Materials and Design 146 (2018) 249–259

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Materials and Design

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

Performance of biocompatible PEEK processed by fused deposition

additive manufacturing
M.F. Arif a, S. Kumar a,⁎, K.M. Varadarajan b,c, W.J. Cantwell d
a
Department of Mechanical and Materials Engineering, Khalifa University of Science and Technology, Masdar Institute, Masdar City, P.O. Box 54224, Abu Dhabi, United Arab Emirates
b
Department of Orthopaedic Surgery, Harris Orthopaedics Laboratory, Massachusetts General Hospital, 55 Fruit St, Boston, USA
c
Department of Orthopaedic Surgery, Harvard Medical School, A-111, 25 Shattuck Street, Boston, USA
d
Department of Aerospace Engineering, Khalifa University of Science and Technology, P.O. Box 127788, Abu Dhabi, United Arab Emirates

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

• Horizontally 3D printed PEEK with ras-

ter angles of 0o and 90o exhibits tensile
flexural and fracture properties compa-
rable to those of molded PEEK
• Specimens built vertically are prone to
delamination, exhibiting poorer me-
chanical performance due to high ther-
mal gradient in the build-direction
• Stick-slip fracture and lower Poisson’s
ratio are observed for specimens built
vertically, due to the presence of interfa-
cial voids.
• Minimizing thermal gradients across
beads is the key to producing parts
with excellent macroscopic properties

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

Article history: In this study, the tensile, flexural and fracture behavior of PEEK processed by fused filament fabrication (FFF) is
Received 13 December 2017 reported. Three different configurations, viz., specimens built horizontally with a raster angle of 0° (H-0°) and
Received in revised form 4 March 2018 90° (H-90°), and vertically with a raster angle of 90° (V-90°) are examined. The best performing specimen in
Accepted 5 March 2018
terms of its tensile, flexural and fracture toughness properties is H-0°, followed by H-90° and V-90°. The H-0°
Available online 7 March 2018
and H-90° specimens exhibit 85% and 75% of tensile and flexural strengths of molded bulk PEEK, respectively.
Keywords:
The fracture toughnesses of the H-0° and H-90° specimens are 78% and 70% of molded bulk PEEK, respectively.
Additive manufacturing However, V-90° specimens show lower tensile, flexural and fracture toughness properties compared to those
Fused filament fabrication (FFF) of H-0°, H-90° and molded PEEK. The fracture surface and microtomography analyses indicate that the degree
Biocompatible PEEK of interfacial bonding between beads during layer-by-layer buildup, is affected by the thermal gradient across
Fracture toughness the beads. The PEEK specimen configurations examined here have different thermal gradient in the build direc-
Interfacial bonding tions and such variations manifest themselves in their macroscopic mechanical behavior. The findings of this
Fused deposition modeling (FDM) study provide guidelines for FFF of PEEK to enable its realization in applications such as orthopedic implants.
© 2018 Elsevier Ltd. All rights reserved.

⁎ Corresponding author.
E-mail address: s.kumar@eng.oxon.org (S. Kumar).

https://doi.org/10.1016/j.matdes.2018.03.015
0264-1275/© 2018 Elsevier Ltd. All rights reserved.
250 M.F. Arif et al. / Materials and Design 146 (2018) 249–259
1. Introduction
Compared to established technologies, additive manufacturing
(AM) offers the possibility of cost-effective automation of the fabrica-
tion process, it enables a digital inventory, and provides greater flexibil-
ity to locally design the material architecture in three-dimensions [1–4].
Fused filament fabrication (FFF), also known as fused deposition model-
ing (FDM) is the most commonly used AM technique for thermoplastic
polymers. In the FFF process, a thermoplastic filament is fed into a
heated nozzle, melted or liquefied, and subsequently extruded and de-
posited onto a build plate. A gantry moves the nozzle in the horizontal
x − y plane as the molten material is deposited. The build plate then
moves vertically (in the z axis) after completing the deposition in the
x − y plane. The deposited layers solidify and bond/weld with adjacent
layers, forming the desired 3D geometry. FFF has been used in the AM of
numerous thermoplastics. The most widely used polymer for FFF is ac-
rylonitrile butadiene styrene (ABS) [5,6] and polylactic acid (PLA) [7].
Moreover, high impact polystyrene [8], Nylon [8], Ultem® [9], polycar-
bonate [8], poly(vinyl alcohol), polypropylene [10] and the mixtures
of any two thermoplastics [11] or reinforced thermoplastic composites
[12,13] are suitable for FFF. Nanocomposite feedstocks, such as
graphene [14,15] or CNT [16] reinforced filaments, are currently
attracting interest, due to their superior thermal, electrical and mechan-
ical properties.
Processing parameters, material type and geometrical features were
found to influence the final properties of the products made by FFF. For
optimal properties of components or devices manufactured by FFF, tem-
perature control is critical. The distribution and variation of temperature
and residual stresses in structures or parts produced by FFF must be op-
timally controlled so as to ensure sufficient internal stress relaxation
and a good bonding quality between the adjacent polymer beads. For
example, warping and interlayer delamination are frequently observed
due to the residual stresses accumulated during the layer-by-layer build
up. These stresses originate from the thermal gradient generated during
the solidification process that influence the layer's volume contraction,
warping and bonding/diffusion quality between beads [17,18]. This
has shown to pose important challenges particularly for processing of
semicrystalline polymers as a high degree of crystallinity and high
shrinkage coefficient can negatively affect the dimensional stability of
the part [19]. By using a heated build plate and by controlling the tem-
perature of the 3D printer chamber, thermal gradients and their effects,
such as warping can be minimized [20,21].
In recent years, there has been a growing interest in the fabrication
of high-performance polymers such as polyphenylsulfone, polyether
ether ketone (PEEK), polyether ketone ketone (PEKK), etc. via AM due
to their outstanding mechanical properties and chemical stability.
PEEK is an expensive thermoplastic having excellent mechanical and
chemical resistance properties even at temperatures up to 240 °C.
PEEK also exhibits excellent hydrolysis resistance and provides fire,
smoke, and toxicity performance. PEEK is one of the few polymers con-
sidered for metal replacement in high temperature applications. PEEK
has been used in automotive, aerospace, oil & gas and space applica-
tions. This study focuses on FFF of PEEK for bioimplants in order to effec-
tively utilize its properties such as biocompatibility, excellent fatigue
and wear resistance for such applications [22]. PEEK is typically fabri-
cated by an injection molding or extrusion process. AM of high perfor-
mance PEEK in particular, holds tremendous promise for biomedical
applications, such as for design of novel knee replacement implants
that more closely mimic native physiology. Effort has been made to ad-
ditively manufacture PEEK via the selective laser sintering (SLS) method
[23]. Oxford Performance Materials, Inc. has developed OsteoFab® tech-
nology for 3D printing of facial and cranial implants for bone replace-
ment using PEKK powders via SLS process [24]. SLS uses a high power
laser to selectively sinter powders, which causes them to coalesce to-
gether due to interfacial and free surface diffusion. SLS can be used to
fabricate very complex geometries because it uses the same powder to
support the overhang portions, unlike FFF which requires supporting
parts. However, the inherent cost of SLS is high, owing to relatively ex-
pensive capital costs and high power laser source.
Recently, FFF has been promoted as a cost-effective alternative to SLS
for the fabrication of high-performance polymers, such as PEEK.
Valentan et al. [25] developed FFF systems to fabricate two grades of
PEEK-Optima®. The strength of the FFF samples in their study was ap-
proximately half of the tensile strength of molded PEEK (~100 MPa).
Vaezi and Yang [26] developed the FFF system to fabricate PEEK-
Optima® samples. A nozzle temperature of 400–430 °C, an ambient
temperature of 80 °C and a build plate temperature up to 130 °C were
identified as optimal parameters. The FFF process with 100% infill den-
sity results in a sample porosity of 14% and a tensile strength of
75 MPa. Wu et al. [27] showed that the warping deformation of FFF-
PEEK samples reduces with increasing chamber and nozzle tempera-
ture. Wu et al. [28] evaluated the influence of layer thickness (200,
300 and 400 μm) and raster angle (0°/90°, 30°/−60° and 45°/−45°)
on the mechanical properties of FFF–PEEK samples. A maximum tensile
strength of 56.6 MPa was achieved for samples with a 300 μm layer
thickness and a 0°/90° raster angle. Cicala et al. evaluated the tensile
properties of FFF-PEEK samples with raster angle of 0°/90°, 30°/60°
and 45°/−45° and found an average tensile strength of 69.04 MPa and
a tensile modulus of 3.53 GPa for all tested samples [29]. Yang et al.
[30] studied the effect of ambient temperature, nozzle temperature
and post heat-treatments on crystallinity and tensile properties of
FFF–PEEK with a 0° raster angle. In general, a higher ambient tempera-
ture, higher nozzle temperature and a higher post treatment tempera-
ture and time resulted in higher crystallinity, strength and stiffness.
The maximum tensile strength and modulus were found to be 84 MPa
and 4 GPa, respectively.
The aforementioned studies mostly focused on the development of
new FFF machines to accommodate the high processing temperature
of PEEK, and to evaluate the effect of process parameters on the final
properties of the samples. However, for the latter, the analysis of the
mechanical performance of the fabricated parts is presented with little
detail, especially on how the spatial thermal gradients during the layer
by layer build-up of the sample, can influence the properties. In the cur-
rent study, the tensile and flexural properties of samples built horizon-
tally (x − y plane) with raster or bead angles of 0° and 90°, and vertically
with a bead angle of 90° with respect to loading direction are evaluated.
These three configurations are associated with different thermal histo-
ries during FFF-PEEK part build up. Digital image correlation (DIC) anal-
ysis is used to measure the axial and lateral strains in the gauge length
zone of dogbone specimens. Moreover, the fracture behavior of FFF–
PEEK samples is also investigated. The fracture study is important,
since formation of micro-cracks, particularly in the diffusion/bonding
zones between beads, could lead to premature failure of fabricated
parts during their service life. To date, the fracture behavior and inter-
layer cohesion studies of FFF fabricated samples are limited to ABS
[31,32] and PLA [33,34] through single edge notch bending (SENB) or
double cantilever beam (DCB) testing configurations. In this work, the
fracture behavior of FFF–PEEK specimens is evaluated for the first time
using compact tension tests for the same fabrication configurations as
those used in tensile and flexural testing.
2. Experimental methods
The configurations used to fabricate the specimens by FFF are
discussed, followed by tensile, flexural and fracture toughness testing,
including optical strain mapping with DIC.
2.1. FFF configurations
FFF specimens were fabricated using an Indmatec HPP 155 device
(Apium Additive Technologies GmbH). This FFF device is able to fabri-
cate samples with a maximum build volume of 135 × 145 × 148 mm3.
 M.F. Arif et al. / Materials and Design 146 (2018) 249–259 251

Filaments with 1.75 mm diameter made of Victrex® PEEK 450G were
used. The filament exhibited glass transition and melting temperatures
of 153 °C and 340 °C, respectively, based on the 2nd heating cycle data
from a differential scanning calorimetry (DSC) investigation with a
heating rate of 10 °C/min. These transition temperatures closely corre-
spond to those found in the Victrex® PEEK 450G database [35]. The fil-
ament was fed into a 0.4 mm diameter nozzle by a feeding pressure
mechanism via a driver motor and a counter-rotating set of grooved
gears. The Simplify3D software package was used to determine the slic-
ing sequence and define the FFF process. The FFF process parameters
used in this study were as follows:
• Nozzle movement speed: 800 mm/min; first layer: 300 mm/min
• Nozzle temperature: 410 °C; first layer: 390 °C
• Bed temperature: 100 °C.
• Layer height: 0.1 mm; first layer: 0.18 mm
• Extrusion width: 0.48 mm
• Infill pattern: Rectilinear
• Infill density: 100%.
The nozzle movement speed, nozzle temperature and layer height
for the first layer were set differently in order to enhance adhesion be-
tween the sample and the glass build plate. Adhesion was further en-
hanced by applying a glue on the plate surface and by the addition of
brim. Brim is an outline to create a fabricated large ring that surrounds
the part and is attached to it. This holds the edges of the FFF fabricated
part and thus helps to improve bed adhesion and prevent warping.
After fabrication, the chamber was cooled to room temperature by nat-
ural convection and the parts were then removed from the build plate.
The brim structure surrounding the specimen was detached by hand.
Three FFF configurations for the tensile, flexural and compact tension
specimens used in this work are depicted in Fig. 1.
One specimen for each of the configurations was produced per fab-
rication cycle, except for V-90°, tensile and flexural specimens. Four
and three V-90° tensile and flexural specimens were fabricated respec-
tively in a single fabrication sequence. The molten polymer in the V-90°
dogbone and flexural samples is deposited onto a small cross-sectional
area, as seen in Fig. 1b and thus the nozzle travel time in the x − y plane
is very short prior to moving in the z direction. This can induce a fabri-
cation failure, since the molten polymer is deposited onto a layer that
is still in a molten state. To avoid this, we increased the number of spec-
imens so that the fabrication cycle could be done successfully, while en-
suring acceptable degree of adhesion between the beads normal to the
loading direction (z-direction). A reduced number of specimens re-
sulted in fabrication failure while increasing the number of specimens
might increase the thermal gradient between beads in the vertical di-
rection, ΔT Δz , due to the longer travel time in x − y plane, leading to a
weak bonding. The length of the clamping zone of V-90° sample was re-
duced to reduce the fabrication time, as seen in Fig. 2. H-90° samples

a) q b)

r
p s

c) d) e)
p p
r

q q
s

Horizontally fabricated in Horizontally fabricated in Vertically fabricated in direction,

plane, 0o beads orientation w.r.t plane, 90o beads orientation w.r.t 90o beads orientation w.r.t loading
loading direction loading direction direction
(H-0o) (H-90o) (V-90o)

Fig. 1. AM of PEEK by FFF: FFF configurations of tensile and compact tension specimens. The specimens were fabricated either a) horizontally or b) vertically. The deposition pattern of
specimens fabricated horizontally with either c) 0° beads orientation or d) 90° beads orientation, and e) specimens fabricated vertically with 90° beads orientation. Sub-figures p and q
in c) and d) illustrate the magnified view of the corresponding regions p and q in a). Similarly, r and s in e) illustrate the magnified zone of corresponding regions r and s in b).
Flexural specimen configuration is similar to that of tensile specimen.
252 M.F. Arif et al. / Materials and Design 146 (2018) 249–259
Fig. 2. FFF-PEEK tensile specimens.
were fabricated without outside perimeter/outline in order to avoid
beads with opposing orientations. In H-0° sample, the polymer melt
was initially deposited in the x − y plane following the outline contour
of the dogbone sample and was continued until completely printing the
entire gauge length zone, leaving the gap only at the central areas of the
clamping zone. These clamping zones were then fabricated with beads
of 45°/−45° orientation to ensure sufficient strength in the transition
zone and thus avoiding sample failure in this zone.
2.2. Tensile testing
Tensile tests were performed according to ISO 527 at a constant
crosshead speed of 1 mm/min at ambient temperature (~20 °C) on a
Zwick-Roell Z005 universal testing machine (UTM) with a 2.5 kN load
cell. The load cell accuracy was b±0.25% for a load N 10 N and b±1%
for a load range of 2.5 to 10 N, and crosshead travel resolution was
0.041 μm. DIC technique was used for full-field measurement of strain
on the specimens. Random black–white speckle patterns of acrylic
paint were sprayed on the specimen using an airbrush prior to testing.
Consecutive speckle images were acquired as a function of load using
a monochrome 5.0 MP camera for strain evaluation. The average engi-
neering strain in the axial and lateral directions over the gauge length
zone was evaluated using Vic-2D software. These strain values were
then used to construct the engineering stress–engineering strain
curve. The tensile properties of the samples were extracted from the
stress-strain curve. Each of the specimen configurations was tested at
least three times to assess repeatability. The FFF–PEEK tensile
specimens are shown in Fig. 2.
a)
3‒15 mm
Fig. 3. a) Geometry of the compact tension specimen, b) FFF-PEEK compact tension specimen and c) magnified view of the sharp crack tip region of the specimen prior to testing.
V-90o
H-90o
H-0o
2.3. Flexural testing
Three point flexural tests were performed according to ISO 178 at a
constant crosshead speed of 2 mm/min at ambient temperature (~20
°C) on a Zwick-Roell Z005 universal testing machine (UTM) with a
2.5 kN load cell. The H-0° specimens slipped from the supports after
the maximum load had been reached but didn't exhibit final failure.
Therefore, testing for H-0° was stopped when the load had reduced by
20% from the maximum. Each of the specimen configurations was
tested three times to ensure repeatability.
2.4. Fracture tests
Fracture tests were conducted to evaluate the Mode I fracture tough-
ness of the 3D printed PEEK. The compact tension fracture properties of
FFF-PEEK specimens were evaluated following ASTM D5045-14 stan-
dard for measuring the plane strain fracture toughness of polymers.
Compact tension samples were fabricated in the configuration shown
in Fig. 3a, where W = 13–15 mm. After fabricating rectangular blocks,
holes for loading pins (∅ 3 mm) were drilled using a benchtop drilling
machine. A notch was introduced by a high precision circular saw of
152.4 mm diameter and 0.508 mm thickness. A sharp notch was subse-
quently generated by a slow tapping motion with a fresh razor blade.
These specimens were manufactured without either holes or a notch,
to ensure a consistent thermal history. The FFF of the holes and the ini-
tial cracks would clearly require a change in the deposition patterns of
the filament beads, leading to a change in specimen's thermal history.
Prior to testing, the samples were kept in oven for 12 h at 70 °C to re-
move moisture. A crosshead speed of 1 mm/min in a Zwick-Roell
b) c)
 M.F. Arif et al. / Materials and Design 146 (2018) 249–259 253

a) b)
A B C D
A
D (%) (%) (%) (%)
H-0o
B 4.50 3.00 0.40 25.50
4.05 2.70 0.36 22.95
H-90o 3.60 2.40 0.32 20.40
3.15 2.10 0.28 17.85
2.70 1.80 0.24 15.30
2.25 1.50 0.20 12.75
1.80 1.20 0.16 10.20
1.35 0.90 0.12 7.65
0.90 0.60 0.08 5.10
C 0.45 0.30 0.04 2.55
V-90o 0.00 0.00 0.00 0.00

Fig. 4. Tensile properties of the FFF-PEEK tested in different directions corresponding to the different build directions: a) Representative stress-strain curve of H-0°, H-90° and V-90°, insert
shows extended ×-axis of H-0° specimen, b) axial strain contour at point A, B, C and D in a).

Z005 UTM was used. Critical stress intensity factor KIC was determined
following the method given in ASTM D5045. The adopted scheme as-
sumes a linear elastic fracture behavior of compact tension specimen
and therefore restriction on linearity of load-displacement response
was imposed. The 5% secant line criterion of the load-displacement
curve was employed to ensure validity of the KIC, as described in
ASTM D5045 Section 9.1.1. Moreover, the specimen size was appropri-
ately chosen to ensure a plane strain-state at the crack tip. The size cri-
terion stipulates that the value of 2.5(KIC/σy)2 must be less than the
specimen thickness, crack and ligament lengths. In the current study,
the yield strength (σy) of the molded PEEK was used as a reference
due to different thermal histories associated with 3D printed tensile
and compact tension specimens. Moreover, introducing a sharp crack
exactly terminating at the bead-to-bead interface is practically
impossible.
3. Results and discussion
3.1. Tensile and flexural properties
and tensile strength. The H-90° offered a Young's modulus and tensile
strength values that were 7% and 12% lower than those of H-0°, respec-
tively. The H-90° specimens exhibited properties approaching those of
the H-0° specimen, due to the excellent interfacial bonding between
beads. The H-90° had a short bead deposition path in the horizontal
plane as the nozzle travelled across the width of the specimen, as seen
in Fig. 5a. Consequently, the molten polymer diffused and bonded well
with adjacent beads, since the deposited beads were still in a molten
state. The H-0° samples had a longer deposition path in the horizontal
plane as the nozzle travelled across the length of the specimen (see,
Fig. 5b). It is likely that the bead was deposited when the neighboring
bead had been solidifying, resulting in poorer interfacial bonding be-
tween beads compared to that of the H-90°. Even though the nozzle
travel speed was constant, the build-rates were different for H-0° and
H-90° configurations due the different deposition paths. It can be seen
from Fig. 5 that the global in-plane (x − y) build direction for H-90°
sample was in the direction of specimen's length, while the build direc-
tions for H-0° and V-90° samples were in the direction of specimen's
width and thickness, respectively. Therefore, the build-rate in x direc-
tion for H-90° samples, V x ¼ Δx Δt and the build-rate in y direction for H-

The tensile performance of specimens fabricated in three different
configurations was evaluated. According to ISO 527-1:2012, tensile
strength is the stress at which the first local maximum is observed dur-
ing a tensile test. Therefore, the tensile strength of the H-0° sample was
evaluated at the yield point while those of the H-90° and V-90° speci-
mens were evaluated at the failure point, as seen in Fig. 4. The H-0°
specimen exhibited the highest Young's modulus and tensile strength,
followed by the H-90° and V-90° (Fig. 4 and Table 1). In the H-0° spec-
imen, the tensile loading direction is parallel to the orientation of the fil-
aments or beads and thus this sample showed higher Young's modulus
0° and V-90° samples, V y ¼ Δy
Δt . The build-rate in z direction for H-0°,
H-90° and V-90° samples, V z ¼ Δz Δt . As seen in Table 2, the global in-
plane build-rate for H-90° sample (62.5 mm/min) was higher than
that of H-0° sample (4.74 mm/min) and hence lower thermal gradient
leading to superior interfacial bonding between beads in x − y plane.
It should be noted that Vy for H-0° specimen was evaluated without con-
sidering the build-speed in the middle portion of the clamping zones
that had alternating 45°/−45° bead orientations.
The difference in thermal history between H-0° and H-90° speci-
mens can be seen qualitatively from the specimen color (see, Fig. 2).

Table 1
Mean values and standard errors for the tensile and flexural properties of H-0°, H-90° and V-90° specimens. Tensile elongation is evaluated at break. The properties of molded Victrex®
PEEK 450G [35] are presented for comparison.

H-0° H-90° V-90° PEEK 450G

Tensile properties
Young's modulus, Et (GPa) 3.80 ± 0.03 3.54 ± 0.05 3.03 ± 0.01 4.0
Tensile strength, σm (MPa) 82.58 ± 1.03 (at yield) 72.88 ± 1.92 (at break) 9.99 ± 0.94 (at break) 98 (at yield)
Tensile elongation, εb (%) 110.97 ± 5.31 2.91 ± 0.14 0.33 ± 0.03 45
Poisson's ratio, ν 0.44 ± 0.02 0.43 ± 0.01 0.37 ± 0.005 –

Flexural properties
Flexural modulus, Ef (GPa) 3.08 ± 0.22 3.06 ± 0.21 2.54 ± 0.07 3.8
Flexural strength, σf (MPa) 142.0 ± 5.56 124.3 ± 7.98 16.40 ± 2.18 165
254 M.F. Arif et al. / Materials and Design 146 (2018) 249–259

a) deposition path
c)

b)

deposition path
Δy
Fig. 5. Schematic of the thermal gradient and build-rate during FFF-PEEK process in a) H-90°, b) H-0°, and c) V-90° samples. Vx ¼ Δx
Δt is the build-rate in x for H-90° samples. Vy ¼ Δt is the
build-rate in y for H-0° and V-90° samples. Vz ¼ Δz
Δt is the build-rate in z for H-0°, H-90° and V-90° samples.

The gauge length zone of the H-0° specimen with a higher thermal gra- is observed, as seen in Fig. 6c. It can also be seen clearly from the SEM
dient between beads in the x − y plane, and thus weak interfacial bond- images of the H-0° and H-90° specimens where the weak interface
ing, had a brownish color. While the H-90° specimen that had a lower can be observed between the beads in vertical fabrication direction
thermal gradient between beads in the x − y plane, and thus better in- (Fig. 6a and b). It should be noted that, the time to build a single layer
terfacial bonding between beads, had a more pale or whiter color. This in the horizontal plane (x − y) of H-0° and H-90° samples was
color was relatively similar to that of the clamping zone for the H-0° 1.52 min, which was approximately five times higher than that of the
specimen which was purposely fabricated with alternating 45°/−45° V-90° samples (0.28 min), due to larger x − y deposition area compared
bead orientations to have a shorter deposition path, and to avoid failure to that of V-90° samples. Therefore, the H-0° and H-90° samples had
in the transition or clamping zone during tensile testing. Moreover, the lower build-rate (0.07 mm/min) in vertical direction than that of V-
surface finish can be used as an indicator of the degree of diffusion be- 90° samples (0.36 mm/min), as seen in Table 2, and thus larger thermal
tween beads. As seen from Fig. 2, the surface finish of the H-90° speci- gradient in z direction. Therefore, we expect poorer interfacial bonding
men was relatively rough. Since the molten polymer was deposited in the vertical direction for H-0° and H-90° samples. However, the effect
next to a bead that was still in its molten state (due to the short deposi- of thermal gradient in the z direction has less influence on the mechan-
tion path), the beads flowed more easily, forming an overlap region be- ical properties of the H-0° and H-90° samples since the weak interfaces
tween beads. In contrast, the H-0° specimen had a relatively smooth between beads in the z direction do not experience normal traction
surface, since the molten polymer was deposited next to a bead that under tensile loading. A heating zone at the top of the printer's chamber
had started to solidify. However, even though the interfacial bonding has been installed to maintain the top surface temperature of the sam-
in H-90° was better than that in H-0° specimen, the H-0° specimen ex- ple and to regulate the chamber temperature, with temperature control
hibited superior properties, since the macroscopic performance was pri- being a proprietary technology of the manufacturer. Though it ensures
marily due to the strength and strain tolerance of the filament, as that the top surface of the sample remains heated, it cannot fully elimi-
discussed earlier. nate the low interfacial bonding in the z direction as the minimum ther-
The interfacial bonding between beads is critical, especially between mal gradient between beads is restricted by the fact that the preceding
the layers in the vertical direction, particularly for V-90° specimens
where the loading direction is normal to the interface between beads Table 2
in the z direction (see, Fig. 5c). A lower thermal gradient between Build-rate (Vi) in x, y and z directions, and the deposition time (txy) in a single horizontal
beads in the z direction required for promoting interfacial adhesion in plane during the FFF-PEEK process.
vertically-fabricated specimens was restricted by the fact that the pre- Vx Vy Vz txy
ceding layer should be fully or partially solidified so as to lay the (mm/min) (mm/min) (mm/min) (min)
succeeding layer properly. Therefore, four tensile specimens of V-90°
Tensile specimens H-0° – 4.74 0.07 1.52
configurations were fabricated simultaneously to increase the deposi- H-90° 62.5 – 0.07 1.52
tion time in the horizontal plane (x − y), and thus reducing the build- V-90°a – 12.64 0.36 0.28
rate in the vertical (z) direction and avoiding the fabrication failure. Re- Flexural specimens H-0° – 5.68 0.05 1.9
H-90° 42.11 – 0.05 1.9
sults show that the tensile strength and modulus of V-90° samples were
V-90°b – 10.96 0.27 0.33
significantly lower compared to those of H-0° and H-90° samples, as Compact tension H-0° – 27.63 0.16 0.58
seen in Fig. 4 and Table 1. These results indicate incomplete sintering specimens H-90° 24.81 – 0.16 0.58
between layers in the vertical direction due to unavoidable large ther- V-90° – 26.17 0.4 0.25
mal gradient in the vertical fabrication direction (z). This can be seen a
Four specimens in one fabrication batch.
from the SEM image of V-90° sample where brittle-like fracture surface b
Three specimens in one fabrication batch.
 M.F. Arif et al. / Materials and Design 146 (2018) 249–259 255

a) b) c)

Fig. 6. SEM fracture surface morphology of a) H-0°, b) H-90° and c) V-90° specimens. The H-0° specimen was evaluated at 110% strain to failure and thus lower in cross sectional area and
larger macroscopic void. Red, yellow and white (arrows and circles) indicate the z-fabrication direction, the raster angle and the load direction, respectively. The circle indicates the
direction normal to the surface.

layer should be fully or partially solidified so as to lay the succeeding
layer.
To further confirm the interfacial defects and morphology in the z di-
rection, micro-computed tomography (μCT) images of the H-0°, H-90°
and V-90° tensile samples under no-load have been acquired via Phoe-
nix Nanotom® m system. μCT analysis is important to complement the
SEM observations since it provides details of 3D microstructure and en-
ables visualization of cross-sectional 2D image from the 3D volume,
though it has lower resolution than that of the SEM images. As seen in
Fig. 7a and b, the interfacial defects between the beads in the vertical di-
rection in H-0° and H-90° samples cannot be seen as the void dimen-
sions were mostly below the μCT voxel size or resolution (3 μm).
However, the presence of interfacial defects between beads in the verti-
cal fabrication direction was confirmed earlier from the SEM images of
tensile fracture surface, as seen in Fig. 6a and b, and also from the SEM
images of fractured surface of compact tension H-0° and H-90° samples
(see, Fig. 11a and b). In fact, some interfacial defects were found in the
μCT H-0° and H-90° samples. However, the number of defects observed
was small and the defects were randomly scattered in a few zones of the
sample volume. It is interesting to note that our H-0° and H-90° samples
possess qualitatively a very low void fraction, although FFF process
tends to produce large gaps or voids between deposited beads. A low
void fraction was achieved in this study by choosing a 100% infill den-
sity, a small layer height (0.1 mm) and high nozzle temperature (410
°C) that allowed an optimum viscous flow of the molten polymer. More-
over, the vertical build-rate for the H-0° and H-90° samples was lower
(0.07 mm/min) due to the large fabrication area in the x − y plane
and thus the preceding layer had sufficient time to solidify. Therefore,

a) c)

1 mm

d)
voids

b)

1 mm

Fig. 7. μCT images of FFF-PEEK samples at no-load; a) 2D image of H-0° sample, the insert shows voids at cross junctions between beads, b) 2D image of H-90° sample, c) 2D image of V-90°
tensile sample, the insert shows 3D reconstructed image of voids, d) 2D image of V-90° compact tension sample, the insert shows 3D reconstructed image of voids. Red, white and yellow
(arrows or circles) respectively indicate z-fabrication direction, load direction and raster angle. The circle indicates direction normal to the surface.
256 M.F. Arif et al. / Materials and Design 146 (2018) 249–259
H-0o
H-90o
V-90o
Fig. 8. Flexural stress-strain curves for the H-0°, H-90° and V-90° FFF-PEEK specimens.
the succeeding horizontal layer was deposited onto a surface that had
already solidified, inducing a stable deposition of the polymer melt
and thus preventing a void formation at the interface. Concomitantly,
this led to weak interfacial bonding due to high thermal gradient be-
tween beads along the vertical direction. Different interfacial defects
and morphologies were observed for V-90° tensile samples under no-
load, and those results were further confirmed from the V-90° compact
tension samples. Voids at the interfaces between beads were observed
in both tensile and compact tension V-90° samples, as seen in Fig. 7c
and d. As discussed earlier, the deposition of molten polymer in V-90°
configuration occurred on the surface of the preceding horizontal
layer that was not fully solidified in order to promote an acceptable de-
gree of interfacial adhesion between the beads in the vertical fabrication
direction, without inducing a fabrication failure. Consequently, good ad-
hesion between beads was achieved over a certain area of the interface,
but voids were created primarily due to undulations of the molten layer
being laid on a partially solidified preceding layer, and shrinkage of the
polymer. Inserts in Fig. 7c and d show the 3D reconstructed image of V-
90° tensile and compact tension samples, respectively, which describe
more clearly the voids formed at the interface between the beads in
the vertical fabrication direction. It should be noted that, these voids
cannot be seen clearly from the SEM images of tensile and compact ten-
sion samples in Figs. 6c and 11c. These images were taken on the
interfacially debonded surfaces between beads in the vertical fabrica-
tion direction. Voids were mostly developed between the undulating
beads normal to surface view and thus they cannot be seen clearly.
Some voids were also observed in H-0° samples particularly at the
cross-junction between beads, as seen in insert of Fig. 7a. It shows an av-
erage bead dimension of 0.5 × 0.1 mm2, which corresponds to a layer
height of 0.1 mm and extrusion width of 0.48 mm.
a) b)
Fig. 9. Load-displacement curve of FFF PEEK with a) H-0°, b) H-90° and c) V-90° specimens.
Table 3
Mean values and standard errors of the fracture toughness (KIC) of the FFF-PEEK
samples.
KIC (MPa·m1/2)
H-0° 5.32 ± 0.17
H-90° 4.76 ± 0.39
V-90° 0.97 ± 0.03
Molded PEEK
Karger-Kocsis and Friedrich [37] 7
Beguelin and Kausch [38] 6.75
Gensler et al. [39] 6.8
Rae et al. [40] 6.87
Samples loaded below the yield point (for H-0°) and below failure
point (for H-90° and V-90°) showed uniform axial strain along the
gauge length zone, as can be seen in Fig. 4b, with the maximum stan-
dard deviation in longitudinal strains of 0.15%, 0.12% and 0.019%, re-
spectively. This indicates that the samples were macroscopically
uniform, even though the samples were built layer-by-layer. The sam-
ple loaded beyond the yield point for H-0° didn't exhibit a uniform
axial strain along the gauge length, with the maximum strain occurring
in the middle portion due to its excessive straining. The Poisson's ratio
of the H-0° and H-90° samples were approximately the same (see the
mean values and their corresponding standard error, in Table 1).
Much lower Poisson's ratio was observed in V-90° sample and this
could be attributed to two factors, namely, the bead orientation and
the proliferation of voids during loading. The tensile loading in V-90°
specimen is normal to numerous weak bead-to-bead interfaces. This re-
sults in significant void growth during loading and thus exhibits lower
Poisson's ratio.
The flexural properties of the FFF-PEEK were also evaluated. It was
found that the flexural properties followed the same trend as those of
tensile properties, as the H-0° specimen had the highest flexural
strength and modulus, followed by the H-90° and V-90°, as seen in
Table 1 and Fig. 8. This is due to nearly the same build-rate and deposi-
tion time in x − y plane for tensile and flexural samples, as seen in
Table 2. The flexural properties reported here confirms the observation
of the effect of printing configurations on tensile properties discussed
earlier. Both tensile and flexural strength of H-0°, H-90° and V-90° spec-
imens were 15%, 25% and 90% lower than those of molded PEEK 450G,
respectively (Table 1). However, the tensile and flexural moduli didn't
exhibit similar levels of reduction compared to the PEEK 450G. The ten-
sile and (flexural) moduli of the H-0°, H-90° and V-90° specimens were
5% (19%), 11% (19%) and 24% (33%) lower than those of molded PEEK
450G, respectively. This is due to the fact that the interface zones of
the layered structure of the FFF-PEEK samples provide strain-tolerance
to the system (due to their lower compliance) under bending load
and thus lower the flexural modulus of the samples. The Young's mod-
ulus and tensile strength of the H-0° and H-90° specimens were similar
to those reported elsewhere [30] or indeed higher [25,26,28,29] than
the previously reported FFF-PEEK samples. The flexural modulus and
strength of the H-0° and H-90° specimens were higher than the
c)
 M.F. Arif et al. / Materials and Design 146 (2018) 249–259
Fig. 10. Photograph of fractured compact tension samples of a) H-0°, b) H-90° and c) V-90°
specimens.
previously-reported FFF-PEEK samples [26,28]. For the V-90° sample, al-
though it had a relatively high Young's modulus, the tensile strength
was significantly lower than those of H-0° and H-90° specimens and
molded PEEK. The tensile strength of V-90° falls within the range of
molded LDPE [36].
3.2. Fracture toughness
The fracture test results showed the influence of the FFF fabrication
configurations and bead orientation on the fracture toughness. The H-
0° specimen showed the best performance, followed by H-90° and V-
90°, as can be seen in the load-displacement curves (Fig. 9) and KIC
(Table 3). Based on build-rate data presented in Table 2, the interfacial
bonding between beads in H-0° compact tension sample was better
than that in H-0° tensile and flexural samples. On the other hand, H-
90° compact tension sample exhibited lower interfacial bonding be-
tween beads compared to those of tensile and flexural samples. The
build-rates in z direction (Vz) were almost the same for compact ten-
sion, tensile and flexural samples and thus exhibited poor interfacial
bonding between beads, as discussed earlier. Interestingly, the build-
rate in x − y plane for H-0° and H-90° compact tension samples was
a) In-plane crack
propagation
Out-of-plane crack
propagation
b)
Fig. 11. SEM images of fracture surfaces of a) H-0°, b) H-90° and c) V-90° specimens. Red, yellow and white (arrows or circles) respectively indicate z-fabrication direction, raster angle and
load direction. Circle indicates direction normal to the surface.
257
almost the same and thus we expect similar degree of interfacial bond-
ing between beads in x − y plane for both samples. For the ASTM D5045
standard adopted here, it is most likely that the sharp tip of the intro-
duced crack in H-0° sample is terminating well within the bead (but
not exactly at the interface between beads) and thus the fracture tough-
ness value estimated doesn't fully represent the fracture behavior of lay-
ered structure of FFF-PEEK. Such limitation was also encountered for H-
90° and V-90° samples as it was difficult to generate a sharp crack ex-
actly terminating at the interface between beads. Regardless of these
limitations, it can be seen that the trend of KIC was almost the same as
those observed for the tensile and flexural tests. Results indicate that
the bead orientation with respect to the loading direction contributes
the most to the mechanical performance, followed by the interfacial ad-
hesion between beads. Interfacial adhesion is affected by the thermal
gradient dictated by the in-plane and out-of-plane build-rates (see
Table 2).
The crack tip in H-90° and V-90° compact tension specimens exhib-
ited a higher probability of advancement through the bead-bead inter-
face where the interfacial zone between beads acted as the weakest
link, unlike the H-0° specimen wherein the crack tip advanced normal
to the bead orientation (see, Fig. 10). The crack tip in H-0° specimen re-
quired more energy to break the beads transversely, resulting in higher
fracture toughness. This effect can also be seen on the fracture surface,
where the crack path in H-0° specimen sometimes deflected into the
weakest link, leading to out-of-plane crack propagation, while the
crack propagation in H-90° and V-90° specimens consistently
delaminated along the bead-bead interface, as shown in Figs. 10 and
11. The difference in performance between H-90° and V-90° specimens
was related to the different degree of interfacial bonding between beads
associated with the different thermal gradients, as discussed in the pre-
vious section. After the maximum load had reached, a softening re-
sponse was observed as seen in Fig. 9b due to the deflection of crack
into neighboring weak bead-bead interface. The SEM images of the frac-
ture surfaces of compact tension samples shown in Fig. 11a, b and c
helped to draw a similar conclusion to those of tensile samples as
weak interfacial bonding can be found between beads in the vertical
fabrication direction. The stick-slip crack growth (after the maximum
load) was observed in V-90° sample under constant applied extension
rate loading conditions due to the presence of voids at the interface be-
tween beads. These voids act as a crack arrester. Stick-slip fracture in
this case was characterized by oscillatory crack tip velocities and crack
growth jumps resulting in periodic load fluctuations (see, Fig. 9c) [41].
The strain contour at maximum load of the three sample configurations
was evaluated. It showed that the strain was a maximum at the crack
front, as seen in Fig. 12. The highest value of maximum strain was
found in H-0°, followed by H-90° and V-90° specimens. The H-0° speci-
men had the highest strain tolerance as the crack tip advanced normal
In-plane crack
propagation
c)
258 M.F. Arif et al. / Materials and Design 146 (2018) 249–259
a) (%)
6.10
b)
5.23
4.36
3.49
2.62
1.75
0.88
0.01
-0.86
-1.73
-2.6
Fig. 12. DIC contour of strain at maximum load of a) H-0°, b) H-90° and c) V-90° specimens.
to the bead orientation, and thus the highest fracture toughness of the
sample. While comparing the current results with those from tests on
bulk, molded PEEK using compact tension geometry at room tempera-
ture, we noticed that the fracture toughnesses of H-0° and H-90° sam-
ples, respectively were 78% and 70% of the molded PEEK fracture
toughness (see, Table 3). The low fracture toughness in the V-90° con-
figuration reduced the full potential of PEEK to be applied in high
load-bearing applications but the value was still within the range of
brittle polymers such as acrylic, epoxy and polystyrene [42].
4. Summary
The tensile and flexural properties of PEEK fabricated by FFF have
been studied. The fracture behavior of FFF-PEEK has been reported for
the first time. Three specimen configurations; H-0°, H-90° and V-90°
have been tested to failure in conjunction with optical strain mapping.
The configuration that exhibited a superior performance, in terms of
tensile strength and modulus, flexural strength and modulus, and frac-
ture toughness, was H-0°, followed by H-90° and V-90°. The H-0° and
H-90° showed 85% and 75% attainable tensile and flexural strengths of
the bulk molded PEEK respectively. The fracture toughnesses of the H-
0° and H-90° specimens were 78% and 70% of the molded PEEK fracture
toughness, respectively. However, the V-90° sample exhibited low ten-
sile, flexural and fracture toughness properties compared to those of H-
0°, H-90° and bulk PEEK. The performance of these three configurations
represents different thermal gradients between beads during layer by
layer buildup in FFF.
It was found that different fabrication path can promote a different
degree of interfacial adhesion between beads which in turn can have a
significant influence on the tensile and fracture toughness properties.
This information is directly relevant to the fabrication of biomedical im-
plants with sufficient mechanical strength for long-term in-vivo appli-
cations. Short polymer deposition path in x − y plane promoted the
best bead-to-bead interfacial adhesion since the diffusion is faster
when the beads were in molten condition. However, it had drawback
in the final surface roughness due to the formation of bead-to-bead
overlap zone. Therefore, short deposition path could be considered for
the inner part of the sample while the long deposition path could be
employed for the outer surface to obtain better surface quality. The
short deposition path need not necessarily be implemented with a 90°
bead orientation as alternate bead orientations such as 45°/−45° and
60°/−60° also exhibit almost the same thermal gradient in the horizon-
tal layer as that of the 90° bead orientation.
Diffusion lines (interfaces at which the bonding is weak) were found
at the interface between the beads in the vertical fabrication direction in
all specimen configurations due to high thermal gradient across beads.
This had a dramatic effect when the load was applied normal to this
weakest zone, as exemplified by the tensile, flexural and fracture tough-
ness properties of V-90° samples. Results suggest that minimizing ther-
mal gradients across beads during FFF of thermoplastics with a high
(%)
4.30 c) (%)
0.47
3.71 0.41
3.11 0.34
2.51 0.28
1.92 0.21
1.33 0.15
0.73 0.09
0.14 0.02
-0.46 -0.04
-1.05 -0.11
-1,65 -0.17
melting temperature is the key to producing parts with excellent mac-
roscopic material properties and dimensional stability. Thermal gradi-
ent effects remain an important issue in FFF, leading to limitations in
mechanical performance relative to conventionally molded samples.
Ways such as precise control of the chamber temperature, post heat-
treatment of the FFF fabricated samples [30] and microwave heating
of FFF samples fabricated with coated-CNT filament [43], would help
to minimize these limitations. The Poisson's ratio calculation can be
used as a comparative indicator of the specimen's quality. For example
the V-90° specimen had much lower Poisson's ratio compared to the
H-0° and H-90° specimens which was mostly due to the opening of
the voids during loading. The current study serves as an important
first step in the development of comprehensive guideline for the FFF
of high temperature and high performance thermoplastics (e.g. PEEK)
to enable high-end engineering applications such as for biomedical
implants.
Acknowledgements
Authors would like to thank to Abu Dhabi Education Council (ADEC)
for providing the research grant (EX2016-000006) through “the ADEC
Award for Research Excellence (A2RE) 2015”. SK would like to thank
Professor Brian Wardle, Massachusetts Institute of Technology for his
comments on the MS.
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