Journal of Natural Fibers

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

ThermoMechanical Characterization of Calotropis

gigantea Stem Powder-Filled Jute Fiber-Reinforced
Epoxy Composites

A. Vinod, R. Vijay & D. Lenin Singaravelu

To cite this article: A. Vinod, R. Vijay & D. Lenin Singaravelu (2017): ThermoMechanical
Characterization of Calotropis gigantea Stem Powder-Filled Jute Fiber-Reinforced Epoxy
Composites, Journal of Natural Fibers

To link to this article: http://dx.doi.org/10.1080/15440478.2017.1354740

Published online: 06 Sep 2017.

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 JOURNAL OF NATURAL FIBERS
https://doi.org/10.1080/15440478.2017.1354740

ThermoMechanical Characterization of Calotropis gigantea Stem

Powder-Filled Jute Fiber-Reinforced Epoxy Composites
A. Vinoda, R. Vijayb, and D. Lenin Singaravelub
a
Department of Mechanical Engineering, Sri Lakshmi Ammal Engineering College, Chennai, Tamil Nadu, India;
b
Department of Production Engineering, National Institute of Technology, Tiruchirappalli, Tamil Nadu, India
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ABSTRACT KEYWORDS
Filler performs key tasks in enhancing the strength of the composites. Calotropis Calotropis gigantea stem
gigantea is a weed waste typically called White Madar, widely grown in Asian powder; filler; hand lay-up;
countries. It is ground to powder and used as filler. Thus the present work deals mechanical characteristics;
natural fiber composite;
with the development of three different jute fiber reinforced epoxy composite
thermal stability
filled without and with various weight proportion of Calotropis gigantea stem
powder namely 5 and 10 weight percentage using conventional hand lay-up 关键词
technique. The developed composites are tested for its mechanical properties as 干粉末; 填料; 手托; 机械
per ASTM standards and thermal stability using the Thermo Gravimetric 特性; 天然纤维复合材料;
Analyzer. The composite which is filled with 10 weight percentage Calotropis 热稳定性
gigantea powder filler showed superior properties in both thermal and mechan-
ical characteristics due to its higher filler content which possess constituents like
cellulose, lignin, etc. Scanning Electron Microscopy helped to analyze the fiber
pullout, fractured interface, filler distribution, voids of the composites.

摘要
填料在增强复合材料强度方面起着关键作用。calotropisgigantea是杂草垃圾
通 常 被 称为 白 色的 马 塔尔，在亚洲 国家广泛种植。它是地 面 粉 作为 填
料。因此，目前的工作与三种不同的黄麻纤维增强环氧复合材料的发展和
不同重量比例的calotropisgigantea干粉即5和10重量百分比的使用传统的手
糊工艺。用ASTM标准 测试了复合材料的力学 性能 和 热稳定性。复合材料
具有10重量百分比的calotropisgigantea粉末填料均热特性，由于其 较 高 的
填料含量具有成分如纤维素、木质素和力学性能优越，等扫描电子显微镜
帮助分析纤维的拔出、断裂的接口填料分布，复合材料的空隙。

Introduction
The natural fibers, such as jute, sisal, kenaf, etc., are used as a reinforcement in polymer composites which
provides high strength to low weight ratio, eco-friendly nature, abundant source, etc. However the usage of
synthetic fibers is declined due to its high cost, manufacturing constraints and nonrecycling nature. So the
globe has now moved to the use of natural fibers due to its vital advantages for various applications, namely
automobile windshields, bumpers, doors, ceilings and furniture. The manufacturing and synthesizing the
natural fibers are relatively easy when compared to synthetic fibers (Vijay Kumar Thakur, Thakur, and
Gupta 2014). Fillers and reinforcements in the composites are mainly added to enhance the strength
properties of the materials to an extent, when the optimal percentage is exceeded these detroit the properties
(Biswas and Satapathy 2010). Arumuga Prabu et al. investigated the influence of red mud filled banana-
polyester composites on its mechanical, damping, chemical characteristics and concluded that 4 µm and 8
weight percentage of fillers produced better results (Arumuga Prabu et al. 2014). Raghavendra et al. made a

CONTACT A. Vinod vinodmech90@gmail.com Assistant Professor, Department of Mechanical Engineering, Sri Lakshmi
Ammal Engineering College, Tambaram East, Chennai, Tamil Nadu 600126, India.
Color versions of one or more of the figures in the article can be found online at www.tandfonline.com/wjnf.
© 2017 Taylor & Francis
 2 A. VINOD ET AL.

comparative analysis with and without reinforcing flyash particles on woven jute/glass hybrid composites,
results showed that 5 weight percentage of flyash particles was good in case of flexural strength, whereas 10
weight percentage of flyash particles was superlative in case of tensile strength (Raghavendra et al. 2016).
Raghad Usama Abass fabricated and tested the mechanical characteristics of orange peel filled polyester
composite with various fillers loading percentage. The results showed 10 weight percentage of orange peel
filler produced better results when compared to other(Raghad Usama Abass 2015). Bruno D. Mattos et al
evaluated the thermo chemical, physical and mechanical properties of the eucalyptus particles and mate tea
waste filled polypropylene composites ranging from 0 to 60 percentage with 40 weight percentage fixed
polypropylene and concluded that the use of eucalyptus particles than mate tea waste produced better
mechanical properties except hardness, water absorption were more in case of 60 percentage eucalyptus
particles and 54 percentage of the mate tea waste. In case of thermal stability mate tea waste filled composites
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showed better results due to its inorganic constituents (Bruno D. Mattos et al. 2014). Ratna Prasad et al.
fabricated with and without incorporating organically modified montmorillonite (MMT) nano clay in wild
cane grass fiber reinforced polyester resin composites using hand lay-up method. It was concluded that use
of nanoclay in composites improved all the mechanical properties to a considerable extent (Ratna Prasad
et al. 2015). There is no research work incorporating Calotropis gigantea stem powder as a filler in the
composites. Thus the present work deals with fabrication of three different jute fibers reinforced epoxy
composites incorporating Calotropis gigantea stem powder in 5 and 10 weight percentages compared with
unfilled one. The samples were developed using conventional hand lay-up methods and mechanical
characteristics namely tensile, flexural, compression, impact, and hardness were found as per ASTM
standards and thermal stability of the filler and developed composites were found using the
Thermogravimetric Analyzer. SEM studies helped in analyzing the desired characteristics of the tested
composites.

Materials and methods

Materials
Calotropis gigantea is a weed that grows commonly in Asian countries like India, Malaysia, Thailand,
China, Pakistan, and Indonesia. It has various medicinal properties, so it is used in Ayurveda medicines
and also as a good mosquito repellent. Calotropis gigantea has toxic properties as well, which causes
diarrhea, vomiting, dilated pupils, and even death (Singh and Javed 2015). As it is a common weed plant,
which could be positively used as filler in polymeric composites. Calotropis gigantea stems are collected
and dried in sunlight until the moisture content is removed. The stem is then chopped into pieces. The
chopped stem is ground to powder form, again kept in hot air oven at 50°C to remove the moisture traces
and sieved to 100–150 mesh. Figure 1 shows the SEM image of Calotropis gigantea powder. Bi woven jute
fibers mats are used in this work and it is produced primarily from the plants of genus Corchorus.
Pultrusion is a process used in glass fiber manufacturing and bi woven glass mats are used in the present
study. The main purpose of glass fiber used in this work is to increase the surface finish as it has very
strong and light fiber reinforcements. The epoxy resin (LY556 grade) and hardener (HY951grade) were
used for the curing process in the ratio 10:1.

Manufacturing of composites
A conventional hand lay-up method was used for fabricating the composite material for this current work.
The biwoven jute fibers mat was kept in hot air oven for 10 minutes at 40°C to remove the traces of
moisture. Smooth and flat surface was used and a layer of wax was applied, followed by wiping off using a
soft cloth. Then a layer of polyvinyl alcohol was applied, which acts as a releasing agent for the removal of
the fabricated composite. The coated surface was left in hot sunlight for drying and to settle down. In order
to make C-2 and C-3 filler based composites 5 and 10 weight percentages of Calotropis gigantea powder
were mixed with 95, 90 weight percentage of resin and hardener, respectively using Sonicator to form
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Figure 1. SEM image of Calotropis gigantea filler.

mixture. Then a layer of this mixture was applied using a roller as per the desired size and a layer of bi
woven mat glass fiber was placed, followed by a layer of this mixture, over which a jute fiber mat was placed.
A coat of the mixture was given with the roller and again a layer of jute fiber mat was placed. Finally, a layer
of glass fiber was placed above the jute fiber for good surface finish and a coat of mixture was applied.
Twenty-five kilogram dead load was positioned over the composites to enable even distribution and kept
untouched for 24 h in normal room temperature (Vijay and Lenin Singaravelu 2016). Care should be taken,
to ensure there was no air traps. In case of C-1 Composite, 100 weight percentage of resin and hardener was
used to develop the composite with similar procedure as stated above.

Testing of fabricated specimens

The saw cutter was used to cut the developed laminates to the desired shapes for making the different test
specimens. In order to check the repeatability results, three specimens on each test for each composite
were tested. Tensile, flexural, compression properties were obtained for the developed composites in a
universal testing machine at room temperature conditions following ASTM: D638, ASTM: D790, ASTM:
D695 standard procedures respectively, in case of flexural testing alone three point bend set up was used.
Charpy Impact test setup was used to measure the energy absorbed following ASTM: D256 standard.
Hardness was measured using SHORE-D hardness tester having 1.25 mm diameter hardened steel rod
indenter, having 30°Conical point of 0.1 mm radius tip and 4.550 kg load was applied as per ASTM:
D2240 standards. Five readings are taken down for each specimen and the average is noted. Thermal
Stability of the filler and the developed laminates were tested using Thermo Gravimetric Analyzer (TGA)
in nitrogen environment. The samples with weight of 5 milligrams were used and it was tested in
temperature ranging from room temperature to 800°C at 10°C/min heat rate with a gas flow of 20 mL/
min. Scanning Electron Microscopy (SEM) studies was done using Tescan VEGA 3LMU SEM machine
of Czech Republic (Vijay and Lenin Singaravelu 2016).

Results and discussion

The various characteristics of the tested specimen are shown in Figure 2 and the detailed discussion
follows below.
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Figure 2. Various mechanical properties of the developed composites.

Tensile properties
Tensile strength is the maximum force to which a material can withstand without fracture when stretched
and it is also an indication of strength of the material. The fabricated specimens are characterized for tensile
load and strength; the results are shown in Figure 2. The results showed that the C-3 produced 1.75 and 1.89
times higher ultimate tensile load than C-2 and C-1, respectively. Similarly, the tensile strength of C-3 was
1.385 and 1.39 times higher than C-2 and C-1, respectively. The C-3 composite mainly consists of higher
percentage of Calotropis gigantea filler which chiefly constitutes of cellulose, hemicelluloses, and lignin when
compared to jute fiber as explained elsewhere (Ashori et al., 2009; Balaji, Karthikeyan, and Vignesh 2016;
Karthik et al., 2012). Higher the cellulose and lignin content imparts more stiffness which are responsible for
the increase in strength values; this is in accordance with the literature findings (Huang et al. 2016). This
higher stiffness prevents the crack to propel further there by forming brittle fracture with increased results.
Another important aspect is that the fillers got adhered to the matrix very firmly due to its fine and uniform
distribution. This fine filler particles possess higher surface area which enables the wetting of filler with the
resin matrix. These fillers reorient themselves during the failure causing effective stress transfer between
filler, fibers and matrix i.e., development of cross-linked structure which limit the free mobility of polymer
chains. The void pores also detorite the results which could be judged using hardness of the composites.
Higher the void pores lower will be the hardness(Manaila et al. 2016). In case of C-3, hardness is also more
since it has fewer voids and even those voids are also filled with the fillers which is clearly evident in the SEM
Figure 3a as indicated by “B” and also the firm bonding of fiber with matrix as indicated by “A.” It is also
evident that there is also good reduction in the percentage elongation of the composite which indicates the
capability of the material to resist shape change before crack generation. Thus, there is an increase in cross-
linking density that has negative impact on the ductility leading to increase in the tensile strength. Elasticity
behavior is the ability of the material to return to its original shape after being stretched commonly known as
stress. There is a limit of the amount of stress that can be applied to a material before reaching its elastic limit
and deforms irreversibly. The decrease in elongation is irregular and complex mechanism (adding of rigid
fillers to ductile polymers). This will restrict the flow and the strain energy decreases leading to the reduction
in elasticity and segment mobility (Bensalah et al. 2017). The similar trends are also seen in literatures
namely Arundo Donax filler filled epoxy composites with 10 weight percentage showed better tensile
strength (Fiore et al. 2014) and wood saw dust filled natural rubber ecocomposites (Manaila et al. 2016) but
the reverse trend is seen in Argan Nut shell particles based composites in which lower the filler content,
higher the tensile strength (Essabir et al. 2015), it is clearly explained that the type of filler plays an important
role in deciding the nature. In case of C-1 composite, which has no filler and only jute fibers, there is a poor
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Figure 3. SEM images of tensile tested specimen of (a) C-3 composite representing the firm bonding of fibre and void filled by fillers (b) C-1
composite representing improper wetting of jute fibre with resin, more fibre pullout, fibre tear and more matrix crack.

wetting of resin with the fiber, and also many voids due to which deterioration in the properties of the
composite, as stated early voids cause more detoriation of the properties. Also, the fiber debonding once it is
initialized it will occur rapidly leading to further elongation. SEM Figure 3b represents the C-1 composite
tested for its tensile properties, in which there is less wetting of fiber with resin, more fiber pullout and fiber
tear, and high depth matrix crack which attributed to the decrease in properties and these are denoted by “D,
E, F, G,” respectively.

Flexural properties
Flexural is a combination of compression and tension properties. The flexural characteristics obtained for
the tested composites are presented in Figure 2. It is evident from the test results that the C-3 composites
produced ultimate flexural load and flexural strength of 0.88 KN and 195.19 N/mm2 followed by C-2 having
0.74 KN and 164.14 N/mm2, C-1 having 0.52 KN and 115.34 N/mm2, respectively. There are several factors
which play an important role in controlling the mechanical properties of the composites namely intrinsic
fillers, matrix properties, filler content, filler distribution, and very important is the interfacial adhesion. The
C-3 composite has intercalation between the filler-fiber-resin matrixes which increases the interfacial
adhesion. It is also visualized that adequate optimal uniform and fine sized fillers distribution (Salehian
and Jahromi 2015) is evident in the composite, SEM Figure 4a represents the C-3 flexural tested specimen in
which the fracture with less fiber pullout which also proves the better adhesion enabling superior results it is
denoted by “C.” While the properties are little less in case of C-2 due to the lack of adequate quantity of fillers
which is seen in Figure 4b as indicated by “J.” It is seen that C-2 and C-3 composites visualized waviness in
the plots which is due to the fact that fillers which act as reinforcement comes to existence and hinders the
crack propulsion leading to enhancement in strength. In case of C-2, due to inadequate fillers, the plot
showed more waviness. There is more reduction in strain percentage which enhances the strength and
brittleness of the composite which enters to the plastic zone, i.e., more brittle nature. This is due to the higher
lignin content and rigid fillers (Benazir et al. 2010). The increase in the tensile and flexural properties is in
accordance with the rule of mixtures for fiber-filled polymer composites. The increase in flexural strength is
also mainly due to the presence of fibers and an intrinsic toughening mechanism due to the presence of
Calotropis gigantea fillers along the path of crack. Thus, these fillers are to withstand more bending stress
transfer leading to the enhanced results. The similar trend is visualized by Tapan Kumar Patnaik and Nayak
in their silicon carbide reinforced jute epoxy composites where increased fillers percentage showed better
results (Patnaik and Nayak, 2016).
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Figure 4. SEM images flexural tested specimen of (a) C-3 composite showing better adhesion of fibre and filler with the matrix (b)
C-2 composite visualizing the inadequate fill of fillers.

Compression properties
The compression characteristics of the developed composites are shown in Figure 2. The test results
followed the trend of C-3 > C-2 > C-1 in which the due to fine and nonagglomeration of fillers in C-3
showed better results. C-1 samples showed poor results due to the presence of kinking. It is assumed
that the kink band formation process is similar during both the decortication process and the loop test.
This point of failure is determined as merely the point at which the kinking process has occurred over
the full diameter of the fiber (Bos, Van Den Oever, and Peters 2002). Thus, there is micro buckling of
the fibers leading to buckling of the composites outward causing the fibers splitting leading to the
compressive failure, which is seen in C-1 composite. In case of C-3, there are interstitial spaces between
the resin and fibers were firmly adhered by the Calotropis gigantea filler which prevented the failure
i.e., the fillers occupy the interstitial position on the crack path preventing the failure of the composite
as shown in SEM Figure 5, this is also clear from the stress-strain curve which showed distributed curve
over the span since it is due to fillers occupying the failure path. The matrix crack propulsion gets

Figure 5. SEM image showing filler distribution along the crack path in C-3 composite.
 JOURNAL OF NATURAL FIBERS 7

reduced in C-3 composites since fillers prevent the crack to propel further during the debonding or
failure of fiber thereby getting the desired load bearing characteristics (Hulugappa, Achutha, and
Suresha 2016).

Impact and hardness properties

The average values of impact and hardness properties of the tested composites are shown in Figure 2.
Impact strength of the composites is mainly influenced by toughness, nature of interfacial region and the
friction work occurs due to the pulling out fiber from the matrix. The interfacial nature is very crucial in
determining the toughness of the composite since it is directly proportional. The energy absorbed denoted
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the toughness of the composite which is a study of brittle-ductile transition. In the present case, C-3 proved
to be superior due to high filler content which absorbs more energy during the impact testing since it has
got fine particle size, shape, and good energy absorbing characteristics which are present at the plane of
fracture resisting the failure growth. Generally, it is said that highly ductile material will have good impact
when compared to the brittle. But in many cases the contrast has also happened for filler filled composites
namely silicon carbide filled Jute fiber epoxy composites showed that higher the filler, higher was the
impact properties (Patnaik and Nayak, 2016) but in case of SiC filled glass epoxy composites showed
reverse trend (Agarwal, Patnaik, and Sharma 2013), this is very clear that the bonding interface plays an
important role in determining the properties. Similarly the C-2 composites showed intermediate results due
to the smaller weight percentage of the fillers, it showed deep cracks and fiber breakage due to the higher
impact as shown in SEM (Figure 6) as indicated by “I&H,” respectively. Hardness is the resistance to
penetration, percolation of the indenter on the material being tested. The hardness of the C-3 composites is
higher when compared to the C-1 which are due to the facts that fine and uniform distribution of the fillers
on the composite filled the voids there by reducing the pores these eventually increased the stiffness of the
composites leading to the increase in hardness. This is also correlated with the higher tensile strength
reducing of plasticity and flexibility of the composite. Thus by making the composite very rigid due to the
effect of cross linking nature of the polymer–filler matrix as explained elsewhere (Manaila et al. 2016;,Vijay
and Lenin Singaravelu 2016).

Figure 6. SEM image of C-2 composite impact tested specimen showing deep matrix crack and fibre breakage.
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Figure 7. TGA of Calotropis gigantea filler and developed composites.

Thermal stability of the filler and composites

Thermo Gravimetric Analyzer played a crucial role in finding the weight loss w.r.t. temperature for the
raw material and developed composites. Generally it is stated in the literature that components inside the
fiber/filler undergoes carbon-chain breaking followed by secretion of volatile materials such as hydro-
carbon, carbon dioxide, and hydrogen gas. The constituents which are having lower molecular mass will
undergo more degradation when compared to the higher molecular mass. Normally lignin, cellulose
which is burnt firstly when compared to others traces elements (Risnasari et al. 2015). The Calotropis
gigantea filler showed first degradation from 35°C to 100 °C due to water vaporization followed by
second stage which was from 150°C to 230°C due to degradation of lignin followed by hemicellulose
decomposition till 300°C and the maximum degradation temperature is obtained at 340°C(Velusamy
et al. 2014)and till 395°C which is due to cellulose degradation similar to Numm et al. (Nunn TR et al.
1985) and decomposition temperature is similar range since the TGA samples are from the stem of the
plant, though the natural fibers are seasonal and region specific. The residual char left is 21.03 weight
percentage as shown in Figure 7.
The raw material thermal stability played a crucial role in the thermal stability of the developed
composites. The degradation at various stages is due to the decomposition of lignin, hemicelluloses, and
cellulose. The developed composites starts its hemicellulose and cellulose degradation from 220°C and
ends at 500°C and the maximum degradation temperature occurs at 400°C for C-1, 413°C for C-2, 430°C
for C-3, leaving residual char of 19.01, 23.06, 29.41 weight percentage, respectively. Filler based
composites produced higher results due to the better thermal stability of Calotropis gigantea powder
when compared to jute fiber. This is mainly due to the fact that higher filler content reduced the content
of epoxy matrix which undergoes degradation by random chain scission and radical-chain mechanism,
thus, upon its reduction the degradation is mainly due to the filler and fibers and its thermal stability, the
similar trend is seen in bamboo fiber based composites (Shah et al. 2017).

Conclusion
The Calotropis gigantea fillers filled jute fibers epoxy composites were developed by a conventional hand
lay-up process, tested for its thermomechanical properties and compared with un filled one. The higher
weight percentage Calotropis gigantea fillers filled jute fiber composites showed superior results in tensile,
flexural, compression, hardness, and impact properties followed by partially fillers filled and then by no
 JOURNAL OF NATURAL FIBERS 9

filler filled jute fiber composites. TGA was very useful in finding the thermal stability of the fillers and
composites, higher the filler higher was the thermal stability.SEM studies paved way in visualizing the
matrix bonding, cracks, voids, filler distribution, size, fiber pull out, the fracture nature of the tested
composites. Thus, higher Calotropis gigantea filler filled jute fiber epoxy composites (10 weight percen-
tage) proved to be better in both thermal and mechanical properties than the other composites.

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