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International Journal of Impact Engineering 96 (2016) 11–22

Contents lists available at ScienceDirect

International Journal of Impact Engineering


j o u r n a l h o m e p a g e : w w w. e l s e v i e r. c o m / l o c a t e / i j i m p e n g

The energy absorption behavior of hybrid composite laminates


containing nano-fillers under ballistic impact
Edison E. Haro *, Akindele G. Odeshi, Jerzy A. Szpunar
Department of Mechanical Engineering, University of Saskatchewan, Saskatoon, Canada

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

Article history: Hybrid composite laminates consisting of woven Kevlar fiber fabric, epoxy and AA 5086-H32 aluminum
Received 27 November 2015 sheets were produced and the effects of addition of micro and nano-fillers to the fiber on ballistic re-
Received in revised form 15 March 2016 sponse of the hybrid laminates were investigated. The micro and nano-fillers used in this study are powders
Accepted 18 May 2016
of aluminum, gamma alumina, silicon carbide, colloidal silica and potato flour. They were introduced into
Available online 20 May 2016
the Kevlar fabrics by mixing with polyethylene glycol (PEG-400), followed by impregnation of the Kevlar
fabric with the mixture and drying to eliminate the solvent. The energy absorption by the hybrid com-
Keywords:
posite laminates containing the various nano-fillers under ballistic impact were determined and compared
Hybrid composites
Energy absorption with laminate containing no nano-filler impregnation. The ballistic impact resistance of the produced
Ballistic impact hybrid composite laminates was tested according to NATO standards using a caliber 270 Winchester rifle.
Protective armor The projectile penetration and the resulting perforations of the hybrid laminates were studied in order
Nano-fillers to determine the influence of the deposited nano-fillers on Kevlar fibers on their energy absorption and
impact resistance. The relationship between areal density and energy absorbed are discussed to deter-
mine which specimens perform better under ballistic impact. Protection levels achieved by targets were
analyzed in relation to the initial impact energy from low caliber weapons. The results indicate that the
ballistic impact resistance and impact energy absorption of the hybrid composite laminates were en-
hanced by deposition of micro and nano-fillers into surface of the Kevlar fibers fabrics. The highest impact
energy absorption capacity was achieved by deposition of aluminum powder followed be colloidal silica
and silicon carbide powder in that order. Addition of gamma alumina powder and potato flour has pro-
duced the least effect of enhancing the impact energy absorption capability of the laminates. These findings
indicate that introduction of micro- and nano-fillers coating on Kevlar fabrics using PEG-400 is a prom-
ising method for strengthening interfacial bonding between the matrix and fibers in hybrid composite
laminates.
© 2016 Elsevier Ltd. All rights reserved.

1. Introduction with enhanced protection capability [2]. The motivation for the in-
creased interest in the use of nanoparticles with dimensions ranging
Improving the shielding capacity of protective armor materials from 1 to 100 nm in engineering applications include their unique
against ballistic impact has continued to attract the interest of the surface strengthening effect in metal alloys, ceramics, fibers, and
scientific community. Development of hybrid composite laminate even polymers leading to increase in mechanical properties such
structures can offer a solution of providing protective shields that as strength and stiffness, and thermal properties, among others.
are lighter, leaner, and more potent than the conventional protec- Nanoparticles in low concentrations can achieve these purposes
tive armor plates made of monolithic materials. Hybrid materials without compromising the density, toughness or the manufactur-
consist of layer of two or more existing materials configured in such ing process [3–5].
a way that allows the superposition of their properties to meet tar- Most of the studies on armor vests used in ballistic protection
geted service requirements [1]. In hybrid composites, improved have reported ways of improving the resistance of Kevlar fibers to
multilayer structures combining properties of widely diverse ma- ballistic impact failure. One of the most common ways of achiev-
terials such as metal alloys, fibers, natural materials, and even ing this is through impregnation of the Kevlar fabrics with shear
nanoparticles are made possible in order to achieve protective armor thickening fluid (STF). STF consists of oxide particles suspended in
a liquid polymer. It behaves as a non-Newtonian fluid whose vis-
cosity increases when shear stress is applied. The components of
STF are polyethylene glycol and colloidal silica. STF assumes a solid-
* Corresponding author. Department of Mechanical Engineering, University of
Saskatchewan, Saskatoon S7K7Y3, Canada. Tel.: +13062034589; Fax: +1 306 966 5324. like behavior at the moment of impact loading. After impact loading,
E-mail address: eeh866@mail.usask.ca (E.E. Haro). they return to their fluid state [6,7]. Colloidal silica particles create

http://dx.doi.org/10.1016/j.ijimpeng.2016.05.012
0734-743X/© 2016 Elsevier Ltd. All rights reserved.
12 E.E. Haro et al. / International Journal of Impact Engineering 96 (2016) 11–22

a sealing coat, which enhances the resistance of the woven fibers performance (energy absorption capability) of the CFRPs [22]. Ad-
to ballistic impact. Infiltration of aramid fiber fabrics with STF results dition of carbon nanotubes (CNTs) and nano-sized core shell rubber
in a microstructural change as the colloidal silica in the STF create particles (CSR) to Kevlar fiber reinforced epoxy also led to improve-
particle clusters (hydro clusters), which enhance the hydrody- ment in impact energy absorption capacity [23]. Different techniques
namic stress in the suspension and increase the capacity to resist of nano-particles’ dispersion have been employed to enhance in-
ballistic impact [8,9]. Experimental investigations have proved that terfacial bonding between matrix and fibers. For example, CNTs
the resistance of Kevlar fabrics to ballistic penetration is improved particles were impregnated directly on carbon fibers through im-
by impregnation with silica particles (size 450 nm) dispersed in eth- mersion in an aqueous suspension prepared with CNTs, which led
ylene glycol. In addition, it was established that this impregnation to better results compared to that other dispersion techniques such
enhanced the material flexibility and reduced the required thick- as CNTs mixed with epoxy resin or spraying methods [24].
ness for adequate protection when compared with Kevlar fabrics Although many studies have been conducted on the effects of
with no STF-impregnation [10]. According to Majumdar et al. [8], STF, CNTs, and Al2O3 impregnation into the resin matrix of fiber re-
the higher the STF concentration, the better the capacity for impact inforced plastics on their ballistic impact resistance. However, there
energy absorption by fibrous materials, and the lower will be the is no information on the ballistic impact response of hybrid com-
number of fiber layers required for the needed protection. STF in- posites plates consisting of aluminum alloy, epoxy and Kevlar fabrics
creases the friction between the yarns during ballistic impacts and impregnated with other nano-fillers. It is very important to deter-
reduces the number of Kevlar layers used in composite laminates mine whether nano-fillers impregnation into fibers will allow such
by between 40 and 80% [11]. About 50% increase in energy absorp- hybridization with metallic layers to produce high performance pro-
tion capacity was reported when Kevlar was impregnated by STF tective armor. In this study, nano-fillers of silica carbide, aluminum
in comparison with composites made of Kevlar fabric that is not powder, colloidal silica, gamma alumina, and potato flour were mixed
treated with STF [12]. with a solution of polyethylene glycol (PEG-400) and were then in-
In another study, the use of aluminum oxide (Al2O3) nano- filtrated into Kevlar fabrics in order to improve the energy absorption
fillers in epoxy resin reinforced with Kevlar 29 fabrics was reported capacity of the resulting hybrid composite laminates. This is a new
to improve the performance of bulletproof vest made of this com- infiltration method of micro and nano fillers into fabric fibers and
posite material. Composite plates of different thickness were used the feasibility of deposition using polyethylene glycol (PEG-400) will
to show the level of energy absorption by each plates during bal- be evaluated. The objective of this study is to improve the ballistic
listic impact testing. The results showed that by using a stacking impact resistance and toughness of the hybrid composite lami-
sequence of 30 layers cross–ply laminates, the highest energy ab- nates by addition of these nano-fillers to reinforce the Kevlar fiber
sorption was achieved with an impact velocity of 400 m/s [13]. In components without significantly altering the material’s physical
the same way, epoxy resin filled with oxide nanoparticles of silane properties such as weight, thickness or density. The capacity of the
modified iron (III) was impregnated into Kevlar fibers to create re- obtained hybrid composite laminates to absorb energy, as a func-
inforced composite laminates; the oxide nanoparticle impregnation tion of the type of the applied nano-fillers was determined by
resulted in a significant enhancement of the tensile strength of the conducting ballistic impact testing using a 270 caliber Winchester
laminates [14]. Also, Kevlar fibers impregnated with epoxy resin filled rifle and 150 gr power point ammunitions with an average mass
with cork powder, cork/clays, and clays were compared with speci- of 9.72 g.
mens made of epoxy resin reinforced with Kevlar. Previous research
findings indicated that addition of cork powder to polyester resin
2. Material and experimental procedure
reduces the flexural strength, and that the addition of the fillers can
change the mechanical behavior of the matrix. However, for both
2.1. Materials
kinds of specimens, similar fatigue strength was observed [15]. In
another experiment, the results indicated that fillers impregna-
2.1.1. Aluminum alloy AA 5086-H32
tion enhances the impact resistance by 4.5% for laminates filled with
The hybrid composite laminates were built using AA 5086-H32
cork, by 10.4% for laminates filled with cork/clay and by 16.1% for
aluminum alloy sheet, supplied by Onlinemetals.com (US), as the
laminates filled with clay [16]. When carbon fibers were coated with
metallic component. The aluminum alloy sheets have a thickness
carbon nanotubes as nano-fillers in an epoxy resin, the fiber surface
of 1.6 mm and a nominal chemical composition of 95.4 Al, 0.05–
area increased, which provided a stronger interfacial bonding
0.25 Cr, 0.1max Cu, 0.5max Fe, 3.5–4.5 Mg, 0.2–0.7 Mn, 0.4max Si,
between the CNT/carbon fiber/epoxy matrix [17–19]. Hybrid nano-
and 0.25max Zn. The primary role of the AA 5086 aluminum alloy
composites developed using different configurations of fiberglass/
sheet is to act as rigid plates that support the fibrous materials and
epoxy/nano-clay and fiberglass/epoxy/nano graphene were subjected
keep them in their relative positions within the hybrid laminates.
to ballistic impacts from 38 and 9 mm caliber pistols, and the results
They can also help to hinder propagation of crack through the fibers
showed that hybrid nano-composites are able to absorb impact
and protect the fibers from the environment. The aluminum plate
energy ranging from 284 J to 446 J, and that nano-clay and graphene
will enable uniform distribution of impact loads and enhance impact
additions into the epoxy matrix increase the energy absorption ca-
resistance of the laminates.
pacity of the hybrid nano-composites [20].
In another study, woven carbon fibers were reinforced with a
polymer/epoxy matrix containing dispersed short multi-walled 2.1.2. Kevlar fibers 49
carbon nanotubes and significant improvement in inter-laminar The Cross-ply woven Kevlar fiber 49 (#281-38) fabric used in this
damage tolerance was achieved with the carbon nanotubes addi- study was supplied by Aircraft Spruce Canada. The fabric has a thick-
tion (0.5 wt. %) to the epoxy matrix. The static interlaminar shear ness of 0.25 mm and a mass of about 169.8 g/m2. The role of the
strength of the hybrid composite was found to increase by 20%, and Kevlar fibers is to act as reinforcement and enhance the mechan-
interlaminar fracture toughness (Mode I) by 180% in relation to the ical properties such as tensile and flexural strength of the polymer
samples without nano-reinforcement [21]. In an effort to improve matrix. Their high tensile strength prevents significant stretching
the impact resistance of a carbon fiber reinforced plastic (CFRP), and deflection of resultant composite materials during ballistic
about 0.5% by weight of multi-wall carbon nanotubes (MWCNTs) impacts. These fibers slow down the projectile penetration through
were dispersed in the epoxy matrix (Bisphenol A). The MWCNTs in- the initial tensile elongation, inter-laminar delamination and fiber
clusion enhanced the fracture resistance and ballistic impact pullout. In addition, their high strength and elastic modulus enhance
E.E. Haro et al. / International Journal of Impact Engineering 96 (2016) 11–22 13

the kinetic energy absorption and the transverse deformations pro-


duced by high-velocity impacts [25,26].

2.1.3. Polyethylene glycol (PEG-400) Layers of Al


Polyethylene glycol (Carbowax PEG-400 NF) supplied by Fisher 5086/H32
Chemical (Canada), with a pH of 4.5–7.5 (5% sol) and a density of
1.13 g/ml was the solvent used in dispersing the nano-fillers into Layers of Kevlar 49/285
the Kevlar fabric. It is made of Carbowax (C2H4 on H2O) and has low impregnated with STF /
volatility and good thermal stability. The use of PEG-400 enables micro hard particles
an efficient dispersion of nano-fillers into Kevlar fabrics [27].
Fig. 1. Configuration of hybrid composite laminate.
2.1.4. Epoxy resin
Epoxy resin Pro-set (LAM-125) mixed with hardener (LAM-
229) was used as the polymeric component of the hybrid composite
composites made of palm fruit fibers for use as bullet proof plates
laminate. These resins were supplied by Aircraft Spruce Canada.
in armored vehicles [28].
Epoxy plays a critical role of bonding the various components of
the laminates together. It has low viscosity and it is very effective
in bonding Kevlar and carbon fiber fabrics. Pro-set LAM-229 is a slow 2.2. Target preparation
curing hardener, which requires 4 to 5 hours curing time at room
temperature. This gives room for more processing time in the fab- 2.2.1. Preparation of aluminum alloy AA 5086-H32 and Kevlar layers
rication of composite materials with the epoxy resin. The resin mixed The AA 5086 Al-H32 aluminum alloy sheet was cut into
with hardener also bonds the aluminum plates with the Kevlar fiber 15 cm × 15 cm square pieces. Their surfaces were degreased and
fabrics to achieve a completely rigid structure. grinded with SiC emery paper to remove surface oxide layers. They
were subsequently cleaned with ethyl alcohol and dried in readi-
2.1.5. Micro and nano fillers ness for use in the manufacture of the hybrid laminates. The Kevlar
The 406 colloidal silica (SiO2) manufactured by West System, Inc. fabrics were cut into the same dimension as the aluminum plate.
(USA) used as one of the nano-fillers is an adhesive filler whose com- Fig. 1 provides a schematic representation of the specimen’s con-
ponents are sand and quartz. It has an average size of between 200 figuration of hybrid composite laminates.
and 300 nm and a density of 0.048 g/ml. It is a thickening additive
used as a strong gap filler. When added with PEG, it becomes easy 2.2.2. Dispersion of nano and micro particles
to impregnate colloidal silica into fibrous materials. Its infiltration To enhance the nano-fillers impregnation, polyethylene glycol
into Kevlar fibers improves fiber strength and the impact resis- (Carbowax™ PEG-400) and the fine particles of fillers were mixed
tance of the composite made from such fiber [27]. Uncoated together using a constant proportion of 100 ml of PEG-400 to 50 g
aluminum powder UN1396 purchased from EM Science (USA) with of the fillers for all targets. The mixtures were stirred using a mag-
200 mesh (74 μm) sizes were also applied as an micro additive or netic stirrer rotating at 1200 RPM for 3 hours at room temperature.
micro filler in sealing the voids between fiber bundles in the Kevlar The mixtures of nano-fillers and PEG were thereafter diluted in
fabrics. Silicon Carbide (SiC) supplied by Sigma-Aldrich Co. (Canada) 100 ml of ethyl alcohol using the same procedure for 2 hours, except
in 200–450 mesh (37–74 μm particle size) is another micro filler that the samples made with potato flour that was already a diluted
used in this study. It is an artificial abrasive manufactured in electric- solution. Different STF containing different type of micro or nano-
resistance furnaces by the reaction of silica and carbon at high fillers were impregnated on Kevlar fabrics individually on the both
temperature. Another nano-filler used is gamma alumina (Al2O3) sides using the same amount of solution and on the same quanti-
powder (0.05 μm size) that was purchased from LECO Corpora- ty of Kevlar fabrics. For example, 250 g of STF containing different
tion (UK). Talib et al. [13] concluded that a mixture of these particles nano-fillers diluted in ethyl alcohol solution were impregnated in
with an epoxy resin infiltrated into Kevlar layers can increase the 20 layers of woven Kevlar fabric. The same proportion was used for
level of energy absorbed by composite plates under high velocity all plates produced as indicated in Table 1. In addition, Kevlar fabrics
impact. Potato flour is a natural binder used in glues and as natural were weighed before and after STF impregnation in order to ensure
fillers in fibers in order to develop environmental friendly com- the same amount of STF (with nano-fillers) were impregnated
posites. Potato starch has been used as a natural binding agent in into the fabrics. The impregnated fiber fabrics were then dried for

Table 1
Experimental data sheet showing laminates’ composition and configuration and their physical properties.

Targets configuration K20 + STF (nano-filler solutes metallic, ceramic and naturals)

Al/K20/Al Al/K20/Al Al/K20/Al Al/K20/Al Al/K20/Al Al/K20/Al


(K untreated) (silica carbide) (potato flour) (aluminum powder) (colloidal silica) (alumina)

Al 5086 thickness 1.6mm (g) 190 190 190 190 190 190
weight only K pure (g) 75 75 75 75 75 75
STF solutes (ml) 0 150 150 150 150 150
Additives (g) 0 50 50 50 50 50
PEG-400 (ml) 0 100 100 100 100 100
Ethyl alcohol used (ml) 100 100 0 100 100 100
Resin used (ml) (4:1) 100 100 100 100 100 100
Target weight measured (g) 332 378 386 390 398 434
Target thickness (mm) 8.1 9.7 9.5 10.8 10.6 11.8
Target areal density (g/cm2) 1.5 1.7 1.7 1.7 1.8 1.9

Al = aluminum 5086-32 alloy; K20 = 20 layers of woven Kevlar fiber cloth (i.e. the figures following K indicate the number of fiber layers); K untreated = Kevlar containing
no impregnated nano-fillers.
14 E.E. Haro et al. / International Journal of Impact Engineering 96 (2016) 11–22

Fig. 2. Mass, thickness and areal density of the developed hybrid laminate as a function of the applied nano-filler.

72 hours at room temperature (22 °C) until all the ethanol resi- have the same average areal density of 1.7 g/cm2 while those con-
dues were completely evaporated. taining colloidal silica have an average areal density of 1.8 g/cm2.

2.2.3. Bonding of layers 2.3. Experimental testing


Epoxy resin (LAM-125) and hardener (LAM-229) were mixed in
a proportion of 4:1 according to the supplier’s specifications in order 2.3.1. Microstructure analysis (SEM)
to bond Kevlar fiber layers with one another and with the AA 5086- Microstructural analysis was performed using Hitachi SU6600
H32 aluminum plate in a laminated configuration. Hand lay-up scanning electron microscope (SEM) at accelerated voltage of 3.0 kV
method was used to produce the specimens. The hybrid compos- in order to determine the distribution of nano-fillers and the quality
ite plates were subjected to a compressive pressure of 1600 Pa using of the adhesion between the nano-fillers and the Kevlar fiber surface.
a manual laminating press for 24 h at room temperature. The ap-
plication of pressure was to ensure a proper bonding of fiber layers 2.3.2. Ballistic impact test on the field
with the metallic sheets and also to ensure homogeneous distri- The resistance of the targets developed was evaluated accord-
bution of the epoxy resins in the laminates. The impregnated fabrics ing NIJ 0108.01 standard for protective armor materials [29]. The
were stacked after the resin had reached B-stage to minimize loss tests were performed using high-velocity impact of targets
of resin during the final stage of curing under pressure. Table 1 shows 15 cm × 15 cm in size. Fig. 3 provides a schematic representation of
the components and the configuration of the various hybrid com- the ballistic testing system. The ballistic impact tests were carried
posite plates produced for investigation in this research study. In out using a rifle caliber 270 Winchester and ammunitions of 150 gr
each plate, two aluminum sheets surround 20 Kevlar layers, which power point with an average mass of 9.72 g. In order to determine
were previously treated by impregnation with nano-fillers or not. the initial velocity, two targets were developed and four shots were
The weight and thickness of plates containing impregnated nano- fired at each target (8 shots in total). In subsequent tests to deter-
fillers are higher than those containing no nano-filler. These physical mine energy absorption for each category of laminate, three targets
properties also vary depending on the type of the nano-fillers used. were developed and two shots were fired at each target making a
The comparative values of the weight, thickness, and areal density total of six shots for each type of plate. Shots were performed from
of various specimens developed for various hybrid laminates can a distance of 15 m to penetrate the plate one side and exit on the
be clearly observed in Fig. 2. Such variations can be attributed to other side. This distance is suitable to achieve stability [30] and obtain
variation in the nano-filler residue after the evaporation of PEG- a reliable data depicting the ballistic behavior of the materials. A
400 during the drying of the fibers, and the difference in resin muzzle velocity of about 869 m/s and a muzzle energy of 3667 J of
absorption capability of treated and untreated Kevlar fabric layers. the projectile are usually obtained according to NATO standard
For instance, targets with Kevlar neat showed greater resin absorp- [31,32]. The initial and residual velocities of the projectiles were re-
tion than targets with Kevlar containing impregnated nano-fillers. spectively measured before and after impact in order to determine
The samples treated with gamma alumina powder have the highest the impact energy absorption. Ballistic precision chronographs
thickness, mass and areal density. The areal density was calcu- (Caldwell) were used to measure the entry and residual velocities
lated by dividing the density with the surface area of the plate. An of the projectiles.
areal density of 1.5 g/cm2 was obtained for specimens made of Kevlar The energy absorption by each produced hybrid plate was cal-
with no nano-filler impregnation, which is lower than that of those culated in order to enable classification of the plates according to
plates made with Kevlar impregnated with nano-fillers. The plates NIJ 0108.01 standard for ballistic resistant materials. With that, the
made with Kevlar impregnated with gamma alumina nano-powders calculated energy absorption for each material can be compared with
have the highest areal density (average of 1.9 g/cm2). The lami- the velocity and energy specifications of different low caliber
nates containing potato flour, aluminum powder, and silica carbide weapons according to NATO standards (Table 3). The initial impact
E.E. Haro et al. / International Journal of Impact Engineering 96 (2016) 11–22 15

Fig. 3. Graphical representation of the ballistic testing system.

energy, residual energy, and absorbed energy were calculated based average initial velocity was chosen to produce similar initial con-
on the initial velocities before impact (Vi) and exit or residual ve- ditions for all of the targets.
locities (Vr) after perforation of the target by the projectile of mass The residual and absorbed energy for targets containing differ-
m as follows: ent nano-fillers are graphically displayed in Fig. 4. Specimens
containing Kevlar fabric infiltrated with aluminum powder exhibit
1
Initial (impact ) energy ( J) = mVi2 (1) the highest energy absorption (693 J), which represents an 18.8%
2 of the initial energy, followed by targets made of Kevlar fabrics im-
pregnated with colloidal silica (679 J) and silicon carbide (666 J)
1
Residual energy of projectile after impact ( J ) = mVr2 (2) particles. The energy absorption of the laminates containing col-
2 loidal silica and silicon carbide particles are only 0.39% and 0.73%
lower than that containing aluminum powder, respectively. The
Velocity absorbed (m/s ) = Vi − Vr (3) targets specimens containing impregnated potato flour and gamma
alumina were able to absorb 553 J and 543 J, respectively. The lowest
1 1 energy absorption of 507 J was determined for plates made of Kevlar
Energy absorbed or dissipated ( J) = mVinitial
2
− mVresidual
2 (4)
2 2 fabric with no nano-filler impregnation. These results suggest that
deposition of nano-fillers on Kevlar fabrics used in producing hybrid
⎛ dissipated energy ( J) ⎞ composite laminates improved the energy absorption capability of
% Energy dissipated = ⎜ ⎟⎠ × 100 (5)
⎝ initial energy the laminates. Kostopoulos et al. [22] also reported that CNT inclu-
sion in the matrix of CFRP composites increases their energy
3. Results and discussion absorption capability and impact damage resistance.
A comparative analysis of the correlation between the areal den-
3.1. Effects of target configuration and filler addition on absorbed sities of the targets and their energy absorption during ballistic
and residual energy impact are presented in Fig. 5. Both the energy absorption and the
areal density of targets containing Kevlar fabric with no nano-
The results of previous studies have shown that the kinetic energy filler addition are less than those of the other targets containing
of a projectile is transformed into work and a fraction of the initial nano-fillers. On the other hand, specimens containing gamma
energy is absorbed in deforming the target. The absorbed energy alumina powder impregnation have low energy dissipation, but the
by the target represents the loss in kinetic energy through elastic highest areal density of all targets. Targets with higher energy ab-
and plastic deformations while the residual kinetic energy is the sorption (aluminum powder, silica carbide and colloidal silica) have
projectile energy that remains after the ballistic impact [33]. a similar average areal density of 1.7 g/cm2. A previous study by Lee,
The effects of the applied nano-fillers on the energy absorption et al. [10] also indicated that whereas impregnated fibers with STF
capability of the hybrid composite plates produced in this study are had an areal density similar to that of Kevlar with no STF impreg-
provided in Table 2. The average initial velocity of 871 m/s, with a nation, Kevlar containing impregnated STF has reduced thickness
standard deviation of 6.70 m/s, was recorded by the ballistic chro- and absorbed more impact energy. The impact energy absorption
nograph, which is comparable to the muzzle velocity of 869 m/s for has been reported in other ballistic impact tests and stabbing ex-
the same ammunition as provided in NATO specifications. This periment to increase by about 30 and 40% with STF impregnation

Table 2
Ballistic impact data sheet for various laminate targets produced.

Targets INITIAL velocity INITIAL energy RESIDUAL velocity RESIDUAL energy Velocity Energy Energy
average (m/s) average (J) average (m/s) average (J) absorbed (m/s) absorbed (J) absorbed (%)

Al/K20/Al (aluminum powder) 871 3687 785 2994 86 693 18.8%


Al/K20/Al (colloidal silica) 871 3687 787 3008 84 679 18.4%
Al/K20/Al (silica carbide) 871 3687 788 3021 83 666 18.1%
Al/K20/Al (potato flour) 871 3687 803 3134 68 553 15.0%
Al/K20/Al (gamma alumina) 871 3687 804 3144 67 543 14.7%
Al/K20/Al (untreated) 871 3687 809 3180 62 507 13.7%
16 E.E. Haro et al. / International Journal of Impact Engineering 96 (2016) 11–22

Fig. 4. Residual and dissipated energy during ballistic impact.

in comparison with specimens made with Kevlar neat, i.e. with no 3.2. Energy absorbed by the targets vs the initial impact energy of
impregnation with STF or any other nano filler [9,10,34]. Avila et al. projectiles fired by different light weapons
[20] also reported an improvement in the energy absorption capa-
bility of fiber reinforced epoxy composite by the addition of The initial velocity and energy specifications of nine low caliber
nanoparticles of clay and graphene. The addition of the nanoparticles weapons according to NATO standard specifications [32] are pre-
was observed to strengthen fiber/matrix bonding and they acted sented in Table 3. The initial energy of 3687 J used in this study is
as barrier to crack propagation leading to increase in penetration higher than the energy specifications shown in this table. Thus, the
resistance. results obtained in this experiment can be compared with the data
In the current investigation, the thickening fluids formed by nano- provided in Table 3. The horizontal lines in Fig. 6 represent the ab-
fillers and PEG-400 coated the Kevlar fibers and produced a nano- sorbed energy determined for each hybrid laminate tested. The initial
filler sealing on the fiber layers in the hybrid laminate structure. impact energy of ten low caliber weapons is presented in vertical
The nano-filler impregnation enhanced the amount of energy ab- bars. The results indicate that hybrid composite laminates built with
sorbed during the projectile penetration. Therefore, treatments of the configuration Al/K20/Al and Kevlar that is untreated with nano-
Kevlar fabrics with thickening fluids containing nano-fillers en- fillers, and those containing Kevlar impregnated with potato flour
hanced the ballistic impact resistance of the fabrics. As a result, or gamma alumina powder cannot resist the ballistic impacts from
failure resistance and the energy absorption are greater. This sug- those weapons. The reason for that is that the energy they can absorb
gests that deposition of nano-fillers coating on Kevlar fabrics using are below the initial energy produced by lowest caliber HK and
PEG-400 offers a promising method for strengthening the interfa- Parabellum pistols (9mm), which are 570 J and 561 J, respectively.
cial bonding between the matrix and fibers in hybrid composite The configuration Al/K20/AL containing impregnated aluminum
laminates. powder, colloidal silica, and silica carbide are able to absorb impact

Fig. 5. Relation between the absorbed energy and areal density of targets.
E.E. Haro et al. / International Journal of Impact Engineering 96 (2016) 11–22 17

Table 3
Velocity and energy specifications of low caliber weapons.

Low caliber weapons Cartridge (mm) Cartridge weight (g) Bullet weight (g) Velocity (m/s) Energy (J)

270 Winchester rifle 7.06 150 9.72 869 3667


AK-47 rifle 7.69*39 24 8 715 2045
M14 rifle 7.62*51 25.4 9.33 838 3275
FAL rifle 7.62 24 9.5 823 3217
M16 rifle 5.56*45 12.31 4.02 991 1974
HK rifle 5.56 4.1 936 1796
AUG rifle 5.56 4 940 1767
Beretta M9 pistol 9 *19 8.1 4.1 600 756
HK pistol 9 7.45 4.5 390 570
Parabellum pistol 9 9.5 5.2 460 561

Reference: NATO EPVAT testing, Quick LOAD, SAAMI, standard.

Fig. 6. Absorbed impact energy from targets vs initial energy from different low caliber weapons.

energy ranging from 666 J to 693 J. This means that they can resist The average diameter of the crater entry on the front face, and the
bullets from pistol HK and Parabellum 9 mm, but they are not able average diameter of the crater exit on the back face were mea-
to resist shots from pistols Beretta M9, whose initial impact energy sured. The total depth of penetration (Fig. 7) on the transverse section
is 756 J; and also from 5.56 mm caliber rifles and higher caliber of each specimen was measured as well. Fig. 8 shows the morphol-
weapons. ogy of the penetration channel at the entry and exit sides of the
targets that were produced by the projectile (diameter 7.06 mm)
3.3. Analysis of deformation and penetration behavior of the targets ogive (spitzer ogive shape). The diameter of the crater (perfora-
tion) at the entry side ranged between 8.8 mm and 9.4 mm for all
The projectile penetration data for the various hybrid lami- targets. The exit diameter of the crater on the back side ranged
nates during the ballistic impact testing are presented in Table 4. between 13.5 mm and 15.8 mm, forming an open petal after com-

Table 4
Penetration morphology in the laminate after ballistic impact.

Targets Energy Initial target Target areal Entry crater Exit crater Penetration
absorbed (J) thickness (mm) density (g/cm2) diameter (mm) diameter (mm) depth (mm)

Al/K20/Al (Al powder) 693 10.8 1.7 9.4 13.5 25.2


Al/K20/Al (colloidal silica) 679 10.6 1.8 8.8 15.8 24.2
Al/K20/Al (silica carbide) 666 9.7 1.7 9.4 15.2 23.7
Al/K20/Al (potato flour) 553 9.5 1.7 9.0 15.0 22.3
Al/K20/Al (gamma alumina) 543 11.8 1.9 9.1 14.5 26.1
Al/K20/Al (untreated) 507 8.1 1.5 9.1 14.9 21.1
18 E.E. Haro et al. / International Journal of Impact Engineering 96 (2016) 11–22

Total depth
penetration (mm)

Fig. 7. Total depth penetration channel on the transverse section of the targets.
Fig. 9. Rear and front faces of targets after ballistic impacts.

plete projectile penetration. The petal shaped appearance depends


on several factors such as the target configurations, thickness, nano- made of hybrid laminates usually depends on the configuration and
filler impregnation and type of nano-filler used and the energy the number of layers of each component of the laminate. The thick-
absorption capability of the aluminum and Kevlar fabric compo- ness of the hybrid laminate targets produced in this study are
nents. The morphology of the crater at the entry and exit sides can provided in Table 1. Laminates containing 20 layers of untreated
be more clearly seen in Fig. 9. Similar morphology was observed in Kevlar fabric (i.e. no infiltration with nano-filler) have an average
the craters of GLARE specimens made of 2024-T3 aluminum layers, thickness of 8.1 mm in comparison with those made of Kevlar treated
E-glass fibers and epoxy resin during ballistic impact testing; a petal with nano-fillers, whose thickness range between 9.5 and 11.8 mm.
shape was observed on the back aluminum layers. Although as the Figs. 10 and 11 provide the relationship between weight and thick-
impact energy were increased, larger petals were observed, but be- ness in relation to the energy absorbed by the laminates, respectively.
havior was determined to be similar for all targets [35]. Weight and thickness are higher for the targets treated with gamma
The total depth of penetration depends basically on two factors: alumina powder than other laminates as can be observed in the
the thickness and the configuration of the targets. The penetra- graphs. Despite that, they are not capable of absorbing more impact
tion depths on the transverse sections of hybrid laminate targets energy than the targets containing other nano-powders. Targets con-
produced in this study are provided in Table 4. They ranged between taining impregnated silica carbide exhibited a top ballistic
21.1 mm and 26.1 mm. In addition, it can be concluded that targets performance because their average energy absorption of 666 J this
made of Kevlar neat, which have the lowest thickness and low energy was obtained with the lowest density (weight 378 g and thickness
absorption capacity, have the lowest penetration depth of 21.1 mm. 9.7 mm) in comparison to targets containing other nano fillers.
Thus, this implies that these targets have less resistance to the pro-
jectile penetration. The targets containing Kevlar fabric infiltrated 3.5. Microstructure analysis and mechanisms of energy absorption
with potato flour have a penetration depth of 22.3 mm. Laminates
with better ballistic performance in terms of penetration depth are Fig. 12 shows the results of the scanning electron microscopic
those targets containing impregnated aluminum powder, colloi- (SEM) evaluation of the impregnation of the Kevlar fabrics with nano-
dal silica, and silica carbide powder. They showed penetrations powders. Fig. 12a shows Kevlar fabric neat (with no nano-powder
depths of between 23 and 25 mm. Targets with gamma alumina ex- impregnation) indicating void spaces between fibers bundles. When
hibited the highest penetration depth of 26.1 mm, but a low energy joined with other layers of Kevlar fabrics by using epoxy resin, the
absorption. This may also be due to the fact that they have the loops were filled with only resin. This suggests that the hybrid lami-
highest thickness compared to the other laminates. nate structure containing Kevlar neat can be less effective in resisting
ballistic impact damage. Targets built with Kevlar containing im-
3.4. Targets’ thickness and weight influence on ballistic response pregnated nano-fillers show fewer voids between fibers bundles and
between fiber layers. The properties of the nano-fillers, the surface
Thickness is an important factor in the energy absorption ca- morphology of the Kevlar fibers, and the fiber size are factors that
pability of targets during ballistic impact. The thickness of a target have significant effects on the impregnation state of the nano-

Exit

Entry

Fig. 8. Morphology of penetration channel at the entry and exit sides of the targets.
E.E. Haro et al. / International Journal of Impact Engineering 96 (2016) 11–22 19

800 800
693 679
700 666 700

Target weight measured (g)

Energy absorbed (J)


600 553 543 600
507
500 500
390 398 378 386 434
400 332 400

300 300

200 200

100 Target weight measured (g) 100


Energy absorbed (J)
0 0
Al/ K20 /Al Al/ K20 /Al Al/ K20 /Al Al/ K20 /Al Al/ K20 /Al Al/ K20 /Al
(Aluminum (Colloidal (Silica (Potato (Gamma (untreated)
powder) silica) carbide) flour) alumina)

Fig. 10. Relation between the absorbed energy and target weight.

powders. The nano-powder filled the gaps existing between Kevlar micrographs show good adherence to the fibers and sealed up the
fiber fabrics and provide extra reinforcement for the hybrid com- voids between fiber bundles. This may account for the highest energy
posite laminates. This also facilitated stronger bonding of the Kevlar absorption capacity achieved in hybrid composite laminates infil-
fiber layers leading to strong structure with improved energy ab- trated with aluminum powder. SEM micrographs of the coating of
sorption capabilities during ballistic impact. Nano-fillers created a gamma alumina (Al2O3) powder on the Kevlar fabric (Fig. 12d) in-
sealing coating on the Kevlar surface as shown in Fig. 12. dicates a partial coating on the Kevlar fabric surface. Gama alumina
Fig. 12b shows a complete coating of the surface of the Kevlar is an excellent filler for plastics when mixed with resins. However,
fiber with nano-powders of colloidal silica (SiO2). The hard oxide impregnation of Kevlar fabric with alumina mixed with PEG did not
particles suspended in a liquid polymer (PEG-400) behave like non- produce a good adherence of the nanoparticle to the fibers, thereby
Newtonian fluid, whose viscosity increases when shear stress is contributing to the observed low ability of the laminates contain-
applied. The homogeneity of distribution of the silica nanoparticles ing alumina nanoparticles to withstand high velocity impacts.
on the fibers is highly dependent on the size of these particles. As The coating of silica carbide particles (SiC) on the Kevlar fabrics
a result, the concentrations of the solutes (SiO2) and solvents (PEG- is continuous as in the case of aluminum powder (Fig. 12e). Voids
400) have a direct influence on the efficiency of the impregnation within fiber bundles were completely sealed with the mixture of
of the fibers with the nano-powders and this was confirmed in an the particles and the solvent (PEG-400) and bonding of Kevlar layers
earlier study by Rao et al. [36]. SEM micrographs of Kevlar impreg- was enhanced leading to a good energy absorption capability. The
nated with aluminum powder mixed with PEG-400 showing coated micrographs in Fig. 12f suggests weak bonding between the potato
fiber with improved bonding capability with other fiber layer or alu- flour particles and the Kevlar fabric. Thus, a non-continuous coating
minum plate are presented in Fig. 12c. Aluminum powders in the of the nanoparticles on Kevlar fabrics was obtained. The low ad-

20 800
693 679
18 666
700
16
Energy absorbed (J)
Target thickness (mm)

553 543 600


14 507

12 10.8 10.6 500


11.8
9.7 9.5
10 8.1 400
8 300
6
200
4
2 100
Target thickness (mm) Energy absorbed (J)
0 0
Al/ K20 /Al Al/ K20 /Al Al/ K20 /Al Al/ K20 /Al Al/ K20 /Al Al/ K20 /Al
(Aluminum (Colloidal (Silica (Potato (Gamma (untreated)
powder) silica) carbide) flour) alumina)

Fig. 11. Relation between the absorbed energy and targets’ thickness.
20 E.E. Haro et al. / International Journal of Impact Engineering 96 (2016) 11–22

SEM micrographs taken on the longitudinal section of the per-


forations in the laminates provide information on the energy
absorption, deformation of various components of the laminates and
the sequence of impact damage (Fig. 13). The deformation of the
target is influenced by the projectile shape (nose), impact velocity
as well as the physical and mechanical properties of the hybrid com-
posite laminate. A terminal ballistic analysis was performed to
analyze the behavior of the projectiles upon impacting the various
laminates. This analysis was done on the longitudinal section of the
penetration channels produced by projectiles after ballistic impacts
(Fig. 13). The SEM micrographs provide indication of the mecha-
nism of failure and fracture of the laminates as they were perforated
by the sharp-nosed projectile. The damage in various components
of the laminates was inspected and evaluated from the SEM mi-
crographs. The damage sequence involved an initial indentation of
the face of the frontal aluminum plate produced by a localized stress
in the initial region of contact. These created a small puncture due
to pressure exerted by the projectile. In the initial phase of pene-
tration, a ductile crater enlargement can be observed (Fig. 13a).
Horizontal striations are produced by lands and groves that come
from the rifling process of the ogive. Fig. 13a shows the impres-
sion marks of the bullet as it travels through the barrel, suggesting
rotation of the bullet in the barrel. Also, vertical striations are
shown in the Fig. 13a that can be traced to the initial reaming of
the barrel.
On piercing the frontal aluminum plate, the projectile contin-
ued the perforation of the plates with breakage of fibers layers
adjacent to the frontal aluminum plate. The fibers are broken by
compression force exerted by the projectile, which created an en-
larged ductile crater as a result of shear plugging, and tensile fracture
of the first fiber yarn. As a result, Kevlar fibers are broken and ex-
pelled due to projectile penetration. The nature of the tensile failure
of the Kevlar fiber failure differed from one plate to the other de-
pending on the type of nanoparticle infiltrated into the Kevlar fabric.
For instance, the untreated Kevlar fibers (no nano-filler) suffered a
high yarn pullout, debonding, plastic deformation and fracture while
the fragmented fibers were expelled from the channel during the
penetration. On the other hand, the amount of the fiber pull-out
and delamination in the targets containing Kevlar infiltrated with
nano-fillers was less due to better fiber/Kevlar adhesion. As a result,
laminates containing nano-fillers exhibited more elongation and
better resistance to projectile penetration.
Delamination between Kevlar layers, and between aluminum
plates and Kevlar layers can be observed in Fig. 13. Such delami-
nation is an effect of the elastic wave propagation and force
distribution of the target plates where the fibers were working as
reinforcement. Shear forces increased and a dynamic friction between
layers also increases as a result of the projectile penetration. The
last layers participate in this process and the deformation in-
creased to absorb the impact energy at the maximum level. Fig. 13b
shows the back of aluminum plates after a complete projectile pen-
etration through the hybrid laminates. Radial cracking formed by
the projectile penetration leading to the formation of a sheeting of
open petals. The radial fracture produces wrinkles in each petal,
which end taking a form of a highly deformed tip. This shape
depends on the behavior in terms of energy absorption. The more
the energy absorbed by the target, the greater is the deformation
produced (Fig. 9b) on the rear face of the targets. The damage mode
Fig. 12. SEM image of Kevlar fibers impregnated with reinforced nano-powders. observed in the hybrid laminates produced in this study is similar
to that observed in carbon fiber reinforced plastic in previous studies
[37]. Yaghoubi and Liaw also observed similar pattern of delami-
nation during ballistic impact study on fiber metal laminates (FMLs)
herence of the particle to the Kevlar could be due to dissolution of plates made of aluminum plates and glass fiber fabrics [38]. Bal-
the potato powder in the PEG-400 during mixing. Thus, the potato listic impact testing of aluminum plates coated with polyurea also
flour could not effectively serve as filler. Hence the poor ballistic exhibited similar deformation mode showing petalling when sub-
impact resistance of hybrid targets containing potato flour. jected to ballistic impact [39].
E.E. Haro et al. / International Journal of Impact Engineering 96 (2016) 11–22 21

Fig. 13. Fracture surface along perforation in the target.

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