Article

Evaluation of Mechanical, Thermal, and Tribological Properties

of 3D-Printed Nylon (PA6) Hybrid Composites Reinforced with
MWCNTs and Carbon Fibers
Palaiam Siddikali and P. S. Rama Sreekanth *

School of Mechanical Engineering, VIT-AP University, Amaravati AP 522337, Inavolu, India

* Correspondence: happyshrikanth@gmail.com

Abstract: Three-dimensionally-printed carbonfiber-reinforced composites are increasingly

replacing thermosetting polymers and metals due to their lightweight structure and en-
hanced mechanical performance. This investigation examines the mechanical, thermal and
tribological characteristics of 3D-printed nylon (PA6) composites reinforced with 0.5 wt.%
multi-walled carbon nanotubes (MWCNTs), 15 wt.% short carbon fibers (CF), and a hybrid
combination of both, consisting of 0.5 wt.% MWCNTs and 15 wt.% CF. This study focuses
on evaluating the individual and synergistic effects of these reinforcements on the perfor-
mance of nylon-based composites. A series of characterizations, including mechanical,
thermal, tribological, morphological and FTIR analyses, are conducted. The tensile and
flexural strengths of the hybrid composite are improved by 35% and 42%, respectively,
compared to pure nylon. The findings emphasize the substantial influence of hybrid rein-
forcement on enhancing mechanical, thermal, and tribological properties, providing useful
information on the possible utilization of these composites in engineering applications
requiring high-performance materials.

Keywords: nylon; MWCNTs; carbon fiber (CF); 3D printing; mechanical, thermal, and
tribological properties

Academic Editor: Francesco

Tornabene

Received: 18 February 2025 1. Introduction

Revised: 15 March 2025 Polyamides, also referred to as nylons, are widely-used engineering thermoplastic ma-
Accepted: 21 March 2025
terials valued for their exceptional properties. These include high resistance to temperature
Published: 24 March 2025
and corrosion, excellent toughness, high modulus, anti-fatigue performance, and oil-proof
Citation: Siddikali, P.; Sreekanth,
characteristics, making them suitable for a broad variety of applications [1]. Among the
P.S.R. Evaluation of Mechanical,
various polyamides, poly(ε-caprolactam) (PA6), commonly known as polyamide-6 or
Thermal, and Tribological Properties
of 3D-Printed Nylon (PA6) Hybrid
nylon-6, is a versatile semi-crystalline engineering thermoplastic. It is highly regarded
Composites Reinforced with for its exceptional mechanical strength, superior stiffness, and remarkable chemical resis-
MWCNTs and Carbon Fibers. J. tance to various solvents and hydrocarbons [2]. CF-reinforced polymer (CFRP) composites
Compos. Sci. 2025, 9, 155. https:// have an increasingly widespread use as structural materials in industries such as aviation,
doi.org/10.3390/jcs9040155
aerospace, defense, and automobiles, where a combination of high strength and low density
Copyright: © 2025 by the authors. is crucial [3]. The performance of CFRP is strongly affected by the interface properties
Licensee MDPI, Basel, Switzerland. between the fibers and the polymer matrix. It is a significant design concern that the
This article is an open access article
unidirectional fiber-reinforced polymer composites exhibit uniform mechanical behavior
distributed under the terms and
under transverse deformation, interfacial characteristics, such as interfacial shear strength.
conditions of the Creative Commons
Attribution (CC BY) license
A variety of studies have explored how the matrix and interfacial properties influence
(https://creativecommons.org/ the mechanical performance of composites, utilizing both experimental and numerical
licenses/by/4.0/). methods [4,5].

J. Compos. Sci. 2025, 9, 155 https://doi.org/10.3390/jcs9040155

J. Compos. Sci. 2025, 9, 155 2 of 16

The process of 3D printing, which is an additive manufacturing method using material

extrusion, is frequently used for the production of thermoplastic polymer composites.
This approach offers several advantages, including simple equipment requirements, cost-
effectiveness, and the ability to produce complex components with ease [6–8]. Short fibers
are commonly blended with polymers to produce composites with enhanced properties.
Specifically, incorporating carbon fibers into polymer feedstock improves thermal conduc-
tivity, reduces thermal expansion, minimizes warping in larger prints, lowers residual
stresses within the part, and enhances the dimensional accuracy of printed components [9].
To enhance the mechanical characteristics of 3D-printed thermoplastics, short (discontinu-
ous) or long (continuous) CFs and MWCNTs are commonly used as reinforcements. As a
result, 3D-printed composite structures exhibit properties that significantly surpass those
of pure thermoplastics. Moreover, the properties of these composites are comparable to
metals, making them suitable for various industrial applications, especially when short
fibers are used as reinforcement [10].
Alarifi et al. [11] improved the mechanical properties (flexural strength) of nylon
reinforced with CF and glass fiber (GF) fabricated by 3D printing. Lu et al. [12] enhanced
the mechanical properties (tensile-94%, flexural-111%) of PEEK (polyether-ether-ketone)
through the addition of CF fabricated by 3D printing. Islam et al. [13] investigated the frac-
ture behavior of short and continuous CF-reinforced nylon matrix composites under tensile
loading. Their study improved tensile strength and modulus, proving that continuous CF is
superior to short CF in 3D-printing applications. Palaniappan et al. [14] investigated the me-
chanical properties (tensile and flexural) of CF-reinforced nylon composites fabricated using
3D printing. Their study found that tensile strength was significantly influenced by printing
speed, while impact and flexural strength were primarily affected by layer thickness and
raster angle. Uematsu et al. [15] examined the transverse tensile behavior of unidirectional
CF-reinforced polyamide 6 (PA6) composites, focusing on the PA6 matrix morphology.
Their study highlighted that unidirectional CFs influenced the mechanical behavior under
transverse tension. Dubey et al. [16] investigated the mechanical and viscoelastic behavior
of short CF-reinforced 3D-printed nylon composites, focusing on the impact of different
infill patterns. Their study found that the rectilinear pattern enhanced tensile strength,
while the triangular pattern provided better flexural strength. SV et al. [17] investigated
the mechanical behavior of PETG and nylon polymers fabricated using Material Extrusion
(MEX) in 3D printing. Their study found that the tensile strength of both materials is
significantly influenced by printing parameters, including nozzle and bed temperatures,
infill densities, printing speeds, and layer heights. Sun et al. [18] investigated the effects of
CF content and heat treatment on the mechanical, thermal, and microstructural properties
of PA6-CF composites fabricated using 3D printing. They achieved a maximum tensile
strength of 163 MPa under optimal heat treatment conditions (120 ◦ C for 7.5 h), representing
a 406% increase compared to unreinforced composites. Liu et al. [19] explored strategies
to enhance the mechanical properties of continuous fiber-reinforced PA6 by incorporating
various nanofillers into the polymer matrix. Their study demonstrated improvements in
both tensile strength and modulus. Rashid et al. [20] studied the effect of infill patterns and
densities on the mechanical properties of CF-reinforced PA6 composites. Triangular and
hexagonal patterns performed better at lower infill densities, while rectangular patterns
provided superior strength and elongation at higher densities.
This study investigates the mechanical, thermal, and tribological behavior of
MWCNTs-reinforced nylon composites, short CF-reinforced nylon composites, and a hy-
brid combination, which were produced by 3D printing. The emphasis is placed on the
investigation of how these reinforcements, either alone or in combination, influence the
strength, stiffness, wear resistance, scratch resistance, and hardness of the composites. Fur-
 J. Compos. Sci. 2025, 9, 155 3 of 16

ther, thermal properties are analyzed through differential scanning calorimetry (DSC) to see
how the reinforcements affect the melting trend of the nylon matrix. Ultimately, this study
aims to provide insights into the synergistic effects of MWCNT and CF reinforcements,
with potential applications in industries requiring lightweight, high-performance materials.

2. Material and Experimental Characterizations

2.1. Nylon, MWCNTs and CF Specifications
This study utilized thermoplastic nylon polymer (PA6)—a semi-crystalline material
obtained from Gujarat State Fertilizers & Chemicals Limited (GSFC), Gujarat, India—as
the base material. Amine-functionalized multi-walled carbon nanotubes (MWCNTs) from
Shilpa Enterprises, Maharashtra, India and short carbon fibers (CF) with a 3–6 mm length
and 7–10 µm diameter from NitPro composites, India were incorporated into the nylon
matrix to create nanocomposites and improve the material’s properties. The specifications
for the MWCNTs used are detailed in Table 1.

Table 1. Properties of MWCNTs.

Parameter Description
Purity (%) ~99
NH2 ratio (%) 2–5
Length (µm) >10
Outer dia. (nm) 10–20
Inner dia. (nm) 5–10

2.2. Filament Extrusion and Specimen Fabrication

The 3D-printing filaments, with a nominal diameter of 1.75 mm, were fabricated by
i. 2025, 9, x FOR PEER REVIEW extruding a polymer matrix reinforced with MWCNT, CF, and a hybrid combination4 of 18 of
MWCNT and CF. The compositions included 0.5 wt.% MWCNT, 15 wt.% CF, and a hybrid
mixture containing 0.5 wt.% MWCNT and 15 wt.% CF. To eliminate moisture, the mixture
was vacuum-dried at 80 ◦ C for 3–4 h. The fillers were uniformly dispersed within the
polymer matrix using a co-rotating twin-screw extruder (Aasabi/25TS/CO/300/30). The
extrusion process was carefully managed, with screw speeds maintained between 36 and
Nozzle diameter 0.4 mm 0.8 mm
40 rpm, melting temperatures ranging from 240 to 260 ◦ C, and a winding speed of 10 m per
Fill density 100% 100%
minute. The filament’s outer diameter variation was controlled to within ±0.1 mm. Both
Printthe
speed 35 mm/s
pure and reinforced specimens were manufactured using 35 the
mm/sMarkforged Mark Two
Temperature
(Genof2)nozzle 260
FDM 3D printer. Figure °C
1 illustrates 270 °C
the filament extrusion and 3D-printing process.
TemperatureTheofspecific
print bed 60 °C employed for specimen60fabrication
3D-printing parameters °C are detailed in
Orientation
Tableof2.layer 45° and 135° 45° and 135°

Figure 1. PresentFigure
work 1. Present the
involves work involves the
extrusion extrusion of
of filaments andfilaments and3D-printed
obtaining obtaining 3D-printed specimens.
specimens.

2.3. Differential Scanning Calorimetry (DSC)

DSC analysis was carried out on pure and reinforced nylon composite specimens in
a nitrogen atmosphere using a Perkin Elmer STA 8000, USA, from 30 to 300 °C at a tem-
perature rise of 10 °C per minute, and a 300 to 30 °C cooling ramp at 10 °C per minute was
performed.
J. Compos. Sci. 2025, 9, 155 4 of 16

Table 2. Key printing parameters of a 3D printer.

Nylon/CF and
Printing Parameters Nylon/MWCNT
Nylon/MWCNTs/CF
Height of layer 0.2 mm 0.2 mm
Nozzle diameter 0.4 mm 0.8 mm
Fill density 100% 100%
Print speed 35 mm/s 35 mm/s
Temperature of nozzle 260 ◦ C 270 ◦ C
Temperature of print bed 60 ◦ C 60 ◦ C
Orientation of layer 45 and 135◦
◦ 45 and 135◦
◦

2.3. Differential Scanning Calorimetry (DSC)

DSC analysis was carried out on pure and reinforced nylon composite specimens in
a nitrogen atmosphere using a Perkin Elmer STA 8000, Waltham, MA, USA, from 30 to
300 ◦ C at a temperature rise of 10 ◦ C per minute, and a 300 to 30 ◦ C cooling ramp at 10 ◦ C
per minute was performed.

2.4. Tensile Test

Tensile testing of both pure and reinforced nylon composite specimens was performed
using a Tinius Olsen H10KL universal testing machine (UTM), Tinus Olsen India Pvt. Ltd.
(Uttar Pradesh, India) in accordance with ASTM D638 Type V standards. The tests were
conducted at a strain rate of 5 mm/min at ambient temperature. In total, five specimens
were evaluated for each test condition, and the average results were documented.

2.5. Flexural Test

Flexural tests were carried out on both pure and reinforced nylon composite specimens
using a Tinius Olsen H10KL UTM in a three-point bending arrangement, following ASTM
D790 standards. The tests were conducted at a strain rate of 1 mm/min under ambient
temperature conditions. Five specimens were tested under each test condition, and the
average findings were provided.

2.6. Fourier Transform Infrared Spectroscope (FTIR)

FTIR spectroscopy was carried out on both pure and reinforced nylon composite
specimens using the attenuated total reflection (ATR) method. The spectral data were
obtained with an Agilent Technologies Cary 630 spectrometer (Santa Clara, CA, USA). In
total, 64 scans were recorded across the wavelength range of 600–4000 cm−1 . Standard
Normal Variate (SNV) normalization was applied to the data. This technique involves
subtracting the mean from each spectral intensity value and then dividing by the standard
deviation [21,22].

2.7. Surface Morphology (Scanning Electron Microscopy)

The surface morphology and microstructure of the pure nylon and its composite
specimens were analyzed after the tensile test using a CARL ZEISS EVO10 machine (Zeiss
Microscopy, LLC, White Plains, NY, USA). To examine the surface morphology of the
fractured specimens post-tensile testing, the fracture surfaces were coated with gold via
sputter coating.

2.8. Tribological Analysis

2.8.1. Wear Characterization
The wear characteristics of pure nylon and its composites were evaluated using a pin-
on-disc tribometer (Model TR-20LE, Ducom, Bangalore, India). The tests were conducted
J. Compos. Sci. 2025, 9, 155 5 of 16

under conditions of a 200 rpm rotational speed, a 30 N normal load, and a duration of 30
min. The square specimens were each 8 mm × 8 mm in size and 5 mm thick. For the wear
tests, these specimens were firmly affixed to a rectangular holder with adhesive.

2.8.2. Scratch Test

The scratch resistance of the pure nylon and its composite specimens was assessed
using a CSM Micro-Scratch Tester (MST) from Neuchatel, Switzerland. The evaluation
included both single- and multiple-scratch tests. A conical diamond indenter, featuring a
200 µm diameter and a 120◦ cone angle, was utilized to create 10 mm long scratches at a
speed of 1 mm/min with a normal force of 30 N. All scratches were performed at room
temperature. Instantaneous and residual scratch depths were measured for an applied load
and number of scratches. The scratch hardness is determined by Equation (1):

4P
Hs = (1)
πd2
where P is the normal force in N and d is the scratch width determined from the software.

2.8.3. Hardness Test

The hardness (measured in HV) of pure nylon and its composite specimens was
determined using an RS Scientific FMV1-MC-AT Micro Vickers hardness tester equipped
with a diamond indenter. A load of 0.05 kg was applied to the sample surface for a dwell
time of 5 s. The hardness value was calculated using the following Equation (2):

F
HV = 1.889 (2)
d2
where F represents the applied force (N), and d is the diagonal length of the square indenta-
tion (mm).

3. Results and Discussion

3.1. DSC Test Results
Figure 2 shows the effect of MWCNTs, CF, and their hybrid fillers on the melting (Tm )
and crystallization (Tc ) temperature behavior of a nylon composite by using DSC. For pure
nylon, the Tm was recorded at 215.2 ◦ C with a melting enthalpy (∆Hm ) of 54.82 J/g. Upon
incorporating 0.5 wt% MWCNTs, the Tm increased to 218.3 ◦ C. These observations, along
with additional data, are detailed in Table 3. This increase can be attributed to the MWCNTs
acting as nucleating agents, promoting enhanced crystallization and increasing the degree of
crystallinity in the PA6 matrix. This leads to a more stable crystalline structure, requiring a
higher thermal energy input to break the ordered regions during melting, thereby increasing
Tm. Additionally, the formation of a MWCNT network within the polymer restricts the
molecular motion of polymer chains, limiting their ability to reorganize into a lower-energy
state upon heating, further contributing to the observed increase in Tm [23–25]. In contrast,
the inclusion of 15 wt.% CFs into the nylon matrix resulted in an increase in Tm to 219.3 ◦ C.
This increase is primarily due to the disruptive effect of the CFs on the crystalline structure
of nylon. The fibers interfere with the orderly packing of the polymer chains, leading to an
increase in crystallinity and, consequently, a higher melting temperature [15,26,27].
J. Compos. Sci. 2025, 9, x FOR PEER REVIEW 7 of 18

J. Compos. Sci. 2025, 9, 155 6 of 16

Firstheating
Figure2.2.First
Figure heatingscan
scanof
ofDSC
DSCthermographs
thermographsof
ofnylon
nylonand
andtheir
theircomposites.
composites.

3. DSC datathe
TableMoreover, of hybrid
nylon/MWCNT/CF composites.
composition, which combined MWCNTs and CFs, exhibited a
Tm of 221.2 °C, slightly higher than that of the 15 wt.% CF composites. This behavior
Material/Reinforcement Tm /◦ C Tc / ◦ C ∆Hm
suggests that while the CFs enhance the crystalline lattice, the presence of MWCNTs may
Nylon (N) 215.2 178.2 54.82
form a reinforcing network that further improves the structural integrity and thermal sta-
N+0.5% MWCNT 218.3 179.3 61.48
bility of the nylon
N+15%matrix.
CF 219.3 180.1 64.78
N+0.5% MWCNT+15%CF 221.2 181.5 67.64
Table 3. DSC data of nylon/MWCNT/CF composites.

Material/Reinforcement
Moreover, the hybrid composition, Twhich m /°C combined MWCNTs
Tc/°C and CFs, ∆H
exhibited
m

a Tm of 221.2 ◦
Nylon (N)
C, slightly 215.2
higher than that of the 15 wt.% CF178.2
composites. This54.82
behavior
N+0.5% MWCNT 218.3 179.3 61.48
suggests that while the CFs enhance the crystalline lattice, the presence of MWCNTs may
N+15% CF
form a reinforcing network that further 219.3 180.1 integrity and
improves the structural 64.78
thermal
N+0.5% MWCNT+15%CF
stability of the nylon matrix. 221.2 181.5 67.64
Furthermore, the heat of fusion, indicative of a polymer’s crystallinity, is determined
Furthermore, the heat
by integrating the area of the
under fusion, indicative
melting of a polymer’s
temperature crystallinity,
(Tm ) peaks is determined
in DSC curves. For nylon
by integrating the area under the melting temperature (T m) peaks in DSC curves. For ny-
(PA6), the heat of fusion for a 100% crystalline sample is reported as 188 J/g [26,28]. This
lon (PA6),
value servestheasheat of fusiontofor
a reference a 100%the
calculate crystalline sample is reported
weight percentage as 188
crystallinity J/g [26,28].
of both virgin
This value serves as a reference to calculate the weight percentage crystallinity
PA6 and its composites, such as those reinforced with MWCNTs, CF, or a combination of bothof
virgin PA6 and its composites, such as those reinforced with MWCNTs, CF,
both, as shown in Figure 3. The degree of crystallinity (Xc ) of a polymer can be calculatedor a combi-
nation of both,
using the as shown
following in Figure
Equation (3): 3. The degree of crystallinity (Xc) of a polymer can be
calculated using the following Equation (3):
∆Hm
=𝑐 =  ∆𝐻𝑚 X×
Xc 𝑋 100%
100% (3)
(3)
∆H f 𝑓1(1−𝑤
∆𝐻 − w𝑓 )f
In this formula, Xc represents the degree of crystallinity, ΔHm is the measured melting
In this formula,
enthalpy Xc represents
of the composite, ΔHf the degree
denotes theofenthalpy
crystallinity, ∆Hm for
of fusion is the measured
100% melting
crystalline PA6
enthalpy of the composite, ∆H f denotes
(taken as 188 J/g), and wf is the mass the enthalpy of fusion for 100% crystalline
fraction of carbon fiber in the composite. PA6
(taken as 188 J/g), and wf is the mass fraction of carbon fiber in the composite.
 J. Compos. Sci. 2025, 9, x FOR PEER REVIEW 8 of 18
J. Compos. Sci. 2025, 9, x FOR PEER REVIEW 8 of 18
J. Compos. Sci. 2025, 9, 155 7 of 16

Figure Crystallinity
3.Crystallinity
Figure 3. of of nylon
nylon andand its composites.
its composites.
Figure 3. Crystallinity of nylon and its composites.
3.2. TensileTest
3.2. Tensile TestResults
Results
3.2. Tensile
Figure
Figure Test Results thethe
44illustrates
illustrates tensile
tensile properties
properties of various
of various nylonnylon composites,
composites, highlighting
highlighting
the Figure of
the impact
impact 4ofillustrates
different
different the tensile properties
reinforcements
reinforcements on of
on their various
tensile
their nylon composites,
performance.
tensile performance. highlighting
Pure nylon
Pureexhibits
nylon exhibits
the impact
excellent of different
excellent ductility,
ductility,with reinforcements
witha astrain
strain on
capacity their tensile
exceeding
capacity 300%
exceeding performance.
and and
300% Pure
an ultimate nylon exhibits
tensiletensile
an ultimate strength strength of
excellent
of ductility,40
approximately with a strain
MPa. In capacitythe
contrast, exceeding
inclusion300%
of and
0.5 an ultimate
wt.% MWCNT tensile strength
improves the
approximately 40 MPa. In contrast, the inclusion of 0.5 wt.% MWCNT improves the tensile
of approximately
tensile strength to 40 47.4MPa.
MPaIn contrast,
but the inclusion
significantly of 0.5 wt.%
reduces ductility. ThisMWCNT
strength improves
enhancement the
strength to 47.4 MPa but significantly reduces ductility. This strength enhancement is a
tensile strength
is a result of thetouniform
47.4 MPa but significantly
dispersion reduces
of MWCNTs ductility.
and Thisinterfacial
enhanced strength enhancement
adhesion be-
result
is of the
a result uniform dispersion ofofMWCNTs and enhancedinterfacial
interfacial adhesion be- between
tween the of the
MWCNTs uniformanddispersion MWCNTs
the nylon polymer and thus
matrix, enhanced
facilitating load adhesion
transfer and
the
tween MWCNTs
the MWCNTs
stress distribution
and the nylon polymer
andnanocomposite.
in the the nylon polymer matrix, thus
matrix, thus
The decreased
facilitating
facilitating
elongation
load transfer
load transfer
is a result and
of the inter-
and stress
distribution
stress
ference by MWCNTin the
distribution innanocomposite.
the nanocomposite.
particles The
with polymerThedecreased
decreased
chain elongation
elongation
mobility. isaaresult
is
This constrainedresultofofthe
the
mobility interference
inter-
re-
by MWCNT
ference by MWCNTparticles with
particles polymer
with chain
polymer mobility.
chain mobility. This
This constrained
constrained
sults in additional resistance to the alignment of the chains upon loading, which is vital mobility
mobility re-results in
sults in additional
additional
for high resistance
elongation resistance
to thetoalignment
[27,29]. the alignment of the
of the chains
chains upon
upon loading,which
loading, which is is vital
vital for high
for high elongation
elongation [27,29].[27,29].

Figure 4. (a) Tensile stress–strain curves (b) Ultimate tensile strength of nylon and its composites.
Figure (a)Tensile
Figure 4.4.(a) Tensile stress–strain
stress–strain curves
curves (b) Ultimate
(b) Ultimate tensiletensile strength
strength ofand
of nylon nylon and its composites.
its composites.
On the other hand, the incorporation of 15 wt.% CF substantially enhances tensile
Onthe
On
strength the52.2
to other
other hand,
hand,
MPa duethe totheits incorporation
incorporation 15of
reinforcingofeffect, 15 wt.%
wt.% it CF substantially
CF substantially
though reduces strain enhances
theenhances break, tensile
at tensile
strength
strength toto
indicating 52.2MPa
a52.2 MPa
stiffening ofdue
due to reinforcing
tocomposite
the its its reinforcing effect,
effect,
[30]. The though
hybrid though it reduces
it reduces
combination ofthe the
0.5strain
wt.% atstrain
break, at break,
MWCNT
indicating
indicating
and 15 wt.% aastiffening
stiffening
CF of in
results thethe
of composite
the composite
highest [30].[30].
tensileThe hybrid combination
The hybrid
strength of of 0.5 wt.%
60.9 combination
MPa among MWCNT
of 0.5
the wt.%15MWCNT
and
and
and 15
wt.%15 wt.%
MWCNT
wt.% CFCF results
and in the
CF tested.
results in the highest
The tensile
increased
highest strength
tensile
tensile of 60.9
strength
strength MPa
ofmightamong amongand
the 0.5
be attributed
60.9 MPa 15
to the
the 0.5 and 15
wt.% MWCNT and CF tested. The increased tensile strength might be attributed to the
wt.% MWCNT and CF tested. The increased tensile strength might be attributed to the
proper alignment of CF within the polymer matric, as well as its even distribution, balance
between effective fiber–matrix adhesion, orientation, and. This enhances elastic modulus,
facilitates effective load carrying, and ensures efficient load transfer between the CF and the
matrix. However, the strain capacity remains similar to that of the CF-reinforced composite,
suggesting that the reduction in ductility is primarily governed by the CF content. Overall,
J. Compos. Sci. 2025, 9, 155 8 of 16

the tensile strength improved by 16, 24, and 35% with the addition of 0.5 wt.% MWCNT,
15 wt.% CF, and the hybrid reinforcement, respectively, compared to pure nylon.
To understand the underlying mechanisms of reinforcement effects on the mechani-
cal properties of the polymer composite, fractography analysis was performed. Figure 5
presents SEM micrographs of the fractured surfaces of pure nylon and its composites after
tensile testing. Figure 5a shows the fractured surface of pure nylon, characterized by a
rough texture with visible fractures and irregularities. On the other hand, Figure 5b reveals
significant changes in the fracture surface topography of the nanocomposite, showing
that the presence of functionalized MWCNT promotes the polymer’s interfacial adhesion
thereby enhancing the mechanical properties by improving load transfer and stress distri-
bution within the nanocomposite. Furthermore, Figure 5c,d depict CF stacked with nylon,
exhibiting good distribution within the matrix. This uniform distribution
J. Compos. Sci. 2025, 9, x FOR PEER REVIEW 10 ofcontributes
18 to
improved mechanical properties and also plays a critical role in enhancing the interlaminar
fracture toughness of the composite. Failure mechanisms such as debonding, fiber breakage,
and fiber pull-out are observed in the samples.

Figure
Figure5. 5.
SEMSEM
micrographs at a magnification
micrographs of 1200× and
at a magnification 2500×
of 1200 × (a)
andPure nylon
2500 × (a)(N),Pure
(b) nylon (N),
N+MWCNTs, (c) N+CF, and (d) N+MWCNT+CF.
(b) N+MWCNTs, (c) N+CF, and (d) N+MWCNT+CF.

3.3. Flexural Test Results

Figure 6 illustrates the flexural behavior of pure nylon and its composites with dif-
ferent reinforcements. Pure nylon exhibits a flexural stress of 73.1 MPa. The addition of
0.5 wt.% MWCNT improves the flexural strength to 108 MPa, indicating a significant en-
hancement compared to pure nylon. This enhancement is credited to the even distribution
 J. Compos. Sci. 2025, 9, 155 9 of 16

3.3. Flexural Test Results

Figure 6 illustrates the flexural behavior of pure nylon and its composites with different
reinforcements. Pure nylon exhibits a flexural stress of 73.1 MPa. The addition of 0.5 wt.%
MWCNT improves the flexural strength to 108 MPa, indicating a significant enhancement
2025, 9, x FOR PEER REVIEW 11 of 18
compared to pure nylon. This enhancement is credited to the even distribution of MWCNTs
and the improved bonding at the interface with the polymer matrix, which facilitates better
load transfer and stress distribution in the nanocomposite. A further enhancement is
observed with the addition of 15 wt.% CF, which increases the composite’s flexural strength
to 112 MPa. The hybrid combination of 0.5 wt.% MWCNT and 15 wt.% CF achieves the
improvement in highest flexural
mechanical stress of 127 MPa,
performance. This demonstrating a synergistic
substantial increase improvement
in strength can beinat-
mechanical
performance.
tributed to the proper alignmentThisand
substantial increase in strength
even distribution canfibers
of carbon be attributed
withinto thepolymer
the proper alignment
and even distribution of carbon fibers within the polymer matrix, which enhances stiffness,
matrix, which enhances stiffness, load-carrying capacity, and efficient load transfer. Ad-
load-carrying capacity, and efficient load transfer. Additionally, this combination achieves
ditionally, this combination achieves a high strength-to-weight ratio.
a high strength-to-weight ratio.

Figure
Figure 6. (a) Flexural 6. (a) Flexural
stress–strain andstress–strain andflexure
(b) ultimate (b) ultimate flexure
stress stressand
of nylon of nylon and its composites.
its composites

Overall, the flexural strength is improved by 32%, 35%, and 42% with the addition
Overall, the flexural strength is improved by 32%, 35%, and 42% with the addition of
of 0.5 wt.% MWCNT, 15 wt.% CF, and the hybrid reinforcement, respectively, compared
0.5 wt.% MWCNT, 15 wt.% CF, and the hybrid reinforcement, respectively, compared to
to pure nylon. These results highlight the superior performance of the hybrid composite,
pure nylon. These results highlight
demonstrating the superior
the effectiveness performance
of combining of the hybrid
reinforcements composite,
to enhance nylon’s mechanical
demonstrating the effectiveness
properties. of combining reinforcements to enhance nylon’s mechan-
ical properties.
3.4. FTIR Analysis
3.4. FTIR Analysis Figure 7 depicts the FTIR spectra of pure nylon and its composites, which establish the
anticipated chemical structure of polyamide polymers. The amine primary group’s N-H
Figure 7 depicts the FTIR spectra of pure nylon and its composites, which establish
bending vibration is represented by the 3296 cm−1 absorption band. The C-H symmetric
the anticipated chemical structure of polyamide polymers. The amine primary group’s N-
and asymmetric stretching vibrations are represented by the linked bands at 2855 cm−1
H bending vibration is represented by the 3296 cm⁻1 absorption band. The C-H symmetric
and 2930 cm−1 , respectively. The distinctive bands of the amide groups occur at 1635 cm−1
and asymmetric (amide
stretching
I, C=Ovibrations
stretchingarevibration),
represented 1534by
cmthe linked II,
−1 (amide bands
C-N at 2855 cm⁻¹
stretching and CO-N-
and 2930 cm⁻1, respectively. The distinctive bands
− 1 of the amide groups
H bending vibration), 1461 cm (amide III, C-N stretching and C-H occur at 1635 cm⁻ 1 bending
in-plane
(amide I, C=O stretching
vibration), vibration),
and 1262 cm1534−1 (amide
cm⁻1IV,(amide II, C-N stretching
C-CO stretching and CO-N-H
vibration) [30].
bending vibration), 1461 cm⁻ (amide of
1
The incorporation III,0.5C-N stretching
wt.% MWCNT intoandthe
C-H in-plane
nylon matrixbending
results invibra-
a slight increase
in the intensity − 1 − 1
tion), and 1262 cm⁻ 1 (amide IV,ofC-CO
the N–H at 3296 cm
stretching and Amide
vibration) [30].I peaks at 1534 cm compared to pure
The incorporation of 0.5 wt.% MWCNT into the nylon matrixand
nylon. This suggests interactions between the MWCNT the nylon
results in a matrix, likely due to
slight in-
hydrogen
crease in the intensity bonding
of the N–H or at physical
3296 cminteractions,
−1 and Amide which restrict
I peaks chaincm
at 1534 mobility and enhance the
−1 compared
structural stability of the polymer. In contrast, the addition of 15 wt.% CF leads to a slight
to pure nylon. This suggests interactions between the MWCNT and the nylon matrix,
reduction in the intensity of the Amide I and N–H peaks. This decrease in peak intensity
likely due to hydrogen bonding or physical interactions, which restrict chain mobility and
enhance the structural stability of the polymer. In contrast, the addition of 15 wt.% CF
leads to a slight reduction in the intensity of the Amide I and N–H peaks. This decrease
in peak intensity indicates a partial disruption of hydrogen bonding within the matrix,
likely caused by the fiber–matrix interactions [14,31,32]. Furthermore, the hybrid combi-
 J. Compos. Sci. 2025, 9, 155 10 of 16

indicates a partial disruption of hydrogen bonding within the matrix, likely caused by the
fiber–matrix interactions [14,31,32]. Furthermore, the hybrid combination of MWCNT and
J. Compos. Sci. 2025, 9, x FOR PEER REVIEW 12 of 18
CF demonstrates a partial recovery in the intensity of the N–H stretching peak compared
to the CF-only composition. This suggests that the reinforcing effect of MWCNT partially
counteracts the disruption caused by CF, contributing to improved structural retention in
the hybrid system.

Figure 7. FTIR spectrum of pure nylon and its composites.

Figure 7. FTIR spectrum of pure nylon and its composites.
3.5. Tribological Analysis
3.5. Tribological
3.5.1. Wear Rate Analysis
Analysis
3.5.1.Figure
Wear 8Rate Analysis
presents an analysis of the tribological performance of nylon and its com-
posites. Initially, all specimens
Figure 8 presents an analysis exhibit a rapid
of the increase
tribological in wear rateof
performance within
nylontheandfirst 200
its compo-
s, indicating
sites. anall
Initially, initial wear phase.
specimens exhibitAmong
a rapidthem, pure nylon
increase in wear demonstrates
rate within the
thehighest
first 200 s,
wear rate, peaking at approximately 60 µm. This highlights its susceptibility to wear
indicating an initial wear phase. Among them, pure nylon demonstrates the highest wear
under operational conditions, primarily due to adhesive wear, fatigue wear, and plowing
rate, peaking at approximately 60 µm. This highlights its susceptibility to wear under op-
mechanisms. The increased wear rate in pure nylon can be attributed to its relatively low
erational conditions, primarily due to adhesive wear, fatigue wear, and plowing mecha-
hardness and lower fatigue resistance. Additionally, nylon’s tendency to absorb moisture
nisms. The increased wear rate in pure nylon can be attributed to its relatively low hard-
and soften at elevated temperatures may further contribute to its higher wear rate. The
ness and lower fatigue resistance. Additionally, nylon’s tendency to absorb moisture and
incorporation of 0.5 wt.% MWCNTs into the nylon matrix significantly reduces the wear
softenwhich
rate, at elevated
stabilizestemperatures
at around 50 may µmfurther contribute
after the to its higher
initial phase. wear rate.wear
The subsequent The incor-
is
mainly due to abrasive interactions between the nylon composite (N+MWCNT) surfacerate,
poration of 0.5 wt.% MWCNTs into the nylon matrix significantly reduces the wear
which
and thestabilizes
metal disc.atThisaround 50 µm
reduction after rate
in wear the initial phase.toThe
is attributed subsequent
the formation of awear is mainly
protective
due to
layer byabrasive
MWCNTs, interactions between
which minimizes the contact
direct nylon composite (N+MWCNT)
with the counterface. surface and
Additionally, the the
metal disc.
increased This reduction
hardness in wear
and stiffness rate
of the is attributed
composite lead to the formation
reduced of a protective
deformation under thelayer
by MWCNTs,
load, whichflow.
limiting plastic minimizes
Improved direct contact
thermal with the counterface.
conductivity Additionally,
further enhances performance the in-
creased
by hardness
efficiently and stiffness
dissipating of thepreventing
heat, thereby compositethermal
lead todegradation.
reduced deformation under the
load, limiting plastic flow. Improved thermal conductivity further enhances performance
by efficiently dissipating heat, thereby preventing thermal degradation.
J. Compos. Sci. 2025, 9, x FOR PEER REVIEW 13 of 18

J. Compos. Sci. 2025, 9, 155 11 of 16

Figure 8. Wear rate of pure nylon and its composites.

Figure 8. Wear rate of pure nylon and its composites.
Similarly, the nylon composite reinforced with 15 wt.% CF exhibits an even lower wear
rate ofSimilarly, the nylon
approximately 30 µm,composite
demonstrating reinforced withimprovement
a substantial 15 wt.% CFinexhibits an even lower
wear resistance.
wear rate of approximately 30 µm, demonstrating a substantial improvement
This enhancement is due to the strong load-bearing structure provided by carbon fibers, in wear re-
sistance.
which This surface
reduces enhancement
wear and is improves
due to the strong load-bearing
resistance to deformation. structure provided
Furthermore, by carbon
CF acts
fibers,
as which reduces
a reinforcing surfacefriction
agent, lowering wear and
and improves
minimizingresistance to deformation.
abrasive wear Furthermore
[33,34]. Notably, the
hybrid
CF actscombination of both agent,
as a reinforcing MWCNT and CF yields
lowering theand
friction best minimizing
results, with wear rates wear
abrasive stabi- [33,34]
lizing at around 10 to 15 µm. This substantial enhancement in performance
Notably, the hybrid combination of both MWCNT and CF yields the best results, suggests that with
the synergistic effect of MWCNT and CF significantly improves the tribological
wear rates stabilizing at around 10 to 15 µm. This substantial enhancement in performance properties
of nylon composites. The transition to a steady state, observed around 400 s, indicates that
suggests that the synergistic effect of MWCNT and CF significantly improves the tribo-
the composites stabilize with minimal fluctuations in wear rate.
logical properties of nylon composites. The transition to a steady state, observed around
400 s,Coefficient
3.5.2. indicates of
that the composites
Friction (COF) stabilize with minimal fluctuations in wear rate.
Figure 9 illustrates the variation of the COF with distance for pure nylon and its
3.5.2. Coefficient
composites. ofall
Initially, Friction (COF)
specimens exhibit a sharp peak in COF before stabilizing, reaching
equilibrium
Figureafter approximately
9 illustrates 500 m of sliding
the variation distance.
of the COF withPure nylon (N)
distance for shows the highest
pure nylon and its com-
COF,
posites. Initially, all specimens exhibit a sharp peak in COF before stabilizing,ofreaching
with a static COF of 0.271 and a stabilized kinetic COF of 0.238. The addition
MWCNT
equilibriumsignificantly reduces both static
after approximately 500 m andofkinetic
slidingCOF to approximately
distance. Pure nylon 0.253
(N)and 0.220,
shows the high-
respectively, making it the most effective in lowering friction. The inclusion of CF results in
est COF, with a static COF of 0.271 and a stabilized kinetic COF of 0.238. The addition of
a slightly lower COF than pure nylon, with static and kinetic values around 0.264 and 0.226,
MWCNT significantly reduces both static and kinetic COF to approximately 0.253 and
respectively. The CF content in the nylon composite further reduces the COF compared to
0.220, respectively, making it the most effective in lowering friction. The inclusion of CF
pure nylon, likely due to CF’s unique structure. As a graphitized carbon, CF has hexagonal
resultsaligned
planes in a slightly lower COF
perpendicular to thethan
fiber pure nylon,iswith
axis, which static
believed and kinetic
to contribute values around
to friction
0.264 andwhen
reduction 0.226, respectively.
sliding The[35].
against steel CF Meanwhile,
content in the
thecombination
nylon composite
of MWCNTfurther
andreduces
CF the
COF compared
yields to pure
an intermediate COF,nylon, likelyand
with static due to CF’s
kinetic unique
values structure.
of 0.270 Asrespectively,
and 0.199, a graphitized car-
bon,toCF
due thehas hexagonal
synergetic planes
effect aligned
of MWCNT andperpendicular
CF. to the fiber axis, which is believed to
contribute to friction reduction when sliding against steel [35]. Meanwhile, the combina-
tion of MWCNT and CF yields an intermediate COF, with static and kinetic values of 0.270
and 0.199, respectively, due to the synergetic effect of MWCNT and CF.
J. Compos. Sci. 2025, 9, x FOR PEER REVIEW 14 of 18

J. Compos. Sci. 2025, 9, 155 12 of 16

Figure 9. Coefficient of friction of pure nylon and its composites during wear test using pin-on-disk
apparatus.
Figure9.9. Coefficient
Figure Coefficientofoffriction
frictionofofpure
purenylon
nylonand itsits
and composites during
composites wear
during test test
wear using pin-on-
using pin-on-disk
disk apparatus.
apparatus.
3.5.3. Scratch Test
3.5.3. Scratch Test
The scratch3.5.3.
test results
Scratch are presented in Figure 10. Both MWCNT and CF fillers are
Test
The scratch test results are presented in Figure 10. Both MWCNT and CF fillers are
shown to improve scratch resistance. Pure nylon exhibits greater penetration and higher
shown The scratch test
to improve results
scratch are presented
resistance. Pure nyloninexhibits
Figure greater
10. Both MWCNTand
penetration andhigher
CF fillers are
plastic deformation with a scratch hardness (Hs) of 78. However, the addition of MWCNTs
plastic deformation with a scratch hardness (H ) of 78. However, the addition
shown to improve scratch resistance. Pures nylon exhibits greater penetration and higher of MWCNTs
to nylon reducestoboth penetration
nylondeformation
depth
reduces bothwith
and plastic
penetration depth
deformation
and plastic
with a Hs with
deformation
of 117.
aH
This
plastic a scratch hardness (Hs) of 78. However, the s of 117. of
addition This
MWCNTs
improvement is improvement
due to the lubricating
is due to effect
the of MWCNTs,
lubricating effect which
of MWCNTs,lower the
which coefficient
lower the of
coefficient
to nylon reduces both penetration depth and plastic deformation with a Hs of 117. This
friction (COF) inofthe composite.
friction (COF) in Additionally,
the composite.theAdditionally,
reduced breaking strength
the reduced of thestrength
breaking com- of the
improvement is due to the lubricating effect of MWCNTs, which lower the coefficient o
posite, which is composite,
linked to the MWCNT
which content,
is linked also contributes
to the MWCNT content,to thecontributes
also lower COF to by
thede-
lower COF
friction (COF) in the composite. Additionally, the reduced breaking strength of the com-
creasing the tangential force during
by decreasing scratching,
the tangential as the scratching,
force during friction coefficient is directly
as the friction pro-is directly
coefficient
posite, which
proportional to
is
the
linked to the
tangential
MWCNT
force [35–39].
content, also contributes to the lower COF by de
portional to the tangential force [35–39].
creasing the tangential force during scratching, as the friction coefficient is directly pro
portional to the tangential force [35–39].

Figure 10. VickersFigure 10. Vickers

hardness hardness
(i) Scratch (i) Scratch(ii)
indentation, indentation, (ii) Scratch
Scratch hardness (Hhardness
s) values(H s ) values
of: of: (a) Pure
(a) Pure
nylon (N), (b) N+MWCNT, (c) N+CF, and (d) N+MWCNT+CF.
nylon (N), (b) N+MWCNT, (c) N+CF, and (d) N+MWCNT+CF.
Figure 10. Vickers hardness (i) Scratch indentation, (ii) Scratch hardness (Hs) values of: (a) Pure
In contrast, the N+CF composite shows better performance in terms of scratch width
nylon
In contrast, and (N), (b)
the depth,
N+CF N+MWCNT,
composite shows(c) N+CF,
better and (d) N+MWCNT+CF.
performance in terms of scratch width
with an increase in H s as shown in Figure 10(ii) [39]. This improvement can be
and depth, withattributed
an increase in H
to the s as shown
greater rigidityinofFigure 10ii [39].
CFs, which This improvement
help distribute canevenly
stresses more be across
In contrast, the N+CF composite shows better performance in terms of scratch width
attributed to the greater rigidity of CFs, which help distribute stresses more evenly across
and depth, with an increase in Hs as shown in Figure 10ii [39]. This improvement can be
the nylon matrix and contribute to a reduction in COF. Furthermore, the hybrid nylon
attributed to the greater rigidity of CFs, which help distribute stresses more evenly across
the nylon matrix and contribute to a reduction in COF. Furthermore, the hybrid nylon
J. Compos. Sci. 2025, 9, 155 13 of 16

composite, which combines both MWCNT and CF, exhibits the highest Hs of 524, with the
the nylon matrix and contribute to a reduction in COF. Furthermore, the hybrid nylon
smallest width, depth, and plastic deformation among all the materials. This is due to the
composite, which combines both MWCNT and CF, exhibits the highest Hs of 524, with the
synergistic effect of MWCNTs
smallest and and
width, depth, CFs.plastic deformation among all the materials. This is due to the
synergistic effect of MWCNTs and CFs.
3.5.4. Hardness Test
3.5.4. Hardness Test
The Vickers hardness of nylon and its composites, along with the corresponding mi-
cro-indentations, isThe Vickers hardness
illustrated in Figureof 11.
nylon
Theand its composites,
hardness along
increases withthe
with theincorporation
corresponding micro-
indentations, is illustrated in Figure 11. The hardness increases with the incorporation
of reinforcements into the nylon matrix. Pure nylon exhibits a hardness of 40 HV, while
of reinforcements into the nylon matrix. Pure nylon exhibits a hardness of 40 HV, while
the addition of MWCNTs raises it to 43 HV. Similarly, CF reinforcement further enhances
the addition of MWCNTs raises it to 43 HV. Similarly, CF reinforcement further enhances
the hardness to 45 HV [33], and the hybrid combination of both reinforcements achieves
the hardness to 45 HV [33], and the hybrid combination of both reinforcements achieves
the highest value
the of 48 HV.
highest The of
value improvements in hardness result
48 HV. The improvements from the
in hardness enhanced
result load-
from the enhanced
bearing capacity, improved
load-bearing interfacial
capacity, bonding,
improved andbonding,
interfacial reducedand creep andcreep
reduced plastic
anddefor-
plastic defor-
mation. The synergistic
mation. The effect of MWCNTs
synergistic effect ofand CF contributes
MWCNTs to the maximum
and CF contributes hardness
to the maximum hardness
enhancement in nylon composites.
enhancement in nylon composites.

Figure
Figure 11. Vickers 11. Vickers
hardness hardness (i)marks,
(i) Indentation Indentation marks, (ii)
(ii) Hardness Hardness
values values
of: (a) Pure of: (a) Pure
nylon nylon (N),
(N), (b)
N+MWCNT, (c)(b) N+MWCNT,
N+CF, and (d)(c) N+CF, and (d) N+MWCNT+CF.
N+MWCNT+CF.
4. Conclusions
4. Conclusions The work examined the influence of MWCNT and CF individually and their hybrid,
The workon examined the influence
the mechanical, thermal, of
andMWCNT and
tribological CF individually
properties and their
of PA6 composites at hybrid,
various weight
on the mechanical, thermal,
percentages. andtest
All the tribological
specimens properties
were preparedof PA6
via 3Dcomposites at various
printing followed by diverse
characterizations.
weight percentages. Thespecimens
All the test main conclusions are as follows:
were prepared via 3D printing followed by
•
diverse characterizations. Theproperties
Mechanical main conclusions
improvedare
dueastofollows:
the synergistic effect of MWCNTs and CFs.
The hybrid reinforcement (0.5 wt.% MWCNTs and 15 wt.% CF) significantly enhanced
• Mechanical properties improved due to the synergistic effect of MWCNTs and CFs.
tensile and flexural properties through proper alignment and even distribution within
The hybrid reinforcement (0.5 wt.% MWCNTs and 15 wt.% CF) significantly en-
the polymer matrix.
hanced tensile and flexural properties through proper alignment and even distribu-
• The addition of MWCNTs and CFs to the nylon interferes with the orderly packing of
tion within the polymer
the polymermatrix.
chains, leading to an increase in crystallinity and, consequently, a higher
• The addition melting
of MWCNTs and CFs to the nylon interferes with the orderly packing
temperature
of the polymer
• Thechains, leading
synergistic toofanMWCNTs
effect increase and
in crystallinity
CF contributes and, consequently,
to the a
maximum hardness
higher melting temperature
enhancement in nylon composites. The improvements in hardness result from the
• enhanced load-bearing
The synergistic effect of MWCNTs and capacity and improved
CF contributes to interfacial
the maximumbonding. This could
hardness en- result
hancement ininnylon
enhanced creep resistance
composites. and reduced plastic
The improvements deformation.
in hardness result from the en-
hanced load-bearing capacity and improved interfacial bonding. This could result in
enhanced creep resistance and reduced plastic deformation.
J. Compos. Sci. 2025, 9, 155 14 of 16

• The presence of MWCNT and CF has considerably lowered the wear during the run-in
phase thereby marking a lower static coefficient of friction and subsequently a lower
kinetic friction coefficient.
• Tangential force during scratching is lowered, which reduces the plastic deformation
and thereby enhances the composites’ performance. The penetration depth and plastic
deformation of the composite samples were observed to be reduced due to increased
scratch hardness.

Author Contributions: P.S.: conceptualization, methodology, software, validation, testing, and

writing—original draft preparation. P.S.R.S.: visualization, investigation, supervision, and writing—
reviewing and editing. All authors have read and agreed to the published version of the manuscript.

Funding: This research received no external funding.

Institutional Review Board Statement: Not applicable.

Informed Consent Statement: Not applicable.

Data Availability Statement: Made on request.

Acknowledgments: The authors gratefully acknowledge the invaluable technical support received
from Sivanagaraju, VIT-AP university during the sample fabrication and also for his in-depth technical
discussion which helped in results analysis. The authors also declare that they have no known
competing financial interests or personal relationships that could have appeared to influence the
work reported in this paper.

Conflicts of Interest: The authors declare no conflicts of interest.

Abbreviations
The following abbreviations are used in this manuscript:

N Nylon
PA6 Polyamide
MWCNT Multi-walled carbon nanotubes
CF Carbon nanofiber
Hs Scratch hardness
Tm Melting point

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