j m a t e r r e s t e c h n o l .

2 0 2 0;9(6):12187–12200

Available online at www.sciencedirect.com

https://www.journals.elsevier.com/journal-of-materials-research-and-technology

Original Article

Optimization of surface treatment in Calotropis

Gigantea (CG)-fibre yarn by simple techniques and
characterization of CG fibre yarn reinforced
laminate

K. Renugadevi a,∗, P.K. Devan b, M. Chandra Sekhara Reddy a, P. Karthik c , Tiju Thomas d
a Department of Mechanical Engineering, Sri Venkateswara College of Engineering, Karakambadi Road, Tirupati 517507, India
b Department of Mechanical Engineering, R M K College of Engineering and Technology, Puduvoyal, Tiruvallur District 601206, India
c Department of Mechanical Engineering, Loyola ICAM College of Engineering and Technology, Loyola Campus, Nungambakkam, Chennai

600034, India
d Department of Metallurgical and Materials Engineering, Indian Institute of Technology, Madras, Chennai 600036, India

a r t i c l e i n f o a b s t r a c t

Article history: Calotropis Gigantea (CG) is a shrub plant that grows rampantly in South Asia. Here we report
Received 8 May 2020 the development of CG bast fibre yarns, which could yield replacements for artificial fibres
Accepted 12 August 2020 in engineering applications. Most of the researchers concentrated only in the short form
Available online 17 September 2020 of natural fibres, this leads to dropping the fibre reinforcement in continuous and lengthy
products. An attempt has been made in this research by taking CG fibre in the form of twisted
Keywords: yarn as reinforcement. The surface treatment is done to enhance the properties of the CG
Natural fibre yarn fibres and to reduce hydrophilic and hygroscopic behaviour using NaOH (aq.). Determining
Modulus the appropriate NaOH concentration in the treatment solution is essential to reduce the
Alkali treatment hydrophilicity of the fibres while retaining its mechanical properties. Generally optimised
Contact angle measurement NaOH concentration found by completing fibre characterization, which is a very lengthy and
Unidirectional orientation time-consuming process. In this research work, the optimum concentration of NaOH found
Fibre weight ratio by a quick and short process using simple techniques. Two techniques were used such as
Contact angle measurement of fibre surface and microscopic observation of xylem structure
to find an optimum concentration of NaOH in the aqueous solution. On treated CG fibres, the
contact angle is found to be as high as 112◦ for 4 wt.% NaOH (aq.) concentration; indicating
that the treatment renders the fibre hydrophobic and the observation of xylem structure
(voids) confirms in a minimum amount in the same 4 wt.% NaOH treated fibre. The mecha-
nism involved is rationalized using infrared/vibrational spectroscopy based measurements
of untreated and treated sampled. The orientation of the fibre helps with optimization of the
properties. The elastic modulus (measured as per ASTM standards) obtained are 4.18 GPa
(along the fibres) and 3.05 GPa (perpendicular to the fibres).
© 2020 The Authors. Published by Elsevier B.V. This is an open access article under the
CC BY-NC-ND license (http://creativecommons.org/licenses/by-nc-nd/4.0/).

∗
Corresponding author.
E-mail: renukasarath12@gmail.com (K. Renugadevi).
https://doi.org/10.1016/j.jmrt.2020.08.058
2238-7854/© 2020 The Authors. Published by Elsevier B.V. This is an open access article under the CC BY-NC-ND license (http://
creativecommons.org/licenses/by-nc-nd/4.0/).
12188 j m a t e r r e s t e c h n o l . 2 0 2 0;9(6):12187–12200
1. Introduction
Green engineering is essential in the wake of global warm-
ing and progressive environmental degradation. Considering
this, most of the automobile industries have started the use
of natural fibre composites which decompose readily. Given
this backdrop, work on natural fibres and their composites
have gained relevance. To this end, Joshi et al. [1] have found
that emissions of COx and NOx from the incineration of China
reed fibre composites and glass fibre composites are less when
compared to that from artificial fibres. Natural fibre compos-
ites have more amount of fibre volume fraction and hence
offer promise from the standpoint of delivering performance
equivalent to that of glass fibre composites. This approach
offers prospects for light-weighting and hence offers a means
to achieve increased mileage of the vehicle [2]. This explains
the transition from glass fibre composites to natural fibre com-
posites in several automobile accessories and interior parts.
Mazlan et al. [3] have made a case for considering end-
of-recycling as an important factor to justify the use of the
material in a product. It turns out that such considerations
to indicate the prospects associated with natural fibre com-
posites. In fact, the automobile industry has been reasonably
quick at making this transition. Mercedes Benz used jute based
composites to replace E-glass, A-glass, and S-glass compos-
ites in the interior parts of a vehicle [3]. This has impacted
the adoption of natural fibres beyond the automotive sector as
well. For instance, Tara Sen and Jagannatha Reddy [4] demon-
strated the usage of natural fibres like bamboo, coir, sisal, jute
and hemp in construction. Likewise, Jute fibres are being used
as cement reinforcements, bamboo fibres are used in floor tiles
manufacturing, coir fibres are used to make fishing nets, and
find use in the production of mattresses [4].
In this present work, Calotropis Gigantea based plant bast
fibre is taken as reinforcement for composites. Bast fibre
means a fibre bunch derived from outer layer cells of various
plant stems. In fact, this was spurred by the work of Gane-
shan et al. [5], wherein they examined the suitability of CG
stem fibres as potential reinforcements for natural fibre com-
posites based on the microstructure analysis like crystallinity
index, morphology and thermogravimetric properties. Certain
bast fibres are already in use in engineering applications to
produce composites such as hemp, kenaf, jute etc. [6].
Ashori and Bahreini [7] evaluated the chemical con-
stituents of bark and seed fibres derived from CG for suitability
as a raw material in the composites. Extracted Calotropis
Gigantea bark fibre has 57% cellulose, 19% hemicelluloses, 18%
lignin, and 23% of alkali-soluble substances [7]. While select-
ing the new fibres, the chemical constituents play a major
role in determining the mechanical properties of the fibre in
natural fibre composites. Especially reduction of the hemicel-
lulose content can aid in the reduction of moisture absorption
property; this usually requires chemical or surface treatments.
Most of the natural fibres which are in use as reinforcements in
composites have the same range of hemicellulose content [8].
Table 1 lists the chemical constituents of natural fibres which
are already in use as reinforcement in natural fibre composites
along with CG fibre [8].
From the literature review, it is inferred that the CG fibre has
an equivalent range of cellulose to produce better mechanical
properties when compared with existing fibre.
2. Materials and methods
2.1. Extraction of fibre
Calotropis Gigantea (CG) plant is a shrub plant abundantly
available in South Asian countries, such as India, Malaysia,
Thailand, etc. CG fibres are extracted from the stem bark of
the plant. CG fibres are derived from the CG plant stem using
a retting process [9]. Initially, it is separated as short fibres with
a maximum length of ∼1 m. Later the bunch of short fibres is
twisted as a yarn to produce continuous lengthy fibres with
∼150–160 twists per meter. These twisted yarns have an aver-
age diameter of 1 mm [10,11]. The extraction process of CG
fibre from the CG plant has been shown in Fig. 1(a)–(f). Ini-
tially, the stem is separated from the plant and the flowers
and leaves are removed; also the bark of the stem is removed.
Stems are allowed to dry in sunlight for one or two days, to
render the bark separation process easy. This is done since the
process efficiency improves when dried stems are used. Later
the fibres are separated from the stem outer layer as well as the
inner layer of the bark. Usually, 100 feet of the fibre is separated
and twisted out from the plant in 3 h. Fig. 1(f) shows the final
form of CG fibre yarn which are used in the present work as
reinforcement for natural fibre composites. Ramasamy et al.
[12] measured the fibre density to be 1.324 g/cm3 according to
ASTM standard D 3800-99.
2.2. NaOH (alkali) treatment
Natural fibre composites offer good mechanical strengths
but have to be treated with chemical and physical treat-
ments. These treatments work by changing the internal and
external structure. This, in turn, results in the reduction of
moisture and water absorption by the fibre. This is of sig-
nificant value since the hygroscopic nature of these fibres is
a major drawback and is the primary limitation associated
with its practical use. Xue Li et al. [13] listed various chemical
treatments involved in natural fibre composites such as alka-
line treatment, silane treatment, acetylation of natural fibres,
benzoylation treatment, acrylation and acrylonitrile grafting,
maleated coupling agents, permanganate treatment, peroxide
treatment, isocyanate treatment, etc. to improve the mechan-
ical properties of plant fibre composites.
Hemicellulose and lignin contribute significantly to the
moisture absorption property since these constituents con-
tain hydroxyl groups which absorb moisture present in the air
[14]. Hemicellulose contains glucose and other water-soluble
sugars in the form of hydroxyl groups; it is responsible for
20–35% of the dry weight of cellulose generally [15]. By elimi-
nating the hydroxyl groups present in the hemicelluloses, the
moisture uptake typically reduces in the natural fibres. This
also leads to shrinkage of the fibre and weight loss. Physi-
cal treatments mainly involve the conversion of fibre bunches
into individual filaments to attain better mechanical prop-
erties. Mukhopadhyay and Fangueiro [16] employed physical
 j m a t e r r e s t e c h n o l . 2 0 2 0;9(6):12187–12200 12189

Table 1 – Chemical constituents of various natural fibres used as reinforcement (abstracted from [8]).
S. No. Fibre name Cellulose (%) Hemicellulose (%) Lignin (%) Density (g/cm3 )

1 Calotropis Gigantea 57.00 19.00 18.00 1.15–1.20

2 Flax 64.10–71.90 16.70–20.60 2.00–2.22 1.50
3 Hemp 70.20–74.40 17.90–22.40 3.70–5.70 1.48
4 Jute 61.00–71.50 12.0–20.4 11.80–13.00 1.30
5 Kenaf 45.00–57.00 21.50 8.00–13.00 1.45
6 Okra 60.00–70.00 15.00–20.00 5.00–10.00 –
7 Ramie 68.60–76.20 13.10–16.70 0.60–0.70 1.50
8 Roselle 64.50 20.23 6.21 1.33

Fig. 1 – Extraction process of CG fibre from CG plant (a) image of the whole plant, (b) plant stem, (c) separated stems, (d) fibre
separation from bast area, (e) fibres in individual and twisted form, and (f) twisted CG fibre yarn.

treatments like steam explosion process and thermomechan-
ical processes for achieving the same. Koohestani et al. [17]
investigated major factors such as enhancement in mechan-
ical properties, energy consumption and effluent (sewage)
generation in natural fibre processing. They emphasized the
significance associated with silane, alkaline, acetylation and
maleated coupling to eliminate soluble sugars present in the
hemicellulose.
The process chosen should be such that it offers an
effective approach for the elimination of hemicellulose. The
chemistry of hemicellulose hence becomes essential. Gibson
[18] reported hemicelluloses to include 500–3000 monomer
units with acidic groups. It also mainly consists of xyloglu-
cans, xylans, glucomannans, etc. When the fibre is treated
with alkali, the acidic groups react with base and get neu-
tralised (hence resulting in the formation of water). Xylose
(C5 H10 O5 ) is the main monomer of hemicelluloses; relevant
alkali reaction is shown with the help of this monomer in an
Eq. (1).
(C5 H10 O5 )n + NaOH → Fibre − O − Na + H2 O (1)
The reason for the selection of alkaline treatment in this
study is that it offers an easier approach (when compared
12190 j m a t e r r e s t e c h n o l . 2 0 2 0;9(6):12187–12200
Fig. 2 – Dimensional shrinkage of CG fibre after alkali
treatment through visual image.
to say the silane treatment) [19]. There has been prece-
dence; Oushabi et al. [20] investigated the effect of the alkali
treatment in Date palm fibres and found the optimum con-
centration of alkali by testing tensile properties, FTIR analysis,
TGA analysis and morphology.
Here sodium hydroxide (NaOH) aqueous solution is taken
in different concentration by weight for soaking the CG fibres.
The concentrations are increased slowly from 0 wt.%, 1 wt.%,
2 wt.%, 3 wt.%, 4 wt.% and 5 wt.% respectively and soaked for
1 h [20]. Soaked fibre yarns are removed from NaOH aqueous
solution and it is cleaned with demineralised water until it
reaches the value of pH 7. The washed fibres are dried in sun-
light for one day and then kept in an oven at the temperature
of 70◦ C for 4 h. The dried fibre shows dimensional shrinkage
due to removal of lignin, wax and partial removal of hemicel-
lulose and alkali-soluble substances present in the fibre. CG
fibres have dimensional shrinkage of ∼30%; the final diame-
ter reduces from 1 mm to 0.7 mm after NaOH treatment. Fig. 2
shows the dimensional shrinkage of CG fibre yarn visually.
2.2.1. Optimization of alkali concentration in CG fibre
using contact angle method
Generally the Optimization of Alkali concentration of any nat-
ural fibre found by finding its mechanical properties after
preparation of natural fibre reinforced laminate. Afolabi et al.
[21] investigated the Fabrication of pandanus tectorius (screw-
pine) natural fibre using vacuum resin infusion by doing
surface treatment using various alkali concentrations. After
the determination of tensile strength, the optimum con-
centration of NaOH found to produce better mechanical
properties. The drawback of this method is the optimum con-
centration may lie in between the selected range also. Hassan
et al. [22] optimised the tensile behaviour of Banana pseu-
dostem fibre reinforced composites using surface response
methodology contour plots of tensile specimens by treating
with an increase in concentration from 3% to 9% and con-
cluded that by considering three individual parameters of fibre
like length, NaOH content and fibre loading in ANOVA soft-
ware. In this research work, optimum NaOH concentration for
CG fibre is found through contact angle measurement.
Water absorption plays a major role in natural fibre com-
posite (NFC) reinforced laminates. The presence of cellulose
enhances the mechanical properties of the NFC laminates.
However, cellulose renders the system hydrophilic. A rele-
vant study here is that of Prasanna Venkatesh et al. [23] who
investigated the reduction in water absorption using alkali
treatment. It is shown to increase the mechanical properties
of the Sisal/polyester composites. They also found that long
fibres produce more strength than short fibres.
In this work, water absorption property is found by
using the Image-Pro software on images taken [24]. Water
droplet images were taken with a high-resolution camera and
imported to Image Pro software for the measurement of con-
tact angle that indicates the quantity of water absorption of
the material. Surfaces that show an acute contact angle that
absorbs water readily; obtuse contact angle correlates only
with partial hydrophilicity.
2.2.2. Optimization of alkali concentration in CG fibre
using microscopic examination of voids (xylem tissue)
The second simple technique used to find an optimum con-
centration of Alkali in CG fibre is by observing vascular
bundles in natural fibre after its alkali treatment E-Glass fibres
have been replaced by plant fibres through proper surface
treatments which reduce the hydrophilicity and hygroscopic
behaviour [26]. This also improves the mechanical properties
of treated fibre [27]. Major modification occurs in vascular bun-
dles of cell walls (fibres), which also reduce water absorption
of fibres after the alkali treatment [26]. Initially, pores are cov-
ered by lignin and a waxy layer of a primary wall in the raw
fibre. After NaOH treatment, tracheid pores (associated with a
specific kind of dead xylem cells) become opened through the
partial removal of lignin, hemicellulose and wax present in
the primary wall [27]. The untreated and alkali (NaOH) treated
CG fibres are examined through a microscope to identify the
impurities and the structure of xylem after alkali treatment
of CG fibre. The binocular microscope with 10WF (wide field)
and 40× magnification of lens are used to study the structure.
Phloroglucinol, concentrated hydrochloric acid and glycerine
in equal mixing ratio used as a staining solution to observe
the samples in the microscope [28].
2.2.3. Justification of alkali concentration using FTIR
analysis
The optimum concentration of alkali found using simple tech-
niques and the results were justified with FTIR analysis. FTIR
analysis was done at SAIF IITM Chennai. CG fibre is taken
and alkali-treated in the range of 0–5% by weight. These
Treated fibres are taken into thin layers and tested in Fourier
Transform Infra-Red (FTIR) spectra. Presence of peaks within
selective absorption bands indicates and ensures the presence
of chemical compounds in the alkali-treated fibre[32]. Results
are obtained for all various alkali concentrations ranges from
0% to 5% through FTIR analysis.
2.3. Optimised alkali-treated CG fibre yarn
specification
Optimised alkali-treated CG fibre yarn (4 wt.%) taken as rein-
forcement for laminate preparation further. The density of CG
fibre yarn is calculated by taking the ratio between the vol-
ume of a certain length by measuring the diameter of fibre
yarn using micrometre and weighed mass of the same length.
 j m a t e r r e s t e c h n o l . 2 0 2 0;9(6):12187–12200 12191

Table 2 – Technical specifications of alkali-treated CG Table 3 – Mechanical properties of Araldite used as a

fibre yarn used as reinforcement. binder (resin) for laminate preparation.
Property Specification Sl. No Property Value
3
Density () 1.19 g/cm 1 Density (g/cm3 ) 01.19
Diameter (d) 0.7 mm 2 Tensile strength (MPa) 52.00
Twist level (T) 150 tpm 3 Tensile modulus (GPa) 02.80
Twisting angle () 5◦ 4 Elongation at break (%) 11.00
Packing fraction () 0.7 5 Shear modulus (GPa) 01.23

The image of the CG fibre yarn is transferred to Image pro soft-

ware (Image pro plus–Media Cybernetics) and the twist angle
is measured at various places. Packing fraction of CG fibre is
calculated using the Eq. (2).
Rask et al. [33] showed that the twisting action of flax fibre
does not influence the composite stiffness flax fibre. Peças
Paulo et al. [2] found that the twist angle plays an important
role in the cohesion of fibres and yarn strength up to the opti-
mum angle. Beyond that the fibre loses its strength owing to
high obliquity leading to a decrease in the binding strength in
between fibre and matrix. Naik et al. [34] analysed the effect
of different twisting angle (0◦ , 5◦ , 10◦ , 15◦ ) on E-glass and car-
bon fibre yarn reinforced composites. Twisted yarns produce
low elastic modulus when compared to the untwisted strands
due to micro buckling of fibres inside; when the twisting angle
increases the modulus decreases further [34]. Twisting angle of
5◦ produces better properties than increased twisting angles.
This is done with 190 twists per metre (TPM). This is consis-
tent with the work of Mike et al. [35], who analysed the effect of
twisting angle and packing fraction of reinforced fibre on ten- Fig. 3 – Fibre orientation of fabricated laminate.
sile strength of unidirectional plant fibre composites (PFCs).
Mike et al. observed that due to the increase in the twist-
ing angle of fibre yarn, the tensile strength of PFCs drastically ability, compression, etc. The hardener provides sufficient gel
reduces. Owing to the short length of staple fibres, it needs to time, viscosity and increases the re-mould time. The prop-
be twisted to produce yarns for reinforcement. He also derived erties of matrix are given by Huntsman distributors [41] for
an analytical expression to calculate the packing fraction from Araldite/HY 951 after 12 h of curing and tested as per ISO
the twisting level of the fibre yarn. norms. Table 3 lists the properties of binder or matrix used
in the fabrication of composite.
Packing fraction () = 0.7(1 − 0.78e−0.195T ) (2)
2.5. Fibre orientation in mat preparation
T = twist level per metre (TPM).
If the packing fraction lies above 0.6, it usually results in The optimum concentration of NaOH treatment for CG fibre
good mechanical properties. In fact, the packing fraction of is found to be 4 wt.% through contact angle measurements,
the sample reported here is 0.7; details of the CG fibre yarn microscopic examination and FTIR analysis. Treated CG fibre
geometry is given in Table 2. has been used to form a two-layer mat in the orientation of
0◦ /0◦ and 90◦ /90◦ (ref: Fig. 8) in single-ply condition to find
2.4. Resin maximum and minimum ultimate tensile strength and elastic
modulus [36]. Fig. 3 indicates the direction of fibre reinforce-
Muthukumar et al. [31] listed the major properties and ment and loading of the specimen.
suitability of the epoxy resin for developing natural fibre com- Fibre orientation in the matrix plays a major role in com-
posites. Araldite (Epoxy) is considered to be a good matrix posites to withstand against the load without failure. Michael
material for making natural fibre composite. This is because, et al. [37] investigated the maximum possible orientation
the epoxy resin possesses desirable properties like excellent of fibre in the matrix to yield enhancement of mechanical
adhesion to fresh surfaces of a wide range of chemistries, properties by taking Lyocell fibre as the reinforcement in the
high resistance to chemical and atmospheric attack, and high polypropylene matrix. He has taken five different orientations
dimensional stability [40]. Araldite and Hardener HY951 are from 0◦ to 90◦ and concluded that if the fibre orientation is
purchased from Huntsman Distributors, Chennai. 10% weight <±45◦ , the material becomes softer and deforms easily with
of Hardener (HY951) is mixed to prepare the matrix along with larger elongation. If the orientation is >±45◦ , the opposite phe-
the epoxy resin. The hardener (HY951) influences the physi- nomena take place due to the delamination effect of the fibre.
cal and mechanical properties such as tensile ability, flexural This cause an elongation decrease considerably leading to a
12192 j m a t e r r e s t e c h n o l . 2 0 2 0;9(6):12187–12200
Fig. 4 – Fabrication Process of CG fibre reinforced laminate: (a) female part of die, (b) male part of die, (c) combined die set up,
(d) preparation of mat, (a) Fabricated laminate and (f) prepared specimens for tensile test.
further drop in ultimate tensile strength and Young’s modulus.
Plant fibre composites (PFC) are mainly fabricated to replace
synthetic fibres in the field of automotive, constructive and
packaging industries. While selecting the PFCs for any appli-
cation, it also requires good tribological behaviour to increase
the lifetime of the product. Surface treatments of fibre and
fibre orientation are important factors that can affect the tri-
bological properties of PFCs [38]. Yousif and chin analysed the
tribological properties of Kenaf fibre reinforced composites in
different orientations by taking load as the justifying factor.
The importantly normal orientation of fibre enhances wear
performance of epoxy by ∼85% when compared to parallel and
anti-parallel loading condition [39].
2.6. Laminate preparation by hand lay-up technique
4 wt.% alkali-treated CG fibre yarn is tightly wound on the
setup. It is then stitched with cotton thread by hand to render
in the form of a mat. Mild steel hand lay-up set up is fabricated
to prepare a laminate with the area of 81 square inches. The
setup is kept on a table and petroleum jelly is applied as a lubri-
cant to separate the die and laminate after curing. Araldite and
Hardener (HY951) mixed in a standard ratio of 10:1 to prepare
a matrix and it is applied as a base layer in the hand lay-up
setup; the CG fibre mat is kept as reinforcement. Fig. 4 shows
the fabrication process of laminate and specimens prepared
to examine mechanical properties.
Two layers of CG fibre mats are kept and the composite
laminate is prepared in single-ply condition. The male part
of the die is kept on the female part after the completion of
layers and 20 kg of weight is applied on the hand lay-up setup
to reduce void formation. The whole set up is left for one day
for the curing process of matrix and reinforcement adhesion.
Specimens are prepared as per ASTM standards using abrasive
water jet cutting process to obtain good surface finish.
The fibre and matrix weights are calculated to attain 35%
of fibre volume fraction after laminate preparation. Mike J
Clifford et al. [42] investigated the best fibre volume fraction
for flax fibre yarn reinforced laminates. They showed it to be
∼35%, to obtain reasonable mechanical properties. They also
derived the equation to calculate fibre volume fraction of a
laminate analytically. Eq. (3) [42] is used to calculate the fibre
volume fraction of CG fibre reinforced laminate after fabrica-
tion.
c mf
Fibre volume fraction (Vf ) = (3)
f mc
where, c = Density of composite (1.16 g/cm3 ); mf = Mass of the
fibre (92 g); f = Density of fibre (g/cm3 ) = 1.19 g/cm3 ; mc = Mass
of the composite (257 g); Vc = Volume of the Composite
(.552 × 20 × 20) cm3 .
The density of the CG fibre yarn laminate could be calcu-
lated by measuring the mass and volume of the laminate.
The main drawback of hand layup process is the forma-
tion of voids; this may be reduced by creating vacuum bagging
 j m a t e r r e s t e c h n o l . 2 0 2 0;9(6):12187–12200
Table 4 – Physical properties of 4 wt.% CG fibre reinforced
fabricated laminate.
Sl. No. Property
1. Fibre volume fraction (%)
2 Theoretical density (g/cm3 )
3 Experimental density (g/cm3 )
2 Void content (%)
as well as applying rollers for the penetration of resin in
between the fibre yarns in the fabrication process [43]. Many
factors are involved in the formation of voids in the fabrica-
tion process; curing pressure plays an important role in the
void formation. By controlling the curing pressure the voids
can be reduced considerably and the mechanical properties
increased correspondingly [44]. Void volume fraction in the
fabricated laminate can be calculated using Eq. (4) [45] and
tabulated in Table 4.
 
%mmatrix %mfibre
Vv = 100 − composite + (4)
matrix fibre
where, Vv = Void volume fraction (%); %mmatrix = Percentage of
matrix mass present in the fabricated laminate (64.20 wt.%);
%mfibre = Percentage of fibre mass present in the fabricated lam-
inate (35.80 wt.%); m and f = density of the matrix and CG
fibre (1.19 g/cm3 for both fibre and matrix).
Table 4 indicates the optimum level of parameters obtained
by taking the quantity of the raw materials in a suitable man-
ner referred from literature. Precautions could be taken to
Fig. 5 – Alkali-treated CG fibre mats for contact angle measurement.
12193
reduce void content by applying vacuum bag gaging and grad-
ual curing pressure. It leads to achieve minimal void content of
acceptable value as 2.52 [42], this will lead to producing better
Value
mechanical properties evidently.
34.9
1.19 2.7. Mechanical and morphological properties
1.16 ± 0.025
2.52 ± 0.003
2.7.1. Tensile test
Tensile properties of CG fibre yarn reinforced laminates were
tested according to ASTM Standards D638 [31] at Microlabs
situated in Ambattur, Chennai. Crosshead movement of with
a feed 1 mm/min by a gradual increase in load applied up to
ultimate loading point. Three identical specimens were tested
in UTM to produce repeatability. CG fibre laminate prepared
by using two layers with 0◦ orientation and three specimens
are cut along the direction and three specimens are cut at 90◦
direction (ref: Fig. 3). Two strain gauges are fixed in the gauge
length of the specimen to measure linear and lateral strains.
Young’s modulus and Poisson’s ratio are calculated from the
stress-strain curve of the tested samples in both orientations.
2.7.2. Flexural test
Three-point bend test (Flexural Test) is performed according
to ASTM standards D790 in a Universal Testing Machine (UTM)
at Microlabs Ambattur, Chennai. The flexural test allows mea-
surements regarding the Dynamic condition of the material.
The specimens are taken with well-defined dimensions of
length, width and thickness (100 × 12.7 × 5.3 mm). The spec-
imen is tested with a crosshead speed of 1 mm/min under
uniform load in the UTM machine. Three specimens were
12194 j m a t e r r e s t e c h n o l . 2 0 2 0;9(6):12187–12200

Fig. 6 – Contact angle measurement on alkali-treated CG fibre with droplet.

specimens was coated with auto fine coater before taking

Table 5 – Measured contact angle for various treated CG
fibre. Evidently appropriate choice of the alkali microstructural images to improve the absorption of electrons
concentration is key to reducing hydrophilicity. and to produce better images. Scanning Electron micrographs
were taken with a magnification of 100 X with the voltage
Sl. No Alkali Contact angle Increase in
concentration (◦ ) angle (%) range of 5–30 kV to analyse morphological features of the lam-
(wt.%) inates at SAIF, IIT Madras.

1 0 70 00.00
2 1 98 40.00
3 2 102 45.71
4 3 108 54.29
2.8. Optimization of alkali concentration in CG fibre
5 4 112 60.00
6 5 75 07.14
2.8.1. Optimization of alkali concentration in CG fibre
using contact angle method
tested and results were derived from the flexural test data. The alkali-treated CG fibre with concentration ranges from 0%
Flexural strength and modulus calculated using the following to 5% is prepared as small mats and are shown in Fig. 5.
Eqs. (5) and (6). [46,47] Water droplets are dropped using a syringe and the
droplets are captured using Nikon DSLR D3400 camera with
3fl
Flexural strength (F) = (N/mm2 ) (5) 24.2-megapixel resolution. The captured images are then
2bd2
transferred to Image Pro software and the surface contact
angles are measured. The images of a droplet on the mats are
ml3
Flexural modulus (EI) = (N/mm2 ) (6) shown in Fig. 6 and measured contact angles are tabulated
4bd2
systematically (Table 5).
where, f = maximum load until rupture (295 N); m = slope Table 5 shows an increase in contact angle – from raw fibre
between load and deflection (295/3.4) in N/mm; L = free length to 4% alkali-treated samples. Increase in NaOH concentration
of the specimen (67.82 mm); b = breadth of the specimen removes the impurities as well as voids present in the cellu-
(12.7 mm); d = depth of the specimen (5.34 mm). lose. The reduction in voids decreases the water absorption
of the CG fibre. Table 5 shows that 4 wt.% alkali-treated CG
2.7.3. Morphological properties – SEM analysis fibre produces highly obtuse angle; this indicates the optimum
Tensile strength tested specimens are used to study about fail- alkali concentration of CG fibre. This is consistent with our
ure characteristics of CG fibre yarn laminate through scanning previous work [25] wherein we fabricated CG fibre reinforced
electron microscopy (SEM). Fractured area of tensile tested spring with various concentration of alkali-treated CG fibre.
 j m a t e r r e s t e c h n o l . 2 0 2 0;9(6):12187–12200 12195

Fig. 7 – Microscopic examination of alkali-treated CG fibre with untreated CG fibre. (a) 0% – in the raw material, impurities
cover the voids of the fibre; (b) 1% – initial stage of elimination of impurities and partial opening of voids; (c) 2% – fully open
of voids and partial removal of impurities.

Fig. 8 – Microscopic examination of alkali-treated CG fibre with various concentration. (a) 3% – initial breakage of voids and
incomplete removal of impurities; (b) 4% – breakage of voids and complete removal of impurities; (c) 5% – breakage of voids
and also fibres indicating the presence of excess hydroxyl groups; (d) a clear image of xylem (void) structure and breakage
of xylem vessel identified in high magnification (40×).

2.8.2. Optimization of alkali concentration in CG fibre
using microscopic examination of voids (xylem)
Alkali-treated CG fibre with various concentrations has been
observed through a binocular microscope to study about
xylem structure. Eradication of voids takes palace while
increasing the alkali concentration, but full elimination of
voids is not possible due to excess rupture of cellulose takes
place when the alkali-concentration increases.
Fig. 7 shows the images of alkali-treated fibres, along with
untreated CG fibres – ranging from 1 wt.% to 5 wt.% treated
samples. Fig. 7(a) shows the presence of impurities such as
waxy layers and lignin layers on cell walls. Fig. 7(b) indicates
the presence of tracheid in the spiral shape; this acts as voids
in the fibre. This, in fact, is an indication of the elimination of
impurities due to the sodium hydroxide treatment. Fig. 7(c)
illustrates the 2 wt.% alkali-treated fibre which shows clear
indications of voids and partial elimination of impurities.
Fig. 8(a) shows the initial breakage of voids and the near-
complete elimination of impurities through the increase of the
sodium hydroxide solution concentration to 3 wt.%. Fig. 8(b)
shows complete elimination of waxy and lignin layers present
in the cell wall (fibre); also the breakage of voids is clear.
Fig. 8(c) shows the breakage of voids as well as the rupture
of cellulose owing to the presence of excess hydroxyl groups
12196 j m a t e r r e s t e c h n o l . 2 0 2 0;9(6):12187–12200
Fig. 9 – Variation of peak intensity between 4 wt.%
alkali-treated CG fibre with untreated CG fibre.
in the 5 wt.% solution of NaOH (aq.) [27]. Fig. 8(d) indicates that
the voids collapse, as seen in this high magnification (100×).
2.8.3. Justification of Alkali concentration in CG fibre
using FTIR analysis
FTIR analysis is used to analyse the impact of alkali treatment
of the CG fibre as well as to justify the results obtained from
new techniques such as contact angle measurement and void
examination in the fibre. FTIR analysis done for various alkali
concentrated CG fibres ranges from 0% to 5%. The maximum
difference in peak intensities observed in 4 wt.% alkali-treated
fibre and the same compared with untreated fibre[29-30]. Fig. 9
shows the peak difference in the graph and Table 6 shows the
difference in arbitrary units between treated and untreated
fibres. Table 6 inferred that alkali treatment removes the waxy
layers present in the fibre outer layer as well as water-soluble
sugars present in the fibre in the maximum level when the
NaOH concentration is 4 wt.%.
2.9. Mechanical test properties
In this work, the optimum valued 4 wt.% alkali-treated CG fibre
reinforced laminate fabricated and cut as per ASTM dimen-
sions for tensile testing. The tensile test is carried out in 0◦ and
90◦ orientation of the CG laminate to determine maximum and
minimum strength of fibre reinforced laminate. Fig. 10 shows
the tested specimens of CG fibre laminates after completion
of the test.
The tensile test is done in the universal testing machine
and stress-strain curves are plotted to determine Young’s
modulus and Poisson’s ratio of the material in both major (0◦ )
and minor (90◦ ) directions of load conditions (ref: Fig. 3). Three
specimens were taken in each orientation and tested and the
results obtained with minimal standard deviation of 0.35. Ini-
tially Matrix material is brittle and it has an elastic modulus of
∼2.8 GPa. After reinforcement, CG fibre ductility is observed to
have improved. In fact, it has an elastic modulus of 4.18 GPa in
0◦ orientation specimen and 3.05 GPa in 90◦ orientation. Due to
CG fibre reinforcement young’s modulus increases up to 49.3%
Fig. 10 – Tensile test specimens after breakage. (a) 0◦
orientation specimen after breakage, (b) 90◦ orientation
specimen after breakage.
in 0◦ orientation and up to 8.92% in the 90◦ orientation. Pois-
son’s ratio is 0.38 in major direction and 0.32 in minor direction
of fibre orientation. CG fibre reinforced laminate is anisotropic
in nature, due to delamination when the load applied in the
transverse direction (90◦ ) Table 7 [48] gives the mean value of
tensile test outputs for 0◦ and 90◦ orientations with standard
deviation 0.35.
Fig. 11(a) shows the graph drawn between the induced
stress and strain when the load is applied gradually on the
specimen in both orientations. The graph clearly shows that
the 0◦ orientation of fibre gives better results with the one.
Fig. 11(b) shows the comparison between the matrix and
fibre reinforced laminates in 0◦ and 90◦ . Fig. 11(b) Graph
indicates that 0◦ fibre orientation laminate produces better
performance comparatively; also Young’s modulus and shear
modulus increases by 49.28% and 23.58% in this case.
Table 8 compares the overall consolidated mechanical
properties of tested specimens. Table 8 indicates that CG
fibre reinforcement in the matrix improves the mechanical
properties of composite laminates in 0◦ orientation and 90◦
compared with original matrix properties. Orientation also
impacts on properties of CG fibre reinforced composites; hence
0◦ orientation produces maximum properties than 90◦ orien-
tation laminate.
Table 9 lists the mechanical properties of various plant
fibres used technologically. Some of the natural fibres produce
improved mechanical properties when it is subjected to differ-
ent surface treatments. The mechanical properties of most of
the natural fibres match with the selected natural fibre. Max-
imum level mechanical properties attained in this CG fibre
yarn reinforced laminate by optimising important parameters
while fabricating the laminate by hand lay-up technique.
Tensile tested specimen’s fractured zone of 4 wt.% alkali-
treated fibre laminate specimen micrographs are obtained
 j m a t e r r e s t e c h n o l . 2 0 2 0;9(6):12187–12200 12197

Table 6 – Difference in peak intensity of chemical compounds between 4 wt.% alkali-treated CG fibre with untreated CG
fibre.
S. No. Absorption Chemical Available compounds in fibre 4% alkali-treated Difference in
band (cm−1 ) group fibre – peaks absorption peaks
(intensity in arb. (%) from graph
units)

1. 3600–3000 O–H Cellulose, hemicellulose, and aliphatic 3310 +3

Hydroxyl hydroxyl of lignin
groups
2. 3000–2800 C–H Cellulose, methyl groups of 2810 0
Aliphatic hemicellulose, methoxyl groups of lignin
and alkyl and methylene groups of waxes
groups
3. 1800–1700 C=O Carbonyl of acetyl ester and the carboxyl 1760 −4
of hemicellulose, ketone and carboxyl of
carboxylic acid of lignin, carboxyl ester of
pectin, and carbonyl ester of waxes
4. 1700–1600 C=C Aromatic group of lignin 1690 −65
5. 1500–1300 O–CH3 , Methoxyl group of lignin 1450 −61
O–H, C–H
6. 1300–1200 C–O–C, Presence of ether in lignin 1290 −58
C–C
7. 1200–1000 C–O Alcohol of cellulose, aliphatic alcohol and 1020 −57
ethers of lignin and pectin
8. 900–800 C–O–C, Aromatic hydrogen of lignin (weakest 810 −30
C–C intensity)
9. 800–700 C–H Aromatic hydrogen of lignin (weakest 740 −74
intensity) and waxes

Table 7 – Mean values of load, stress, strain in axial and lateral directions for 0◦ and 90◦ orientation specimens.
S. No. 0◦ specimen orientation 90◦ specimen orientation

Load (N) Axial stress (MPa) Axial strain Lateral strain Load (N) Axial stress (MPa) Axial strain Lateral strain

1. 101 1.48 0.004 0.001 78 1.38 0.002 0.002

2. 779 12.16 0.008 0.003 533 9.10 0.004 0.002
3. 955 19.00 0.010 0.005 800 14.80 0.006 0.002
4. 1213 30.25 0.012 0.006 1001 22.68 0.008 0.003
5. 1493 39.76 0.015 0.008 1212 28.90 0.009 0.004
6. 1838 50.79 0.018 0.010 1490 36.13 0.010 0.004
7. 2526 62.63 0.022 0.011 1777 40.60 0.011 0.004
8. 3453 90.49 0.027 0.012 2023 45.07 0.013 0.005
9. 4162 109.73 0.033 0.014 2168 50.53 0.015 0.005
10. 4817 137.05 0.037 0.015 2369 54.70 0.017 0.006
11. 5891 154.03 0.041 0.017 2471 59.80 0.019 0.006
12. 6761 171.14 0.046 0.018 2667 65.63 0.021 0.007
13. 8083 207.24 0.050 0.019 2861 71.27 0.023 0.007

Table 8 – Mechanical properties of 0◦ and 90◦ orientation specimens compared with epoxy resin properties.
S. No Properties Properties of epoxy resin After CG fibre reinforcement

◦
0 orientation specimen 90◦ orientation specimen

1 Ultimate tensile stress (MPa) 52.00 207.24 71.27

2 Yield stress (MPa) – 165.79 57.02
3 Young’s modulus (GPa) 02.80 4.18 ± 0.282 3.05 ± 0.244
4 Elongation at break (%) 11.00 4.97 ± 0.206 2.33 ± 0.047
5 Poisson’s ratio 00.14 0.38 ± 0.014 0.314 ± 0.024
6 Shear modulus (GPa) 01.23 1.52 ± 0.103 1.16 ± 0.113

from the scanning electron microscope analysis [56]. Fig. 12(a)
confirms the failure of the specimen initiated from the matrix
and not from the fibre while observing specimens SEM image
after the tensile test; this shows that CG fibre reinforcement
improves the property of the composite laminates. Fig. 12(b)
ensures the uniform distribution of matrix and fibre as well as
a negligible amount of void present in it.
Fig. 12(a) shows the microstructure and failure occurring
in the fractured specimens of tensile test. Fig. 12(a) shows the
fracture of the matrix and there is a pulling force between the
12198 j m a t e r r e s t e c h n o l . 2 0 2 0;9(6):12187–12200

Fig. 11 – Tensile test results: (a) stress-strain curves for 0◦ and 90◦ orientation specimens, and (b) properties comparison of
matrix, 0◦ and 90◦ fibre oriented-reinforcement (with respect to matrix).

Table 9 – Mechanical properties of existing natural fibre laminates with CG fibre yarn laminate.
Sl. No Natural fibre Tensile Young’s Strain at Flexural Flexural Density References
strength modulus break (%) strength modulus (Ef ) (g/cm3 )
(MPa) (GPA) (MPa) (GPa)

1 Calotropis Gigantea 207.24 4.18 4.97 82.87 3.50 1.16 –

fibre yarn (4 wt.% NaOH
treated)
2 Coir fibre(5 wt.% NaOH 23.80 2.96 0.52 40.40 3.75 1.15–1.46 [49]
treated)
3 Bamboo fiber (6 wt.% 363.00 11.20 3.30 84.30 4.91 0.60–1.10 [50]
NaOH treated)
4 Jute (5 wt.% NaOH 12.46 1.05 1.50–1.80 38.68 3.08 1.30–1.46 [51]
treated)
5 Date Palm fibre 25.62 1.36 7.00 34.68 1.85 1.10 [52]
(1 wt.%NaOH
treated)/PP/EPDM
6 Ramie fibre untreated 86.00 9.56 2.0–3.8 103.00 – 1.50 [53]
7 Sisal fibre untreated 8.63 1.31 3.00 39.00 3.05 1.33–1.50 [54]
8 Flax fibre untreated 68.29 5.87 1.98 101.57 2.14 1.50 [55]
(weft direction)

Fig. 12 – SEM Analysis results (a) SEM image shows matrix failure in the composite, (b) Presence of voids and uniform
distribution of matrix and fibre.
 j m a t e r r e s t e c h n o l . 2 0 2 0;9(6):12187–12200
fibre and matrix that result in a twisting action prior to fail-
ure. Fig. 12(b) implies that the uniform distribution of matrix
and fibre and formation of the negligible amount of void in
between matrix and fibre.
3. Conclusion
Many of the researchers concentrate on natural fibres in short
form as reinforcement due to its easiness to fabricate the
composite laminates. Short form of fibres is cannot able to
reinforce in long and continuous structures. In this research
work, this main drawback was addressed and CG fibre yarn
is taken to reinforce in laminates. Initially, CG fibre yarn
and fabrication parameters were optimised to produce bet-
ter mechanical properties. Alkali-treated natural fibre yarn of
Calotropis Gigantea (CG), a tropical shrub with high seasonal-
ity, is used as reinforcement for a laminate. The hygroscopic
nature of the natural fibre is substantially reduced by using an
alkali treatment. The optimum concentration of NaOH in sur-
face treatment of fibre is found using new techniques in a short
time. 4 wt.% alkali-treated CG fibre produces better mechan-
ical properties comparatively due to reduction in the volume
of voids present in the fibre. This, in fact, leads to an increase
in contact angle – from an acute angle to obtuse angle 112◦
(60%).
Presence of voids and impurities are eliminated through
the use of NaOH (aq.) (4 wt.%). Past this concentration, cellu-
lose ends up having excess hydroxide groups which reduce the
strength of the fibre. Observation of xylem structure (voids)
through microscopic examination of CG fibre also shows a
reduction of tracheid pores. FTIR analysis is used to justify
the impact of alkali treatment of the fibre.
4 wt.% alkali-treated CG fibre yarn reinforced using Araldite
matrix in 0◦ orientation produces high elastic modulus
(4.18 GPa) with an ultimate tensile strength of 207.24 MPa. A
lower modulus of 3.05 GPa and ultimate tensile strength of
71.27 MPa is observed for the 90◦ oriented sample. This is due
to ease delamination of fibre from the matrix in the latter.
Fractography of the samples is also studied using scanning
electron micrography. It indicates that fracture initiated from
the matrix and move to the fibre gradually, hence fibre pro-
duces strength to the matrix in the reinforced composites.
Given the prospects generated by this work, we anticipate
further activities to be spurred in use of tropical shrubs,
duly treated, for developing novel mechanical fibre yarn com-
posites to produce continuous products in structural and
engineering applications.
Conflicts of interest
The author declares no conflicts of interest.
references
[1] Joshi SV, Drzal LT, Mohanty AK, Arora S. Are natural fiber
composites environmentally superior to glass fiber
reinforced composites? Compos Part A Appl Sci Manuf
2004;35(3):371–6.
12199
[2] Paulo P, Hugo C, Hafiz S, Marco L. Natural fibre composites
and their applications: a review. J Compos Sci 2018;2:1–20.
[3] Mazlan N, Ramli N, Ando Y, Leman Z, Abdan K, Aziz AA, et al.
Natural fiber for green technology in automotive industry: a
brief review. IOP Conf Ser Mater Sci Eng 2018;368(1):1–8.
[4] Sen T, Jagannatha Reddy HN. Application of sisal, bamboo,
coir and jute natural composites in structural upgradation.
Int J Innov Manage Technol 2011;2(3):186–91.
[5] Ganeshan P, NagarajaGanesh B, Ramshankar P, Raja K.
Calotropis gigantea fibers: a potential reinforcement for
polymer matrices. Int J Polym Anal Charact 2018;23(3):271–7.
[6] Summerscales J, Dissanayake NPJ, Virk AS, Hall W. A review
of bast fibres and their composites: Part 1. Fibres as
reinforcements. Compos Part A Appl Sci Manuf
2010;41(10):1329–35.
[7] Ashori A, Bahreini Z. Evaluation of calotropis gigantea as a
promising raw material for fiber-reinforced composite. J
Compos Mater 2009;43(11):1297–304.
[8] Ramasamy R, Obi Reddy K, Varada Rajulu A. Extraction and
characterization of calotropis gigantea, bast fibers as novel
reinforcement for composites materials. J Nat Fibers
2017;15:527–38.
[9] Ekundayo G, Sam A. Reviewing the development of natural
fibre composites: a case study of Sisal and Jute. Am J Mech
Mater Eng 2019;3(1):1–10.
[10] Ismail AE, Che Abdul Aziz MA. Fatigue strength of woven
kenaf fiber reinforced composites. IOP Conf Ser Mater Sci
Eng 2015;100:1–9.
[11] Martinez JG, Richter K, Persson NK, Jager EWH. Investigation
of electrically conducting yarns for use in textile actuators.
Smart Mater Struct 2018;27:1–10.
[12] Bora R, Padmini T. Fiber extraction from Calotropis gigantea
stem with different retting methods and its comparison. Int J
Chem Stud 2019;7(3):144–50.
[13] Li X, Tabil LG, Panigrahi S. Chemical treatments of natural
fiber for use in natural fiber-reinforced composites: a review.
J Polym Environ 2007;15(1):25–33.
[14] Ma E, Zhou H, Xu R. Effects of removal of chemical
components on moisture adsorption by wood. Biosources
2016;11:3110–22.
[15] Asif M. Sustainability of timber, wood and bamboo in
construction. Sustain Constr Mater 2009:31–54.
[16] Mukhopadhyay S, Fangueiro R. Physical modification of
natural fibers and thermoplastic films for composites – a
review. J Thermoplast Compos Mater 2009;22(2):135–62.
[17] Koohestani B, Darban AK, Mokhtari P, Yilmaz E, Darezereshki
E. Comparison of different natural fiber treatments: a
literature review. Int J Environ Sci Technol 2019;16(1):629–42.
[18] Gibson LJ. The heirarchial structure and mechanics of plant
materials. J R Soc Interface 2012;9:2749–66.
[19] Asim M, Jawaid M, Abdan K, Ishak MR. Effect of alkali and
silane treatments on mechanical and fibre-matrix bond
strength of kenaf and pineapple leaf fibres. J Bionic Eng
2016;13:426–35.
[20] Oushabi A, Sair S, Oudrhiri Hassani F, Abboud Y, Tanane O, El
Bouari A. The effect of alkali treatment on mechanical,
morphological and thermal properties of date palm fibers
(DPFs): study of the interface of DPF e polyurethane
composite. South Afr J Chem Eng 2017;23:116–23.
[21] Afolabi LO, Megat-Yusoff PSM, Moahamad Ariff Z, Hamizol
MS. Fabrication of pandanus tectorius (screw-pine) natural
fiber using vacuum resin infusion for polymer composite
application. J Mater Res Technol 2019;8:3102–13.
[22] Hassan MZ, Sapuan SM, Roslan Siti Amni, Aziz SA, Sarip S,
Optimization of tensile behavior of banana pseudo-stem
(Musa acuminate) fiber reinforced epoxy composites using
response surface methodology, J Mater Res Technol.
12200 j m a t e r r e s t e c h n o l . 2 0 2 0;9(6):12187–12200
[23] Prasanna Venkatesh R, Ramanathan K, Srinivasa Raman V.
Tensile, flexural, impact and water absorption properties of
natural fibre reinforced polyester hybrid composites. Fibres
Text East Eur 2016;24(3):90–4.
[24] Mehmood S, Madsen B. Properties and performance of flax
yarn/thermoplastic polyester composites. J Reinf Plast
Compos 2012;31:1746–57.
[25] Renugadevi K, Devan PK, Thomas T. Fabrication of Calotropis
Gigantea fibre reinforced compression spring for light weight
applications. Compos Part B Eng 2019;172:281–9.
[26] Punyamurthy R, Venkateshappa SC, Dhanalakshmi S,
Bennehalli B. Effect of alkali treatment on water absorption
of single cellulosic abaca fiber. Bioresources 2012;7:3515–24.
[27] Oushabi A, Sair S, Oudrhiri Hassani F, Abboud Y, Tanane O.
The effect of alkali treatment on mechanical, morphological
and thermal properties of date palm fibers (DPFs): study of
the interface of DPF–Polyurethane composite. South Afr J
Chem Eng 2017;23:116–23.
[28] Marina V, Katie P, Fachuang L, John R, Ray H, Daniel Jones A,
et al. Molecular and biochemical basis for stress-induced
accumulation of free and bound p-Coumaraldehyde in
cucumber. Plant Physiol 2011;157:1056–66.
[29] Romanzini D, Ornaghi HL, Amico SC, Zattera AJ. Preparation
and characterization of ramie-glass fiber reinforced polymer
matrix hybrid composites. Mater Res 2012;15:415–20.
[30] Gonzalez M, Cabanelas JC, Baselga J. Applications of FTIR on
epoxy resins–identification, monitoring the curing process,
phase separation and water uptake. In: Infrared spectroscopy
– materials science engineering and technology. Spain:
University Carlos III Madrid; 2012. p. 261–84.
[31] Muthukumar V, Venkatasamy R, Sureshbabu A, Arunkumar
D. A study on mechanical properties of natural fiber
reinforced laminates of epoxy (LY 556) polymer matrix
composites. Int J Prod Technol Manage Res 2011;2:67–72.
[32] Jayamani E, Loong TG, Bin Bakri MK. Comparative study of
Fourier transform infrared spectroscopy (FTIR) analysis of
natural fibres treated with chemical, physical and biological
methods. Polym Bull 2019:0123456789.
[33] Rask M, Madsen B. Twisting of fibres in yarns for natural fibre
composites. In: 18th international conference on composite
materials (ICCM). 2011. p. 1–5.
[34] Naik NK, Madhavan V. Twisted impregnated yarns: elastic
properties. J Strain Anal Eng Des 2000;35:83–91.
[35] Clifford MJ, Shah DU, Schubel PJ. Modelling the effect of yarn
twist on the tensile strength of unidirectional plant fibre
yarn composites. J Compos Mater 2013;47:425–36.
[36] Wang HW, Zhou HW, Gui LL, Ji HW, Zhang XC. Analysis of
effect of fibre orientation on Young’s modulus for
unidirectional fibre reinforced composites. Compos Part B
Eng 2014;56:733–9.
[37] Cordin M, Bechtold T, Pham T. Effect of fibre orientation on
the mechanical properties of polypropylene–lyocell
composites. Cellulose 2018;25:7197–210.
[38] Omrani E, Menezes PL, Rohatgi PK. State of the art on
tribological behavior of polymer matrix composites
reinforced with natural fibres in the green materials world.
Eng Sci Technol 2016;19:717–36.
[39] Yousif BF, Chin CW. Potential of kenaf fibres as reinforcement
for tribological applications. Wear 2009;267:1550–7.
[40] Lee JK, Kwak SW, Ha J-H, Lee WC, Kim HC, Research article,
Bioinorganic chemistry and applications, vol. 2017, Article ID
2582849, 8 p.
[41] https://www.generaladhesivos.com/proveedor-pegamento/
888hoja-tecnica-Aradur%20HY-951.pdf.
[42] Clifford MJ, Shah DU, Schubel PJ, Licence P. Determining the
minimum, critical and maximum fibre content for twisted
yarn reinforced plant fibre composites. Compos Sci Technol
2012;72(15):1909–17.
[43] Marques AT. Fibrous and composite materials for civil
engineering applications. Woodhead Publishing Limited;
2011. p. 191–215.
[44] Liu X, Chen F. A review of void formation and its effects on
the mechanical performance of carbon fiber reinforced
plastic. Eng Trans 2016;64:33–51.
[45] Wang H, Memon H, Arshad Ali M. Effect of jute fiber
modification on mechanical properties of jute fiber
composite. Materials 2019;12:1–11.
[46] Monteiro SN, Braga FO, Margema JI, Gomes VA, Margem FM,
Ribeiro CGD. Flexural behavior of epoxy matrix composites
reinforced with malva fiber. Mater Res 2015;18:114–20.
[47] Salman SD, Leman Z, Sultan MTH, Ishak MR, Cardona F.
Influence of fiber content on mechanical and morphological
properties of woven kenaf reinforced PVB film produced
using a hot press technique. Int J Polym Sci 2016:1–11.
[48] Verma CS, Chariar VM, Purohit R. Macro mechanical analysis
of Bamboo lamina. Int J Chem Petrochem Technol
2012;2:1–11.
[49] Yan L, Chouw N, Huang L, Kasal B. Effect of alkali treatment
on microstructure and mechanical properties of coir fibres,
coir fibre reinforced-polymer composites and
reinforced-cementitious composites. Constr Build Mater
2016;112:168–82.
[50] Liang W, Zhang K, Wang F, Wang Z, Duan Z, Yang B. Thermal
and mechanical properties of bamboo fiber reinforced epoxy
composites. J Polym 2018;10:1–18.
[51] Gopinath A, Senthil Kumar M, Elayaperumal A. Experimental
investigations on mechanical properties of jute fiber
reinforced composites with polyester and epoxy resin
matrices. In: 12th Global Congress on Manufacturing and
Management, GCMM, Procedia Engineering.; 2014. p.
2052–63.
[52] Farsani RE. Effect of fibre treatment on the mechanical
properties of date palm fiber reinforced PP/EPDM
composites. J Adv Compos Mater 2015;24:27–40.
[53] Irawan AP, Soemardi TP, Widjajalaksmi K, Reksoprodjo AHS.
Tensile and flexural strength of ramie fiber reinforced epoxy
composites for socket prosthesis application. Int J Mech
Mater Eng 2011;6:46–50.
[54] Ibrahim ID, Jamiru T, Sadiku ER, Kupolati WK, Agwuncha SC,
Ekundayo G. Mechanical properties of sisal fibre-reinforced
polymer composites: a review. Compos Interfaces
2016;23:15–36.
[55] Cerbu C. Mechanical characterization of the flax/epoxy
composite material. In: 8th international conference
interdisciplinarity in engineering, INTER-ENG 2014. Procedia
Technology, vol. 19. 2015. p. 28–75.
[56] Ahmad F, Bajpai PK. Evaluation of stiffness in a cellulose
fiber reinforced epoxy laminates for structural applications:
experimental and finite element analysis. Defence Technol
2018;14:278–86.