b),
areas of the surface of the fibers are covered by randomly
distributed organic material. This organic material is prob-
ably a residue left by the extraction of the fibers from the

Fig. 4. The cleaner parts of the fibersÕ surface show the common
topographic aspects characteristic of natural fibers (!) and an array of
protrusions.

Fig. 3. (a) General aspect of the piassava fibers; (b) Organic residue
attached to the surface of the fibers. Fig. 5. Magnifying view of the protrusions.
1476 J.R.M. d’Almeida et al. / Composites: Part A 37 (2006) 1473–1479

Table 1
Mechanical properties of the piassava fibers
Gage length (mm) ry (MPa) rr (MPa) er (%)a E (GPa)a
15 75.8 ± 18.0 134.8 ± 22.5 21.9 ± 4.3 1.07 ± 0.27
25 81.7 ± 12.4 147.3 ± 25.6 16.3 ± 2.4 2.27 ± 0.52
50 78.4 ± 14.3 131.1 ± 27.1 11.9 ± 4.3 2.58 ± 0.39
80 75.6 ± 8.5 132.8 ± 12.5 8.4 ± 1.9 3.57 ± 0.52
120 69.8 ± 12.6 108.5 ± 16.0 6.4 ± 2.3 3.55 ± 0.86
150 80.2 ± 25.0 142.9 ± 46.8 7.8 ± 3.9 4.59 ± 0.55
Tensile test.
a
Uncorrected values due to test apparatus compliance. See the text for
explanation.

Young´s modulus, GPa 4


Fig. 6. EDS spectrum of the protrusions, showing that they are Si rich
compounds.
3

160 2

140
1
120
0 20 40 60 80 100 120 140 160
100 gage length, mm
srtessM,Pa

80 Fig. 8. Values of the corrected YoungÕs modulus as a function of the gage


length (j). Uncorrected values (H). The value predicted by the procedure
60 described in Appendix A is shown as a dashed line.

40

20 more prominent. Therefore, the elastic modulus decreases


while the deformation increases. To eliminate the elastic
0 contribution of the test machine, the values of the YoungÕs
0 1 2 3 4 5
modulus were corrected using the procedure summarized in
strain, %
Appendix A. Fig. 8 shows the effect of the correction on the
Fig. 7. Typical stress–strain curve of the piassava fibers. fibersÕ modulus as a function of the gage length. As could
be expected, an average constant value is obtained, inde-
pendent of the gage length. Moreover, the corrected values
[17,18] and cellulose [19], and to a lesser extend banana fi- approach the one obtained using the linear fit described in
bers [20]. The experimental results obtained are shown in Appendix A.
Table 1, where ry is the 0.2% offset yield stress, rr is the The corrected value obtained is, however, low when
stress at rupture, er is the strain at rupture and E is the compared with other common natural fibers, as for exam-
YoungÕs modulus. Despite a fairly large variation, that in- ple jute (E = 13–26.5 GPa [2,21]) or flax (E = 50 GPa [3]),
deed are common to lignocellulosic fibers, some clear although it is on the range of cotton (E = 1.1–12.6 GPa
trends could be established. At first, one can see that both [2,22]) and coir (E = 3–6 GPa [22]) and near the lower
the YoungÕs modulus and the deformation at rupture are bound for sisal (E = 9.4–22 GPa [2]).
varying with the gage length. Since the YoungÕs modulus From Table 1, it is also apparent that both the yield
is actually not dependent from gage length, these results stress and the stress at rupture were not dependent on
must be due to the contribution of the compliance of the the test apparatus compliance, as one should expect. There-
test machine. In fact, from the data shown in Table 1, fore, average values could be calculated from the results of
one can see that as the gage length is reduced the contribu- all tested specimens. The computed values for these proper-
tion of the elastic elongation of the test apparatus becomes ties are ry = 76.9 ± 4.2 MPa and rr = 133.0 ± 13.5. To cal-
J.R.M. d’Almeida et al. / Composites: Part A 37 (2006) 1473–1479 1477

culate these values, the actual area of each fiber was mea- One can see that the temperature at which piassava fibers
sured at five different points along the gage length. The begin to degrade is close to that of lignin, being situated
average area value of each fiber was then used on the at the lower bound of the temperatures of the other com-
calculations. mon lignocellulosic fibers. The TGA also shows that a res-
As for the YoungÕs modulus, the tensile strength of the idue of about 40% remains at 400 °C. This value is similar
more common natural fibers are higher than that found to the value of 32.8% reported for lignin [25].
for piassava fibers. For instance, jute (rr = 550–900 MPa In Fig. 9, it is also shown the curve of the first derivative
[22]), sisal (rr = 507–640 MPa [21,22]) or banana (rr = of the weight loss versus temperature. One can clearly no-
529–914 MPa [23]). However, the well reported coir fiber tice the presence of two peaks at high temperatures, occur-
has tensile strength level comparable to the one found here ring at 276 and 347 °C, respectively. The peak at 347 °C
for piassava, viz. rr = 106–270 MPa [22,23]. can be associated with the decomposition of a-cellulose.
The results of the thermogravimetric analysis are shown A value of 345 °C was, indeed, found for the decomposi-
in Fig. 9. One may note that following a small low temper- tion of a-cellulose in jute fibers [24]. Both values are, how-
ature loss of weight between 75 and 85 °C, the onset of the ever, slightly higher than the one listed in Table 2 for a pure
fiber thermal degradation does not occur until 225 °C. The a-cellulose sample [25]. The peak at 276 °C could be asso-
low temperature weight loss of 5.18% can be attributed to ciated to the decomposition of hemicellulose. Values rang-
water in the form of absorbed moisture or combined water. ing from 260 [26] to 281 °C [27] are found in the literature.
Similar results for this low temperature loss of weight were A clear peak for lignin was not observed, but this can be
obtained for other lignocellulosic fibers like luffa, 5% [10], attributed to the upper limit temperature of the test appa-
jute, with a fairly higher value of 10.2% [24], flax (6.3%) ratus used, that reaches only 400 °C. Values of 375 °C or
and wheat straw (7.3%), as well as for a-cellulose (7.6%) higher are reported for degradation temperature of lignin
and lignin, 5.8% [25]. The temperature determined for the [26,28], and acid treated lignin, as investigated in this work,
onset of thermal degradation of piassava fibers also agrees are expected to have higher degradation temperatures due
with the values reported on the literature for other lignocel- to condensation [26].
lulosic fibers and materials. Table 2 compares these data. The X-ray diffraction spectrum for piassava is shown in
Fig. 10. The result obtained is very similar to those of other
lignocellulosic fibers, like sisal [29], and reflects the crystal-
line lattice of cellulose I [29].
The chemical composition of piassava fibers is shown in
Table 3, where the composition of the most commonly
used lignocellulosic fibers are also listed for comparison.
The results obtained revealed that piassava has a higher lig-
nin content than any of the other common lignocellulosic
fibers. This could be responsible for its inherent flexural
rigidity and water proof resistance. The figures here re-
ported, however, agree very well with previously reported
data for piassava fibers [30,31]. One can note from Table
3, and from the previously listed data of the mechanical
properties, that piassava has many similarities with coir
fiber.

Fig. 9. TGA curves: (a) weight loss vs. temperature; (b) derivative of the
weight loss vs. temperature.

Table 2
Temperature of the onset of lignocellulosic fibers degradation TGA
Fiber Temperature (°C)
Piassaba 225
Sisal [9] 302
Luffa [10] 250
Sabai [16] 244
Jute [24] 282
Wheat straw [25] 283
Flax [25] 330
a-cellulose [25] 322
Fig. 10. X-ray spectrum. The peak at 24.7° corresponds signs the presence
Lignin [25] 213
of cellulose I.
1478 J.R.M. d’Almeida et al. / Composites: Part A 37 (2006) 1473–1479

Table 3 composite materials. With this regard, it is interesting to


Chemical composition, in wt%, of piassava and other lignocellulosic fibers note that coir fibers have also a regular array of structural
Fiber Lignin (%) Cellulose (%) Hemicellulose (%) features at their surface.
Piassava 48.4 31.6 – The chemical analysis performed showed that piassava
Jute [21] 13.0 61.0 20.4 is a lignin rich fiber, showing again similarities with lignin
Sisal [21] 8.0 78.0 10.0 rich coir fibers. Their thermal degradation behavior dis-
Coir [21] 45.0 43.0 0.3
Flax [21] 2.2 71.0 18.6
played many similarities with the thermal behavior of pure
Hemp [21] 3.7 74.4 17.9 lignin. X-ray analysis revealed that cellulose I is the main
crystalline constituent of piassava fibers.
The strong similarities between piassava and coir are a
promising sign that todays relatively large amount of pias-
5. A note on piassava–polyester composites sava leftover can be used as an effective reinforcement for
resin matrix composite materials.
Since the mechanical properties obtained place piassava
on the group of low strength–low modulus lignocellulosic Acknowledgments
fibers, one has to ask if they are worth for being used as
reinforcement. Preliminary results on unidirectional pias- The authors thank the Brazilian Agencies CNPq and
sava–polyester composites show that, in fact, piassava pro- FENORTE for their support.
duces an outstanding reinforcement effect. For composites
with mass fraction of fibers ranging from 0.30 to 0.50, Appendix A. Correction of the elastic contribution of the test
tested in three-point bending at a crosshead speed of machine
1 mm/min, values of up to 42 MPa were obtained for the
stress at rupture [11]. This is a very promising result, be- The elastic deformation of the grips and frame from the
cause it is comparable to the flexural data from other ligno- test apparatus can result on misleading data when fibers are
cellulosic reinforced composites, such as jute–polystyrene tested. Mechanical or electrical extensometers cannot be
(r = 45–55 MPa) [32], coir–polyester (r = 29–41 MPa) used for these slender specimens. Therefore, a correction
[17], straw–polyester (r = 34–56 MPa) [33] or banana– has to be made, otherwise one can find a dependence of
polyester (r = 28–97 MPa) [34]. the YoungÕs modulus, E, with the gage length of the tested
It is worth mentioning that the value obtained, i.e., specimen. The correction here used was earlier described by
42 MPa, for the stress at rupture of the piassava-polyester Guimarães and Chawla [37].
composites is also comparable to the values shown by com- The stiffness, ks, of the system formed by the test speci-
mercial wood based materials and bagasse boards that are men and the test machine is given by:
largely used as furniture. For example, the stress at rupture 1=k s ¼ 1=k m þ 1=E  L0 =A0 ; ðA:1Þ
of plywood typically ranges from 15 to 21 MPa [35], and
that of low density particle board from 5 to 10 MPa [36]. where km is the stiffness of the test machine and E, L0 and
Moreover, it can also be emphasized that the low cost of A0 are, respectively, the YoungÕs modulus, the gage length
piassaba fibers associated with their large diameter, which and the cross-section of the test specimen. The value of ks is
can facilitate handling, are valuable characteristics of these obtained from the linear portion of the load times elonga-
fibers. tion curve and, thus, is directly related to the uncorrected
One can also expect that chemical treatments could im- YoungÕs modulus. Namely, ks = P/D‘ where P and D‘
prove the stress transfer at the fiber/matrix interface. are elements of a coordinate pair on the linear part of the
Therefore, composites are now being prepared with surface load–deflection curve. The plot of this value against L0/
treated fibers and their tensile and flexural behavior will be A0, when varying the gage length of the test specimens
presented in a future work. while maintaining a constant cross-section, will permit
one to obtain E and km. For cellulosic fibers, as shown in
6. Conclusions Fig. 1, the cross-section also varies. Therefore, each fiber
had its mean cross-section measured by a micrometer along
An investigation on the mechanical properties, surface its length, in order to minimize errors. At least five mea-
morphology, chemical composition and crystalline charac- sures were made per fiber.
ter of piassava (A. funifera) fibers was presented. The re- The correctness of this approach can be established by
sults of the tensile mechanical tests showed that piassava the adherence of the experimental points to a straight line.
fibers have lower stress at rupture and lower YoungÕs mod- Fig. A1 shows the plot obtained using the above method.
ulus than the more common jute or sisal fibers, but their The coefficient of correlation obtained was 0.973. The val-
mechanical properties are comparable to that of coir fibers. ues obtained for km and E were:
The fibers present a regular array of silicon rich star-like
protrusions, which could help their mechanical interlock k m ¼ 82 kN=m;
with resins when used as reinforcements in resin matrix E ¼ 6:2 GPa.
J.R.M. d’Almeida et al. / Composites: Part A 37 (2006) 1473–1479 1479

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