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Accepted Manuscript

Effect of addition of areca fine fibers on the mechanical properties of Calotropis


Gigantea fiber/phenol formaldehyde biocomposites

S. Venkatarajan, B. V.Bhuvaneswari, A. Athijayamani, S. Sekar

PII: S0042-207X(18)31288-0
DOI: https://doi.org/10.1016/j.vacuum.2019.04.022
Reference: VAC 8663

To appear in: Vacuum

Received Date: 28 November 2018


Revised Date: 9 April 2019
Accepted Date: 12 April 2019

Please cite this article as: Venkatarajan S, V.Bhuvaneswari B, Athijayamani A, Sekar S, Effect
of addition of areca fine fibers on the mechanical properties of Calotropis Gigantea fiber/phenol
formaldehyde biocomposites, Vacuum (2019), doi: https://doi.org/10.1016/j.vacuum.2019.04.022.

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ACCEPTED MANUSCRIPT

Effect of addition of Areca fine fibers on the mechanical properties of Calotropis Gigantea
fiber/phenol formaldehyde biocomposites
S.Venkatarajana, B.V.Bhuvaneswaria, A.Athijayamanib, S.Sekarc
a
Department of Physics, A.C.G.C.E.T, Karaikudi-630 003, Tamilnadu, India
b
Department of Mechanical Engineering, G.C.E, Bodinayakanur-625 582, Tamilnadu, India

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c
Department of Mechanical Engineering, H.I.T, Coimbatore-641 032, Tamilnadu, India

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ABSTRACT
The present investigation is carried out to understand the effects of addition of Areca Fine

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Fibers (AFFs) with the Calotropis Gigantea Fiber (CGF) / Phenol formaldehyde (PF)
biocomposite. For that, the hybrid composites are prepared with Glass Fibers (GFs) to evaluate
and compare their mechanical properties. The CGF/AFF/PF hybrid composites are prepared with

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the total weight percentages of 25, 35 and 45%. Hybrid composite having 35 wt% showed the
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better mechanical properties as compared to the other (25 and 45 wt%) hybrid composites. The
GFs are hybridized for comparative study with the CG and AF fibers in PF composites. The
CGF/GF/PF and AFF/GF/PF hybrid composites are prepared with the weight percentage of 35
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wt% in 1:1 ratio. The mechanical properties of hybrid composites are evaluated and compared.
The CGF/AFF/PF hybrid composites showed the maximum level of mechanical properties when
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compared with the CGF/GF/PF and AFF/GF/PF hybrid composites. But, it shows the lower level
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of mechanical properties compared to the GF/PF (35 wt%) composites. Furthermore, it is proved
that the CGF/AFF/PF hybrid composites can be used in any structural application instead of the
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GF/PF composites.
Keywords: Polymer-matrix composite, Areca fine fiber, Calotropis Gigantea fiber, Glass fiber,
Mechanical Properties, Scanning Electron Microscopy
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1. Introduction
Recently, the fiber-reinforced polymer composites play a vital role in the various fields of
engineering applications. Fiber-reinforced polymer composite materials are a composite material
which consists of fiber with the high strength and modulus surrounded in or bonded to a polymer
matrix with dissimilar interfaces between them. Both the fiber and the polymer matrix hold their

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physical and chemical identities and produce a combination of properties that cannot be achieved
with either of the materials acting alone. In fiber-reinforced polymer composites, fibers are the

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principal load-carrying element, while the polymer matrix keeps the fibers in the desired location
and orientation, acts as an applied load transfer medium between them, and protects the fibers

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from environmental damages [1-3].
Even though natural cellulose fibers are the most widely reinforcements used in the

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polymer composites for their high specific strength and stiffness, corrosion resistance and low
cost, the advantages of the natural fiber are significantly reduced because of its weakness to the
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overall combination of the physical and mechanical properties and especially to impact damage.
With the purpose of improving the properties of natural fiber-reinforced polymer composites,
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several approaches have been taken by numerous researchers to improve the physical and
mechanical properties of natural fiber-reinforced polymer composites [4-6]. One of the important
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possible ways is the fiber hybridization by combining two or more different types of fibers
(natural/natural or natural/synthetic) in a common polymer matrix to get a collection of
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properties that cannot be obtained in a polymer composite with a single kind of reinforcement.
Therefore, in recent years, the preparation of natural fiber-reinforced polymer hybrid composites
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and evaluation of their performances have been carried out by several authors (7-9) to obtain
materials with sufficient physical and mechanical properties. Gupta & Srivastava (2016) stated
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that the incorporation of two or more fibers into a single polymer matrix leads the development
of hybrid composite. Hybridization can improve the mechanical properties of single fiber-
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reinforced polymer composite. They also stated that mechanical properties of natural fiber-
reinforced polymer composite increase due to incorporation of comparably high elongation
fibers (10). Sathish et al. (2018) prepared the epoxy hybrid composites with sisal, kenaf, flax
and pineapple fibers by compression molding techniques and characterized based on their
mechanical properties such as tensile, flexural and impact. The authors found that the flax / kenaf
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/ epoxy composite shows better tensile, impact and flexural strength compared to other hybrid
composites (11).
Present paper deals with the developments of the plant based natural fiber-reinforced
polymer hybrid composites made by hand lay-up methods. The hybridization of natural/natural
(12) and natural/synthetic fiber (13) reinforced polymer matrix hybrid composites has been

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developed to build their applications in the field of automobiles, aerospace, structural, house
holding appliances, etc. Very few literatures are available in the combination of Areca fine fibers

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and Calotropis Gigantea fibers. Therefore, this investigation is taken to understand the effects of
addition of Areca Fine Fibers (AFFs) with the Calotropis Gigantea Fiber (CGF) / Phenol

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formaldehyde (PF) biocomposite. For that, the hybrid composites are prepared with Glass Fibers
(GFs) to evaluate and compare their mechanical properties.

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2. Experimental details
2.1. Materials
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The CGFs were extracted from the stem of the plant manually and cut into three different
lengths 3, 9 and 15 mm for the use as a reinforcement agent for phenol formaldehyde resin
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matrix. The resole type Phenol Formaldehyde (PF) liquid resin with the density of 1.3 g/cm3 and
specific gravity of 1.14 (g/cm3 at 25°C) was used as a polymer matrix with the cross-linking agent
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(divinylbenzene) and acidic catalyst (hydrochloric acid). All the chemicals are procured from the
POOJA Chemicals (Satyen Polymers Pvt. Ltd, Bangalore) Madurai, Tamilnadu, India.
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2.2. Fabrication of composites


Composite plates were prepared using hand lay-up technique by a mould with the
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size of 150 × 150 × 3 mm (14). First, poly vinyl alcohol as a releasing agent was applied on the
inner side of the mould to ensure easy removal of cured composite plates. Then, the fibers in a
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calculated amount are mixed with PF resin and stirred by a mechanical stirrer for 30 min. After
that, the cross-linking agent (divinylbenzene) and acidic catalyst (hydrochloric acid) are added to
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the mixture of the fibers and PF resin with a ratio of 2:1.5:100 and again stirred by a mechanical
stirrer for 15 min. The mixture is poured into the mould and pressed using a laboratory hot press
of 150oC. Finally, the mould box containing the composite plate was allowed to cure at room
temperature under atmospheric pressure for 48 hours. The digital images of fabricated CGF/PF
and CGF/AFF/PF hybrid composite specimens are given in Figs. 1 and 2.
Fig.1. Digital image of fabricated CGF/PF composite specimens
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Fig.2. Digital image of fabricated CGF/AFF/PF hybrid composite specimens

2.3. Mechanical testing


For mechanical tests, composite specimens with the size of 150 × 20 × 3 mm are
cut from the prepared composite plates. Tensile tests are performed according to ASTM D638-10

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on an FIE (Fuel Instruments &Engineers) universal testing machine (model: UTE-10) at a
crosshead speed of 2 mm/min in room temperature and humidity of 50%. Flexural tests are also
conducted on same FIE universal testing machine at same condition. Izod impact tests are

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conducted on TO (Tinius Olsen) impact tester (model: IT503&504) according to ISO180:2000 at
room temperature and humidity of 50%. The test procedures for the determination of tensile,

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flexural and impact property values using universal testing machine, and impact tester are given
in Fig.3. Totally, five specimens were tested for each combination to obtain the average value

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Fig.3. Schematic diagram of the producers used by the mechanical testing equipments in
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the present investigation: (a) tensile test, (b) flexural (three point bending) test, and (c) impact
test
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2.4. Fractographic study


The microstructure of the fracture surface of composite specimens after
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mechanical tests was taken by scanning electron microscope (HITACHI N-3000S) and examined
to identify the mode of failure.
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3. Results and discussion


3.1. Tensile properties
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Fig.4 illustrated the tensile properties of neat phenol formaldehyde and the CGF/AFF/PF
hybrid composite. It is observed that the tensile properties of hybrid CGF/AFF/PF composite are
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increased up-to 35 wt% and then decreased. The decreasing tendency of hybrid composite after
35 wt% may be due to poor adhesion between hybrid fibers and resin matrix. The hybrid
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composite CGF17.5/AFF17.5 shows the maximum value of tensile strength (58.9 MPa) and
tensile modulus (1298.3 MPa). This maximum value of tensile strength and modulus may be due
to strong interfacial adhesion between the fibers and the matrix, and minimum numbers of voids
present in the hybrid composite. The tensile strength of CGF17.5/AFF17.5 hybrid composite is
found to be improved by 105.8%, 41.2% and 17.1% as compared to neat phenol formaldehyde,
CGF12.5/AFF12.5, and CGF22.5/AFF22.5 composite respectively. Similarly,
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CGF17.5/AFF17.5 hybrid composite shows 16.71%, 5.63% and 3.71% of the improvement in
tensile modulus as compared to neat phenol formaldehyde, CGF12.5/AFF12.5, and
CGF22.5/AFF22.5 hybrid composite. Fracture surface of the CG/AF/PF hybrid composite after
tensile test is examined by scanning electron microscope. SEM image (Fig.5) showed the
fracture of the fibers and matrix de-bonding after the tensile test. The voids and fiber pull-out are

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also identified on the fractured surface of the hybrid composite (CGF17.5/AFF17.5) (15).
Fig.4. Variations of the tensile properties of neat PF and the CGF/AFF/PF hybrid composite

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Fig.5. SEM image of the fractured surface of CGF17.5/AFF17.5 hybrid composite after tensile
test

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3.2. Flexural properties
The flexural properties of the phenol formaldehyde and the CGF/AFF/PF hybrid

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composite are presented in Fig.6. The flexural properties of hybrid composite are also found to
be increased up-to 35 wt. % and then started to decrease. The maximum value of flexural
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properties is identified at CGF17.5/AFF17.5 hybrid composite, i.e., the maximum value of
flexural strength (73.1MPa) and flexural modulus (1346.7 MPa). The flexural strength of
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CGF17.5/AFF17.5 hybrid composite is 130.6% higher than the neat resin sample. The flexural
strength of CGF17.5/AFF17.5 hybrid composite is found to improve by 27.35% and 18.48% as
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compared to CGF12.5/AFF12.5, and CGF22.5/AFF22.5 hybrid composites respectively. The


flexural modulus of CG17.5/AF 17.5 hybrid composite is found improved by 4.52%, and 6.53%
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as compared to CGF12.5/AFF12.5, and CGF22.5/AFF22.5 hybrid composites respectively. It is


observed from the SEM image (Fig.7) that the fiber breakage is not the more brittle manner due
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to the applied load. The fiber de-bonding and pull out are also identified. It may be due to the
poor interfacial adhesion between the fiber and the resin matrix (15).
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Fig.6. Variations of the flexural properties of neat PF and the CGF/AFF/PF hybrid composite
Fig.7. SEM image of a fractured surface of CGF/AFF/PF hybrid composite (CG17.5/AF 17.5)
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3.3. Impact strength

The effect of addition of AF fibers on the impact strength of CG fiber reinforced phenol
formaldehyde composites is shown in Fig. 8. From the Fig. 8, it is observed that the impact
strength of CGF17.5/AFF17.5 hybrid composite was higher as compared to other hybrid
composites. The CGF17.5/AFF17.5 hybrid composite shows 23.68% increase in the impact
strength as compared to the neat resin sample and 4.44% and 2.29% increase in impact strength
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with that of CGF22.5/AFF22.5 hybrid composite and CGF12.5/AFF12.5 hybrid composite. The
impact strength of CGF17.5/AFF17.5 hybrid composite is higher because the interfacial
adhesion at CGF17.5/AFF17.5 hybrid composite is higher and it behaves like better load
carrying material to resist the applied impact load. The inclusion of AF fibers significantly
enhanced the mechanical properties of the CGF/PF composites (16).

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Fig. 8. Variations of the impact strength of neat PF and the CGF/AFF/PF hybrid composite

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3.4. Comparison of hybrid composites
For comparative study, the Glass Fibers (GFs) are hybridized with the CG and AF fibers

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in PF composites. The CGF/GF and AFF/GF hybrid composites are prepared by total of 35 wt%
at 1:1 ratio (17.5:17.5 wt%) using hand lay-up technique. Because of CGF/AFF/PF hybrid
composites showed the maximum mechanical properties at 35 wt% (CGF17.5/AFF17.5).

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Moreover, the GFs are also reinforced with the PF resin matrix for the comparative study (Fig.
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9). Composites prepared for comparative study are subjected to mechanical characterization and
their mechanical properties are analyzed and compared. The results revealed that the CGF/AFF
fiber-reinforced phenol formaldehyde hybrid composites exhibited better mechanical properties
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than the CGF/GF/PF hybrid composites and AFF/Glass/PF hybrid composites. But, the
CGF/AFF/PF hybrid composites showed the lower mechanical properties as compared to the
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GF/PF composites. The AF fibers contain a fairly higher proportion of stiff natural cellulose than
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the CG fibers. The mechanical properties of CGF/AFF/PF hybrid composites tend to be inhibited
by the cellulose content and micro fibril angle and also fiber composition. From health point of
view, the CGF/AFF/PF hybrid composites are comparatively better than CGF/GF/PF hybrid
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composites, AFF/GF/PF hybrid composites, and GF/PF composites.


Fig.9. Digital image of prepared CGF/GF/PF and GF/PF hybrid composites
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3.5. Tensile properties


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Fig.10 shows the variations of tensile properties for CGF/GF/PF, AFF/GF/PF,


CGF/AFF/PF and GF/PF composites. The results showed that the CGF/AFF/PF hybrid
composite showed better tensile strength (58.9 MPa) than the CGF/GF/PF (51.7 MPa) and
AFF/GF/PF (54.7 MPa) hybrid composites. The CGF/AF/PF hybrid composite showed 13.9%
and 8.67% of improvement compared to the CGF/GF/PF and AFF/GF/PF hybrid composites
respectively. The tensile of strength value of CGF/AF/PF hybrid composite is 21.04% lower than
the GF/PF composite. The tensile modulus value of CGF/AF/PF hybrid composite is also higher
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than the CGF/GF/PF and AFF/GF/PF hybrid composites and lower than the GF/PF composite. It
is observed that the CGF/GF/PF hybrid composite showed the lowest tensile properties as
compared to the other hybrid composites. It may be due to the poor interfacial bonding between
the fibers and the matrix. The poor interfacial bonding leads to the fiber breakage due to the
applied load, followed by the fiber pullout (16), as shown in Fig.11.

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Fig.10. Variations of the tensile properties of hybrid composites
Fig.11. SEM image of a fractured surface of the CGF/GF/PF hybrid composite (35 wt%) after

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the tensile test
3.6. Flexural properties

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Fig.12 shows the effect of reinforcements of glass fiber addition on the mechanical
properties of CGF and AFF hybrid composites. From the results it is observed that the

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CGF/AFF/PF hybrid composite showed better flexural properties than the CGF/GF/PF and
AFF/GF/PF hybrid composites. All hybrid composites show the lowest level of flexural
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properties as compared to the GF/PF composite. The CGF/AFF/PF hybrid composite showed
higher flexural strength than CGF/GF/PF and AFF/GF/PF hybrid composites, i.e., the
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improvement of 16.4% and 8.13%, respectively. The flexural strength of the CGF/AFF/PF
hybrid composite was found out to be a decrease of 17.31 %, when compared to the GF/PF
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composite. The CGF/AFF/PF hybrid composite shows 8.77% increase in the flexural modulus as
compared to the CGF/GF/PF hybrid composite and 4.04% increase in the flexural modulus with
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that of the AFF/GF/PF hybrid composite. The fiber fracture and pullout are identified due to the
de-bonding of the fiber from the resin matrix, which leads to the poor transfer of applied load
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from the matrix to the fiber (Fig. 13) (16). Therefore, the CGF/GF/PF hybrid composites showed
the lowest level of flexural properties compared to the CGF/AFF/PF hybrid composites.
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Fig.12. Variations of the flexural properties of hybrid composites


Fig.13. SEM image of a fractured surface of the CGF/GF/PF hybrid composite (35 wt%) after
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the flexural test


3.7. Impact strength
The variation of impact strength of hybrid composites and GF/PF composite is shown in
Fig. 14. The impact strength of CGF/AFF/PF hybrid composite is higher as compared to other
two hybrid composites. The CGF/AFF/PF hybrid composite shows 6.8% increase in the impact
strength as compared to CGF/GF/PF hybrid composite and 3.68% increase in the impact strength
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with that of AFF/GF/PF hybrid composite. But, the impact strength of CGF/AFF/PF hybrid
composite is also lower as compared to the GF/PF composite. The brittle fracture of the fibers is
observed in the SEM image of a fractured surface of the CGF/AFF/PF hybrid composite (35
wt%), as shown Fig. 15. It may be due to the better interfacial bonding between the fiber and the
matrix.

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Fig. 14. Variations of the impact strength of hybrid composites
Fig. 15. SEM image of a fractured surface of the CGF/AFF/PF hybrid composite after impact

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test
From the comparative study, it is observed that the CGF/AFF/PF hybrid composites are

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comparatively better than CGF/GF/PF hybrid composites, AFF/GF/PF hybrid composites, and
GF/PF composites. The CGF/AFF/PF hybrid composites can be used in the various fields of

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engineering and structural applications instead of GF/PF composites.
4. Conclusion
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The CG and AF fiber- reinforced phenol formaldehyde hybrid composites have been
fabricated by hand lay-up method and their mechanical properties like tensile, flexural and
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impact strength as per ASTM standards has been evaluated. Composite having the CG fiber
content of 17.5 wt% and the AF fiber content of 17.5 wt% shows the higher tensile properties
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than the other hybrid composites. The flexural properties have been studied as per fiber loading
and observed that the maximum level flexural strength and modulus values are obtained at
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CG17.5/AF17.5 hybrid composite. The impact strength is also reaching the higher value at
hybrid composite having the designation of CG17.5/AF17.5. Finally, it is observed that the
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CG17.5/AF17.5 hybrid composite showed better mechanical properties than the other hybrid
composites. It is proved that the interfacial bonding between the fibers and the matrix at
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CG17.5/AF17.5 hybrid composite is higher than the other hybrid composites. The addition of AF
fibers significantly enhanced the tensile, flexural and impact properties of CG/PF composites. In
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comparative studies, CGF17.5/AFF17.5 hybrid composite shows better mechanical properties


than the CGF17.5/GF17.5 and AFF17.5/GF17.5 hybrid composites. But, this hybrid composite
can be used instead of GF/PF composites in the various fields of engineering applications. In
future, the strength values of this hybrid composite can be further increased by the chemical
modification of both the reinforcements and the matrix.
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Figure Captions

Fig.1. Digital image of fabricated CGF/PF composite specimens


Fig.2. Digital image of fabricated CGF/AFF/PF hybrid composite specimens
Fig. Error! No text of specified style in document.. Schematic diagram of the producers used by

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the mechanical testing equipments in the present investigation: (a) tensile test, (b) flexural (three
point bending) test, and (c) impact test
Fig.4. Variations of the tensile properties of neat PF and the CGF/AFF/PF hybrid composite

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Fig.5. SEM image of the fractured surface of CGF17.5/AFF17.5 hybrid composite after tensile
test

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Fig.6. Variations of the flexural properties of neat PF and the CGF/AFF/PF hybrid composite
Fig.7. SEM image of a fractured surface of CGF/AFF/PF hybrid composite (CG17.5/AF 17.5)

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Fig. 8. Variations of the impact strength of neat PF and the CGF/AFF/PF hybrid composite
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Fig.9. Digital image of prepared CGF/GF/PF and GF/PF hybrid composites
Fig.10. Variations of the tensile properties of hybrid composites
Fig.11. SEM image of a fractured surface of the CGF/GF/PF hybrid composite (35 wt%) after
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the tensile test


Fig.12. Variations of the flexural properties of hybrid composites
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Fig.13. SEM image of a fractured surface of the CGF/GF/PF hybrid composite (35 wt%) after
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the flexural test


Fig. 14. Variations of the impact strength of hybrid composites
Fig. 15. SEM image of a fractured surface of the CGF/AFF/PF hybrid composite after impact
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test
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Fig.1. Digital image of fabricated CGF/PF composite specimens

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Fig.2. Digital image of fabricated CGF/AFF/PF hybrid composite specimens

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(a) (b) (c)

Fig. Error! No text of specified style in document.. Schematic diagram of the producers used by
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the mechanical testing equipments in the present investigation: (a) tensile test, (b) flexural (three
point bending) test, and (c) impact test
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Fig.4. Variations of the tensile properties of neat PF and the CGF/AFF/PF hybrid composite

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Fig.5. SEM image of the fractured surface of CGF17.5/AFF17.5 hybrid composite after tensile
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test
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Fig.6. Variations of the flexural properties of neat PF and the CGF/AFF/PF hybrid composite
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Fig.7. SEM image of a fractured surface of CGF/AFF/PF hybrid composite (CG17.5/AF 17.5)

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Fig. 8. Variations of the impact strength of neat PF and the CGF/AFF/PF hybrid composite
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Fig.9. Digital image of prepared CGF/GF/PF and GF/PF hybrid composites


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Fig.10. Variations of the tensile properties of hybrid composites

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Fig.11. SEM image of a fractured surface of the CGF/GF/PF hybrid composite (35 wt%) after
the tensile test
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Fig.12. Variations of the flexural properties of hybrid composites


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Fig.13. SEM image of a fractured surface of the CGF/GF/PF hybrid composite (35 wt%) after

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the flexural test

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Fig. 14. Variations of the impact strength of hybrid composites


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Fig. 15. SEM image of a fractured surface of the CGF/AFF/PF hybrid composite after impact
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The developments of the plant based natural cellulose fiber-reinforced polymer hybrid
biocomposites made by hand lay-up methods.

To understand the effects of addition of Areca Fine Fibers (AFFs) with the Calotropis Gigantea
Fiber (CGF) / Phenol formaldehyde (PF) biocomposite.

The fiber hybridization by combining two or more different types of fibers (natural/natural) in a

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common polymer matrix is examined to get a collection of properties that cannot be obtained in a
polymer composite with a single kind of reinforcement.

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Improvements in mechanical properties due to the hybridization of AFFs and CGFs with the
Phenol formaldehyde (PF)

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