International Journal of Mechanical Sciences 212 (2021) 106728

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International Journal of Mechanical Sciences

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Enhanced creep resistance of GFRP composites through interpenetrating

polymer network
B.N.V.S. Ganesh Gupta K , Bhaskar Sen , Mritunjay Maharudrayya Hiremath , Rajesh
Kumar Prusty *, Bankim Chandra Ray
FRP Composite Laboratory, Department of Metallurgical and Materials Engineering, National Institute of Technology, Rourkela 769008, India

A R T I C L E I N F O A B S T R A C T

Keywords: Fiber reinforced polymer (FRP) composites have become promising materials of modern times and find
Fiber reinforced polymer composites numerous applications in critical engineering fields including aerospace, marine and automobile sector. Due to
Thermosets their increasing demand, it becomes apparently essential to employ advanced techniques, which can predict the
Creep
long-term behavior of such materials in various in-service conditions. Epoxy and vinyl ester based composites are
Interface/interphase
Time-temperature superposition principle
most commonly used in structural FRP composites. As each polymer has its own advantages and disadvantages,
Mechanical testing hybridization or blending of different polymers is a trending technology to improve the performance of resulting
FRP composite. The present article aims at comparing the performance of glass fiber reinforced epoxy-vinyl ester
interpenetrating polymer network (GEVIPN) composite with that of the base materials, i.e. glass fiber reinforced
epoxy (GE) and glass fiber reinforced vinyl ester (GVE) composites. Flexural testing has been conducted at
various in-situ temperatures (30 ◦ C, 60 ◦ C and 90 ◦ C) where GEVIPN composite showed highest properties at 30
◦
C. The lifetime prediction of the composite materials has been carried out using accelerated deformation and
time-temperature superposition (TTSP) principle. It was observed that GEVIPN composite showed highest creep
resistance as compared to the other two composites at lower temperature, whereas opposite trend was observed
at elevated temperature. At 30 ◦ C, GEVIPN composite showed positive reinforcement efficiency for ~385 days
with respect to GE and ~46.27 years with respect to GVE. Similar studies were done for the other reference
temperatures. Following this, fractography analysis of the fractured surface was done under FESEM to identify
the failure mechanisms and draw a comparison between the composites.

due to their inherent characteristics [6–9]. On conflict, epoxy polymer

1. Introduction
Fiber reinforced polymer (FRP) composites are widely being
accepted in various applications like aerospace, marine, automotive,
energy, chemical and civil industries [1–3]. Moreover, FRP composite
materials become a competitive material in structural industries, where
weight saving is the highest priority. FRP composite materials replace
the traditional metallic structures due to their high strength to weight
ratio, low density, good corrosion resistance and ease of handling, which
is essential for the modern industrial applications [4,5]. A major con­
stituent of a FRP composite is the matrix, which plays a vital role in
transferring the stress to fibers along with keeping the fibers at their
respective locations. Therefore, selection of the appropriate polymer
(or) appropriate polymers for these purposes becomes critical. Among
various thermosetting polymers, epoxy and vinyl ester are extensively
used in structural, aerospace, marine, electrical & electronics industries
behaves as brittle when it reacts with catalyst. Additionally, the poor
fiber-matrix interphase/interface of the laminate results in the poor
mechanical performance of the composite [10–14]. Due to which the full
potential use of the FRP composites in various critical applications be­
comes limited. To overcome these problems and to obtain improved
mechanical properties, the epoxy polymer is being modified with
different polymers such as thermoplastic, thermoset and elastomer. Such
blending sometimes leads to the formation of IPN, which was first
coined by Sperling [15–17].
IPN has been described as crosslinking of two polymers which coexist
in an entangled network [18,19]. The studies on various IPN structured
polymer obtained by blending polymers like polyurethane and vinyl
ester resin, polyurethane and epoxy resin along with polyester and
epoxy resin are being investigated in great depths by various research
scientists [5,20–22]. Chen et al. [23] have reported that the damping
and tensile behavior of epoxy matrix could be improved by the

* Corresponding author.
E-mail address: prustyr@nitrkl.ac.in (R.K. Prusty).

https://doi.org/10.1016/j.ijmecsci.2021.106728
Received 19 April 2021; Received in revised form 2 August 2021; Accepted 5 August 2021
Available online 14 August 2021
0020-7403/© 2021 Published by Elsevier Ltd.
B.N.V.S. Ganesh Gupta K et al.
Abbreviations
ASTM American Society for Testing and Materials
CTE Coefficient of Thermal Expansion
DMTA Dynamic Mechanical Thermal Analysis
FESEM Field Emission Scanning Electron Microscope
GE Glass fiber reinforced Epoxy
GEVIPN Glass fiber/Epoxy-Vinyl ester Interpenetrating Polymer
Network
GFRP Glass Fiber Reinforced Polymer
GVE Glass fiber reinforced Vinyl ester
IPN Interpenetrating Polymer Network
MEKP Methyl Ethyl Ketone Peroxide
RT Room Temperature
TETA Triethylenetetramine
TTSP Time Temperature Superposition Principle
UTM Universal Testing Machine
formation of graft IPN with polyurethane. Their group also reported that
with the increase in polyurethane content, the IPN’s damping properties
increased but hampered the glass transition temperature. The unsatu­
rated polyester and epoxy IPN network showed its ability of absorbing
the crack energy which, in-turn, reflected the toughness improvement as
reported by Lin et al. [24]. Mahesh et al. [25] have modified the
polyurethane-epoxy IPN system with bismaleimide and evaluated its
mechanical, thermal and morphological behavior. Improvement in both
flexural as well as tensile strength was observed with a slight decrease in
impact strength by incorporating bismaleimide into the IPN system.
Many researchers have also reported other functional usage of IPNs
[26,27]. For instance, Bird et al. [18] developed a polyurethane and
polymethyl methacrylate IPN material that could exhibit high degree of
optical transparency and comparable mechanical performance. But for
applications like building ship hulls and aircrafts, many researchers
have reported the advantages of blending the two thermoset polymers,
specifically epoxy and vinyl ester polymers and using it as matrix in FRP
composites [26,28]. Mészáros et al. [28] reported that there was
increment of 10% and 7% in flexural strength and impact strength,
respectively, by using the blended epoxy and vinyl ester polymer as
matrix compared to epoxy in carbon fiber reinforced composite. Their
group also showed that better fatigue resistance could be obtained by
using blended epoxy and vinyl ester polymer. Karger-Kocsis et al. [29]
predicted that epoxy and vinyl ester hybrid resin may act as promising
matrix material and supported the prediction with two facts. The first
one is the presence of epoxy group which would enhance the fiber/­
matrix interfacial adhesion provided fiber surface should contain suit­
able reactive groups and the second one is the low viscosity of this
hybrid resin would impart excellent wet-out on fibrous surface. The
homopolymer when used as a matrix in glass fiber reinforced polymer
(GFRP) composite would exhibit relatively inferior interlaminar shear
strength (ILSS) due to relatively poor interfacial interaction at the
fiber/matrix interface [11]. Hence, blending is believed to be a prom­
ising and economical method to enhance the properties when incorpo­
rated in FRP composites and hence extend the range of applications of
the blended polymer for the global demand compared to the respective
constituent polymers.
But in spite of IPN being used in so many applications; much less
attention is being paid on its long-term durability. With increasing
research on the means to develop new composite materials systems with
improved mechanical properties, it is also essential to determine the
service life of materials and study its behavior and durability under
certain environmental conditions to which the component is exposed to
during its real-time applications [30–33] External conditions like tem­
perature, applied load, humidity etc., affect the properties of polymer
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International Journal of Mechanical Sciences 212 (2021) 106728
Notations
Adj R2 Adjusted R squared
CComp Compliance of composite in consideration
CGE Compliance of GE
R Universal gas constant
Tg Glass transition temperature
Tref Reference temperature
aT Shift factor
e Euler’s number
f Test frequency
s Creep compliance in Pa− 1
tr Reduced time
ΔH Activation energy
δ (t) Deflection due to applied load
η(%) Percentage efficiency
composites throughout their service life [34–39]. Sun et al. [40] inves­
tigated the creep behavior of polymeric composites under humid envi­
ronments. They have suggested that polymeric composites’ mechanical
properties strongly depend on service environmental condition and
time, due to the polymer matrix’s viscoelastic nature. Moreover, the
combined effects of mechanical loading and aggressive environment
severely influence the FRP materials’ mechanical performance, thus
limiting the widespread use of composites. Guedes et al. [41]stated that
FRP composites’ strength and stiffness might decay rapidly over pro­
longed exposure to service conditions due to the polymer’s viscoelastic
nature, damage accumulation between composite material constituents,
and thus results in creep failure. Moreover, their group also suggested
that an accelerated methodology is the most effective approach and
could be used to evaluate the long-term durability prediction of polymer
composites. Bonning et al. [42] have studied the creep predictions for
polymer films at cryogenic temperatures using the superposition prin­
ciple. Their group stated that polymeric materials’ performance was
severely influenced at elevated and cryogenic operating temperatures.
They stated that the superposition principle could be used to shift the
compliance of polymer material from its value at short times and predict
its value at long times. Yang et al. [43] also suggested that short-term
and long-term durability assessment of structural members are of
great concern, which is an essential approach for evaluating the struc­
tural integrity of composite materials to meet the global requirements
and extend their applications. Hence, it becomes an essential require­
ment to study the performance of composite materials especially its long
term properties which are time-dependent in nature and governs the
service life of the FRP composites [44–47].
Time dependent properties like creep is a significant factor to control
the long term properties of the material especially at higher tempera­
tures. Creep deformation occurs under the influence of prolonged me­
chanical stresses [48–50]. Generally, for perfectly elastic materials,
strain is directly related to the stress exhibiting time-independent
properties, whereas for viscoelastic materials like most of the polymer
resins, this relationship changes. Viscoelastic material store elastic en­
ergy upon their deformation and consumes this energy to return to its
original state. Though it is practically impossible to conduct experi­
mental tests for the lifetime to determine the service life of the com­
posites, prediction using different accelerated techniques becomes a
necessity. TTSP principle is one such approach which helps in deter­
mining service life of a material using creep response [15].
The TTSP is a beneficial approach for design engineers to predict the
mechanical performance of GFRP composites at different test tempera­
tures. In this regard, data relevant to GEVIPN composites does not yet
exist. Therefore, the objective of the present investigation focuses on the
B.N.V.S. Ganesh Gupta K et al.
preparation of epoxy-vinyl ester interpenetrating polymer network
(EVIPN) by simultaneous polymerization technique, with TETA as
hardener for epoxy along with MEKP as catalyst for vinyl ester. The
comparative analysis of mechanical properties and lifetime prediction of
GEVIPN, GE and GVE composites was reported. Furthermore, the
viscoelastic behavior of all fabricated composites was studied using the
DMTA approach. Additionally, to understand the failure mechanism of
the experimented composites, fractography analysis was also
performed.
2. Experimentation
2.1. Constituent materials
Bisphenol A Diglycidyl ether grade of epoxy polymer and TETA
(corresponding hardener), were procured from Atul Industries Ltd, India
bearing trade name of Lapox L-12 as well as K-6 respectively. Vinyl ester
resin trade name of P-111 and MEKP (corresponding hardener), were
supplied by Pliogrip Resins & Chemicals Pvt. Ltd, India. 3 K Plain weave
E-glass fabric with an areal weight of 360 gsm and average filamentary
diameter of 15 μm was obtained from Owens Corning, India, which was
used as reinforcement in the present experimental work.
2.2. Preparation of epoxy/vinyl ester interpenetrating polymer network
(EVIPN)
Epoxy and vinyl ester resins act as primary constituents for prepa­
ration of IPN, which is a special kind of blend of polymers. The weight of
the glass fiber for preparation of epoxy-vinyl ester interpenetrating
polymer network (EVIPN) is measured. In a flask, 1/4th by weight ratio
of epoxy polymer has been taken with respect to fiber weight percent­
age. Similarly, 1/4th by weight ratio of vinyl ester polymer has been
taken with respect to fiber weight percentage (wt.%). Next, to obtain the
1:1 wt ratio of EVIPN, the epoxy polymer was poured in to the glass
Fig. 1. The schematic diagram represents the EVIPN preparation and fabrication steps involved for the GEVIPN composite. The step starts with epoxy polymer being
poured into the glass flask. After this, vinyl ester polymer was also poured into the same flask, and then the required amount of curing agents such as MEKP and TETA
were poured into the flask, followed by a magnetic stirrer approach in order to obtain homogenous polymeric suspension. Later, the hand layup method was used to
fabricate GEVIPN composite and finally hot compaction at 80 ◦ C and 10 kg/cm2 pressure for 20 min.
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International Journal of Mechanical Sciences 212 (2021) 106728
flask. After this, vinyl ester polymer was also poured into the same flask,
then the curing agent of vinyl ester i.e. MEKP was first poured followed
by curing agent of epoxy i.e. TETA was poured into the flask. A ho­
mogenous mixture was obtained by thoroughly mixing the two polymers
and their reactive agents using a magnetic stirrer for about 5 min at an
ambient temperature environment. This 1:1 wt ratio of epoxy and vinyl
ester exhibited clear IPN structure, due to the well balance between
thermoset resin components and their curing reaction components [29,
51]. Ganesh et al. [52] have reported that 1:1 wt ratio of epoxy-vinyl
ester IPN structured matrix significantly enhanced the mechanical
properties of the GFRP composites. Fig. 1 represents the schematic steps
for EVIPN preparation and fabrication of GEVIPN composite.
2.3. Fabrication of the laminates
Fabrication of the GE laminate was done using 6 layers of glass fibers
which were cut in the dimensions of 300 length £ 250 width mm2. Hand
layup technique has been adopted for fabrication and the volume frac­
tion of the constituent materials i.e. epoxy (matrix) and glass fiber (re­
inforcements) were maintained as equal weight ratios. The curing agent
TETA was mixed in the epoxy polymer by 10 wt.%. Later, the fabricated
laminate was kept under hot compaction machine at 80 ◦ C and 10 kg/
cm2 pressure for a period of 20 min [52]. This hot compression method
facilitated uniform thickness. Finally, the composite laminate was then
left to cure at RT for 24 h.
GVE composite laminate was also prepared with the same fabrication
route as the GE composite laminate, in which the catalyst MEKP was
mixed in vinyl ester resin by 1.5 wt.% (w.r.t. weight of vinyl ester). After
preparation of EVIPN, similar fabrication steps as that of GE and GVE
composites were employed. Hand lay-up method was used for fabri­
cating the
GEVIPN laminates using 6 layers of glass fiber. Next, the laminate
was compacted at 80 ◦ C for a period of 20 min, under 10 kg/cm2 pres­
sure using a hot press compaction machine and left to cure at RT for 7
B.N.V.S. Ganesh Gupta K et al.
days due to its plasticization behavior [52,53]. Following curing, as per
the ASTM D7264 and ASTM D7028 standards, the samples for all the
composites were cut with a diamond tip wheel cutter and prepared
accordingly for Flexural, DMTA and Creep tests respectively. Later, the
test specimens of the different laminated composites were kept in hot air
oven chamber under 200 ◦ C for a duration of 6 h for post curing purpose
[52]. This post cure process facilitates better cross linking in the com­
posite material and also helps for removal of moisture and residual
stresses, which were developed during the fabrication and specimen
preparation time, respectively [54].
3. Material characterizations
3.1. Flexural test
To evaluate the flexural behavior of different types of (GE, GVE and
GEVIPN) composites, the flexural test was performed. As per the ASTM-
D7264 standard, the flexural test was conducted in Instron 5967 UTM
equipped with an environmental chamber (3-point bending fixture) at a
cross-head velocity of 1 mm/min at different testing temperatures, i.e.
30 ◦ C, 60 ◦ C and 90 ◦ C. To conduct the flexural testing at elevated
temperatures, the samples were mounted in UTM machine equipped
with an environmental chamber. After the required temperature was
attained, the samples were held for 10 min to allow thermal stabiliza­
tion. The experimental set-up is shown in Fig. 2. For each composite, the
flexural test was performed as per ASTM D7264 standard for 5 different
samples and their average value with standard deviation is reported.
Additionally, for each composite, the flexural stress vs flexural strain
curve which was closest to the average value was plotted for comparison
and is reported in the later sections.
3.2. Fractography
After the flexural testing, the fractured samples of experimented
composites were analysed with the help of Field Emission Scanning
Electron Microscope (FESEM) (Make and model: FEI Nova nanoSEM
450). For the testing, adequate sample preparation was done by coating
Fig. 2. Flexural experimental set-up. Fig. 2(a) represents the Instron 5967 UTM equipped with an environmental chamber (using a 3-point bending fixture). Fig. 2(b)
shows the arrangement of fabricated composites test specimen (GE/GVE/GEVIPN laminate) placed above two anvils of the flexural fixture and load being applied
through the top load cell. The span length is maintained 16:1 ratio as per ASTM D7264 test standard.
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International Journal of Mechanical Sciences 212 (2021) 106728
the surface of the composite specimens with a thin platinum layer using
a sputter coater. This layer of platinum on the top surface acts as the
conductive surface which prevents the accumulation of static charge
resulting in a better resolution of the fractographs.
3.3. Dynamic mechanical thermal analysis (DMTA)
DMTA is the one of the efficient tool aiming to observe viscoelastic
response of the composite material and initial regions where molecular
mobility takes place. In accordance to ASTM D7028 standard, the DMTA
was done to study the viscoelastic behavior of the GE, GVE and GEVIPN
composite samples using Netzsch DMA 242-E instrument. The DMTA
test was carried out using the 3-point bending fixture at 30 to 200 ◦ C
temperature range with heating rate of 5 ◦ C/min and 1 Hz frequency in
N2 (Nitrogen gas) atmosphere. Fig. 3 represents the experimental set-up
of DMTA test. For each composite, as per ASTM D7028 standard, DMTA
and long-term creep test was carried out for 3 different samples.
3.4. Long term creep analysis (Master creep)
For the lifetime prediction of the composite, the same Netzsch DMA
242-E instrument equipped with the 3-point bending fixture inside an N2
(Nitrogen gas) atmosphere was used. As per, ASTM test standard for
each composite type, the long term creep test was carried out for 3
different samples. And stepwise isothermal creep and recovery cycles
were carried out in 30 to 100 ◦ C temperature range, with the step size of
5 ◦ C. Each creep cycle consisted of application of 40 MPa stress (cor­
responding load of 11.56 N) on the specimen for a period of 1 h followed
by another 1 h recovery. This was repeated till all the temperature cycles
were completed, i.e. from 30 to 100 ◦ C. Using this data, stress, strain and
creep compliance for the given composites was determined as a function
of time under 40 MPa loading conditions using the following equations.
3PL
Stress (σ ) = (1)
2bd2
Strain (ε) =
6dδ(t)
(2)
L2
B.N.V.S. Ganesh Gupta K et al. International Journal of Mechanical Sciences 212 (2021) 106728

Fig. 3. DMTA (Netzsch DMA 242 E) experimental set-up. Fig. 3(a) shows the arrangement of fabricated composites test specimen (GE/GVE/GEVIPN laminate)
placed above supporting anvils of the flexural fixture according to ASTM D7028 test standard. The mechanical load being applied through the top load cell, and
operating temperature is maintained 30 to 200 ◦ C, which is monitored by thermocouple. Fig. 3(b) represents the test specimen dimensions of fabricated composites
(GE/GVE/GEVIPN laminate).

Fig. 4. Flexural stress-strain curves of fabricated composite laminates at different test temperature. Fig. 4(a) GE composite only (black curve square bullets for 30 ◦ C,
black curve round bullets for 60 ◦ C and black curve down triangle bullets for 90 ◦ C), Fig. 4(b) GVE composite only (green curve square bullets for 30 ◦ C, green curve
round bullets for 60 ◦ C and green curve down triangle bullets for 90 ◦ C), Fig. 4(c) GEVIPN composite only (blue curve square bullets for 30 ◦ C, blue curve round
bullets for 60 ◦ C and blue curve down triangle bullets for 90 ◦ C). .

5
B.N.V.S. Ganesh Gupta K et al. International Journal of Mechanical Sciences 212 (2021) 106728

Separate comparison of the flexural stress versus flexural strain

ε(t) 4bd3 δ(t)
Creep compliance (s) = = (3)
σ PL3
Where, ε(t)= creep strain and σ = creep stress (= 40 MPa) for a given
composite sample and b = width, d = thickness, P= load applied, L=
support span (mm) and δ (t) is the deflection due to the applied load.
4. Results and discussion
4.1. Flexural test
The flexural test is carried out to measure and draw a fair comparison
of the mechanical properties of fabricated GE, GVE, GEVIPN composites.
The employed a blend of epoxy and vinyl ester interpenetrating polymer
network as the matrix, and it is expected to improve the mechanical
properties compared to GE and GVE composites due to a higher degree
of cross-linking. A change in trend is expected at elevated temperatures
due to the presence of multiple factors that can directly or indirectly
affect mechanical properties’ enhancement.
The flexural stress versus flexural strain curve for GE, GVE and
GEVIPN composites at 30 ◦ C, 60 ◦ C and 90 ◦ C temperatures shown in
Fig. 4. It can be inferred that the influence of temperature is stronger on
GVE and GEVIPN composites than GE composite.
behavior of GE, GVE and GEVIPN composite materials is done w.r.t. the
30 ◦ C and 90 ◦ C testing temperatures (Fig. 5 (a), (b)). It can be clearly
deduced from these figures that at RT, GEVIPN composite dominate over
the other composites, whereas when the temperature increases to 90 ◦ C,
GEVIPN specimen showed the poor flexural behavior (in terms of
strength and modulus) in comparison to GE and GVE composites.
The flexural properties for different composites i.e. GE, GVE and
GEVIPN composites were plotted against temperature as shown in
(Fig. 5 (c), (d)). At RT, the matrix and fiber are in well intact with each
other, and for GEVIPN composite to exhibit such high flexural strength
exclusively depends on the IPN formation [10,52]. This formation of IPN
endures sufficient absorption of energy before breakage. Additionally,
better load transfer occurs from matrix to the fiber through the interface
due to the better cross-links formed between fiber and the epoxy-vinyl
ester IPN system as shown in Fig. 6 (schematic of cross-links network
structure of experimented composites). While in GE and GVE composite
there is no such formation of IPN, which leads to its failure at lower
stress levels [10]. And the similar trend is observed for the flexural
modulus of different composite specimen as that of flexural strength
(Fig. 5 (d)).
On the other hand, at higher temperatures, GEVIPN composite ex­
hibits poor flexural properties over GE and GVE composites. This is

Fig. 5. Comparison of flexural stress–strain curves for GE, GVE and GEVIPN composite at 30 and 90 ◦ C test temperature. Fig. 5(a) represents all fabricated composite
samples tested at 30 ◦ C, Fig. 5(b) represents all fabricated composite samples tested at 90 ◦ C (black curve with square bullets for GE composites, green curve with
round bullets for GVE composites and, blue curve with down triangle bullets for GEVIPN composites). Also, it represents the variation in flexural responses of
fabricated composites at 30 ◦ C, 60 ◦ C, 90 ◦ C test temperatures (according to ASTM D7264 test standard). The flexural strength and flexural modulus responses of GE,
GVE and GEVIPN composites are shown in Fig. 5(c) and Fig. 5(d), respectively. Furthermore, GE, GVE and GEVIPN composites are represented by a black, green, and
blue color bar for respective composites.

6
B.N.V.S. Ganesh Gupta K et al.
caused by the dissimilar CTE values of the composite constituents [44]
(range of Epoxy 64–68 × 10− 6/ ◦ C), (range of Vinyl ester 16–22 × 10− 6/
◦
C), (range of Glass fiber 5–6 × 10− 6/ ◦ C) [55,56]. With increase in
temperature, matrix as well as the glass fibers have a tendency to expand
and the expansion rate is dependent on their respective CTEs [57].
Composites that have different CTEs may induce residual stresses at the
fiber/matrix interface, assuming that this interface was stress free at RT
[34,44]. Due to which the constituents expand at different rates and lead
to the decrement in efficient load transfer from matrix to the fiber. This
process occurs severely in the case of GEVIPN composite and fails at
lower loads. Additionally, the testing temperature is almost near to Tg of
GEVIPN composite, while the Tg of GE and GVE composite is higher than
GEVIPN composite. It was noticed that at 30 ◦ C the flexural strength and
flexural modulus of GEVIPN composite was found to be better than other
experimented composites. But compared to 90 ◦ C, the said GEVIPN
composite exhibited inferior property.
Fig. 7. Perception of fiber/matrix interface (from top left to right) and the delaminated surface (from bottom left to right) in experimented composites at 30 ◦ C. Fig. 7
(a, a′ ) for GE, Fig. 7(b, b′ ) for GVE, and Fig. 7(c, c′ ) for GEVIPN .
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International Journal of Mechanical Sciences 212 (2021) 106728
Fig. 6. Schematic of the cross-links network structure of experi­
mented composites. Fig. 6(a). Schematic representation of a cross-
linked epoxy resin (blue color background for GE composite),
Fig. 6(b). Schematic representation of a cross-linked vinyl ester
resin (dark yellow color background for GVE composite), Fig. 6(c).
Schematic representation of a cross-linked EVIPN resin (orange
color background for GEVIPN composite). All the fabricated
composites samples post-cured at 200 ◦ C for 6 h.
4.2. Fractography
Fractography study was done to assess the fractured surface of the
composites after flexural testing. Detailed analysis also provides insights
into the extent of bonding and prominent failure mechanism exhibited
by various composites, i.e., GE, GVE and GEVIPN.
The mechanical behavior of any composite material strongly de­
pends on the fiber/matrix interface. Therefore, the field emission scan­
ning electron microscope (FESEM) analysis of the GFRP composite
specimen was done to get the fiber/matrix interface perception at the
microstructural level [11,52]. The interfacial microstructures and the
delaminated surface of flexural tested GE, GVE and GEVIPN composites
at 30 ◦ C and 90 ◦ C test temperatures are illustrated in Fig. 7. and Fig. 8,
respectively.
Fig. 7(a) reveals that a weak interface between fiber and matrix re­
sults in GE composite’s gross failure at RT. Although GVE composite
could exhibit good mechanical performance than GE composite only to
B.N.V.S. Ganesh Gupta K et al.
Fig. 8. Perception of fiber/matrix interface (from top left to right) and the delaminated surface (from bottom left to right) in experimented composites at 90 ◦ C. Fig. 8
(a, a′ ) for GE, Fig. 8(b, b′ ) for GVE, and Fig. 8(c, c′ ) for GEVIPN .
some extent, after which it experienced interfacial fiber/matrix
debonding (Fig. 7(b)). As it can be observed from Fig. 7(c), that the
blending of epoxy and vinyl ester resin could significantly improve fiber
and matrix adhesion, which results in enhanced stress transfer across the
interface [52].
For comparison, delaminated surfaces of experimented composites
have been shown to understand the inter-fiber matrix region’s nature.
Apart from weak interface, smooth fiber imprints were observed in GE
composite (Fig. 7(a′ )), resulting in lower mechanical performance. Fig. 7
(c′ ) shows nicely oriented shear cusps, which supports the fact of
GEVIPN composite exhibiting higher flexural strength as discussed in
the above section (4.1) at RT. Additionally, the images (Fig. 7) indicate
that, due to the energy absorbed by the IPN matrix, the shear cusps get
distorted more in GEVIPN composite as compared to other composites
[11, 58].
After exposing the composites to 90 ◦ C temperature, there is a huge
variation in the composites’ flexural performance, as explained in the
earlier section (4.1). High-temperature exposure worsens the adhesion
at the interface between fiber and matrix in all the composites. As can be
seen in Fig. 8(a), there is weak interfacial debonding between the fiber
and matrix in GE composite, whereas relatively higher harm can be
observed in the case of GVE composite, and addtionally, matrix drainage
and interfacial debonding are the prominent failure modes as shown in
Fig. 8(b). The matrix drainage occurs from the fiber/matrix interfacial
slippage due to the severe plastic deformation and higher softening
nature of polymeric materials at elevated temperatures [34,59]. The
GEVIPN composite (Fig. 8(c)) witnesses the most severe damages like
matrix drainage and delamination, thus result in inadequate mechanical
response at elevated temperatures.
Fig. 8. represents the fiber/matrix interface and delaminated surface
of experimented composites at 90 ◦ C test temperature. The slanted im­
prints and microvoids are the prominent failure mode in GVE composite
at elevated test temperature and result in a drop in flexural response,
evident from Fig. 8(b′ ). On the other hand, as can be seen in Fig. 8(c′ ),
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International Journal of Mechanical Sciences 212 (2021) 106728
along with the slanted fiber imprints, matrix deformation and micro-
cracks are seen in GEVIPN composite material, when exposed at 90 ◦ C
test temperature. This may be one of the cause for the deteriorating
flexural response of GEVIPN composite at higher temperature. However,
in the GE composite case, the smooth fiber imprints are observed from
the delaminated surface at higher temperature environments, as shown
in Fig. 8(a′ ). However, the fiber/matrix interfacial debonding is rela­
tively low (Fig. 8(a)), which can be attributed to the lower rate of
degradation in flexural properties of GE composite at elevated
temperature.
4.3. DMTA analysis
DMTA was done to assess the fabricated GE, GVE and GEVIPN
composites’ viscoelastic properties. Also, a change in the damping
ability can be expected in GEVIPN composite than other composites due
to the introduction of epoxy and vinyl ester IPN blend results in a higher
degree of the cross-linking network.
Viscoelastic properties of the experimented GFRP composites over
30 to 200 ◦ C temperature range have been reported in Fig. 11. From
DMTA analysis relative viscoelastic responses namely, storage modulus
(E’), loss modulus (E’’), damping factor (tanδ) can be observed.
Fig. 9(a) depicts the storage modulus continuously decreases with
increasing temperature which is because of the easy movement of
polymeric chains of epoxy resin at higher temperature [60]. After a
certain temperature, the fall in the storage modulus (E’) is rapid due to
transition of the resin matrix from a glassy state to rubbery state when
temperature reaches the range of Tg. Peaks obtained in the loss modulus
curve from Fig. 9(c) are the result of increased mobility of the
cross-linked polymeric chains, due to matrix dissipates maximum heat
to the surrounding when the external load is applied to the composite
material [61].
The Tg as obtained from the onset of the change of slope in storage
modulus curve is shown in Fig. 9(d), where GEVIPN exhibiting the
B.N.V.S. Ganesh Gupta K et al.
Fig. 9. Viscoelastic response of fabricated composites. Fig. 9(a) Storage modulus (E’) response, Fig. 9(b) tanδ, response, Fig. 9(c) Loss modulus (E’’) response (black
curve with square bullets for GE composites, green curve with round bullets for GVE composites and, blue curve with down triangle bullets for GEVIPN composites),
Fig. 9(d) Tg (◦ C), and black, green, blue color bar represents the GE, GVE and GEVIPN composites respectively.
lowest Tg among all the composites due to extensive movement of the
polymeric chains as temperature is raised. This occurs since the acti­
vation energy as required for the onset of Tg is the least for GEVIPN
composite compared to the other composites. This is supported by the
corresponding curves in the later section. Also, GEVIPN experiences this
because of the non-attainment of full cure of epoxy-vinyl ester IPN
system [62]. Fig. 9(b) denotes the damping factor response of experi­
mented composites, where GEVIPN composites recorded the highest
damping factor (0.39 ± 0.05). The recorded high damping factor in­
dicates that GEVIPN composite exhibits improved damping ability than
GE (0.34 ± 0.07) and GVE (0.20 ± 0.04) homo polymer-based com­
posites; this may be attributed to broader intramolecular friction and
molecular relaxation [63]. The GEVIPN composite material can be
suggestable for damping applications due to its high damping capacity.
Moreover, this E/V IPN based GEVIPN composite material is the po­
tential to control the noise generated by vibration in structural compo­
nents, due to better cross linked molecular chains and complex
interaction of GEVIPN composite materials constituents [64,65].
4.4. Creep analysis
Creep analysis of the composites, i.e., GE, GVE and GEVIPN com­
posites, was done to assess these composites’ creep resistance at various
reference temperatures. Furthermore, from the creep resistance
behavior at several temperatures, the composites’ lifetime prediction
can be done using accelerated deformation and time-temperature su­
perposition principle to evaluate the reinforcement efficiency of the
9
International Journal of Mechanical Sciences 212 (2021) 106728
epoxy/vinyl ester IPN.
Usually, at nominal temperature, load and environmental condi­
tions, FRP Composites often takes a long time to undergo deformation
and hence it is practically impossible to determine the tentative service
life of a given polymer composite by experimental means [66,67].
Hence, alternate methods like accelerated deformation and TTSP can be
employed to predict a composites’ service lifetime [15,68,69] which
indicates the tentative extent and behavior of the FRP composite system
at the given conditions. Viscoelastic materials tend to behave as liquids
above a certain temperature exhibiting flowing behavior due to which
their deformation becomes time-dependent. It has been observed that
the fiber/matrix interface plays a major role in affecting the
high-temperature behavior of the composites, namely creep [70].
Accelerated deformation and TTSP involves extrapolating the results to
obtain the lifetime of the composites in consideration. For this creep,
compliance is taken into account, which is given by the formula in Eq.
(3). Creep compliance is a measure of the ease with which a given ma­
terial tends to undergo deformation [47,49,71]. It can also be inferred as
the inverse of the stiffness factor for a given composite.
The creep compliance (s) for GE, GVE and GEVIPN with time (t) is
shown in Fig. 10(a). The initial trend is shown in Fig. 10(a’). It can be
observed from Fig. 10(a’) that initially IPN network improves the creep
resistance of fiber-reinforced polymer composite till a certain tempera­
ture as it exhibited the lowest creep compliance. GVE composite also had
slightly better creep resistance, but it lasted for only a short period.
Initially, the IPN network had the lowest creep deformation, but
following some time, this trend changes drastically, with the IPN
B.N.V.S. Ganesh Gupta K et al.
Fig. 10. Master creep compliance (s) versus Time (t) curve for fabricated composites. Fig. 10(a) Master creep compliance (s) versus Time (t) curve for GE, GVE and
GEVIPN composites and Fig. 10(a’) Shows the initial magnified trend of the curve (black line for GE composites, green line for GVE composites and, blue line for
GEVIPN composites).
network showing rapid creep deformation followed by the GVE and GE
composites. This may be attributed to IPNs higher polymer matrix
softening nature at a higher temperature. Lifetime Predictions of the
material based on the creep properties or time duration to failure at a
definite applied load appears to be a more realistic method. The TTSP is
considered the most suitable alternative to predicting the lifetime creep
performance of a polymeric composite structural material [72].
Moreover, TTSP is mostly used to evaluate polymeric composite
material’s viscoelastic response at short and long time durations or
frequencies, which is done by considering the short-term creep response
using accelerated deformation models [32]. A shifting parameter (aT) is
associated with the creep behavior curves at each reference tempera­
ture, which is essential in generating the master creep curve [15,73].
To carry out creep analysis of the GE, GVE and GEVIPN composite
specimens, unshifted creep compliance curves are first obtained from
the step-wise isothermal creep test. The specimen is subjected to peri­
odic loading and relaxation till a certain period of time with increasing
temperature. The deformation is measured corresponding to the time. In
between two loading cycles, relaxation cycles are also present where the
applied load is removed. As it is known, from TTSP, when compliance
curves are plotted on a logarithmic scale, each of the curves can be
shifted by an appropriate shifting factor given by equation 4.
logaT = logt − − logtr
where, log aT is called the shifting factor, t is the real test time, tr is the
reduced time which is selected time scale for a certain temperature. tr is
the expansive time scale of the real time taken in consideration. Here for
the reference temperature (T=Tref), the creep compliance is not shifted
and hence the shift factor (aT) for the creep profile at the reference
temperature is zero. For other temperature profiles, the creep compli­
ance regime may be shifted with either a positive or negative shifting
factor as calculated. For temperatures more than the selected reference
temperature i.e. (T>Tref), the shifting factor (logaT) is negative hence
the curve of creep compliance is shifted to right side. For temperatures
which are less than that of reference temperature (T<Tref), the shifting
factor is positive hence the corresponding compliance curve gets shifted
to the left side. This creates a creep compliance regime which is
continuous till temperatures well below Tg of the composite. At tem­
peratures near the Tg of the FRP composite, discontinuous nature is
observed and hence needs to be adjusted. This adjustment is done by
modifying the obtained shifting factor to better fit the creep compliance
curve profile. This manually shifting of the creep curves creates an
International Journal of Mechanical Sciences 212 (2021) 106728
almost continuous creep compliance regime, which can be fine-tuned by
trimming the extra values, to obtain a single continuous master creep
compliance profile [48].
The frequency function of a given dynamic property, for example
compliance (s), at a certain temperature Tref exhibits a similar shape in
neighbouring temperature ranges. Hence a plot of creep compliance (s)
versus logarithm time (t) may be shifted accordingly along the tr scale
till overlapping of the temperature profile occurs. This yields a contin­
uous creep compliance regime at a fixed reference temperature which
indicates the qualitative analysis of the extent of deformation, the
composite will undergo at the given reference temperature. Also, from
the same creep compliance curve, one can obtain the service life of the
composite at the given loading conditions and temperature. Hence, this
is the basis of the lifetime prediction of the composites using TTSP and
accelerated deformation mechanism. Many researchers have used the
above method to predict the lifetime of various nanofiller reinforced
polymer nanocomposites. Arrhenius equation [15], which helps in
determining the shifting factor for each curve of a given composite while
constructing the master creep compliance curve, is given by the
following equation 5.
( )
ΔH 1 1
logaT = − loge
R T Tref
(4) (5)
where T is the corresponding test temperature, Tref is the isothermal
reference temperature, ΔH is activation energy and R is the universal gas
constant (8.314 × 10− 3 kJ mol− 1 K− 1). This Eq. (5) is valid for conditions
that temperature is less than that of Tg of the sample [74]. This activa­
tion energy which is defined as the barrier which must be overcome
leading to increase of mobility of the polymeric chains using thermal
energy hence causing the glassy to rubbery state [75]. This activation
energy is dependent on the Tg as well as frequency (f) and is calculated
using the results obtained from DMTA for estimating the logaT. Fig. 11
(a)-(c) depicts the tanδ curves for each composite sample at 5 different
frequencies (i.e. 0.33, 1.00, 3.33, 10.00 and 33.33 Hz). From the tanδ
versus Temperature curves, Tg was obtained and reported in Table 1. It
can be noted that the highest peak in tanδ curve was displayed by
GEVIPN and lowest by GVE composite. This can be attributed to the
higher damping properties of IPN system over homopolymer. Fig. 11(d)
shows the linear fitted curve of ln (f) versus 1000/Tg (K− 1) plot for the
three composites from which the slope was obtained and substituted in
the equation 6.
10
B.N.V.S. Ganesh Gupta K et al. International Journal of Mechanical Sciences 212 (2021) 106728

Fig. 11. tanδ curves at various frequencies obtained by DMTA testing for fabricated composites Fig. 11(a) GE only, Fig. 11(b) GVE only, Fig. 11(c) GEVIPN only,
(0.33 Hz, 1.00 Hz, 3.33 Hz, 10.00 Hz, 33.33 Hz represented by black, red, blue, pink, and green curves respectively). Fig. 11(d) shows ln(f) versus 1000/Tg (K− 1) for
all the 3 composites (GE, GVE and GEVIPN composites represented by black, green and blue lines, respectively).

d(lnf )
Table 1 ΔH = − R ( ) (6)
Glass transition temperature Tg obtained by the d T1g
tanδ method for various composites.
Composite Tg (◦ C) The activation energies as required for the glass transition temper­
GE 121.1 ± 3.4
ature onset for the composites are tabulated along with the adjR2 (how
GVE 117.7 ± 1.5 well that the points fit a curve) value in Table 2. Lower activation energy
GEVIPN 105.1 ± 1.0 indicates the lower Tg and an early onset of the transition. Similarly,
higher the Tg, higher is the activation energy. This is extremely useful in
determining the appropriate shift factors for the composite while con­
structing the master creep compliance curve and serves as a good
method for lifetime prediction. From Table 2 it can be observed that GE
displayed the highest activation energy i.e. 426.05 KJ/mol followed by
GVE with 359.78 KJ/mol and GEVIPN 341.07 KJ/mol.
Fig. 12 shows the unshifted and shifted master creep compliance
curve for (a) GE, (b) GVE and (c) GEVIPN composite at a Tref of 30 ◦ C.
The unshifted curves of creep compliance (s) for the composite materials
Table 2 were plotted on a logarithmic time (t) scale. Using the shifting factor
Calculated Activation Energy (ΔH) in KJ/mol values with the Adj. R2 for GE, obtained from Eq. (5), each individual curve was shifted by an appro­
GVE and GEVIPN composites. priate factor and then further adjustments were made to obtain a
Composite Activation Energy ΔH (KJ/mol) Adj R2 continuous creep compliance curve for the composites [15]. Here it can
GE 426.05 0.97
be observed that the creep compliance for GEVIPN rises at a rapid rate as
GVE 359.78 0.99 compared to GVE and GE composite. This indicates that GEVIPN com­
GEVIPN 341.07 0.98 posite tends to undergo rapid creep deformation after a certain

11
B.N.V.S. Ganesh Gupta K et al.
Fig. 12. Unshifted and shifted master creep compliance curve for fabricated composites at 30 ◦ C reference temperature. Fig. 12(a) GE only, Fig. 12(b) GVE only,
Fig. 12(c) GEVIPN only (different colours used to distinguish the test temperature experimented composites of unshifted and shifted master creep compliance curves).
temperature when subjected to a continuous stress of 40 MPa. At higher
time duration, GEVIPN composite exhibited lowest creep resistance
followed by GVE and GE respectively. This accelerated creep deforma­
tion of the GEVIPN composite is attributed to the fact that GEVIPN’s
flexural strength is the lowest as compared to other experimented
composites at higher temperatures. Additionally, the Tg of GEVIPN
composite is low. Therefore, as the testing temperature approaches its
Tg, it tends to undergo higher deformation as compared to others. This is
supported by the results in flexural performance section. GVE also tends
to undergo rapid creep deformation after certain time at 40 MPa loading
condition as compared to GE composite though the extent was not as
significant as GEVIPN composite.
The curve generated due to the shifting factor obtained by activation
energy overlaps well with the corresponding temperature curves, well
below Tg because of the assumption that activation energy is constant
for the given GFRP composite. Constant activation energy assumption is
valid for temperatures well below Tg. Manual shifting of the curves was
done to remove the discontinuity between the curves and to obtained
smooth overlap creep compliance curves for such temperatures [15].
Fig. 13(a)-(d) shows the shifted creep compliance curves for the com­
posites at reference temperature of 30 ◦ C, 50 ◦ C, 70 ◦ C and 90 ◦ C along
with magnified plot of the initial curve in (a’)-(d’) respectively. At the
initial stage, it can be observed from the magnified images, that at all the
12
International Journal of Mechanical Sciences 212 (2021) 106728
reference temperatures, GEVIPN showed the lowest creep compliance
depicting highest creep resistance at the former period of time followed
by GVE and GE. However, after some period of time, GVE and GEVIPN
composites started exhibiting rapid deformation under the given loading
conditions and tend to deform at a rapid rate as compared to GE. GE,
which showed highest creep deformation initially, did not exhibit much
rise in the creep compliance curve leading to a very small increment
even after sufficient time had elapsed. This shows that the GEVIPN
composite is better than the rest two FRP composites in terms of creep
resistance at the beginning and hence undergoes least amount of creep
deformation. However, eventually the rise in creep compliance for
GEVIPN and GVE was much higher than that of GE and hence it indi­
cated that after elapsing of considerable amount of time, GE composite
has the best creep resistance among the rest of the composites. This
trend was observed at all the reference temperatures. With increase in
the reference temperatures, the time taken by the rise in creep compli­
ance of GEVIPN and GVE to surpass GE also decreased significantly.
The reinforcement efficiency, which is the measure of how good is a
given composite as compared to the reference composite, here w.r.t GE
composite at a particular time and reference isothermal temperature is
given by the formula;
CGE − Ccomp
η(%) = × 100 (7)
CGE
B.N.V.S. Ganesh Gupta K et al. International Journal of Mechanical Sciences 212 (2021) 106728

Fig. 13. Master curve of creep compliance for all fabricated GE, GVE and GEVIPN composites at different test temperatures. Fig. 13(a) At 30 ◦ C only, Fig. 13(b) At 50
◦
C only, Fig. 13(c) At 70 ◦ C only, Fig. 13(d) At 90 ◦ C only, and the magnified plot of the initial curve of experimented composites of individual test temperatures
shown in Fig. 13(a’), Fig. 13(b’), Fig. 13(c’) and Fig. 13(d’) respectively (GE, GVE and GEVIPN composites represented by black, green and blue lines respectively).

13
B.N.V.S. Ganesh Gupta K et al. International Journal of Mechanical Sciences 212 (2021) 106728

where CGE and Ccomp are the creep compliance of GE composite and the
FRP composite specimen under consideration, i.e. GVE and GEVIPN.
Fig. 15(a)-(d) shows the master creep compliance curves for the com­
posites at reference temperature of 30 ◦ C, 50 ◦ C, 70 ◦ C as well as 90 ◦ C
along with their reinforcement efficiency ƞ (%) in Fig. 15(a’)-(d’)
respectively. Predicted lifetime of the composites are denoted the ver­
tical solid lines.
For the initial stage, GEVIPN exhibited the best creep resistance
properties due to its low creep compliance followed by GVE when
compared to the GE leading to a higher positive reinforcement efficiency
for the Tref of 30 ◦ C, 50 ◦ C, 70 ◦ C as well as 90 ◦ C. For all reference
temperatures, the reinforcement efficiency started decreasing with time
and eventually changed from positive to negative value indicating that
after long time periods, GE composite was better than both the com­
posites in terms of creep resistance even though a different trend was
observed at the beginning. This also indicates that the extent of
improvement in the creep properties or the positive reinforcement ef­
ficiency is time and temperature dependent. Moreover, the creep
rupture of a composite material is the result of combined events, such as
viscoelastic deformation, chain slippage, void formation, void growth,
fiber breakage, shear yielding and crazing results into fracture [76].
Additionally, physical and chemical interaction between the
constituents of FRP composites at interface/interphase plays vital role
on FRP composite material creep life performance [77]. Fig. 14. shows
the schematic representation of polymeric chains during creep and re­
covery stages at RT (30 ◦ C) and elevated temperature (90 ◦ C) for all
experimented (GE, GVE and GEVIPN) composites. At RT, GEVIPN
composite (Fig. 14(c)) tends to exhibit lesser movement of polymeric
chains, due to a higher degree of cross-linking and entanglement present
as compared to homo polymer-based composites i.e., GE (Fig. 14(a)) and
GVE (Fig. 14(b)). These cross-links restrict the movement of polymeric
chains in the matrix and lead to better creep resistance of the GEVIPN
composite [16]. However, at elevated temperature, irrespective of a
higher degree of cross-linking, the GEVIPN composite exhibits more
movement in polymeric chains. Moreover, this may result from a higher
degree of softening nature of the EVIPN matrix in the GEVIPN composite
(Fig. 14(c’)). Moreover, this higher softening nature of the EVIPN matrix
results in interfacial slippage and a high degree of stretch of the GEVIPN
composite at elevated temperatures. The interfacial slippage and
stretching of the EVIPN polymeric chain compensate for the presence of
cross-links and hence, leads to low creep resistance in the GEVIPN
composite compared to GE (Fig. 14(a’) and GVE composites (Fig. 14(b’).
The time period till which positive reinforcement is observed for
GEVIPN composite at the reference temperature of 30 ◦ C is estimated to

Fig. 14. Schematic representation of polymeric chains during creep and recovery response for all experimented composites. Fig. 14(a) for GE, Fig. 14(b) for GVE,
Fig. 14(c) for GEVIPN composites at RT (30 ◦ C) and Fig. 14(a’) for GE, Fig. 14(b’) for GVE, Fig. 14(c’) for GEVIPN composites at elevated temperature (90 ◦ C). GE,
GVE and GEVIPN composites creep and recovery response represented by aqua blue color background, yellow color background, and dark orange color background,
respectively.

14
B.N.V.S. Ganesh Gupta K et al. International Journal of Mechanical Sciences 212 (2021) 106728

Fig. 15. Master curve of creep compliance for GE, GVE and GEVIPN composites at different Tref temperatures. Fig. 15(a) 30 ◦ C only, Fig. 15(b) 50 ◦ C only, Fig. 15(c)
70 ◦ C only and Fig. 15(d) 90 ◦ C only along with the reinforcement efficiency (η (%)) in (a’), (b’), (c’) and (d’) respectively (GE, GVE and GEVIPN composites
represented by black, green and blue curves respectively).

15
B.N.V.S. Ganesh Gupta K et al.
be ~385 days in comparison to GE composite and ~46.27 years in
comparison to GVE composite. The creep compliance for GEVIPN
increased at a rapid rate leading to high creep deformations surpassing
rest of the two composites. Similarly, the lifetime of GVE at a reference
temperature of 30 ◦ C is ~2 days as compared to GE composite after
which the creep deformation rate increased and negative reinforcement
efficiency is observed. Also, the reinforcement efficiency of both
GEVIPN and GVE gradually decreases with increasing reference tem­
perature. At the reference temperature of 50 ◦ C, GEVIPN showed posi­
tive reinforcement efficiency till ~172.54 min as compared to GE
composite and ~6 days as compared to GVE composite. Here the effect
of temperature can be easily observed where there is a huge drop in the
lifetime of the composite with rise in temperature. For GVE, positive
reinforcement was observed for even less than a minute as compared to
GE composite. Maximum effect of temperature can be observed from the
comparison at 70 ◦ C and 90 ◦ C, where, positive reinforcement efficiency
at reference temperature of 70 ◦ C for GEVIPN was observed for only
~5.68 s as compared to GE composite and ~7.41 min as compared to
GVE composite whereas for GVE positive reinforcement was observed
for negligible amount of time.
Similarly, at 90 ◦ C, positive reinforcement efficiency was observed
for negligible amount of time of both GEVIPN and GVE as compared to
GE composites. Hence, this indicates that with increase in temperature,
the usability of a FRP composite decreases and the expected service life
due to creep response is drastically reduced and at elevated tempera­
tures [15], GEVIPN and GVE exhibited less creep resistance as compared
to that of GE composite. This creates the need to predict the useful
service life of a FRP composite where long-term creep behavior plays a
vital role.
5. Conclusions
The article suggests that the process of blending of epoxy and vinyl
ester polymers is basically sound and can in principle be used in FRP
composite meticulously over homopolymer. While the present article
aims at studying the mechanical response and long-term creep perfor­
mance of GEVIPN composite in comparison to neat GE and GVE com­
posites. The following conclusions can be drawn from this work:
■ In the current research work, the methodology employed was flex­
ural test in order to have better insight of mechanical performance of
experimented composites. Apparently at RT, GEVIPN showed the
highest flexural properties with 14.02% enhancement in flexural
strength as well as 9.11% increase in flexural modulus with respect
to GE composite. In order to remove the ambiguity, the results were
confirmed from DMTA analysis. However, at elevated temperature i.
e., at 90 ◦ C, GEVIPN exhibited lower flexural properties.
■ The prime outcome has been obtained from fractographic studies
under FESEM, which indicated the preferred deformations and fail­
ure mechanisms like severely oriented shear cusps, interfacial fiber/
matrix debonding, smooth fiber imprints, micro voids, micro cracks
and matrix drainage for experimented composites. The interfacial
microstructure revealed that at RT the blending of epoxy and vinyl
ester resin could significantly improve fiber and matrix adhesion.
Perhaps, the oriented shear cusps supported the fact of GEVIPN
composite exhibiting higher flexural strength. On the other hand, at
elevated temperature, the GEVIPN composite witnesses the most
severe damages like matrix drainage and delamination.
■ The requirement to conduct the DMTA analysis was to acknowledge
the Tg as obtained from the maximum point or peak of tanδ method.
It indicated that GE exhibited the highest Tg followed by GVE and
GEVIPN composites. The test also revealed that significant
enhancement in damping ability response was obtained in GEVIPN
composite as compared to GE and GVE composites.
■ The trend for all the composites with respect to Master creep
compliance curve was observed. Initially GEVIPN exhibited better
16
International Journal of Mechanical Sciences 212 (2021) 106728
creep resistance due to low creep compliance curve followed by GVE
and GE but with time, GEVIPN and GVE underwent rapid creep
deformation surpassing GE leading to an inversion of the trend.
■ At Tref of 30 ◦ C, the lifetime of GEVIPN was found to be ~385 days
and that of GVE was found to be ~2 days w.r.t GE composite. The
obtained trend changes drastically after long period duration due to
increased creep deformation. Similarly, at reference temperature of
90 ◦ C, positive reinforcement for GEVIPN and GVE was observed for
a negligible time duration due to decrease in creep resistance.
CRediT authorship contribution statement
B.N.V.S. Ganesh Gupta K: Conceptualization, Data curation,
Investigation, Validation, Writing – original draft, Writing – review &
editing. Bhaskar Sen: Writing – review & editing, Data curation. Mri­
tunjay Maharudrayya Hiremath: Writing – review & editing, Valida­
tion. Rajesh Kumar Prusty: Conceptualization, Supervision, Resources,
Project administration, Funding acquisition. Bankim Chandra Ray:
Supervision, Resources, Project administration.
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.
Acknowledgements
The authors would like to extend their warm thanks to National
Institute of Technology – Rourkela and Science and Engineering
Research Board (SERB) - (ECR/2018/001241) for granting the facilities
as well as providing the funding associated with this project for a smooth
conduction of the whole work. Technical assistance as provided by Mr.
Rajesh Patnaik throughout this project is also highly appreciated.
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