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Comparative study of pineapple leaf microfiber and aramid fiber reinforced natural
rubbers using dynamic mechanical analysis
PII: S0142-9418(19)31896-3
DOI: https://doi.org/10.1016/j.polymertesting.2019.106289
Reference: POTE 106289
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* Corresponding author
Email: taweechai.amo@mahidol.edu
1
Abstract
polymer matrix composites. However, some natural fibers have relatively high mechanical
properties with modulus close to that of high-performance synthetic fibers. Since the
reinforcing efficiency of a short fiber is determined not only by the fiber modulus, but also by
other physical properties such as the length to diameter ratio. Here it is shown, for the first
time, that pineapple leaf fiber, whose modulus is somewhat lower than that of aramid fiber,
can be used to reinforce natural rubber more effectively than aramid fiber. The situation was
achieved by breaking down the fiber bundles into the constituent microfibers to gain very
high aspect ratio. Comparisons were made at fiber contents of 2, 5 and 10 parts (by weight)
per hundred of rubber (phr) using dynamic mechanical analysis over a range of temperature.
The results reveals that at temperature below the glass transition of the matrix rubber and low
fiber contents of 2 and 5 phrs, aramid fiber displays slightly better reinforcement efficiency.
At high temperatures of 25 and 60 °C and high fiber content of 10 phr, pineapple leaf
microfiber clearly displays higher reinforcement efficiency than does aramid fiber. Surface
efficiency.
Keywords: fiber reinforced rubber; natural rubber composites; pineapple leaf fiber; adhesion
2
1. Introduction
A great deal of attention has been paid to the use of natural fibers as reinforcement for
polymer matrix composites. Natural fiber reinforced plastics are studied much more than are
rubbers and have reached commercial production, see for example [1]. The major problem
with high extensibility of rubbers is that failure is more sensitive to the size of the filler
incorporated [2,3]. There have been several attempts to use natural fibers to reinforce rubbers
[4 - 13]. We have shown that pineapple leaf fiber (PALF), whose size is relatively small
compared to other natural fibers, can be used to reinforce rubber effectively [14]. However,
the composites fail at rather low elongation at break. Only when PALF is combined with an
appropriate hybrid particulate filler can the elongation at break of the composite be extended
remarkably [15,16]. In addition, the stress-strain curves of PALF- reinforced rubbers can be
manipulated by way of different techniques such as an increase in the rubber mastication time
[17], controlling the distribution of hybrid particulate filler [18], adjusting the degree of
crosslinking [19] or adding polar rubber [20]. Despite the different approaches that have
been tried, all the composites display failure with fiber pull-out. So there is still some room
for improvement. Rubber reinforced with aramid fiber has been studied as its properties can
be used as a benchmark [21]. Such composites show excellent mechanical properties without
any sign of fiber pull-out. For reinforcement with only aramid fiber, the rubber composites
break at relatively low elongations. It has been confirmed that only with a combination of
hybrid particulate filler do the aramid fiber reinforced rubber composites have high
elongation at break. So, with present knowledge, PALF cannot compete with aramid fiber as
reinforcing agent in rubber composites. This is especially the case when comparison is made
over large strains or deformations when good interfacial adhesion is required. In order to
evaluate the true potential of PALF itself, it is important to compare the composite properties
at very low strains when interfacial adhesion and stress transfer are still effective.
3
According to the short fiber reinforced composite model, the composite modulus is
determined by both the fiber’s modulus and its aspect ratio. For PALF, it is possible to
prepare the fiber so as to have a very high aspect ratio and this could, in effect, compensate
The objective of this paper is to compare the reinforcing efficiency of aramid and
PALF in rubber matrix composites at very low strain over a temperature range using a
elementary fibers that can be easily separated using sodium hydroxide solution [22]. So far
PALF reinforced rubbers show lower moduli than do aramid fiber reinforced rubbers (cf. [16]
and [21]). To get the best effect of PALF, the fiber bundles need to be separated into their
elementary micron size form while keeping their length the same. This will be called
pineapple leaf microfiber (PALMF). The effect of was compared at fiber loadings of 2, 5 and
10 In addition, surface treatment of the PALMF with silane was carried out in order to
2. Experimental
2.1 Materials
Natural rubber (NR) was STR5L grade and was purchased from M.B.J. Enterprise
Co., Ltd. (Bangkok, Thailand). The curing additives, i.e., zinc oxide (ZnO), stearic acid,
aramid fiber was Kevlar® (DuPont, USA), supplied by Polymer Innovation Co., Ltd.
(Bangkok, Thailand). It was supplied in the form of a masterbatch in rubber with a fiber
4
Sigma-Aldrich. Sodium hydroxide (NaOH) was purchased from Alfa Aesar. Toluene and
Pineapple leaf fiber (PALF) was obtained from Bang Yang District, Phitsanulok
Province, Thailand. The process for separating pineapple leaf fiber followed the method
proposed by Kengkhetkit and Amornsakchai [23]. PALF was treated with 10% w/v NaOH
solution for 30 min. Then, it was stirred using a homogenizer for 30 min. The fiber was
washed with distill water until the pH became 7. This fiber was called pineapple leaf
microfiber (PALMF)
PALMF. A predetermined amount of silane-69 (3% wt. of fiber) was dissolved in absolute
ethanol (analytical grade) and stirred for 1 hour. Then PALMF was added into the silane
solution keeping the ratio of fiber and the solution at 1 g to 40 ml. The fiber was left in the
silane-69 solution for 72 hr. After that the solvent was removed by drying in a hot air oven at
The masterbatch of PALMF-NR was prepared at 30% of fiber using a small scale
two-roll mill. First NR was masticated for 16 minutes. Then, PALMF was slowly added and
mixing continued for 12 minutes. Finally, it was taken from the mill.
5
2.3 Composite preparation
Compounds were prepared using a small scale two-roll mill. Rotor speed and nip gap
were kept the same for all formulations at 50 rpm and 0.25 mm, respectively. The sequence
of mixing is shown in Table 1. The Kevlar and pineapple leaf fiber in masterbatch forms
2.4 Characterization
The pineapple leaf fiber surface was analyzed with a VG Scienta SES2002
hemispherical analyzer and an electron gun to compensate the charging effect. The high-
resolution spectra and wide scan were recorded with pass energis of 100 eV and 500 eV,
respectively. The analyzed zone had a surface of 24 mm2. The decomposition of the spectra
into different components was performed with Gaussian-Lorentzian line shape, after having
expressed in atomic percentages was determined using integrated peak areas of each
component taking into account the transmission factor of the spectrometer, the mean free
path, and the sensitivity factors of each atom. Wide-scan and high resolution scan were used.
The sample was measured under high vacuum. The x-rays can penetrate the surface of
The specimens were cut into 30 x 10 x 1 mm3. Experiments were performed with fixed
gauge length of 20 mm. First, the specimen was set up in the closed chamber with controlled
6
temperature. The condition was 1% pre-strained, 0.5% dynamic strain, and 10 Hz frequency.
The sample was measured in tension mode. The temperature was decreased from room
temperature to -90°C with liquid nitrogen at the scan rate 10°C/min. The specimen was held
at -90°C for 15 min. Then, the temperature was increased from -90°C to 100°C at the rate of
2°C/min.
Morphologies of fiber and rubber composites were observed with FEI Quanta 400
scanning electron microscope at different magnifications. Samples were stuck to carbon tape
3. Results
3.1 PALMF
PALF was defibrillated and transformed into pineapple leaf microfiber (PALMF) as
described above. The size, shape and the surface of PALMF are shown in Figure 2.
Silanization was used to modify the PALMF surface in order to promote the
interfacial adhesion with the NR matrix. XPS was used to confirm the presence of silane-69
on the PALMF surface. Figure 3 displays wide scan and high-resolution spectra of the
controlled PALMF and Si69 treated PALMF (Si69PALMF). The spectra show the presence
of sulfur and silicon atoms on the surface and their contents are 2.42 and 2.57, respectively.
The analysis of XPS spectra of Si69PALMF for the C1s peak indicates the amount of C-C
increases from 26.43% to 47.39%, while that of C-OR and O-C-O decrease from 33.58% to
20.5% and 6.72% to 2.84%, respectively (Table 2). The O/C ratio for Si69PALMF decreases
7
from 0.50 to 0.27. These results indicate that silane-69 was successfully grafted onto the
surface of PALMF.
microfiber and Kevlar were determined at very low strain. Figure 4 shows the storage
modulus and tan delta over a range of temperature of the composites. At low temperatures all
composites exhibit high storage modulus and the effects of fiber and fiber content are
relatively small. As the temperature is increased, the modulus remains roughly constant until
about -50 °C when the modulus drops significantly. It is in this region that the effect of both
fibers in improving modulus is more obvious and the effect becomes greater with increased
fiber loading. As temperature is increased further, the modulus remains almost constant
again. Tan delta of the composites shows a broad peak at a temperature of about -44 °C and
the magnitude of tan delta at the peak decreases in line with increasing fiber loading.
However, the difference in the effect of Kevlar and PALMF is difficult to observe in these
graphs. In order to illustrate the difference, the moduli and tan delta values of the composites
at specific temperatures were extracted and are shown in Figure 5. At temperature lower than
the glass transition temperature (Tg), -75 °C, storage moduli of composites with low fiber
content of 2 phr are very similar. As fiber content increases, it becomes apparent that Kevlar
fiber has a slightly greater effect than does PALMF. As the temperature is increased to 25 °C
and 60 °C, the effect of both fibers remains similar at low fiber contents. Only at a fiber
content of 10 phr does PALMF demonstrate a much greater effect that does Kevlar. Also, the
tan delta peaks of the PALMF composites display correspondingly lower values.
8
3.4 Fracture surfaces
Figure 6 displays the cryogenic fracture surfaces of the composites in the plane
perpendicular to the fiber orientation direction. The spotty images clearly indicate uniaxial
orientation and also good dispersion of the fiber. High resolution images also indicate good
4. Discussion
Pineapple leaf microfiber (PALMF) was prepared from PALF by alkali treatment and
mechanical force. Generally, alkali solution removes cementing material that holds
elementary microfibers together to form bundle. So the treatment carried out here provides
two simultaneous effects, i.e, breaking down bundles and cleaning the fiber surfaces for
effective later silanization [24]. The PALMF shows a smooth surface similar to that of alkali
treated PALF [22]. However, the cementing material cannot be completely removed as seen
from the XPS results in Figure 3. The C/O ratio of the PALMF surface is 0.50. This is closer
to the C/O ratio of lignin at 0.33 [25, 26] than that of cellulose at 0.83. Although lignin can
be completely removed, this would significantly weaken the microfiber [26, 27]. Despite the
remaining materials on the fiber surface, some grafting of silane is confirmed using XPS.
This layer is very thin and could not be observed with using SEM. That is similar to what is
All fibers are well dispersed in the matrix rubber as seen in the SEM images in Figure
6. The images also show that the fiber can be uniaxially oriented to a very high degree by
The objective of the research was to compare the mechanical properties of the natural
and synthetic filler composites. At low fiber content, aramid fiber performs slightly better
than PALMFs in reinforcing rubbers. As the fiber content is increased to 10 phr, both types
9
of PALMFs overtake aramid fiber in their reinforcing effect. This clearly demonstrates the
This fact raises the question as to how it could occur given that PALMF has a lower
modulus than does aramid fiber. The modulus of an uniaxial short fiber composite can be
calculated from different models. A useful one is the shear lag model originally proposed by
= + 1− (1)
/
= 1 −
/
(2)
= $
(3)
! "# '
%&
matrix, is shear lag factor or modulus adjustment variable for short fiber, is a constant
value that depends on shape and orientation of fiber. It is assumed that the composite has
Although there are a few fiber composite models that differ in detail, all depend on
the modulus of the reinforcing fiber and its aspect ratio. The latter contributes to the term ηl
and the higher the aspect ratio the closer it gets to unity. Thus, for reinforcing fiber with
Aramid fiber can have a modulus from about 64 GPa for as-spun fiber and above that
for different heat-treated grades. That of PALF has been reported to be 34.5-82.5 GPa [13].
We have found that, for the variety of pineapple used in this study, when in the form of
bundle it has a modulus of about 50 GPa [22]. It is likely that PALMF in its elementary fiber
form would have a greater modulus, The PALMF used in this work is 6 mm long and its
10
diameter is around 3 µm, giving it a very high aspect ratio of 2000. Aramid fiber, according
to product specification, is only 1-2 mm long and about 10 µm in diameter yielding an aspect
ratio in the range of 100-200. However, fiber breakage did occur during the mixing and the
size of the fiber can be determined by considering the toluene extracted fibers from the two
mixtures. The images of fibers extracted from uncured rubber compounds are shown in
Figure 7 and it is still confirmed that PALF is longer than aramid fiber. Such a large
difference in aspect ratio could cause the ηl to increase from 0.22 for aramid fiber to 0.74 for
PALMF. This is more than 70.5 % increase. It is in this way that PALMFs show a greater
effect on the rubber composite modulus than does the aramid fiber.
very low temperatures, when the matrix is glassy and its modulus is closer to the reinforcing
fiber, the modulus of all composites are very close to each other being less than 5% apart. As
the temperature increases, the matrix becomes softer and rubbery and matrix deformation
makes a significant contribution to the total deformation of the composite. Stress transfer
from matrix to the reinforcing fiber occurs through better friction and traction at the interface.
In this state of large matrix deformation and high traction, the advantage of very high aspect
There are also other contributing factors. Generally, mechanical modelling starts with
a representative elementary cell and properties derived from that single isolated cell. It has
been shown that, by using finite element method, the way these isolated cells pack or arrange
together affects the modulus of the composite. Hexagonal arrangement of the cells with a
regular overlapping of fiber ends will provide a higher modulus than does the arrangement
without overlapping [30]. The difference becomes greater with increasing fiber volume
fraction. So PALMF, with an aspect ratio much greater than aramid will have more overlap
11
Treatment of PALMF with silane-69 improves not only the adhesion between fiber
and NR matrix, but also the filler dispersion. It does this by reducing the polarity difference
between the reinforcing fiber and the matrix rubber. The silane-69 treatment of the fiber
allows the formation of chemical bonds bridging the fiber surface with the rubber [31], thus
improving the interfacial adhesion. As a result, the overall modulus of so treatd composite is
greater than that of unmodified PALMF-NR composites. Such an effect of silane treated
5. Conclusions
Silane-69 can be successfully grafted onto the surface of PALMF. Both untreated
PALMF and silane-69 treated fiber exhibit reinforcing efficiency comparable to that of
Kevlar fiber. Silane treatment yields fibers with a slight improvement over the untreated
counterparts. At high fiber content, both types of PALMF exhibit greater reinforcing
efficiency than does Kevlar fiber. The reinforcing mechanism in short fiber reinforced rubber
composites is different at low and high fiber contents. At low fiber content the modulus of
the reinforcing fiber dominates. At high fiber content the fiber aspect ratio becomes more
important. So naturally sourced PALMF has very high potential as a high performance
Acknowledgements
The authors gratefully acknowledge partial financial support of the project by the
12
Data Availability
The raw/processed data required to reproduce these findings are available upon
request.
References
13
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16
Table Captions
Table 2 Surface elements, chemical state and atomic content from XPS analysis of
PALMFs.
17
Table 1 Sequence of NR reinforced with aramid fiber mixing
1 NR 0-2
microfiber
Total time 14
18
Table 2 Surface elements, chemical state and atomic content from XPS analysis of
PALMFs.
19
Figure Captions
Figure 1 Steps in preparations of pineapple leaf microfiber (a) and rubber composites to
Figure 2 SEM micrograph of PALMF (a and b) and Si69-PALMF (c and d) at low and high
magnification.
Figure 3 XPS wide scan and high resolution spectra of C1s of PALMF (top) and silanized
PALMF (bottom).
Figure 4 Elastic moduli (Eꞌ) and tan δ of natural rubber and its composites containing
Figure 5 Elastic moduli of natural rubber and its composites containing different amounts
distribution at low and high magnification. Aramid fiber(a and d), PALMF (b and
Figure 7 PALF (left) and aramid fiber (right) extracted from their respective uncured rubber
compounds.
1
(a)
(b)
Figure 1 Steps in preparations of pineapple leaf microfiber (a) and rubber composites to
2
(a) (b)
200.0 µm 20.0 µm
(c) (d)
200.0 µm 20.0 µm
Figure 2 SEM micrograph of PALMF (a and b) and Si69-PALMF (c and d) at low and high
magnification.
3
14000
PALMF O1s Wide scan PALMF
12000
C-OR
10000
C-C, C-H
Intensity
Intensity
8000
C1s
6000
4000 C=O
2000
0
1000 800 600 400 200 0 292 290 288 286 284 282 280
0
6.0x10
Si69PALMF Si69PALMF
C1s
O1s Wide scan
C-C, C-H
0
4.0x10
Intensity
Intensity
0
2.0x10
C-OR
S2p
Si2s C2
S2s Si2p C-Si C-S
0.0
1000 800 600 400 200 0 292 290 288 286 284 282 280
Figure 3 XPS wide scan and high resolution spectra of C1s of PALMF (top) and silanized
PALMF (bottom).
4
11
10 5.0
NR
4.5
10 K2NR
10 4.0 PALMF2
3.5 Si69PALMF2
9
10
3.0
Tan delta
E' (Pa)
8
10 2.5
2.0
7
10 1.5
6 1.0
10
0.5
5
10 0.0
-50 0 50 -50 0 50
11 5.0
10
NR
4.5
10 K5NR
10 4.0 PALMF5
3.5 Si69PALMF5
9
10
3.0
Tan delta
E' (Pa)
8 2.5
10
2.0
7
10 1.5
6 1.0
10
0.5
5 0.0
10
-50 0 50 -50 0 50
11
10 5.0
NR
4.5
10 K10NR
10 4.0 PALMF10
9 3.5 Si69PALMF10
10
3.0
Tan delta
E' (Pa)
8
10 2.5
2.0
7
10
1.5
6 1.0
10
0.5
5
10 0.0
-50 0 50 -50 0 50
Temperature (°C) Temperature (°C)
Figure 4 Elastic moduli (Eꞌ) and tan δ of natural rubber and its composites containing
5
6000
NR -75 οC
K
5000 PALMF
Si69PALMF
4000
E' (MPa)
3000
2000
1000
0
0 2 5 10
40
25 οC
30
E' (MPa)
20
10
0
0 2 5 10
30
60 οC
20
E' (MPa)
10
0
0 2 5 10
Fiber content (phr)
Figure 5 Elastic moduli of natural rubber and its composites containing different amounts
6
(a) (b) (c)
distribution at low and high magnification. Aramid fiber(a and d), PALMF (b and
7
1 mm 1 mm
Figure 7 PALF (left) and aramid fiber (right) extracted from their respective uncured rubber
compounds.
8
Highlights
• Reinforcement efficiency of short pineapple leaf microfiler and aramid fiber in natural
• At low fiber content of 2 phr, aramid fiber provides slightly higher reinforcing effect
☒ The authors declare that they have no known competing financial interests or personal relationships
that could have appeared to influence the work reported in this paper.
☐The authors declare the following financial interests/personal relationships which may be considered
as potential competing interests: