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Journal of Natural Fibers

ISSN: 1544-0478 (Print) 1544-046X (Online) Journal homepage: https://www.tandfonline.com/loi/wjnf20

Characterization of New Cellulosic Cyrtostachys


renda and Ptychosperma macarthurii Fibers from
Landscaping Plants

Tamil Moli Loganathan, Mohamed Thariq Hameed Sultan, Mohammad


Jawaid, Qumrul Ahsan, Jesuarockiam Naveen & Velu Perumal

To cite this article: Tamil Moli Loganathan, Mohamed Thariq Hameed Sultan, Mohammad Jawaid,
Qumrul Ahsan, Jesuarockiam Naveen & Velu Perumal (2020): Characterization of New Cellulosic
Cyrtostachys�renda and Ptychosperma�macarthurii Fibers from Landscaping Plants, Journal of
Natural Fibers, DOI: 10.1080/15440478.2020.1758865

To link to this article: https://doi.org/10.1080/15440478.2020.1758865

Published online: 12 May 2020.

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JOURNAL OF NATURAL FIBERS
https://doi.org/10.1080/15440478.2020.1758865

Characterization of New Cellulosic Cyrtostachys renda and


Ptychosperma macarthurii Fibers from Landscaping Plants
Tamil Moli Loganathan a, Mohamed Thariq Hameed Sultana,b,c, Mohammad Jawaid b
,
Qumrul Ahsand, Jesuarockiam Naveene, and Velu Perumalf
a
Department of Aerospace Engineering, Faculty of Engineering, Universiti Putra Malaysia, Serdang, Malaysia;
b
Laboratory of Biocomposite Technology, Institute of Tropical Forestry and Forest Products (INTROP), Universiti Putra
Malaysia, Serdang, Malaysia; cPrime Minister’s Department, Aerospace Malaysia Innovation Centre (944751-A),
Cyberjaya, Malaysia; dFaculty of Manufacturing Engineering, Universiti Teknikal Malaysia Melaka, Durian Tunggal,
Malaysia; eSchool of Mechanical Engineering, Vellore Institute of Technology, Vellore, Tamil Nadu, India; fDesign and
Architecture, Faculty of Engineering, Universiti Putra Malaysia, Serdang, Malaysia

ABSTRACT KEYWORDS
Cyrtostachys renda (CR) and Ptychosperma macarthurii (PM) fibers, as new Cyrtostachys renda;
cellulosic fibers were studied. The objective of this research is to evaluate Ptychosperma macarthurii;
the fibers from stem, leaf stalk, and frond of these two plants as reinforce- stem top; stem middle; stem
bottom; leaf stalk; frond
ment in the polymer composites. The density, chemical composition, func-
tional group, crystallinity index, and thermal stability were studied for CR 关键词
and PM fibers. From the analysis, the density and thermal stability of both Ptychosperma macarthurii;
leaf stalk fibers are found almost similar. The highest crystallinity index 茎顶; 茎中部; 茎底; 叶茎;
(55.67%) of the leaf stalk of CR was attributed to the highest cellulosic 前叶
content (38.99%) and the functional group (C-H stretching). From the
results, the optimized properties were found for the leaf stalk of CR fiber.
The tensile strength, interfacial shear strength (IFSS), morphology of the leaf
stalk of CR were explored. The ultimate tensile strength, Young modulus,
and IFSS of the leaf stalk of CR is 51.82 ± 9.41 MPa, 0.69 ± 0.18 GPa, and
3.27 ± 0.5 MPa, respectively. The Scanning Electron Microscopy observation
revealed that the leaf stalk fiber of CR possesses anti-microbial properties
which has been corroborated through the presence of silica bodies over the
fiber surface. Hence, the leaf stalk of CR acts as a potential reinforcement in
the polymeric composites for lightweight applications.

摘要
研究了Cyrtostachys renda(CR)和Mactyhurs macarthurii(PM)纤维,作
为新的纤维素纤维. 这项研究的目的是评估来自这两种植物的茎,叶茎和
叶的纤维,作为聚合物复合材料中的增强材料. 研究了Cyrtostachys renda
和Ptychosperma macarthurii纤维的密度,化学组成,官能团,结晶度指
数和热稳定性. 通过分析,发现两种叶茎纤维的密度和热稳定性几乎相似.
Cyrtostachys renda叶茎的最高结晶度指标(55.67%)归因于最高的纤维
素含量(38.99%)和官能团(C-H拉伸). 从结果中,发现了Cyrtostachys
renda纤维的叶茎的优化特性. 研究了Cyrtostachys renda叶茎的拉伸强
度,界面剪切强度(IFSS)和形态. 圆柏的茎秆的极限抗拉强度,杨氏模
量和IFSS分别为51.82±9.41MPa,0.69±0.18 GPa和3.27±0.5 MPa. 扫描电子
显微镜观察表明,Cyrtostachys renda的叶茎纤维具有抗微生物特性,该
特性已通过纤维表面上存在二氧化硅主体而得到证实. 因此,Cyrtostachys
renda的茎秆在轻质应用的聚合物复合材料中起到潜在的增强作用.

CONTACT Mohamed Thariq Hameed Sultan thariq@upm.edu.my Department of Aerospace Engineering, Faculty of
Engineering, Universiti Putra Malaysia, 43400 UPM Serdang, Selangor, Malaysia.
© 2020 Taylor & Francis
2 T. M. LOGANATHAN ET AL.

Introduction
A global trend and drastic transformation from synthetic fibers to biodegradable and recyclable
materials are emerging due to the stringent rules and regulations (Bajwa and Bhattacharjee 2016)
by the automobile and aerospace industries. This leads to an increased researchers’ attention
toward enhancing the properties of the existing lignocellulosic fiber by some modification or
exploration of a new lignocellulosic fiber (Brinchi et al. 2013; Jawaid et al. 2011) to have
comparable properties with the synthetic-based end product. Researchers have acknowledged
that lignocellulosic fiber has the ability to be used as a fiber reinforcement for most applications
to enhance the production, recyclability, and environmental approachability. Adesina et al.
reported that okra fiber and banana fiber composites are suitable for automotive car bumper
(Adesina et al. 2019), while Davoodi et al. proposed a hybridization of kenaf and glass fiber-
reinforced composite as a structural component in car bumper beams by improving the mechan-
ical features of the fibers (Davoodi et al. 2010). Jute fibers can substitute glass fibers effectively in
vehicle’s front bonnet (Kumar et al. 2019). As proposed by a recent study, the global market for
natural fiber composites is anticipated to expand at an annual compound growth rate of 11.8%
from 2016 to 2024, where it was valued at 4 USD.46 billion in 2016 as reported in (Natural Fiber
Composites Market Size, NFC Industry Report, 2018–2024 2018). Therefore, the current projec-
tions on future green, sustainable, and renewable products suggest the increasing use of agricul-
tural biomass over the next decade. Many of the carbon-neutral, recyclable, and renewable
lignocellulosic materials have received considerable attention and thus, have a remarkable poten-
tial to be utilized in the production of bio-based products. The chemical composition, age of the
plant, soil condition, climate, and biological location the plant was grown are significant to the
mechanical strength of a fiber which eventually effect the matrix bonding in the composites
(Loganathan et al. 2020).
Some lignocellulosic fibers from agro-waste products such as betel nut (Maheshwaran et al. 2018), oil
palm empty fruit bunches (Hanan, Jawaid, and Md Tahir 2020), coconut husk (Pandiselvam et al. 2020),
and sugar palm (Atiqah et al. 2018) have been used as reinforcements in composites. However, their
production does not meet the growing industrial demand, especially in high-load bearing applications.
Therefore, an exploration of new lignocellulosic fibers is required, particularly for the use in structural
applications to substitute the nonrenewable and unsustainable synthetic fibers. Exploring new natural
fibers could expand their potential use in feasible environmentally friendly applications. As such, some
researchers explored the physico-chemical, mechanical, and thermal properties of the integration of
new natural fibers such as Furcraea foetida (Manimaran et al. 2018), Tridax procumbens (Vijay et al.
2019), and Heteropogon Contortus (Hyness et al. 2018). The Fourier Transform Infrared Spectroscopy
(FTIR) analysis and thermal characterization of lyocell, viscose, and model investigated by Carrillo et.al.
(2004) found that lyocell is the most crystalline fiber with high thermal stability.
Besides agro-wastes, there are some other potential plant fibers which had not been extensively
explored from the Arecaceae family, i.e., Cyrtostachys renda (CR) (Figure 1a) and Ptychosperma
macarthurii (PM) (Figure 1b). CR is originated in Thailand, Malaysia, Sumatra, Borneo, and
Indonesia. It is a clustering palm tree with a slender multi-stemmed with a maximum height of
10 m (Loganathan et al. 2020). It has a bright red crown shaft and leaf sheath, which makes it unique
from other Arecaceae species. Meanwhile, PM is native to Australia and New Guinea, and this plant
is currently abundantly available spreading throughout the Peninsular of Malaysia as an ornamental
plant planted in highways, hotels, and housing projects. These two plants have been selected in the
current study for the following reasons:
(1) Their adaptability, availability, and high growth rates which enable access to large raw material
stocks. (2) These plants are only used for landscaping purpose and their wastes are underutilized. (3)
These plants have physical similarities and are from the same family of Areca catechu.
To the best of our knowledge, this is the first study that investigates the characterizations of CR and
PM. The aim of this research is to select a suitable fiber from different parts of the plants, i.e. top stem,
JOURNAL OF NATURAL FIBERS 3

Figure 1. Selected part from (a) Cyrtostachys renda (CR) and (b) Ptychosperma macarthurii (PM).

middle stem, bottom stem, leaf stalk, and frond, to be proposed as a novel fiber reinforcement in polymer
composites by considering their cellulose content, crystallinity, and thermal properties. In the present
study, the chemical composition, functional group (FTIR), crystallinity index (XRD), and thermal
stability are analyzed. The tensile and droplet tests were carried out only on the leaf stalk of CR, based
on the results obtained from the FTIR, XRD, and Thermogravimetric Analysis (TGA) analyses.

Materials and Methods


Parts of the CR and PM plants were cut from the growing plants in Telok Panglima Garang,
Selangor, Malaysia (Figure 2a). The small-chopped parts were oven-dried at 80°C for 24 hours.

Figure 2. Sample preparation in powder form for chemical analysis, FTIR, XRD, and TGA.
4 T. M. LOGANATHAN ET AL.

Prior to testing on the chemical composition, FTIR, XRD, and TGA, the dried fibers were ground
into powder form (Figure 2c) by using the Thomas Wiley grinding machine (Figure 2b).

Density
The densities of the listed parts of both plants were measured. The true density of the fibers was
determined by a Gas Pycnometer (AccuPyc II 1340 brand by Micromeritics Instrument Corp., USA).
Prior to this testing, the mass of the empty pycnometer and the pycnometer filled with the chopped
fibers are measured in order to obtain the mass of the fiber.

Chemical composition analysis


A chemical composition analysis was carried out, where the percentages of Neutral Detergent Fiber
(NDF), Acid Detergent Fiber (ADF), and Acid Detergent Lignin (ADL) were analyzed according to
ISO 16472, EN ISO 13906, and EN ISO 13906, respectively, using the Fibertec system (van Soest).
The chemical composition was measured for all the listed parts of CR and PM.

Fourier transform infrared spectroscopy (FTIR)


The fibers were analyzed with an FTIR analyzer (Thermo Scientific, Nicolet iS10) using attenu-
ated total reflectance (ATR) technique. The IR spectra were then analyzed by a quantitative
software known as OMNIC. The samples were scanned for 32 times from 500 cm−1 to 4000 cm−1
with a resolution of 2 cm−1. The FTIR analysis was also carried for all the listed parts of CR
and PM.

X-ray diffractometry (XRD)


The XRD analysis was performed using an x-ray diffractometer (PANalytical Philips X’Pert PRO
MPD PW3040) with a monochromatic radiation source of CuKα (α = 1,54060 Å) to generate
diffraction patterns from the crystalline powder samples at 25°C ambient temperature. The 2θ angles
were ranged from 5° to 80° with a step size of 0.0330° and a step time of 19.685 s to characterize the
crystallographic properties of the natural fibers. To calculate the relative amount of ordered crystal-
line in cellulose, the empirical formula proposed by Segal et al. as shown in Equation 1 has been
employed.
ðI002  IAM Þ
Percentage of crystalline index; %CrI ¼ X 100 (equation 1)
I002

Thermogravimetric analysis (TGA)


The Mettler Toledo TGA/DSC 1 (Schwerzenbach Switzerland) analyzer was employed to analyze the
thermal stability of fibers. The fibers which weigh approximately 15 mg were placed in an alumina
crucible and underwent the pyrolysis process with a nitrogen flow of 30 mL/min. The temperature
was set between 30°C and 580°C with a heating rate of 20°C/min. The TGA analysis is used to
measure the changes in mass loss of the fiber subjected to the change of temperature in a controlled
atmosphere condition. This TGA analysis was only carried out for the leaf stalk of CR and PM.

Tensile properties
The single fiber pull testing was only carried out for the leaf stalk of the CR fiber. The fiber was attached
with a mixture of epoxy adhesive. The paper frame was designed with a gauge length of 40 mm. Prior to
JOURNAL OF NATURAL FIBERS 5

the tensile testing, the diameter of fibers was measured at four different locations of the fibers and the
average diameter was calculated. The tensile test was performed according to the ASTM D3822-07 (2007)
using 5 kN Instron 5567 with a crosshead speed of 1 mm/min for five replicates.

Micro-droplet test
The micro-droplet test, also known as the interfacial shear stress (IFSS), was carried out in
accordance with the ASTM C1557 − 03(2008) to analyze the interfacial shear bonding between
the leaf stalk of CR fiber and the phenolic matrix. Phenolic was diluted with ethanol with wt % of
70:30, then applied to the middle of the fiber using a needle and cured in the oven at 100°C for
15 minutes as shown in Figure 3. The diameters of every single fiber (D) and the embedded length of
the droplets (L) were measured using an optical microscope (Olympus SZX model) attached with an
image analyzer. The micro-droplet test was carried out using INSTRON 3365, Dual Column
Tabletop Universal testing systems. The load and speed rates applied were 5 kN and 0.5 mm/min,
respectively. The analysis of the interfacial shear stress was calculated based on Equation 2:

F
τ¼ (equation 2)
πDL
where τ is the interfacial shear strength (MPa), F is the maximum load applied, D is the fiber
diameter (m), and L is the embedded length (m).

Scanning electron microscopy (SEM)


The morphology of the tensile-fractured fibers was examined under SEM of S-3400 N model Hitachi,
Japan brand with a voltage of 10kV. All the fractured fibers were sputtered by the sputtering in a thin
layer of gold coater to prevent the accumulation of electron charges.

Figure 3. Procedure of micro-droplet testing.


6 T. M. LOGANATHAN ET AL.

Results and discussion


Density
The density of CR and PM fibers is tabulated and compared with other families of palm fiber in
Table 1. The table shows that the stem exhibits the highest density compared to the frond and leaf
stalk. The lowest density (0.8 g/cm3) was observed for the leaf stalk of both plants. However, stem of
both plants exhibited highest density in comparison of leaf stalk and frond due to the moisture
content (Bou-Rabee et al. 2016). Stem structured from high-density fibrous tissue packing for
endospermic protection to storage the water for supply to the other part of the plant (Gartner 1995).

Chemical composition
Table 2 demonstrates the chemical composition obtained for each of the selected parts of CR and
PM compared with other palm fibers. The leaf stalk of CR possessed the highest cellulose content in
comparison with other parts derived from the CR and PM plants. The cellulose content of the CR
fibers of different parts in descending order is as follows: leaf stalk > stem top > frond > stem
bottom> stem middle. Likewise, for the PM plant, the leaf stalk fiber also showed the highest
cellulose content. The cellulose content of the PM fibers according to its parts in descending
order is as follows: leaf stalk > stem middle > stem top > frond > stem bottom. Based on Table 2,

Table 1. Density of CR and PM fibers compared to other palm fibers.


Fiber Part Density (g/cm3) Ref.
CR Stem top 0.91 present study
Stem middle 0.90
Stem bottom 0.96
Leaf stalk 0.80
Frond 0.84
PM Stem top 0.98 present study
Stem middle 0.94
Stem bottom 0.90
Leaf stalk 0.80
Frond 0.83
Oil palm empty fruit bunch fiber Fruit 1.04 (Jawaid et al. 2011)
Sugar palm fiber Stalk 1.29 (Bachtiar et al. 2010)

Table 2. Chemical composition of CR and PM in comparison with other palm fibers.


Plant Part % Cellulose % Hemicellulose % Lignin Ref
Cytostachys renda stem top 35.64 18.67 19.73 Present study
stem middle 21.48 18.41 23.63
stem bottom 30.73 19.59 16.06
leaf stalk 38.99 19.15 18.24
frond 32.83 20.00 15.93
Phychosperma macarthurii stem top 31.52 24.32 9.87 Present study
stem middle 32.62 21.64 13.13
stem bottom 26.69 18.61 16.31
leaf stalk 36.42 20.79 14.22
frond 30.76 25.02 12.56
Nipah palm Frond 35.1 26.4 17.8 (Tamunaidu and Saka 2011)
Husk 36.5 21.8 27.3
Leaf 28.9 23.6 32.0
Sugar palm frond 66.49 - 18.89 (Sahari et al. 2012)
bunch 61.76 - 23.48
Ijuk 52.29 7.36 31.52
Trunk 40.56 - 46.44
Oil palm empty fruit bunch fiber 37.26 14.62 31.68 (Sudiyani et al. 2013)
leaf sheath 28.16 28.16 28.16 (Zhang et al. 2015)
JOURNAL OF NATURAL FIBERS 7

sugar palm exhibited the highest cellulose content in sugar palm especially in the front part. CR
exhibited the highest cellulosic content compared to oil palm and nipah palm.
These chemical composition findings are also in a good agreement with the FTIR results, where
sharp peaks were observed at 2917 cm–1 and 2849 cm–1, indicating the C-H stretching vibration
from CH and CH2 in cellulose, respectively. The leaf stalk of both CR and PM showed the highest
intensity at these peaks compared to other parts of the plants, thus proving that the cellulose content
is the highest in the leaf stalk. The type and content of cellulose in natural fibers, known as the major
structural component, have significant effects on the mechanical features of the natural fibers (Kian
et al. 2019; Pickering, Efendy, and Le 2016).

Fourier transforme infrared spectroscopy (FTIR)


Infrared spectra provide information on the functional groups present in the natural fibers. The infrared
spectra of the fibers from different parts of CR and PM are shown in Figure 4a and Figure 4b,
respectively.
Several sharp and prominent spectra were obtained between 3283 cm−1 and 1027 cm−1 as shown in
Figure 4. The range from 3283 cm−1 to 2917 cm−1 is mainly due to the presence of hydroxyl (OH) and

Figure 4. FTIR of different parts of (a) CR (b) PM.


8 T. M. LOGANATHAN ET AL.

CH groups (Jothibasu et al. 2020; Sharba et al. 2016). It can be observed that the IR spectra of fibers from
both CR and PM parts showed almost similar peaks. The peak at 3283 cm−1 and 3288 cm−1 in Figure 4a
and Figure 4b, respectively, indicates the presence of strong and broad O-H stretching from cellulose and
hemicellulose. Compared to the fibers from other parts, the peak at 2917 cm−1 for leaf stalks of both CR
and PM in Figure 4a and Figure 4b, respectively, is the most intense. The peak indicates a strong
C-H stretching of the leaf stalk derived from CH3 of lignin and is supported by the observed peak at
2849 cm−1 in both plants, which represents a medium strength C-H stretching of – OCH3 benzene ring
in an aromatic lignin structure. However, the fibers of the bottom stem only showed a blunt peak as
shown in the red circle regions in Figure 4a and 4b. Most C = C stretching vibration or C = O stretching
vibration (after oxidation) of the cellulose structure occurred at 1732 cm−1 or 1734 cm−1, 1603 cm−1 or
1605 cm−1, and 1516 cm−1 or 1518 cm−1 as depicted in Figure 4a and 4b, respectively. The peaks shown in
the range between 1432 cm−1 and 1317 cm−1 in Figure 4 indicate the C-H deformation vibration of the
lignin structure and – O–CH3 of the ether fragments. Whereas the peak at 1243 cm−1 in Figure 4
represents the C-C skeletal vibration. The peaks at 1031 cm−1 and 1027 cm−1 in Figure 4a and 4b,
respectively, correspond to the stretching vibration of Si–O–C bonds. Meanwhile, the peak at 895 cm−1
in Figure 4a and 4b is attributed to the Si-O stretching vibration.

X-ray diffractometry (XRD)


Natural fibers with high modulus are preferred to obtain reliable and durable composites. A higher
crystallinity index increases the mechanical properties of the natural fiber and could subsequently
increase the mechanical properties of the natural fiber-reinforced composites. Figure 5 illustrates the
XRD pattern of PM and CR and the corresponding planes involved.
Table 3 displays the calculated value of the crystallinity index (Crl%) from Figure 5 using Equation 1.
According to Table 3, the leaf stalks of CR and PM fiber showed the highest CrI% compared to other
parts of CR and PM. The cellulose crystallinity depends on the arrangement of cellulose chains forming
crystalline structures (Conley et al. 2016; Mostafa et al. 2016). The presence of silica bodies which are also
a crystalline structure may increase the percentage of the crystallinity index. The higher crystallinity
index value corroborates to a higher tensile modulus eventually improved the mechanical properties of
the fiber (Madhu et al. 2019). Crystalline cellulose significantly provides a better stiffness than the other
constituents such as hemicellulose and lignin (Petroudy 2017; Sultan et al. 2009). Therefore, high
cellulose content and high cellulose crystallinity are desirable when choosing plant fibers for use as
fiber reinforcement in polymer composites in structural applications.

TGA
Based on the analyses conducted in Sections 3.2, 3.3, and 3.4, the leaf stalk fibers of both CR and PM
plants, are shown to have the best properties to be the alternative reinforcement in composites.
Therefore, the following analyses focus mainly on these two fibers. The thermal decomposition
curves of the leaf stalk fibers of CR and PM are shown in Figure 6. The fibers exhibited three main
stages of weight loss associated with water loss, degradation of hemicellulose and cellulose, and lastly,
degradation of lignin (Chee et al. 2019; Nor et al. 2019). From the TGA curves, the water loss
occurred at temperatures between 30°C and 100°C. The biomass lost 5–10 wt% due to water
evaporation or water loss at ≤100°C (Zakikhani et al. 2016). Next, two stages of decomposition
occurred, starting with the dehydration and emission of volatile components at a temperature
around 275°C and followed by a rapid weight loss due to the oxidative decomposition corresponding
to the formation of char as the temperature increased. Therefore, the thermal stability of natural
fibers is influenced by several parameters such as the initial temperature of degradation, major
temperature degradation, the final temperature of degradation, and the amount of char formation
(Salman et al. 2015).
JOURNAL OF NATURAL FIBERS 9

Figure 5. XRD pattern on (a) CR (b) PM fibers.

Table 3. Percentage of crystallinity index of different parts of


CR and PM.
Name of the plant Part Crl%
CR stem top 48.09
stem middle 44.72
stem bottom 47.50
leaf stalk 55.67
frond 47.36
PM stem top 36.79
stem middle 42.00
stem bottom 32.54
leaf stalk 47.72
frond 39.49

From Figure 6 and Table 4, the leaf stalk fiber of CR had a higher initial (229.62°C) and major
degradation (328°C) temperatures than those of the leaf stalk fiber of PM (175.91°C and 325°C,
respectively). As the thermal stability of the natural fibers depends on constituents like cellulose,
hemicellulose, and lignin, the CR leaf stalk fiber showed better thermal properties compared to the
PM leaf stalk fiber. This is contributed by the higher content of cellulose (38.99%) and hemicellulose
10 T. M. LOGANATHAN ET AL.

Figure 6. TGA-DTG thermograms of leaf stalk of (a) CR and (b) PM.


JOURNAL OF NATURAL FIBERS 11

Table 4. Thermogravimetric data for leaf stalk of CR and PM fibers.


Plant Stages Range of temperature (°C) Peak temperature (°C) Decomposition Residue (%)
CR Initial 30-100 62.5 Water loss 26.42
First 125-275 267 Hemicellulose
Second 300-361 328 Cellulose
PM Initial 30-130 58.33 Water loss 27.58
First 127-295 275 Hemicellulose
Second 300-347 325 Cellulose

(19.15%), and a comparable content of lignin (18.24%) in the CR leaf stalk fiber compared to those in
the PM leaf stalk fiber. The hemicellulose began to degrade at 125–275°C in the CR leaf stalk fiber, and
at 127–295°C in the PM leaf stalk fiber. The hemicellulose is decomposed easily at low temperatures due
to its composition of various saccharides such as xylose, mannose, glucose, and galactose which are
amorphous in nature. It is decomposed into volatiles such as CO, CO2, and some hydrocarbons.
The lower DTG temperature curve, therefore, represents the decomposition of hemicellulose,
while the higher temperature peak corresponds to that of cellulosic materials. The cellulose degraded
at a higher temperature range (300–360°C) with the maximum weight loss rate (38.38 wt.%) attained
at 328°C. When the temperature was higher than 400°C, almost all cellulose was pyrolyzed with
a lower number of solid residues left.

Tensile strength
Figure 7 shows the tensile strength of CR fibers at different diameters. It can be seen that the tensile
strength of the fiber decreases linearly with the increase in diameter. A high aspect ratio of length to
diameter is required to allow a significant fraction of load to be transferred to the fiber through the
matrix (Chawla 2012). In this case, as the diameter of the fiber is constant, by increasing the length
of the fiber to a certain range in the composite fabrication, it will be able to improve the interfacial
load transfer between the fiber and the matrix. The smaller lumen structure as described in the
literature could be another possible reason for increased tensile strength (Vijay et al. 2019). Figure 8
shows the typical tensile stress–strain curves of single CR fibers.

Figure 7. Tensile strength versus diameter of CR fiber.


12 T. M. LOGANATHAN ET AL.

50
CR Fiber

40
Stress (MPa)

30

20

10

0
0.0 0.5 1.0 1.5 2.0 2.5

Strain (%)

Figure 8. Tensile strength versus diameter of CR fiber.

The stiffer the fiber is, the more load to be sustained. The chemical composition of the CR fiber
influences the mechanical properties. Cellulose content in the fibers plays a significant role in
determining the tensile strength (Vijay et al. 2019), where the higher cellulose content leads to
higher tensile strength. CR fiber content moderate cellulose content (38.99%) therefore exhibited
a moderate tensile strength of the fiber when compared to other natural fibers. Hemp fiber’s tensile
strength up to 277 MPa with cellulose content of 64% and 94% of cellulose crystallinity (Thygesen
et al. 2007). Kenaf’s tensile strength about 426 MPa with cellulose content of 74% reported by
(Tabrej Khan, Hameed Sultan, and Ariffin 2018) however, jute fiber with cellulose content of ranged
between 45% and 72% possess tensile strength between 393 and 800 MPa (Najeeb et al. 2020). Anish
Khan et al. reported that Cortaderia selloana grass fibers exhibited lower tensile strength of about
20 ± 1.0 MPa with cellulose content of 35% (Anish Khan et al. 2020).
In this study, the mean ultimate tensile strength obtained was 51.82 ± 9.42 MPa, Young Modulus
0.69 ± 0.18 GPa, and strain to failure 3.04 ± 1.46% as shown in Table 5. The leaf stalk of CR fiber
exhibited almost similar maximum stress values with other types of palm such as oil palm empty
fruit bunch and date palm fibers.

Table 5. Tensile properties of leaf stalk of CR and with other palm fibers.
Fiber Maximum Young’s Specific tensile Specific Young’s
diameter stress modulus strength Modulus
Fiber (μm) (MPa) (MPa) (MPa cm3/g) (MPa cm3/g) References
Leaf stalk of CR 480-620 51.82 649.63 62.80 812.04 Present study
Oil Palm Empty Fruit 180–440 52.00 2407 50.00 2314.42 (Hanan, Jawaid, and Md
Bunch fiber Tahir 2020)
Date palm fiber 100–1000 58–203 2000–7500 124.28 4523.81 (Boumaaza, Belaadi, and
Bourchak 2020)
JOURNAL OF NATURAL FIBERS 13

Micro-droplet test
Interfacial shear strength (IFSS), also known as micro-droplet, was carried out in order to determine the
interfacial adhesion or bonding between the fiber and phenolic resin. Hence, the selection of phenolic
resin extracted from chestnut shell liquid (CNSL), is naturally flame retardant and bio-based resin.
During this testing, the resin strained causing the fiber to be failure. The strain will be increased until the
resulting fragments of fibers are too small to transfer the sufficient load causing the failure. The lengths of
the fragments at this point reflect the elastic existence of the interface between CR fiber and the phenolic
matrix. Therefore, the main factors that affect the IFSS values are the ultimate tensile strength of the fiber
and their interaction between fiber and matrix. The IFSS of the composite for the leaf stalk of CR fibers is
tabulated in Table 6. A comparison with the IFSS for untreated leaf stalk of CR shows a moderate
interfacial strength. On the other hand, the oil palm fiber with phenolic resin exhibited an improved
IFSS.

Scanning electron microscopy (SEM)


Figure 9 illustrates the SEM images of the native leaf stalk structure of CR, which shows the
abundance of embedded silica bodies on the surface of the fiber strands. The spread of the strand
surface along the fiber axis is uniform and linear as can be seen in Figure 8. The main constituents

Table 6. Interfacial shear stress for CR fiber in comparison with other natural fibers.
IFSS Diameter Tensile strength
Fiber Matrix (MPa) (µm) (MPa) Ref.
Untreated leaf stalk of CR fiber Phenolic 3.27 620 51.82 Present study
Sugar palm fiber Polyester 2.5 156.96 (Bachtiar et al. 2010)
Oil palm empty fruit bunch Phenolic 4.00 472 80.92 (Ramlee et al. 2019)
Sugarcane bagasse 2.40 434 50

Figure 9. SEM morphology on the fractured surface of tensile of the fiber.


14 T. M. LOGANATHAN ET AL.

present in the silica bodies are silicon and oxygen. These embedded silica bodies are also observed in
other natural fibers such as piassava and oil palm fruit bunch (Rosli et al. 2017). It is believed that
these silica bodies contribute to the strength and rigidity of the fiber (Omar, Mohammed, and
Baharuddin 2014). In previous works reported that silica bodies could act as a defensive barrier that
protects against bacterial and fungal attacks. Therefore, embedding these fibers in the polymer is
considered inherent to the antibacterial resistance claimed that the tray table is the dirtiest surfaces
on airplanes (Zorthian 2017).

Conclusions
Due to the high demand for sustainable materials for non-load bearing applications, it is essential to
explore new potential cellulosic fibers for green composites. The new cellulosic CR and PM fibers of
palm family were characterized in this study and the following conclusions were drawn:

● The density of the leaf stalk of CR and PM fibers showed the lowest value (0.8 g/cm3).
● From the chemical composition analysis, the highest cellulosic content (38.99%) was found in
the leaf stalk of CR compared to other parts of CR and PM fiber.
● The XRD results revealed that the leaf stalk fiber of CR exhibited the highest crystallinity index
(55.67%) compared to other parts of CR and PM fiber due to the presence of the functional
group in the leaf stalk of CR.
● From the TGA analysis, the major degradation temperature was found between 125°C and 295°
C for the leaf stalk of both plants.
● The SEM analysis displayed that the leaf stalk of CR has a hollow brick-and-mortar arrange-
ment structure and silica bodies on the surface.
● The tensile and IFSS results have shown that the leaf stalk of CR exhibited better mechanical
properties and interfacial bonding, which is suitable to be used as a reinforcement in the
polymeric composites for lightweight applications.

Acknowledgments
This work is supported by UPM under GPB grant, 9668200. The authors would like to express their gratitude and
sincere appreciation to the Department of Aerospace Engineering, Faculty of Engineering, Universiti Putra Malaysia
and Laboratory of Biocomposite Technology, Institute of Tropical Forestry and Forest Products (INTROP), Universiti
Putra Malaysia (HICOE) for the close collaboration in this research.

Funding
This work was supported by the Geran Putra Berimpak (GPB) [9668200]; Universiti Putra Malaysia [9668200].

ORCID
Tamil Moli Loganathan http://orcid.org/0000-0001-6908-0457
Mohammad Jawaid http://orcid.org/0000-0001-5348-5740

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