Composites Communications 23 (2021) 100546

Contents lists available at ScienceDirect

Composites Communications
journal homepage: www.elsevier.com/locate/coco

Thermal post-processing of bagasse fiber reinforced

polypropylene composites
Manish Kumar Lila a, *, Ujendra Kumar Komal b, Inderdeep Singh b
a
Department of Mechanical Engineering, Graphic Era Hill University, Dehradun, 248001, India
b
Department of Mechanical and Industrial Engineering, Indian Institute of Technology Roorkee, Roorkee, 247667, India

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

Keywords: The current experimental investigation is focused on the thermal post-processing of bagasse fibers based poly­
Natural fiber reinforced composites propylene composites. Bagasse fiber-based polypropylene composite with different fiber weight fractions (10, 20
Thermal post-processing and 30%) have been fabricated using extrusion injection molding process. Subsequently, the specimens have
Mechanical behavior
been exposed to temperature below their softening point for different time duration. The effect of thermal post-
SEM analysis
Crystallinity
processing has been compared with neat polypropylene specimens subjected to similar conditions. A significant
increase in mechanical as well as crystalline properties has been observed in neat polypropylene and composite
specimens, but the increment reduces with an increase in fiber reinforcement as well as time. This may be
attributed to the poor thermal conductivity of natural fibers. The fracture behaviour is analyzed using scanning
electron microscopy, which also confirms the enhanced interfacial adhesion between fibers and matrix after
exposure of the composite specimens to elevated temperature.

1. Introduction commercial and fast techniques to fabricate composite products [7–9].

In the past few decades, research and engineering interest has been
shifting from monolithic materials to reinforced polymeric materials (or
composites) in order to ensure specific properties and characteristics in
various products. Natural fibers have proven themselves as a better
reinforcement material than synthetic fibers due to their low cost, low
density, easy availability, eco-friendliness, non-toxic nature, better
flexibility in design, renewability, biodegradability, less abrasive nature,
comparable mechanical properties and ease of processing [1–3]. Natural
fibers are derived from various parts of the plant, therefore, there is a
limitation of maximum fiber length, which can be extracted from the
source. Hence, their use in the form of continuous fibers is usually ful­
filled by spinning the fibers into yarns and these spun yarns are weaved
into the desired orientation into mats, which further can be used be­
tween the polymer sheets to produce structural polymer matrix com­
posites. Converting the fibers into yarn increase the cost, carbon
emission as well as process complexity, while the extraction of short
fibers is rather easier and cheaper as compared to long/continuous fibers
[4–6]. Also, short fibers are easier to mix and blend with the thermo­
plastic polymer pellets and the final product can be fabricated using
extrusion and injection molding processes, which are considered as
While using injection molding for the fabrication of the products, higher
barrel temperature is preferred for proper melting and better interfacial
adhesion between fibers and polymers. High barrel temperature results
in a faster solidification rate in mold, resulting in segregated nucleation
and further leads to a better elongation as well as mechanical properties
[10–12]. This can be managed up to a certain degree by keeping higher
mold temperature and longer cooling time, but at the same time, this
results in lower productivity [13,14]. In metals, various post-processing
techniques, i.e. annealing, carburizing, nitriding, etc. are used to
alter/enhance their properties as per the desired application. Some of
these techniques such as carburizing, nitriding etc. cannot be used for
thermoplastic polymers because of their inert nature. However, thermal
post-processing of polymer based composites can be experimentally
investigated.
Thermoplastic polymers are semi-crystalline in nature and their
crystallinity is directly related to chain length, branching as well as
density [15–17]. A variety of characterization techniques can be used to
determine the crystallinity and crystallite size of semi-crystalline poly­
mers, including differential scanning calorimetry (DSC) and X-ray
diffraction (XRD). Thermal treatment of thermoplastics can be per­
formed mainly at two stages (a) above melting temperature and (b)

* Corresponding author.
E-mail addresses: manish.lila@gmail.com (M.K. Lila), ujendrakomal@gmail.com (U.K. Komal), inderfme@iitr.ac.in (I. Singh).

https://doi.org/10.1016/j.coco.2020.100546
Received 21 April 2020; Received in revised form 25 October 2020; Accepted 26 October 2020
Available online 4 November 2020
2452-2139/© 2020 Elsevier Ltd. All rights reserved.
M.K. Lila et al. Composites Communications 23 (2021) 100546

Table 1 mechanical and crystalline behavior of processed composite materials.

Basic properties of matrix material used.
Property Standard/Source Unit Value
Tensile Strength ASTM- 3039 MPa 29.90
Tensile Modulus ASTM- 3039 MPa 1053
Flexural Strength ASTM- 7264 MPa 49.66
Flexural Modulus ASTM- 7264 MPa 1556
Melting Point (Tm) DSC ◦
C 168
Density Tech Data Sheet g/mm3 0.912
Melt Flow Index Tech Data Sheet g/10 min 11
below melting temperature, but when post-processing is concerned,
thermal processing below melting point is preferred. Thermal
post-processing not only depends on the processing temperature but also
on the processing time and it leads to variation in the crystalline
behavior of the thermoplastic polymers [16,18]. Hedesiu et al. [19]
experimentally studied the effect of annealing temperature on isotactic
propylene (iPP) and reported a significant increase in crystallinity. In a
similar type of study, Bai et al. [16] reported that annealing results in
molecular chain rearrangement in both the crystalline and amorphous
phases in polypropylene (PP). Viswanath et al. [20] reported that
photo-thermal annealing can be used to attain maximum crystallinity in
shorter annealing times in metal particle reinforced polymer nano­
composites. A significant change in crystalline properties was also re­
ported after annealing of Nano-hydroxyapatite/Poly-lactic-co-glycolic
acid composites [21]. A significant reduction in shrinkage and warpage
was reported after annealing of PP-multi walled carbon nanotube
composites fabricated by injection molding process [10]. Ivey et al. [22]
experimentally investigated the effect of annealing on short carbon fiber
reinforced PLA composites fabricated by additive manufacturing process
and reported a substantial increase in mechanical as well as crystalline
properties of developed composites. Various phenomena/mechanisms
have been taken into account to explain the variation in crystalline
behavior, including thickening of polymer crystallites, recrystallization,
solid-state thickening of lamella etc.
Overall, apart from processing of neat polymeric specimen, very few
articles have reported the effect of thermal post-processing on the me­
chanical behavior of developed/treated composites [11,16,23,24]. Also,
articles reporting the thermal post-processing/annealing of short natural
fiber reinforced composites are rare. In the current experimental
investigation, bagasse fiber reinforced (10%, 20% and 30% by wt.)
polypropylene composites have been fabricated using extrusion injec­
tion molding process and subsequently subjected to an elevated tem­
perature for different time duration. The effect of thermal
post-processing and time duration has been studied in terms of
2. Materials and methods
Polypropylene (Propel 1110MAS) is used as matrix material and was
procured from M/s IOCL, India. The basic properties of polypropylene
used as a matrix material are given in Table 1.
Raw bagasse was collected from M/s Uttam Sugar Mills Limited,
Roorkee, which contained a lot of residues, dust, pulp, pith, moisture
and uncrushed sugarcane. Initially, the raw bagasse was kept in sunlight
for 2 days to remove foul gases and to reduce the moisture content and
subsequently dried (Fig. 1a) and screened to separate the uncrushed
sugarcane (Fig. 1b). The sieved material was again screened through
another sieve to separate fibers from pith and dust (Fig. 1d). The residual
fibers (Fig. 1e) were then soaked in lukewarm water for 3 h to separate
pulp content (Fig. 1c). The pulp is lighter as it contains hemicellulose,
therefore, it absorbs water and floats on the water surface, and is easily
removable [25]. The collected fibers (Fig. 1f) at the bottom were then
washed 3–4 times in water to reduce the sucrose content in fibers, and
subsequently dried completely in a hot air oven at 80 ◦ C for 6 h and kept
in Zip-lock pouches for characterization and fabrication of composite
materials. The length and diameter of fibers were measured using op­
tical microscope and observed as 6.7–18.7 mm and 0.23–0.84 mm,
respectively, which is expected to change after fabrication of composites
due to shearing action, while processing.
2.1. Fabrication of composites
Dried fibers were initially weighed and mixed (10%, 20% and 30%
by weight) with polypropylene pellets. The fiber-pellet mixture was then
extruded separately in a single screw extruder (Make: SAI Extrumech,
India) to form composite wires of 4 mm diameter at 450 rpm and 180 ◦ C,
and further shredded to a length of 5 mm to form composite granules.
These granules were then preheated for 6 Hours at 80 ◦ C to remove the
absorbed moisture during the extrusion process and fed into injection
molding machine (Model: Endura-60, Make: Electronica, India) to
fabricate composite specimens.
The specimens (PP, 10BP, 20BP and 30BP) were fabricated at an
injection temperature of 180 ◦ C, injection pressure of 50 bar and a
cooling time of 20 s. The dimensions of the fabricated specimen were
150 × 15 × 4 (mm) for tensile testing and 100 × 15 × 4 (mm) for
flexural testing. All specimens were fabricated in accordance with ASTM
D3039 and ASTM D7264 for tensile and flexural testing, respectively.

Fig. 1. Extraction of bagasse fiber from sugarcane waste.

2
M.K. Lila et al.
Fig. 2. DSC curve for neat polypropylene.
Table 2
Thermal constants of neat polypropylene.
Material/ Thermal Thermal Specific Heat
Property Conductivity (W/m. Diffusivity (m2/s) Capacity (kJ/kg.K)
K)
PP 1110MAS 0.1792 ± 0.0024 0.0997 ± 0.0012 1.796 ± 0.043
2.2. Differential scanning calorimetry (DSC)
Differential Scanning calorimetry of polypropylene was performed
on NETZSCH DSC 200 F3 in a Nitrogen environment at a heating rate of
10 ◦ C/min. The temperature cycle of the investigation was taken as
100◦ C-200◦ C–100 ◦ C, as the melting point of polypropylene lies in this
range. It was observed that heating of the material is endothermic within
the selected range, as energy is required to break the bonds among
molecular chains to get them in free moving condition. Cooling of the
material is exothermic one, as the energy is released during solidifica­
tion/crystallization. The DSC curve recorded for neat polypropylene is
shown in Fig. 2.
On increasing the temperature, the first onset (softening point) was
observed at 142 ◦ C and melting point (Tm) was observed at 168 ◦ C. Upon
cooling, the first onset was observed at 134 ◦ C, while the solidification
point (Ts) was observed at 128 ◦ C. The temperature for thermal post-
processing can be selected anywhere between its softening tempera­
ture and melting temperature, but it could result in dimensional changes
in the developed composites. When polymers are thermally treated
below their melting point, it is considered as solid-state processing and
can be carried out with lower energy consumption. The selected final
temperature (T∞ ) was kept 1 ◦ C lower than the softening point (142 ◦ C)
of the matrix (based on DSC curves) as it is considered as maximum
temperature for any microstructural transformation as well as to elim­
inate the possibility of any dimensional change in the fabricated speci­
mens. It has been reported in various articles that reinforcement doesn’t
significantly affect the thermal degradation behavior of developed
composites, therefore the softening point is considered the same as that
of neat polypropylene [11,14,25].
2.3. Analysis of thermal constants
Initially, the thermal constants (thermal conductivity, diffusivity and
specific heat capacity) of polypropylene were evaluated using thermal
constant analyzer (Make: Hot disk, Model: TPS 2500S) with Kaptan
insulated sensor (Design: 5501, Radius 6.4 mm). The results obtained for
different thermal properties are given in Table 2. The thermal constants,
i.e., thermal conductivity, specific heat capacity, etc. vary with fiber
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Composites Communications 23 (2021) 100546
Fig. 3. Thermal post-processing of specimens.
fraction, fiber orientation. Therefore, these values were measured for
neat polypropylene samples only. Also, the thermal constants of the
developed composite specimen were hard to analyze due to limitations
of the apparatus available, as it is designed for isotropic materials only,
while short fiber reinforced composites are considered as quasi-isotropic
materials.
2.4. Thermal post-processing
The heating of the polymers can be considered as a lumped system, in
which, the temperature remains uniform within the body and changes
with time only [26,27]. According to this, at time t = 0, when an object is
placed in a medium at temperature, Tx, the heat transfer takes place
between the body and the environment, with a heat transfer coefficient,
h. During a differential time interval, dt, the temperature of the body
rises by a differential amount, dT.
An energy balance of the solid for the time interval dt can be
expressed as.
Heat transfer into the object during dt = Increase in the energy of the
object.
This expression can be written in mathematical terms as
h.As (Tx − T).dt = m.Cp .dT (1)
dT can be written as d(T - Tx) as Tx is constant = T∞.
d(T − Tx )
h. As . dt = − m. Cp . (2)
T − Tx
At time t = 0, temperature T = Ti, and after time t, the temperature
T=Tt, By integrating both sides in Eq. (2):
[ ]
Tt − T∞ hAs
ln =− .t (3)
Ti − T∞ mCp
where h (10 J/m2sK) is the heat transfer coefficient of the medium (air),
As (11720 mm2) is the surface area of the specimen to be heated, m
(15.7 g) is the mass of the specimen, Cp (1.796 kJ/kg K) is the specific
heat of the specimen material, Ti (21 ◦ C) is the initial temperature of the
specimen, T∞ (141 ◦ C) is the temperature of the hot air oven, and Tt
(140 ◦ C) is the temperature of the specimen after time t.
By using the above parameters, the time required to completely heat
up the specimen up to the desired temperature was calculated as 19min
(1151s) for neat polypropylene. The total time duration for thermal
post-processing was selected as 0.5 h (A), 1 h (B), 1.5 h (C), 3 h (D), 4.5 h
(E) and 6 h (F), which includes the heating of specimens as well. 5
specimens of each sample were selected for thermal post-processing.
2.5. Thermal processing of specimens
Hot air oven was preheated at the desired temperature, T∞ (141 ◦ C),
and the first lot (F) was placed in the oven, as shown in Fig. 3. After 1.5
M.K. Lila et al.
Fig. 4. (a) Stress-strain curves for tensile testing (b) Flexural properties after thermal post-processing.
h, 2nd lot (E), and subsequently other lots were placed in the oven at
specified time durations, selected as per the experimental design. After a
total of 6 h, the oven was switched off for ensuring slow cooling, while
the specimens were kept inside. The specimens were removed from the
oven after 10 h and kept at ambient conditions for 2 days to remove any
thermal stress. Subsequently, the thermally post-processed specimens
were characterized for their mechanical and crystalline properties as
compared to unprocessed specimens (U).
2.6. Analysis of mechanical properties
Tensile and flexural tests of neat polymer and composite specimens
have been performed on Universal Testing Machine (Model: 5982,
Make: INSTRON Inc., USA). Tensile testing has been performed at a
crosshead speed of 2 mm/min with a gauge length of 50 mm according
to ASTM standard D-3039. Extensometer (Model: 2630-113, Make:
INSTRON) is used for efficient determination of modulus properties of
developed composites. Flexural tests have been conducted at a cross­
head speed of 2 mm/minute with a span length of 60 mm as per ASTM
standard D-7264. Five specimens of each sample were used to measure
the average mechanical properties of the developed composites.
2.7. Scanning electron microscopy
The microstructural examination of fractured composite specimens
under tensile loading was performed at room temperature using a
scanning electron microscope (SEM) (Make: LEO, Model: 435VP) at
different magnification levels. A very thin film of gold was coated onto
the specimen for enhancing the conductivity using Sputter Coater
(BALTEC-SCD-005).
Fig. 5. (a) Tensile and (b) Flexural strength of thermally post-processed composite specimens.
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2.8. Crystallinity analysis
DSC has also been performed on thermally processed polypropylene
specimens to evaluate the change in enthalpy for measuring the crys­
tallinity based on Eq. (4).
ΔHf
% Crystallinity = x 100 (4)
ΔHP
where ΔHf is the enthalpy of fusion for the specimen, ΔHP is the
enthalpy of fusion for 100% crystalline material. The value of ΔHP for
100% crystalline polypropylene is considered as 207J/g [25]. The
sample used for DSC is very small (10 mg) and there are chances of
getting erroneous results due to the random distribution of fibers in the
composite specimens, therefore, X-ray diffraction technique was used to
measure the crystallinity of thermally post-processed specimens.
The tests were conducted on X-ray diffractometer (Make: BRUKER,
Model: D8 Advance) with Cu target (λ = 0.1542 nm) with Intensity
accounted between 5◦ and 30◦ (2θ angle range) at 40 kV voltage and 30
mA current. The crystallinity index was calculated by Ruland- Vonk
Method [28] using Eq. (5).
Crystalline Area
% Crystallinity = X100 (5)
Total area under the curve
where, the crystalline area is the difference between the total area under
the XRD curve and the amorphous area. Crystallinity of thermoplastic
polymers is an important aspect, which exhibits its elongation
properties.
M.K. Lila et al.
Fig. 6. SEM images of fractured (20 BP) specimens for different thermal exposure duration (a) Untreated (b) 30 min (c) 1 h (d) 3 h (e) 4.5 h and (f) 6 h.
3. Results and discussion
3.1. Analysis of mechanical properties
Initially, the neat polypropylene specimens were tested for their
mechanical properties to evaluate the effect of thermal post-processing
on their behavior. The typical stress-strain curve obtained for tensile
testing and flexural properties of unprocessed and processed neat
polymeric specimens are shown in Fig. 4(a) and (b), respectively.
An increase in tensile and flexural strength was observed when pure
polypropylene specimens were subjected to an elevated temperature for
different time durations. As compared to untreated specimens, an in­
crease of 4.2%, 7.6%, 8.4%, 9.0%, 9.7% and 10.2% in tensile strength
was observed for a time duration of 30min, 1 h, 1.5 h, 3 h, 4.5 h and 6 h,
respectively. An insignificant increase in elongation at maximum load
was also observed during tensile loading with an increase in exposure
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time while an insignificant change was observed in tensile modulus. The
increase in elongation suggests a definite increase in crystallinity due to
more slippage of molecular lamellas over each other. The increase in
flexural strength was observed as 6.2%, 9.08%, 13.93%, 14.19%,
16.90% and 17.76% for a respective increase in time duration of thermal
post-processing as compared to unexposed specimens, while an increase
of 17.67% and 21.97% in flexural modulus was observed with exposure
for 30 min and 1 h, respectively. The increase in all the properties
suggests a definite change at a microstructural level due to thermal post-
processing and the rate of increase was observed maximum up to 1.5 h of
processing, after which the change in values was insignificant.
An increasing trend was also observed in tensile and flexural strength
values of bagasse fiber reinforced polypropylene composites with
different fiber weight fraction, as shown in Fig. 5(a) and 5(b), respec­
tively. A significant decrease in tensile strength and an increase in
flexural strength was observed with an increase in fiber weight fraction
M.K. Lila et al.
Fig. 7. (a) XRD spectra of thermally processed PP specimens (b) crystallinity of different samples.
in the polypropylene matrix, which is typical behavior for short natural
fiber reinforced polymer composites [23,24,29].
Similar to neat PP specimens, an increase was observed in the tensile
and flexural properties of the composites with increased exposure
duration of thermal post-processing. Yet the cumulative increment rate
(CIR), which can be defined as a percentage increase over time, was
observed as reduced with an increase in fiber weight fraction as the
lowest increase was observed in 30% fiber reinforced composites. This
can be attributed to the thermal insulating behavior of natural fibers due
to their low thermal coefficients as compared to polymers [16,19,30].
This behavior may lead to non-uniform heat transfer within the com­
posite specimen, thereby, exhibiting less effect of thermal
post-processing on the mechanical properties of the fabricated
composites.
Maximum CIR was observed for tensile and flexural strength for an
exposure duration of 1–1.5 h and 1.5–3 h of thermal post-processing,
respectively. This increase in mechanical properties can be attributed
to either improvement in crystallinity or enhanced interfacial adhesion
between fibers and the matrix due to thermal post-processing, which can
be further confirmed with the fractographic study of the fractured
specimen as well as their crystalline behavior.
3.2. SEM analysis
The SEM images taken for 20BP specimens exposed for different time
durations are shown in Fig. 6a to Fig. 6f. The fracture behavior of the
specimen revealed that fiber fracture became a dominant mode of fail­
ure when the specimens are processed for a prolonged duration. Less
fiber pullout was observed when composites were subjected to the
thermal post-processing for the prolonged duration. This confirms an
increase in interfacial bonding between fibers and the matrix, which
restricts the fiber pull out, lead to fiber fracture and subsequent increase
in the mechanical properties of thermally processed composite
specimens.
3.3. Crystallinity analysis
Thermoplastics are semi-crystalline in nature and usually consist of
large molecular chains of Carbon (C) and Hydrogen (H), which are
bonded by strong covalent bonds. These large molecular chains form
irregular and entangled coils (snarls), when in a molten condition. When
solidified, these chains rearrange themselves and form ordered (crys­
talline lamella) and unordered regions (amorphous) with a typical size
of the order of 10–30 nm [31]. The chains are closely packed with each
other within the crystalline region by weak Van der Waals forces and
slides over each other when an external load is applied in the direction of
their orientation The XRD spectra obtained for thermally post-processed
PP specimens and calculated crystallinity for the different specimen of
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Composites Communications 23 (2021) 100546
PP based composites is shown in Fig. 7(a) and (b), respectively. A
noticeable increase was observed in the crystallinity of neat PP and 10BP
specimen. The maximum increase in intensity was observed along (110)
and (040) Bragg’s planes at 2θ value of 14.1◦ and 16.9◦ , respectively,
with an increase in exposure duration. The maximum increase in crys­
tallinity was observed as 69% (unprocessed specimen) to 75.2% (6 Hrs.
treated) neat PP specimen, while 58.5%–62.8% for 10BP specimens for
the same time duration. An insignificant increase was also observed in
the crystalline properties of 20BP and 30BP composite specimens. The
increase in peak height at different Bragg’s planes also signifies the
reduction in full width at half maxima (FWHM), that also represents an
increase in crystallite size as per Scherrer’s equation [32] The increase in
crystallinity can be attributed to molecular chain condensation in the
polymeric matrix due to thermal post-processing that also led to the
strengthening of the interface between fibers and the polymeric matrix
[33,34]. The change in crystalline properties reduces with an increase in
fiber fraction even at prolonged time duration, which can be attributed
to the thermal insulating behavior of incorporated natural fibers. This
behavior restricts the uniform heat flow in the composite specimens,
leading to comparatively lesser transformation in molecular chains.
4. Conclusions
The effect of thermal post-processing has been experimentally
investigated to analyze its effect on the mechanical and crystalline
properties of bagasse fiber reinforced polypropylene composites. The
results exhibit significant increase in mechanical and crystalline prop­
erties of neat PP specimens as well as its composites with increased
exposure duration, which can be attributed to structural rearrangement
of molecules due to thermal post-processing. The increment in me­
chanical properties and crystallinity reduces with an increase in fiber
fraction due to thermal insulating behavior of natural fibers. This ther­
mal insulating behavior restricts the flow of heat and leads to non-
uniform heating of the composites. Improvement in mechanical prop­
erties as well as SEM analysis established the enhancement in interfacial
adhesion between fibers and matrix as fiber fracture became the domi­
nant mode of fracture with an increase in exposure time. The overall
investigation suggests that thermal post-processing can be employed to
different natural fiber-based thermoplastic composites in order to
improve their properties up to a certain limit.
CRediT authorship contribution statement
Manish Kumar Lila: Conceptualization, Investigation, Writing -
original draft. Ujendra Kumar Komal: Resources, Formal analysis.
Inderdeep Singh: Validation, Writing - review & editing, Supervision.
M.K. Lila et al.
Declaration of competing interest
The authors declare that they have no known competing financial
interests or personal relationships that could have appeared to influence
the work reported in this paper.
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