INVESTIGATION ON PARA-ARAMID FIBER

REINFORCED PEKK (POLY-ETHER KETONE KETONE)

HIGH-PERFORMANCE COMPOSITE

1Sombit Mandal, 1*Shantanu Bhowmik, 2M. Ramu

1Department of Aerospace Engineering, Amrita Vishwa Vidyapeetham, Coimbatore,
641112, India
2Department of Mechanical Engineering, Amrita Vishwa Vidyapeetham, Coimbatore,
641112, India

ABSTRACT
An experimental investigation is conducted to develop a high-performance composite by
reinforcing para-aramid fiber in Poly-Ether-Ketone-Ketone (PEKK) resin film. The bonding
between matrix and fiber is enhanced after surface modification. The surface of PEKK and
para-aramid fiber has been modified by low-pressure plasma to enhance the surface energy of
the polymeric film and reinforcement fiber. A contact angle test was carried out to analyse the
surface energy of the matrix and the fiber. The tensile strength of the composites is compared
between prior and post-plasma treatment. An accelerated aging test was carried out with the
composite. In this test, the tensile specimens are dipped into concentrated HNO 3 and NaOH
medium for 15 days. The ultimate tensile strength (UTS) of the virgin specimen was compared
to the environmentally aged that was dipped into the acidic and basic medium for 14 days. In
this investigation composite panel of 15mm×15mm dimension was developed and a bullet test
was carried out in the Ballistic Laboratory of National Forensic Sciences University (NFSU)
Gandhinagar, Gujrat, India. The composite panel was tested with four 9mm handgun bullets
fired from a distance of 5 meters with a speed of 430 m/s. The composite panel was able to
stop all the bullets. There’s no brittle failure as such, rather back facing signature could be seen
since it has essentially absorbed the impact energy of bullet.

Highlights:

 Film stacking method of PEKK and Aramid fiber.

 Ballistic composite panel with layers of PEKK and Aramid fiber.
 Enhancement of mechanical properties of the composite panel with plasma surface
treatment.
 Ballistic testing of composite panel.

1
Keywords

Film stacking method, aramid fiber, Poly-Ether-Ketone-Ketone, compression molding, plasma

surface modification, accelerated aging test, ballistic application.

*
Corresponding Author: b_shantanu@cb.amrita.edu

I. INTRODUCTION
A composite material is created by combining two substances with various physical and
chemical properties. As a result of their combination, a material with enhanced mechanical and
thermal properties is developed. From commonly used items like sports equipment, automobile
parts, and furniture to complex engineering structures like wind turbine blades and aerospace
components, composite materials are used in a wide range of products. Fiber-reinforced
composites (like carbon fiber reinforced polymer), particle-reinforced composites (like metal-
matrix composites), and structural composites are a few typical forms of composites (such as
sandwich panels). Depending on their reinforcement and matrix materials, the many types of
composites can be categorized. In this investigation, we have utilized polymer matrix
composite (PMC).

Composites have been utilized by individuals for hundreds of years. The first man-made
composites were created by Mesopotamians in Iraq about 3400 B.C. To make plywood in
ancient society, wood strips were bonded together at various angles. Following this, the
Egyptians began to create death faces out of cotton or papyrus that had been dipped in plaster
in approximately 2181 B.C. Later, both of these tribes began using straws to fortify their
building materials, mud bricks, ceramics, and watercraft [1].

Compared to conventional materials like metal, wood, and concrete, composite materials have
a wide range of benefits. A high strength-to-weight ratio index is one of the most important
benefits of a composite. Composite materials combine strength to create perfect products for
specific situations where lightweight structure is essential. They can weigh up to ten times less
than concrete and more than five times less than steel, respectively. Composites are not as
prone to corrosion as metals, which can cause rust and caused material degradation. They are
indeed excellent for use in extreme conditions. Composites can be made to match particular
applications and have custom stiffness, strength, and fatigue life. This enables improved

2
performance and more design freedom. Composites have excellent resistance to wear, impact,
and fatigue. They also require less maintenance and have a lengthy service life. Composites
are resistant to deformation and deterioration at high temperatures and during thermal cycling.
Composite is robust to a wide range of chemicals, making them perfect for usage in corrosive
situations such as chemical processing.

Composites are potential structure components for a multitude of applications, including

aerospace, automotive, construction, sports gear, and many more, since they offer a wide range
of advantages. Because of its excellent strength-to-weight ratio, resistance to corrosion, and
longevity. composites are widely employed in the aerospace industry. They are employed in
the production of wing, fuselage, and rear sections for aircraft. With the technological hurdles
posed by subtle and specialized materials like composite materials, there has been significant
advancement within material science and aerospace engineering. Composites are utilized to
create high-performance lightweight body framing and hoods. They aid in enhancing fuel
economy and lowering emissions. Composites are utilized to make construction supplies
including panels, tubes, and reinforcement bars. They are perfect for severe situations since
they can withstand corrosion, weathering, and fire.

ROLE OF PARA-ARAMID FIBER

A family of synthetic fibers called aramid fiber is renowned for its extreme strength, tenacity,
and heat resistance [2]. Aramid fibers are perfect for a wide range of applications thanks to a
unique mix of qualities. They are robust to distortion and can tolerate significant stress and
strain because of their high strength and modulus. Moreover, they exhibit good resilience to
fatigue, impact, and abrasion [3, 4].

Aramid fibers are renowned for their heat stability in addition to their mechanical qualities.
They withstand chemicals and ultraviolet radiation and can endure extreme heat without
melting or degrading [5]. Aramid fibers are employed in various products, such as body armor,
sporting goods, aerospace, and automobiles. The para-connected benzene amide makes a very
high internal rotation potential because the amide link created an n-conjugated shape with
phenyl groups [6]. The para-aramid fiber's molecular structure is a kind of quasi-crystalline
polymer cross-linked structure that resembles a stiff straight chain with a high degree of
orientation and crystallinity and regular chain segment arrangement. The para-aramid fiber
outperforms the meta-aramid fiber in terms of high-temperature tolerance and other qualities.

3
Since para-aramid fiber has a limiting oxygen index (LOI) of more than 28, it would not burn
after leaving the flame [7]. Figure 1 shows the chemical structure of aramid fiber.

Figure 1 Chemical structure of para-aramid fiber

ROLE OF POLY-ETHER-KETONE-KETONE

In this investigation, Poly-Ether-Ketone-Ketone (PEKK) has been used as matrix material

and aramid fiber (AF) as reinforcement material. The family of polyaryletherketone includes
the high-performance thermoplastic polymer known as PEKK. PEKK is a newly developing
polymeric substance. The PEKK bio-materials exhibit ultra-high efficacy among all
thermoplastic composites for great mechanical durability, resistance to chemicals, and high
thermal stability [8]. They have very good properties to absorb superior shock and resistance
to fracture[9, 10]. As a potential high-performance thermoplastic matrix solution for advanced
composites, a unique semicrystalline polyether ketone ketone (PEKK) polymer has been
developed. Table 1 shows the properties of PEKK. PEKK has an additional ketone group,
which raises the polarity and axis rigidity, raising the glass transition & melting temperature
[9]. Moreover, it has exceptional dimensional stability, minimal flammability, and great
chemical resistance. These characteristics make PEKK appropriate for high-performance
applications that call for strength, stiffness, corrosion, and wear resistance [11]. PEKK can be
processed using several methods like injection molding, extrusion, including 3D printing [12],
[13]. It is available in different forms like granules, powders, and films. To create composites
with even more strength and stiffness, PEKK is frequently combined with other substances like
carbon fibers or glass fibers [5, 6]. PEKK is utilized in the aerospace sector for ducting,
brackets, and structural sections of aircraft. It is utilized for surgical equipment and implanted
devices in the medical sector. It is utilized in the automotive sector for high-performance and
lightweight elements like body panels and engine components [14]. Besides being employed

4
in commercial settings, PEKK also has good chemical and heat resistance in fields like oil and
gas exploration [15]. Figure 2 shows the chemical structure of PEKK.

Table 1 Properties of PEKK

Properties Value

Density (g/cm3) 1.27

Glass transition temperature (℃) 160

Melting temperature (℃) 305

Tensile strength (MPa) 115

Figure 2 Chemical structure of PEKK

SURFACE MODIFICATION BY PLASMA TREATMENT

Surface modification can be done physically, chemically, or electrically. In this

investigation, the electrical process has opted for surface modification. Surface modification
with physical or chemical processes is complicated and difficult as compared to electrical
processes. In the physical process, a constant temperature should be maintained and in the
chemical process, some special chemical should be put on the surface of the material within a
certain time [16]. Plasma surface treatment is one such technique for treating surfaces, as it
provides a more stable and long-lasting surface energy augmentation than any other technique

5
[17]. Surface energy measures the breaking of intermolecular connections that take place when
a surface is formed. In the study of fiber-reinforced composite, surface energy plays a crucial
role. The bonding between the reinforced fiber and the matrix is proportional to the surface
energy [18]. Figure 3 shows the different contact angles of droplets on different surfaces.

Figure 3 Different contact angels of the surface

Based on this information, this investigation has been carried out to find out its application
essentially for ballistic since PEKK- para-aramid fiber composite has not been researched so
far. Therefore attention is given to testing the composite under 9mm handgun bullet with a
speed of 430m/s from a distance of 5m and the results are highlighted and established.

EXPERIMENT

FABRICATION AND DEVELOPMENT OF THE COMPOSITE:

PEKK films and Aramid fiber of dimensions 150mm×150mm×0.1mm and

150mm×150mm×0.5mm were cut respectively. The aramid fiber and the PEKK film were
stacked layer by layer. Kepton film has been used to prevent dislocating from the original shape
of the mold. Figure 4 shows the schematic diagram of stacked layers of polymer and fiber. The
composite was made under compression mold with a pressure of 2 bar with and elevated

6
temperature of 310℃. Figure shows how the temperature was monitored by infrared
thermometer during the compression molding process. Figure 5 shows the stacked layer of the
composite. After applying the pressure of 2 bar, 15 min of holding time was given. Table 2
shows the processing parameters of the compression molding machine. After cooling down,
the applied pressure was removed and the final product was bought out from the compression
molding machine.

Figure 4 schematic diagram of stacking

7
 Figure 5 Stacking of PEKK film & aramid fiber

Figure 6 Measurement of mold temperature

Table 2 Process parameters of compression molding machine

Temperature (℃) Pressure (bar) Holding time (min) No. of lyres

310 2 15 25

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Calculation of volume percentage:

Volume of a PEKK film = Thickness of the polymeric film × Length × Width

The volume of one film = 900mm3

Since,

The thickness of the composite panel is 5mm, the volume of fiber = volume of the composite
panel – volume of the polymeric film. So, the volume percentage of the polymeric film can be
derived from Eqn 1 which is 26.4% and the volume percentage of fiber is 73.6%.

𝑣𝑜𝑙𝑢𝑚𝑒 𝑜𝑓 𝑝𝑜𝑙𝑦𝑚𝑒𝑟𝑖𝑐 𝑓𝑖𝑙𝑚 (1)

× 100%
𝑣𝑜𝑙𝑢𝑚𝑒 𝑜𝑓 𝑡ℎ𝑒 𝑐𝑜𝑚𝑝𝑜𝑠𝑖𝑡𝑒 𝑝𝑎𝑛𝑒𝑙

Calculation of mass ratio:

For the ballistic test, 45 layers composite panel was used.

Mass of one PEKK film = 4.02g, then mass of 46 PEKK film = 184.92g

Again,

Mass of one aramid fiber =8.31g, Then mass 45 aramid fiber = 373.95g

The calculated mass of the composite panel is 558.87g

THERMOGRAVIMATRIC ANALYSIS:

Thermogravimetric Analysis, or TGA, is a procedure for analyzing a material's thermal

characteristics [19]. It entails measuring a sample's weight changes while exposing it to
controlled temperature variations. TGA is frequently used in several disciplines, including
chemistry, polymers, medicines, and materials development. TGA characterization technique
was done for the composite by SDT Q600 V20.9. The purpose was to study about the
decomposition temperature of polymer and fiber in the composite.

CONTACT ANGLE MEASUREMENT:

A surface with low surface energy will usually have poor wetting, which will lead to a high
contact angle. This is because there is no energy benefit for liquids to break down bulk bonds

9
in favor of interacting with the surface. After all, the surface cannot create strong bonds.
Hydrocarbons are an example with low surface energy because they are kept together by mild
Van der Waals forces [20]. In this experiment, plasma surface modification has been done with
a plasma-based sputtering machine. Surface modification has been done for both fiber and
polymeric film. The motive of the surface modification is to attach some polar molecule to the
target substance like the OH group [18].

TENSILE TEST:

The most important technique for assessing the mechanical performance and characteristics of
composites is tensile testing. It includes applying tension to a composite material until it fails,
allowing for the assessment of important characteristics like strength, elasticity, etc. It helps
in the choice of materials, quality assurance, design, investigation, and failure evaluation. The
fabricated composite panels were machined to standard dimensions for testing using waterjet
cutting. The effect of plasma treatment on the mechanical properties of the composites was
characterized by the measurement of tensile strength. The tensile strengths of the fabricated
tensile specimens of the composite was measured using a Universal Tensile Testing machine
(Zwick Roell Z010) based on the ASTM D3039—Standard Test method for tensile properties
of Polymer Matrix Composite Materials.

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 II. RESULTS AND DISCUSSION

THERMO-GRAVOMATRIC ANALYSYS TEST:

Figure 5 TGA test result of the composite

Figure 5 shows the thermogravimetric analysis test result. This figure represents the curve
weight loss vs. temperature and derivative weight vs. temperature. 2.106 g of the sample was
taken in a TGA holder and heated at a rate of 10 °C min-1 from room temperature to 700 °C.
Table 4 shows the process parameters of the TGA test.

Table 3 Process parameters of the TGA test

Material of Gas Gas flow Temperature Initial Final Initial

pan rate increasing temp(oc) temparature mass
(ml/min) velocity (ºC (ºC) (mg)
/min)
Aluminium Nitrogen 200 10 37 700 2.106

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CONTACT ANGLE MEASUREMENT:

(a)

(b)
Figure 8 Contact angle of (a) without modified surface and (b) Plasma surface modified.

From the figure 8(a) and figure 8(b) it can be seen that the plasma modified surface is attracting
the water molecule more than without modified surface. As a result, the contact angle between

12
surface and water molecule of plasma modified surface is 46° and the contact angle between
surface and without modified surface is 78°.

TENSILE TESTING:

(a)

(b)
Figure 9 Stress-strain curve for (a) untreated specimen and (b) surface treated specimen

13
 700

600
Ultimate tensile strength(MPa)

500

400

300

200

100

0
Without surface treatment Plasma surface treatment

Figure 10: Comparison between surface untreated and treated specimen

Two tensile specimens were fabricated according to ASTM D039 from the composite panels.
The ultimate tensile strength (UTS) of untreated specimens determined by this stress-strain
relationship is 395 MPa. After surface modification, the test demonstrated that the ultimate
tensile strength (UTS) was enhanced by 553 MPa as the intermolecular interaction between the
matrix and fiber had increased. The ultimate tensile strength (UTS) has risen from the untreated
specimen by 1.4 times once surface treatment is complete. Figure 9(a) displays the stress-strain
curve derived from the tensile test. Figure 9(b) displays the stress-strain curve of the plasma
surface treated specimen. Figure 10 shows the comparison of ultimate tensile strength between
surface-treated and surface-untreated specimens.

14
ACCELARETED AGING TEST:

500

450

400
Ultimate tesile strength(MPa)

350

300

250

200

150

100

50

0
Virgin Dipped into basic medium Dipped into acidic medium

Figure 11: Comparison of Ultimate tensile strength under aggressive environmental exposure

In this test, materials were exposed to a very aggressive medium for extended duration.
After the exposure specimens were tested for the mechanical properties of the material. In this
case, two specimens were taken and immersed into a concentrated acidic medium and a strong
basic medium for 15 days. 390 MPa of Ultimate tensile strength is observed for the specimen
which was immersed in the alkali medium. Sodium hydroxide a PH of 12 was used for the
strong basic medium and 68% concentrated nitric acid of PH of 1.2 was used for the acidic
medium. 247 MPa UTS were obtained for the specimen which was submerged in a strong
acidic medium. Figure 11 demonstrates the comparison between ultimate tensile strength under
various aggressive environmental exposures. From these results, it can be concluded that the
composite can sustain in a very aggressive atmosphere without degrading.

15
BALLISTIC TEST RESULT:

(a)

(b)
Figure 12: Result after ballistic test (a) composite panel of 25 layers and (b) composite panel
of 45 layers after the bullet test

The ballistic test was conducted twice in line with NIJ level 3A standards. The test was
carried out at National Forensic Science University (NFSU), Gandhinagar, Gujrat. The first

16
trail was conducted with an untreated composite panel of 25 layers and the second was
conducted with an untreated composite panel of 45 layers. The ballistic tests were carried out
with 9mm handgun bullet with a speed of 430m/s at a distance of 5 meters. Figure 12(a) shows
the condition of the composite of 25 layers after the test and figure 12(b) shows the condition
of 45 layers of composite after the ballistic test.

Table 4 BFS of the hit bullets

1st shot 21.75 mm

2nd shot 26.35 mm

3rd shot 19.53 mm

4th shot 20.02 mm

DISCUSSION
In TGA test results for FRP materials like GFRP or CFRP will show two weight loss curves
[21]. In this TGA test, two-step degradation is shown for the composite. From the result, it is
observed that the sample of the composite starts to degrade at 290ºC on the first step of weight
loss. Now in the second step of degradation of the curve, which is sowing the sample starts to
degrade at 510ºC. It indicates that degradation of the fiber started at 510ºC. In this test result,
the derivative weight curve (weight%/ºC) cab shown with the blue line in the graph. The peak
indicates the maximum weight loss at the temperature of 589.09ºC. From this data plot, we can
justify that the melting point of the reinforced fiber is greater than the matrix of the composite.
For fabricating the fiber-reinforced composite, the melting point of the fiber should be higher
than the matrix. If it is not then the fiber will melt before melting the matrix and the composite
can not be fabricated.

The polar and dispersive elements of surface energies of all of the compounds were assessed
through measurements of their contact angles by the sessile drop method using two test liquids,
deionized water and formamide, of known bipolar and dispersive aspects of surface energy
[22]. In this particular case, a contact angle goniometer was used to evaluate the surface energy
of the specimen after plasma modification. In this test, the modified surface of the polymeric
film and fiber was kept on a plane surface, and one tiny droplet of distilled water was put on
the targeted surface. Then the contact angle between the modified and unmodified surfaces was
17
compared. It can be seen, that the changed surface's contact angle is significantly lower than it
would be. As we know one oxygen atom and two hydrogen atoms compose a water molecule.
In comparison to hydrogen, the oxygen atom is more electronegative [23]. As a consequence
of this, oxygen pulls the remaining electrons[18,24]. Therefore, the hydrogen atom will create
a positive pole at one side and the oxygen atom will create a negative pole on the other side
[25]. The difference in contact angle between surfaces with and without surface modification
is shown in Figures 8(a) and 8(b). The polymeric film and fiber surface formed an organic
oxide layer following plasma treatment, which resulted in an increase in hydrophilic functional
groups and decreased the water contact angle.

Among the mechanical tests that were conducted, the tensile test was one of the standard tests
that was used to measure the tensile strength of the composite. After testing various samples,
one can able to draw the conclusion that the ultimate tensile strength of the surface-treated
composite increases while maintaining the same volume ratio of matrix and fiber, which in turn
indicates the load capacity increases. The tensile strength increases because of the strong
molecular bond between matrix and fiber. For ballistic applications, the bonding between the
matrix and the fiber for the surface untreated composite is a blessing. No surface treatment is
needed for the ballistic application with this combination of the composite. On the other hand,
the surface-treated composite can be used for the structural application.

In the ballistic trial of the composite of 25 layers, the composite panel was unable to absorb the
energy of the bullet. The 12mm thick composite was pierced and perforated by the bullet. Again
a ballistic test was carried out on a 20mm thick composite panel of 45 layers with a standard
procedure with a firing distance of 5m. This time, four bullets penetrated the composite panel,
but it was unable to pierce it instead, a bulge known as the back-facing signature (BFS) was
created. Table 5 displays the BFS for each shot made by bullets. After the bullet strikes on the
composite, the panel successfully absorbed the bullet impact within the composite. Moreover,
there was no propagation of crack and it was essentially a ductile fracture. A total of four bullet
shots were taken and all the kinetic energy of four bullets was absorbed by the composite panel.
This occurred because of toughness of the composite. Due to the high toughness of the fiber,
the composite panel is able to absorb the kinetic energy of the bullets. This is the reason behind
sustaining even after such a high impact.

The process of making Para-aramid/PEKK using the stacking method is quite a challenging
process. Since the composite panels are handmade in normal room conditions, the accuracy of

18
orientation is compromised. This may lead to errors in the results. That’s why, great care has
been taken to keep the magnitude of error very low. In this experiment, a knife has been used
for cutting the reinforcement fiber. It is quite challenging to maintain the dimensions of the
fiber mat. By using advanced autoclave and labs, the composite panels can be fabricated with
minimum error hence resulting in enchantment of its mechanical properties.

NOVELTY:

Although there is lots of use of Aramid fiber in ballistic applications, there has never been a
case of application of PEKK is reinforced with Aramid fiber. In this investigation, the high
toughness has been achieved by compression of the stacking layer of the film and the fiber.
With a huge toughness between two layers, it has essentially dissipated high impact force of a
bullet. The dissipation of kinetic energy of a bullet through layers of polymeric film and fiber
and high toughness are the main reasons for the bullets to be stopped. There is no brittle failure
rather there is a ductile failure. A certain amount of back facing signature has been observed
which is according to the standard. That is the real novelty of this investigation.

19
 III. CONCLUSION

The conclusion allows you to make a final judgment on the topics discussed in this paper,
summarise your ideas, and highlight how important the concepts are. In this chapter, the final
results of the project we obtained are discussed. The final results are concluded below. After
doing the plasma surface modification the surface energy will enhance for both fiber and
polymeric film. That is the reason the bonding between polymeric film PEKK and aramid fiber
is stronger than the unmodified composite and the ultimate tensile strength of the modified
composite is 1.4 times greater than the unmodified composite. A composite has been developed
in this project which can be used in ballistic and structural applications both. The composite
has tested in a very aggressive medium which we discussed before. From that test, we can
conclude that the composite can be used for a long time without degrading. A 150mm×150mm
composite panel has been made and tested all correct for ballistic application.

Nomenclature:

ASTM American Society for Testing and Materials

UTS Ultimate tensile strength

PEKK Poly Ether Ketone Ketone

AF Aramid Fiber

BFS Back Facing Signature

NIJ National Institute of Justice

GFRP Glass Fiber Reinforced Polymer

CFRP Carbon Fiber Reinforced Polymer

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