Materials and Design 140 (2018) 209–221

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Materials and Design

journal homepage: www.elsevier.com/locate/matdes

Screw extrusion-based additive manufacturing of PEEK

Jian-Wei Tseng a, Chao-Yuan Liu a, Yi-Kuang Yen a, Johannes Belkner a, Tobias Bremicker a,
Bernard Haochih Liu c, Ta-Ju Sun a, An-Bang Wang a,b,⁎
a
Institute of Applied Mechanics, National Taiwan University, Taipei 106, Taiwan
b
Institute of Medical Device and Imaging, National Taiwan University, Taipei 106, Taiwan
c
Department of Materials Science and Engineering, National Cheng Kung University, Tainan 701, Taiwan

H I G H L I G H T S G R A P H I C A L A B S T R A C T

• A new screw extrusion-based 3D print-

ing system was designed to solve the
problems of conventional filament feed-
ing ones.
• High viscosity and melting temperature
material e.g., polyether-ether-ketone
(PEEK), has been printed with good
quality.
• Stable flow ability (b3% variation) with
high printing speed (up to 370 mm/s)
and reproducible quality was demon-
strated.
• 96% of the mechanical strength of the
bulk material (PEEK) in additive
manufacturing printing was achieved.
• SEM and XRD results revealed the ther-
mal condition was the major factor af-
fecting mechanical strength.
• The post annealing process had no signif-
icant effect on the material properties.

a r t i c l e i n f o a b s t r a c t

Article history: Polyether-ether-ketone (PEEK) has high mechanical strength, thermal performance, and biocompatibility, and is
Received 31 August 2017 widely used in biomedical and chemical engineering applications. However, to date there are no guidelines for
Received in revised form 15 November 2017 the building of a 3D printer for highly viscous materials, e.g., PEEK. In this paper, a screw extrusion method
Accepted 16 November 2017
was developed to overcome the existing problems of the filament-feeding method. Excellent flow stability
Available online 23 November 2017
(b 3% variation) and high printing speed (up to 370 mm/s) for PEEK printing were achieved. Highly reproducible
Keywords:
mechanical tests of the printing products were demonstrated with 96% of the bulk material strength for the first
Screw extrusion time. Furthermore, an exchangeable printing head was built to cover both line- and plane-printing needs to
3D printing system widen its applications and improve printing surface quality (up to 0.945 nm in Ra). All printed material had a
Polyether-ether-ketone more brittle character in comparison with the bulk material and the post annealing process was found to have
Printing strength and quality no significant effect on the mechanical strength. Additionally, porous artificial intervertebral cages with control-
lable size and distribution were manufactured to demonstrate potential applications.
© 2017 Elsevier Ltd. All rights reserved.

⁎ Corresponding author at: Institute of Applied Mechanics, National Taiwan University, Taipei 106, Taiwan.
E-mail address: abwang@iam.ntu.edu.tw (A.-B. Wang).

https://doi.org/10.1016/j.matdes.2017.11.032
0264-1275/© 2017 Elsevier Ltd. All rights reserved.
210 J.-W. Tseng et al. / Materials and Design 140 (2018) 209–221
1. Introduction
For the applications in the biomedical field, polyether-ether-ketone
(PEEK), a semi-crystalline thermoplastic, is a well-known alternative
to metal implants because of its excellent biocompatibility and compa-
rable modulus to human cortical bones, which can potentially reduce
the stress shielding effect after implantation [1–3]. Moreover, it is
radio-transparent, which can provide better evaluation of postoperative
recovery situations and has been widely used in clinical applications
such as for intervertebral cage fusion and craniomaxillofacial recon-
struction [4–6]. Although PEEK possesses several bio-favorable proper-
ties, it still suffers from inadequate osseointegration [7], rendering
porosity expression in artificial implants necessary to enhance the bio-
interaction inside the human body to more closely mimic natural tissue.
Meeting this requirement would largely increase the manufacturing
complexity, especially in forming pore interconnectivity and would in-
troduce contamination issues [8,9].
Recently, particulate leaching and selective laser sintering (SLS)
have been identified as promising methods to overcome the
manufacturing bottlenecks due to their more physical mechanism and
flexible platform compared to currently available fabrication processes
[10,11]. However, these techniques still suffer from limited capability
of designing microstructure for particulate leaching and expensive ap-
paratus requirements for the SLS method [12]. An alternative, which
balances the economic concerns, is fused deposition modeling (FDM),
which has been recognized as the most efficient method in additive
manufacturing (AM) to construct products for tissue engineering
(e.g., scaffolds) due to its wide material compatibility, low-cost appara-
tus, and great flexibility in terms of structural design [13]. Commercial
FDM incorporates a metal (e.g., copper) nozzle in which the melted fil-
ament is extruded to construct layer-by-layer structures by the relative
motion between the nozzle and substrate.
The filament feeding mechanism is the most commonly used meth-
od in FDM additive manufacturing, but it is mainly restricted to the ex-
trusion of low viscosity materials such as poly lactic acid (PLA, 10 Pa·s)
and acrylonitrile butadiene styrene (ABS, 140 Pa·s) to avoid buckling
and back-flow induced flow instability. The gap between the filament
and feeding tubes is the main cause for these problems, especially dur-
ing filament feeding in the fast printing process [14]. Once the melted
material flows back to the lower temperature region, it increases in re-
sistance and begins to solidify, which inhibits feeding efficiency due to
the buckling effect of the feeding filament and lowers the printing pre-
cision and can even cause clogging.
Despite these challenges, Valentan et al. [15] first demonstrated the
feasibility of using FDM for the highly viscous PEEK by a custom-made
machine in 2013, although it suffered from quality incompleteness
(e.g., warpage, delamination and bubbles) and non-reproducibility
(e.g., due to non-uniform filament) of the printed products. In 2015
Vaezi & Yang [16] also used filaments to print PEEK specimens with dif-
ferent porosities (14% and 31%) for mechanical test comparison with
the bulk material. The printed specimens had reduced mechanical
strength because of air gaps between the infill pattern and entrapped
micro-bubbles inside the filaments. Similarly, Wu et al. [17] and Yang
et al. [18] investigated the mechanical strength of the FDM products
and showed the importance of printing orientation with respect to the
load direction and the necessity of thermal management during print-
ing process to improve the mechanical properties of the printed
specimens.
In contrast to the filament feeding mechanism, Vaezi & Yang [16]
also chose powder as a raw material to avoid the use of filaments and
used a pushrod (or syringe) to provide higher pressures to overcome
the back flow issue, and successfully extruded melted PEEK through
the printing nozzle. A similar design appeared in a previous study by
the present author [19] except a PEEK pellet was used as the raw mate-
rial. However, the pushrod mechanism has the inherent drawbacks of a
batch process incapable of continuous printing, and suffers from lower
printing quality due to the manufacturing imperfectness of the pushrod
mechanism, especially for extruding the highly viscous PEEK material
for fast printing.
In addition to printing PEEK material, different methods of generat-
ing 3D PEEK composite for various biomedical applications have been
developed. For instance, Vaezi et al. [20] used first FDM to print a porous
hydroxyapatite (HA) scaffold and then compressed melted PEEK into
the HA scaffold to form a PEEK/HA composite to enhance the bioactivity
of PEEK material. Similarly, in an attempt to develop smart materials,
Yang et al. [21] added carbon fiber (CF) to the melted PEEK in the print-
ing process, forming PEEK/CF and PLA/CF composites, to bend the
resulting material by the electrocaloric effect for biomimetic robotic ap-
plication, e.g., artificial muscle. Based on this trend of composite print-
ing, it is likely that more PEEK composites will be developed
combining new 3D printing technology for future applications.
In the following Experimental section, the main facilities and test
procedures are described. The design of the screw extrusion mechanism
by directly using raw pellets, system stability & operation test for the
line- and plane-printing head, tensile and compression tests, determi-
nation of crystallinity under various operation conditions with some
printed PEEK examples (e.g., an artificial intervertebral cage with pore
size of 0.4 mm and 50% porosity and a high aspect ratio of hollowed
Taipei 101) are described in the Results and Discussion section.
2. Experimental descriptions
2.1. PEEK extrusion system
The schematic diagram of the newly designed additive manufactur-
ing system for highly viscous material (here PEEK) is shown in Fig. 1(a).
This system includes three main subsystems, i.e., the extruder, thermal
control, and traversing subsystems. The extruder subsystem was firmly
installed on a rigid frame fixed on a heavy granite plate (L × W × H:
600 mm × 600 mm × 50 mm). To eliminate the need for pre-
generation of the filament (commonly 1.75 or 3 mm in diameter)
used in conventional filament-based 3D printers and to maintain the
printing quality without interference by the filament cross-section
change, a user-friendly pellet feeding design was used to satisfy eco-
nomic concerns for practical use of the system. Two versions of the ex-
trusion systems have been previously tested in the development of the
3D PEEK printing process, the first incorporating the pushrod mecha-
nism [19] and the other by screw extrusion mechanism. The latter
method is used in this paper and its detailed design is described in the
next section. A microbalance (Nevada Weighing LLC) was used for the
extruded flow rate measurement.
The thermal control subsystem includes a thermal control panel,
heat plate (installed on the XY traversing unit), and heaters (installed
either within or around the extruder). Simulations for heat up time
and thermal distribution in the extruder design were conducted by
the circuit analogue method using the free open-source software-suite
Scilab Xcos [22]. For easy control of the extruder operation temperature,
three thermal modules were designed to separately control the temper-
ature settings in the feeding, compression, and metering zones
(Fig. 1(b)) using proportional–integral–derivative (PID) controllers.
The typical temperature settings were 180, 340, and 380 °C for the feed-
ing, compression, and metering zones, respectively. Electric heaters
were installed in the middle of each functional zone and covered by
an insulator and stainless-steel box for easy operation and maintenance.
The substrate was installed on the traversing subsystem with a
stroke of 100 mm in three directions. Two different substrates, quartz
glass and stainless-steel, were tested and their influence on the process
and final products were compared. The latter was mainly used in the
measurements described herein, if not specially mentioned. To control
the thermal boundary condition of the substrate, the stainless-steel
base plate (60 × 120 mm2) was fixed at 280 ± 2.5 °C by a PID controller
(CAHO, model H481).
 J.-W. Tseng et al. / Materials and Design 140 (2018) 209–221
Fig. 1. The additive manufacturing system for the PEEK material. (a) Schematic diagram of the present screw extrusion printing system and (b) configuration of screw sections, and
(c) notations for screw geometry.
The X-Y-Z traversing unit is comprised of an X-Y stage (OPM In-
strument Inc., M-JTH200-100-C7, with repeatability of ± 1 μm and
positioning accuracy of ± 50 μm) and a Z stage (OPM Instrument
Inc., M-MT90-100-C7, with repeatability of ± 1.25 μm and position-
ing accuracy of ± 50 μm). To control the traverse position with re-
spect to the extruder head, the G-code commands of moving
segments in 3 axes from a commercial slicing program (Reptier-
host) for the printing path were interpreted by the LabView program
and synchronized by a stepper motion control card (National Instru-
ments, PCI-7344).
Additionally, a light, compact, and exchangeable coater, namely a
slot printing head, which has been previously used for bio-material
coating [23,24], was modified and adapted for use in the present system.
The slot printing head was designed as a fishtail-type structure with an
upstream spread angle of 60°. This coater was designed to ensure a uni-
form flow velocity across the slit width and was constructed with struc-
tural steel via the dual phase doping process in a typical screw
manufacturing process. The slit of coater is 0.3 mm in depth and
20 mm in width at the coater exit. The total interior volume of the coater
is approximately 160 μL. Two plane heater strips were built in the coater
for heating to 390 °C. An atomic force microscope (AFM, MultiMode 8-
HR, Bruker Corporation, USA) was used to measure the printed surface
profile.
2.2. Adhesion test and printing material
Since good and uniform adhesion strength between the semi-
melted materials and the substrate/previous layer relies on a well-
controlled thermal environment in the printing process, a pair of infra-
red (IR) heaters were mounted around the nozzle head. This enabled
the control of the melting material properties (e.g., surface tension) of
each newly extruded layer to prevent delamination and/or warpage
caused by the residual thermal stress. The substrate temperature (Ts)
was controlled to have less than a 1.3% variation within the test area
of 2 × 2 cm2 over the range of 200 to 340 °C. For the adhesion test, a
pushrod-force-sensor system was designed for the adhesion force mea-
surement (Fig. 4) and a pushrod was programmed to move at a constant
speed of 6.25 mm/s to push the adherent drop after it is laid on the sub-
strate with a push delay time (Δt) of 3, 4, and 10 s, and the force was
measured by a three-axes balance (Bertec, model 3191111).
In this study, two kinds of raw PEEK pellet material from Victrex®
(PEEK 90G and PEEK 450G), were used for assessment of additive
manufacturing by using both line- and plane-printing heads. The PEEK
211
90G pellets had a median diameter size of 2.6 mm and height of
2.8 mm with a melt viscosity of 90 Pa·s. The PEEK 450G had a higher vis-
cosity of 350 Pa·s with a median diameter size of 2.1 mm and height of
3.3 mm, and was used to evaluate the flow rate stability. All raw mate-
rials were baked to ensure dehumidification at 180 °C for 4 h before the
printing process to avoid void formation.
2.3. Mechanical tests
One of the challenges in additive manufacturing is achieving good
mechanical strength of the printed parts compared to the bulk material,
especially for medical implants, in which sufficient strength must be en-
sured for practical usage. Based on the ASTM standards, the mechanical
strength of the printed material was assessed in tensile (ASTM D638-
02a, Type V) and compressive (ASTM D695-02a) tests in this study.
Moreover, the samples used in the tensile tests were printed with a 0°
raster angle (defined as the loading direction with respect to the print-
ing path direction in the additive manufacturing process), 100% infill
rate and 3.2 mm in height. The compressive test samples were printed
by the route of concentric circles to form cylinder stubs with the size
of 12.7 mm in diameter and 25.4 mm in height. Due to the different
loading range, two material test machines, a MTS Criterion 42.503
(with a full scale of 2 kN) and a MTS Landmark 370.02 (with a full
scale of 25 kN) were used for the tensile and compressive tests in an
air-conditioned room (temperature of 25 ± 2 °C), respectively. The
strain rate was set as 3.8 × 10−5 s− 1 for the tensile test, and 8.5
× 10− 4 s−1 for the compressive test. To test the annealing effect on
the mechanical performance, the printed specimens were annealed fol-
lowing the Victrex® protocol for PEEK injection molding. The samples
were first baked at 150 °C for 3 h, heated at 10 °C/h to 200 °C where it
remained for 4 h, cooled at a rate of 10 °C/h to 140 °C, and then cooled
to room temperature by switching off the power of the furnace.
After material mechanical test, the fracture surface of samples was
measured by scanning electron microscopy (SEM, NOVA NanoSEM
450, FEI, USA) to analyze differences in the microstructure. Further-
more, to calculate the polymer crystallinity of the samples, X-ray diffrac-
tion (XRD) and differential scanning calorimetry (DSC) were used. An
X-ray diffractometer (Bruker D2 phaser) was used to scan within the
range of 2θ = 0–60°. DSC (Perkin Elmer - DSC4000) was performed
by first holding the sample temperature at 50 °C for 5 min, then repeat-
ing 3 cycles of sample heating (50 to 400 °C) and cooling (400 to 50 °C)
with same heating and cooling rates of 10 °C/min.
212 J.-W. Tseng et al. / Materials and Design 140 (2018) 209–221
3. Results and discussion
3.1. Mechanics design of the screw extruder
To further improve the feeding mechanism of the 3D printer for
highly viscous materials with high printing speed, flexibility, and better
printing quality, the screw extrusion mechanism was used in this study.
This concept is based on a conventional plastic extrusion machine,
which offers high extrusion pressure and good and consistent quality
of the products. Based on the mechanical principles of a screw, this tech-
nique can provide high pressure to inhibit backflow, purge the
entrapped air, and precisely control the extrusion flow volume by the
screw spin rate. In fact, similar ideas have also been adopted by Gibson
et al. [25] and Tarik et al. [26] who used screw extrusion printing for fab-
ricating polycaprolactone (PCL) material with much lower viscosity
(1 Pa·s) and melt temperature (60 °C). No additional descriptions of
the screw extrusion design for 3D printers could be found in the litera-
ture. Therefore, a brief description of the design process of the screw
extrusion-based 3D printer will be given here for the printing of highly
viscous material, i.e., PEEK.
As shown in Fig. 1(b), the screw configuration can be divided into 3
sections according to their functions, i.e., material feeding, compression,
and metering zones. The nomenclature of the screw apparatus can be
found in Fig. 1(c). As previously mentioned, the design of the screw ex-
trusion system used in this study is based on a conventional screw ex-
trusion machine, but with some modification for fitting the practical
machining constraints. In the screw design of a PEEK extrusion machine,
two critical parameters should be first determined, the aspect ratio L/D
(where L is the total length and D is screw exradius) and the compres-
sion ratio ε (defined as the ratio of feeding to metering zone depths).
Generally, to ensure sufficient time for melting PEEK and exhausting
entrapped air, the optimal aspect ratio L/D is between 18:1–24:1, and
the compression ratio ε is between 2:1–3:1 for a stable flow at the noz-
zle outlet based on the Victrex PEEK material processing guide [27]. In
the present design, the aspect ratio was chosen to be 20:1 and the
length of the feeding, compression, and metering zones were set as 9,
5, and 6 times the screw exradius D, respectively. To minimize the sys-
tem size, D was chosen to be 14 mm, which is the minimum screw
exradius that can be fabricated. The other specifications of the screw
are the fixed pitch (t = 14 mm = D), clearance to barrel (λ = 100
μm), flight width (s = 1 mm), and helix angle (ψ = 17.65°), as listed
in Table 1. The core diameter Dc in the compression section was
linearly increased from 8 (Dc, F) to 12 (Dc, M) mm, which represents
the fixed Dc in the feeding and metering section. The compression
ratio is defined as the volumetric compression ratio and can be
described by:
h F ðt−sÞðD−h F Þ
ε¼ ; ð1Þ
hM ðt−sÞðD−hM Þ
where hF is the feeding zone depth and hM is the metering zone depth.
By setting hF = 3 mm and hM = 1 mm, the designed value of ε becomes
2.56, which is within the suggested range of 2:1–3:1 [28]. Furthermore,
since PEEK adheres well to metal, dual-phase nickel and chromium-rich
Table 1
Detailed dimensions of the screw.
alloys (e.g., 18NiCr5 steel) were chosen for the screw material to ensure
lower friction between the PEEK and screw compared with that be-
tween the PEEK and barrel for better extrusion efficiency.
Another important aspect is to ensure the flight, the thinnest part of
the screw, has sufficient strength to withstand the strongest friction and
shear forces during the extrusion process. For a simplified but conserva-
tive estimation, a Newtonian fluid assumption was applied for estimat-
ing the upper bound of the screw strength under the most harsh
extrusion conditions with high shear rate and viscosity, although the
melted PEEK has a shear-thinning nature. There are two kinds of forces
at work on the screw extrusion, the pressure and shear force. The force
on the flight can be estimated using the following equation:
F ¼ ΔPAN þ μAN γ: ð2Þ
where ΔP is the required extrusion pressure, AN is the active surface of
screw parallel to the screw axis in the metering zone (276 mm2), μ is the
viscosity of the printing material (here using 350 Pa·s for PEEK 450G),
and γ is the shear rate (using 200 rpm, i.e., 7536 s− 1). Based on the
Hagen-Poiseuille equation, ΔP can be estimated by:
8μΔLQ N
ΔP ¼ ð3Þ
πr4
where ΔL is the channel length, QN is the flow rate, and r is the nozzle
radius. In general, the flow rate is set to 60 mg/min for screw extrusion,
which is much higher than that used in this study and the correspond-
ing value of ΔP for the upper bound is 1.2 MPa. Therefore, the maximum
shear stress is estimated to be 3.84 MPa (τmax = F/AS, where AS is the
active surface of screw perpendicular to the screw axis in the metering
zone (276 mm2)) which is far lower than τallowed (850 MPa), ensuring
the safety of the screw design.
3.2. Thermal design of the screw extruder
To prevent PEEK degradation, the residence time of the melted ma-
terial in the extruder was designed to be shorter than 30 min. The sim-
ulation of the whole screw extruder using Scilab was conducted and
shown to be quite promising for optimizing the trial-and-error process
in the system design. The simulation result for part of nozzle section is
shown as a representative example in Fig. 2. Fig. 2(a) is the real model
of the nozzle section, including the nozzle and its adapter, used in this
study. Since the thermal transfer is more complicated in reality, the
block diagram of the heat transfer model was built by Scilab and
shown in Fig. 2(b) with its associated symbols. Numbers (1–7) in
Fig. 2(b) represent the heat transfer conditions of their related positions
in Fig. 2(a), e.g., 1: the thermal resistance between the nozzle and
adapter, 2: the conductive resistance and thermal capacity of the nozzle,
3: the convective and radiative transfer to the ambient surroundings
(20 °C), 4: the convective and radiative transfer to the melted PEEK,
5: the conductive resistance and thermal capacity of the nozzle adapter,
6: the convective and radiative transfer to the ambient surroundings
(20 °C), and 7: the convective and radiative transfer to the melted
PEEK. Fig. 2(c) shows the steady simulation results of temperature
distribution around the extruder by using different arrangements of
heating cartridge(s) under the same heating power (50 W). The blue
point shows the position of heater. The type III arrangement with sym-
metrical heating installation at four corners has the most uniform tem-
perature distribution with a 3.1 °C maximal temperature difference. The
type I arrangement has the worst temperature distribution with up to a
25 °C temperature difference, which may cause degradation of the ex-
truding material. Therefore, the type III arrangement, where each corner
has one heater, was adopted to achieve temperature homogeneity in
the present design and 16 heating cartridges (50 W) were installed
around the extruder tube together with an auxiliary heating cartridge
(20 W) at the nozzle adapter. By using the overall heating power
(820 W), the instantaneous temperature of the extruder wall and
 J.-W. Tseng et al. / Materials and Design 140 (2018) 209–221 213

Fig. 2. Thermal modeling and heating performance. (a) Real model of the nozzle section, (b) electrical-circuit analogue modeling, (c) temperature distribution. The biggest temperature
difference for Type I: 25 °C, Type II: 6.2 °C, Type III: 3.1 °C (d) Heat up time of the screw extruder estimation.

melted PEEK could be obtained and are shown as solid-lines and dotted-
lines in Fig. 2(d), respectively. It is worth noting that the initial condi-
tions for the melted PEEK were determined under the steady setting
temperature of the extruder wall. The heat up time is defined as the
time when all temperatures at the A–D monitoring locations
(i.e., different functional zones) of the extruder have reached their tar-
get temperature after overshoot. The simulation values of the heat up
time were 23 and 21 min for the extruder wall and melted PEEK, respec-
tively. The former is quite consistent with the experimental data of
24 min and within the design limit of 30 min that was set to avoid ma-
terial degradation.
3.3. Flow rate stability test
The screw extrusion system was designed and developed to prevent
back flow and achieve a stable flow rate during the high speed additive
manufacturing process. The relationship between PEEK flow rate, Q, and
screw spin speed, S, was calibrated for two types of nozzles (0.3 and
0.4 mm in diameter) used in this study and shown in Fig. 3. The flow
rate was measured by the extruded weight within a 1 min period. Five
extruded PEEK samples were measured for each data point. The symbol
represents the average value and the error bar shows its related
variations. The dotted- and solid-lines indicate the fitting curves of the
experimental data for the upward and downward operation of screw
spin speed, i.e., the flow rate. As shown in Fig. 3, a highly linear Q – S re-
lationship for Dn = 400 μm was found without hysteresis for both PEEK
90G and 450G. Using least–squares curve fitting, the linear equations of
Q = 0.1236S − 0.0185 and Q = 0.133S − 0.0251 were obtained with
the root-mean-square error of 0.0042 and 0.0021 for PEEK 90G and
450G, respectively. The extrusion flow rate was insensitive to the extru-
sion viscosity. Similarly, no significant hysteresis was found for the
smaller nozzle diameter of Dn = 300 μm, and all measured data are
within the band of 3% deviation from the mean value. A linear logarith-
mic equation of Q = 0.8804 log S − 1.7257 obtained using least–
squares curve fitting for the operation design with a root-mean-
square error of 0.1174. This result indicates that a solid base of reliable
extrusion flow rate for the 3D printing can be obtained only by the con-
trol of screw spin speed.
3.4. Choice of substrate temperature
Substrate temperature control during the printing process is vital to
ensure good adhesion without delamination. The removing force of the
PEEK drop was measured by the pushrod-force-sensor system, shown
214 J.-W. Tseng et al. / Materials and Design 140 (2018) 209–221
Fig. 3. The flow rate calibration curves for different nozzle sizes. The dotted- and solid-line
indicates the fitting curves of the flow rate by upward and downward measurements,
respectively, to specify the severity of hysteresis. Error bars represent the standard
deviations of five independent experiments.
in Fig. 4(a), and normalized by the drop weight to obtain the equivalent
coefficient of adhesion friction (μs). Fig. 4(b) shows the measured μs
data related to substrate temperature for three delay times, Δt, of 3, 4,
and 10 s. In general, the μs value increases to a peak of approximately
3 and then decreases again with further increasing Ts. Among the
three experimental curves, it is worth noting that the increasing curve
shifts toward higher Ts for Δt = 10 s. This is likely caused by the crack
at the edge perimeter of the cone due to large temperature gradient
for Ts ≤ 250 °C. After enough propagation time, the edge crack grows to-
ward the middle, e.g., for Δt = 10 s, and the contact area between the
cone and substrate is reduced so that the pushrod can easily remove
the cone. For higher Ts values, the viscosity of the printed material be-
comes lower for better wetting and the time to achieve full solidification
is longer when Δt is constant. The real contact area between the printed
material and substrate can increase due to the reduced volume of the
trapped air during printing and solidification processes, increasing the
adhesion force with higher surface temperature.
After reaching the μs peak, the adhesion force decreases for
increasing substrate temperature due to incomplete solidification of
Fig. 4. (a) Schematic diagram of the pushrod mechanism for adhesion force measurement and (b) the measured coefficient of adhesion friction for different substrate temperatures.
the printed material. It is important to note that with longer the delay,
the peak of the μs-Ts curve moves to the right, i.e., toward the higher
substrate temperature. This is because more adhesion area forms due
to the longer solidification time. For Ts near the melting temperature
(343 °C), a low adhesion force of melted PEEK is observed for all cases.
Similar phenomena are observed for the quartz glass substrate with
lower thermal conductivity (data not shown).
Considering the printing process is not isothermal and it takes time
to build the structures, Fig. 4(b) offers a good reference for the macro-
mechanic interactions between the printed material and substrate for
determining the suitable substrate temperature. Based on Fig. 4(b),
one can easily find the optimal operation window for the substrate tem-
perature as well as the best adhesion conditions (i.e., highest μs). It is
therefore reasonable to choose the lower range of the substrate temper-
ature (to save energy), with higher adhesion coefficients in the longer
time curve (Δt = 10 s) to determine the optimized substrate tempera-
ture. In this study, unless otherwise mentioned, the substrate tempera-
ture was maintained at 280 °C.
3.5. Plane printing test
To smoothen the printing surface and to minimize the iterative ef-
forts by integration of printing lines for the regular plane or block for-
mation, the melted material was uniformly extruded from a slot
channel (of the slot printing head) to print a plane film, as shown in
Fig. 5(a), instead of from the commonly used point nozzle to form a
line film. The plane-printing process is basically similar as the conven-
tional line-printing except the former should overcome more difficul-
ties in layers binding due to the much wider printing film, which may
cause delamination or bubbles entrapment in interlayers. This means
that more cares have to be taken to ensure good binding between layers
during the nozzle design and printing processes. In Fig. 5(a), a pair of IR
heaters (as shown in green bars) were used not only to control the
suitable thermal environment around the printing head but also to pro-
long the enough wetting time for the printed film on the substrate dur-
ing the solidification process. In Fig. 5(b), the AFM-scanned surface
profile of a printed five-layered (n = 5) PEEK film with dimensions of
40 × 20 × 1.5 mm (L × W × H) is compared with the single-layered
(n = 1) printing films of thicknesses ranging from 123 to 313 μm. All
profiles show variation in their surface height within a similar range
of ± 4 nm. To get a detailed overall view for comparison, the profiles
 J.-W. Tseng et al. / Materials and Design 140 (2018) 209–221
of the thinnest single-layered and the thickest five-layered printing
films are shown in Fig. 5(c) and (d) with surface roughness (Ra) of
0.945 and 3.46 nm, respectively. The nanometer level surface roughness
demonstrates the smoothness of the surface resulting from the highly
stable flowrate of the system. Moreover, this integrated printing system
comprising of line- and plane-printing process is highly suitable for fast
printing and to meet the manufacturing needs of high quality and uni-
formity (e.g., for microfluidic channels) [29,30].
3.6. Mechanical properties assessment – tensile specimens test
The dimensions and the photos of the test specimens produced by
line- and plane- printing are shown in Fig. 6(a). To analyze the influence
of thermal conditions on the line- and plane-printing in the
manufacturing processes, specimens were prepared by line-printing
(denoted as cases 1–3) and plane-printing (denoted as case 4) and
were tested for comparison with the bulk material (denoted as case
5). The thermal treatment conditions for cases 1–4 were: 370 °C with-
out annealing for case 1, 370 °C with annealing for case 2, 390 °C with-
out annealing for cases 3 and case 4, respectively. Fig. 6(b) shows the
results of the stress-stain relationship for the PEEK specimens of cases
1–5. All strains referred to in this study are engineering strains. For re-
peatability analysis, six samples were tested independently for each
case and the error bars show the variations of the measured data of
the ultimate tensile strength tests in Fig. 6(c). It is important to note
that, in Fig. 6(b), the measured data of all cases overlap excellently in
the elastic region and have almost the same average value of tensile
elastic modulus (obtained by the slopes in case 1–4) of 3.93 GPa,
which is only 3.2% different from that of the bulk material (case 5). All
printed specimens have much lower strains (0.018–0.029) than that
of the bulk material (about 0.25) and the zoom-in view in the red
framed region is shown in the upper-right panel of Fig. 6(b). The results
reveal that the different thermal conditions and line- and plane-printing
in the manufacturing processes do not affect the elastic moduli of PEEK
but all printing specimens exhibit brittle behavior. The brittleness of the
Fig. 5. The laminated thin films by plane-printing additive manufacturing: (a) schematic diagram of the plane-printing process; (b) the AFM-measured surface profiles of printed single (n = 1)
and five layered (n = 5) PEEK films and the photo of the latter (inset); (c) AFM surface morphology of the single layered film with a surface roughness of 0.945 nm in Ra; (d) AFM surface
morphology of the five layered (n = 5) film with a surface roughness of 3.46 nm in Ra by plane-printing.
215
manufactured PEEK can possibly be mitigated with proper control of
nozzle temperature and annealing treatment. Further investigations
on the process parameters should be conducted as a separate study.
The comparison of tensile strength in samples with different thermal
histories is shown in Fig. 6(c). The best ultimate tensile strength (Us) of
the printed parts is obtained at 390 °C for cases 3 and 4 with the value of
94.0 ± 3.88 MPa, which is almost the same (96%) as that of the bulk
specimen in case 5 (98.0 ± 1.99 MPa). The data obtained in this study
was also compared with literature data in Table 2 and shows that the
printing material that can achieve high ultimate tensile strength compa-
rable to that of the bulk material. The present data in both cases at 390
°C (cases 3 and 4) have significantly higher Us-value than reported pre-
viously [16,17]. It is worth noting that cases 3 and 4 show much better
printing property, defined as the ratio of ultimate tensile strength by
printing with respect to that of the bulk specimen, at 96% compared to
66% in the work by Vaezi & Yang [16]. A similar comparison can be
made with respect to the porosity, P, of the samples, which is calculated
Vi −ðmρÞ
by P ¼ Vi  100%, where Vi, m, and ρ are the nominal volume, mass
and, density of the printed specimen, respectively. Here, the value of
ρ(1.3 g/cm3) is provided by Victrex plc. The P value of 14% in [16] is sig-
nificantly higher than that obtained in the present work (2.6%) by line-
printing, so the Us-value reduces correspondingly.
The analysis of fractured surface by tensile tests was performed for
cases 1–5 by SEM, and shown in Fig. 7(a–e). The inset in each panel
shows the five-times magnified image of the local area. From the SEM
images in Fig. 7(a) and (b), it is clear that inferior layer-to-layer bond-
ing, as shown by the arrow, occurs for the lower operation temperature
of 370 °C in cases 1 and 2. The cross sections of cases 3 and 4 at 390 °C
operation temperature revealed a solid-like cross section (Fig. 7(c–d))
instead of the layered morphology as in cases 1 and 2, suggesting a
higher strength than the parts printed at a lower nozzle temperature.
In case 5, Fig. 7(e) shows the clear necking of the cross-section on the
right-hand side and the larger area of burnished surface due to the
slow crack propagation for a ductile material.
216 J.-W. Tseng et al. / Materials and Design 140 (2018) 209–221

Fig. 6. (a) The (i) dimensions and the printed test specimens by (ii) line- and (iii) plane- printing before the tension test; comparisons of (b) tensile stress and strain curves and (c) the
ultimate tensile strengths of the materials prepared using different manufacturing processes.

3.7. Compressive specimen test
The dimensions of the compressive tests and the photos of the spec-
imen prepared by line printing and machined from bulk material are
shown in Fig. 8(a). Fig. 8(b) shows the result of the compressive test
for four different manufacturing processes in cases 1–3 (by line-
printing) and case 5 (machined from the bulk material). Six samples
were tested independently for each group and the error bars show the
variations in the measured data in Fig. 8(c). Again, the modulus of elas-
ticity was calculated from the slope of the initial linear section and the
compressive yield strength was determined from the stress-strain dia-
gram by the same linear slope at a 0.2% strain. Similar to the results of
tension test (in Fig. 6(b)), Fig. 8(b) shows excellent overlap of the data
points for all printed samples, although the averaged compressive elas-
tic moduli obtained by the slopes of cases 1–3 (2.55 ± 0.22 GPa) is
slightly lower (20.5%) than that in the bulk material (case 5). The reason

Table 2
The comparison of mechanical properties of the AM-PEEK specimens made by different manufacturing processes.
J.-W. Tseng et al. / Materials and Design 140 (2018) 209–221 217

for the major difference in the compressive stress-strain curve between

the bulk specimen and the printed specimens is likely caused by radial
deformation, which is perpendicular to the printing direction and con-
tributes to the weakened tensile strength of the printed samples.
These deformations also provoke the delamination of the printed layers
during the compression process and the printed specimens often failed
in the manner of a big burst of either part (as shown in the sketched se-
quence A for cases 1 and 3 in the inset of Fig. 8(b)) or complete breakup
(as shown the sketched sequence B for case 2 in the inset of Fig. 8(b))
after accumulating enough compressive energy. The whole breakup of
the specimen explains the sudden fall to zero for the green stress
curve in Fig. 8(b), but this behavior can also be interpreted as a two-
stage bursts from A and then B due to the unavoidable structural hetero-
geneity (e.g., manufacturing defects).
The average of compressive yield strength in cases 1–3 is 98.5 ±
2.79 MPa, which is similar to that (96% of) the bulk material
(103 MPa), as shown in Table 2. The ultimate compressive strength
values are 135, 130, and 140 MPa for cases 1, 2, and 3, respectively.
However, the bulk-PEEK was determined to be more ductile and ho-
mogeneous than the printed samples since its stress-strain curve
continuously moved upward with a strain up to 40% without rup-
ture, as shown in Fig. 8(a)–(iv), up until the loading limit. The com-
parison of the compressive strength for samples with different
thermal histories is shown in Fig. 8(c). The result exhibits that the
mechanical strength of printed specimens is not influenced by the
annealing process.
When quantitatively comparing the mechanical properties of the
AM-PEEK specimens and those from the literature in Table 2, all values
of the compressive ultimate strength for the samples prepared herein
are 2.2 times higher than those reported by Wu. et al. [17]. It is worth
mentioning that the bulk material processed by injection molding
with annealing from Vaezi & Yang [16] has the same value of yield
strength (Ys), but much lower elastic modulus (E) compared to the
present data. Combining the previous data and the result obtained
here, the annealing process could likely be eliminated to save energy
in the manufacturing process. Furthermore, the porosity values listed
in Table 2 were 8.2 ± 2.0% for cases 1 and 2, and 2.6 ± 1.0%, and 1.9
± 0.5% for cases 3 and 4, respectively. By assuming the porosity, P, to
be zero for the bulk specimens, a clear trend of increasing porosity
emerges for decreasing Us and Ys in the compressive and tensile tests
presented herein.
The porosity can be further examined from the measurement of frac-
tured surfaces by SEM, as shown in Fig. 9(a–c). The inset in each photo
shows the five-times magnified image of the local area. The PEEK spec-
imens printed at 370 °C (the lower temperature, cases 1 and 2 corre-
sponding to SEM images in Fig. 9(a) and 9(b), respectively) have
regular “holes” and clear welding lines (as indicated by the arrow) be-
tween the infill filaments. However, the SEM image in Fig. 9(c) shows
no layered morphology for specimens printed at the higher tempera-
ture of 390 °C (case 3). This coincides with the higher P value at 370
°C compared with that at 390 °C, creating more voids at the microscale
to allow multiple crack propagations in the shear mode along the
welding line direction, resulting in a lower strength than the sample
printed at 390 °C. This further indicates that void formation during the
printing process can be greatly restrained by the screw feeding mecha-
nism, resulting in higher printing stability. This can also be achieved by
increasing the liquidity of the printing material by increasing the pro-
cessing temperature to 390 °C.

Fig. 7. SEM images of the fractured cross-section after tension tests of the specimens
manufactured at (a) 370 °C without annealing, (b) 370 °C with annealing, 390 °C
without annealing by (c) line-printing and (d) plane-printing, and (e) the bulk material.
The inset in each photo shows the five times magnification of the area indicated by the
red rectangular frame.
218 J.-W. Tseng et al. / Materials and Design 140 (2018) 209–221

Fig. 8. (a) The (i) dimensions, (ii) printed test specimens and test specimens manufactured from bulk PEEK (iii) before and (iv) after the compressive test; comparisons of (b) compressive
stress and strain curves and (c) the ultimate compressive strengths of samples produced by different manufacturing processes.

3.8. Crystallinity of the PEEK specimen
The crystallinity of both the annealed and unannealed AM-PEEK
specimens was measured after the tensile and compressive tests. As
a reference, the crystallinity of the bulk specimens after the me-
chanical tests was also measured. The percentages of crystallinity
in the specimens are summarized in Table 3. The results show that
the crystallinity in the 370 °C annealed group is 39.5% after the ten-
sile test and 36.2% after the compressive test, which are both slight-
ly higher than that at 370 °C without annealing (38.8% in the tensile
test and 35.0% in compressive test). The average of all the
unannealed groups in this study is 39.7 ± 4.1%, which is much
higher than the bulk material (20.8%). In fact, unlike the random ori-
entation of the polymer chain structure in the bulk specimen, the
melted PEEK polymer is subjected to a shearing strain by the extru-
sion process and the configuration of the polymer adopts a more or-
dered state, increasing the crystallinity of the long-chain polymers.
The annealing process for the 370 °C printed specimens contributes
slightly to the increased crystallinity (1.7% and 3.3% in the tensile
and compressive tests, respectively). This corresponds with the
mechanical strengths of cases 1 and 2 mentioned previously (only
a 3–4% difference in mechanical properties). Meanwhile, despite
the crystallinity in the group of specimens printed at 390 °C being
comparable to those at 370 °C, their ultimate tensile strength is
higher by 34%. This further indicates that the temperature of the
nozzle head during the printing process is a more critical factor af-
fecting the mechanical properties of the material than its crystallin-
ity. In fact, as a semi-crystalline polymer, PEEK possess a maximum
crystallinity between 35% and 39% [31], and once the crystallinity
approaches this level, the post processing heat treatment could
not further increase this value. Based on this approach, the screw
extrusion PEEK printer was shown to provide a high degree of crys-
tallinity and is compatible with pellets, gives high printing preci-
sion, and rapid printing speed, making it suitable for industrial
applications.
3.9. Additive manufactured PEEK structure
Fig. 10 shows structures printed by the screw extrusion printing sys-
tem including: (a) an artificial intervertebral cage (50% porosity); (b) a

Table 3
Crystallinity (%) of the AM-PEEK specimens produced from different manufacturing processes.
 J.-W. Tseng et al. / Materials and Design 140 (2018) 209–221
Fig. 9. SEM images of the fractured cross-section after compression tests of the samples
prepared at (a) 370 °C without annealing, (b) 370 °C with annealing, (c) 390 °C without
annealing. The inset in each photo shows the five times magnification of the area
indicated by the red rectangular frame.
corrosion protective sleeve; (c) a bio-scaffold structure, and (d) a brac-
ing frame-free hollowed structure (Taipei 101). The achieved printing
resolution was 125 μm. In fact, the artificial implants, such as the inter-
vertebral cages with interconnected channels of different pore sizes and
changeable porosity distributions, can be easily realized by using the
flexibility of the 3D printing process.
A summary of the mechanical properties of cortical bone and related
biomaterials are listed in Table 4. The mechanical strengths that lie
within the range of cortical bone in the first row are marked grey. It is
obvious that PEEK has good biocompatibility and extraordinary me-
chanical properties that can be used to mimic bone structure to prevent
stress sheltering. Furthermore, the 30 vol% carbon fiber (CF30)/PEEK
and glass fiber (GF30)/PEEK composites have better mechanical
strength and have the potential to be used in 3D printing. In addition
to the potential of PEEK for use in medical applications, the use of
219
Fig. 10. 3D PEEK structures: (a) intervertebral cage; (b) corrosion protective sleeve;
(c) bio-scaffold; and (d) Taipei 101, an empty structure without a supporting frame.
supporting frames for building floating structures (e.g., inverted cone
and hollowed pyramid), commonly used in conventional additive
manufacturing processes, can potentially be eliminated due to the high-
ly viscous nature of PEEK with suitable printing design. The hollowed
Taipei 101 was printed without any supporting frame during the print-
ing process because of the viscous polymer, naturally preventing struc-
tural collapse. This is a significant feature that distinguishes PEEK from
conventional FDM, which require an additional nozzle to fabricate a
water-soluble or break-away supporting structure (BASS) [32,33] for
constructing some 3D materials.
In short, the novel screw extrusion PEEK printer has demonstrated
the ability to perform line and plane printing without the need for fila-
ments, and offers a reliable manufacturing platform producing printed
parts with excellent mechanical properties that are applicable in general
CAD/bio-laboratories.
4. Conclusion
To improve the reliability of the printing properties of the fused de-
position modeling method, a new screw extrusion additive manufactur-
ing system with a pellet-feeding mechanism was successfully
developed and described in this paper for the first time. This system
was systematically tested using PEEK biomedical material under differ-
ent operating conditions and allowed the melted PEEK to be efficiently
and homogeneously layered onto a heating substrate by suitable control
of the temperature and extrusion rate. The commonly used annealing
process did not improve the mechanical properties of the material
after printing and its removal is recommended for the related additive
manufacturing processes. Nozzle temperatures in the range of
370–390 °C and a heated plate up to 280 °C were ideal conditions to
maintain an extrusion rate of 1.5 g/min within a 3% variation to meet in-
dustrial demands. In addition, maintenance of the extrusion tempera-
ture at 390 °C proved to significantly inhibit void formation/residual
stresses during the printing process, and to greatly improve the me-
chanical properties of the printed materials which approached (96%)
those of the bulk material. Moreover, this novel screw extrusion print-
ing system further realized the line- and plane-printing additive
manufacturing through an exchangeable printing head design, which
improved surface roughness (up to 0.945 nm Ra for plane-printing)
and printing speed (up to 370 mm/s for line-printing). This highly reli-
able, user-friendly, and easily adaptable screw extrusion additive
manufacturing method is expected to be used in laboratories to perform
3D printing in the future.
220 J.-W. Tseng et al. / Materials and Design 140 (2018) 209–221
Table 4
Summary of the mechanical properties of cortical bone and biomaterials.
Acknowledgement
The authors appreciate the financial support of Ministry of Science
and Technology, Taiwan (MOST 104-2221-E-002-138-MY3 and 104-
2218-E-002-009).
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