International Journal of Adhesion & Adhesives 106 (2021) 102823

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International Journal of Adhesion and Adhesives

journal homepage: http://www.elsevier.com/locate/ijadhadh

Compressive, dynamic and thermo-mechanical properties of cellulosic

pineapple leaf fibre/polyester composites: Influence of alkali treatment
on adhesion
K. Senthilkumar a, d, N. Saba b, M. Chandrasekar c, M. Jawaid b, *, N. Rajini a, e, **,
Suchart Siengchin d, Nadir Ayrilmis e, Faruq Mohammad f, Hamad A. Al-Lohedan f
a
Centre for Composite Materials, Department of Mechanical Engineering, Kalasalingam Academy of Research and Education, Krishnankoil, 626126, Tamilnadu, India
b
Laboratory of Biocomposite Technology, Institute of Tropical Forestry and Forest Products (INTROP), Universiti Putra Malaysia, 43400, UPM, Serdang, Selangor,
Malaysia
c
School of Aeronautical Sciences, Hindustan Institute of Technology & Science, Padur, Kelambakkam, Chennai, 603103, Tamilnadu, India
d
Department of Materials and Production Engineering, The Sirindhorn International Thai-German Graduate School of Engineering (TGGS), King Mongkut’s University of
Technology North Bangkok, Bangkok, 10800, Thailand
e
Department of Wood Mechanics and Technology, Faculty of Forestry, Istanbul University-Cerrahpasa, Bahcekoy, Sariyer, 34473, Istanbul, Turkey
f
Surfactants Research Chair, Department of Chemistry, College of Science, King Saud University, P.O. Box 2455, 11451, Riyadh, Saudi Arabia

A R T I C L E I N F O A B S T R A C T

Keywords: This study presents the influence of fibre treatment and fibre loading on the mechanical, physical, crystalline,
Alkali treatment and thermal properties of pineapple leaf fibre (PALF) reinforced polyester (PE) composites. Fibre treatment with
Fibre composites NaOH modified the fibre surface from smooth to rough and KOH treatment induced fibrillation, as evident from
Compression strength
micrographs of the elementary fibres. Fibre surface modification with NaOH helped in improving the fibre-
Natural frequency
Coefficient of thermal expansion
matrix adhesion while it resulted in inferior damping characteristics for the composite. Composites with the
KOH treated fibres were found to have superior damping characteristics and poor fibre-matrix adhesion. The
compressive strength of composites produced with treated fibres was lower than the composite with untreated
fibre and could only be improved with the addition of more fibres. Maximum compressive strength was observed
for NaOH and KOH PALF/PE composites with 45 wt% fibre loading. Thermo-mechanical analysis indicated that
PALF/PE composite with 45 wt% fibre loading displayed the least dimensional change indicating better
dimensional stability. Superior vibration damping, dynamic mechanical and thermomechanical characteristics of
the treated PALF/PE make them a promising candidate for applications requiring vibration damping charac­
teristics and dimensional stability.

1. Introduction
This century has seen exceptional developments in the field of green
composites owing to concerns about the environment and sustainability
issues [1]. Disposal of synthetic fibre reinforced composites creates
landfill, and technological limitations in recycling methodologies have
emphasized the importance of environment-friendly materials [2]. Ef­
forts have been taken by researchers to produce bio-composites either by
partially substituting or entirely replacing synthetic fibres with natural
fibres as reinforcement in composites for structural applications. The
main features of natural fibres are (i) lightweight (ii) abundance (iii) low
cost (iv) high specific strength and modulus (v) low energy consumption
and (vi) biodegradability [3,4]. Compared to other natural fibres,
pineapple leaf fibre (PALF) has a higher cellulose content, a low
microfibrillar angle (14◦ ) [5] and superior mechanical and thermal
properties [6–8]. PALF is extracted from Ananuscosomus plant leaves
belonging to the Bromeliaceae family through the retting process.
Many researchers have used natural fibres as reinforcements in
polymer matrices and have studied their mechanical, thermal and free
vibration properties [9–11]. Fartini et al. [12] reported that the elastic
modulus and compression strength of a napier/polyester composite
improved by increasing the napier fibre content. Efficient stress transfer

* Corresponding author. UPM, Serdang, Selangor, Malaysia.

** Corresponding author. Krishnankoil, India.
E-mail addresses: jawaid@upm.edu.my (M. Jawaid), rajiniklu@gmail.com (N. Rajini).

https://doi.org/10.1016/j.ijadhadh.2021.102823

Available online 9 February 2021

0143-7496/© 2021 Elsevier Ltd. All rights reserved.
K. Senthilkumar et al. International Journal of Adhesion and Adhesives 106 (2021) 102823

Table 1
Mechanical, physical and chemical composition of pineapple fibre [43].
Mechanical Properties Physical Properties Chemical composition

Tensile strength Elongation at Young’s modulus Diameter Density (g/ Cellulose Hemicellulose Lignin Pectin Ash Fat & wax
(MPa) break (%) (MPa) μm cm3) (%) content (%) (%) Wt. (%)
(%)

170 3 6210 20–80 1.526 70–82 18.8 5–12 1.1 1.1 3.2

via the interface was responsible for the improvement in compressive

Table 2
properties. A similar trend was reported by Senthilkumar et al. on the
Properties of PE resin.
compressive properties of PALF/PE composites [13]. Singha and Thakur
[14] reported optimum mechanical properties for Test Test value Unit
saccaharumcilliare/resorcinol-formaldehyde composites at 30 wt% Appearance Pale yellowish clear Nil
fibre loading. Ramanaiah et al. [15] fabricated typha angustifolia fibre liquid
Viscosity at 25 C (Brookfield 510 cP
reinforced polyester composites by varying the fibre content from 18.3
◦

Viscometer LV DV II + Pro Spindle 62, rpm

wt% - 35.5 wt%. Their results indicated that mechanical properties
improved with certain fibre loading. However, higher fibre loading was
detrimental to the thermal conductivity of the composite. In their study,
dharbai fibre/polyester composites were found to have better strength
and modulus at 25 wt% fibre loading and a fibre length of 30 mm [16].
The major drawback of using natural fibre as reinforcement in a
composite is the relatively weak bonding between the hydrophilic fibre
and the hydrophobic polymer matrix [17]. This incompatibility leads to
inefficient fibre/matrix bonding resulting in a reduced strength/modu­
lus. Earlier studies [17–21] have revealed that NaOH and KOH fibre
treatments have successfully enhanced the mechanical, physical, and
thermal properties of natural fibre reinforced composites. NaOH and
KOH fibre treatments are effective in modifying the fibre surface; hence,
NaOH and KOH have been chosen in this study.
Once the fibre is immersed in an aqueous alkali solution containing
NaOH or KOH, fibre constituents such as hemicellulose, lignin, pectin
and surface impurities, etc. get removed from the fibre surface [22].
Removal of these constituents from the fibre leads to a rougher fibre
surface and fibrillation, which enables better mechanical interlocking
with the matrix. The reaction between the fibre and alkali solution,
which is responsible for the removal of fibre constituents are given
below in equation (1) and equation (2) [23].
Fibre – OH + NaOH → Fibre – O– Na+ + H2O
Fibre – OH + KOH → Fibre – O– K + H2O +
Mishra et al. [9] noticed a considerable improvement in the tensile,
flexural and impact strength after the chemical treatments. Free vibra­
tion properties of jute/PE [24], sisal/PE [25,26], and banana/PE [27],
coconut sheath/PE [28], woven banana/jute/PE, jute/PE and bana­
na/PE [29] have been investigated by researchers. A general observa­
tion was that fibre treatment influenced free vibration characteristics
such as natural frequency and damping of the composites.
Currently, dynamic mechanical analysis is the most advanced ther­
mal technique to understand the stiffness and damping characteristics of
materials [30]. The storage modulus (E′ ), loss modulus (E”), tan delta
(damping factor), and glass transition temperature (Tg) are the essential
dynamic properties that can provide vital information about the melting
behavior of polymeric materials resulting from varying temperatures
and frequencies [31]. Asim et al. have reported that higher E′ and E′′
values can result from the use of silane treated, 50% fibre loaded kenaf
fibre composites owing to enhanced fibre/matrix adhesion [32]. In
another study, sansevieria cylindrical/polyester matrix composite was
subjected to dynamic mechanical analysis by varying the fibre length,
fibre loading and several surface treatments (alkali (10%),
benzoyl-peroxide (6%), KMnO4 (0.5%) and stearic acid (1%)) [33].
Results from the study revealed that the KMnO4 treated composites
exhibited the maximum increase in E′ and E’’. In another recent study,
Mohamed et al. [34] reported significant enhancements in E′ and E′′
with 50 wt% of date palm fibre/epoxy reinforced composites.
50)
Density at 25 ◦ C 1.106 g/cm3
Volatile content 38.6 %
Acid value 16.28 mg
KOH/
g
Gel time at 25 ◦ C 16 min
Crystalline changes due to fibre treatment have been evaluated
through the determination of crystallinity index (CI) from x-ray
diffraction spectra (XRD) [35,36]. It has been reviewed from previous
studies that reinforcement of treated fibres in composites improved the
damping factor and CI values [37–40]. Madhu et al. [41] treated pro­
sopis juliflora fibres with alkali, benzoyl peroxide, KMnO4, and stearic
acid, and these treated fibres were subjected to XRD analysis. They
found that the treated fibres showed higher CI than the untreated fibres.
Rajini et al. [39] studied the XRD patterns of untreated, NaOH, and
silane treated coconut sheath fibres and reported that the intensity
increased in the order NaOH > silane > untreated. In another study,
XRD analysis revealed that the cellulose I in abaca fibres was shifted to
cellulose II after the NaOH treatment (15 wt%). Due to the modifications
in crystal structure or lattice, differences in cellulose I and II charac­
teristics occur [42].
(1) Studies on the use of NaOH for fibre surface modification and the
mechanisms responsible for improvements in various properties of the
(2)
composites reinforced with NaOH treated fibre, has been well docu­
mented in the literature. According to the authors, the use of KOH for
PALF treatment, surface modification mechanisms of the fibre and their
influence on various properties of PALF/PE composites has not been
reported. Recently, the authors of this work published the influence of
KOH treatments on tensile, flexural, inter-laminar shear, and impact
properties of the PALF/PE at different fibre loadings. The results were
compared with those of the composites reinforced with untreated,
NaOH, and KOH treated PALF [18]. In the present study, characteriza­
tion has been further extended to compression, void content, vibration
damping, dynamic mechanical, thermo-mechanical and crystalline
properties of the NaOH and KOH treated PALF/PE at different fibre
loadings. Damping characteristics essential for applications in the
automotive component, construction industries and machine support
industries and the development of lightweight structures is assessed
from dynamic mechanical and free vibration analysis.
2. Materials and methods
2.1. Materials
• PALF was obtained from Nirmala Industries, Andhra Pradesh, India.
The specifications of PALF are tabulated in Table 1.
• Isophthalic unsaturated polyester matrix (PE) (VBR4503), catalyst
methyl-ethyl-ketone peroxide (MEKP) (VBR 1204), and accelerator

2
K. Senthilkumar et al.
Fig. 1. NaOH treatment of PALF: (a) NaOH pellets; (b) PALF added with distilled water; (c) PALF treated in NaOH solution; (d) PALF after washing with distilled
water; (e) Treated PALF after drying.
cobalt naphthenate (VBR1201) were procured from Vasivibala Resin
(P) Ltd, Tamilnadu, India. The specifications of PE are tabulated in
Table 2.
2.2. Alkali treatment
Initially, the PALF was cut to 3 mm fibre length, and the chopped
fibres were soaked in 1 N NaOH aqueous solution for 1 h [38,44], as
shown in Fig. 1. Then the treated PALF was cleaned several times and
allowed to dry at room temperature. Likewise, the fibre treatment with
KOH was carried out by immersing the untreated fibres in 1 N KOH
aqueous solution for 1 h. Then, the fibres were cleaned by dilute hy­
drochloric acid [20] to remove the remaining KOH from the fibre sur­
faces, and these fibres were left to dry at room temperature.
2.3. Fabrication of composites
In this study, PALF/PE composites were fabricated using a
compression molding machine, as reported previously [13,18]. During
fabrication, the matrix solution was prepared by mixing 100 g of iso­
phthalic unsaturated PE resin with 1.5 ml of MEKP (catalyst) and cobalt
naphthenate (accelerator). The fabrication process involved arranging
3
International Journal of Adhesion and Adhesives 106 (2021) 102823
short PALF inside the rectangular cavity of the mold followed by
pre-compression for a few minutes. Care was taken to distribute the fi­
bres uniformly within the matrix at each fibre loading as the distribution
of fibres has a profound effect on mechanical and thermal properties.
The degassed resin mixture was then poured into the pre-compressed
randomly oriented fibres, and a roller was used to remove air bubbles.
The closed mold was placed in a compression molding machine and
subjected to a pressure of 17.0 MPa (170 bar). The composites were
removed from the mold after 24 h.
2.4. Characterization
2.4.1. X-ray diffraction analysis (XRD)
Fibre crystallinity of PALF/PE composites was tested by D8
ADVANCE Eco (Bruker). The diffracted intensity of Cu Kα radiation was
recorded between 10◦ - 40◦ (2θ angle range).
2.4.2. Void content
Void contents and the experimental densities of treated and un­
treated PALF/PE composites were calculated according to ASTM 2734-
70. The density of treated fibre was measured using an electronic
densometer (resolution 0.001).
K. Senthilkumar et al. International Journal of Adhesion and Adhesives 106 (2021) 102823

Equations (3) and (4) were used to calculate the theoretical and
experimental densities of the untreated and treated PALF/PE
composites.

Td = 100/ (Rm/Dm + rf/df) (3)

Where

Td = Theoretical density of the composite (g/cm3)

Rm = Resin weight %
Dm = matrix density (g/cm3)
rf = fibre weight %
df = fibre density (g/cm3)

Void content = 100(Td -M)/Td (4)

Where, M = measured fibre density (g/cm3)

2.4.3. Compressive testing

All the fabricated PALF/PE composite samples were cut into di­
mensions of 60 × 20 × 3 mm3 as per the ASTM D3410 standard. The
Fig. 2. XRD spectra of treated and untreated PALF.
compression test was conducted at a crosshead speed of 1.27 mm/min.
Data on the stress-strain plot and compressive strength was obtained.
Five samples from each configuration were tested, and the average test Table 3
results were reported. CI of treated and untreated PALF.
PALF CI (%) I22.7/I20.4
2.4.4. Free vibration analysis
Free vibration properties of the manufactured composites were Untreated 63.1 1.37
NaOH treated 65.5 1.87
performed on a sample size of 200 × 20 × 3 mm3 [26] with a Kistler
KOH treated 66.2 2.05
display 9722A500 setup. The composite sample was equally spaced and
marked over the surface. Then the sample was excited at the marked
locations by a sharp hardened impact hammer. The Kistler type model 3. Results and discussion
8778A500 was attached at one end (i.e., free end) of the composite
laminate to receive the displacement signals. These were fed to a com­ 3.1. XRD
puter using a data acquisition (DAQ) card. Fast Fourier transform of the
time signal was acquired by DEWESoft 7.0 software in the computer. The XRD spectra obtained from the untreated and chemically treated
The natural frequency was then obtained from the peak of the frequency fibres are given in Fig. 2 to investigate the crystalline behavior of the
response function curve, and the half-power points were obtained from PALF. The lignocellulosic PALF has crystalline and amorphous regions in
3 dB below the peak curve when a logarithmic scale was used, or in the their fibre structure. The crystalline arrangements present in the PALF
case of a linear scale, the bandwidth would be the difference between were responsible for the attainment of the degree of crystallinity [45].
the frequency values cut by the horizontal line measured from the The Segal empirical method, shown in equation (6), was employed to
maximum amplitude
value below the maximum amplitude of the curve. calculate the crystallinity index (CI), and the values are tabulated in
Table 3.
√2
In this work, the damping was calculated by using the half-power
bandwidth method based on equation (5) [25]. CI (%) = ((I22.8◦ – I18◦ ) / I22.8◦ ) × 100 (6)
Δω where, I22.8◦ is the maximum intensity of the [002] lattice reflection of
ξ= (5)
2ωn the cellulose crystallographic form (I),and I18◦ is the intensity of
diffraction of the amorphous material.
where, Δω is the bandwidth and ωn is the natural or resonant frequency.
A CI value of 63.1% was recorded for the untreated PALF. The ob­
tained value lies within the range of 48.7–64.4% reported for six
2.4.5. Dynamic mechanical analysis (DMA)
different varieties of PALF [45]. Thus, it is clear that the CI of PALF
The dynamic mechanical properties of the untreated and treated
primarily varies based on the fibre variety and geographical location
PALF/PE composites were assessed with a DMA Q800 instrument (TA
[46]. On the other hand, CI was influenced by the fibre treatment with
Instruments) in accordance with ASTM D4065-01 under 3-point bending
NaOH and KOH. There was a slight increase in the CI for the chemically
mode at an oscillation frequency of 1 Hz in a nitrogen atmosphere. The
treated PALF compared to the untreated fibres. The highest CI of 66.2%
composites had a thickness of 3 mm, a width of 12.5 mm, and a length of
was recorded for the KOH treated fibres followed by the NaOH treated
60 mm. The heating rate was fixed to 5 ◦ C/min, and the temperature
fibres. The observed variation in CI due to the KOH and NaOH treatment
range was between 30 - 150 ◦ C.
is in close agreement with previous studies, which also reported a higher
degree of crystallinity and crystallite ratio for PALF due to the alkali
2.4.6. Thermo mechanical analysis (TMA)
treatment [46–50]. The intensities at 2θ = 22.7◦ and 20.4ocorrespond to
A TA Instruments Q400 thermomechanical analyser was used to
cellulose I and cellulose II, respectively, for the PALF. A higher ratio of
examine the thermal expansion behavior of the fabricated composites as
I22.7/I20.4 for the treated fibre indicates the presence of a larger pro­
per ASTM D696. Test specimens were cut to 5 mm × 5 mm of the length
portion of cellulose I than the cellulose II.
and breadth. The composite specimens were heated between 30 - 200 ◦ C
and at a ramp-up rate of 5 ◦ C/min. The coefficient of thermal expansion
(CTE) of the composite specimens in the thickness direction was 3.2. Void content
measured in the dilatometric mode.
The void content of the PALF/PE composite calculated according to

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K. Senthilkumar et al. International Journal of Adhesion and Adhesives 106 (2021) 102823

Table 4 Table 5
Void content of treated and untreated PALF/PE composites. Compressive strengths (MPa) of treated and untreated PALF/PE composites at
PALF/PE Fibre Theoretical Measured Void
different fibre loadings.
loading (wt. density (g/cm3) density (g/cm3) content PALF/PE Fibre loading (wt. %)
%) (%)
25% 35% 45%
Untreated 25 1.23 1.18 3.95
35 1.26 1.17 7.24 Untreated 14.13 ± 2.14 16.38 ± 3.83 23.54 ± 9.38
45 1.29 1.20 7.40 NaOH treated 12.33 ± 3.78 14.35 ± 0.71 17.08 ± 3.42
KOH treated 13.03 ± 0.53 13.28 ± 0.04 19.50 ± 1.62
NaOH 25 1.29 1.26 2.65
treated 35 1.32 1.19 9.92
45 1.35 1.19 11.78
the samples in the initial stages of the compression tests led to the
KOH 25 1.37 1.23 10.02
treated 35 1.39 1.23 11.27 occurrence of inflection in the stress-strain plots. Table 5 shows that the
45 1.41 1.16 17.50 compressive strength of the PALF/PE composites increased when the
fibre loading was increased regardless of whether the fibre was un­
treated or alkali-treated.
Among the different fibre loaded composites, the 45 wt% of treated
and untreated PALF/PE exhibited the highest compressive strength. This
trend reflects the typical behavior of the composites according to the
rule of mixtures. The greater number of fibres in the 45 wt% loading
enabled the composites to exhibit superior resistance to the applied
compressive load. However, the increment in strength was compara­
tively lower for the composites with treated fibres over their untreated
counterpart. The difference in compressive properties between the
composites reinforced with the untreated fibre and treated fibre is
explained through the microstructure of fractured specimens under
compression as shown in Fig. 4(a)-(i).
All the fractured composite specimens shown in Fig. 4(a)–(i) were
found to have fibre-matrix de-bonding and matrix cracks due to the
crushing of the specimens under compression. It could be noticed from
Fig. 4(d)–(f) that the extent of matrix cracks and fibre-matrix de-bonding
were minimal for the composites with NaOH treated fibres. This
observation is an indication of good compatibility between the NaOH
treated fibre and the polyester matrix. The physical changes to the
elementary fibre subjected to NaOH and KOH treatment are shown in
Fig. 5(a)-(c).
Fig. 3. Compressive stress-strain plots of treated and untreated PALF/
It can be observed from Fig. 5(b) that NaOH treatment modified the
PE composites.
surface from smooth to rough while the KOH treatment resulted in the
splitting of elementary fibres into multiple strands corresponding to the
equations (3) and (4) are listed in Table 4. The results indicate that the
fibrillation (Fig. 5(c)).These physical changes to the fibre due to the
void content was influenced by both the fibre loading and fibre
alkali treatment is supposed to promote better mechanical interlocking
treatment.
between the fibre and matrix [22]. However, PALF/PE composites with
As the fibre loading increased, with the untreated PALF/PE com­
NaOH and KOH treated fibres still displayed lower compressive strength
posites, the void content increased. The highest void content of 7.40%
in each fibre loading than their counterpart with the untreated fibre.
was observed at 45 wt% for the composite with the untreated PALF. A
According to recent studies [21,54], the compressive properties of
recent study has reported higher void contents at greater fibre loadings
composites are not only dependent on fibre-matrix interfacial adhesion
for short fibre reinforced thermoplastic composites [50]. Fibre
but are also governed by fibre strength and modulus. Fibre surface
agglomeration and difficulty in maintaining a uniform distribution of
modification with NaOH and KOH could have weakened the elementary
fibres within a thermoset matrix at larger fibre loadings were the
fibres. Hence, the treated fibres were ineffective in stress transfer within
probable factors responsible for a noticeable variation in void content.
the matrix leading to inferior compressive strength. Another factor that
Previous studies have highlighted that micro-voids usually occur due to
adds to the loss of strength in the case of the composites with treated
trapped air molecules within composites [51], improper distribution of
fibres is the agglomeration of treated fibres. Since the fibres are of
chopped fibres within the matrix [52], shrinkage of the matrix during
particulate size, some fibres remain clustered even after manual segre­
the curing process [53] and a lack of vacuum during hot press molding.
gation of the oven-dried fibres after treatment. The agglomeration of
NaOH and KOH treated fibre composites had a higher void content
treated fibres can create more fibre bundles and thick matrix regions.
than that of untreated fibre composites. This could be due to the exis­
Fibre distribution and matrix rich regions affect stress distribution while
tence of unquantifiable fibre accumulation regions and irregular distri­
the fibre agglomerated regions act as stress concentration pockets within
bution of the treated fibres within the composite. The increased void
the composite. The increasing void content with fibre loading, as shown
content at higher fibre loading due to the fibre agglomeration and their
in Table 4, further provides supportive evidence on fibre agglomeration
impact on mechanical and physical characteristics were also reported in
at higher fibre loadings.
a previous study [53].

3.3. Compression properties 3.4. Free vibration analysis

Fig. 3 shows the compressive stress-strain plots for the PALF/PE In general, the fibre reinforced composite has higher damping than
composites. The figure clearly shows a nearly linear stress-strain rela­ the conventional metal structures owing to the viscoelastic behaviour,
tionship for the samples subjected to uniaxial compression. Slippage of fibre and matrix interaction, and the natural damping characteristic

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K. Senthilkumar et al. International Journal of Adhesion and Adhesives 106 (2021) 102823

Fig. 4. Micrograph of PALF/PE composites failed under compression: (a) 25 wt% untreated; (b) 35 wt% untreated; (c) 45 wt% untreated; (d) 25 wt% NaOH treated;
(e) 35 wt% NaOH treated; (f) 45 wt% NaOH treated; (g) 25 wt% KOH treated; (h) 35 wt% KOH treated and; (i) 45 wt% KOH treated.

Fig. 5. SEM images of single fibre: (a) untreated PALF; (b) NaOH treated PALF showing rough surface and; (c) KOH treated PALF showing fibrillation.

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K. Senthilkumar et al. International Journal of Adhesion and Adhesives 106 (2021) 102823

Table 6
Natural frequency and damping of treated and untreated PALF/PE composites.
Composites Fibre loading (wt. %) Mode I Mode II Mode III

Natural frequency (Hz) Damping Natural frequency (Hz) Damping Natural frequency (Hz) Damping

Untreated 25 21.97 0.1939 175.78 0.0242 351.56 0.0121

35 26.86 0.1884 119.63 0.0431 195.31 0.0255
45 31.74 0.1324 195.31 0.0215 383.90 0.0109

NaOH treated 25 21.97 0.0768 56.15 0.0300 114.75 0.0147

35 21.97 0.1783 80.54 0.0486 161.13 0.0243
45 21.97 0.3349 61.04 0.1241 126.95 0.0596

KOH treated 25 19.53 0.2816 39.06 0.1408 136.72 0.0402

35 19.53 0.3064 65.92 0.0907 144.04 0.0415
45 17.09 0.3399 161.13 0.0314 139.36 0.0306

during the damage [40]. Bio-composites have intrinsic damping prop­

Fig. 6. E’of treated and untreated PALF/PE composites.
erties compared to synthetic fibre composites due to their lignocellulosic
content [55]. It is because of this nature, they have found applications in
automobile structures such as interior (door panels, insulation, seat
coverings, trunk panel, seat base rest, glove box) and exterior parts
(floor panels). However, the design of new material with improved vi­
bration and damping characteristics for a structural application is a
continuous process. From Table 6, it could be observed that PALF/PE
composites with the raw fibres exhibited maximum natural frequency in
all modes at 45 wt%. Composites with the NaOH treated fibres displayed
no changes in Mode I frequency with the fibre loading. For Mode II and
Mode III, a slight increase in magnitude was observed at 35 wt%
compared to the other fibre loadings. For KOH treated PALF/PE com­
posites, each Mode followed a different trend, unlike the NaOH treated
composites. This observation on the lower natural frequency of NaOH
and KOH treated PALF/PE composites was consistent with the lower
natural frequency observed for the treated coconut sheath/banana
fibre/polyester [37] and coconut sheath/nano-clay/polyester compos­
ites [39].
On the other hand, damping showed an increasing trend and higher
values (Mode I) for KOH treated fibre composites than the untreated and
NaOH treated fibre composites. Among the different fibre loaded

Fig. 7. E’’of treated and untreated PALF/PE composites.

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K. Senthilkumar et al. International Journal of Adhesion and Adhesives 106 (2021) 102823

Fig. 8. Tan delta of treated and untreated PALF/PE composites.

Fig. 9. Cole-Cole plots of treated and untreated PALF/PE composites.

composites, the 45 wt% of treated composites exhibited the highest
damping values. Thus, the damping behavior can be tailored with
respect to (i) fibre loading (ii) constituent properties and (iii) the level of
fibre-matrix interfacial bonding.
KOH treated PALF/PE composites were found to have superior
damping characteristics than the NaOH treated and untreated PALF/PE
composites. This behavior for the KOH treated PALF/PE composite was
ascribed to reduced wettability between the fibre and matrix.
3.5. Dynamic mechanical properties
Figs. 6–9 illustrate the storage modulus (E′ ), loss modulus (E′′ ), tan
delta, and Cole-Cole plots of the PALF/PE composites respectively, as a
function of temperature. The initial observation showed that both the
fibre surface modification and fibre loading influenced the E′ , E′′ and tan
delta of the composites.
The E′ values, obtained from DMA gives a measure of the stiffness of

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K. Senthilkumar et al. International Journal of Adhesion and Adhesives 106 (2021) 102823

Table 7 from the fibre to the matrix, with an increase in fibre loading. Alkali
Variation of E’ of PALF/PE composites with fibre loading at different treated PALF/PE composite displayed comparatively higher E’ relative
temperatures. to untreated fibre composites. Similar results were observed by Indira
PALF/PE Storage modulus (MPa) et al. [59] on a banana fibre/phenol formaldehyde matrix.
50 ◦ C 100 ◦ C 150 ◦ C
E′′ represents the viscous response or damping properties of the
material. It gives the amount of energy dissipated by the sample due to
25 wt% untreated 1459.09 132.97 95.80
molecular mobility. The E′′ of PALF/PE composites were higher at 45 wt
35 wt% untreated 1204.53 152.18 117.94
45 wt% untreated 1607.50 218.32 152.15 %, as shown in Fig. 7. The addition of fibre increases the fibre/matrix
25 wt% NaOH treated 1859.2 198.251 137.82 interaction in the composites, which in turn results in larger energy
35 wt% NaOH treated 1282.39 134.96 90.5565 dissipation in the composites. Among the studied configurations, E′′
45 wt% NaOH treated 2041.05 314.516 195.82 increased at all fibre loadings, in the order NaOH < untreated < KOH
25 wt% KOH treated 1629.83 168.623 119.984
35 wt% KOH treated 1277.81 115.913 82.4355
fibre composites. The enhanced interfacial bonding between the fibre
45 wt% KOH treated 1908.33 144.726 92.6847 and matrix owing to the fibre treatment with NaOH reduces the mo­
lecular mobility of polymeric chains within the matrix and provides
good frictional resistance [33,60]. Thus, the amount of energy dissi­
Table 8
pated is higher, leading to greater E′′ for composites with the NaOH
Peak tan delta values and Tg of treated and untreated PALF/PE composites. treated fibre.
From Fig. 8, it was observed that tan delta increased with increasing
PALF/PE Fibre loading (wt. Peak height of Tan Tgfrom Tan delta
%) delta (◦ C)
temperature until peak magnitude and then decreased with a further
increase in temperature. Peak tan delta values and glass transition
Untreated 25 0.3539 82.055
temperatures obtained from the tan delta plots are shown in Table 8.
35 0.3064 78.812
45 0.3214 82.678 Peak tan delta values of 0.3781 (corresponding to higher damping Mode
NaOH 25 0.3274 79.541 I = 0.3399 from free vibration analysis) and 0.3480 (corresponding to
treatment 35 0.3186 77.737 Mode I = 0.3064) were observed for KOH treated composites at 45 wt%
45 0.2608 76.502 and 35 wt% loading. Moreover, the tan delta values of KOH treated
KOH treatment 25 0.3223 80.131
35 0.3480 76.389
composites (shown in Table 8) increased with fibre loading, supporting
45 0.3781 84.735 the damping values (Mode I) obtained from the free vibration analysis
(Table 6). The maximum peak value for the 45 wt%/KOH treated PALF/
PE formulation, shown in Table 8, indicates higher damping charac­
the materials and are shown in Fig. 6. The maximum E′ peak was teristics, which correspond to poor fibre-matrix adhesion and increased
observed for 45 wt% of untreated and treated PALF/PE composites molecular movement in the polymer chains. The glass transition tem­
(Fig. 6). A similar observation of E′ peak at higher fibre loading was also perature increased in the order KOH < untreated < NaOH with the
reported in the earlier studies [56–58]. Increasing the fibre content in treated fibre composites.
the polymers resulted in an improvement in stiffness at higher temper­ Fig. 9 shows the Cole-Cole plots of PALF/PE composites in which E′′
atures. The E′ of PALF/PE composites at temperatures between 50 – is plotted as a function of E’. According to Joseph et al. [61], a perfect
100 ◦ C is tabulated in Table 7. It is clear from Table 7 that increased E′ semi-circle indicates a homogeneous polymeric system, and an elliptical
was observed at 45 wt%. This is because of the improved stress transfer curve or imperfect circle represents a heterogeneous system. It can be

Fig. 10. Strain-temperature plots for treated and untreated PALF/PE composites.

9
K. Senthilkumar et al.
Table 9
CTE of treated and untreated PALF/PE composites.
PALF/PE Coefficient of thermal expansion (μm/m◦ C)
Fibre loading (wt. %)
25% 35% 45%
Untreated 0.45 0.30 0.15
NaOH treated 0.55 0.50 0.05
KOH treated 0.10 0.55 0.15
noticed from Fig. 9 that the plots became more irregular with an increase
in fibre loading for the composites with both untreated and treated fi­
bres. This attribute reflects the heterogeneity of the PALF/PE composites
at higher fibre loadings and agrees with the larger void content and
lower compressive strength observed at 45 wt% for the composites with
treated fibre.
3.6. TMA
TMA was also performed for both untreated and treated fibre com­
posites in order to investigate the thermal expansion (dimensional
change) behavior, as shown in Fig. 10, as a function of temperature in
the thickness direction. The CTE of PALF/PE (both untreated and
treated) composites at different fibre loadings obtained from the slope of
the strain-temperature plot (Table 9).
Table 9 shows that the CTE of the untreated fibre composites
decreased as fibre loading increased. Lee et al. [62] reported that the
CTE could be presumed to be equal in all directions for a polymer
composite with short and randomly oriented fibres, and that a decrease
in CTE with an increase in fibre content would imply less dimensional
change in the composite at the higher fibre content. The treated
PALF/PE composites followed the same pattern as composites with the
untreated fibre. The trend for PALF/PE composite with KOH treated
fibres, however, was distinct. CTE increased from 0.1 at 25 wt% to 0.55
and 0.5 at 35 wt% and 45 wt%, respectively.
4. Conclusions
NaOH and KOH treated PALF/PE composites were fabricated and
characterized under fibre loadings between 25 wt% to 45 wt%. The
crystallinity index of the PALF increased slightly due to fibre treatment
with NaOH and KOH. Compressive strength improved by 38.5% and
50% as the fibre content increased from 25 wt% to 45 wt% for NaOH and
KOH treated composites. However, the compressive strength for the
composites with treated fibres were inferior compared to their coun­
terpart with untreated fibres. The rough fibre surface and fibrillation
caused due to the NaOH and KOH treatment could have improved the
fibre-matrix adhesion, however it could have weakened the individual
elementary fibres. On the other hand, Agglomeration of fibres at higher
fibre loadings could have affected the fibre dispersion in the matrix and
act as a stress concentration region leading to lower compressive
strength. The agglomeration of fibres and uneven dispersion into the
matrix was also evident from the larger void % at 45 wt% fibre loading
and heterogeneity of the Cole-Cole plot from DMA results. A significant
influence in vibration damping was observed in treated fibre compos­
ites, which was ascribed by changes in fibre-matrix adhesion. TMA re­
sults revealed the lowest CTE for the composites at 45 wt% fibre loading
regardless of the fibre treatment, indicating that higher fibre loading is
desirable for applications requiring greater thermal stability.
Acknowledgements
The authors are thankful to Universiti Putra Malaysia, Malaysia for
funding through HICOE Grant no: 6369108. This research was partly
supported by the King Mongkut’s University of Technology North
10
International Journal of Adhesion and Adhesives 106 (2021) 102823
Bangkok, Thailand by Grant KMUTNB-BasicR-64-16. The KSU authors
are grateful to the Deanship of Scientific Research, King Saud University
for funding through Vice Deanship of Scientific Research Chairs.
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