Investigation on the Mechanical Behavior Impact of Plasma Treated Propylene in

Carbon Fiber Composites

1
M. Senniangari, 2K.Navienkumar, 3V.S.Sanjay, 4S.Arunkumar,5A.Sanjeev
1
Assistant Professor, 2,3,4,5UG Students - Final Year, Department of Mechanical
Engineering, Nandha Engineering College, Perundurai 638 052, Tamil Nadu, India
Abstract

Improved mechanical characteristics for composites using a linear low-density

propylene (PP) matrix and a carbon fibre (CF) filler were the focus of this study. The
material was fabricated by a hand layup process in an oven. Oxygen plasma treatment of
the PP matrix enhanced adherence. Before being filtered and dried for manufacture, CF
and PP were first combined with standard stirring, ultrasonication, and mechanical
stirring. The highest tensile strength was achieved in plasma-treated propylene (PPP)
with 10 wt. percent CF, with overall property performance increasing by 13.46 percent
comparison to non-PP with the same CF addition. Tensile strength was reduced from
19.4 MPa to 18.3 MPa when carbon fibers were added at 14 and 16 wt. percent. As a
result of CF aggregation with plasma-treated and untreated PP, tensile strength (TS) was
reduced.Better tensile qualities were seen in a factory setting with temperatures of 180°C
for 20 minutes.After plasma treatment, the PP/8% CF blend had a flexural strength (FS)
of 26.19 MPa, which was higher than that of untreated PP by a significant margin.
Keywords: propylene; carbon fiber; mechanical properties; plasma treatment.
1. Introduction
Thin films, adhesives, medical implants, electronics, batteries, and orthopedics are
just some of the many uses for propylene, which is why it is one of the most useful
polymers. For commercial use, rotomolding is the typical method of production. Fillers
and reinforcements are added to the propylene (PP) matrices to increase their usefulness
in a variety of contexts. The bond strength between fibres and the matrix is a major factor
in how well composites perform mechanically. Increased compatibility between fibres
and matrix is one of these benefits, and plasma treatment of propylene matrices is one
way to achieve it. By applying a plasma to composites, the surface roughness and
hardness can be increased.Better bonding is achieved via plasma treatment with oxygen
when two polarity-opposed matrices, such as propylene and polyamide (PA), are
sandwiched together. The 7.689 N/mm peel strength is more than twice as high as that of
untreated samples. PP samples delaminated without intervention. The flexural strength of
PP and PP treated with plasma was 35.40 MPa, which is higher than the flexural strength
of an untreated mixture (31.80 MPa) [8]. Improved tensile, flexural, and impact
properties were observed in PP that had been treated with plasma, and the material's
inherent reinforcements were not compromised in the process.Adherence of composites
is improved by the treated PP's functional groups reacting with the hydroxyl groups in
the lignocellulosic coir fibres [9].. Tensile strength was greatest in 10% glass fibre (GF)
reinforced plasma polypropylene (PP) composites. We found that plasma-treated PP with
20% GF had the highest tensile modulus [10].

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 Carbon fiber is a very desirable material for use in a wide variety of industries,
including the automotive, sporting, and aviation sectors owing to its exceptional
corrosive resistance, mechanical characteristics, and outstanding coefficient of thermal
expansion. Composites made from polypropylene (PP) and high-density propylene
(HDPP) have improved impact, tensile, and flexural characteristics by 60%, 18%, and
23%, respectively, when up to 20% carbon fibre was added [13]. When the fiber-to-resin
ratio increases, the mechanical characteristics of the composites suffer because of a
phenomenon called agglomeration. Using 80% by weight carbon fiber led to a
maximalFS of 65.21 MPa and enhanced hardness equated to further epoxy resin
mixtures. The TS and tensile modulus (TM) of HDPP were enhanced when carbon fibres
were introduced at a concentration of up to 25 weight percent. The TS and TM of
CF/high-density polypropylene (HDPP) composite were improved by spraying 2%
weight percent carbon nanotubes (CNTs) over the materials. Recycled carbon fibers can
be used in cars and other industrial uses much like fresh carbon fibers, but at a far lower
price. But they don't have the mechanical properties of polymer matrices.
Carbon fibres' tensile characteristics were marginally improved after treatment with
oxygen plasma at 80 W. Shear strength at the interface increased to 72 MPa after being
treated with 20 W of plasma [19]. Epoxy-based matrix polymers with shape memory
enhanced mechanical capabilities when combined with continuous and short carbon
fibres. Carbon strengthened materials likeCF, single- and multi-wall CNT, and carbon
black (CB) have found usage in electrical conductivity applications with a wide range of
thermo- and thermo-setting polymers. Composites produced from propylene showed a
decrease in mechanical properties when carbon black and carbon nanotube fillers were
added. Plasma treatment of a composite comprising polycarbonate, carbon fiber, and
CNT improved the composite's dynamical mechanical characteristics. Surface roughness
was enhanced and mechanical interlocking between CF and PEEK was achieved using
radiofrequency plasma treatment with air, argon, or a mixture of the two gases. The
interfacial strength of the PEEK composites improved as a result. Surface-energy-rich
materials including glass/PP, pure polypropylene, and HDPP composites have their
interfaceconnection improved with the use of oxygen plasma.
According to the research, plasma therapy is a viable method for enhancing matrix-
fiber phase interaction. Recycled carbon fibre has similar mechanical capabilities to
normal carbon fibre without the high price tag. It is also better for the environment. In
order to make recycled carbon fibres commercially viable, more research is needed in this
area. The flexural strength, flexural modulus, tensile strength, tensile modulus, and
morphological properties of plasma-treated propylene and carbon fibres have not been
investigated in any published work. In this research, FTIR and XPS measurements were
used to determine how plasma therapy affected PP. The optimum settings for oven
processing were determined by applying various fabrication circumstances. As a last step
of verification, plasma treatment was applied to carbon fibres.

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2. Materials and Methods
2.1. Materials
The matrix material was supplied from Dow Corporate and consisted of a hexane-
based linear low-density propylene (PP) polymer powder designated as DowlexTM
2629.10UE. The density is 0.9370 g/cm3 (ASTM D792) Index of Melt Flow
Density:3.80 Density in Larger Quantities = 0.352 g/cm3. To make chemical barrels and
other bulk and freezer containers [3]. Propylene and carbon fibres were treated with
plasma but not pretreated. Surface treatment with plasma was given to propylene powder
(PPP) using an industrial-use apparatus (LA 400) (a. s. Turnov, Czech Republic). Two
microwaves, with a combined 2 kW of power, were used to apply the plasma. Treatment
with oxygen plasma was performed for 30 seconds at a gas flow rate of 100 sccm. As was
the case previously [3,] we applied the plasma treatment approach.
The PP matrix was filled with recycled carbon fibres that were made from PAN
fibres that were 99 percent pure and ranged in size from 80 to 350 µm. MSV
STUDENKA sro of Bilovec, Czech Republic, was the supplier of the recycled carbon
fibres. The fibres measured 8 mm in length, 7 µm in diameter, 1.8 g/cm3 in density, and
250-550 g/L in bulk volume. These fibers are useful in a wide variety of contexts because
of their many desirable features, including as higher strength and elasticity, minimal
density, heat, abrasion, corrosion, electricity, and electrical conduction. Industrial
equipment (LA 400) used a 100 sccm oxygen flow to cure the carbon fibres.
2.2. Fabrication
Using the hand layup method, composites made of carbon fibre and linear low-
density propylene (PP) were created. Carbon fibre (CF) was added to the polypropylene
(PP) matrix at 4, 6, 8, 10, 14, and 16 weight percent for reinforcement. Before anything
else, carbon fibres were mixed with isopropyl alcohol (IPA). Ultrasonication (at 50 °C,
40 kHz for 60 minutes) was used to combine the PP matrix, IPA, and carbon fibre, and
then mechanical stirring was used to distribute the mixture (for 10 min). After removing
the isopropyl alcohol by filtering the mixture through filter paper, it was dried in a hot
oven with ambient air. To lessen the amount of leftover mixture, the dried powders were
sifted before being pressed into 100 x 25 x 3 mm3 silicon molds. The samples were rolled
using a roller, then dried in an oven at 180°C for 20 minutes before being chilled to room
temperature. Both the PP and CF plasma treatments followed the same protocols. The
optimal conditions for fabrication were determined by testing temperatures between 180
and 200°C and times ranging from 20-60 minutes. Plasma-treated polypropylene
improved matrix/fiber adhesion.
2.3. Method of testing
ISO 527 tensile testing was done using a UTM set at a 6 cm gauge length and a
speediness of 6 mm/min. The results of all mechanical tests were averaged among ten
different samples. A three-point bending test was conducted at a speediness of 2 mm/min
using the same ASTM D 790 standard equipment to assess flexural properties. After
subjecting the material to tensile testing, the distribution and adhesion of carbon fibres
within the PE matrix were examined using scanning electron microscopy [JSM-7600F
(JEOL, JP)].

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 The chromium layer was sputtered off so that the electron beams could penetrate
the material without causing any charge. The working voltage ranged from 1 to 5 kV, and
the working distance was measured from 5.4 to 10 mm.
3. Results
3.1. Tensile Testing

Figure 1. TS of Carbon Fiber/PP composites.

As anoutcome of plasma treatment, the tensile strength of carbon fibre
(CF)/polypropylene (PP) composites was significantly improved (Fig 1). The first
combination of plasma treatment without carbon fibre yielded less spectacular tensile
results (2.94 percent). Two types of PP, plasma-treated (PPP) and untreated (PP), are
shown in Figure 1. Plasma-treated PP (denoted as 4P) and untreated PP (denoted as 4N)
both have a CF of 4%. Like 6P and 6N, 8P and 8N, 10P and 10N refer to CF
concentrations of 6, 8, and 10 weight percent in plasma- and non-plasma-treated
polypropylene. Similar rules apply to the other permutations (14P, 14N, 16P, and
16N)treated with oxygen plasma has been demonstrated to have improved wettability,
leading to better matrix adhesion with fillers.
The fundamental mechanism of the oxygen plasma therapy was etching, which also
stimulated the surface. This indicates that polymer powder wettability can be improved
without introducing oxygen groups. The creation of polar groups was made possible by
the plasma and was made possible by the brief duration of the plasma treatment.
Additional abrasion was created on the PP composites through prolonged exposure,
making their surfaces rougher. Improved adherence and application were achieved
through oxygen plasma treatment of the polymers.The highest tensile strength was
attained at 22.6 MPa with 10 wt. percent CF, while improvements in characteristics
reached as high as 13.46 percent in comparison to non-plasma PP with the similar
quantity of Carbon fiber. The tensile strength properties dropped from 19.4 MPa to 18.3
MPa when carbon fibres were added at 14 and 16 wt. percent. Agglomeration of CF with
plasma-treated and untreated PP led to decreased tensile strength. No additional increase
in tensile strength of the PP composites was seen after including plasma-treated CF with
plasma PP (Figure 2). With the addition of 6, 8, and 10 wt. percent CF, the tensile
strength dropped to 21.6 MPa, 21.7 MPa, and 21.9 MPa, respectively, after plasma
treatment of CF.

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 Figure 2. Comparison of tensile strength of plasma and non-plasma
composites
Fig 3 is a normal probability plot values of TS measurements for 4, 6, 10, and 16
weight percent carbon fiber with plasma PP, all of which are within the allowable range.
In terms of tensile strength, the combination of CF and PP with 10 weight percent CF and
plasma treatment yielded the best results, with a value of 21.8 MPa. Several iterations of
composite combinations were tried, each with a unique set of fabrication parameters
(Figure 4). The first round of tests was run at 180 degrees Celsius for 20 minutes (or "T
180 20"). A similar range of temperatures and times was used for the T180 40, T180 60,
T200 20, T200 40, and T200 60 fabrication circumstances. There was a decline in
characteristics across the board for all fabrication circumstances except T180 20.
Probability Plot of 4 CF/ Plasma PP Composites Probability Plot of 6 CF/ Plasma PP Composites
Normal - 95% CI Normal - 95% CI
99 99
95 95
Mean 19.92 Mean 20.84
90 90
StDev 0.9052 StDev 0.8151
N 10 N 10
80 80 AD 0.278
AD 0.561
P-Value 0.109 P-Value 0.567
70 70

60 60
Percent
Percent

50 50

40 40

30 30

20 20

10 10
5 5
1 1
16 17 18 19 20 21 22 23 24 18 19 20 21 22 23 24
Tensile Strength (MPa) Tensile Strength (MPa)

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 Probability Plot of 16 CF/ Plasma PP Composites
Probability Plot of 10 CF/ Plasma PP Composites
Normal - 95% CI
Normal - 95% CI
99
99 95
95 Mean 27.73
Mean 21.5 90
90 StDev 0.7573
StDev 0.4163
N 10
N 10 80 AD 0.338
80 AD 0.345
P-Value 0.424
P-Value 0.406 70
70

60 60

Percent
Percent

50 50

40 40

30 30

20 20

10 10
5 5
1 1
20.0 20.5 21.0 21.5 22.0 22.5 23.0 15 16 17 18 19 20 21
Tensile Strength (MPa) Tensile Strength (MPa)

Figure 3. Normal probability plot for TS: (a) 4% Carbon Fiber/plasma PP, (b)
6% Carbon Fiber /plasma PP, (c) 10% Carbon Fiber /plasma PP and (d) 16%
Carbon Fiber /plasma PP combinations.

Figure 4. TS of 10 weight% CF/plasma PP under Various Fabrication

Circumstances

Figure 5. Comparison of Tensile modulus of CF/PP composites

Figure 5 displays the dramatic increase in tensile modulus characteristics of the
Carbon Fiber/PP composite after plasma treatment of the propylene and carbon fibre

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insertion. Tensile modulus values of 488, 551.1, 626.2, and 679.8 MPa were attained by
incorporating carbon fibres into plasma-treated PP at 4, 6, 8, and 10 wt. percent,
respectively. Incorporating the same amount of carbon fibre into non-plasma-treated PP
resulted in improved characteristics. At 10 weight percent Carbon Fiber with plasma PP,
both the TS and TM improved.TM characteristics were shown to decrease with
increasing CF content between 14 and 16 wt.

3.2. Flexural Testing

Figure 6. Comparison of Flexural strength of Carbon Fiber/PP composites

Fig 6 demonstrates that similar to the tensile characteristics, the FS of CF/PP

composite rises with PPP and CF insertion.FS was somewhat increased from the starting
combination's 18.53-19.2 MPa after plasma treatment to PP.The flexural characteristics
of a composite made from plasma propylene powder and 4 weight percent carbon fibres
were improved from 19.47 MPa to 20.45 MPa. With plasma-treated PP incorporating
carbon fibres at 6, 8, and 10 wt. percent, similar improvements in flexural characteristics
were reported. The combination of plasma-treated polypropylene and eight percent
carbon fibre reached a maximum flexural strength of 26.19 MPa.
Flexural characteristics at 25.54 MPa were nearly identical in PP treated with 10
wt. percent CF/plasma. Flexural strength for 14 and 16 wt. % CF with plasma-treated PP
was lowered to 25.98 and 24.2 MPa. Polar groups including hydroxyl, carbonyl, and
carboxyl were found to be present when oxygen was treated with plasma. Functional
groups can be added to or interlocked with the surface of polymers by inducing the
production of polymer chains containing free radicals, as observed in the presence of
these polar groups. This would have improved the composites' adhesion, which in turn
would have helped activate the polymer surface. The flexural characteristics of the
polymer composites were diminished due to the agglomeration of carbon fibres.
Incorporating plasma-treated PP into 14 and 16 wt. % CF improved the characteristics
compared to adding the same amount of carbon fibre to untreated PP. The results of
adding 6, 8, and 10% CF to plasma-treated PP-based composites showed no significant
increase in FS(Figure 7). The flexural propertiesof plasma-treated 6, 8, and 10 wt. percent
CF/plasma PP were reduced from 24.5 to 23.8 MPa, 27.29 to 26.3 MPa, and 26.64 to
26.08 MPa, respectively, when equated to the similarcarbon Fiber combination without
plasma/PPP. When the filler and matrix stopped interacting so strongly, the combination's
FS dropped. Flexural strength in 4, 6, 10, and 16 wt. percent carbon fiber with plasma PP

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all fall within the acceptable range of fluctuation, as indicated in Fig 8's normal
probability plot. The PP matrix's enhanced mechanical characteristics were the result.
Increased adhesive in the fiber phase with reduced void after plasma treatment in PP is
seen in images as well, improving the polymer composites' tensile and flexural
capabilities.

Figure 7. FS of Carbon Fibers/plasma PP composites

Probability Plot of 4 CF/ Plasma PP Composites Probability Plot of 6 CF/ Plasma PP Composites
Normal - 95% CI Normal - 95% CI
99 99
95 95
Mean 19.21 Mean 23.40
90 90
StDev 0.8215 StDev 1.049
N 10 N 10
80 AD 0.283 80 AD 0.561
P-Value 0.55 P-Value 0.109
70 70

60 60
Percent

Percent

50 50

40 40

30 30

20 20

10 10
5 5
1 1
16 17 18 19 20 21 22 19 20 21 22 23 24 25 26 27 28
Flexural Strength (MPa) Flexural Strength (MPa)

Probability Plot of 16 CF/ Plasma PP Composites

Probability Plot of 10 CF/ Plasma PP Composites Normal - 95% CI
Normal - 95% CI 99
99 95
95 Mean 23.14
Mean 25.54 90
90 StDev 0.7135
StDev 0.9131 N 10
N 10 80 AD 0.506
80 AD 0.432
P-Value 0.152
P-Value 0.242 70
70
60
60
Percent
Percent

50
50

40 40

30 30

20 20

10 10
5 5
1 1
22 23 24 25 26 27 28 29 20 21 22 23 24 25 26
Flexural Strength (MPa) Flexural Strength (MPa)

Figure 8. Normal probability plot for FS: (a) 4% Carbon Fiber/plasma PP, (b)
6%CarbFiber /plasma PP, (c) 10% Carbon Fiber /plasma PP and (d) 16% Carbon Fiber
/plasma PP combinations.

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 Figure 9. Flexural modulus of CF/PP composites

Figure 10. FTIR spectrum analysis of untreated and plasma-treated polypropylene

(PP) samples
Fig.9 shows that the CF-based composites' flexural modulus tends to improve after
plasma treatment of the PP. With the same amount of carbon fibre added to either the
pure PP matrix or plasma-treated PP, it is evident that the qualities associated with the
flexural modulus of the latter improved. Mechanical characteristics were also
significantly improved in PP composites thanks to the CF filler. Eight weight percent
CF/plasma PP showed the highest flexural modulus characteristics, at 816.1 MPa. Neither
the treated nor the untreated PP samples underwent any modifications to their functional
groups, as shown by the FTIR study (Figure 10). The extending vibration of Carbon-
Hydrogen asymmetric and Carbon-Hydrogen symmetric groups account for the peaks at
2965cm1 and 2847 cm-1 for both PP samples. C-H groupdeformation vibration also
contributed to the peak at 1508 cm-1 [6]. From the XPS analysis clearly demonstrates
that the concentration of O-C=O groups in the PP that was treated with plasma for 30
seconds is significantly lower than predicted. In the yellow line represents an Oxygen-
Carbon=Oxygen bond, the orange line a Carbon-Carbon bond, and the maroon and pink
lines, respectively, C=O and C-O bonds. The percentage of C-O groups was 2.2%, while
the percentage of C=O groups was just 0.6%. We recently reported [27] that functional

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 groups in plasma-treated PE were equivalent to those in untreated PP. During plasma
treatment of PP, a single O2 atom bonds chemically with the polymer surface, resulting
in -OH groups and functional groups with richer O2 [3].
4. Water absorption Testing

Fig.7.11 Water Absorption Test Machine

Water-absorption test a test to determine the moisture content of soil as a percentage of

its dry weight (British Standard 1377, 1967). The sample is weighed, dried in an oven, and
then reweighed under standard conditions. Water absorption gives an idea of strength of
aggregate. Aggregates having more water absorption are more porous in nature and are
generally considered unsuitable unless they are found to be acceptable based on strength,
impact and hardness tests. Water absorption is defined as the amount of water absorbed by a
material and is calculated as the ratio of the weight of water absorbed to the weight of the dry
material. The amount of water is determined by subtracting the dry weight from the initial
weight, and the moisture content is then calculated as the amount of water divided by the dry
weight or total weight, depending on the reporting method. Even this simple loss-on-drying
method is mined with potential variability traps.
 Sample preparation: Cut the composite material into specimens of a standardized size
and shape. The specimens should be representative of the material and its intended
application.
 Initial weighing: Weigh each dry specimen using a precise balance and record their
initial weights (Wi).
 Immersion: Submerge the specimens in a container filled with the liquid environment of
interest, such as water or a specific solution. Ensure that the specimens are fully
immersed and free from air bubbles.
 Time intervals: Define specific time intervals for measurements based on the test
duration requirements. Common intervals include 24 hours, 48 hours, 7 days, and so on.
 Removal and drying: After each time interval, carefully remove the specimens from the
liquid environment, and gently blot or wipe them to remove any excess surface
moisture.

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 Weighing after absorption: Weigh the wet specimens (Wf) immediately after removing
excess moisture.
Conclusions
 Mechanical qualities, such as tensile and flexural strength, were enhanced
when plasma-treated PP and CF were incorporated into CF/propylene (PP)
composites.
 A greater TS of 22.6 MPa and an increase in characteristics up to 13.46
percent were achieved with 10 wt. percent CF related to non-plasma PP
with the similar carbon fiber addings.
 With the accumulation of CF at 14 and 16 wt. percent, the TS dropped from
19.4 MPa to 18.3 MPa. Carbon fiber aggregation with both plasma-treated
and untreated polypropylene led to a decrease in tensile strength.
 When equated to other fabrication conditions, the tensile properties were
best under an oven temperature of 180°C for 20 minutes.
 Analyzing tensile test results with a scanning electron microscope (SEM)
demonstrated enhanced adhesion of carbon fiber filler with plasma
polypropylene (PP), with less surface deformations.
 Tensile modulus values of 488 MPa, 551.1 MPa, 626.2 MPa, and 679.8
MPa were attained by incorporating carbon fibres into plasma-treated PP at
4, 6, 8, and 10 wt. percent, respectively. These numbers were better than
those seen for similar quantities of carbon fibre added to PP that hadn't been
plasma treated.
 Tensile modulus, including tensile strength, improved at 10 wight percent
carbon fiber with plasma PP.
 The flexural characteristics of a composite made from plasma propylene
powder and 4 weight percent carbon fibres were improved from 19.47 MPa
to 20.45 MPa. Flexural characteristics were similarly improved in plasma-
treated PP containing carbon fibres at 6, 8, and 10 wt. percent.

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  The combination of plasma-treated polypropylene and eight percent carbon
fibre reached a highestFS of 26.19 MPa. The FS of 25.54 MPa was nearly
equal after adding 10 wt. % CF/plasma-treated PP.
 After combining CF with plasma PP, the flexural strength of 14 and 16
weight percent decreased to 25.98 MPa and 24.2 MPa.
 The greatest flexural modulus value of 816.1 MPa was achieved with a
CF/plasma PP composition containing 8 wt. percent CF.
 Tensile and flexural characteristics of propylene composites were not
improved by oxygen-carbon fiber plasma treatment.
 These mixtures have limited car industry use. The electrical conductivity
properties can be examined in further studies
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