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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
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
production, ton.
behavior, such as the onset of thermal degradation, must 60000
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.
160 2
140
1
120
0 20 40 60 80 100 120 140 160
100 gage length, mm
srtessM,Pa
40
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
0.045 [15] Mattoso LHC, Ferreira FC, Curvelo AAS. Sisal fiber: morphology
and applications in polymer composites. In: Leão AL, Carvalho FX,
Frollini E, editors. Lignocellulosic–plastics composites. Botucatu,
0.040
Brazil: Unesp Publishers; 1997. p. 241.
[16] Chand N, Rohatgi PK. Potential use, mechanical properties and
0.035 thermal studies of sabai grass fibre. J Mater Sci Lett 1992;11:578–80.
[17] Prasad SV, Pavithram C, Rohatgi PK. Alkali treatment of coir fibres
1 / ks ,mm/N