Composites: Part A 163 (2022) 107272

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Composites Part A
journal homepage: www.elsevier.com/locate/compositesa

A new approach for the reuse of scrap carbon fiber in high-added value
continuous fiber reinforced composite structures
Hürol Koçoğlu a, b, Mehmet Kodal c, d, M. Cengiz Altan e, Babür Özçelik a, f, Güralp Özkoç d, g, *
a
Gebze Technical University, Mechanical Engineering Department, 41400 Kocaeli, Turkey
b
Bolu Abant Izzet Baysal University, Mechanical Engineering Department, 14030 Bolu, Turkey
c
Kocaeli University, Chemical Engineering Department, 41380 Kocaeli, Turkey
d
Nanotechnology Research and Application Center SUNUM, Sabancı University, 34956 Tuzla, İstanbul, Turkey
e
University of Oklahoma, School of Aerospace and Mechanical Engineering, 73019 Oklahoma, OK, USA
f
Konya Technical University, Mechanical Engineering Department, 42250 Konya, Turkey
g
Istinye University, Department of Chemistry, 34010 Zeytinburnu, Istanbul, Turkey

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

Keywords: This study proposes an innovative processing approach for high-added value hybrid fiber-reinforced composite
Carbon fibres (A) structures by reusing scrap carbon fiber (CF). Thermoplastic prepregs were produced via wet-laid method using
Laminates (A) chopped polyamide 6.6 fibers as matrix and short scrap CFs as the reinforcing phase. These prepregs were then
Interface/interphase (B)
hot stacked with woven glass fabrics, forming a novel hybrid lightweight composite laminate. Silane treatment
Compression moulding (E)
was used to improve the adhesion of glass fabric to the novel wet-laid scrap CF/PA6.6 prepregs. Tensile, flexural,
dynamic-mechanical, and morphological properties of the composites were examined to characterize the
effectiveness of the hybridization of short scrap CFs and glass fabric. The results showed that short scrap CF in the
laminates increased the tensile strength up to 30 % and flexural strength up to 60 %. Moreover, silane surface
modification of the glass fabric yielded a 140 % improvement in the flexural strength of scrap CF/PA6.6 prepreg-
glass fabric hybrid laminates.

1. Introduction
The continuous increase in global awareness of the environment and
sustainability has led to stricter environmental regulations. The Euro­
pean Union (EU) has established strict regulations to reduce CO2 emis­
sions and set challenging targets for the automotive and commercial
aviation industries to be implemented in the coming years [1]. In 2021,
the CO2 emissions of all cars were required to reduce by 40 % compared
to the averages of 2015 (Regulation(EU)-2019/63), while the CO2
emissions of airplanes produced after 2024 should be reduced by 20–30
% compared to those recorded in 2014 (EuropeanComission-2014,
Clean Sky2). Reducing part/vehicle weight has appeared to be one of the
most effective methods to overcome these regulations due to its effect on
CO2 emissions and fuel economy [2]. Hence, developing lightweight
composite materials and better product designs have long been a prime
interest in the aerospace and automotive industries [1].
Fiber-reinforced plastic composites (FRPC) have empowered
designers to reach the zero-emission era [3]. Thanks to their outstanding
strength-to-weight ratio, long service life, better wear, and corrosion
resistance, FRPCs have been introduced as an alternative to heavy
metallic materials in diverse applications, particularly automotive,
aerospace, marine, sports equipment, etc., and energy industries [4–7].
Its durability in aggressive conditions at high temperatures and its high
abrasion resistance have distinguished carbon fiber (CF) and carbon
fiber reinforced composites (CFRCs), among others [7]. Although car­
bon fibers have a wide range of usage due to their outstanding proper­
ties, their use is only feasible in high-performance/value applications
since the production of virgin CF (vCF) is energy-intensive and costly
[8]. However, despite the cost-related concerns, the demand for CF has
been projected to grow steadily over the years. The growth in the de­
mand for CF and CFRPs in various industries results in significant
challenges for their recycling and reuse. This high production volume
will likely generate a high level of production scraps and future end-of-
life CFRC waste, and thus, waste management will become increasingly

* Corresponding authors at: Istinye University, Chemistry Department, 34010 Zeytinburnu, Istanbul, Turkey (G. Özkoç). Nanotechnology Research and Application
Center SUNUM, Sabancı University, 34956 Tuzla, Istanbul, Turkey (G. Özkoç).
E-mail address: guralp.ozkoc@istinye.edu.tr (G. Özkoç).

https://doi.org/10.1016/j.compositesa.2022.107272
Received 8 August 2022; Received in revised form 29 September 2022; Accepted 15 October 2022
Available online 20 October 2022
1359-835X/© 2022 Elsevier Ltd. All rights reserved.
H. Koçoğlu et al.
challenging [9]. In the early 2000 s, the commonly used disposal method
for the waste CFs was mostly through landfilling, which could result in
hazardous long-term impacts on the environment [7,10]. However, due
to rising worldwide consciousness and existing government legislation
such as the EU directive 1999/31/EC and EU directive 2000/53/EC, the
reuse of CF waste has gained tremendous attention. Therefore, reusing
low-quality waste fibers or scraps in high-added value applications
would offer a potential solution to waste management and sustainable
use of resources by reducing energy consumption and CO2 emission
[11].
Plastic injection molding is the most common method for reusing this
waste or production scrap fibers [12,13]. However, excessive fiber
bending and breakage triggered by the high shear stresses during pro­
cessing could hamper the effective utilization of CFs [7,9,11]. For this
reason, reusing waste CFs in injection molding and producing high-
valued structural parts would not be feasible for most applications.
During the last decade, thanks to advanced textile technologies, newer
and innovative composite manufacturing methods have been developed
to improve the properties of both waste CFs and discontinuous vCFs. The
dry- and wet-laid methods could be used to prepare hybrid nonwoven
mats, which would be later used in hot-stacking/compression molding
for the rapid fabrication of medium to large composites. However, the
discontinuity of the CFs limits the mechanical properties and prevents
the reutilization of scrap CFs in high-performance structural
applications.
Carding machines have been commonly used to manufacture dry-
laid hybrid nonwovens. CF and thermoplastic fibers are blended and
fed to a carding machine with several metallic strippers and doffer
cylinders during the carding process. At the end of the process, highly
oriented nonwoven structures termed hybrid webs have been obtained
[7]. Nonwoven structures produced by dry laying exhibit nearly aniso­
tropic structure, depending on the machine direction [9]. In the litera­
ture, composite production with hybrid mats has generally been carried
out by stacking and hot pressing. In these studies, waste CF is used
together with fibers such as polypropylene (PP) fiber [14], PET fiber
[15], and PA6 fiber [15]. For example, Wölling et al. obtained a tensile
strength of 151 MPa with PP fiber [14], while Manis et al. obtained a
flexural strength of 405 MPa in the composites produced with PA6 fiber
[15]. In another study, Xiao et al. brought a different approach by
applying stretching to nonwoven structures obtained by the dry-laid
method using short virgin CF and thermoplastic fiber having PA6.6
core and PA6/PP copolymer shell. They observed that the flexural
strengths of the composites produced were over 800 MPa and the tensile
strengths were over 450 MPa [16].
The hybrid yarn spinning method, another textile technology, starts
with mixing two different fibers in a carding machine to manufacture
hybrid nonwoven webs similar to the dry-laid method [7,9]. Then,
carded webs are converted to hybrid slivers. Subsequently, the slivers
are transformed into hybrid yarns after a series of drafting, drawing, and
spinning processes [17,18]. Then, these hybrid yarns were wound on a
frame and hot pressed to obtain unidirectional composites [5,17–20].
Among these studies on hybrid yarn manufacturing, Hasan et al. reached
a tensile strength of 1030 MPa with waste CF and PA6 fibers [17], and
Hengsterman et al. obtained a tensile strength of 1110 MPa and flexural
strength of 738 MPa with the waste CF and PA6 fibers [19].
Despite the promising results, especially of the hybrid yarn spinning
method, the fact that the carding machine is not suitable for working
with fiber lengths of 30 mm or less creates an important limitation for
these two methods. In addition, wrapping the yarns on the frame limits
the production of geometrically complex parts with the spinning
method. Unfortunately, obtaining fibers over 30 mm is not possible in
most recycling processes. Therefore, innovative processing methods for
reusing shorter waste CFs are needed. At this point, the wet-laid method
can be further developed as an alternative. The most common wet-laid
method based on CF is the papermaking process. In this method,
different fibers are mixed and dispersed in water to induce random
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Composites Part A 163 (2022) 107272
orientations, which is more straightforward than the dry-laid method.
After the water is filtered away and the preforms are dried, a nonwoven
structure is obtained [9]. Hybrid nonwovens can be directly hot-pressed
to produce composite laminates. Recent studies have reported the
manufacturing of hybrid nonwoven mats (HNM) produced via CFs and
other types of thermoplastic fibers such as polyamide 6 (PA6) [21,22]
and PP [14,23]. Since discontinuous CFs are used as primary rein­
forcement, the mechanical properties remained modest, often lower
than 200 MPa for tensile strength. Using a woven fabric with a ther­
moplastic/scrap carbon fiber mat and fabricating a ternary composite
laminate will likely result in much higher mechanical properties. Hence,
it would be possible to utilize scrap CFs for high-performance structural
applications.
This study presented a new approach for reusing the short (<30 mm)
scrap CFs to produce structural thermoplastic composites for high-added
value, lightweight applications. A novel approach was developed to
prepare a ternary hybrid thermoplastic composite laminate with woven
glass fabrics and polyamide 6.6/CF prepregs. The polyamide 6.6/CF
thermoplastic prepregs were manufactured through the wet-laid method
before the ternary laminate production. The effect of PA6.6/CF ratio and
glass fabric surface modification on the mechanical and dynamic me­
chanical properties of the composite laminates were investigated with
tensile and three-point bending tests and dynamic mechanical analyses
(DMA). In addition, scanning electron microscopy (SEM) analyses were
carried out to examine the interfacial interactions between the
components.
2. Experimental
2.1. Materials
Unsized, 12-mm-long scrap CFs were obtained from DowAksa
(Turkey). KraTos Mikro PA6.6 fibers (with a length between 6 and 12
mm) as matrix material were kindly provided by Kordsa (Turkey). As the
continuous fiber component, plain-woven E-glass fabric (GF)
(E6CRWR300A with epoxy sizing and 300 g/m2 areal weight) was ob­
tained from Kologlu Kimya (Turkey), a local reseller of Jushi Co. ltd.
(China). Prior to composite manufacturing, this fabric batch was divided
into 150 × 150 mm2 pieces using a cavity-shaped mold template and a
circular utility knife. The physical properties of the fibers used in this
study are given in Table 1. Dynasylan® AMEO 3-aminopropyltriethoxy­
silane (3-APTS) was purchased from Evonik and was used for glass fabric
surface modification.
2.2. Woven glass fabric surface modification
Since the type of surface treatment of the glass fibers is unknown, we
aimed to introduce an amino silane coupling agent onto the fiber sur­
face, which is known to be compatible with the polyamide matrix
[24,25]. Woven glass fabric surface modification was conducted via heat
treatment to remove the existing sizing, then hydrolysis, and silane
treatment (Fig. 1). To remove the existing sizing on the glass fabric, a
heat treatment was applied. During heat treatment, the fabric pieces
were kept at 350 ◦ C [26] for 24 h in an oven and then washed with
distilled water to remove inorganic residues that may occur on the
Table 1
The physical properties of raw materials.
Fiber Density (g/ Fiber diameter Fiber length Sizing type
cm3) (µm) (mm)
Scrap carbon 1.68 ± 0.08 6 ± 0.5 12 without sizing
fiber
PA6.6 fiber 1.14 ± 0.05 54 ± 2.5 6–12 –
Glass fabric 2.54 ± 0.06 15 ± 1.2 continuous epoxy
compatible
H. Koçoğlu et al.
Fig. 1. Process steps of the silane treatment. (For interpretation of the references to colour in this figure legend, the reader is referred to the web version of
this article.)
surface. Simultaneously with heat treatment, a silane coupling agent
solution was prepared with 3-APTS (5 vol% in the solution), ethyl
alcohol (90 vol% in the solution), and distilled water (5 vol% in the
solution). The solution was mixed in a beaker and hydrolyzed for 24 h at
room temperature under continuous mixing. After heat treatment, the
fabrics were soaked in the hydrolyzed silane solution for 24 h to perform
the silanization reaction between silane molecules and glass fiber (see
Fig. 2). The silane-treated fabrics were then removed from the solution,
rinsed with distilled water to remove excess solvent and unbound silanes
that might be present on the fabric surface, and left to dry in an oven at
80 ◦ C for 24 h to crosslink the silanes on the glass surface.
2.3. Preparation of the thermoplastic PA6.6/CF prepregs (TPP)
The production of the TPP was schematically given in Fig. 3. 12 mm
chopped CFs as the reinforcement and 12 mm long PA6.6 fibers as the
matrix were used for the TPP production based on the wet-laid method.
Fig. 2. (a) Hydrolysis reaction mechanism, (b) Illustration of the functionalized glass fiber surface. (For interpretation of the references to colour in this figure
legend, the reader is referred to the web version of this article.)
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Composites Part A 163 (2022) 107272
The fibers of PA6.6 and CF were mixed in water using the following CF
weight ratios, 0 %, 10 %, 20 %, and 30 %. For each prepreg batch, the
total fiber-to-water ratio was 6 g/600 cc. The follow-on mixing process
was carried out at 9000 rpm for 10 min with the help of a disperser
(VMA-GETZMANN), ensuring the homogeneous distribution of CFs
throughout the TPP structure. This mixture was then poured into a metal
container (150 × 150 mm2) having a 300-mesh sieve at the bottom, and
the water was drained. The drained water was reused for repeated
production. Then, the filtered fiber mixture was laid on waxed paper and
kept in an oven at 80 ◦ C for 24 h for drying. Consequently, the 266 g/m2
TPP was separated from the paper to be used for the subsequent com­
posite fabrication step.
2.4. Manufacturing of the sheets and composite laminates
In this study, three groups of composites with different material
compositions were fabricated. The first group, called sheets (S), contains
H. Koçoğlu et al.
Fig. 3. Preparation stages of the thermoplastic PA6.6/CF prepreg. (For interpretation of the references to colour in this figure legend, the reader is referred to the
web version of this article.)
PA6.6 or PA6.6/CF. The second group, referred to as composite lami­
nates (C), contains PA6.6/glass fabric without CF, and the third group,
referred to as hybrid composite laminates (H), contains PA6.6/CF/glass
fabric. All these samples were manufactured by hot stacking in a
150x150 mm2 aluminum mold cavity placed in a hot press. The sche­
matic representation of composite laminate manufacturing is given in
Fig. 4. For hybrid composite laminates, seven woven glass fabrics and
eight TPPs staked in alternating order were used. Mold cavity height is
provided by a 2.5 mm spacer placed between female (lower) and male
(upper) mold parts.
Before composite laminate manufacturing, glass fabrics and prepreg
mats were stacked to prepare the preforms, as shown in Fig. 4. Then,
these preforms were laid on waxed paper and dried in an oven at 80 ◦ C
for 24 h to remove any possible moisture. After drying, a silicone
lubricant was applied to the upper and lower surfaces of the aluminum
mold and preforms were placed in the mold cavity. During hot-pressing,
the contact between the mold and press surfaces was first held until the
press temperature reached 270 ◦ C, leading to the homogeneous tem­
perature distribution. Depending on the material composition, this
dwell time varied between 10 and 12 min. Then, compression molding
was performed at 270 ◦ C under 60 bar pressure for 2 min. Afterward, the
composite laminates were cooled to 25 ◦ C under pressure in the mold.
The recipes for the manufactured sheets and laminates are presented
in Table 2. In addition, the laminate nomenclature used in the study is
shown in Fig. 5.
2.5. Characterization
2.5.1. FTIR analysis
Fourier transform infrared (FTIR) spectroscopy analyses were used to
confirm the silane bonding on the GF surface. PerkinElmer Spectrum
100 FTIR spectrometer was employed to analyze the surface chemistry
of the de-sized and silane-treated glass fiber fabrics. All the spectra were
recorded with a wavelength between 4000 and 650 cm− 1.
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Composites Part A 163 (2022) 107272
2.5.2. Void content and fiber volume fractions
The actual matrix, GF, CF, and void contents of the laminates and
sheets were determined according to ASTM D2734 test method. The
void content (vol%) of samples was calculated as follows:
( ( ))
ρ mc mg mp
Void content = 100 × 1 − com + + (1)
mcom ρc ρg ρp
to calculate the weights of composites (mcom), all specimens were first
weighted by a precision balance and heated to 500 ◦ C for two hours to
complete the ignition of the PA6.6 matrix. Then the samples were
weighed again, and the weight of the PA6.6 matrix (mp) was calculated.
After this point, the CF and GF layers were separated and weighed (mc
and mg). The density of the composites (ρcom) was measured by an
electric densimeter (Mettler Toledo XS204 model). The density of CF
(ρc), GF (ρg), and PA6.6 (ρp) were supplied by the manufacturers. To
calculate the volume fraction of CF (Vc), GF (Vg), and total fibers (VT),
Eq. (2) was used.
mc /ρc mg /ρg
Vc = 100 × ; Vg = 100 × ; VT = Vc + Vg (2)
mcom /ρcom mcom /ρcom
2.5.3. Characterization of mechanical properties and fracture morphology
Test samples were prepared using a water jet, as can be seen in Fig. 6,
to investigate the mechanical properties of all laminates and sheets
manufactured (Table 2). The water jet method was chosen to avoid in­
ternal damage to the specimens.
Llyod Instruments LRX plus test machine was used to perform three-
point bending tests. The tests were conducted according to the ASTM D-
790 standard, and a 2 mm/min displacement rate was used. The di­
mensions of the specimens are given in Fig. 6a. The support span was set
to 16 times the laminate thickness. For all specimen codes (Table 2), 30
samples cut from 3 sheets/laminates were tested for three-point bending
experiments.
Tensile tests were performed by Instron 6800 universal test machine
with 50 kN capacity. The test configuration was arranged according to
ASTM D-3039, and the specimen dimensions were adjusted as in Fig. 6b.
H. Koçoğlu et al. Composites Part A 163 (2022) 107272

Fig. 4. Schematic illustration of laminate manufacturing. (For interpretation of the references to colour in this figure legend, the reader is referred to the web version
of this article.)

In addition, a crosshead speed of 2 mm/min was used for all samples.

Table 2
The tensile test was applied on 12 samples cut from 3 plates/laminates
The recipes of the manufactured sheets and laminates.
for each sample code in Table 2.
Specimen Materials Matrix CF GF surface After mechanical tests, failure surfaces of the tensile test specimens
codes (wt%) modification
underwent SEM observations to explain the damage mechanisms and to
Sheets S00 PA6.6 0 – observe the compatibility between the components. The morphological
S10 PA6.6/CF 10 –
observations were performed using QUANTA FEG 450 model SEM at 15
S20 PA6.6/CF 20 –
S30 PA6.6/CF 30 –
kV voltage. The samples were gold coated to prevent arching before
testing.
Comp. CA PA6.6/GF 0 As-received
Laminates CD PA6.6/GF 0 De-sized 2.5.4. Dynamic mechanical analyses
CS PA6.6/GF 0 Silanized The dynamic mechanical characteristics of all samples were obtained
with Metravib DMA50 dynamic mechanical analyzer. The test samples
Hybrid Comp. H10A PA6.6/CF/ 10 As-received were cut by a water jet for DMA analyses to get proper test dimensions,
Laminates GF as shown in Fig. 6c. The DMA tests were performed dual cantilever mod
H20A PA6.6/CF/ 20 As-received (Fig. 6c) at 3 Hz frequency and between 20 and 200 ◦ C with a 10 ◦ C/min
GF
heating rate.
H30A PA6.6/CF/ 30 As-received
GF
H10S PA6.6/CF/ 10 Silanized 3. Results and discussion
GF
H20S PA6.6/CF/ 20 Silanized FTIR measurements were carried out on pure silane, heat-treated
GF
(de-sized), and silane-treated (silanized) glass fabrics. FTIR analyses
H30S PA6.6/CF/ 30 Silanized
GF were carried out to confirm the removal of the organic sizing from the
fabric surface by the heat-treatment and the success of the fabric surface
CF: scrap, discontinuous carbon fibers.
modification by the silanization process. As shown in Fig. 7, the ab­
GF: plain woven glass fabric.
sorption bands located at 1200 to 800 cm− 1 were Si-O- bonds in the de-
sized glass fiber structure [27]. The peak of 3374 cm− 1 for the pure

5
H. Koçoğlu et al. Composites Part A 163 (2022) 107272

Fig. 5. Nomenclature examples of the composite sheet, composite laminate, and hybrid composite laminates. (For interpretation of the references to colour in this
figure legend, the reader is referred to the web version of this article.)

Fig. 6. Dimensions of test specimens for (a) three-point bending, (b) tensile testing, and (c) dynamic mechanical analyses. (For interpretation of the references to
colour in this figure legend, the reader is referred to the web version of this article.)

silane spectrum and the absorption band between 3200 and 3500 cm− 1
for silanized glass fabric spectrum indicated the presence of the amine
group (NH2) [28]. In addition, another characteristic peak of the amine
group was observed at about 1635 cm− 1 on the spectrum of the pure
silane and silanized glass fabric [29]. Other prominent peaks were
detected at 2925 cm− 1 and 2858 cm− 1 for silane-treated glass fabric.
These peaks resulted from the stretching vibrations of the methylene
group (CH2) and methyl group (CH3), respectively [26,30,31]. When the
FTIR spectra of de-sized and silanized glass fabrics are compared, it is
confirmed that the silanization process has been carried out successfully.
The void fraction and total fiber volume fractions of sheets (con­
taining PA6.6 or PA6.6/CF) and laminates (containing PA6.6/GF or
PA6.6/CF/GF) are summarized in Table 3. The results of the GF volume
fraction showed that all three composite laminates had almost identical
vol% GF content. As expected, the heat and silane treatment did not
influence the GF volume fraction of the composite laminates. Moreover,
the CF and GF volume fractions of composite and hybrid composite
laminates with the same CF content were found to be similar. On the
other hand, some differences in the void volume fraction were detected
as the CF content increased from 10 to 30 wt%, as seen in Table 3. The
void fraction results revealed that the silane treatment reduces the void
volume fractions of hybrid composite laminates for any given mixing
ratio, which can be attributed to the enhanced possible covalent and/or
physical interfacial interaction between the silanized glass fiber surface
and PA6.6 [24]. These findings are also supported by SEM analyses, as
discussed later.
Fig. 8 shows the change in tensile strength and elastic modulus with
respect to the CF content and the glass fabric surface modification type.
The tensile test results are summarized in Table 4, and the tensile
stress–strain curves of the specimens are illustrated in Fig. 9. Tensile test
results of sheets revealed that the increasing CF content in the matrix
increases the tensile strength and elastic modulus as expected. Among
all sheets, S30 has the highest tensile strength of 212.0 MPa and the
highest elastic modulus of 5.41 GPa. Contrary to the tensile strength and
elastic modulus results, the elongation at break decreased dramatically
in the presence of CF. Therefore, the addition of CF contributed to the
tensile strength and the modulus of PA6.6 considerably. These results
indicate that the mixing of the PA6.6 and CF in an aqueous solution was
successful in obtaining a homogeneous fiber dispersion suitable for
subsequent compression molding. Moreover, as shown in Fig. 9a, CF-
reinforced PA6.6 composite sheets exhibited brittle failure as ex­
pected. On the other hand, plastic deformation is much easier for neat

6
H. Koçoğlu et al. Composites Part A 163 (2022) 107272

compared to their as-received counterparts. For instance, composite

Fig. 7. FTIR spectra of pure silane, heat-treated (de-sized), and silane-treated
glass fabrics. (For interpretation of the references to colour in this figure
legend, the reader is referred to the web version of this article.)
PA6.6 compared to composite sheets since the elastic modulus of CF is
higher than PA6.6 [32]. Besides, it was observed that the elongation at
break values did not change as the CF fiber loading level increased. In
this study, the tensile test results for CF-reinforced PA6.6 sheets are
comparable with the literature. For instance, You et al. [33] prepared
PA6.6/CF composites in the presence of 1 wt% multi-walled carbon
nanotube by conventional methods (melt blending and injection mold­
ing). They observed that injection molded PA6.6/CF composites yielded
similar results where an increase from 100 MPa to 181 MPa in the tensile
strength was observed with the increase in CF content from 10 wt% to
30 wt%. In an industrial-based study, ELG Carbon Fiber has developed
several recycled carbon fiber products via carding line processes to meet
the market’s needs. They observed that the tensile strength of recycled
CF-reinforced PA6.6 composites increased from 177.9 MPa to 217.1
MPa as the recycled CF content increased from 30 to 40 wt% [34], which
was consistent with the results of our findings for PA6.6/CF sheets.
The tensile test results also indicated that silanized glass fabric-
reinforced composites substantially improved tensile properties
laminates containing as-received glass fabric (CA) have 277.7 ± 21.1
MPa tensile strength, whereas, after the silanization process, the tensile
strength increased by 21 % to 336 MPa. Elongation at break values of the
composite laminates also improved after GF silanization by up to 15 %
(Fig. 9b). These improvements could be attributed to the formation of
the interphase between glass and PA6.6, which resulted from the
chemical interactions between –COOH groups of PA6.6 and –NH2
group of 3-APTS. Thus, the breakdown of the fiber-polymer interphase
was delayed [35]. In addition, the elastic modulus of the composite
laminates was also enhanced to 5.85 GPa, representing a 10 % increase
after silanization. This can be attributed to the immobilization of PA6.6
chains onto the high-modulus fiber surfaces, allowing a more efficient
homogenous stress transfer and distribution within the interphase.
Similar improvements in tensile properties of silane-treated fiber rein­
forced PA6.6 can be found in the literature [36,37]. Yu et al. [36]
investigated the effect of amino-silane treatment with different amino
groups for basalt fibers on the mechanical properties of PA6.6 com­
posites. The authors found 90.91 MPa tensile strength of de-sized basalt
fiber reinforced composites. On the other hand, silanization of basalt
fibers enhanced the tensile strength values by up to 30 %. In another
study [37], the surface of basalt fiber treated with two types of alkoxy
silanes (N-(2-aminoethyl)-3-aminopropyltrimethoxysilane and 3-(tri­
methoxysilyl) propylsuccinic anhydride) to balance the stiffness and
toughness ratio of styrene-ethylene/butylene-styrene (SEBS) toughened
PA6.6. 3-(trimethoxysilyl) propylsuccinic anhydride-silanized basalt
fiber showed improved interfacial interaction between the basalt fiber
and PA6.6, resulting in a further increase in the tensile strength to
111.94 MPa.
A similar trend for mechanical properties was observed in hybrid
composite laminates except for H30A and H30S (Table 4). Both elastic
modulus and tensile strength values of hybrid composite laminates
increased as the CF content increased from 10 to 20 wt%, achieving their
highest level of 6.56 GPa and 378.5 MPa, respectively, for the 20 wt%
CF. On the other hand, a decline in mechanical properties of hybrid
composite laminates was observed for 30 wt% CF loading level (H30A
and H30S) (Figs. 8, 9c, and d) due to the lack of fiber wetting at this
higher fiber content, evidenced by the increasing void fraction in the
composite laminates [23].
Furthermore, it was found that hybrid composite laminates exhibited
higher tensile properties compared to the PA.6.6/glass fabric composite

Table 3
Fiber and void volume fractions of sheets, composite, and hybrid composite laminates.
Laminate Materials Void content (vol CF volume fraction (vol GF volume fraction (vol Total fiber volume fraction (vol
codes %) %) %) %)

Sheets S00 PA6.6 4.7 ± 0.4 – – –

S10 PA6.6/CF 5.5 ± 0.2 6.5 ± 0.6 – 6.5 ± 0.6
S20 PA6.6/CF 4.5 ± 0.3 13.7 ± 0.6 – 13.7 ± 0.6
S30 PA6.6/CF 5.5 ± 0.2 20.2 ± 0.2 – 20.2 ± 0.2

Comp. Laminates CA PA6.6/GF 5.7 ± 0.9 – 31.9 ± 0.6 31.9 ± 0.6

CD PA6.6/GF 5.3 ± 1.0 – 31.7 ± 0.7 31.7 ± 0.7
CS PA6.6/GF 5.0 ± 1.4 – 31.0 ± 0.6 31.0 ± 0.6

Hybrid Comp. H10A PA6.6/CF/ 4.0 ± 1.2 3.6 ± 0.4 31.6 ± 1.0 34.7 ± 0.9
Laminates GF
H20A PA6.6/CF/ 5.5 ± 0.5 6.5 ± 0.8 30.7 ± 0.6 37.0 ± 1.3
GF
H30A PA6.6/CF/ 6.8 ± 1.9 12.7 ± 0.5 27.0 ± 0.7 39.6 ± 0.9
GF
H10S PA6.6/CF/ 2.8 ± 1.0 3.8 ± 0.3 30.8 ± 0.5 34.7 ± 0.5
GF
H20S PA6.6/CF/ 3.7 ± 0.5 6.7 ± 0.8 30.2 ± 0.8 37.5 ± 0.7
GF
H30S PA6.6/CF/ 5.9 ± 1.1 12.7 ± 0.5 27.7 ± 0.9 40.5 ± 0.9
GF

7
H. Koçoğlu et al. Composites Part A 163 (2022) 107272

Fig. 8. Tensile strength and modulus of sheets, composite, and hybrid composite laminates. (For interpretation of the references to colour in this figure legend, the
reader is referred to the web version of this article.)

Table 4
Tensile and flexural properties of sheets, composite, and hybrid composite laminates.
Laminate codes Tensile strength (MPa) Elastic modulus (GPa) Elongation at break (%) Flexural strength (MPa) Flexural modulus (GPa)

Sheets S00 63.7 ± 4.0 0.76 ± 0.03 84.6 ± 5.9 97.0 ± 2.0 2.45 ± 0.23
S10 98.7 ± 7.2 2.67 ± 0.08 3.8 ± 0.5 178.2 ± 13.0 6.23 ± 0.52
S20 162.9 ± 2.3 4.13 ± 0.08 4.3 ± 0.4 243.2 ± 12.0 9.05 ± 1.28
S30 212.0 ± 3.4 5.41 ± 0.23 4.9 ± 0.7 283.4 ± 9.4 11.08 ± 1.29

Comp. Laminates CA 277.7 ± 21.1 5.32 ± 0.34 7.5 ± 0.5 150.3 ± 13.5 9.28 ± 0.73
CD 282.7 ± 23.6 5.61 ± 0.24 7.7 ± 0.6 288.2 ± 22.4 11.51 ± 0.59
CS 336.0 ± 22.5 5.85 ± 0.20 8.6 ± 0.6 356.4 ± 27.5 13.14 ± 0.62

Hybrid Comp. Laminates H10A 285.8 ± 18.2 5.64 ± 0.30 8.2 ± 0.6 225.7 ± 28.2 12.41 ± 0.95
H20A 344.2 ± 15.9 6.43 ± 0.13 7.6 ± 0.9 239.4 ± 24.0 13.91 ± 1.08
H30A 288.5 ± 13.8 6.27 ± 0.16 7.7 ± 0.5 231.5 ± 24.7 13.29 ± 1.31
H10S 352.4 ± 13.1 6.04 ± 0.12 7.8 ± 0.9 499.3 ± 17.9 14.74 ± 0.85
H20S 378.5 ± 15.4 6.56 ± 0.11 6.7 ± 0.6 567.4 ± 29.9 20.29 ± 0.94
H30S 375.0 ± 17.2 6.13 ± 0.10 7.2 ± 0.4 531.3 ± 23.2 16.53 ± 1.03

laminates without CFs. These results indicate the successful hybridiza­
tion of conventional, compression molded composites and demonstrate
the feasibility of using short, scarp CFs together with glass fabrics as
reinforcement to achieve higher structural performance. For instance,
277.7 MPa tensile strength of CA escalated to higher values in H20A
laminates (344.2 MPa, 24 % improvement), as can be seen in Fig. 9b and
c. In addition, similar enhancement in mechanical properties was ob­
tained for silane treated hybrid laminates. The highest tensile strength of
378.5 MPa was achieved by H20S, representing a 13 % improvement
over CS (Fig. 9b and d). Similarly, the silane treatment of the glass fabric
also made a noticeable impact on the tensile strength and elastic
modulus of hybrid composite laminates for each CF ratio (Fig. 9c and d).
The macro image of the fracture surfaces formed after the tensile
failure of the CA, CD, CS, H20A, and H20S laminates are shown in
Fig. 10. For the composite laminates of CA, CD, and H20A containing as
received or de-sized glass fabrics exhibited a pronounced fiber pull-out
together with remarkable matrix cracks. On the other hand, the com­
posite laminates composed of silanized glass fabrics (i.e., CS and H20S)
had mostly simultaneous fiber–matrix failure that suggested better
interfacial bonding, as discussed earlier.
The 3-point bending tests were also carried out since they reveal a
clearer picture of the mechanical properties of the interior layers and the
surface. Flexural strength is the ability of the composites to withstand
bending forces applied perpendicular to their longitudinal axis. The
average flexural strength and flexural modulus values obtained from the
3-point bending tests are given in Table 4. The three-point bending test
results for each sheet and composite are shown in Fig. 11. Moreover, the
typical flexural stress–strain curves for sheets, composite laminates, and
hybrid composite laminates are illustrated in Fig. 12.
As can be seen from Fig. 11 and Table 4, the highest flexural prop­
erties among sheets were obtained for S30 (283.4 MPa of flexural
strength and 11.08 GPa of the flexural modulus) containing 30 wt% CF.
Moreover, as expected, a steadily increasing trend was obtained with
increased CF content on the flexural strength and modulus.
De-sizing and silane treatment applied to glass fiber fabrics increased
the flexural strength and modulus (Fig. 12b). It was found that the
flexural strength of CD produced with heat-treated fabrics increased by
91.7 % by reaching 288.2 ± 22.4 MPa, compared to CA. Besides, sila­
nization further increased the flexural strength to 356.4 MPa (137.1 %
increase) of composite laminates. Compared to the CA, a similar sig­
nificant improvement was also obtained in the flexural modulus in both
CD and CS samples, in agreement with the literature. For example, Kiss
et al. manufactured composite laminates by compression molding of
PA6 films stacked with glass fabrics having different surface modifica­
tions. They stated that amino silane-treated glass fabric reinforced
laminates exhibited nearly-three times higher flexural properties (519.8
MPa) than de-sized glass fabric ones [38]. In a recently published study,
the effects of different silane coupling agents (3-(methacryloxy) pro­
pyltrimethoxy silane (3-MPS), 3-(glycidyloxy) propyltrimethoxy silane
(3-GPS), and 8-(methacryloxy) octyltrimethoxy silane (8-MOTS))
modified glass fibers on the mechanical properties of dental resin
composites were studied by Thadathil Varghese et al. [39]. The authors
found the least flexural strength of dental composites in the presence of
unsilanized etched fibers; however, silanization of glass fiber

8
H. Koçoğlu et al. Composites Part A 163 (2022) 107272

Fig. 9. Tensile stress-elongation curves of (a) sheets, (b) composite laminates, (c) hybrid composite laminates with as-received glass fabrics, and (d) hybrid composite
laminates with silane-treated glass fabrics. (For interpretation of the references to colour in this figure legend, the reader is referred to the web version of this article.)

Fig. 10. Macro images of the tensile test specimen’s failure zones.

Fig. 11. Flexural strength and modulus of sheets, composite, and hybrid composite laminates. (For interpretation of the references to colour in this figure legend, the
reader is referred to the web version of this article.)

9
H. Koçoğlu et al. Composites Part A 163 (2022) 107272

Fig. 12. Typical flexural stress–strain curves of (a) sheets, (b) composite laminates, (c) hybrid composite laminates with as-received glass fabrics, and (d) hybrid
composite laminates with silane-treated glass fabrics. (For interpretation of the references to colour in this figure legend, the reader is referred to the web version of
this article.)

significantly enhanced the flexural properties of dental composites,
regardless of silane type. In another recent study, Cho et al. [40]
investigated the influence of surface modification of S-glass fibers on the
mechanical properties of a dental resin, a mixture of urethane dime­
thacrylate and triethylene glycol dimethacrylate monomers. A selective
atomic level metal etching process and silanization process were used to
surface modification of glass fibers. The flexural strength of dental resin-
based composites improved after the silanization of glass fibers with an
elective atomic level metal etching process. All these findings in the
literature are evidence of improvement in the mechanical properties of
polymer composites having silanized glass fiber materials, which is
consistent with our results.

Fig. 13. Macro images of the flexural test specimen’s failure zones (a) CA, (b) CS, (c) H20A, (d) H20S.

10
H. Koçoğlu et al.
According to the flexural test results of CF hybridized composites, the
flexural strength increased with CF content up to 20 wt%, while a slight
decrease was observed when CF content was increased to 30 wt%
(Fig. 12c and d). This was due to the insufficient PA6.6 matrix content in
the TPP layers. In hybrid composites laminates, 60 % and 50 % increases
were achieved respectively in flexural strength and modulus for H20A
compared to CA. Similarly, 60 % flexural strength and 55 % flexural
modulus improvements were observed for H20S with respect to CS.
Matrix fiber adhesion is a factor that indirectly affects mechanical test
results. In this context, it may be possible to make some inferences by
examining the failure zones of the samples subjected to three-point
bending [38].
Fig. 13 presents macro images of the three-point bending failure
zones of CA, CS, H20A, and H20S laminates. As can be seen from
Fig. 13a and c, interlaminar delamination was observed in the damaged
region, and micro-buckling was observed on the samples’ compression
side. These failures are due to insufficient fiber–matrix adhesion. When
the adhesion between the fiber–matrix is increased to a sufficient level,
the resistance to micro-buckling increases and the formation of fiber­
–matrix failures can be prevented. On the other hand, no interlaminar
matrix-fiber failure was observed for CS and H20S laminates produced
with silane-treated fabrics (Fig. 13b and d). As can be easily seen from
Fig. 13b and d, sample failure occurred in the tensile region. These
findings can be attributed to the significant improvement in the inter­
facial interaction between glass fiber and matrix.
Surprisingly, the flexural strength of hybrid composite laminates
composed of as-received fabric (H10A, H20A, and H30A) remained
below those of S20 and S30 sheets. Therefore, it can be concluded that
using glass fabric without surface modification is ineffective in hybrid
composites laminates. Knowing that the bending test depends more on
the interlaminar stress transfer than the tensile test, an improved matrix-
fiber interface by appropriate surface treatment is essential in using
hybrid scrap CF/PA6.6 TPP with continuous glass fibers. Imperfections
at the interface or insufficient adhesion between the components can
cause premature delamination and micro-buckling (as can be seen in
Fig. 13a and c), which cause limited load transfer from the matrix to the
glass fabrics under flexural loading.
SEM analyses were conducted to evaluate the fracture surface
morphology and the interfacial behavior of the composites. SEM pic­
tures of composite laminates and hybrid composite laminates were
presented in Figs. 14, 15, and 16, respectively.
As can be seen from Fig. 14a that the glass fiber surfaces are smooth,
clean, and free from any polymeric layers, indicating a poor interfacial
interaction between CA and PA6.6. As a result of this poor interphase,
failure occurred at the interphase, and the polymer matrix was peeled-
off from the surface of the glass fibers. On the other hand, a small
amount of matrix residues was observed on the glass fiber surfaces after
heat treatment (Fig. 14b), which indicates that the failure occurred in
the matrix rather than the interphase due to the limited fiber/matrix
interaction. After the silanization process, the surface of glass fabrics
was completely covered by a sheath of PA6.6, indicating a much-
improved interfacial interaction between the components (Fig. 14c).
Fig. 14. SEM images of the tensile fractured surfaces of (a) CA, (b) CD, and (c) CS laminates.
11
Composites Part A 163 (2022) 107272
SEM images of the H20S hybrid composite laminate having silane-
treated glass fabric at low magnification are shown in Fig. 15a and b.
In Fig. 15a, it is seen that the adhesion between the layers of CF/PA6.6
and glass fabric has good adhesion. PA6.6 matrix in the CF/PA6.6 layer
has diffused between the individual glass fibers during compression
molding and could wet all fiber tows, ensuring good adhesion and
structural integrity of the layers. In addition, the SEM image (Fig. 15b)
taken from the CF/PA6.6 layer of the same laminate shows that the CFs
are generally randomly distributed in the composite and are embedded
in the matrix. The interphase between the CF and PA6.6 is seemed to be
compatible, as revealed by the excellent wetting of PA6.6.
SEM images of the glass fabric regions of all hybrid composite lam­
inates are presented in Fig. 16. As shown in Fig. 16a, c, and e, the glass
fibers are stripped from the matrix, creating widespread fiber pull-out
due to the poor adhesion between the fabric and the polymer matrix.
These results reveal the cause of micro-buckling failures between glass
fabric and TPP observed in laminates produced with as-received glass
fabric, especially during the three-point bending test (Fig. 13a and c). On
the contrary, a significant amount of matrix residue was detected on the
glass fiber surfaces in the failure zone (Fig. 16b, d, and f), indicating
improved interfacial interaction and mechanical properties in the
presence of a silane coupling agent. The excellent adhesion between the
glass fiber–matrix observed in the SEM images confirms the images
obtained in the three-point bending test damage region (Fig. 13b and d).
DMA is generally used to examine the fiber–polymer matrix interface
in a fiber-reinforced polymer material. DMA analyses performed in dual
cantilever mode were applied to all samples in this study. The variations
of storage modulus (E’) and tanδ values depending on temperature were
given in Fig. 17.
E′ is essentially an indicator of the carrying capacity of materials
[41]. For materials with similar manufacturing conditions, E’ is ex­
pected to be directly proportional to the interface strength of fiber-
reinforced composites. As the transfer of stress from the matrix to the
fibers improves with the increase of interfacial adhesion, the E’ value
can be expected to increase [42–44] due to the more rigid structure of
the matrix. It is also possible to make inferences about the fiber–matrix
interface strength with tanδ, which is the loss and storage modulus ratio,
also called the damping factor. Moreover, tanδ is a sensitive indicator
affected by molecular motions; it indirectly expresses the amount of
damping of the mechanical energy on the material [45]. The magnitude
of the tanδ is inversely proportional to interfacial adhesion. The weak
adhesion between the fiber–matrix can cause more mechanical energy
dissipation due to the frictions formed at the interface [42,45]. More­
over, the temperature of the tanδ curve’s peak gives the material’s glass
transition temperature (Tg).
As shown in Fig. 17a, adding CF to neat PA6.6 increased E’ and
decreased the magnitude of tanδ, correspondingly decreasing dissi­
pating mechanical energy. The DMA results indicated that the presence
of CF improves the materials’ stiffness via the CF reinforcement effect.
Furthermore, the tanδ curves also shifted to higher temperatures with
increasing CF content. It can be concluded that the Tg values of the
sheets increased with increasing CF content due to the restriction of the
H. Koçoğlu et al. Composites Part A 163 (2022) 107272

Fig. 15. SEM images of H20S (a) all layers, (b) CF/PA6.6 region.

Fig. 16. SEM images of the tensile fractured surfaces of (a) H10A, (b) H10S, (c) H20A, (d) H20S, (e) H30A, and (f) H30S hybrid composite laminates.

12
H. Koçoğlu et al.
Fig. 17. Storage modulus and tan δ results of (a) sheets, (b) composite laminates, (c) hybrid composite laminates with as-received glass fabrics, and (d) hybrid
composite laminates with silane-treated glass fabrics. (For interpretation of the references to colour in this figure legend, the reader is referred to the web version of
this article.)
CFs on polymer chain mobility.
It can be pointed out from Fig. 17b that surface modifications of glass
fabrics improved E’ values and lowered the magnitude of tanδ compared
to as-received composite laminates. Over the range of temperatures
investigated, silane-treated composite laminates (CS) exhibited the
highest storage modulus compared to the other composite laminates.
The superior properties of CS laminates can be attributed to the strong
fiber–matrix interfacial interaction, which leads to enhanced stress
transfer from the matrix to the fibers [42]. These findings corroborate
mechanical test results, macro-images, and SEM observations, as
mentioned before.
As the dynamic-mechanical behavior of hybrid composite laminates
is investigated (Fig. 17c and d), similar storage modulus and tanδ vari­
ation were observed depending on the CF loading level. The highest
storage modulus was obtained at 20 wt% CF content in both as-received
and silane-treated hybrid composite laminates. However, the tanδ of
materials did not change as the CF content increased. Besides, a
threshold region was observed regarding the storage modulus of the
hybrid composite laminates. The storage modulus of hybrid composite
laminates increased with CF loading to 20 wt% and decreased beyond
that content.
The hybridization of glass fabric with scrap CF/PA6.6 laminates
resulted in an impressive effect on the mechanical properties of samples.
For instance, hybridization increased the storage modulus by ~50 %
compared to composite laminate samples without carbon fibers. When
the storage modulus of the hybrid composite laminates is compared in
terms of surface modification, silane-treated hybrid composite laminates
showed higher modulus than their as-received counterparts, as well as a
significant decrease in tanδ amplitudes (Fig. 17c and d). This decrease in
tanδ magnitude indicates that silanization of glass fabrics significantly
increased the interface quality of hybrid composite laminates.
13
Composites Part A 163 (2022) 107272
4. Conclusion
This study showed that the scrap CFs shorter than 30 mm could be
effectively utilized in high-added value continuous fiber-reinforced
composite laminates via a novel processing method. The new method
first fabricates the wet-laid prepregs of scrap short CFs and PA6.6 fibers,
which are subsequently hot-stacked with a conventional glass fiber
fabric and compression molded. Compared to conventional injection
molding or spinning, the new approach developed in this study has
considerable advantages, such as the utilization of shorter scrap carbon
fibers in structural parts, ease of operation, and low tooling cost.
Moreover, composite parts of the desired thickness or carbon fiber
composition can be produced in one step by the traditional hot-stacking
method, resulting in design flexibility in part performance and
geometry.
The mechanical properties of the laminates produced with TPP with
CF at 20 % by weight, independent of the glass fabric surface modifi­
cation, provided the highest increase in flexural and tensile properties.
The addition of CFs resulted in flexural and tensile strength values as
high as 567.4 MPa and 378.5 MPa, representing improvements of 60 %
and 30 %, respectively. Surprisingly, flexural properties of hybrid
composite laminates without silanization exhibited lower flexural
strength values than PA6.6/CF sheets. On the other hand, the silaniza­
tion of glass fabrics significantly affected the mechanical properties of
hybrid laminates. It was found that the silanized hybrid composites
laminates with 20 wt% carbon fiber nearly have a flexural strength of
600 MPa, close to the flexural strength of structural parts used in
aerospace and automotive applications. It is observed that the best
performance is achieved with 20 wt% carbon fibers. The mechanical
properties slightly decreased after further increasing carbon fiber con­
tent to 30 wt%. The reason for this decrease could be the amount of
PA6.6 being insufficient for completely wetting the carbon and glass
fibers hence if the PA6.6 prepregs are fabricated with higher areal
H. Koçoğlu et al.
densities, the hybrid laminates with more than 20 wt% carbon fibers can
be effectively used, resulting in even higher performance.
CRediT authorship contribution statement
Hürol Koçoğlu: Investigation, Visualization, Methodology, Writing
– original draft. Mehmet Kodal: Visualization, Writing – review &
editing, Methodology. M. Cengiz Altan: Conceptualization, Writing –
review & editing, Methodology. Babür Özçelik: Supervision, Writing –
review & editing, Methodology. Güralp Özkoç: Supervision, Concep­
tualization, Writing – review & editing, Methodology.
Declaration of Competing Interest
The authors declare that they have no known competing financial
interests or personal relationships that could have appeared to influence
the work reported in this paper.
Data availability
Data will be made available on request.
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