The International Journal of Advanced Manufacturing Technology (2021) 112:1917–1930

https://doi.org/10.1007/s00170-020-06535-9

ORIGINAL ARTICLE

Thermo-mechanical properties of low-cost “green” phenolic resin

composites reinforced with surface modified coir fiber
Hala Bensalah 1 & Marya Raji 2 & Hind Abdellaoui 2 & Hamid Essabir 2,3 & Rachid Bouhfid 2 & Abou el kacem Qaiss 2

Received: 12 September 2020 / Accepted: 15 December 2020 / Published online: 5 January 2021
# The Author(s), under exclusive licence to Springer-Verlag London Ltd. part of Springer Nature 2021

Abstract
The focus of this work was the possibility to expand the use of coir fibers, as byproduct of the coconut industry by turning them
into new eco-composites. The evaluation of coir fiber-reinforced composites focuses on the chemical treatment and processabil-
ity of the coir fiber, how well it interfaces with a phenolic resin as Bakelite, and an analysis of how the mechanical properties of
the final product change when adding treated coir fibers. The results show that the flexural stress value of composite shows a
stabilization and the ductile behavior of composites was improved around 34.45% as compared to the neat Bakelite matrix.
However, dynamic mechanical analysis showed a change in the rheological properties of the biocomposites with increasing
temperature and fiber loading; the increase of temperature tends to enhance the free volume of the system and thereby decreases
the fibers-matrix adhesion surface leading to decrease the complex modulus. This study represents a new opportunity to valorize
biomass residues into green materials, which could reduce domestic dependence on petroleum-based thermoplastics.

Keywords Bakelite . Coir fibers . Bio-composite . Mechanical properties . Dynamic mechanical analysis . Thermal conductivity

1 Introduction structural material for residential housing construction and is

largely found in nonstructural housing components [1].
In the last two decades, the natural fiber-reinforced compos- Research and development efforts are being made to use nat-
ites have attracted substantial importance as a potential ural fibers as reinforcement for the automotive and building

Statement of Novelty
Our work is important and suitable to the Journal of Composite Materials
in terms of:
1- Experimental techniques and characterization approach: In this work,
besides the structural, morphological, thermal, and mechanical
characterization in two modes as quasi-static (flexural test) and dynamic
(rheology in the solid state), this combination offers a global investigation
of the material behavior under different solicitations.
2- Compatibilization: The idea in this work is to improve interfacial
adhesion between fibers and matrix. For this reason, the modification is
due by alkaline treatment to ensure a good interfacial adhesion (chemical
interaction). Alkali treatment detached the main non-cellulosic compo-
nents of coir fibers increasing the crystallinity and the thermal stability.
Besides, alkali treatment enhanced the interfacial adhesion coir fibers and
Bakelite matrix and subsequently.
3- This research offers an ecological alternative to upgrade to the valoriz-
ing abundant and unexploited resources to help improve the overall prop-
erties of biocomposites especially in terms of mechanical properties. In
addition, the possibility of finding uses for coir fiber in biocomposite
manufacturing will help open new markets for what is normally consid-
ered waste or for use in low value products.

* Hamid Essabir
h.essabir@uiz.ac.ma
Extended author information available on the last page of the article
1918
industries. Phenolics are thermosetting resins [2–4], which are
used in the composites field in applications requiring excellent
fire resistance properties, since they have better thermal insu-
lation and resistance to high temperatures [5, 6]. However, it
generally has low toughness and poor crack resistance [7, 8].
For this reason, many recent studies, particularly in the scien-
tific field, are interested in the incorporation of natural fibers
[9, 10] thermosetting matrices to limit this disadvantage and
improve their mechanical properties [11–13].
Thermoset polymers are among the most important mate-
rials in many industries and being used increasingly in engi-
neering applications [14, 15]. They are generally amorphous,
highly cross-linked polymers, possessing various excellent
properties such as high tensile strength and modulus, easy to
process, good thermal and chemical resistance, and dimen-
sional stability [16]. However, they have low toughness and
poor crack resistance. This is the basic reason why a large
body of literature has been on the subject of the incorporation
of natural fibers in petrochemical based thermoplastics [10,
17] and thermoset matrices[18].
Polyester [19], epoxy [20], and phenolic resins [21, 22]
were used as the thermoset matrices and are reportedly the
most widely used matrices for natural fiber-reinforced poly-
mer composites. Phenolic resins (Bakelite) show superior fire
resistance to other thermosetting resins[23]. Bakelite resin is
made by combining phenol and an aldehyde [24]. When these
organic compounds are mixed, and both pressure and heat are
applied, it causes polymerization, which is a chemical reaction
that can be used to mold solids. Bakelite resins are preferred in
a wide range of applications, from commodity and construc-
tion materials to high technology aerospace industry [21, 25].
This recognition emerges from the fact that these resins
(Bakelite) have several desirable characteristics, such as supe-
rior mechanical strength, heat resistance, dimensional stabili-
ty, flame resistance, excellent abrasive properties, low cost, as
well as, high resistance against various solvents, acids, and
water [26]. Singh et al. [27] investigated the effect of the
reinforming secondary (2°) recycled acrylonitrile butadiene
styrene (ABS) by Bakelite powder (BP). The results highlight-
ed that reinforcement of BP improves the mechanical proper-
ties and the melt flow index (MFI). New composites were
made by Azeem et al. [28] which investigated the thermal
conductivity enhancement of a graphite particulate filled
Bakelite composite. The experimental results of thermal con-
ductivity found that the addition of graphite has a significant
impact on the thermal conductivity of Bakelite. It was found
that the Mori–Tanaka model for prolate inclusions and the
Hamilton–Crosser model yield the closest approximation to
the measured thermal conductivity of filled composite system
where the particle shape morphology is important. The study
conducted by Ünlü et al. [29] deals on investigation of tribo-
logical behaviors of journal bearings manufactured from pure
Bakelite, particle-reinforced composite structures of 50%
Int J Adv Manuf Technol (2021) 112:1917–1930
CuSn10, 50% Fe, and 25% CuSn10 + 25% Fe-Bakelite jour-
nal bearings. Tribological properties of bronze particle-
reinforced Bakelite composite bearings have significantly im-
provement. So, the intrinsic properties of the used particles
have a significant impact in the performances of the
manufactured composites. These key properties add to their
market growth, and as a result of innovative research, new
products and applications continue to emerge, demonstrating
the versatility and the potential of phenol resins to cope with
the ever-changing requirements and challenges of advanced
technology [21, 30].
Thermoset material with natural fiber can constitute of both
an ecofriendly bio-composite with enhanced properties. The
new materials associated with bio-renewable resources are
now being explored especially in the automotive and biomed-
ical industries on a large scale. There are many kinds of ther-
mosetting matrix like the Bakelite, polyester, epoxy, and phe-
nolic resin. Among from this latter, the Bakelite resins are
preferred in a wide range of applications, from raw materials
and building materials to the high-tech aeronautical industry,
and this is because these resins have several desirable charac-
teristics, to be cited as superior strength, heat resistance, di-
mensional stability, flame resistance, low cost, and high resis-
tance to various solvents, acids, and water [31, 32].
Natural fibers have recently attracted the attention of scien-
tists and engineers because of the advantages they provide
over conventional reinforcing fibers such as glass fibers
[33]. The development of composites with natural fibers has
been a subject of interest for the last ten years. These natural
fibers are low cost [34, 35], low-density fibers and have spe-
cific properties such as biodegradability [36, 37], specific me-
chanical properties [38, 39], and good thermal and acoustic
insulation [40] and renewable resource [41]. There are several
types of natural fibers like oil palm [42], kenaf [43], doum [31,
44], and coir fibers [45], generally used as charge to enhance
the overall mechanical and thermal properties [46, 47], but the
composite materials based on natural fibers slightly long allow
the maintenance of the matrix after fracture [48], hence the use
of coir which is the thickest and most resistant natural fibers
[49]. However, there are a number of difficulties associated to
the integration of these fibers in polymer matrix, including
fiber matrix incompatibility. The fiber-matrix adhesion can
be improved by modifying the surface of the fiber, using var-
ious treatments. These treatments improve the wettability of
the fiber with the matrix and create a strong connection at the
fiber-matrix interface. Good adhesion at the interface contrib-
utes in turn to improve the load transfer between the fibers and
the matrix and mechanical properties are increased [50].
Coir or coconut fiber are natural fibers extracted from the
outer husk of coconut which are found in tropical countries.
Because of its hard-wearing quality, durability, and other ad-
vantages, it is used for making a wide variety of floor furnish-
ing materials, doormats, brushes, and mattresses etc. But,
Int J Adv Manuf Technol (2021) 112:1917–1930
these traditional coir products consume only a small percent-
age of the potential total world production of coconut husk
[30, 51]. Hence, apart from the conventional uses of coir as
mentioned above, research and development efforts have been
under way to find new use areas for coir fibers, including use
of coir as reinforcement in polymer composites.
The purpose of this work was to study the impact of chem-
ically treated coir fiber and the manufacturing process on
structural, morphological, thermal, and mechanical properties
of natural fibers-based Bakelite composites, because they dis-
play a diverse interaction mechanism between fibers and poly-
mer matrix. Coir fibers as natural fibers are grinded and alkali
treated. The alkali treatment has been selected as chemical
method to purify the fiber’s surface which leads to reduction
of the hydrophilicity of the fiber in order to improve interfacial
bonding between fibers and matrix. The short alkali-treated
coir fibers were used as reinforcement phase into matrix
(Bakelite), using in each case a fiber content ranging from 0
to 30 wt. %. Thus, the objective of this study is to prepare
composite materials using short alkali-treated coir fiber and
Bakelite matrix. The combined effect of fiber content and
treatment on the thermal conductivity, mechanical, and rheo-
logical properties of biocomposites is also reported.
2 Materials and methods
2.1 Materials
The PF 31 resin (Bakelite 9005-S 6) was obtained from
Momentive Specialty Chemicals at a density of 1.43 g/cm3,
and then treated to have a granulates of 150-μm sieve size.
The coir fibers originated from Ivory Coast and were supplied
as bundles of roughly 20 cm length fibers, and before further
use, raw fibers were grinded in a precision grinder (FRITSCH
Pulverisette 19) equipped with a 250-μm sieve size.
Chemicals used in this study to treat coir fibers were sodium
hydroxide (NaOH, 98%) from Sigma-Aldrich (France) and
acetic acid (CH3COOH, 99-100%) which is from Riedel-de
Haёn.
2.2 Alkaline treatment
The raw coir fibers were alkali treated by immersion for 48 h
in a 1.6 mol/L sodium hydroxide aqueous solution at room
temperature under stirring, then filtered, and washed with tap
water. To neutralize the remaining hydroxide, the fibers were
treated several times with an acetic acid solution (10 wt%).
The alkali treatment is used to remove hemicelluloses, lig-
nin’s, waxes, and oils covering the external surface of the fiber
cell wall which is known to limit the fiber–matrix adhesion.
1919
2.3 Composite preparation
To study the effect of alkali-treated coir fibers content on the
properties of Bakelite matrix, six different concentrations
were used: 5, 10, 15, 20, 25, and 30% wt. Compounding
was done on in an automatic hot press molding (CARVER).
So, in order to obtain the desired sample, molding is carried
out between two rectangular plates having dimensions of (100
* 100 * 4) mm3 (Fig. 1) using a hot molding machine
(CARVER INC, USA). The press used is an automatic press,
having two trays heated to 170 °C, and then a pressure of 40
bars was applied.
3 Characterization
3.1 Scanning electron microscopy
Electron microscopy is a technique based on the principle of
electron-matter interactions, capable of producing high-
resolution images of the surface of a sample. A focused elec-
tron beam is deflected through electromagnetic lenses, sweeps
the surface of the sample to be analyzed, which, in response,
reemits different types of emissions. Morphological analysis
of untreated and steam exploded fibers was done by scanning
electron microscopy. Scanning electron microscopy (SEM)
micrographs of coir fiber surface were taken using a scanning
electron microscope model JEOL JSM840a. Prior to SEM
evaluation, the samples were coated with a thin layer of Au/
Pd for 5 min by means of a plasma sputtering apparatus. To
obtain clean and precise fractures, all composites were frac-
tured after immersion in liquid nitrogen, and then coated.
3.2 X-ray diffraction technique
X-ray diffraction (XRD) characterization of coir fibers was
carried out on Bruker D8 Discover, using the CuK radiation
(λ = 1.54184 nm), and a GADDS detector. The scanned an-
gular range (2θ) was from 1° to 36° at a step size of 0.02°, at a
working voltage and current of 40 kV and 80 mA, respective-
ly. The use of XRD counts offers an easy way to evaluate the
crystalline index of plant particles as AS, which is calculated
from Eq. (1):


I DRX ¼ I 002 −I amp =I 002 ð1Þ
Where, IXRD is the crystalline index;
I002 the maximum intensity of the 002-lattice diffraction
plane at a 2θ angle between 22° and 23°; and Iamp the inten-
sity diffraction at an angle 2θ close to 18° representing amor-
phous materials in coir fibers.
1920 Int J Adv Manuf Technol (2021) 112:1917–1930

Fig. 1 Mold used to press sample

3.3 Fourier transforms infrared spectrometry the Data Logger Temperature (Teslo 176T4). Figure 2 shows
the schematics of the experimental setup.
Infrared spectroscopy is considered as simple, direct, and sen-
sitive characterization technique for identification of the
3.6 Physical control of elaborated composites
chemical structure and groups in different materials, which
may include coir fibers and their composites. Fourier trans-
3.6.1 Experimental density
form infrared (FTIR) spectroscopy is used to determine the
assignment of absorbance bands to specific molecular struc-
Density of the molded composite specimen was measured
tures. Fourier transform infrared spectra were recorded on an
using a gas pycnometer (IsoLab GmbH, Germany). The mea-
ABB Bomem FTLA 2000-102 spectrometer (ATR: SPECAC
surement is based on nitrogen displacement technique as the
GOLDEN GATE). The spectra were obtained with an accu-
inert gas. Three replicates for each composites sample were
mulation of 16 scans and with a resolution of 4 cm-1.
tested.

3.4 Thermo gravimetric analysis 3.6.2 Theoretical density of elaborated composites

Thermal stability is an important property for polymeric ma- The theoretical density of elaborated composites can be ob-
terials. In general, the thermal degradation of polymers can be tained as per the following equations [34]:
improved by the addition of thermally stable fillers.
Thermogravimetric analysis (TGA) is the main tools that de- ρsTheo ¼ ρ f V f þ ρm V m ð1Þ
termine the thermal properties of natural fiber-reinforced poly-
mer composites. TGA analyses were carried out using a Q500
instrument from TA Instruments. The thermal analyses were
done in an air atmosphere under a flow rate of 100 mL/min
using an alumina crucible with a pinhole. An average mass of
10 mg of the sample with a constant heating rate of 10 °C/min
was maintained from room temperature to 800 °C.

3.5 Thermal conductivity

Evaluation of the effect of coir fibers on the fire resistance of

Bakelite was performed by the use of the two-plate method.
Thermal conductivity was measured using an MCR 500
Rheometer equipped with Pelitier Plat TEK-150P-C.
Rectangular samples (50 × 50 × 4 mm3) were placed between
two plates, heated from the bottom plate until 60 °C and make
an insulation on the top plate. The evolution in the time of
temperature specimen was measured between sample and the
top plate. The temperature readings were taken every 4 s using Fig. 2 Fixture used to measure thermal conductivity (two plates method)
Int J Adv Manuf Technol (2021) 112:1917–1930
M f ρf M m ρm
Vf ¼ Mf Mm and V m ¼ M m ð2Þ
=ρ f þ =ρm =ρm þ M f=ρ f
ð2Þ
Where Vf is the fiber volume fraction, Vm is the resin vol-
ume fraction, ρm is the resin density 1.43 g/cm3, and ρfis the
fiber density equal to 1.29 g/cm3.
3.7 Flexural test
Mechanical properties of natural fiber-reinforced polymer com-
posites are commonly characterized using tensile, flexural, im-
pact, and hardness tests. Those properties of various natural
fiber polymer composites are described below. Flexural tests
were carried to measure the force necessary to break a sample.
The flexural properties of each composites system were per-
formed, using a universal testing machine Tinius Olsen. The
bending test used in this work is the three points. The specimen
dimensions are 100 × 15 mm × mm and the sample support
spanning 80 mm. The used machine is Tinius Olsen Horizon
H10KT with the load cell of 5KN at a cross head of 5 mm/min
in compression mode. The tests were performed for five spec-
imens for each composite according to the ASTM D790 stan-
dard. A total of five samples were tested to obtain an average
value comprising at least three similar data points.
3.8 Dynamic mechanical thermal analysis
Dynamic mechanical thermal analysis (DMTA) is a method to
characterize the material’s viscoelasticity by applying a sinu-
soidal strain and measuring the stress as response. The rheom-
eter solid analysis (RSA) was used to evaluate the dynamic
mechanical thermal properties of the composite materials.
Due to the stiffness of the studies’ material, a dual cantilever
configuration was used as a fixture of RSA machine. Dynamic
mechanical analysis is used to measure the mechanical prop-
erties of the sample as it is deformed over a range of fibers
loading and temperature. The test was performed with a Q800
analyzer (TA Instruments, USA) at a heating rate of 10 °C
min-1 over room temperature to 155 °C with the frequency of
1 Hz. The complex modulus (E*) and tan δ were determined
as a function of temperature.
4 Results and discussions
4.1 Chemical composition of coir fibers
The major components of natural fibers as cellulose, hemicel-
luloses, lignin, and other no cellulosic components greatly
1921
depend on the fiber’s nature and fibers type. The amount of
these constituents of the fiber varied from plant to plant, and
within different parts of the same plant. The discrepancy in
different properties of some natural fibers was made by stan-
dard methods (Fourier transform infrared spectra (FT-IR), X-
ray diffraction (XRD)) and the results were resumed in
Table 1. These analyses show that the flax fibers have the
higher content in cellulose (71%), followed by sugarcane ba-
gasse fibers (50%), coir fibers (43%), and then by bamboo and
kenaf fibers (21–42%). But in terms of density, the coir fibers
have the lowest density a. The specific coir fibers were select-
ed due to the wide amount of research material currently avail-
able and due to the worldwide availability of such plants. But,
these traditional coir products consume only a small percent-
age of the potential total world production of coconut husk.
4.2 Morphological analysis by SEM
As essential factor in polymer composites-based fibers is fiber
morphology and size. For this reason, the morphological prop-
erties of the coir fibers were investigated by scanning electron
microscopy (SEM), to monitor the effect of the chemical treat-
ment on structure changes of fiber. Contrasting for color of
fibers, there is no physical scale for measuring color other than
the visual comparison of color fibers appearances after the
chemical modifications. Generally, in a composite material,
the content and orientation of reinforcement fibers determine
the elastic properties. Similarly, natural fibers, the properties
of fibers are mainly determined by the chemical and physical
composition such as structure, cellulose percentage, micro
fibril angle, and degree of polymerization. Figure 3 a shows
the SEM micrograph of the untreated raw coir fiber. It is
clearly observed that the fibers are tubular with circular sec-
tion; an enlargement of single fiber shows that each fiber was
composed of microfibers. The fiber surface appears to be
smooth due to the presence of waxes and oil. However, the
presence of pores could be observed on the surface (Fig. 3b).
Though coir fiber has high lignin content, the moisture ab-
sorption capability is comparable with the other fibers. In or-
der to evaluate the effect of chemicals treatment on coir fiber
morphology. Some physical changes such as a rougher fiber
surface and the size of fibers can be observed in Fig. 3 a and c,
after the fiber undergoes the alkaline process. Figure 3 a
shows an untreated coir fiber bundle where the individual
fibers are bound together by lignin characterized with the nat-
ural waxy substances on the fiber surface and by a diameter of
82.86 μm. The alkali fibers depicted in Fig. 3 c have diameters
approximately 41.23 μm. The arrangement of cellulose fibers
within the matrix of lignin is clearly seen in this picture. The
removal of cementing materials, primarily lignin, from the
surface of the raw fiber occurs during this step. The diminu-
tion of fibers diameters is attributed to defibrillation of fiber
and to the removing surface impurities occurred by alkali
1922
Table 1 Chemical properties of
natural fibers [30] Fiber Cellulose
Kenaf 31–39
Bamboo 26–42
Coir 43
Sugarcane bagasse 50
Flax 71
treatment. The lignin gets depolymerized and dissolved, out at
this step which is evident from the chemical analysis. As a
result, defibrillation of the fiber occurs because of the removal
of the cementing materials. The micrographs show that
alkalization of fiber with NaOH is capable of elimination of
lignin and hemicelluloses, which is important to increase their
overall composite properties. As seen in Fig. 3 c, the chemical
treatment resulted in further defibrillation. The defibrillation
previously occurred during the alkali treatment process. The
fiber bundles were disintegrated into individual cells by the
use of alkali treatment and the diameter will be decreased until
the size of micro-fibrils. This phenomenon helps to facilitate
the chemical functionalization of coir fibers.
4.3 X-ray diffraction analysis
The crystallographic structure and chemical composition
of untreated, alkali-treated coir fibers were carried out by
XRD technique. The alkali treatments of coir fibers could
influence its chemical structure. The characteristic of main
peaks of cellulose at the 2θ of 15.8°, 17°, and 21.9° can be
observed (Fig. 4). These peaks are indicative of highly
organized crystalline cellulose [52]. The XRD pattern ob-
tained after alkali shows an increase in the cellulosic peaks
intensity at 2(θ) of 18° and 21.9°. From the figure a by
using the Eq. (1), it is clear that the raw coir fiber has
almost lower crystalline nature (C.I = 0.45 %) and the
crystallinity keeps on increasing gradually with processing
stages to reaches 73% by using alkali treatment. During
alkali treatment, the matrix materials react with sodium
hydroxide and get start to dissolve along with the forma-
tion of traces of the sodium salt of the cellulose. The steam
explosion will facilitate the ease of access of the alkali in to
the inner part of the raw coir by defibrillation of coir fiber
[52]. Besides, it will lead to the swelling of the fiber and
subsequent increase in the reacting surface area of the fi-
ber. Alkalization of coir fibers changes the surface topog-
raphy of the fibers and their crystallographic structure. The
lower crystallinity of the raw fiber reveals that each crys-
talline cellulose component embedded with amorphous lig-
nin components and upon the gradual removal of the lignin
by various treatments, the cellulose components tend to
form an ordered arrangement.
Int J Adv Manuf Technol (2021) 112:1917–1930
Hemicellulose Lignin Ash Waxes Density (g/cm3)
15–19 21 4.2 1.3 1.45
30 21–30 1.2 0.8 1.3
0.25 45 – 4 1.25
20 25 4.3 0.7 1.42
20.6 2.2 4.5 1.7 1.5
4.4 Fourier transforms infrared spectrometry
Fourier transforms infrared spectra (FT-IR) were employed to
study the chemical structure of coir fibers and the effects of
alkalization treatment on the fibers surface, and also to dem-
onstrate the chemical structure of the Bakelite matrix. Fourier
transform infrared spectroscopy (FTIR) of untreated and treat-
ed coir fibers were recorded using an ABB Bomem FTLA
2000-102 spectrometer (ATR: Specac Golden Gate). The
spectra were obtained with an accumulation of 16 scans with
a resolution of 4 cm-1. As presented in Fig. 5, the FTIR spec-
trums of untreated and treated coir fiber show a band at 3330
cm-1 corresponds to hydroxylic group (—OH ) [30, 53], an-
other band at 2900 cm-1 due to the ester bond, the transmit-
tance bands around 1650 cm-1, 1340 cm-1 corresponding to
the presence of lignin (C=C). Two more bands are the C—
O—C symmetric glycosidic stretch at 1100 cm-1 and the C—
OH stretching vibration of the cellulose backbone near 1050
cm-1 [33, 36, 54]. Alkali treatment shows a disappearing of the
C—O (carbonyl) band at 1729 cm-1 due to the removal of
reducible hemicelluloses found on the fibers surface. An
added band at 1230 cm-1 peak related to the C—O stretching
of the acetyl groups of lignin indicates that lignin is partially
removed from the coir fiber surface after the alkali treatment
[30, 33, 36, 55].
The IR spectra of Bakelite in the 4000–700 cm-1 range
were presented in the Fig. 5 b. The spectrum of the Bakelite
showed a band at 3267 cm-1, which corresponds to the vibra-
tion of the phenolic O–H bond [22]. The peaks at 3020 and
2918 cm-1 are attributed to the aromatic and aliphatic CH and
CH2-stretches, respectively [23]. The peaks at 1594 and 1504
cm-1 corresponded to the C=C aromatic ring vibrations [23].
The peaks at 1450 and 1370 cm-1 are associated to the scis-
soring vibration of -CH2-. The peak at 1229
cm-1corresponded to the C-O-C asymmetric stretch [22].
The peak at 1007 cm-1 corresponded to C-O stretching of
hydroxymethyl, while the peaks at 874, 808 and752 cm-1
belonged to the C-H out of plane vibrations [22, 23].
4.5 Thermal stability
Thermal degradation of natural fibers is a very important prop-
erty that must be controlled to the implementation of compos-
ite materials. It is well known that all the lignocellulose fibers
Int J Adv Manuf Technol (2021) 112:1917–1930 1923

Fig. 4 XRD analysis of untreated and treated coir fiber

Fig. 5 FTIR spectrum of (a) untreated and treated coir fibers; (b) Bakelite
Fig. 3 SEM pictures: (a, b) raw coir fiber, (c) alkali-treated coir fiber matrix
1924
are submitted to chemical and physical changes when heated
to a temperature range of 100–260 °C. Some of the physical
changes involved changes in the physical, structural, or chem-
ical structures such as dehydration, oxidation, recrystalliza-
tion, depolymerization, hydrolysis, and decarboxylation.
Figure 6 a and b shows the thermogravimetric analysis of
raw and treated coir fibers. The DTG curves indicate the de-
composition of untreated coir fibers as a three-step process,
Fig. 6b, indicate the presence of different components that
decompose at different temperatures. Due to the differences
in the chemical structures between lignin, cellulose, and hemi-
cellulose, they usually decompose at different temperatures.
The first process at about 290 °C is due to the thermal degra-
dation of hemicellulose. The strong second peak at about 320
°C indicates the degradation of cellulose, leading to the for-
mation of flammable volatiles and char products, while the
third small peak at 437 °C is attributed to the lignin degrada-
tion. In the other hand, it was examined that alkali-treated coir
fibers degrading displayed higher thermal stability. Also, the
percentage of the solid residue left after the degradation of the
raw coir is higher than the percentage weight of the solid
Fig. 6 a TGA of untreated and treated coir fiber and b DTG of untreated
and treated coir fiber
Int J Adv Manuf Technol (2021) 112:1917–1930
residue left after the pyrolysis of the nanocellulose which is
extracted from coir fiber. Degree of polymerization of hemi-
cellulose and lignin is very low when compared with cellu-
lose. The higher amount of residual char for raw coir fiber is
due to the strong cellulose–lignin complex and the aromatic
nature of the lignin complexes. This was evidenced by the
degradation rate of the treated coir fibers with higher temper-
ature and by lowering the weight loss compared to the untreat-
ed fibers. The presence of other macromolecules (hemicellu-
lose, lignin) which decomposed at low temperatures help to
cause early onset of degradation of the fiber; the alkali treat-
ment reduces the hemicelluloses and lignin content of the
fibers. As a result, fibers became more thermally stable and
reach a high temperature during the compounding process.
The natural fibers are a subjected to degradation during com-
posite processing. The thermal degradation of the coir fibers
(which is a critical feature for their application as filler or
reinforcement) is increased to a high level by alkali treatment.
4.6 Thermal conductivity
Thermal conductivity is one of the key parameters in the field
of thermal insulation materials.
Thermal conductivity of the materials directly influ-
ences the efficiency of energy transport, and the mate-
rials’ resistance to thermal stress and thermal shock.
Since the thermal conductivity of a composite depends
on its component materials and the arrangement of the
materials, it is possible to optimize the property through
constitutional and structural design. Typical curves of
temperature versus time for Bakelite composites at 10
and 20 wt.% fibers content are presented in Fig. 7.
Figure 8 shows that the thermal conductivity of composites
decreases with the addition of alkali-treated coir fiber. The
values of temperature decrease of 54.4 °C and 52.17 °C in
900 s in the case of composites at 10 wt.% and 20 wt.% fiber
Fig. 7 Variation of thermal conductivity as function with fiber loading
Int J Adv Manuf Technol (2021) 112:1917–1930
Fig. 8 a Flexural stress vs flexural strain curves. b Flexural stress at break
and total energy. c Stress and strain at break as function of coir fiber
loading
content, respectively. Accordingly, there is a remarkable de-
crease in the thermal conductivity of the composites and their
slops by adding the coir fibers, this is due to the thermal
contact resistance between the thermal insulators matrix
(Bakelite) and the thermal conductor’s fibers [26]. During
the alkali treatment, the impurity and waxes on the coir fibers
surface are removed, which increases the number of pores on
the fibers surface. These pores are zones of attachment of the
polymeric chains and hence reduce the percentage of areas of
voids between the fibers and the matrix (good interfacial ad-
hesion) on the composite structure [56].The good
1925
compatibility, better dispersion/distribution, and the high in-
terfacial adhesion, created by chemical modification of coir
fibers, in which the fiber-Bakelite interfacial adhesion acts as a
barrier to prevent the thermal conduction and makes the com-
posite more insulating.
4.7 Composites density
Density has a major role in determining the dimensional sta-
bility of the composites that are produced. Therefore, deter-
mining the percentage of porosity makes it possible to evalu-
ate the quality of the composite. Table 2 summarizes the the-
oretical and experimental density of different manufactured
composites. From Table 2, it is clear a decreased theoretical
density with adding coir fibers from 1.423 g/cm3 in case of
composites with 5 wt.% to 1.391 g/cm3 for composites at 30
wt.% of fibers. That is due to the lower density of coir fibers in
comparison with Bakelite matrix. By substitution of amount
of Bakelite by coir fibers, it is normal that the density
decreased.
However, by comparing the experimental results and the
theoretical ones, it is clear that the experimental density is
highest. It is known that a low-density composite is a material
that is able to trap more moisture and hold more water than
high-density composites. The reason is that low-density com-
posites have more voids, porosities, and spaces within the
composite’s components [56]. In the theoretical measurement,
the two parameters are the intrinsic density of compounds and
the weight fraction; however, in experimental measurement,
the interfacial adhesion (porosity, voids) is a determinant key.
In our case, the reason of using alkali treatment is that treat-
ment allows the removal of non-cellulosic compounds from
the surface of coir fibers, which improves interfacial adhesion
and increases resin penetration by reducing the void percent-
age on the structure of the composites[30, 38, 55], and that
explained the fact that the experimental density is highest that
the theoretical one because there is a high interfacial adhesion.
In the other hand, by watching the experimental results, it is
clear there are two trends of evolution; the first step, the den-
sity increases with coir fiber to reach a maximum at 10 wt.%
and the second step the density decrease. This evolution on the
Table 2 The experimental and theorical density of different composites
Specimens Exp density Theo density
Bakelite 1.46 1.43
Coir fibers 1.31 1.29
5 1.5021 1.423
10 1.4819 1.417
20 1.4482 1.404
30 1.4216 1.391
1926
experimental density is related to two effect, the first one is the
difference on the intrinsic density between coir fiber and
Bakelite. The second fact is related to the affinity and interfa-
cial adhesion between two phases. At low fiber content, there
is a good dispersion/distribution of fibers into matrix allowing
a good interfacial, while above 10 wt.%, the fiber-fiber inter-
action take place leading to formation of agglomeration and
the interfacial adhesion becomes bad giving birth to cavitation
and voids between fibers and matrix and in final affect the
density which decreased.
4.8 Flexural test
The flexural property is one of the important parameters in
composites mainly useful to quantify in structural applica-
tions. The flexural properties and stored energy were evaluat-
ed by integration under stress-strain curves (Fig. 8a), to extract
the flexural modulus, flexural stress, and flexural strain and by
exploiting the area under curves to calculate the total energy.
Figure 8 b illustrates the flexural modulus when varying the
fiber content in the composite. As seen in this figure, the
incorporation of fibers has resulted on linear increase in the
flexural modulus of the composites. The flexural modulus
decreased from a value of 7.6 GPa for an unfilled matrix to
a minimum value of 8.22GPa for a 30 wt. % coco fibers
composite; this corresponds to an 8.15%, increase in flexural
modulus. This increase is due essentially to the intrinsic prop-
erties of coco fibers which increased the stiffness of the com-
posites by giving it stiffer and fragile character to the Bakelite
matrix [53, 54, 57].
A study of the total energy absorbed by the composites has
shown the effects of fiber content. Figure 8 b shows an in-
crease in total energy of composites with increasing fiber load-
ing, reaching 48.48 % increase sat 30 wt. % coir fibers rein-
forcement, which is attributed to the fragile character of the
added coir fiber when compared to neat Bakelite [58, 59].The
combined effect between the stiffness character of fibers and
the good interfacial adhesion by the creation of hydroxyl
bonding give to the composites a good resistance to the flex-
ural stress, which is confirmed by the stabilization of the flex-
ural stress at break in Fig. 9 b. The fracture of the composites
requires a lot of energy by adding coir fibers [59].
The ductility of the various composites was evaluated also
through the plastic energy. It was observed in Table 2 that
with the incorporation of coir fiber, the absorbed plastic ener-
gy by the composites decreased until a maximum at 30 wt.%
coconut content, contrary to elastic energy which increase
with fibers addition. The presence of fibers into matrix with
their fragile character limits the plasticity compared to elastic-
ity behavior [60]. In the composites, the fragile behavior dom-
inates the plastic behavior, leading to a higher elastic’s energy
compared the plastics energy and thus stored more elastics
energy in the composite material with adding coir fibers.
Int J Adv Manuf Technol (2021) 112:1917–1930
The flexural stress and strain at break curves of composites
are presented in Fig. 8 c, the figure show that with the incorpo-
ration of coir fiber, the flexural stress at break, and the flexural
strain at break decreased until an optimum at 30 wt.%. The
flexural stress at break decrease slightly from 60 to 58.5 MPa
at 10 wt.% (loss of 2.8%) and then the trend is stable until 30
wt.% of coir fiber. This stabilization of the flexural stress at
break means a good interfacial adhesion between fiber and
Bakelite matrix. This stabilization is due essentially to the
Alkali treatment which improves the interfacial adhesion of
the fiber with the matrix and allows the resin to penetrate the
fiber bundle during the manufacturing process. The removal of
waxes and non-cellulosic compounds during the treatment ex-
poses hydroxyl groups on the coir fibers surface and promotes
interfacial bonding between the fiber surface and the Bakelite
resin matrix. This interaction has a positive effect on the bend-
ing properties of composites by increasing the stress transfer
capacity of the matrix to the fiber via interfacial adhesion [56,
61]. On the other hand, Fig. 8 c shows a slight decrease in the
flexural strain at break; this is due to the decreased in ductility
of the composites by increasing the brittle (fragile) character on
the matrix by coir fibers. Also, the creation of a strong chemical
bonding between fibers and matrix especially the hydroxyl
bonding gives the composites some stiffness [62–64].
The toughness value related to the area under the stress-
strain curve corresponds to the fracture energy per unit of
sample volume. From Table 3, toughness value was found
decreased by increasing fibers content. The change on the
fracture toughness can be attributed to interfacial interaction
of fiber and matrix and the dispersion/distribution of fiber into
matrix, as well as the absorbed energy when the fibers pulled
out from Bakelite matrix in the bending test. In our case, by
increasing fibers, the interfacial adhesion increases until a
maximum and then the fiber-fiber interaction takes place to
create agglomeration leading to decreased properties [33, 56].
On the basis of the above experimental comparison, we came
to the following conclusions. Adding coir fibers with a larger
diameter can improve flexural modulus and energy absorption
capacity, but it cannot improve the ductility of the composites.
4.9 Dynamic mechanical analysis
It is possible to evaluate the changes in molecular relaxations
and that occur in Bakelite composites in a wide temperature
range using DMTA. Figure 9 a shows that the addition of fibers
and variation of temperature changes the complex modulus
(E*) values of composite. The modulus of Bakelite/ coir fiber
composites, especially at low temperature, is affected by the
content of coir fibers used. At 40 °C temperature, the E*of
Bakelite-coir fiber composites decrease as concentration of fi-
bers increased; this is due to the decrease in the wettability of
the fibers within the matrix[65]. The complex modulus of
Bakelite-coir fiber composites filled by 5 wt.% composites
Int J Adv Manuf Technol (2021) 112:1917–1930 1927

Fig. 9 DMA curves of Bakelite

and composites as function of
temperature. a Complex modulus
(E*). b Loss factor (Tan δ)

showed an increased by 48.75% as compared to neat Bakelite surface interaction between the fibers and the matrix that act as
matrix at 40 °C. The modulus increased due to high modulus of internal link and restricts the segmental motion of the Bakelite
coir fibers and due to the good dispersion-distribution and good molecules. Thus, the curves show a decrease in complex mod-
ulus with increases the temperature, which can be related to the
softening of materials led to the enhance the ability of the
Table 3 Total energy as function of fiber loading
matrix chains to move freely [66].
The loss factor (tan δ) is the ratio of the loss modulus (E”)
Samples Wt (J/m3) We (J/m3) Wp (J/m3) Wp/ and the storage modulus (E’). Figure 9 b illustrates the evolu-
We
tion of the tan δ versus temperature and fiber loading. It shows
0% 20.77 15.11 5.66 0.374 that the tang δ values decrease with increasing fiber loading;
5% 23.48 18.39 5.09 0.276 for example, in the case of the composites at 30wt.% coir fiber
10% 25.31 20.36 4.95 0.243
loading, the value is about 8% lower than that of neat matrix.
20% 29.83 25.81 4.02 0.155
Plasticizing effect of fiber reduces the amount of dragging
30% 30.84 27.01 3.83 0.141
force for plastic flow of the materials which ultimately reduces
the tan δ values. However, an increase in temperature changes
1928
the tan δ curve to higher values. The increase in the free
volume with temperature results in movement of large seg-
ments of the molecular chain over the polymer backbone until
the reach of a Bakelite composite rubbery state, the movement
of chains segments become slaky [30, 67], leading to decrease
the interfacial interaction between the matrix and fibers that
lessen the effective stress transfer from the matrix to the fiber
[53, 54].
5 Conclusion
In this paper, we present a new approach by introducing short
alkali coir fiber as reinforcing fillers in phenolic resin
(Bakelite). For exploration of synergistic effect between in-
trinsic character of fibers and chemical modification of short
coir fiber, the thermal, mechanical, and rheological properties
of Bakelite composites were comparatively studied in pres-
ence of neat Bakelite as matrix. The measurement of density
shows a significant change by adding coir fibers. Thermal
conductivity exposed that addition of coir fibers increases
the thermal insulation of the composites despite the thermal
conductivity of coir fibers; the reduction of voids on the struc-
ture of the composites leads to a decrease in their thermal
conductivity. Both flexural modulus and total energy (absorp-
tion capacity) of composites get enhanced by the addition of
coir fibers; however, 30wt.% fiber loading shows better im-
provement compared to the rest of composites, ascribed on the
basis of better dispersion, wetting of fibers, and interfacial
bonding between fibers and Bakelite. Dynamic mechanical
analysis showed the effect of temperature and fibers loading,
on the complex modulus (E*) and damping factor (tan d)
values of the composites. The result show that the variation
of temperature and the incorporation of fibers loading en-
hances the damping factor and lessen the complex modulus
values. In summary, on the basis of the present study, alkali-
treated coir fiber and Bakelite composite will provide a
pioneering way on the development of natural fiber-based
phenolic resin technology and engineering.
Author contribution Hala Bensalah wrote the manuscript and carried out
the experiments with support from Marya Raji.
Marya Raji fabricated the sample and contribute to the interpretation of
mechanical results.
Hind Abdellaoui discussed the results and contributed to the final
manuscript.
Hamid Essabir conceived and planned the experiments, verified and
discussed the results, and helped supervise the project.
Rachid Bouhfid and Abou el kacem Qaiss conceived and planned the
experiments, conceived the original idea, helped supervise the project,
and contributed to the final manuscript.
Data availability The authors confirm that the data supporting the find-
ings of this study are available within the article [and/or] its supplemen-
tary materials.
Int J Adv Manuf Technol (2021) 112:1917–1930
Compliance with ethical standards
Ethical approval This research does not deal with human subjects, so
we do not need an ethical approval.
Consent to participate This research does not deal with human subjects,
so we do not need informed consent to participate.
Consent to publish This statement is to certify that all authors have seen
and approved the manuscript being submitted. We warrant that the article
is the authors’ original work. We warrant that the article has not received
prior publication and is not under consideration for publication elsewhere.
On behalf of all co-authors, the corresponding author shall bear full re-
sponsibility for the submission.
Conflict of interest The authors declare that they have no conflict of
interest.
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Affiliations
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2 Sciences of Agadir, Ibn Zohr University, Agadir, Morocco
Composites and Nanocomposites Center, Moroccan Foundation for
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