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journal homepage: www.elsevier.com/locate/jmrt

Original Article

Investigations on fatigue analysis and biomimetic

mineralization of glass fiber/sisal fiber/chitosan
reinforced hybrid polymer sandwich composites

Soundhar Arumugam a, Jayakrishna Kandasamy a,**,

Mohamed Thariq Hameed Sultan b,c,d,*, Ain Umaira Md Shah c,
Syafiqah Nur Azrie Safri b
a
School of Mechanical Engineering, Vellore Institute of Technology, Vellore, 632014, India
b
Laboratory of Biocomposite Technology, Institute of Tropical Forestry and Forest Products (INTROP), 43400, UPM
Serdang, Selangor Darul Ehsan, Malaysia
c
Department of Aerospace Engineering, Faculty of Engineering, Universiti Putra Malaysia, 43400, UPM Serdang,
Selangor Darul Ehsan, Malaysia
d
Aerospace Malaysia Innovation Centre (944751-A), Prime Minister’s Department, MIGHT Partnership Hub, Jalan
Impact, 63000, Cyberjaya, Selangor Darul Ehsan, Malaysia

article info abstract

Article history: In this study, chitosan/sisal/glass fiber (CS/SF/GF) reinforced hybrid polymer composite for
Received 17 September 2020 femur bone fracture plate was developed. The CS/SF/GF hybrid composite possesses
Accepted 30 November 2020 exclusive sandwich assembly and includes epoxy/GF/CS as the peripheral layers and
Available online 17 December 2020 epoxy/CS/SF as the inner layers. The composite arrangement be similar to the human bone
assembly spongy interior cancellous medium and stiff peripheral cortical. The objective of
Keywords: this investigation was to determine the fatigue properties of CS/SF/GF hybrid sandwich
Hybrid polymer composites composites, because cyclical loading is the foremost loads experienced by a femur plate
Tensile properties during normal day to day activities such as walking and running. Tensile and fatigue
Fatigue behavior properties were studied as per ASTM (D3039 and D3479) standards. Morphological behav-
Simulated body fluid iour of fractured fatigue samples was considered using scanning electron microscope. The
Bone plate biomimetic activity of CS/SF/GF composites was examined using biomimetic mineraliza-
tion techniques with the help of simulated body fluid (SBF). The tensile study results
proved that the A6 hybrid CS/SF/CTS composites impart higher ultimate tensile strength of
146 MPa and tensile modulus of 6.814 GPa compared to other combinations. The fatigue
results revealed that the fatigue life of A5 hybrid CS/SF/GF composites withstand more
than 1 million cycles (1.20
106) compared to other combinations. The presence of bone
like apatite layer (Ca, Sr, Pb, Si, Ba, K, Pd and CI) from Simulated Body Fluid (SBF) onto CS/
SF/GF layer were confirmed by XRD, SEM-EDAX and FT-IR. Further, the calcium/phosphate
(Ca/P) ratio was found to be approximately 1.67 which is needed for the biological apatite
layer formation, this proved the formation of apatite layer on the CS/SF/GF composite
surface. The experimental test results proved that GF/SF/CTS/EP hybrid composite can be
used for orthopaedic bone fracture plate applications.

* Corresponding author.
** Corresponding author.
E-mail addresses: mail2jaikrish@gmail.com (J. Kandasamy), thariq@upm.edu.my (M.T.H. Sultan).
https://doi.org/10.1016/j.jmrt.2020.11.106
2238-7854/© 2020 The Author(s). 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/).
 j o u r n a l o f m a t e r i a l s r e s e a r c h a n d t e c h n o l o g y 2 0 2 1 ; 1 0 : 5 1 2 e5 2 5
© 2020 The Author(s). 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/).
1. Introduction
Fiber reinforced polymer composites (FRPC) are being pro-
gressively utilized in different structural applications like
wind turbine blade, airframes and ship hulls. The components
of such structure are subjected to different sorts of fatigue and
static loads [1]. Therefore, from certification and safety view-
point of these polymer composites, FRPC structures should
possess more fracture toughness and fatigue resistance [2].
FRPCs are widely utilized as metallic alloy substitute to
possess extraordinary mechanical properties in contrast to
metal alloys [3].
Fatigue is a phenomenon related with the damage progress
in a material when subjected to below the ultimate strength of
applied loading cycles for a prolonged period [4]. In many
applications like marine, automotive, and biomedical, the
most important property is resistance to fatigue. Behaviour of
fatigue in various natural fibre composites are examined by
several researchers [5,6,7]. However, limited work related to
synthetic/natural hybrid composites fatigue life estimation
has been reported [8]. Liao and Thew (2003) studied the hy-
bridization effect of glass and bamboo fiber reinforced poly-
mer sandwich composites. Results revealed that
hybridization of bamboo and glass fiber improved the fatigue
life of the composites [9]. Wu et al. (2010) reported the fatigue
nature of various fibre composites like basalt, benzobisox-
azole, polyparaphenylene, glass and carbon. The authors
concluded that epoxy/carbon/basalt composites showed im-
provements in fatigue resistance as compared to basalt/epoxy
composites [10]. Shahzad (2011) investigated the effect of
layering sequence on hemp-glass reinforced polyester com-
posites using compression moulding. The results of fatigue
analysed showed that, placing hemp fibres as the peripheral
layer and glass fiber as the innermost layer to improve the
fatigue strength of the composites as compared to inner layer
of hemp fibres and two outer layers of glass fibres [11]. Jaga-
nathan et al. (2013) investigated the glass fiber reinforced
hybrid composite subjected to spectrum load condition of
standard helicopter rotor for fatigue life prediction. It is
noticed, during the fatigue loading period the stiffness dete-
rioration of the neat epoxy glass fiber is higher in contrast to
modified epoxy glass fiber composites. The modified glass
fiber composite show diminished crack and delamination
progress level that enhances the fatigue under spectrum load
order [12]. Asim and Isaac (2014) examined the lifespan of
fatigue hemp fiber and glass FRC in tensionetension mode.
The study results showed hemp fiber composites to exhibit
lesser fatigue sensitivity as compared with glass fiber. The
authors recommend hemp fibre as a suitable alternate for
glass fiber under fatigue loading conditions [13]. Liang et al.
(2012) reported the fatigue behaviour of glass and flax fiber
epoxy composites under tensionetension mode. They
concluded that under fatigue load, the stiffness of glass/epoxy
513
composites decreases considerably as compared to flax/epoxy
composites. The modulus of glass/epoxy deteriorated up to
25% of true modulus, remarkably flax/epoxy showed increase
in modulus up to 2% under fatigue load conditions [14].
Bagheri et al. (2014) investigated that the fatigue properties of
carbon fiber/flax/epoxy composite for bone fixation applica-
tion. The results confirmed that carbon fiber/epoxy/flax
composite possess high cycle fatigue strength in the range of
200e220 MPa, which is comparable to clinical conditions on
the femur during day to day activities [15].
Mostfa (2019) studied the fatigue and tensile behaviour of
woven glass/jute/epoxy composites. The results showed that
inclusion of jute fibres to reduce the fatigue sensitivity of
hybrid composites. The study recommends that the biode-
gradable natural fibres may possibly suitable to hybridize with
glass fibres for structural applications under cyclic loading
[16]. Suhad et al. (2016) reported the tensile-compression
behaviour of woven kenaf fiber reinforced composites. The
hybrid composite showed increase in tensile properties in
contrast to compression, owing to sandwich configuration
effect, and also revealed that the fatigue life of the composite
improved by reducing maximum applied stress [17]. Branco
et al. (2008) observed that stress ratio (R) as a significant
constraint that affect the fatigue strength. In common, a rise
in R causes decrease in fatigue properties of the composites.
The fatigue behaviour of composite specimens has been done
with a stress ratio series from 1 to 1 [18]. Fatigue mode
assumed on the stress ratio can be categorized into three
types, Tension-Compression (∞ ˂ R ˂ 0), TensioneTension
(0  R  1) and Compression- Compression (1 ˂ R ˂ ∞) [19].
Researchers reported that the composite laminates develop
temperature at higher frequency under cyclic loading that
affects the fatigue life of the composites. They recommended
to maintain the frequency below 5 Hz to prevent the specimen
from heating [20,21].
Table 1 summarizes the fatigue testing literature of syn-
thetic/natural fibre reinforced composites. Under fatigue
loading conditions, hardening effect has been observed in
natural fibres. The hardening effect shows a growth in the
natural fibres modulus, which causes an improvement in the
Table 1 e Fatigue test reported on synthetic/natural fiber
composites.
Reinforcement Matrix Reference
Glass/bamboo Polypropylene Thew and liao (2003) [9]
Glass/hemp Polyester Shahzad (2011) [11]
Carbon/flax Epoxy Bagheri et al. (2014) [15]
Glass/flax Epoxy Asgarinia et al.(2015) [23]
Glass/kenaf Polyester Sharba et al. (2016) [43]
Kevlar/kenaf Epoxy Suhad et al.(2016) [17]
Glass/kenaf Epoxy/polypropylene Sivakumar et al. (2018) [24]
Glass/jute Epoxy Mostafa (2019) [16]
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fatigue strength [22,23]. Sivakumar et al. (2017) prepared
hybrid composites using kenaf/glass fiber with different
combination of matrix materials such as polypropylene and
epoxy resin. Results proved that the ultimate tensile strength
and tensile modulus of epoxy/kenaf/glass hybrid composites
are about 15 and 17% higher than those of polypropylene/
kenaf/glass hybrid composites [24]. Seghini et al. (2020) caried
out a comparative study on the fatigue life of a flax/basalt
woven-ply hybrid composites and non-hybrid composites
such as 100% flax and 100% basalt composites. Results proved
that the hybridization improves the fatigue resistance of flax/
basalt hybrid composites. The average fatigue life cycles of
hybrid basalt/kenaf at 35% UTS is 3.30
105 as compared to
non-hybrid composites (8001 cycles) [25]. Prakash et al. (2020)
investigated the fatigue behaviour of Caryota urens fibre rein-
forced epoxy composite. Results imparts that the fatigue
behaviour of silane surfaceemodified C. urens epoxy com-
posite to show high fatigue life cycle of 18,315 for 25% of UTS
as compared to acid and base treated C. urens fibres [26]. Only
few researchers have studied the fatigue properties of syn-
thetic/natural fiber composites, as carrying fatigue trials
would consume longer test period and more number of
specimens to determine the fatigue life of the composites
[26,27]. Therefore, there exist a need for a predicting model to
calculate the number of cycles to failure of the composites.
In general, engineering composite materials consists of a
thermosetting epoxy matrix reinforced by synthetic and nat-
ural fibres [28]. Epoxy is an extremely cross-linked and amor-
phous structure, this cross-linked microstructure brings about
numerous beneficial properties like low creep, high modulus
and failure strength [29]. Conversely, epoxies are brittle and
possess lower resistance to initiation of crack growth which
may impact the fracture and fatigue effect of FRP composite
[30]. Numerous studies have noticeably revealed that en-
hancements in the fatigue life and a decrease in the fatigue
crack progress level of epoxies are witnessed when altered by
accumulation of nanoparticles like carbon nanotubes, silica
nanoparticles and multiwall carbon nanotubes [31,32].
Recently, Soundhar and Jayakrishna (2019) proved that
imbibing chitosan particles in epoxy improves the mechanical
properties of epoxy composite for bone fracture applications
[33]. However, detailed studies on the fatigue nature of chi-
tosan reinforced epoxy resin is newer one. Manteghi et al.
(2017) proposed flax/GF/epoxy sandwich hybrid composite for
the fixation plates of bone fracture [34]. Bagheri et al. (2015)
prepared CF/Flax/Epoxy composite plate for bone fracture
plate. They found that CF/Flax/Epoxy composite plate showed
similar cell viability with no adverse effect on gene expression
levels observed during bone formation in comparison to
medical-grade stainless steel. The study results recommend
that the combination of synthetic/natural fiber as a potential
alternate for bone plate applications [35]. Qiao et al. (2019)
prepared Nano hydroxyapatite/polyamide 66/glass fiber (n-
HA/PA66/GF) composite for bone plate applications. Results
revealed that n-HA/PA66/GF plate could fix the fractures
without breakage and had no interference with radiographic
imaging, and also the histological results showed that new
bone grows at the n-HA/PA66/GF interface region, that in-
tegrates with native bone tissue [36]. Sarwar et al. (2020) pre-
pared a new Kevlar/flax/epoxy (KFE) hybrid sandwich
composite for bone plate applications. Results revealed that
hybridization of kevlar with flax fibers improved the strength
(torsion, tension, and compression), stiffness as well as
moisture absorption of KFE hybrid sandwich composites. The
KFE composites showed higher tensile strength
(201.5e335.7 MPa) and tensile modulus (15.3e30.5 GPa) as
compared to human cortical bone tensile strength
(107e146 MPa) and tensile modulus (11.4e19.1 GPa). This al-
lows the composite plates to carry more load and reduce the
negative effects of stress shielding [37]. Addition of chitosan
particles in sisal and glass fiber surface makes amorphous
structure, this will develop rough surface between sisal fiber
and glass fiber. This rough surface makes mechanical inter-
locking between sisal and glass fiber, this improves the me-
chanical properties of the composites.
The primary objective of this investigation is to determine
fatigue life of chitosan/sisal/glass fiber (CS/SF/GF) reinforced
epoxy composites for bone plate subjected to cyclic stress.
Tension - tension fatigue test was carried out to evaluate the
fatigue behaviour and damage progress of CS/SF/GF compos-
ites. A fatigue model is proposed to predict the fatigue
behaviour of CS/SF/GF hybrid composites based on the fatigue
endurance limit. Further, in vitro bioactivity of the GF/SF/CTS
composites was also studied by soaking the samples in
simulated body fluid for 28 days. The ability of new apatite
layer formation on the surface of the CS/SF/GF composite was
analysed using XRD, FTIR and SEM-EDS.
2. Experimental details
The subsequent subsections discuss about materials used and
preparation of CS/SF/GF composite scaffold in this study.
2.1. Materials
In this study, glass fiber plain intertwined mat and sisal fiber
natural interlaced mats were used as primary reinforcements
and chitosan particles as secondary reinforcement in the
epoxy matrix. Glass fiber interlaced mats were procured from
M/s Go Green products, Chennai, India. Sisal fiber interlaced
mats were purchased from M/s Jolly enterprise, West Bengal,
India. The chemical composition and mechanical properties
of sisal fibre as shown in Table 2. Bisphenol-A epoxy resin and
hardener (HY951) was procured from M/s Seenu & Co, Coim-
batore, India. The properties of glass and epoxy resins as
mentioned in Table 3. High molecular weight of chitosan
Table 2 e Chemical composition and mechanical
properties of Sisal fibre.
Properties Sisal fibre
Chemical composition Cellulose % 64
Hemicelluloses % 22
Lignin % 10.2
Wax % 2
Mechanical properties Density (kg/m3) 1400
Flexural modulus (GPa) 13.5
Tensile strength (MPa) 65
Modulus of elasticity (GPa) 3.5
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Table 3 e Properties of glass and epoxy resins. Table 4 e Descriptions and codes of the fabricated
composite laminates.
Property Epoxy Glass fiber
Sample Chitosan Sisal fiber Glass fiber
Density (g/cm3) 1.16 1.78
description (weight (No. of layers) (No. of layers)
Modulus of elasticity (GPa) 3.0e4.0 73
percentage)
Tensile strength (MPa) 73 3950
Maximum elongation (%) 1.5 3e4 A1 0 3 2
A2 0 4 2
A3 1 3 2
A4 1 4 2
(345,500 g mol1) was procured from M/s India Sea Foods, A5 2 3 2
Kerala, India. Chitosan can be attained by deacetylation of A6 2 4 2
chitin at a deacetylation rate of 85%. A7 3 3 2
A8 3 4 2

2.2. Composite laminate preparation

The CS/SF/GF reinforced composites were prepared using 3. Characterizations

inner layer of sisal/chitosan/epoxy and outer layers of
glass/chitosan/epoxy, producing sandwich structure.
Initially a known quantity of bisphenol-A (Epoxy) and CS
particles of various weight ratio (0 wt.%, 1 wt.%, 2 wt.% and
3 wt.%) was mixed for 30 min using ultrasonic sonicator
(Model e Branson, CPXH Ultrasonic Bath) to achieve uniform
mixture. The hardener was added to the modified epoxyeCS
mixture and the resulting mixture was mechanically stirred
for 15 min.
The resulting mixture was dispensed over the bottom
most layer of glass fiber, and the innermost layer of sisal fibres
were arranged over glass fiber, then top layer of glass fiber/
epoxy/chitosan was placed over sisal fiber to build the sand-
wich configurations of composite laminates as shown in Fig.
1. With the aim of removing additional amount of resin
adhesion with the woven fabric, the CS/SF/GF composite
laminates were placed inside the vacuum bag at room tem-
perature for 24 h. The CS/SF/GF laminates were then detached
from the mould for post curing. The obtained composite
laminate possessed sandwich arrangement with rigid
external coating of synthetic fibres (glass fiber) and internal
coatings of natural fibres (sisal), mimicking the overall
arrangement of femur bone [34]. The designation of the
fabricated sample composites and their compositions are
listed in Table 4.
3.1. Fatigue properties
Tensile test was conducted prior to fatigue testing to deter-
mine the ultimate tensile strength (UTS) of CS/SF/GF com-
posites. Tensile test was conducted as per ASTM D3039 with
the specimen dimension of 165
19
4 mm at strain rate of
2 mm/min using Instron Universal Testing Machine (UTM)
[38]. Three GF/SF/CTS composites samples under each desig-
nated composition (A1 to A8) were tested and the cumulative
value was recorded.
Fatigue behaviour of CS/SF/GF samples were tested using
Instron UTM. The test specimens were prepared as per ASTM
D3479M (250
30
4 mm) [39]. The CS/SF/GF composites were
tested at ambient temperature at loading rate of 5 Hz under
constant displacement. The ratio of minimum and maximum
cyclic stress was kept constant for all the specimens (R ¼ 0.1)
with a sinusoidal wave at a rate of 5 Hz. The test rate was
retained at 5 Hz to avoid temperature impacts which corre-
sponds to decreased fatigue life [40].
3.2. SEM
The surface properties of fractured CS/SF/GF composite lam-
inates were studied using Scanning Electron Microscopy (Carl

Fig. 1 e Preparation of CS/SF/GF Epoxy hybrid composites.

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ZeissEVO18 instrument, Germany). The composite laminates

were coated with gold using sputtering instrument for 10 min
under high vacuum conditions before SEM analysis.

3.3. In vitro biomimetic mineralization

The in vitro bioactivity of CS/SF/GF hybrid combinations was

studied by using simulated body fluid (SBF) whose ion ab-
sorption was matched to that of human blood plasma. SBF
was prepared using reagents such as NaCl (7.996 g), KCl
(0.224 g), NaHCO3 (0.350 g), K2 HPO4.3H2O (0.228 g), CaCl2
(0.278 g), MgCl2.6H2O (0.305 g), (CH2OH)3 CNH2 (6.057 g) and
Na2SO4 (0.071 g). Followed by adding 1 L ion exchanged
distilled water to completely dissolve the reagents and
maintain the pH at 7.40 level [41,42]. The samples of CS/SF/GF
hybrid mixtures with measurements of Fig. 2 e Tensile strength versus tensile modulus for three
10 mm
10 mm
3 mm were soaked in 40 ml SBF for a pre- core sisal fiber composites.
scheduled number of days (5, 15 and 28 days) at 37  C. The
specimens were removed from SBF after immersing at various
chitosan decreases the tensile properties; this is due to the
interval of time. The samples were cleaned using de-ionized
agglomeration of chitosan in sisal fiber. The tensile stress of
water and desiccated in an oven at 40  C to remove the
three core layer of sisal fiber samples A3, A5 and A7 are 4.23%,
moisture content. The samples of the CS/SF/GF combinations
16% and 10.16% higher than A1 composites. Similarly, tensile
were investigated before and after immersing in SBF at
modulus of three core layer of sisal fiber samples A3, A5 and
various interval of time. The formation of apatite constitution
A7 are 3.69%, 11.05% and 8.73% higher than that of A1
was confirmed by XRD, SEM and FT-IR. The XRD peaks of CS/
composites.
SF/GF hybrid sandwich combinations were examined by
The effect of reinforcement on tensile strength of four core
means of Bruker D8 advanced diffractometer using Cu me-
layer sisal fiber composites is shown in Fig. 3. Composite A2
dium at 40 kV and 30 mA. FT-IR spectra were reported by KBr
imparts lower tensile strength due to amorphous nature of the
disk method over 400 to 4000 cm1 wave number limits at
4 cm1 resolution using Shimadzu IR affinity-1 instrument.

4. Results and discussion

4.1. Tensile properties

CS/SF/GF composites tensile properties were determined ac-

cording to ASTM D3039. Tensile test was analysed using
100 kN (Instron 8801) UTM at 2 mm/min crosshead speed. For
confirmation of the results, three values of tensile specimens
were measured for each stacking sequence and the average
values were tabulated in Table 5. Higher tensile strength was
observed for the composite specimen A5 and A6 as compared
with other composite specimens. This is due to the strong
bonding of glass fiber and sisal fibres [43]. From Fig. 2, it is
opined that chitosan loading up to 2 wt. % of three core layer
sisal fiber composites, the tensile strength and modulus Fig. 3 e Tensile strength versus tensile modulus for four
increased considerably. Addition of more than 2 wt. % of core sisal fiber composites.

Table 5 e Tensile properties of CS/SF/GF hybrid composites.

Number of layers Samples Weight percentage (wt.%) Tensile stress (MPa) Tensile Modulus (GPa)
3 layers A1 0 118 ± 2.15 5.498 ± 0.160
A3 1 123 ± 1.21 5.701 ± 0.193
A5 2 137 ± 6.41 6.106 ± 0.178
A7 3 130 ± 4.21 5.978 ± 0.188
4 layers A2 0 122 ± 3.84 6.054 ± 0.153
A4 1 131 ± 3.52 6.576 ± 0.106
A6 2 146 ± 5.30 6.814 ± 0.106
A8 3 139 ± 2.13 6.205 ± 0.197
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composite. High tensile strength is observed in A6 composites,
this is due to uniform dispersion of chitosan particles
exhibited in the composites. Reduced tensile strength is
observed in the A8 composites, due to the addition of more
than 2 wt% chitosan causing agglomeration in the matrix due
to the non-uniform dispersion of chitosan over the composite.
The tensile stress of four core layer of sisal fiber composite
samples A4, A6, A8 are 7.37%, 19.67% and 13.93% higher than
that of A2 composites. Similarly, tensile modulus of four core
layer of sisal fiber samples A4, A6 and A8 are 7.37%, 19.67% and
13.93% higher than that of A1 composites. This results clearly
shows that the addition of chitosan particles enhances the
tensile properties of three and four layer of sisal/glass/epoxy
hybrid composites.
4.2. Properties of tensionetension fatigues
Linear SeN curves was generated for CS/SF/GF composites.
Number of cycles to failure (Nf) is presented in X-axis and the
Y-axis shows the ultimate tensile stress of the fatigue cycle as
shown in Fig. 4. The fatigue test was stopped once the sample
is broken due to fatigue damage. The stress test data vs.
number of cycles to failure for the CS/SF/GF laminates were fit
by using Basquin’s law [44].
in a completely catastrophic and brittle manner, normal to the
applied stress direction. Hence, it is anticipated that loss
progress in fatigue was relatively equivalent to tensile testing
[49]. Composite samples A3, A5, A6 and A7 showed higher
fatigue life compared to A1, A2, A4 and A8 composite samples.
Overall, A5 composite laminates showed higher fatigue life
1.20
106 cycles, this is due to the better interfacial bonding
exhibited by sisal fiber and glass fiber in epoxy matrix, and
also due to the homogeneous mixture of chitosan in the
composites which prevents the crack initiation. Addition of
more than 2 wt.% of chitosan in this composite structure
showed decreasing fatigue life, this is due to the non-uniform
dissemination of chitosan in the composites. Also, addition of
more than three layers of sisal fiber in the composite structure
such as A2, A4, A6 and A8 shows lower fatigue life. The
occurrence of more sisal fiber layers in composite laminates
increases the structure brittleness, which leads to premature
failure.
Eq. (2) shows the curve fitting of CS/SF/GF composite lam-
inates as an expression of their fatigue life. The fatigue life of
obtained by Eq. (2) can effectively be applied to predict the
fatigue life over a definite range of ultimate stresses with high
degree of accuracy (R2 > 0.9539). Table 6 presents the fatigue
properties of CS/SF/GF composites.

sm ¼ s0f ðNf Þb (1) sm ¼ 8267:2ðNf Þ0:308 (2)

where s0f - Fatigue strength coefficient; b - fatigue strength

exponent. Table 6 e Fatigue properties of the CS/SF/GF hybrid
Fatigue life curve of CS/SF/GF composite laminates under composites.
tensionetension cyclic loading are presented in Fig. 4. From Specimen Number of cycles to failure (Nf)
this Fig. 4, it is clearly observed that SeN curve of the CS/SF/GF
A1 4.20
105
composite laminates show downward slope confirming high A2 4.97
105
stress level with minimum number of cycles to failure con- A3 7.37
105
tradictory to lower stress levels [45,46]. Most of the composites A4 5.90
105
failed in tensionetension fatigue in the similar way of static A5 1.20
106
tensile test [47,48]. Similar behaviour was noticed for CS/SF/GF A6 8.01
105
A7 8.36
105
specimens too. The CS/SF/GF composite specimens (A1 to A8)
A8 7.20
105
in fatigue at stress ratio of R ¼ 0.1 and 0.55% of UTS, damaged

Fig. 4 e Stress vs. lifetime (SeN Curves) for CS/SF/GF hybrid composites.
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The current CS/SF/GF hybrid composite A5 displayed a
fatigue life of greater than 1 million sequences (1.20
106)
once it is loaded at 55% of UTS (i.e. 75 MPa). As per ASTMF382
for examining fatigue strength of bone plate, 1 million se-
quences appear to be reasonable, as it is observed that the
bone plate developed earlier was not made-up to endure high
stress fatigue cycles higher than 1 million under laboratory
conditions [50]. Moreover, the practical loading conditions
equivalent to 55% UTS (i.e.13.5 kN) is more than clinical loads
applied on regular activities of human femur which is 2.5e3
times of human body mass [15,51]. This recommends that the
CS/SF/GF combinations might be a promising replacement for
bone fracture plate since it can withstand more than 1 million
sequences at 55% UTS with insignificant fatigue loss, which is
adequate period for fractured bone re-union. Table 7 sum-
marizes the works on the natural fibre/synthetic fiber rein-
forced hybrid combinations fatigue test.
The data presented in Table 7 were obtained from previous
researches on fatigue properties of glass fiber and other nat-
ural fiber composites. Based on the previous literature, the
present CS/SF/GF composites proves to withstand higher
loads as experienced by the human femur bone during daily
normal actions like walking and running with a fatigue life-
span greater than 1 million sequences.
4.3. Surface morphology studies
Morphological investigation on the fractured CS/SF/GF fatigue
specimens for the fatigue stress level of 55% ultimate tensile
strength were analysed using SEM micrographs in order to
understand the damage progress during fatigue loading. Fig.5
shows the fractured surface of three core layer hybrid com-
posites (A1, A3, A5 and A7) under tensileetensile fatigue load
conditions. Serious occurrences of sisal fiber debonding and
pull out with epoxy can be noticed in Fig. 5(a). A1 composites
showed lower number cycles to failure during fatigue load
conditions. From Fig. 5(b) sisal and glass fiber pull-outs can be
observed, due to random distribution of chitosan and poor
hybridization between sisal fiber and glass fiber leads to ma-
trix cracks. From Fig. 5(c) it can be observed that A5 compos-
ites shows higher fatigue cycles to failure (1.20
106) which is
due to uniform distribution of chitosan and better virtuous
bonding that exists between the glass and sisal fiber. Fig. 5 (d)
indicates A7 composites to have lower number of cycles to
failure compared to A5 composites. This is due to addition of
more than 3 wt. % of chitosan which develops poor interfacial
bonding leading to failure of the composite.
Fig. 6 shows the fractured surface of four inner layer of sisal
fiber hybrid composites (A2, A4, A6, and A8) under
tensileetensile fatigue conditions. It is evident that the
breakage occurs in the A2 composites (Refer Fig. 6(a)) due to
matrix fracture. Poor adhesion exhibited in A4 composites
(Fig. 6(b)), due to random distribution of chitosan and poor
interfacial bond among sisal fiber and glass fiber. The com-
posites A6 (Fig. 6(c)) showed higher fatigue cycles 8.01
105
compared to A2, A4 and A8 composites, this is because of
improved adhesion between matrix and fiber. Fig. 6(d) repre-
sents matrix transverse crack extensive around the glass and
sisal fiber, creating consequent debonding at fiberematrix
interactions. The outcomes illustrate that interfacial bond is
crucial constraint for fatigue enactment of CS/SF/GF hybrid
sandwich composites.
4.4. In vitro biomimetic mineralization
The biomimetic action of CS/SF/GF composites could be
examined by immersing samples in SBF. SBF plays a signifi-
cant part for evaluating the biomimetic action of constituents
[54]. It is conveyed that apatite which is bone-like is to be
placed on the superficial after which bone bonding potential
can be measured with bone tissue. Different reports on the
apatite formation mechanisms were published on interaction
with SBF [55,56]. Calcium ion as a key cation during apatite
nucleation presented in present work. The existence of C]O
and CeH in sisal fiber and chitosan can perform as an electron
contributor to support absorb Ca2þ, facilitating the combina-
tion with CO2 3 and PO34 [57]. The existence of Ca2þ in SBF
solution can be easily combined with PO3 2
4 and CO3 through
electrostatic interfaces that create the nucleation sites of
apatite.
The optimized FT-IR spectra of CS/SF/GF composite A5
before and after soaking in SBF are presented in Fig. 7. The
3332 cm1 band equivalents to the hydroxyl group stretching
vibration and is moved to high wavenumber (3397 cm1) after

Table 7 e Fatigue properties of synthetic fiber/natural fiber based hybrid composites.

Materials Testing condition Applied stress Type of Number of cycles to References
amplitude loading failure (Nf)
Human femur Physiological condition 40e80 MPa Tension 10e106 Zioupos et al. (2008) [52]
cortical bone
Flax/epoxy 23  C 40e80% UTS Tension 2058e1.15
106 Liang et al. (2012) [14]
Glass/epoxy 23  C 40e80% UTS Tension 700e2
106 Liang et al. (2012) [14]
Glass/kenaf Ambient temperature 40e70% UTS Tension 1000e106 Sharba et al. (2016) [43]
Glass/hemp Ambient temperature 40% UTS Tension 100e105 Shahzad et al. (2011) [11]
Glass/jute Ambient temperature 55% UTS Tension 104e3
105 Mostafa (2019) [16]
Glass/Polypropylene Ambient temperature 10e50% Ultimate Bending 104e106 Baky and attia (2018) [53]
flexural strength
Glass/silica Ambient temperature 100e250 MPa Tension 1000e105 Manjunatha et al. (2010) [54]
nanoparticles
Chitosan/sisal/glass Ambient temperature 55% UTS Tension 1.20
106 This study
fiber
 j o u r n a l o f m a t e r i a l s r e s e a r c h a n d t e c h n o l o g y 2 0 2 1 ; 1 0 : 5 1 2 e5 2 5 519

Fig. 5 e Tensionetension fatigue failure of three inner layer sisal fiber composites a) A1 b) A3 c) A5 d) A7.

Fig. 6 e Tensionetension fatigue failure of four inner layer sisal fiber composites a) A2 b) A4 c) A6 d) A8.
520 j o u r n a l o f m a t e r i a l s r e s e a r c h a n d t e c h n o l o g y 2 0 2 1 ; 1 0 : 5 1 2 e5 2 5

Fig. 7 e FT-IR spectra of optimized GF/SF/CTS composite A5 before and after immersion in SBF.

submersion and turn out broad. It indicates that the hydroxyl

group has strong interface with C]O groups present in sisal
fibres and chitosan. After 28 days of immersion in SBF, the
new peaks were observed that the apatite layer was developed
on the surface of optimized hybrid composite A5. Subse-
quently, after 28 days of CS/SF/GF composites mineralization
in SBF, the development of absorption groups at
1506e1604 cm1 portrays the Pe O vibrations due to the PO3 4
tetrahedral. The peak at 1232 cm1 represents the CeO vi-
brations and confirms the presence of trigonal planar
CO23 groups in the composite surface. The strongest peak for
the tetrahedral PeO bond in calcium phosphate lies between
916 and 1103 cm1. The peak at 827 cm1 contains the HPO2 4
(acidic phosphate) groups due to the PeO bond [58]. The PO3 4
stretching vibration were noticed in 538e557 cm1 range;
peaks confirm the apatite elements accumulation on the
surface of CS/SF/GF composites.
The powder XRD patterns of optimized CS/SF/GF samples
A5 after soaking in SBF at different time interval 10,15 and 28 Fig. 8 e XRD spectra of optimized GF/SF/CTS composite A5
days are shown in Fig. 8. The broad peaks of diffraction before and after soaked in SBF.
pattern were observed at 16.7 ,23.20 and 30 respectively. The
XRD pattern of the composite after SBF immersion was found
to be more intense, sharp and stronger when compared to
composites before immersion (0 days). These patterns were by consuming Ca2þ and PO3 4 ions from the SBF solution. On
related with the diffraction patterns of apatite layer forma- further, increasing the immersion time from 15 days to 28
tion, which confirms that the apatite layers were effectively days, sphere shaped structures were observed on the CS/SF/
formed in A5 hybrid composites after 28 days of immersion GF surface (Refer Fig. 11), this is because each rod-shaped
[59]. particle interlaced and covered with elements developing a
Figs. 9e11 display the SEM images and EDS of CS/SF/GF sphere-shaped structure.
composite at 10, 15 and 28 days after SBF immersion. Fig. 9 The EDS data confirmed the presence of major apatite
shows the rough amorphous structure formation on the top elements such as calcium (Ca), phosphate (P), fluoride (F) and
of the CS/SF/GF composites. After 15 days (Refer Fig. 10) of chloride (CI). When the immersed duration increased from 10
immersion, the CS/SF/GF composite showed rod shaped to 28 days, the increase in atomic percentage of calcium for
crystal apatite particles on the fiber surface. Once the nucle- 10 days, 15 days and 28 days were 2.32%, 3.84% and 5.86%
ation is started, the apatite may grow on the CS/SF/GF surface respectively. Similarly, the increase in atomic percentage of
 j o u r n a l o f m a t e r i a l s r e s e a r c h a n d t e c h n o l o g y 2 0 2 1 ; 1 0 : 5 1 2 e5 2 5 521

Fig. 9 e SEM-EDS evaluation of apatite formation on the optimized A5 composites for 10 days of after immersion in SBF.

Fig. 10 e SEM-EDS evaluation of apatite formation on the optimized A5 composites for 15 days of after immersion in SBF.
522 j o u r n a l o f m a t e r i a l s r e s e a r c h a n d t e c h n o l o g y 2 0 2 1 ; 1 0 : 5 1 2 e5 2 5

Fig. 11 e SEM-EDS evaluation of apatite formation on the optimized A5 composites for 28 days of after immersion in SBF.

Fig. 12 e Elemental mapping of A5 composite after soaked in SBF for 28 days.

 j o u r n a l o f m a t e r i a l s r e s e a r c h a n d t e c h n o l o g y 2 0 2 1 ; 1 0 : 5 1 2 e5 2 5
phosphate is observed to be 1.38%, 2.27%, and 3.55% for 10
days, 15 days and 28 days respectively. Additionally, the
calcium/phosphate (Ca/P) ratio was found to be approxi-
mately 1.67 which is needed for the biological apatite layer
formation, this proved the formation of apatite layer on the
CS/SF/GF composite surface [60]. Elemental mapping analysis
(Refer Fig. 12) confirmed the presence of minor elements such
as Pb, Sr, Ba, K, Na and Y in CS/SF/GF composites, these el-
ements confirms the apatite layer formation in CS/SF/GF
composites.
5. Conclusion
Bone implant materials is of massive demand to heal bone
fractures and defects. Metal bone plates may cause osteo-
porosis, stress shielding and fatigue breakage with pro-
longed implantation in the body. The present study proposes
CS/SF/GF sandwich composites as an alternate to the
metallic orthopaedic bone plates produced using vacuum
bag method.
 The CS/SF/GF tensile properties showed higher tensile
strength of 146 MPa and tensile modulus of 6.814 GPa was
high enough to carry clinical-type loads experienced by a
human femur bone.
 Tensionetension fatigue test reveals that the optimized A5
composite showed higher fatigue life 1.20
106 cycles, this
is due to the better adhesion exhibited between sisal fiber
and glass fiber in epoxy matrix.
 The in vitro biomimetic mineralization study proved that
the major apatite layer formation on CS/SF/GF composites
surface.
In future, the CS/SF/GF hybrid composite can be studied for
their damping behaviour and stiffness degradation based on
dynamic mechanical analysis (DMA). Further, osteogenesis
and cytotoxicity of the CS/SF/GF hybrid composite can be
conducted to ensure that the fabricated hybrid composite will
not cause any unwanted biological reactions to the human
body.
Declaration of Competing Interest
The authors declare that they have no known competing
financial interests or personal relationships that could have
appeared to influence the work reported in this paper.
Acknowledgement
The authors thank Vellore Institute of Technology, Vellore for
providing ‘VIT SEEDGRANT’ for carrying out this research
work. The authors would like to acknowledge the SEM facility
provided by School of Bio Sciences & Technology (SBST) and
Advanced Materials Processing and Testing Lab for Tensile
and Fatigue test from School of Mechanical Engineering
(SMEC), VIT University. The authors would like to thank
523
Universiti Putra Malaysia for the financial support through the
Geran Putra Berimpak (GPB 9668200). The authors would also
like to thank the Department of Aerospace Engineering, Fac-
ulty of Engineering, Universiti Putra Malaysia and Laboratory
of Biocomposite Technology, Institute of Tropical Forestry and
Forest Product (INTROP), Universiti Putra Malaysia (HICOE) for
the close collaboration in this research.
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