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Sådhanå (2023)48:29 Ó Indian Academy of Sciences

https://doi.org/10.1007/s12046-023-02090-7
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An experimental study on low velocity impact characteristics of glass


fiber reinforced epoxy nanocomposites
YASIN YILMAZ* , FATIH OZGUL and INAN AGIR

Department of Mechanical Engineering, Pamukkale University, 20070 Denizli, Turkey


e-mail: yyilmaz@pau.edu.tr; ozgul.fatih@gmail.com; iagir@pau.edu.tr

MS received 16 March 2022; revised 21 November 2022; accepted 3 January 2023

Abstract. In this study, the low velocity impact behavior of glass fiber reinforced epoxy (GFRE) composites
with the addition of organic intercalated nanoclay and spheroidal powder of polyamide nanoparticles individ-
ually and together were investigated experimentally. The weight ratio of the additives was 2% of the epoxy
resin-hardener system. Composite laminates were manufactured using prepreg and hot-pressing techniques.
Impact tests were carried out at different energy levels from 10 J to 45 J up to complete perforation of the
laminates. To evaluate the damage characteristics of the laminates, the results are interpreted in terms of load-
time, load-displacement, energy-time, and observation of the physical damages introduced. Addition of
nanoparticles increased the peak load (up to 22.6%) and damage resistance (up to 40%) of the GFRE laminates
altering damage mechanisms of the composite material from out of plane to in-plane direction at higher impact
energy levels.

Keywords. Low velocity impact testing; nanocomposites; GFRE; nanoclay; polyamide.

1. Introduction brittleness of carbon fiber epoxy composites, the usage of


fiber-glass reinforcement is suggested. It is also mentioned
New developments in advanced material technology have that fiber-glass epoxy composite toughness is highly
focused on multifunctional structural engineering materials dependent on strain rate damage and the matrix behavior
that simultaneously contain many superior features such as itself, and matrix toughness can be enhanced by addition of
high strength, low weight, damage resistance and low cost. nanoclay to epoxy system. However as mentioned by Fer-
Epoxy resins, the most important class of thermoset poly- reira et al [11] there is no apparent consensus on the frac-
mers, and fiber reinforced epoxy resin composites are ture toughness behavior of nanoclay filled composites
widely used in structural applications, automotive, defense looking at the results reported in the literature. Haque et al
and aerospace industries due to their superior mechanical, [12] investigated the effects of nanoclay particles on
thermal and electrical properties. However, in all these mechanical and thermal properties of S2-glass/epoxy
applications, epoxy resins are brittle and have poor resis- polymer nanocomposites using various amounts of (1, 2, 5
tance to crack propagation limiting their usage in most and 10 wt.%) of particles. They concluded that thermo-
applications. Recent studies have shown that the combi- mechanical properties mostly increase at low clay loadings
nation of nanometer-sized additives or fillers with polymer (1–2 wt.%) but decrease at higher clay loadings (5 wt.%
matrices is intensified by efforts to improve the material and above). Aymerich et al [13] investigated the impact
properties of the polymer [1–6]. response of standard and clay modified glass fiber fabric/
Composite structures are exposed to various in-plane and epoxy laminates using three different clay volume frac-
out-of plane loading conditions during their service life. tions, 1%, 3% and 5% with impact energies ranging
According to many studies carried out in the literature, between 1 J and 10.6 J. They observed an increase in
impact events (specifically low velocity impact loading) is absorbed impact energy (up to 30%), a reduction in the
one of the most critical factors to be considered in the impact force (from 10 to 15%) and an increase in damage
design and application of composite structures [7–9]. area with respect to the standard laminates for 3% volume
According to Avila et al [10], the key issue in the design of fraction of nanoclay. In another study, Koricho et al [14]
fiber reinforced composite laminates for impact loading is investigated the quasi-static indentation and low velocity
the damage tolerance of fibers and matrix system. Because impact behavior of pristine and nano-/micro-modified S2-
of the high cost of aramid reinforced composites and glass plain weave fabric reinforced epoxy polymer com-
posites. They used nanoclay, CloisiteÒ 30B and micro-
*For correspondence Glass Bubbles iM16K as nano- and micro- additives,
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respectively at a wight ratio of 1%. They observed that increases, the damage area decreases for the laminates filled
pristine and Glass Bubble modified laminates showed the by nanoclays. Iqbal et al [19] investigated the influence of
highest peak force and low absorbed energy with penetra- nanoclay addition (3 and 5 wt.%) into the epoxy resin of
tion of the impactor through the thickness of the laminate unidirectional carbon fiber-epoxy composites utilizing low
while nanoclay modified laminate showed the highest velocity impact and compression after impact tests. They
absorbed energy and minimum peak reaction force without found that the addition of nanoclay into the carbon fiber/
penetration at high impact energy levels. The hybrid lam- epoxy laminates improved impact damage resistance and
inate (with inclusion of nanoclay and Glass Bubble addi- damage tolerance by providing smaller damage area, higher
tives together into the epoxy) exhibited intermediate residual strength and higher perforation threshold energy
absorbed energy with peak reaction force that was sustained level. They also concluded that the addition of 3 wt.% clay
for longer time. They also observed that nanoclay added was an optimal content for the highest damage resistance.
and hybrid laminates showed an extensive area of damage Mahdi et al [20] carried out low velocity impact tests to
compared to pristine laminate for the same impact energy determine the effect of addition of multiwalled carbon
conditions. Rafiq et al [15] studied the effect of nanoclay nanotubes (MWCNTs) and nanoclay into the 8-harness
addition in glass fiber mat reinforced epoxy composites on satin weave carbon fiber fabric reinforced epoxy resin.
impact response using 1.5 and 3.0 wt.% loading of I.30E They used 0.3 wt.% of MWCNTs, 2 wt.% of nanoclay and
nanoclay. They found that laminates with nanoclay exhib- hybrid of MWCNTs and nanoclay at 0.1 wt.% and 2 wt.%,
ited better impact resistance as compared to neat samples respectively in the fabrication of composite laminates. They
and samples with 1.5 wt.% nanoclay showed better per- found that nanophased carbon fiber/epoxy composites
formance compared to samples with 3.0 wt.% nanoclay. increased the peak load. Hybrid nanoparticle filled com-
According to their study, there is an increase in peak load posite laminates reduced the damage area and increased the
and stiffness, a reduction in physical damage and a decrease absorbed energy compared to neat laminates. Najafabadi
in absorbed energy with the addition of nanoclay to epoxy. [21] investigated the effect of addition of nanoclay Cloisite
They also concluded that 3.0 wt.% nanoclay loading con- 20A to the woven unidirectional carbon fiber fabric rein-
tributed towards limiting the improvement in impact forced epoxy nanocomposites under three impact energy
resistance due to clay agglomeration in samples. levels of 10 J, 15 J, and 20 J. Optimum nanoclay addition
There are also other studies on low velocity impact was found to be 0.2 wt.%. They observed that addition of
characteristics of epoxy nanocomposites with different nanoclay increased the maximum impact force and
types of fiber reinforcement. Reis et al [16] examined the decreased the absorbed energy, maximum displacement
low velocity impact response and damage tolerance of and delamination area. In a recent review study, Balguri
Kevlar/epoxy composites filled with two different types of et al [22] stated that based on the morphology of nanofiller
additives, cork powder and nanoclay 30B with the filler reinforcements, epoxy nanocomposites can be classified as
content of 3 wt.% of the epoxy resin-hardener mixture. isotropic nanofillers (a material having identical dimensions
They found that addition of fillers increases the maximum in all directions usually in spherical shape) reinforced and
impact load and decreases the maximum displacement. anisotropic nanofillers (materials that show variation in
According to their study, the best performance in terms of physical properties along different axes with different
elastic recuperation was obtained for laminates that have properties in different directions like clay-based 2D layered
nanoclay as additive and addition of clays increases the nanofillers) reinforced epoxy nanocomposites.
damage area as compared to the control samples. Minimum In this study, the effects of addition of organic interca-
damage area is observed for laminates manufactured with lated nanoclay and spheroidal powder of polyamide 12,
epoxy resin filled by cork powders. In another work, Reis individually and together, on the low velocity impact
et al [17] studied the low velocity impact response of characteristics of woven glass fiber reinforced epoxy
Kevlar/epoxy composite to determine the ideal amount of (GFRE) laminates were investigated experimentally.
nanoclays (up to 6 wt.%) to obtain the best impact per- Impact tests were carried out at different energy levels until
formance. They found that addition of nanoclays increased full perforation occurs. To evaluate the damage character-
the maximum impact force and damage area. The laminates istics of the laminates, the results were interpreted in terms
manufactured with epoxy resin filled by 3 wt.% and 6 wt.% of load-time, load-displacement, energy-time diagrams, and
of nanoclays showed the best performance in terms of observation of the physical damage introduced.
elastic recuperation and penetration threshold compared to
the control samples. Rahman et al [18] investigated the
effect of nanoclay and graphene inclusion with different 2. Materials and experimental procedures
weight fractions (up to 10 wt.%) on the low velocity impact
resistance of 4-harness satin weave Kevlar-epoxy laminated
2.1 Materials
composites. They observed that nanoclay is more effective
than graphene in impact resistance and the absorption of In the present study, woven glass fiber fabric 0/90° pattern
impact energy. They also found that as the impact energy with areal density of 300 g/m2 was used as primary
Sådhanå (2023)48:29 Page 3 of 13 29

reinforcement. The matrix used was the warm curing epoxy of air bubbles. 10 layers of prepregs covered with waxed
system, Araldite LY 1564 epoxy resin combined with the papers were placed on top of each other and cut in
formulated amine hardener Aradur 3486, both supplied by 400 mm 9 400 mm dimensions, and hot pressed at 5 bar
Huntsman, Switzerland. The mixing weight ratio of resin: pressure and 120 °C temperature for 2 h. Composite lam-
hardener was set to 100:34 as recommended by the sup- inates were cooled slowly to room temperature to avoid
plier. The additives used was organic intercalated nanoclay thermal distortions and stress concentrations, then the
Cloisite 20, a bis(hydrogenated tallow alkali) dimethyl, pressure was removed. The composite plates produced have
supplied by BYK-Chemie GmbH, from Wesel, Germany, an average thickness of 2.3 mm. After manufacturing of
and a spheroidal powder of polyamide 12, Orgasol, with composite plates, they were cut in 100 mm 9 100 mm
30 lm as average diameter and a narrow particle size dis- dimensions by water jet to prepare test specimens for low
tribution, supplied by Grolman GmbH, from Neuss, Ger- velocity impact testing.
many. Orgasol represents a range of ultra-fine polyamide
powders made by the polymerization of lauryllactam
(polyamide 12) and/or caprolactam (polyamide 6). The 2.3 Morphology
physical and descriptive properties of the additives used are
presented in table 1, as reported by the manufacturers. Distribution of nanoparticles in the epoxy resin was
investigated using ZEISS-Supra 40VP model field emission
scanning electron microscope (FE-SEM). First fractured
surfaces of the nanocomposite samples were coated with
2.2 Fabrication of composite laminates
gold (80%) and palladium (20%) using a Quorum - Q10R
The glass fiber-epoxy-additives composite laminates were ES model coating device. Then SEM images of the
manufactured using prepreg and hot-pressing techniques. nanocomposite samples were obtained at different
One of the problems encountered during the production of magnifications.
additive enhanced laminates is the nonhomogeneous dis-
persion of fillers in the polymer. The fact that the additive,
which tends to cluster, is not homogeneously distributed in 2.4 Impact tests
the matrix, that is, agglomeration, affects the mechanical
properties of the composite material negatively. To prevent For impact testing of the specimens, Instron-Dynatup 9250
these agglomeration formations, the ultrasonic mixing HV impact testing machine shown in figure 1 was used. It
consists of a dropping crosshead with its accessories,
technique (mixing of the particles by emission of ultrasonic
pneumatic rebound brakes, a pneumatic clamping fixture
waves) was used in the dispersion process. First, the addi-
and Dynatup 930-I impulse data acquisition system.
tives were weighed precisely at 2.0 wt.% of the epoxy
The weightlifting and holding system enable weight to be
resin-hardener mixture and then the mixture of additives
and epoxy resin were sonicated for 30 min at the temper- dropped on to the sample, by raising the weight box, the
ature of 30 °C by using a Bandelin ultrasonic sonicator and crosshead and the impactor to the desired height, by taking
a cooling system. Four different types of matrix composi- the spring support if necessary. Thus, the impact load is
tions which are pure epoxy named as Neat, polyamide applied to the sample at the desired impact energy level or
at the desired speed by adjusting the height of the dropping
powder (2.0 wt.%) /epoxy named as PA, nanoclay
weight. During all of the impact tests, the total weight of
(2.0 wt.%) / epoxy named as NC and polyamide powder ?
the crosshead with its accessories was 6.32 kg and the nose
nanoclay (1.0 wt.% ? 1.0 wt.%) / epoxy named as PA?NC
of the impactor was a 12.7 mm diameter hemispherical tup.
were used in manufacturing of GFRE nanocomposites.
Epoxy resin-hardener mixtures containing additives in Pneumatic rebound brake system, if activated, prevents
specified ratios were impregnated into the woven glass fiber repeated impacts on the specimen. The velocity detector
fabric by hand lay-up method. Prepregs produced were left measures the impact velocity just before the impact event
on the shelves for three days to form a smooth interface free occurs using a photoelectric-diode and flag system and

Table 1. Physical and descriptive properties of the additives.

Density [g/ Bulked Density [g/ Average particle Moisture


Additives Description cc] cc] size content Appearance
Nanoclay Organic intercalated nanoclay 1.77 0.175 \10 lm (d50) \= 3.0% Off white
(Cloisite 20) 3.16 nm (d001)
Polyamide Spheroidal powder 1.03 0.375 30 ± 2 lm \= 1.0% White
powder
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tests were carried out according to the ASTM D7136


standard.

3. Results and discussion

3.1 Morphology of nanoparticles


and nanocomposites
Figure 2 shows the SEM images of polyamide and nanoclay
particles. Figure 3 presents the SEM images of epoxy
nanocomposites. The presence of large size polyamide
aggregates can be observed at higher magnifications
whereas nanoclay doped nanocomposite shows relatively
uniform microstructure to some extent and rougher surface
with the occasional localizations of small patches of clay
agglomerations.

Figure 1. Instron-Dynatup 9250 HV impact testing machine.


3.2 Low velocity impact test results
Impact tests were carried out at 10 J, 20 J, 30 J, 35 J, 40 J
ensures that the impact velocity is transferred to the data and 45 J impact energy levels and low velocity impact
acquisition card with the signal conditioning unit. Impulse behavior of neat and nano-modified composite laminates
data acquisition system records the load vs time data and were investigated in terms of load-time, load-displacement,
instantaneous velocity at the moment of impact and con- and energy-time diagrams. For 10 J, 20 J and 30 J impact
verts them into load-deflection data based on Newtons energy levels, the impactor deforms the specimens and
second law and kinematics with the assumption that the rebounds which means that the impact energy was not high
impactor was rigid. enough to produce full penetration or perforation. For these
During the impact tests, the specimens were supported energy levels, the impact, rebound and absorbed energies
by a steel plate that has a circular opening of 76 mm for each material configuration can easily be distinguished.
diameter in size and held at four corners by rubber clamps After a critical value of impact energy, perforation of the
using a pneumatic clamping fixture. To examine the dam- composite laminates takes place. As stated by Atas and
age mechanisms and to compare various impact parame- Sayman [23], for higher impact energies resulting in the
ters, composite laminates were impacted at the center with perforation of specimens, the post-perforational frictional
impact energies ranging from 10 J to 45 J up to the com- effects between the impactor and the specimen need to be
plete perforation of the specimens. At each impact energy removed from the diagrams to determine the real dis-
level at least three impact tests were carried out for any placement and energy absorption due to the formation of
composite material system considered. The drop weight damage. Taking this situation into consideration, impact

Figure 2. SEM images of (a) polyamide and (b) nanoclay particles.


Sådhanå (2023)48:29 Page 5 of 13 29

Figure 3. SEM images of (a) PA, (b) NC and (c) PA?NC nanocomposites.

damage performance and resistance of the control and laminate architectures [20]. Figure 4 presents the impact
nanomodified composite laminates were determined con- load vs time responses for neat, polyamide, nanoclay, and
tinuing the tests at 35 J, 40 J and 45 J energy levels until polyamide?nanoclay filled GFRE composite laminates
full perforation occurs. A summary of the impact test impacted at different energy levels. These curves show
results, which will be discussed and analyzed in the fol- typical behavior for composite laminates, and exhibit a
lowing subsections, is given in table 2. regular rise in load up to a critical value, Pmax, followed by
a sudden decrease which indicates an alteration in stiffness
3.2.1 Force-time responses The impact load-time associated with extensive matrix cracking, fiber breakage,
response gives qualitative indications of how the laminate delamination, and large damage area. These curves also
responds and whether there is any significant damage under contain some oscillations at the beginning due to elastic
a given impact energy level and is a good predictor for waves resulting from the vibrations generated in the
evaluating and comparing the impact behavior of different specimens at the time of impact. These vibrations depend

Table 2. Impact test results for neat and nanomodified composite laminates at different impact energy levels.

Impact Peak load Displacement at peak Maximum Total displacement Absorbed


Specimen energy (J) (kN) load (mm) displacement (mm) (mm) energy (J)
Neat 10 3.89 5.64 5.71 2.20 6.26
20 4.98 6.94 7.75 3.60 15.67
30 5.22 6.99 11.27 7.56 28.74
35 5.36 7.13 12.99 12.99 31.58
40 6.00 7.22 12.26 12.26 33.00
PA 10 3.56 5.88 6.14 2.74 7.57
20 4.72 7.95 8.12 3.42 15.06
30 5.18 8.82 9.91 4.34 24.27
35 5.49 9.05 11.36 6.77 32.03
40 5.24 9.70 12.56 7.21 36.20
45 4.71 8.42 13.50 13.50 35.50
NC 10 3.63 6.02 6.14 2.57 6.98
20 4.67 8.28 8.38 3.72 15.08
30 6.01 9.65 9.82 4.07 22.86
35 6.57 9.64 10.08 4.64 27.48
40 6.65 9.93 11.04 4.97 31.44
45 6.11 10.15 12.95 7.00 41.20
PA?NC 10 3.77 5.95 6.11 2.55 6.76
20 4.89 7.72 8.24 3.47 15.32
30 5.37 8.00 10.17 6.54 28.10
35 5.62 6.67 13.40 13.40 35.00
40 5.81 9.11 12.24 12.24 37.00
45 5.28 7.46 13.02 13.02 33.35
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Figure 4. Impact load vs time responses for neat, polyamide, nanoclay, and polyamide?nanoclay filled GFRE composite laminates
impacted at (a) 10 J, (b) 20 J, (c) 30 J, (d) 35 J, (e) 40 J, and (f) 45 J energy levels.

on a variety of factors including the stiffness and the mass laminates, respectively. For 30 J impact energy level, the
of the samples and the impactor [8, 9]. maximum load exhibited by NC laminate is 11.9%, 16.0%
All of the composite laminates show almost elastic and 15.1% higher than that of PA?NC, PA and neat lam-
behavior under 10 J impact energy as the impact load is inates, respectively and for 35 J impact energy level it is
symmetric before and after unloading. No serious sudden 16.9%, 19.6% and 22.6% higher than that of PA?NC, PA
drop of impact load is observed, indicating that the dam- and neat laminates, respectively. The maximum load rep-
ages created in the specimens were not so severe to reduce resents the peak load value that a composite laminate can
the stiffness of the laminates. For 20 J and higher impact tolerate under a given level of impact energy before major
energy levels, there are sudden drops in the impact load damage is occurred [19]. As a result, it can be concluded
demonstrating significant damage in the composite lami- that the addition of nanoparticles increased the damage
nates. In general, the maximum impact load increases as the resistance of the GFRE laminates at higher impact energy
impact energy level increases. levels especially with the addition of nanoclay, that is
As it can be seen from figure 4, the neat laminate showed nanoparticle filled laminates can tolerate higher impact
higher maximum reaction force than nanoparticle dopped energy levels before undergoing major damage. Hybrid
laminates for the impact energy levels of 10 J and 20 J. But laminate (PA?NC) showed intermediate values between
as the impact energy level increased, the maximum reaction NC and PA laminates in terms of maximum impact load.
force exhibited by the nano-modified laminates exceeds According to Rafiq et al [15] and Mahdi et al [20], the
that of neat laminate. In detail, for the impact energy level improvement in impact resistance is mainly due to the
of 10 J, maximum reaction force exhibited by neat laminate tortuous fracture path and effective load transfer mecha-
is 9.3%, 7.2% and 3.2% higher than that of PA, NC and nism between fiber and matrix created by the addition of
PA?NC laminates, respectively. For 20 J impact energy nanoparticles.
level the percent differences in maximum reaction forces It is also observed from figure 4 that the time to reach
are 5.5%, 6.6% and 1.8% in favor of neat laminate. On the maximum reaction force for neat laminate is generally
other hand, the maximum load for 30 J and 35 J impact shorter than the other material configurations. After the
energy levels is demonstrated by NC, PA?NC, PA and neat impact load reached a maximum value, there is a gradual
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Figure 5. Impact load vs displacement responses for neat, polyamide, nanoclay, and polyamide?nanoclay filled GFRE composite
laminates impacted at (a) 10 J, (b) 20 J, (c) 30 J, (d) 35 J, (e) 40 J, and (f) 45 J energy levels.

recovery to peak load for nanoclay and polyamid doped energy level of 30 J for neat laminate because of signifi-
laminates at the impact energy levels of 30 J, 35 J and 40 J. cantly greater localized damage and complete perforation
This load is carried by the partially damaged and remaining introduced by the higher impulse generated by the higher
laminate layers. However, for the neat laminate there is no impact energy. It is also worth to mention that the frictional
recovery of peak load after the sharp drop for the energy force generated between the impactor and laminate after
levels higher than 30 J which shows complete perforation perforation is higher for nanomodified laminates compared
of the laminate. The perforation thresholds of the to neat laminates as can be seen from figures 4d and 4e.
nanoparticle doped GFRE laminates are higher compared to
the neat laminates which will be discussed in the following 3.2.2 Force-displacement responses Figure 5 shows
subsections. For the impact energy levels higher than 20 J, the impact load vs displacement responses for neat,
the nanomodified laminates showed longer contact dura- polyamide, nanoclay, and polyamide?nanoclay doped
tions at peak load between the impactor and the specimen GFRE composite laminates impacted at different energy
compared to neat laminates, that is they exposed peak levels. As can be seen from the figures 5a-c, perforation did
reaction forces sustained for a longer time which implies not occur in any of the specimens examined for 10 J, 20 J
more damage resistance through laminate thickness and and 30 J impact energy levels. The maximum displacement
more damage propagation through interlaminate interface. of the neat specimen is lower than nanomodified laminates
Within the nonperforated samples, the average impact time for 10 J and 20 J impact energy levels, but it becomes
of neat laminates is slightly lower than the nanomodified higher as the impact energy level reaches 30 J. The
laminates for impact energy levels of 10 J and 20 J. But as maximum displacement of the composite laminates
the impact energy level reached 30 J, the average impact increase as the impact energy level increases. In detail,
time for neat laminates reached 14.56 ms and it was the maximum displacement of neat laminate is 5.71 mm and
highest one compared to the nanoparticle filled laminates. 7.75 mm for 10 J and 20 J impact energies, respectively
For this energy level, average impact time is 10.25 ms for whereas maximum displacements of polyamide, nanoclay
NC laminate, 11.15 ms for PA laminate and 12.6 ms for and polyamide?nanoclay doped laminates are 6.14 mm,
PA?NC laminate. Impact duration drops suddenly after the 6.14 mm and 6.11 mm for 10 J impact energy and
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8.12 mm, 8.38 mm and 8.24 mm for 20 J impact energy, Figure 7. Images of the front and back sides of the composite c
respectively. For the impact energy level of 30 J, maximum laminates impacted at 20 J energy level, (a) Neat, (b) PA, (c) NC,
displacement of neat laminate is 11.27 mm, and it is 13.7%, and (d) PA?NC.
14.8% and 10.8% higher than that of polyamide, nanoclay
and polyamide?nanoclay doped laminates, respectively.
Similar observations can be made for total (permanent) discussed in the ‘‘characterization of physical damage’’
displacement of the laminates. As the reduced maximum subsection.
and total displacement indicates the ability of the laminate
to resist perforation, the nanoclay doped laminate shows the 3.2.3 Energy-time responses and perforation
best performance in this regard for high impact energy thresholds Figure 6 depicts the energy vs time
levels. This inference can be justified looking at the responses for neat, polyamide, nanoclay, and
figures 5d, 5e and 5f. Perforation of the neat laminate, polyamide?nanoclay doped GFRE composite laminates
polyamide?nanoclay laminate and polyamide laminate impacted at different energy levels. In general, the impact
come true at 35 J, 40 J and 45 J impact energy levels, energy for which the impactor does not rebound from the
respectively, whereas nanoclay modified laminate is near specimen for the first time is known as the penetration
the perforation limit at 45 J but is not perforated yet. As a threshold while the absorbed energy for which the nose of
result, it can be said that the addition of nanoparticles into the impactor goes through the back face of the specimen for
GFRE laminates increased the impact resistance of the the first time is defined as the perforation threshold. Thus, at
specimens. Based on the study of Rafiq et al [15], this the penetration threshold, the impactor velocity reaches
improvement in impact resistance can be attributed to the zero but for perforation, the impactor velocity may only
enhanced interfacial adhesion and improved interlaminar become zero under the effect of frictional forces between
shear strength with the incorporation of nanoparticles the impactor and the specimen. In this study, since the
which can change the failure mode from interlaminar to specimen thickness is much smaller than the radius of the
intralaminar. Failure modes of the laminates will further be impactor (2.3 mm to 6.35 mm), no definite penetration

Figure 6. Energy vs time responses for neat, polyamide, nanoclay, and polyamide?nanoclay doped GFRE composite laminates
impacted at (a) 10J, (b) 20J, (c) 30J, (d) 35J (e) 40 J and (f) 45J energy levels.
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b Figure 8. Images of the front and back sides of the composite threshold for 30 J impact energy level. It is also observed
laminates impacted at 40 J energy level, (a) Neat, (b) PA, (c) NC, that the absorbed energy is higher for nanomodified
and (d) PA?NC. laminates than the neat laminates for 10 J impact energy
level, whereas the absorbed energy is higher for neat
laminates than for nanomodified laminates for 20 J and
30 J impact energy levels. As the level of impact energy
reached 35 J, perforation of the neat laminate has occurred,
and perforation threshold of the neat laminate was
determined to be around 32 J. For this energy level, the
energy curve does not show a maximum value, but after a
specific energy level (perforation threshold) is reached it
increases steadily up to the end of the curve due to the
dissipation of energy through frictional forces created
between the impactor and the specimen after perforation.
So, the beginning of straight line indicates the completion
of the crash event and the energy at that point shows the
absorbed energy by the specimen. For impact energies
higher than the perforation threshold, the energy absorbed
stays almost the same which shows no further damage to
the specimen can be introduced. Consequently, no
significant change in the behavior of the energy-time
profile was observed at 40 J impact energy level for neat
laminate. Perforation thresholds for PA, NC and PA?NC
Figure 9. Damage area of NC laminate impacted at 20 J. doped GFRE laminates were found to be around 40 J, 45 J
and 37 J, respectively. Thus, nanoclay doped GFRE
laminates showed the best performance in terms of
impact resistance (with percentage increase of around
threshold is observed that is impactor always rebounds for
40% with respect to neat laminate) and energy dissipation
small impact energy levels or perforates the specimen when
at high impact energy levels.
a specific energy level is reached. The total impact energy
which is determined by the height of the impactor from the
specimen is divided into elastic energy and absorbed
3.3 Characterization of physical damage
energy. Elastic energy is stored in the specimen and used
for the rebounding of the impactor. The beginning of the Figures 7 and 8 show the images of front and back faces of
plateau of the energy-time curve is coincident with the loss the neat and nanomodified laminates impacted at 20 J and
of contact between the impactor and the specimen, so, this 40 J energy levels, respectively. In general, the impact
specific energy indicates the energy absorbed by the damages to the composite laminates can be categorized into
specimen as the formation of damage [15, 16]. As can be interlaminar and intralaminar failures which are related to
seen from figures 6a-6c, there is no perforation in any of the delamination, matrix cracking, fiber fracture, fiber splitting
specimens tested at 10 J, 20 J and 30 J impact energy and fiber pullout [20, 21]. As can be seen from figures 7 and
levels but the elastic energy decreases as the impact energy 8, the impacted laminates showed larger back side damaged
level increases which shows the formation of higher areas as compared to front side damaged areas because
damage. The neat specimen is near to perforation delamination is first formed at the middle plane and

Table 3. Total damage areas of neat and nanomodified composite laminates at different impact energy levels.

Impact Energy (J) Specimen Damage Area (mm2) Standard deviation


20 Neat 329.503 0.37
PA 320.483 0.51
NC 330.481 0.52
PA?NC 332.263 0.49
40 Neat 516.014 0.53
PA 646.073 0.65
NC 798.022 0.67
PA?NC 730.808 0.66
29 Page 12 of 13 Sådhanå (2023)48:29

proceeds at the tensile side (back side) of the specimen neat laminate. On the other hand, the presence of
[10]. Looking at figures 7a-d, it is seen that at 20 J impact nanoparticles increases the brittle behavior of the epoxy
energy level, neat and nanomodified laminates showed resin causing damage to propagate through the in-plane
similar damage patterns mainly matrix cracking, fiber direction rather than in the thickness direction.
pullout and delamination spreading away from the point of
impact which implies that approximately the same amount
of energy is dissipated through the formation of damages
4. Conclusions
such as matrix cracking, fiber pullout and delamination.
This situation can also be verifiable looking at the energy
In this study, the effects of organic intercalated nanoclay
time profiles of the laminates (figure 6b) in which all of the
and spheroidal powder of polyamide 12 additives on the
laminates showed the nearly same amount of absorbed
low velocity impact characteristics of GFRE composites
energy, neat laminates being a bit higher. But as it can be
were investigated by drop weight impact testing. The
observed from figures 8a-d, as the impact energy level
nanocomposites were produced using prepreg and hot-
increased to 40 J, the failure mode changed from inter-
pressing techniques. Nanoparticles with weight percentages
laminar to intralaminar with the addition of nanoparticles to
of 2% were dispersed in the epoxy resin-hardener mixture
GFRE laminates. The addition of nanoparticles enhances
by an ultrasonic sonicator. Control samples with no addi-
the interlaminar shear strength. As in low impact energy
tives were also manufactured for comparison purposes. Six
levels penetration of the impactor into the laminate is
different impact energy levels ranging from 10 J to 45 J
negligible, the improvement in interlaminar shear strength
were used to determine load, deflection, and energy
is more observable at high-impact energy levels which
responses of the laminates. Physical damages introduced in
changes failure mode from interlaminar to intralaminar.
the composite laminates were also examined to determine
Neat laminate showed localized damage in terms of matrix
the impact damage characteristics of the laminates. The
cracking, fiber fracture, and edge delamination occurred at
addition of nanoparticles increased the maximum impact
the point of impact. PA, NC and PA?NC nanomodified
load up to 22.6% at higher energy levels. The perforation
laminates impacted at 40 J showed increased damage area
thresholds of the neat and nanomodified laminates were
in terms of matrix cracking, fiber pullout and fiber fracture.
determined. The perforation threshold of nanoclay doped
For this energy level, energy absorbed by the PA?NC
GFRE laminates was the highest followed by that of
laminate is the highest followed by PA, neat and NC
polyamide, polyamide?nanoclay doped and neat laminates.
laminates. But it is important to mention that at 40 J impact
Overall, the addition of nanoparticles increased the impact
energy level, complete perforation of the neat and PA?NC
damage resistance of the GFRE laminates. Analyzing the
laminates has occurred, and PA laminate is near to perfo-
physical damages introduced in the composites, it is
ration limit, whereas NC laminate showed extensive matrix
observed that neat laminates showed localized damages in
cracking, fiber pullout and fiber splitting, but no complete
terms of matrix cracking, fiber fracture, and edge delami-
perforation which indicates an increase in impact resistance
nation occurred at the point of impact whereas nanomodi-
and a further energy absorption capability due to changes in
fied laminates showed increased damage area in terms of
failure mechanism with the inclusion of nanoclay to epoxy
matrix cracking, fiber pullout and fiber fracture at 40 J
matrix.
impact energy level. The addition of nanoparticles altered
The total damage area was calculated by employing
the impact behavior and damage mechanisms of the GFRE
back-lighting method. Specimen photos have been scaled
laminate at high impact energy levels leading a damage to
with reference to sample sizes. Visible damage areas are
propagate through the in-plane direction rather than in the
based on color tone transitions in order to detect the dam-
thickness direction.
age edges. As an example, the damage area of NC laminate
impacted at 20 J was given in figure 9. The calculated
damage areas cover the damage from all modes including
Acknowledgements
delamination, matrix cracking, fiber fracture and fiber
pullout. They were given in table 3. At 20 J impact energy
The authors would like to thank Pamukkale University
level, total damage areas of all of the laminate types are
Scientific Research Council for supporting this study under
nearly equal to each other. As the impact energy level
project contract number 2017FEBE049.
increased to 40 J, nanomodified laminates demonstrated
bigger damage areas compared to neat laminate.
Overall, nanomodified laminates showed better perfor-
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