Abstract
Natural fibres from renewable resources offer a sustainable and biodegradable alternative to
synthetic reinforcements. This study investigates the thermal an d mechanical properties of
Borassus husk fibre/epoxy composites, fabricated via the hand layup process using untreated
and alkali-treated fibres. The fibres were treated with 5% NaOH for varying durations (0.25–2
hours), and their thermal stability was as sessed through thermogravimetric analysis (TGA)
following ASTM E2550. Dynamic mechanical analysis (DMA) was performed according to
ASTM D5418-01 to evaluate their mechanical performance at elevated temperatures. Results
indicate that alkali treatment significantly enhances the thermal stability of the composites, as
evidenced by increased char content (up to 11.5%) and higher integral procedural
decomposition temperature (IPDT), w ith the 0.75 -hr treated fibre/epoxy (0.75TBHFE)
achieving the highest IPDT (580°C). The composites also demonstrated superior energy
dissipation and mechanical stiffness compared to neat epoxy (NE) and other bio -fibres based
composites. The glass transition temperature (Tg) increased from 83.9°C (NE) to 94.6°C
(0.5TBHFE), outperforming compo sites reinforced with other natural fibres. Additionally,
storage modulus and damping factor (tan δ) improved significantly, with 0.5TBHFE exhibiting
the best balance between stiffness and damping. The total mass loss (TML) was reduced by
approximately 34% compared to NE, further confirming the enhanced thermal stability. These
findings suggest that alkali -treated Borassus husk fibre/epoxy composites offer excellent
thermal resistance, mechanical strength and impact resistance, making them promising
Materials
for high-performance applications in the aerospace and automotive industries, which
would also promote sustainable development. However, variations in properties of biofibres
require further research, along with the development of an efficient supply chain for industrial-
scale production.
Keywords
Borassus flabellifer husk fibre, agro -waste, thermal properties, dynamic
mechanical analysis, sustainability
Nomenclature
Subscripts
IPDT
IPDH
q(DSC)
Q
Hd
E'
E''
E*
tan δ
Tg
TML
Integral process decomposition temperature (°C)
Integral process decomposition heat flow (W/g)
Heat flow (mW)
Specific heat flow (W/g)
Specific decomposition enthalpy (J/g)
Storage modulus (MPa)
Loss modulus (MPa)
Shear (Complex) modulus (MPa)
Damping factor
Glass transition temperature (°C)
Total mass loss (%)
T
P
w
t
δ
W
Temperature (°C)
Load (N)
Width (mm)
Thickness (mm)
Phase Angle (°)
Weight (mg)
1. Introduction
Natural fibres from renewable resources offer a sustainable and biodegradable alternative to
synthetic reinforcements. They are lightweight, cost -effective, and environmentally friendly,
with excellent specific properties. Additionally, these fibres provid e superior thermal and
insulating performance while requiring minimal energy for processing, making them an
efficient and eco-friendly choice for various applications [1], [2].
With global temperatures and greenhouse gas emissions rising, the United Nations
Environment Programme's (UNEP) latest Emissions Gap Report warns that current Paris
Agreement commitments could lead to a 2.5–2.9°C temperature increase above pre-industrial
levels by the end of the century, underscoring the urgent need for stronger climate action [3].
Under this agreement, European Union (EU) members have committed to making the EU the
world’s first climate-neutral economy and society by 2050. As part of thi s effort, the EU has
submitted its long-term carbon reduction strategy and pledged to cut emissions by at least 55%
by 2030 compared to 1990 levels [4], [5] . Furthermore, EU agreed to keep global average
temperature rise to well below 2°C above pre-industrial levels, with efforts to limit it to 1.5°C
[6].
A range of polymer composite materials reinforced with natural fibres has been developed
using modified synthetic strategies, enabling applications that extend from automotive to
biomedical fields [7]-[9]. Common natural fibres include coconut, sisal, jute, ramie, banana,
hemp, kenaf, flax, pineapple leaf, abaca leaf, bamboo, date palm, sugarcane fibre, and cotton.
These fibres are incorporated into polymeric resins to improve the performance and properties
of the final products [10]-[12]. Borassus flabellifer (Palmyra palm) husk fibre remains largely
unexplored among conventional natural fibres despite its significant potential. It shares similar
chemical components —cellulose, hemicellulose, and li gnin—while offering mechanical
properties and thermal resistance comparable to well -known fibres such as jute, sisal, hemp,
bamboo, and flax [13]-[16].
Borassus flabellifer, commonly known as the Asian Palmyra palm, is a vital crop supporting
local economies across South and Southeast Asia, valued for its fruit and palm sugar production
[17], [18]. Borassus flabellifer fibres are mainly extracted from the fruit of the palm tree, though
they can also be obtained from the leaves and bark using mechanical or water retting methods.
While the fruit, leaves, trunk, and bark have traditionally been used for household applications,
the fruit shell (husk) has been treated as agricultural waste in Bangladesh [19], [20]. Unlike
other natural fibers such as jute, sisal, flax, and ramie, acquiring the raw material from Borassus
husk requires planting and/or preserving the Borassus flabellifer trees, rather than cutting them
down. To do so, we are contributing towards net -zero carbon emission aim set by Paris
agreement, 2015 [4], [5]. On top of that, it would also help to keep locals safe from ma jor
natural calamities, including flood [21], thunder lightning [22], cyclone [23], riverbank erosion
[24] and keeping local bio-diversity [25] in Bangladesh.
Like other lignocellulosic fibres, Borassus fibres are naturally hydrophilic, meaning they
absorb moisture easily. This reduces their compatibility with hydrophobic polymer matrices,
making composite fabrication challenging. Additionally, the extracted fi bres often contain
impurities, such as , waxes and pectin, further limiting their suitability for engineering
applications [26]-[28]. To enhance compatibility and reduce hydrophilicity by removing
impurities, wax, and hemicellulose, various chemical treatments can be applied, including
alkali, saline, potassium permanganate, benzoylation, and acetic acid treatments. Among these,
alkali treatment is the most widely used due to its cost -effectiveness, efficiency, and ease of
application [26], [27]. However, a high alkali concentration and extended treatment time can
lead to the excessive removal of protecti ve components (cellulose) from the material surface,
significantly weakening the fiber and reducing its strength [28]-[30].
The impact of chemical treatment on the mechanical behaviour of banana fiber -reinforced
polyester composites has been studied, showing that alkali -treated banana fiber composites
display stronger fiber -matrix interactions, resulting in improved mechanical properties [31].
Few studies have explored the impact behavior of natural fiber-reinforced polymer composites.
Jute fibers have been shown to significantly enhance fiber-matrix adhesion, thereby improving
the mechanical properties of jute fiber-reinforced polypropylene (PP) composites [32].
Composites are widely used in spacecraft, military planes, commercial aircraft and unmanned
aerial vehicles (UAVs), and their applications include engine parts, aeroplane coverings, and
interior coatings [33]. Composites are valued for their high specific strength, impact resistance,
fatigue resistance, corrosion resistance, and ability to optimize mechanical properties in high -
stress areas. They are also commonly used in airplanes to reduce weight and improve fuel
efficiency [1], [2], [34] -[36]. One way to meet this requirement is by using polymer matrix
Materials
that can be repeatedly heated and cooled for reuse. When combined with natural
fibers such as flax, jute, date palm, hemp, or sisal, these composites become 100% recyclable
[37]. Balakrishan et al [38] reported that the aircraft industry has a growing demand for
lightweight materials due to rising oil and gas prices, as fuel costs account for nearly half of
operating expenses, even in general aviation. Additionally, the average cost of launching a
heavy-lift system into low Earth orbit is approximately €5,000–15,000 per kg.
Santos et al [36] stated key material criteria for aircraft internal structural components include
being non -toxic, sourced from non -problematic origins (such as avoiding deforestation for
wood), and not generating hazardous waste during or after fabrication that could contribute to
ozone depletion or global warming. Aircraft cabin components must also be resistant to
moisture absorption while remaining lightweight to reduce fuel consumption and carbon
emissions, all without compromising performance [33]. Sustainability should be prioritised by
incorporating end-of-life strategies such as recyclability, biodegradability and ease of reuse or
refurbishment, supporting a circular economy and reducing material waste [39]-[41]. Thermal
comfort is crucial, necessitating materials that maintain a consistent temperature to prevent
internal components from becoming too hot or cold. Furthermore, panels should contribute to
passenger comfort by effectively reducing cabin noise levels [42]-[44]. Hexion L-285 epoxy
resin (with hardener H-285) is widely used in aeronautics, including in gliders and light aircraft,
due to its exceptional mechanical and thermal properties, along with a broad operating
temperature range [45]. Locatelli with co-researchers [46] reported that the wing box of the
Airbus A320-200 was constructed using ramie fiber-reinforced polymer, resulting in a weight
reduction of up to 14% compared to 7000-series aluminum, thanks to its low density, all while
maintaining structural integrity. Flax fiber -reinforced polymer composites were used for the
manufacturing of the tailplane, cabin door, partition panels, tray tables, and baggage
compartments [47], [48], whereas wing was manufactured from hemp, sisal and ramie-based
composites [49].
Natural fiber -reinforced polymer matrix composites have achieved commercial success in
semi-structural and structural applications, including in electronics, sports technology,
automotive, aerospace, and plastics. By using natural fibers and bio -based resins, 100% bio-
based composites with enhanced mechanical properties can be developed for more demanding
structural applications [50]. Flexible and versatile materials are crucial for a range of light
spacecraft applications, such as solar sails, sun shield s, radar systems, rovers, reflect arrays,
solar concentrators, and antennas. As a result, polymer composites now account for
approximately 80% of the components used in satellite launches. Similarly, in the automotive
industry, leading companies like Mazda, Mitsubishi, Toyota, Fiat, Mercedes-Benz, BMW, and
V olkswagen have adopted bio-composites to reduce carbon footprints and lower fuel costs [7],
[43], [51], [52].
Thermogravimetric analysis (TGA) involves measuring the change in a sample's mass as its
temperature or time is varied under controlled conditions. The experiment typically involves
heating or cooling a sample in a pan within a furnace, while its mass is continuously recorded.
A purge gas is used to control the sample environment, with inert gases like nitrogen commonly
employed for pyrolysis to flow over the sample [53]. Researchers [54]-[65] carried out
thermogravimetric analysis (TGA) was conducted on natural fiber -based composites, where
char content and the derivative weight loss rate were recorded. Additionally, to assess the
thermal stability of the test material, researchers used the integral proces s decomposition
temperature (IPDT) [66]-[68]. Meanwhile, to estimate the specific heat capacity (Cp) in
relation to endothermi c and exothermic heat flow, authors suggested integral process
decomposition heat (IPDH), as reported in their previous studies [69], [70].
Dynamic mechanical analysis (DMA) is an essential and effective technique for assessing the
morphology and viscoelastic properties of crystalline polymers and composite materials. It
offers valuable insights into primary relaxation processes and key parameters, including
dynamic/complex viscosity, storage and loss compliance, and damping factor [71]-[74]. The
DMA technique offers significantly greater sensitivity in determining Tg, being up to 100 times
more sensitive than the differential scanning calorimetry (DSC) method [32], [71], [73].
Gupta and Srivastava [54] carried out DMA analysis of jute fiber-reinforced epoxy at different
fiber loadings showed that the epoxy with 25% (w.t) jute fiber exhibited improved storage
modulus and loss modulus, along with a reduced damping factor (tanδ), compared to both neat
epoxy and other composite variations. Manral with co -workers [75] found that 10% sodium
bicarbonate-treated jute fibre reinforced polylactic acid (PLA) composite showed better impact
properties (tanδ) while composite with 20% treated jute fibre achieved maximum storage and
loss modulus values. Kumar with co-researchers [76] carried out DMA at different frequencies
on alkali-treated flax fibre reinforced composites, and found that with increasing frequency,
storage and loss modulus as well as glass transition temperatures, Tg, increased, wherea s
damping factor (tanδ) found to be decreased, compared to neat epoxy. Ram with co-researchers
[77] carried out DMA on alkali -treated Asian Palmyra sprouts fibre reinforced epoxy
composites at different fibre loadings. They found that effectiveness of fibre is highest at 40%
fibre loading with epoxy, and the loss modulus and damping peaks decreased with increase of
fibre loading, whereas storage modulus decreased with increase in fibre loading.
Most previous studies have primarily focused on composites made from fine and coarse fibers
of Borassus, with limited research conducted on Borassus husk fibers. However, preliminary
investigations into the properties of Borassus husk fibers have already b een reported by the
authors [19], [30], [69], [70], [78] . In this study, composites were fabricated using the hand
layup process, incorporating raw and alkali-treated Borassus husk fibers (treated between 0.25-
hr and 2-hr) reinforced with epoxy resin. The primary objective of this paper is to investigate
the thermal properties, including decomposition rates, onset decomposition temperature,
integral process decomposition temperature (IPDT), integral process decomposition heat flow
(IPDH), and specific dec omposition enthalpy, in accordance with ASTM E2550 standards.
Additionally, dynamic mechanical analysis (DMA) was conducted to evaluate properties such
as storage modulus (E ’), loss modulus (E ”), and damping factor (tan δ) following ASTM
D5418-01. Other critical factors, including shear modulus (E*), phase angle (δ), glass transition
temperature (Tg), and total mass loss (TML), were also assessed.
2. Materials and Methods
2.1. Raw materials
Fruit shells of the Palmyra Palm (Borassus flabellifer) were collected fr om rural areas in
Bogura, Bangladesh. The shells were cut into smaller pieces and cleaned thoroughly through a
water-retting process. They were then sun -dried for several days before being chopped and
ground into fine fibers using an electric blender, followed by sieve analysis. Epoxy laminating
resin (EL2) and a compatible slow hardener were sourced from Easy Composites, UK. For
alkali treatment, hydrochloric acid (HCl) and sodium hydroxide (NaOH) were procured from
Sigma-Aldrich, UK.
2.2. Alkali Treatment
The particles were treated with a 5% ( w.t) NaOH (alkali) solution for 0.75 hr, 1 hr and 2 h rs.
The ratio of the distilled wat er to sodium hydroxide to fibre used was 19:1:1 [30], [69], [78],
[79]. Then the solution with samples was neutralised with hydrochloric acid (HCl), and rinsed
with ta p water to eliminate any remaining chemical residue. The optimum mechanical
properties of the composite were observed at a concentration of 5% NaOH [80]-[82]. The fibres
were washed and then conditioned at 80°C for 2 4 hours in a hot air oven before being stored
in desiccator containers.
2.3. Composite preparation
Composites were prepared using the hand lay-up method. First, 10% (w.t) fiber (either treated
or untreated) was mixed with resin in a mixing pot and stirred mechanically for 10 minutes to
achieve a homogeneous mixture. The mixture was then placed in a vacuum chamber at a gauge
pressure of 20 bar for 20 minutes to remove any trapped moisture [30], [78].
Next, the mixture was poured into a 160 x 160 mm mould t o form a 3 mm thick board. Prior
to pouring, the mould was polished with a release agent to prevent the composite from sticking
during removal. The composite was left to cure at room temperature for 24 hours, then
demoulded and placed in an oven at 60°C for 6 hours for post-curing, following the supplier's
technical datasheet instructions. After post -curing, the sample was allowed to cool at room
temperature for 24 hours before being cut to the desired dimensions for the experiments.
Finally, the samples were given representative names for convenience. Figure 1 illustrates the
composite preparation process, and Table 1 lists the names of the representative composites.
Figure 1. Composite preparation by hand layup.
Table 1. Composition of composites and representative names.
Serial
No
Sample Description Representative
Name
01 Neat Epoxy NE
02 Untreated Borassus husk fibre reinforced epoxy UBHFE
03 0.25-hr alkali-treated Borassus husk fibre reinforced epoxy 0.25TBHFE
04 0.5-hr alkali-treated Borassus husk fibre reinforced epoxy 0.5TBHFE
05 0.75-hr alkali-treated Borassus husk fibre reinforced epoxy 0.75TBHFE
06 1-hr alkali-treated Borassus husk fibre reinforced epoxy 1TBHFE
07 2-hr alkali-treated Borassus husk fibre reinforced epoxy 2TBHFE
2.4. Thermogravimetric and Differential Thermal Analysis (TGA/DTA)
TGA/DTA was performed using a TA Instruments SDT -Q600 Simultaneous TGA/DTA
instrument. Sample sizes ranged from 8 to 12 mg, and the heating rate was set to 20 °C/min
under a nitrogen flow of 110 mL/min. Each sample was heated from 25°C to 700°C, following
the ASTM E2550 standard [83].
The integral process decomposition temperature (IPDT) has been adhered to estimate the
thermal stability of materials based on their components, which was proposed by Doyle [67]
for polymeric materials. IPDT was determined from the equation used in previ ous study [66],
[68]:
𝑰𝑷𝑫𝑻 (°𝑪) = 𝑨 × 𝑲 × (∆𝑻) + 𝑻𝟎 (4)
𝑨 = 𝑺𝟏 + 𝑺𝟐
𝑺𝟏 + 𝑺𝟐 + 𝑺𝟑
(5)
𝑲 = 𝟏 + 𝑺𝟐
𝑺𝟏
(6)
∆𝑻 (°𝑪) = 𝑻𝟏 − 𝑻𝟎 (7)
Where, A is the area ratio of the complete experimental curve as found from the TGA
thermogram, K is the coefficient of A, T0 is the starting temperature (˚C), and T 1 is the final
temperature (˚C). S1, S2 and S3 are the areas under the curve depicted in Figure 2.
Figure 2. Schematic diagram of S1, S2 and S3 areas for determining IPDT.
Wang et al. [84] suggested that the bio-fibers are thermally unstable, unlike metals, due to the
presence of various constituents such as wax, pectin, impurities, cellulose, hemicellulose, and
lignin embedded within the material. As a result, they undergo different stages of
decomposition under an inert gas flow. Following the methodology suggested by Doyle [67],
integral process decomposition heat, IPDH, was proposed by the authors [70] to determine
decomposition heat flow for the material. This indicates the material's ability to withst and
specific heat loads during decomposition. The equations are similar to those used for IPDT
[69], [70], [78] However, due to the material's thermal instability, specific heat flow (W/g) is
calculated based on the changing mass of the sample rather than its initial mass. Additionally,
both the starting and final temperatures of the test must remain consistent, along with a constant
heating rate of 20 °C/min, to ensure reliable results. The equations are provided below:
𝑰𝑷𝑫𝑯 (𝑾/𝒈) = 𝑨 × 𝑲 × (∆𝑸) + 𝑸𝟎 (8)
𝑨 = 𝑺𝟏 + 𝑺𝟐
𝑺𝟏 + 𝑺𝟐 + 𝑺𝟑
(9)
𝑲 = 𝟏 + 𝑺𝟐
𝑺𝟏
(10)
𝑸 (𝑾
𝒈 ) = 𝒒𝑫𝑺𝑪
𝑾 (11)
∆𝑸 (𝑾 𝒈⁄ ) = 𝑸𝟏 − 𝑸𝟎 (12)
Where, A is the area ratio of the complete experimental curve as found from the TGA
thermogramme, K is the coefficient of A, heat flow, qDSC is the heat load (mW) sample absorbed
or emitted (can be assessed from the TGA data), and W is the weight (mg) of the sample at that
time. Furthermore, Q0 is the starting specific heat flow (W/g), and Q1 is the final specific heat
flow (W/g). S1, S2 and S3 are the areas under the curve depicted in Figure 3.
Figure 3. Schematic diagram of S1, S2 and S3 areas for determining IPDH.
Additionally, specific decomposition enthalpy (Hd) has been introduced, which represents the
amount of heat energy absorbed by the sample throughout the duration of the experiment, from
start to end. Since bio-fibers are thermally unstable (unlike metals), the analysis considers the
variable mass (weight) of the sample, rather than its initial mass, following a similar approach
used for IPDH evaluation. All the data being gathered from TGA. The equations are provided
below:
𝑯𝒅 = ∫ 𝑸. 𝒅𝒕
𝒕𝒇
𝒕𝒊
(13)
𝑸 (𝑾
𝒈 ) = 𝒒𝑫𝑺𝑪
𝑾 (14)
Where, Hd is the specific decomposition enthalpy (J/g), heat flow, q DSC is the heat load (mW)
sample absorbed or emitted (assessed from the TGA data), and W is the weight (mg) of the
sample at that time. Furthermore, Q is the specific heat flow (W/g), and t i as well as t f is the
stating as well as the ending time of the test [duration], respectively.
2.5. Dynamic Mechanical Analysis (DMA)
Dynamic Mechanical Analysis (DMA) was conducted to assess the viscoelastic behavior of
Borassus/epoxy composites, as well as neat epoxy, following the ASTM 5418-01 standard. The
tests were performed using a TA Instruments DMA Q800 in dual-cantilever mode. The samples
were cut into rectangular shapes with dimensions of 55 mm x 13 mm x 2.5 mm. The
experiments were carried out at a frequency of 1 0 Hz with a controlled amplitude of 10 µm.
The temperature was gradually increased from room temperature to 150°C using sinusoidal
strain, with a heating rate of 3°C/min, under a compressed air atmosphere at 4.6 bar [30], [78].
The storage modulus [71]-[74], loss modulus [85]-[87] and damping factor (tan δ) [73], [88]
can be directly obtained from DMA data. However, shear (complex) modulus that refers to
Material
resistance to undergo deformation, can be calculated from Pythagorean theorem [89]
following the diagram illustrates in Figure 4.
𝑺𝒉𝒆𝒂𝒓 𝑴𝒐𝒅𝒖𝒍𝒖𝒔, 𝑬∗ = √(𝑺𝒕𝒐𝒓𝒂𝒈𝒆 𝑴𝒐𝒅𝒖𝒍𝒖𝒔, 𝑬′)𝟐 + (𝑳𝒐𝒔𝒔 𝑴𝒐𝒅𝒖𝒍𝒖𝒔, 𝑬")𝟐 (18)
Figure 4. Correlation among storage modulus, loss modulus, shear modulus and phase angle.
Where, vertical axis (Y) and horizontal axis (X) represent loss modulus, E ” and storage
modulus, E’ (MPa), respectively. Additionally, the resultant modulus depicts as shear modulus,
E* (MPa), where ‘δ’ is the phase angle (°). Phase angle, δ, can be calculated from the following
equation (Figure 4):
𝐭𝐚𝐧 𝜹 = 𝑳𝒐𝒔𝒔 𝑴𝒐𝒅𝒖𝒍𝒖𝒔, 𝑬"
𝑺𝒕𝒐𝒓𝒂𝒈𝒆 𝑴𝒐𝒅𝒖𝒍𝒖𝒔, 𝑬′ (19)
𝑷𝒉𝒂𝒔𝒆 𝒂𝒏𝒈𝒍𝒆, 𝜹 = 𝐭𝐚𝐧−𝟏( 𝑳𝒐𝒔𝒔 𝑴𝒐𝒅𝒖𝒍𝒖𝒔, 𝑬"
𝑺𝒕𝒐𝒓𝒂𝒈𝒆 𝑴𝒐𝒅𝒍𝒖𝒔, 𝑬′) (20)
Total mass loss, TML (%) refers to the percentage of mass lost by the sample during the
experiment under thermo-mechanical conditions. It is calculated by comparing the difference
between the initial mass (before the experiment) and the fina l mass (after the experiment) of
the sample [90]. In principle, low TML value indicates that the sample should be stable under
designated condition, whereas high value indicates material ’s instability. TML can be
calculated from the following equation:
𝑻𝑴𝑳 (%) = (𝟏 −
𝑴𝒇
𝑴𝒊
) × 𝟏𝟎𝟎 (21)
Where, Mi is the initial mass (g) and Mf is the final mass (g) of the sample.
3. Results and Discussion
3.1. Thermogravimetric Analysis (TGA)
Comparative thermogravimetric analysis (TGA) of all Borassus husk fibre reinforced epoxy
composites are showed in Error! Reference source n ot found.. There are three significant
phases of mass loss observed due to rising temperature. According to Figure 5a, the first weight
loss between 70°C and 170°C corresponds to vaporization of water molecules and/or moisture
content as also observed in the case of natural fibre polymer composites. The second step of
major weight loss is associated with breaking down and volatisation fundamental compositions
of epoxy resin as well as Borassus husk fibre (hemicellulose, cellulose and lignin). The final
step refers to the formation of residue. However, it is evident that pure epoxy composites show
relatively less weight loss up to 17 0°C temperature due to its hydrophobic nature, indicating
the presence of less water molecules, compared to any Borassus fibre reinforced epoxy . The
onset decomposition temperature of epoxy is around 322°C, whereas it can be observed around
330°C [ Figure 5a] for Borassus fibre/epoxy composites although for treated Borassus husk
fibre-based epoxy samples, negligible change in values being observed. The major mass loss
(approximately 83%) was found to be from 340 – 495°C, which is due to chemical
compositions of epoxy resin and husk fibre. From the TGA data, it has been found that T15% of
NE was at 340°C and T75% occurred at 407°C, whereas T15% of UBHFE was at 338°C and T75%
occurred at 409°C, which should be due to the presence of moisture absorbing composition,
hemicellulose. Nevertheless, degradation temperatures of T 15% (340 - 345°C) as well as T 75%
(411 - 414°C) for all the alkali-treated Borassus husk fibre/epoxy composites were found to be
higher, and 0.75TBHFE shows the highest value, which is due to elimination of hemicellulose
and moisture absorptive chemical bonds that was confirmed in authors’ previous work [69] as
well as other research works [91], [92]. The final stage is char formation: The char residue of
the NE found to be 6.42%, whereas in other studies it was around 9.6% [57] and 6.18% [78].
Nevertheless, all the Borassus husk fibre/epoxy samples showed higher char content (Table 2)
compared to neat epoxy, where treated fibre reinforced epoxy composites have ch ar residue
between 8.64% and 11.5%, whereas in authors’ previous work [78], it was found from 7.6% to
10.4% with respect to different heating rate ( 10°C/min). This is due to treated fibre has more
lignin and cellulose contents, which are thermally stable compared to hemicellulose (in raw
fibre). And this has been found in other studies including authors own work [69], [70], [78] .
Gupta with co-researcher [54] found that the char residue found to be below 5% for jute fibre
reinforced epoxy composite samples at different fibre loadings. Gheith et al [57] found the char
content around 19% for 50% date palm fibre reinforced epoxy, and they suggested that afte r
higher fibre loading char content increased. Kumar et al [58] carried out TGA analysis on ramie
root fibre (at different loadings) reinforce polyester composites and found that the char contents
between 5 – 11% with respect to different fibre loadings in composites. Sudhakara et al [79]
incorporated Borassus fine, sisal, jute and coir fibres into polypropylene (PP) resin and carried
out TGA analysis. They found that the char residue of Borassus fibre/polypropylene found to
be 7%, whereas char contents of coir/PP, jute/PP and sisal/PP found to be 9%, 6% and 2%,
respectively. Richmond and co-researchers [93] found the char content of 5.6% for the bamboo
fibre reinforced epoxy composite. Saba et al [94] suggested that the higher residue content
improves the flame resistan ce behaviour of materials . The char residue order for all the
composites:
0.75TBHFE > 0.5TBHFE > 2TBHFE > 0.25TBHFE > UBHFE > 1TBHFE > NE.
Furthermore, the derivative thermogravimetry (DTG) from Figure 5b shows the mass loss rate
of the composite samples. All the samples found to be similar trend up to around 200°C, which
is associated with moisture due to presence of hemicellulose and void creation during
fabrication process. The highest mass loss rate found to be 1.08 %/°C at 379°C for NE. When
Borassus husk fibres (raw and treated) were incorporated with epoxy resin, thermal
decomposition rates and related properties being affected significantly. The mass loss rate was
found to be 1.03 %/°C at 381 °C for UBHFE, which is higher than neat epoxy (NE). The
maximum derivative mass loss rate of alkali-treated Borassus fibre/epoxy composites found to
be ranging from 1.04 %/°C to 1.17 %/°C and corresponding temperature found to be between
343°C and 381°C, depending on different samples. When fibre was treated and incorporated
with epoxy resin, the corresponding temperature of derivative mass loss rates found to be
increased, which is also an indication of improved thermal stability. The fluctuation in the DTG
curve was found for all sample that could be associated with sample preparation, fibre
alignment in the resin and fibre content in the sample [16], [95]-[98]. Furthermore, it was found
to be with increasing heating rate, char content and maximum decomposition rates changes
[99], which was evident from authors’ own previous works, carried out at 10°C/min [69], [70],
[78].
Integral process decomposit ion temperature (IPDT ) proposed early by Doyle [67]-[69] is a
quantitative thermal analysis used to assess the thermal stability of sample containing the
residual carbon yields of the resulting materials at high temperatures, whether TGA degradation
is executed in a single process or multi-process [66]. This value is consistent with char content
found for all samples, where IPDT of NE found to be 486.81°C in this study, and it was found
to 464°C [68] and 428.9°C [78], when the experiment carried out at 10°C/min. All the alkali-
treated fibre/epoxy samples found to be higher IPDT value (529 – 580°C) compared to raw
fibre/epoxy (529°C) and neat epoxy value. Nevertheless, the highest value was found for
0.75TBHFE. This is due to the IPDT value for raw as well as alkali-treated Borassus husk fibre
reinforced epoxy composites found to be hi gher in authors ’ previous works [69], [70] . The
IPDT order for all the composites:
0.75TBHFE > 0.5TBHFE > 2TBHFE > 0.25TBHFE > UBHFE > 1TBHFE > NE.
Integral process decomposition heat flow (IPDH) of NE found to be 6.72 W/g, whereas UBHFE
had 7.12 W/g (Table 2). Nevertheless , including of alkali -treated fibre into epoxy resin
increased the value up to 5.83 W/g. The positive value of IPDH refers to overall much more
exothermic heat flow compared to endothermic one (Figure 5c). However, treated Borassus
fibre/epoxy samples show lower IPDH value compared to NE and among them 0. 5TBHFE
shows the lowest, 4.4 W/g. This was found in authors’ previous work, where they reported that
the IPDH value of raw (untreated) Borassus husk fibre found to be -15.36 W/g [70] and values
ranging from 5.3 W/g to 16 W/g for 0.25 -hr to 2 -hr alkali-treated Borassus husk fibre [30].
They also found that specific heat capacity, Cp, found to be higher with lower IPDH value and
Cp was lower when IPDH value found to be higher for Borassus husk fibre [69]. The IPDH
order for all the composites:
0.5TBHFE < 0.75TBHFE < 1TBHFE < 2TBHFE < 0.25TBHFE < NE < UBHFE.
The specific decomposition enthalpy, Hd, refers to the heat energy (J) experience by a unit mass
(g) of the sample during entire pyrolysis process. The H d value, 13102 J/g, found for the NE
and 12291 J/g found for UBHFE. However, there is diverge values found for the alkali-treated
Borassus husk fibre reinforced epoxy samples. For example, the highest H d value, 6673 J/g,
found for the 2 TBHFE and the least ( 3500 J/g) among treated-fibre based epoxies found for
0.5TBHFE. The discrepancy found in H d values can be associated with sample preparation,
collection and maturity of the source of Borassus husk fibre [82], [100], [101] . Figure 5 and
Table 2 show all the data of TGA for all composites at heating rate of 20°C/min.
Figure 5. TGA thermograms: a. Weight-temperature plot; b. Deri. weight loss rate-
temperature plot; and c. Weight-specific heat flow plot.
Table 2. TGA data from all composite samples.
Samples Max. dev.
Weight loss
rate
(%/°C)
Char
Residue
(%)
Integral process
decomposition
temperature,
IPDT (˚ C)
Integral process
decomposition
heat,
IPDH (W/g)
Specific
Decomposition
Enthalpy,
Hd (J/g)
NE 1.08 6.42 486.81 6.72 13102
UBHFE 1.03 9.05 529.11 7.12 12291
0.25TBHFE 1.17 10.26 555.88 5.83 6445
0.5TBHFE 1.11 11.13 573.27 4.39 3500
0.75TBHFE 1.08 11.47 579.69 4.62 3894
1TBHFE 1.07 8.64 525.02 5.37 6475
2TBHFE 1.04 11.02 568.60 5.72 6673
3.2. Dynamic mechanical properties
3.2.1. Storage Modulus (E’)
The storage modulus (E’) measures the energy (storage) stored in a material during a single
oscillation cycle. It also demonstrates temperature -dependent stiffness behaviour and load -
bearing capabilities of the composite material. Figure 6 depicts the storage modulus -
temperature curve, where neat epoxy along with untreated and alkali -treated Borassus husk
fibre reinforced epoxy composites are presented. It has been evid ent that E’ was found to be
decreased with rising temperature for all samples. Nevertheless, only untreated Borassus husk
fibre reinforced epoxy (UBHFE) shows higher storage modulus loss than neat epoxy (NE).
Rest of the alkali -treated husk fibre reinforced epoxies show higher storage modulus retain
capability during the test, and 0.5TBHFE shows the highest capability . The outcomes agree
with previous studies [78], [86], [88], [102] . Figure 6 shows that in the glassy zone, the E’
broadens due to closely packed and frozen components, resulting in a large storage modulus
value below the glass transition temperature, Tg.
The E’ curves show a sign ificant drop at around 55 - 110˚C, indicating a glass/rubbery state
transition, depending on samples. As the temperature rises, the composites lose their tight
packing structure losing inter-molecular bond strength, resulting in decreased E’ values in the
rubbery zone. The dramatic fall in E’ value near the Tg suggests the material is transitioning
from glass to rubber. Above Tg, untreated fibre/epoxy composite (UBHFE) has a lower storage
modulus than other composites, indicating increased molecular mobility that supports the
phenomenon results from increases in the molecular mobility of polymer chains above Tg.
The storage modulus curves show that adding untreated fibre decreases but incorporating alkali
treated fibre to epoxy significantly raises the E’ values. The inclusion of treated fibre enhanced
the adhesion property between stiff husk fibre and epoxy matrix, improving interfacial
bonding, which has been found in previous studies [28], [103], including authors’ own work in
SEM analysis [69], [70], [78]. This can be attributed to the clear as well as rough surface found
from the scanning electron microscopy (SEM) images revealed in previous studies [69], [81],
[104]-[107], and hemicellulose, moisture absorbing composi tion foun d to be eliminated,
confirmed through Fourier transform infrared spectroscopy (FTIR) analysis [69], [91], [104],
[108].
The untreated fibre/epoxy composite (UBHFE) shows a greater decrease in storage modulus
compared to all treated/epoxy samples. This is because impurities and hemicellulose (as
identified in the FTIR analysis) act as barriers, preventing proper bonding with the matrix [19],
[69]. This observation is further supported by the SEM results [19], [109], [110], where raw
fibre surface was found to be covered with impurities , and in the fractured surface fibre pull -
outs were observed in authors’ previous work [78]. In is notice able that 0. 5-hr treate d
fibre/epoxy composite (0.5TBHFE) shows the highest E’ followed by that of 0.25-hr treated
(0.25TBHFE) and 0.75-hr treated (0.75TBHFE) fibres reinforced epoxy samples, and 1TBHFE
and 2TBHFE samples show least strength in the experiments . This can be attributed to the
prolonged time of alkali treatment removes cellulose [28], [29], [69] , which deteriorates
mechanical properties. At higher temperatures in the rubbery region, above 120˚C, all the alkali
treated samples along with NE exhibit show more flexibility and have enhanced molecular
mobility, except UBHFE; therefore, the influence of alkali treatment is evident . The findings
are in good agreement with previous works, where sisal, jute, palm, banana reinforced epoxy
[111], banana fibre reinforced epoxy [31], flax fibre reinforced epoxy [112], and sisal fibril
reinforced epoxy [113] being used along with authors’ works [78].
Figure 6. Storage modulus-temperature plot.
3.2.2. Loss Modulus (E”)
Loss modulus refers to the amount of energy released as heat during deformation or viscous
reaction of materials. This property assesses the viscous behaviour of a material under stress.
Figure 7 represents the loss modulus-temperature curve, where neat epoxy (NE) shows the least
energy dissipation followed by all Borassus husk fibre/epoxy composites , where 1TBHFE
exhibits the highest value of loss modulus. Adding Borassus husk to composites improves loss
modulus, which follows a similar pattern as storage modulus [30], [78]. Nevertheless, 1 -hr
treated husk fibre/epoxy shows the highest loss modulus followed by 0.25-hr and 0.75 -hr
treated/epoxy composites and this has been found previously in authors own work [30]. The
loss modulus curves demonstrated the highest mechanical energy dissipation, which decreased
at higher temperatures due to the increased mobility of polymer chains [71], [73], [88], [114].
As the temperature rose, the polymer chains exhibited greater freedom of movement, leading
to reduced energy dissipation. The E" value peak height was much larger for Borassus husk
fibre/epoxy composites compared to neat epoxy (NE), indicating increased internal friction and
energy dissipation [30]. The loss modulus of composites increased with the inclusion of
Borassus husk fibre content, but decreased significantly during the rubbery stage.
The glass transition temperature (Tg) calculated from the E” curve is provided in Table 3. The
study found that Tg values derived from the loss modulus were more accurate than those
obtained from damping factor [32], [71]. Thus, this is being crucial point for any materials to
be suitable for engineering designs. The outcomes show good agreement with previous
research works [58], [111], [115]-[117], although Shinoj et al [85] found that alkali treatment
did not influence transition temperatures for oil palm fibre -based composites from the loss
modulus.
Figure 7. Loss modulus-temperature plot.
3.2.3. Damping factor (tan δ)
The damping factor (tanδ) is the ratio of the loss modulus to the storage modulus (Eʹ/Eʺ). The
damping factor may be used to assess the interlocking bonding of the fibre matrix as well as
the curing behaviour of composites [54], [72] . This property is incredibly crucial for
engineering applications, especially in aerospace and automotive, where material needs to
sustain its integrity under the simultaneous effect of heat and mechanical load [2], [31], [71],
[118].
Figure 8 illustrates the tanδ for all composites, where the untreated husk fibre/epoxy composite
(UBHFE) shows the lowest value followed by neat epoxy (NE). Nonetheless, all of the husk
fibre/epoxy displays a single peak, except UBHFE, indicating good interaction between fibre
and matrix due to lower heterogeneity in the composite [30], [85]. For all the sam ples, up to
the peak of the tanδ, damping factor increased with rising temperature, and after that, it dropped
gradually with increasing temperature. Table 3 summarizes the damping factors for all the
samples along with corresponding temperatures. The corresponding temperature with peak of
tanδ is also considered as glass transition temperature, Tg, but this one is suggested for
comparison purpose [90]. After this, material becomes soft and rubbery suggesting inter -
molecular bond strength dropped drastically and material losses its load -bearing capability
[56], [119], [120]. The order of damping factor (tanδ) of all composites:
0.75TBHFE > 0.5TBHFE > 1TBHFE > 0.25TBHFE > 2TBHFE > NE > UBHFE.
It is noticeable that all the alkali -treated fibre/epoxy composites showed higher and
enhancement in tanδ value than NE , and particularly, 0.75TBHFE and 0.5TBHFE exhibit the
maximum values of 1.39 and 1.25, respectively, which found to be similar findings reported in
authors’ previous works [30], [78]. Nevertheless, damping factors found to be higher than those
of found in the literature for other biofibres -based composites, such as, 0.46 for jute /epoxy
[54], 0.42 for woven flax reinfo rced epoxy [76], 0.86 for Borassus sprout reinforced epoxy
[77], 0.43 for kenaf reinforced epoxy [86], 0.62 for date palm reinforced epoxy [57], 0.17 for
ramie root reinforced polyester [58], and 0.58 for banana reinforced epoxy [31].
It is interesting to have found that after the alkali treatment, the adhesion property of Borassus
husk fibre enhanced, resulting better interlocking characteristic between husk fibre and epoxy
matrix that improves heat dissipation and load absorbing capacity of the treated sample, which
also can be attributed to their impact and toughness, whereas, it has been found in the literature
that after incorporating biofibres, such as, ramie, flax, jute, sisal, banana into polymeric resin
that reduced the damping factor [56], [58], [72], [76], [77], [111], [112], [115], [121] -[123],
although Richmond and co-researchers [93] found no considerable changes found in their work
on bamboo fibre reinforced epoxy after 1% alkali treatment (NaOH). Untreated fibre/epoxy
composite (UBHFE) results in decreased damping factor can be attributed to less matrix
(volume) in composites and poor adhesion between resin and fibre as a result of fibre pulled
out, which reduces vibration energy and fibre agglomeration [86], [119].
A larger peak indicates slower polymeric chain movement, resulting in increased crosslinking
density for treated fibre/epoxy composites with improved interfacial interaction and energy
dissipation ability [73], [74] . In contrast , neat epoxy (NE) and untreated husk fibre/epoxy
(UBHFE) composites exhibit a lower d amping factor. This can be attributed to the
heterogeneity of the mixture, limited ability to convert mechanical energy into heat and the
thermal instability of the material [87]. This works show good agreement with previous studies
including authors’ ones [30], [102], [115], [124], [125], although some found decreased value
after the alkali-treatment [72].
Figure 8. Damping factor-temperature plot.
3.2.4. Glass transition temperature, Tg
Tg may be calculated using numerous approaches, including the peaks of loss modulus (E")
and tan δ from Figure 7 and Figure 8, respectively. Nonetheless, Tg determined by the peak E"
(Figure 7) has been deemed more convincing and realistic than damping factor -derived ones
[32], [71], [86]. Table 3 presents the data of Tg of all the samples, where Tg derived by E" was
determined to be lower than that of tan δ curves, as evaluated by previous studies [72], [126],
[127]. The data clearly indicates that incorporating untreated Borassus husk fibre into epoxy
resin introduces heterogeneity. Additionally, the presence of hemicellulose and other impurities
found [69] in the fibre may compromise the composite's integrity during DMA experiments
[30], [78] . As a result, the composite exhibits a lower glass transition temperature (Tg),
corresponding to the peak Eʺ, compared to neat epoxy. On the other hand, all the alkali-treated
fibre/epoxy composites show higher values than neat epoxy because of improved ad hesion
property between resin and fibre that also found in authors own works previously at different
experimental conditions [30], [78]. The order of Tg values corresponding to loss modulus, E”,
is provided below:
0.5TBHFE > 0.25TBHFE > 0.75TBHFE > 1TBHFE > 2TBHFE > NE > UBHFE.
It has been found from the previous studies that after the alkali treatment, Borassus fibre shows
enhanced thermal stability [69], [106] and better mechanical property [80], [81], [110]. 0.5-hr
treated Borassus husk fibre/ epoxy (0.5TBHFE) shows the highest Tg value, 9 4.6˚C,
corresponding to E”, which should be attributed to fibre intrinsic thermal stability found in
author’s previous work [69], [78], compared to other samples [68], [69]. The glass transition
temperature, Tg (from peak loss modulus), in this study for 0.5TBHFE found to be higher than
those of found in the literature, such as, 70˚C for banana reinforced epoxy [31], 70˚ C for kenaf
reinforced epoxy [86], 72.5˚ C for sisal, jute, banana, palm reinforced epoxy [111], 79˚ C for date
palm reinforced epoxy [57] 79˚ C for palm sprouts reinforced epoxy [77], 74.8˚ C for woven flax
reinforced epoxy [76] and 74.5˚ C for jute reinforced epoxy [54]. Nevertheless, it has also been
found that Tg value was gradually decreasing for 0.75TBHFE (88.7°C), 1TBHFE (86°C) and
2TBHFE (84.6°C) with prolonged alkali-treatment, which can be associated with removal (or
damage) of temperature resistant composition s, crystalline cellulose and lignin, in Borassus
husk fibres [30], [78].
Table 3. Glass transition temperatures and damping factor of all composites.
Samples Glass Transition Temperature, Tg (°C) Peak tanδ
(Damping factor)
Tg (°C)
[from E”]
Tg (°C)
[from tan δ]
NE 83.9 100.6 0.88
UBHFE 66.1 93.5 0.73
0.25TBHFE 89.8 97.2 1.05
0.5TBHFE 94.6 107.1 1.25
0.75TBHFE 88.7 100.6 1.39
1TBHFE 86.0 96.5 1.18
2TBHFE 84.6 95.0 1.00
3.2.5. Cole-Cole plot
The Cole-Cole or Wicket plot provides useful insight into the connection between loss modulus
(E”) and storage modulus (E’). In principle, perfect semi -circle curve means homogenous
mixture between fibre and matrix, imperfect semi -circle refers to heteroge neous mixture
between fibre and matrix, and irregular shaped curve represents nonhomogeneous mixture
between fibre and matrix [58], [88], [114], [117].
Figure 9 shows plot for all the sample, where all the samples exhibit imperfect semi -circular
shape compared to kenaf/epoxy composite [86], where it was found that with the perfect semi-
circle, damping factor increased (0.43) so as Tg (70 ˚C) corresponding to loss modulus, E”. In
this study, all alkali -treated Borassus fibre/epoxy show imperfect semi -circular shapes that
refer to heterogeneity in adhesion resulting higher damping factor and energy ab sorbing
property. Interestingly, 1TBHFE followed by 0.25TBHFE composites have greater Cole-Cole
curves than the other composites, similar result reported by previous studies on flax fibre/epoxy
[76] as well as date palm/epoxy [57] and they suggested that a widen curve indicates that strong
interaction between fibre and matrix exists, resulting enhanced strength of the composites. In
this study, NE followed by 2TBHFE showed the least curvature representing low impact
properties comp ared to other alkali-treated composites , which was also found in authors’
previous work [30], [78] . A lkali treatments significantly increased fibre -matrix bonding,
providing strong evidence.
Figure 9. Cole-Cole plot.
3.2.6. Phase angle, Shear modulus and Total mass loss (TML)
Materials
exposed to temperature fluctuations and cyclic loading, such as vibrations, gradually
dissipate internal energy, resulting in a loss of strength over time. This process can also lead to
mass loss. With each vibration, intermolecular bonds weaken, causing molecules to shift from
their original state to new configurations at a specific angle, known as the phase angle (δ).
Under cyclic loading, polymers typically display viscous behaviour, with mol ecules shifting
between positions [117], [128] . If a molecule does not undergo dislocation under applied
mechanical or thermal load (loss modulus, Eʺ = 0), and only temporarily changes its shape, the
phase (change) angle is 0°, indicating the material is fully elastic. In contrast, if the deformation
is permanent (storage modulus, Eʹ = 0), the phase angle is 90°, signifying the material is fully
plastic [87]. Materials that exhibit a combination of elastic and plastic behaviour are termed
viscoelastic. For these materials, the phase angle lies between 1° and 89°, reflecting their ability
to recover from plastic (permanent) deformation. This can influence the damping factor and
Cole-Cole plot of any sample.
Table 4 summarises all the data including phase (change) angle (δ), shear modulus (E*) and
total mass loss (TML) for all samples at initial and peak loss modulus (Eʺ) conditions indicate
that alkali -treated fibre/epoxy composites exhibit higher phase angles at peak Eʺ. The NE
shows the least phase angle change , 17.9˚, followed by UBHFE (17.4˚), indicating its elastic
nature compared to other alkali -treated f ibre/epoxy samples . The 0.25TBHFE showed the
highest phase angle, 23.6˚, followed by other treated fibre/epoxy samples (Table 4). This
suggests that treated fibre/epoxy composites possess superior viscoelastic properties compared
to NE and UBHFE samples. Similarly, in the shear modulus, 0.75TBHFE shows the highest
drop in shear modulus compared to other composite samples. This behaviour can be attributed
to the high damping factors (1.39), Cole-Cole plot and loss modulus (E ”) found earlier from
the DMA experiments. The outcomes in this study found to be consistence with authors ’
previous studies [30], [78].
Additionally, under the specified conditions, all the alkali-treated fibre/epoxy composites show
less total mass loss, except 2-hr treated fibre/epoxy, 2TBHFE (0.58%), compared to neat epoxy,
NE (50%). Nevertheless, 0.75-hr treated fibre/epoxy (0.75TBHFE) shows the lowest mass loss,
0.33%, followed by 0.5TBHFE (0.35%) . Hence, these samples should perform better in
thermo-mechanical condition than NE. UBHFE found to be highest total mass loss of 1.22%,
which can be attributed to the presence of moisture absorbing as well as weak composition,
hemicellulose [91], [92], [129].
Table 4. Phase angles, shear modulus and TML of all composites.
Samples Phase angle, δ
(ͦ )
Shear Modulus, E*
(MPa)
Total mass
loss,
TML (%)
Initial Phase
angle,
δi (ͦ )
Phase angle
at E”,
δg (ͦ )
Initial Shear
Modulus,
Ei* (MPa)
Shear Modulus
Eg*,
at E” (MPa)
NE 0.90 17.9 3190.5 979.5 0.50
UBHFE 1.44 17.4 3262.6 1225.8 1.22
0.25TBHFE 0.94 23.6 2821.9 947.8 0.44
0.5TBHFE 1.01 21.5 2975.8 936.4 0.35
0.75TBHFE 0.99 21.7 3219.0 980.8 0.33
1TBHFE 0.88 22.7 3189.9 1033.9 0.41
2TBHFE 0.94 21.4 2771.1 889.1 0.58
4. Conclusion
In this study, composites were fabricated using the hand layup process, incorporating untreated
(raw) and alkali-treated Borassus husk fibers as reinforcement in an epoxy resin matrix. The
fibers underwent alkali treatment for varying durations, ranging from 0.25 to 2 hours. This
research examines the thermal properties of the composites were analyzed following the ASTM
E2550 standard. Additionally, the effects of elevated temperature on mechanical properties
were assessed through dynamic mechanical analysis adhering ASTM D5418-01 standard. The
Results
of these investigations are presented below:
TGA analysis reve aled a descent char residue (6.4 %) for NE. While incorporating
untreated Borassus husk fibre into epoxy, char co ntent (9 .1%) increased , but after
including alkali -treated fibres into epoxy , char contents (up to 11.5%) increased
significantly, where 0.75TBHFE showed the highest value (11.5%). The gained values
were found to be higher than jute/epoxy (5%), Borassus fine fibre/polypropylene (7%),
jute/polypropylene (6%), sisal/polypropylene (2%), and competitive with ramie root
reinforced polyester value (5 – 11%). This was due to Borassus husk fibre’s intrinsic
thermal resistant property because of the presence of thermal resistant compositi ons,
such as, cellulose and lignin in fibre.
The onset decomposition peak was found to be around 322 °C for NE and with the
inclusion of Borassus husk fibre s (treated and untreated) into epoxy shifted the peak
value to higher temperature (330°C).
The IPDT values for neat epoxy (NE) found to be around 487°C and raw Borassus husk
fibre/epoxy found to be 529°C. Incorporating alkali -treated fibres into epoxy resin
enhanced the IPDT value: t he highest value found to be 580°C for 0.75 TBHFE and
least was for 525°C for 1TBHFE. This was due to the intrinsic thermal stability of
Borassus husk fibre and after alkali treatment, it was enhanced further because of the
removal of hemicellulose.
The IPDH value for UB HFE found to be 7.1 W/g and 6.7 W/g for NE. Nevertheless,
after alkali-treatment, the lowest value found to be 4.4 W/g for 0.5TBHFE followed by
4.6 W/g for 0.75TBHFE.
The storage modulus increased with the incorporation of alkali-treated Borassus husk
fibre in the epoxy composite (NE), surpassing that of polymer composites reinforced
with other biofibres , such as sisal, flax, ramie root, jute, palm sprouts and banana.
Similarly, the loss modulus values also increased with alkali-treated fibres, reaching the
highest value in the 1 -hour a lkali-treated Borassus husk fibre/epoxy (1TBHFE)
composite.
The glass transition temperature (Tg), corresponding to E”, was 83.9°C for neat epoxy
(NE). With the addition of alkali-treated Borassus husk fibre, Tg increased significantly,
reaching 94.6°C for 0.5TBHFE, the highest among the tested composites. Other alkali-
treated samples also showed elevated Tg values, between 84°C and 90°C. However, the
Tg dro pped to 66 °C for the untreated husk fibre/epoxy (UBHFE) composite.
Furthermore, alkali-treated Borassus husk fibre/epoxy composites exhibited higher Tg
values than composites reinforced with other biofibres, such as , kenaf (70°C), flax
(74.7°C), jute (74.5°C), and banana (70°C). This indicates superior thermal stability,
making Borassus fibre-reinforced epoxy composites more suitable for high-temperature
applications.
The lowest tanδ value (0.73) was recorded for the untreated Borassus husk fibre/epoxy
(UBHFE) composite. In contrast, the addition of alkali -treated fibres significantly
increased the t anδ peak values. The highest values were observed in the 0. 75TBHFE
(1.39) and 0.5TBHFE (1.25 ) composites, followed by 1TBHFE (1.18 ), 0.25TBHFE
(1.05), and 2TBHFE (1.00), all of which surpassed NE (0.88 ). This superior damping
performance indicates that alk ali-treated Borassus fibre/epoxy composites possess
enhanced impact resistance compared to both neat epoxy and other bio -fibre
composites.
Cole-Cole plot revealed all the samples show heterogeneity but 1 -hr alkali -treated
Borassus fibre/epoxy composite (1TBHFE) reveals comparatively high curves to other
samples that associated with better adhesion properties between epoxy resin and alkali-
treated fibre.
Phase angle ( δ) data showed that all alkali -treated Borassus fibre/epoxy composites
exhibited a greater change in phase angle from their initial state to the glass transition
point, indicating their better viscoelastic nature. A similar trend was observed in the
shear (complex) modulus, which can be attributed to the treated samples' enhanced
toughness and impact properties.
Total mass loss (TML) is highest for UBHFE (1.22%) followed by 2TBHFE (0.58 %)
composites, as well as NE (0.50%). In contrast, the lower TML values are observed in
0.75TBHFE (0.33%) and 0.5TBHFE (0.35%) composites, which is approximately 34%
lower than that of neat epoxy (NE). This reduction can be attributed to the enhanced
intrinsic thermal stability of the alkali-treated Borassus husk fibres.
Alkali treatment enhances the thermal performance of Borassus husk fibre/epoxy composites,
as evidenced by increased char content and improved integral process decomposition
temperature (IPDT), particularly in the 0.75TBHFE sample. These treated composites exhibit
superior energy dissipation and mechanical stiffness compared to neat epoxy (NE) and other
bio-fibre composites. Their reduced total mass loss (TML), enhanced strength, and higher
damping factor (tan δ) highlight their exceptional intrinsic thermal stability. Among the treated
samples, the 0.5 -hour alkali -treated Borassus husk fibre/epoxy composite (0.5TBHFE)
achieves an optimal balance between stiffness and damping, demonstrated by its high storage
modulus (E’) and tan δ. This makes it a promising candidate for high-performance engineering
applications, particularly in the aerospace and automotive industries, where mechanical
strength, thermal stability, and impact resistance are critical.
However, bio -fibre properties can vary significantly due to environmental conditions,
geographic origin, and fibre maturity. Further research is required to improve their performance
and consistency. Additionally, while Borassus flabellifer husk is locally abundant, developing
an efficient collection and supply ch ain system is crucial for supporting la rge-scale industrial
production.
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