Original Article

High Performance Polymers

1–10
Enhancing the mechanical properties ª The Author(s) 2021
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of SCF/PEEK composites in FDM via sagepub.com/journals-permissions

DOI: 10.1177/09540083211003654
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process-parameter optimization

Bin Hu1,*, Zehua Xing1,*, Weidong Wu1, Xiaojun Zhang2,

Huamin Zhou1, Chun Du1 and Bin Shan1

Abstract
Short-carbon-fiber (SCF)–reinforced poly-ether-ether-ketone (PEEK) is a promising polymer composite material with
good biocompatibility, a high strength-to-weight ratio, and low friction properties. In artificial-bone fabrication and other
applications with more flexible fabrication demands, fused-deposition modeling (FDM) technology enables the rapid and
low-cost fabrication of SCF/PEEK parts with sophisticated structures. Owing to the high viscosity of melting PEEK
composites, great challenges, associated with the poor internal interface, need to be overcome before enhanced
mechanical properties can be obtained. In this study, key processing parameters and various SCF amounts were studied to
investigate their effects on the mechanical properties of PEEK composites. It was revealed that the existence of voids and
gaps between the SCF and PEEK led to a decrease in the strength of the composite systems. The FDM processing
parameters were tuned to eliminate these defects in the PEEK composites. The tensile strength of the 2% SCF/PEEK
sample reached 96.4 MPa, which is comparable to that of PEEK parts prepared by injection molding. Meanwhile, its elastic
modulus reached 2.6 GPa, which is 169% higher than that of the bare PEEK sample.

Keywords
PEEK composites, short carbon fibers, fused-deposition modeling, processing parameter

Introduction While carbon-reinforced PEEK-polymer printing via

As a high-performance composite polymer, carbon-fiber
(CF)/poly-ether-ether-ketone (PEEK) not only maintains
the high temperature-resistance and corrosion-resistance
properties of bare PEEK material, but it also has higher
strength than bare PEEK.1–5 It has been widely used in
various applications, e.g. artificial-bone fabrication and
aerospace-part manufacturing.6–11
At the current stage, common methods of fabricating CF/
PEEK composites include solid-state thermoforming, com-
mingled prepregs with continuous CF, and plain-weave CF
fabrics and laminates. However, these fabrication methods
are limited in terms of rapid prototyping, and a more flexible
fabrication technology is needed to meet the demand.12–15
Additive manufacturing (AM) has been considered as a pro-
mising tool that would enable the rapid and low-cost fabrica-
tion of short-carbon-fiber (SCF)/PEEK parts.16–18 As the
most widely utilized AM method,19–21 fused-deposition mod-
eling (FDM) technology can realize the 3D printing of most
thermoplastic materials, including polylactic acid (PLA),
acrylonitrile butadiene styrene (ABS), PEEK, etc.21–24
FDM technology provides some unique opportunities for
the development of personalized PEEK composite prod-
ucts, it presents additional challenges during the fabrication
process. Specifically, the rigid and non-polar molecular
chains of the PEEK matrix exhibit poor wettability and a
weak bonding force with SCF.25–29 Therefore, voids or
gaps are commonly observed in SCF/PEEK composite
material during the filament extrusion, which leads to
stress-concentrate defects and limited mechanical strength
1
State Key Laboratory of Material Processing and Die and Mould
Technology, School of Materials Science and Engineering, Huazhong
University of Science and Technology, Wuhan, People’s Republic of China
2
Wuyi Sting3D Technology Co., Ltd., Jinhua, People’s Republic of China
* Co-first authors of the article.
Corresponding authors:
Chun Du and Bin Shan, State Key Laboratory of Material Processing and
Die and Mould Technology, School of Materials Science and Engineering,
Huazhong University of Science and Technology, Wuhan, People’s
Republic of China.
Emails: duchun@hust.edu.cn; bshan@mail.hust.edu.cn
2 High Performance Polymers XX(X)
in the composite structures.30 In addition, the existence of
SCF changes the melting and solidification characteristics
of PEEK composites, complicating their manufacturing
conditions during FDM printing.2,31
To solve the problems mentioned above, distinct strate-
gies have been designed and implemented in the literature.
For instance, Han et al.14 studied the mechanical properties
and biocompatibility of FDM-printed 5%-SCF–reinforced
PEEK composites with modified post-processing. They
showed that heat-treatment methods could increase the
crystallinity of PEEK and relieve the residual stress, along
with the shrinkage distortion, which ultimately increases
the mechanical performance of printed PEEK parts.
In another effective strategy, Li et al.32 tested the influence
of sanding and plasma treatments on the shear-bond strength
of 3D-printed polyetherimide (PEI), PEEK, and CF/PEEK. It
was concluded that sanding and plasma decreased the contact
angle and increased the surface free energy, which increased
the interlayer bonding strength of the polymers.
Thus far, only a few studies have focused on the influ-
ence of AM process control. Our previous research showed
that extensive shrinkage (about 5%) occurs in PEEK during
FDM fabrication, and its melting state has high viscosity
and poor liquidity.33 The rheological state of the composite
polymer system is highly correlated with the temperature
and PEEK wire pressure during the FDM printing process.
Therefore, a systematic exploration of the printing para-
meters in FDM serves as a straightforward method to
improve the interface between SCF and PEEK.
In this study, SCF/PEEK composite materials with three
different proportions (0%, 2%, and 5%) were prepared.
Subsequently, the effects of key FDM process parameters
and different amounts of SCF in the PEEK composite mate-
rial were systematically evaluated.
Materials and methods
Raw materials and sample fabrication
PEEK granules (grade: ZYPEEK 550C10 and ZYPEEK
550G) were supplied by Jilin Zhongyan High-Performance
Plastic Co., Ltd. (Changchun, China). ZYPEEK 550G refers
to bare PEEK granules, while ZYPEEK 550C10 refers to a
PEEK composite with 10% (wt) SCF (100–200 mm in
length, 8 mm in diameter), which is used as the master-
batch material to produce SCF/PEEK filaments with 2% and
5% (wt) SCF. The PEEK and SCF/PEEK composite fila-
ments are extruded by a SJ35-28 single-screw extruder
(Zhangjiagang Huiping Machinery Co., Ltd.). According
to the PEEK melting temperature and viscosity, the rotation
speed of the single-screw feeder is set to 70 RPM.
The processing temperature increases uniformly from
345 C to 365 C at the extruder inlet in three steps. At the
outlet, the process temperature falls uniformly from 365 C
to 345 C in two steps. This ensures sufficient melting of the
material. After the molten material is extruded, it under-
goes three cooling steps: a 0.5-m air-cooling stage, a 0.5-m
water-cooling stage and a 1.5-m air-cooling stage. After the
cooling process, the filament material is controlled by an
LST-25 external measuring instrument with a 1.75 + 0.1-
mm diameter of consumable material. The scanning elec-
tron microscope (SEM) image in the inset of Figure 1
shows that the carbon fibers are evenly distributed inside
the filaments.
The FDM printing parameters are summarized in
Table 1. A 3D FDM printer (S-MAKER, Ningbo, China)
was modified to print PEEK and SCF/PEEK composite
samples, as shown in Figure 1.33 All the PEEK and PEEK
composite samples were tested without post-treatments, so
that the mechanical properties of the as-prepared samples
could be clearly evaluated.
Testing method
Tensile bars of bare PEEK, 2% SCF/PEEK, and 5% SCF/
PEEK were fabricated according to the geometry specified
in ISO 527-4(6). The designed dimensions were 75 mm 
10 mm  4 mm. Standard testing was carried out using a
material high-temperature-endurance testing machine
(AG-IC 100kN, Shimadzu, Japan), and the testing speed
was set at 2 mm/s. The same measurement was repeated
on five specimens to obtain the average value. The density
tests were carried out using the GeoPyc 1365 automatic
package-density analysis method (Micromeritics, USA).
A dynamic mechanical analysis (DMA) was carried out
using a Diamond DMA instrument (PerkinElmer Instru-
ments, USA). The specimens were 45 mm  10 mm  2
mm in size. The specimens were tested under tensile con-
ditions, with a sweeping frequency of 1 Hz and a heating
rate of 3 C/min. X-ray diffraction (XRD) spectra of the
printed bare PEEK and SCF/PEEK composites were
obtained from an Empyrean X-ray diffractometer (PANa-
lytical B.V., Netherlands). A thermal gravimetric analysis
(TGA) of the SCF/PEEK composites was conducted on a
Pyris 1 thermal gravimetric analyzer (PerkinElmer Instru-
ments, Shanghai, China) in air with a heating rate of 10 C/
min.
The composite mass change as a function of temperature
was obtained, while the thermal stability of the composite
was analyzed. A differential scanning calorimetry (DSC)
test was carried out on a Diamond instrument (PerkinElmer
Instruments, USA). The temperature range for the DSC test
was 150–380 C, and the heating rate was set to 10 C/min.
The crystallinity of each sample was determined using
Equation (1):
Hm
ð%Þ ¼  100% ð1Þ
H0  vm
where Hm refers to the melting enthalpy of the material,
vm is the PEEK matrix content, and H0 refers to the
Hu et al. 3

Figure 1. Illustrations of PEEK materials, FDM equipment, and bare PEEK samples.

Table 1. FDM printing parameters.

Controlled parameters Others

Nozzle diameter (mm) Processing temperature ( C) Infill angle ( ) Item Value

0.2/0.3/0.5/0.8/1.0/ 420 0 Infill percentage (%) 100

Ambient temperature ( C) 90
Overlap ratio (%) 15
1.0 390/400/410/420/430 0 Heat-platform temperature ( C) 100
Extrusion multiplier 0.9
1.0 420 0/15/30/45/60/75/90 Nozzle moving speed (mm/min) 150
Feeding speed (mm/min) 120
Layer thickness (mm) 0.1
4 High Performance Polymers XX(X)

Figure 2. (a) Tensile-strength results of FDM-printed 0%, 2%, and 5% SCF/PEEK samples, unadjusted/adjusted (nozzle temperature,
nozzle diameters, and infill angle); (b) stress-strain curve of the bare PEEK and adjusted SCF/PEEK; (c) TGA curve; and (d) porosity tests.

melting enthalpy (130 J/g) of the pure-crystalline PEEK
sample. The fractured surface of the printed PEEK speci-
mens was observed by SEM (JSM-7600F, JEOL, Japan) at
an accelerating voltage of 5 kV. The surface quality and the
SCF distribution of the PEEK composites were obtained
through the analysis of SEM images.
Results and discussion
Mechanical properties of CF/PEEK composites
To investigate the effect of SCF on the properties of PEEK
composites, PEEK composites with three SCF amounts
were printed via FDM. The tensile-strength testing results
are summarized in Figure 2(a), which includes the strength
of the SCF/PEEK and the bare PEEK after optimizing the
nozzle temperature, nozzle diameters, and infill angle dur-
ing FDM printing.
When using the same printing parameters as the bare
PEEK, the composite with 2% SCF showed an average ten-
sile strength of approximately 58 MPa, which is lower than
that of the bare PEEK. Meanwhile, the tensile strength of the
5% SCF/PEEK samples decreased to 18 MPa (Figure 2,
“unadjusted” section). To increase the mechanical perfor-
mance of SCF/PEEK, the FDM processing parameters were
optimized to explore their effect on mechanical properties.
The corresponding results are shown in Figure 2(a),
“adjusted” section.
Overall, the tensile properties of both PEEK composite
samples improved after the FDM parameter optimization.
Specifically, the strength of the 2% SCF/PEEK samples
increased to 96.4 MPa, representing the highest value
among all the samples. Without any post-treatment, this
value reached 80% of the tensile strength of injection-
molding parts.34 Compared to those of 3D-printed PEEK
with heat treatments,35 the tensile strength of the SCF/
PEEK composites increased by 18%.
To illustrate the nonlinear relationship between the SCF
amount and the measured tensile strength of the SCF/PEEK
materials, a porosity test and microscopic characterization
were carried out. In the TGA curve, the sample weight
began to drop at 544 C, owing to the PEEK thermal-
decomposition process. At 647 C, the PEEK resin decom-
posed completely, and the remaining weight was that of
SCF. According to the sample weight losses in
Figure 2(b), the actual SCF ratios in the PEEK composites
are calculated as 0%, 2.2%, and 5.5% in weight, close to the
nominal ratios.
Figures 3(a–c) show the interface morphologies of var-
ious PEEK composites. The SCF is oriented along the pro-
cessing direction, which is beneficial to realizing a good
bonding with the PEEK matrix (see white squares). The
Hu et al.
Figure 3. SEM images of (a) PEEK, (b) SCF/PEEK 2%, and (c) SCF/PEEK 5% samples (white square: SCF-PEEK bonding, red circle: void).
SCF alignment was influenced by the FDM processing and
a good bonding was achieved,36 which contributed to the
improved mechanical properties of the FDM-printed SCF/
PEEK composites.
The surface of the bare PEEK sample is relatively
smooth, with some small voids. The PEEK samples with
2% and 5% SCF have more and larger voids (Figures 3(b
and c)). It is proposed that the SCF slows the flow of the
melting PEEK, which prevents the PEEK from completely
filling the entire area in the rapid-cooling stage; hence,
voids emerge. Consequently, the large voids become
stress-concentration spots in the tensile test.2
To quantify the number of voids in the PEEK composite,
density tests were performed on various PEEK samples.
The absolute densities of the bare PEEK, 2% SCF/PEEK,
and 5% SCF/PEEK filaments were 1.35 g/cm3, 1.36 g/cm3,
and 1.37 g/cm3, respectively. In Figure 2(c), the measured
densities of the bare PEEK, 2% SCF/PEEK, and 5% SCF/
PEEK parts are 1.18 g/cm3, 1.17 g/cm3, and 0.87 g/cm3,
respectively, corresponding to the increased porosity of
12.4%, 13.7%, and 35.9%. The porosity increase from
2% SCF/PEEK to 5% SCF/PEEK is far larger than that
from 0% to 2%, which confirms the appearance of a greater
number of voids when more SCF was added.
Processing parameters for SCF/PEEK FDM
fabrication
As mentioned above, adding SCF causes voids and gaps to
appear in the composite systems. To alleviate the stress
concentration and mechanical weakening caused by these
voids and gaps, the FDM processing parameters were care-
fully optimized. The parameters in the FDM printing
change the temperature and pressure of the PEEK during
the extrusion, thereby affecting the flow state of the
thermoplastics.23,37,38
It can be seen from Figures 4(a, c, and e) that the tensile
strengths of the 2% SCF/PEEK are higher than those of the
bare PEEK, while the mechanical properties of the 5%
5
SCF/PEEK are worse than those of the bare PEEK. As
shown in Figures 4(b, d, and f), the 2% and 5% SCF/PEEK
composites exhibit a similar trend in the tensile modulus for
all processing parameters. The average elongation at a
break of the SCF/PEEK is far smaller than that of the bare
PEEK (as shown in Figure 2(b)). This means that the SCF/
PEEK composite is more brittle than the bare PEEK; thus,
the tensile modulus was enhanced.
In Figures 4(a and b), different trends are observed in the
mechanical curves for the bare PEEK and SCF/PEEK com-
posites. The tensile properties (strength and modulus) of
the 2% and 5% SCF/PEEK increase monotonically with
the increasing nozzle diameter, while the performance
of the bare PEEK remains almost the same, as the nozzle
diameter increases. It is proposed that the SCF/PEEK com-
posites are more brittle and have worse fluidity than the
bare PEEK (see Figure 2); hence, the SCF/PEEK compo-
site needs a larger area in the processing channel. As a
result, large nozzles (e.g., 0.8–1.0 mm) should be used to
achieve good performance when printing SCF/PEEK com-
posites using our modified FDM.
Figures 4(c and d) show the mechanical results of the
PEEK composites as a function of the nozzle temperature.
The tensile properties of all three PEEK samples increased
initially and then decreased in the range from 390 C to 430 C,
exhibiting an optimal printing temperature for each composite
sample. This is because a high temperature helps promote the
fluidity of the melting state and improves the interface of
the wires.27 However, an excessive nozzle temperature causes
the PEEK to deteriorate and produces some gases that cannot
be discharged in time.35 The gases will remain in the sample,
resulting in poor mechanical performance.
It was found that the optimal printing temperature of the
composite PEEK sample is approximately 420 C, which is
slightly higher than the 410 C of the bare PEEK sample.
This indicates that SCF changes the thermal-melting per-
formance of PEEK. Figure 4(c) contains no strength data
for the 5% SCF/PEEK sample at 390 C. This is because at
390 C, the 5% SCF/PEEK did not form effective fluid
6 High Performance Polymers XX(X)

Figure 4. Tensile properties (strength and modulus) of PEEK, 2% SCF/PEEK, and 5% SCF/PEEK samples printed with various (a, b)
nozzle diameters, (c, d) nozzle temperatures, and (e, f) infill angles.

wire, which also supports the hypothesis that the heat resis-
tance is improved in the SCF/PEEK composite.
Figures 4(e and f) show the changes in the mechanical
properties of the PEEK composites as a function of the
infill angle. The tensile properties of the PEEK composite
decreased significantly, reaching a minimum at 60 , and
then fluctuated from 60 to 90 . The tensile properties of
PEEK composites are the best at 0 , approximately 1.5
times that at 60 . When the infill angle increases, the bear-
ing direction of the printed sample changes from the axial
direction to the tangential direction. The bonding strength
between the wires gradually becomes the main part, instead
of the wire itself; thus, the tensile strength is relatively low
in the range, except at 0 .39
In Figure 4(f), the elastic modulus of bare PEEK does
not change significantly with the infill angle. After adding
SCF, it changes significantly with the infill angle. This
indicates that the SCF makes the PEEK composite proper-
ties more sensitive to the sample structure.
Additionally, the morphologies of the PEEK samples
printed with different infill angles (Figures 5(a–g)) and
nozzle diameters (Figures 5(h–l)) were investigated and
compared. When filling at 0 , the joints between the PEEK
wires are the closest, with almost no gaps. Under other
printing conditions, gaps emerge between the wires. From
15 to 45 , the gaps become larger and the strengths
decrease further. In the range of 45–90 , the strength of the
interlayer joint becomes the main bearing part; hence, the
strength is relatively low.
In the nozzle-diameter test (Figures 5(h–l)), the differ-
ence in tensile strength may be caused by the difference in
interface bonding. A larger nozzle diameter and a smaller
Hu et al.
Figure 5. Surface topography of different infill angles (a–g: 0 , 15 , 30 , 45 , 60 , 75 , and 90 , respectively) and different nozzle
diameters (h–l: 0.2, 0.3, 0.5, 0.8, and 1.0) of PEEK.
number of interface joints lead to the formation of a more
uniform interface. Overall, the voids increase with the
amount of SCF, which restricts the reinforcement effect
and results in a decrease in the strength and modulus.
When printing SCF/PEEK composites via FDM, the
amount of additional SCF and the FDM printing process
have a significant influence on the standard sample’s
mechanical properties. SCF makes the PEEK composite
properties more sensitive to the sample’s structure and pro-
cessing parameters. This indicates that optimizing the FDM
parameters is particularly important when printing SCF/
PEEK composites.
Crystallinity behavior and thermal properties
The performance of the printed PEEK samples is closely
related to their thermal properties and crystallinity, which
directly determine the fluidity of the material in its molten
state, and ultimately affect the mechanical properties of
FDM printed parts. Therefore, the crystallinity and heat
resistance of SCF/PEEK parts with various SCF amounts
and optimized parameters were measured and analyzed.
In Figure 6(a), the 2% SCF/PEEK and 5% SCF/PEEK
samples have notable SCF absorption peaks, when com-
pared with those of the bare PEEK, indicating the stable
7
physical and chemical properties of SCFs, which act as
reliable reinforcing materials in the PEEK matrix.33 It is
well recognized that a close relationship exists between the
crystallization and the mechanical properties of polymer
materials.28,33,35 DSC testing was applied to obtain the
melting enthalpy and crystallinity information of the PEEK
materials, and the results are shown in Figure 6(b). The
melting enthalpy of different samples was obtained by inte-
grating the melting peaks of the DSC curves. The crystal-
linity was calculated by combining the resin mass fraction
(100%, 98%, and 95%) in the material system.
The results show that the crystallinities of the three
PEEK samples are 18.4%, 21.9%, and 22.0%, showing an
increased crystallinity with the addition of SCF. This is
because micron-sized SCFs play the role of a nucleating
agent in the matrix of PEEK resin and expedite the crystal-
lization process in the solidification of PEEK composites,
which is very important for high-quality fabrication pro-
cesses.25 However, when the SCF amount increases exces-
sively, the voids and gaps begin to negatively impact the
mechanical properties. This helps explain the inferior
strength of the 5% SCF/PEEK sample.
To characterize the effect of the SCF amount on the
PEEK’s thermal resistance, storage modulus, loss modulus,
and loss tangent angle, the glass-transition temperature and
8 High Performance Polymers XX(X)
Figure 6. (a) XRD spectra, (b) DSC curve, (c) loss and storage modulus curve, and (d) tan delta results of PEEK, 2% SCF/PEEK, and 5%
SCF/PEEK samples.
Table 2. Glass-transition temperature (Tg), melting temperature
(Tm), and crystallinity of PEEK, 2% SCF/PEEK, and 5% SCF/PEEK.
PEEK 2% SCF/PEEK 5% SCF/PEEK
Tg/ C 144.0 147.1 148.7
Tm/ C 345.5 346.2 347.7
Crystallinity/% 18.4 21.9 22.0
melting temperature were obtained through DMA tests, as
shown in Figure 6(c) and Table 2. The glass-transition
temperature (Tg) was obtained according to the peak posi-
tion of the loss modulus curve, while the temperature cor-
responding to the peak value of the loss tangent angle was
taken as the melting temperature (Tm).40
By comparing the storage modulus curves, it was found
that adding SCF not only increased the storage modulus
(91%) at 140 C (Tg), but also improved the storage mod-
ulus from 140 to 200 C. According to the loss tangent angle
(Figure 6(d)), the ratios of the loss modulus to the storage
modulus of the PEEK material remain similar for bare
PEEK and 2% and 5% SCF/PEEK below 345 C, while they
increase when the temperature exceeds 345 C.
Based on the polymer viscoelastic theory, the viscosities
of the three PEEK materials are similar below 345 C, while
the fluidity of the SCF/PEEK composite tends to be worse
above 345 C. This means that the mechanical loss of the
SCF/PEEK composite is larger, because the SCF in the
PEEK composite influences the movement of the PEEK
molecular chain and leads to a decrease in the fluidity of
SCF/PEEK. The temperature at which the loss tangent
angle of the 2% and 5% SCF/PEEK reaches the maximum
is 10 C higher than that of the bare PEEK. This is consis-
tent with the optimal nozzle temperature for the bare PEEK
(410 C) and the 2% and 5% SCF/PEEK (420 C). These
experimental results show that SCF works well as a nucle-
ating agent to improve the crystallinity of the PEEK matrix.
Conclusion
Key FDM parameters and various SCF amounts were stud-
ied to evaluate their effects on the mechanical properties of
FDM-printed PEEK composites. In particular, samples of
the bare PEEK and PEEK composites with 2% and 5% SCF
were successfully printed using modified high-temperature
FDM equipment. The nozzle diameter, nozzle temperature,
and infill angle were modified to investigate their influence
on the mechanical properties.
A moderate amount of 2% SCF helped to enhance the
tensile strength in FDM, while an excessive amount of 5%
SCF weakened the tensile strength of the PEEK composite.
Overall, a 59% enhancement was achieved in the tensile
strength of SCF-reinforced PEEK, which is comparable to
that of PEEK parts made by injection molding. The elastic
modulus reached 2.6 GPa, which is 169% higher than that
of the bare PEEK samples. We found that a larger nozzle
Hu et al.
diameter and slightly raised nozzle temperature are bene-
ficial for making high-quality SCF/PEEK composite parts.
Our work offers insight into creating high-performance
SCF/PEEK parts with desired properties through FDM
technology.
Acknowledgement
The authors would like to thank Wuyi Sting3D Technology Ltd.
for their material and technical support of this work. We also
acknowledge the technical support of the Analytical and Testing
Center and of Huazhong University of Science and Technology.
Declaration of conflicting interests
The author(s) declared no potential conflicts of interest with
respect to the research, authorship, and/or publication of this
article.
Funding
The author(s) disclosed receipt of the following financial support
for the research, authorship, and/or publication of this article: This
work was supported by the Hubei Province Natural Science Foun-
dation for Innovative Research Groups (2020CFA030).
ORCID iD
Bin Shan https://orcid.org/0000-0001-7800-0762
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