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A R T I C L E I N F O A B S T R A C T
Keywords: The purpose of this work is to study the influence of different lay-ups on fracture properties for high-impact
Additive manufacturing polystyrene (HIPS) processed via material extrusion. The fracture properties of 3D printed HIPS were studied
Material extrusion based on the essential work of fracture (EWF). The obtained data was in good agreement with the EWF criteria.
High impact polystyrene
Results showed that [− 45/45]5 and [0]5 lay-ups had the highest (10.855 KJ.m− 2) and lowest (1.6338 KJ.m− 2)
Essential work of fracture
resistance to crack initiation (we) of 3D printed HIPS, respectively. Also, the highest and lowest value of non-
essential work of fracture (βwp) were related to [0]5 and [0/90]5 lay-ups with values of 2.4357 and 0.4371
KJ.m− 3, respectively. Furthermore, SEM fractography was used to analyze the fracture mechanism and porosity
(triangular air gaps) of the specimens. A variety of fracture mechanisms, including micro-hills, fibrillated
structures, and pull-out were dominant in this study.
* Corresponding author.
E-mail addresses: faramarz_ashenai_ghasemi@yahoo.com, f.a.ghasemi@sru.ac.ir (F. Ashenai Ghasemi).
1
P.O.B.16785-136, Tehran.
https://doi.org/10.1016/j.addma.2022.103191
Received 17 March 2022; Received in revised form 19 September 2022; Accepted 30 September 2022
Available online 4 October 2022
2214-8604/© 2022 Elsevier B.V. All rights reserved.
S.A. Sajjadi et al. Additive Manufacturing 59 (2022) 103191
For example, Bañuelos et al. [13] and Verma et al. [6] studied the
fracture properties of printed specimens as a function of the raster angle.
Bañuelos et al. reported that in PP-printed specimens, the 0◦ raster angle
showed better fracture parameters, and the 90◦ raster angle showed no
stable crack propagation. Verma et al. also confirmed that the failure
initiation resistance for ABS printed specimens at the 0◦ raster angle is
greater than the 90◦ raster angle. Yin et al. [24] also investigated the
effect of print speed and extrusion temperature on fracture parameters
for PLA and PP samples. They found that the fracture values improved
by increasing the extrusion temperature.
The fracture analysis of 3D printed polymers via material extrusion
according to the EWF method is a new field, and the fracture charac
teristics of all-polymer samples made by 3D printing have not yet been
investigated. Therefore, in the present work, the fracture toughness of
high-impact polystyrene as a function of the raster angle with different
lay-ups via the EWF method is analyzed. The fracture toughness of
different lay-ups was examined with a combination of 0◦ , 45◦ , and 90◦
raster angles. Also, the effect of different lay-ups on the porosity and the
fracture mechanism is investigated by SEM photography.
2. EWF theory
2
S.A. Sajjadi et al. Additive Manufacturing 59 (2022) 103191
Fig. 3. Raster angle and lay-up modes of DENT specimens: a)[0]5 b) [90]5 c) [45]5 d) [− 45/45]5 e) [0/90]5 f) [90/0]5 g) [90/− 45/90/45/90] h) [0/− 45/0/45/0].
where We is the essential work of fracture, WP is the non-essential work 2) The fracture happens under plane stress states.
of fracture, L is ligament length, t is the sample thickness, and β is the 3) Load-displacement curves shall be self-similar for each sample at a
coefficient of the shape of the plastic area. In addition, when the above series of different ligament lengths.
equation is divided by the area of the ligament (L.t), the expressions of
(Wf, we, and wp) are shown in Eq. (2). 3. Experimental
/
wf = Wf (L.t) = we + βwp .L (2) 3.1. Materials
The specific total fracture work (wf) is a linear function of the liga
HIPS with a density of 1.05 g/ cm3, melt flow index (MFI) (200 ◦ C/ 5
ment length. With plotting wf versus ligament length, the two main
parameters, we (intercept elevation), and βwp (line slope) will be ach Kg) of 3 g/ 10 min, IZOD impact strength of 11 KJ/m2, the tensile
strength of 27 MPa, elongation at break of 55% and filament diameter of
ieved. The former is closely related to the fracture toughness of the
specimen, and the latter is closely related to the ductility of the specimen 1.75 mm for manufacturing the test specimens via material extrusion
[32]. Specific essential work of fracture (we) is theoretically dependent process was supplied from eSUN, Shenzhen, China. The recommended
on thickness and equivalent to JIC [33]. However, the EWF method printing temperature for the extruder and heat bed is 230–270◦ C and
offers experimental advantages over the J-integral method as its 100–115◦ C, respectively.
simplicity and applicability for thin samples. Furthermore, the expres
sion βwp includes a morphologically sensitive component that may be 3.2. Sample preparation
used to assess toughness in thin specimens [34]. In addition, conditions
must be met for the correct application of the EWF method, which 3.2.1. Material extrusion process
includes: ANET ET4 FDM printer (Anet Technology Co., Ltd, Shenzhen, China)
was utilized to prepare specimens. To print required geometries, CAD
1) The length of the ligament must be utterly yielded prior to the onset models of specimens were modeled in 3D printable STL format via
of crack propagation. SolidWorks. Since a designed model with specific printing parameters in
3
S.A. Sajjadi et al. Additive Manufacturing 59 (2022) 103191
Fig. 4. Load-displacement diagram for 3D printed specimens with different lay-ups and compression molded specimen: a) HIPS, b) [0]5, c) [90]5, d) [45]5, e) [45/
− 45]5, f) [0/90]5, g) [90/0]5, h) [90/− 45/90/45/90], i) [0/− 45/0/45/0].
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S.A. Sajjadi et al. Additive Manufacturing 59 (2022) 103191
Table 2
Mean maximum load values for 3D printed for different ligament lengths and lay-ups and compression-molded specimens.
Sample Fmax
Average value St. Average value St. Average value St. Average value St. Average value St.
(N) Dev (N) Dev (N) Dev (N) Dev (N) Dev
Molded HIPS 155.5339 10.82 219.1705 1.78 274.7628 4.03 353.2477 3.59 387.3207 6.36
[90]5 105.9741 6.32 159.1091 3.03 201.4900 4.60 232.2986 3.20 276.7728 7.02
[0]5 166.9250 4.28 198.2109 16.77 237.9591 6.76 336.1783 7.75 396.5530 17.80
[45]5 108.0871 19.70 156.7557 3.73 179.1866 6.37 236.7624 7.27 276.3637 17.90
[− 45/45]5 120.0548 3.01 162.8913 11.52 203.1570 7.84 263.7725 15.50 286.7616 7.47
[0/90/0/90/0] 107.9209 5.05 144.9723 4.34 165.4240 3.95 215.9936 29.20 244.2514 8.75
[0/− 45/0/45/0] 136.5276 5.05 202.3571 11.41 213.0235 26.7 285.4951 2.20 302.4554 22.50
[90/0/90/0/90] 114.2434 3.80 159.6995 3.30 189.8279 13.97 220.1262 4.20 252.1018 4.23
[90/− 45/90/45/ 108.6410 3.96 154.9784 9.06 205.6078 8.91 231.3009 22.50 274.7180 12.08
90]
G-code format is needed in order to start the printing process, slicing specimen have self-similarity with increasing ligament length. This
software, Cura, was utilized. The detailed manufacturing parameters for similarity in load-displacement curves, as expressed by Karger-Kocsis
the specimens are listed in Table 1, which are kept constant for all [23], is one of the most important prerequisites for the validation of
specimens. Subsequently, specimens have been extruded layer by layer the EWF method. The self-similarity guarantees that under the same
to achieve a certain number of layers (5 layers) regarding the thickness conditions, the process of failure and crack propagation is independent
and height of each layer. Fig. 2 shows how the material extrusion pro of the ligament length. According to the load-displacement diagrams in
cess work and deposits the molded material layer by layer on the bed. general, increasing the length of the ligament led to an increase in total
Also, the scheme of different orientation types is shown in Fig. 3. energy Wf (total area under the curve), maximum load (Fmax) (the values
of Fmax with standard deviation are reported in Table 2), and extension
3.2.2. Compression molding at failure (εb). Another prerequisite for ensuring the validity of the EWF
To compare and analyze the influence of various preparation test is fully yielding the ligament before the onset of crack growth and
methods on the fracture behavior of HIPS, the hot-press molding tech stable crack propagation. Visual observation of the specimens during the
nique was applied to achieve homogenous specimens. First of all, HIPS experiment showed that fully yielding of the ligament area occurred at
filaments were chopped and placed in a cold mold and preheated to maximum load, meaning that the crack propagated stably [32,35].
245 ◦ C. Then, the pressure was increased slowly to 2 MPa for 3 min and To ensure that EWF data is obtained under plane stress conditions for
held at this pressure for another 2 min. After the molding process, the 3D printed specimens with different lay-ups and molded specimen, net
mold was removed from the hot press and cooled at room temperature. cross-sectional stress (σmax = Fmax /l.t) was calculated for different lig
ament lengths and plotted versus ligament lengths for all specimens in
3.3. Characterization Fig. 5. Based on the data, the mean maximum stress (σm) was calculated,
and if the maximum stress (σmax) is in the range of 0.9σm to 1.1σm, the
3.3.1. EWF properties results are assumed to be valid [23,34].
To study the fracture properties of the specimens, EWF methodology The results clearly show that all experiments are performed under
was carried out by using a Zwick/ Roell machine model Z010 (Zwick plane stress conditions (no data with values higher than 1.1σm) and no
Roell Group company, Germany) with a constant cross-head speed of sample fails before full ligament yielding (no data with values lower
5 mm/ min at room temperature. The ligament lengths of DENT speci than 0.9 σm), which indicates the validity of the results.
mens were 7, 9, 11, 13 and 15 mm. The notches were located precisely For qualitative comparison with samples with regard to tensile
in the direction of the width of the specimens by utilizing a sharp razor strength, this study used mean maximum stress (σm) as this property.
blade to produce a pre-crack tip. The dimensions of the EWF test spec From Table 3, it can be seen that the tensile strength of [45]5 and [90]5
imen were 80 × 25 × 1 mm3. At least 5 specimens for each ligament lay-ups compared to [0]5 one decreased by 28% and 27%, respectively.
length were tested for each orientation type to investigate EWF It is clear that low adhesion between adjacent layer filaments due to
parameters. insufficient pressure during the material extrusion process is a defect.
This defect was minimized for 0◦ , therefore, good adhesion was ach
3.3.2. SEM microscopy ieved for this angle. In general, for a raster angle of 0◦ , more load should
For a better understanding of failure mechanisms and porosity of the be applied to yield and tear the specimens [36].
DENT specimens prepared by the material extrusion process, specimens Poor tensile properties will be obtained when the test specimen is
were investigated using the JEOL JXA-840, scanning electron micro loaded perpendicular to the fabrication direction ([90]5) due to poor
scopy (SEM) with the accelerating potential of 25 kV. To reduce electron interlayer bonding and adhesion [36,37]. At 90◦ raster angle, which the
charging, the fracture surface of the DENT specimens obtained from layers are aligned with a smaller raster length, and a large number of
EWF testing were sputter-coated with a thin layer of gold prior to their raster lengths with less length increases the number of heating and
SEM observation. cooling cycles. This leads to the creation of cracks between the layers,
delamination, and separation between adjacent layers [38–40]. These
4. Results and discussion reasons reduced the tensile strength of [90]5 lay-up compared to [0]5
ones. In addition, the dominant fracture mechanism of [45]5 lay-up was
4.1. Load-displacement curves shear yielding due to the angle of the interlayer bonds. The high tensile
strength of the [45]5 specimens might be due to the fact that the bond
Fig. 4 shows load-displacement curves of the 3D printed DENT area between the layers was larger, as a result, the tensile strength
specimens in different lay-ups and molded specimens for different lig increased [40].
ament lengths. It should be mentioned that the same scale in all axes was The lowest tensile strength was belonged to [0/90]5 and [90/0]5 lay-
not used because of visibility. The load-displacement curves for each ups mainly due to the loading direction parallel to the layers and raster
5
S.A. Sajjadi et al. Additive Manufacturing 59 (2022) 103191
Fig. 5. Sai-Hill criteria diagram for 3D printed specimens with different lay-ups and compression molded specimen: a) HIPS, b) [0]5, c) [90]5, d) [45]5, e) [− 45/
45]5, f) [0/90]5, g) [90/0]5, h) [0/− 45/0/45/0], i) [90/− 45/90/45/90].
6
S.A. Sajjadi et al. Additive Manufacturing 59 (2022) 103191
Fig. 6. Schematic diagram of load-displacement curves with ligament area deformation sequences during EWF test.
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S.A. Sajjadi et al. Additive Manufacturing 59 (2022) 103191
Fig. 7. Wf versus L diagram for 3D printed specimens with different lay-ups and compression molded specimen: a) HIPS, b) [0]5, c) [90]5, d) [45]5, e) [− 45/45]5, f)
[0/90]5, g) [90/0]5, h) [90/− 45/90/45/90], i) [0/− 45/0/45/0].
8
S.A. Sajjadi et al. Additive Manufacturing 59 (2022) 103191
Tablee 4
Values of specific total, essential and non-essential works of fracture and linear regression for 3D printed specimens with different lay-ups and compression-molded
specimen.
Sample wf we βwp we R2
KJ KJ βwp
Ligament 7 Ligament 9 Ligament 11 Ligament 13 Ligament 15 ( 2) ( 3)
m m (m)
Average St. Average St. Average St. Average St. Average St.
value (KJ. Dev value (KJ. Dev value (KJ. Dev value (KJ. Dev value (KJ. Dev
m− 2) m− 2) m− 2) m− 2) m− 2)
Molded 18.9809 0.830 21.6172 1.498 24.3772 2.100 28.6963 3.070 27.2068 4.800 11.573 1.1440 8.0368 0.8473
HIPS
[90]5 22.4651 1.800 19.7824 0.927 27.5532 1.685 31.8105 0.411 39.6889 0.720 2.7832 0.8043 3.4604 0.9756
[0]5 7.9860 1.388 10.7879 1.682 11.8185 1.126 12.5125 3.590 15.1092 1.980 1.6338 2.4357 0.6707 0.8842
[45]5 18.9230 0.146 25.4834 0.621 34.2444 0.239 31.8165 1.382 34.3736 0.851 8.0320 1.9035 4.2196 0.7813
[− 45/ 19.4057 1.632 20.6313 1.303 24.0886 2.320 26.3848 1.800 28.4315 0.806 10.855 1.1991 9.0526 0.9623
45]5
[0/90/0/ 9.3894 1.244 12.2776 0.162 12.6886 0.575 12.5072 0.691 14.2499 0.268 7.3466 0.4371 16.8076 0.7834
90/0]
[0/− 45/ 17.8580 0.602 24.3164 2.590 26.4922 3.280 29.4603 0.741 30.7139 2.100 7.9491 1.6393 4.8491 0.9455
0/45/
0]
[90/0/ 10.3330 1.147 11.4196 0.639 11.5104 1.444 11.9818 0.074 14.3853 0.571 7.1386 0.4299 16.6052 0.7917
90/0/
90]
[90/ 7.7654 1.030 12.2457 1.311 13.7130 1.590 13.5416 0.301 14.1291 0.301 4.3043 0.7338 5.8657 0.7405
− 45/
90/45/
90]
Fig. 8. Schematic representation of porosity in material extrusion process: a) porosity between filaments b) porosity between layers.
(βwp) belonged to the samples with [0]5 and [90/0]5 lay-ups, respec that are prone to stress concentration [36]. These observations are
tively. Rabbi et al. [52] also concluded that the [0/90] lay-up had the similar to the work of Heydari et al. [54], who argued that the nature of
highest crack propagation rate. It has been proven that during loading, the layer structure, particularly the adhesion between layers, had a
cracks propagate along the path with the least resistance from the direct effect on mechanical properties.
material. Comparing the experimental data in Table 4 between the [0]5 and
Porosity (air gap) between two adjacent filaments, as seen in Fig. 8, is [90]5 lay-ups, demonstrated that by changing the printing orientation to
due to the effects of accumulation during the material extrusion process perpendicular to the load, the essential work of fracture increased by
and the formation of unfilled cavities between different layers of molten 70%, and the value of non-essential work of fracture decreased by 67%.
filament. The shape and size of these gaps may vary at different locations This decrease was also reported by Verma et al. [6]. In the specimen
depending on the printing orientation, raster angle, the shape of the with a raster angle of 0◦ (Fig. 9a), the printed orientations were
infill, and the thermodynamic parameters associated with layer cooling perpendicular to the initiate and propagation of the crack, and under
[36]. As a result, porosity creates a weak bond to start and propagate the tensile loading, the failure occurred due to the yielding of individual
crack. So it can be concluded that the crack is easily and quickly between filaments. Also, failure in deposited samples with all 90◦ fabrication
two consecutive bonds of [0/90]5, [90/0]5, and [90]5 lay-ups initiated orientation (Fig. 10b and 11), in which cracks initiated and propagated
and propagated [52]. This confirms the low value of non-essential work in the direction of the printing orientation, was affected by the interlayer
of fracture (βWp) for the mentioned specimens compared to the other bonding area and the intera-layer bonding [43].
samples. Excessive porosity also causes poor interlayer adhesion [53]. Also, considering the [45]5 lay-ups and comparing it with the [0]5
The stress is concentrated in the interlayer bond region, as shown in and [90]5 ones, the value of essential work of fracture and non-essential
Fig. 11b. There are many air gaps in adjacent layers and interlayer bonds work of fracture with a significant improvement reached 8.032 KJ/m2,
9
S.A. Sajjadi et al. Additive Manufacturing 59 (2022) 103191
Fig. 9. Schematic illustration of how cracks propagate in 3D printed specimens with different lay-ups: a) [0], b) [90] c) [45], d) [− 45/45], e) [0/90] or [90/0], f)
[0/45], g) [90/45].
10
S.A. Sajjadi et al. Additive Manufacturing 59 (2022) 103191
11
S.A. Sajjadi et al. Additive Manufacturing 59 (2022) 103191
Fig. 11. Schematic illustration of how intra-layer and inter-layer failure in different raster angle.
range, and the application of high pressure during molding leads to fill [90]5, which was one of the main reasons why the mean maximum stress
the mold completely with the material flow in the mold. Consequently, (σm) of [0/90]5 was weaker than [90]5. From Fig. 12g and f, which
strong bonds are created between polymer chains [63]. As a result, belong to [45]5 and [− 45/45]5, respectively, good interlayer adhesion
macro-scale porosities in the HIPS molded specimen are not seen was inferred because the boundary between the layers at the fracture
(Fig. 12h). surface is not very clear. This adhesion was stronger than [90]5 and [0]5
lay-ups. In Figs. 13b and 12c, which are for orthogonal ([0/90]5) and
4.3.1. Porosity diagonal ([0/45]5) lay-up mode, respectively, interlayer bonding was
An important aspect of investigating material fracture is to under clear indicating poor interlayer adhesion in these specimens.
stand the failure mechanisms. Fracture surface morphology generally
includes many features related to the failure process such as failure 4.3.2. Fracture mechanism
mode and failure type [64]. During the material extrusion process, According to the SEM images of the fracture surfaces in Fig. 12 and
various types of defects may occur that affect the mechanical behavior of the qualitative comparison between the specimens, it can be seen that
the 3D printed specimens via material extrusion. The triangular air gaps the [− 45/45]5 specimen (Fig. 12f) has a very rough fracture surface,
(or physical gaps) that form between the layers, also known as the which indicates proof of being the highest value of we [67]. On the other
interlayer porosity, are shown in Fig. 12 (a-d), which belong to [0]5, hand, by observing the fracture surfaces of [0]5 (Figs. 13c and 12a) and
[0/90]5, [0/45]5, [90/45]5 lay-ups, respectively. The shape and size of [90]5 (Figs. 13e and 12e) specimens, it can be seen that [0]5 specimen
these air gaps may vary at different locations depending on the raster has a very smooth fracture surface compared to [90]5 specimen without
angle and the thermodynamic parameters associated with the layer any jagged area. This smoothness of the fracture surface is proof of the
cooling process. Samples with material extrusion defects are prone to lowest values of we for [0]5 specimen [68].
high-stress concentrations that cause cracks to initiate and propagate The Pull-out mechanism was seen for [0]5 lay-up (Fig. 14a), in which
[65]. a thin strand of filament was pulled out during tensile loading. This
Cracks appeared first around triangular air gaps (Fig. 14a), and then mechanism contributes to the fracture toughness through wasted energy
under loading, cracks propagated and caused to fail the specimen [36]. to break and pull out the filament and ductile failure of the material
Intralayer cavities are also known as gas porosity, may be formed by the [69]. The fibrillation was due to continuous stretching and rupture of
shrinkage of the 3D printed specimen during the cooling process from the ligament between the cavities [6,70]. This mechanism caused
molten to solid during the material extrusion process. These cavities also distortion at the fracture surface [64,69]. In Figs. 13e, 14b, 14c, and
create stress concentrations that eventually cause to propagate the 14d, which are related to [90]5, [45]5, [− 45/45]5, [90/45]5 lay-ups,
cracks. The cavities can be minimized by optimizing the material respectively, a molten polymer with a fibrillated structure was observed.
extrusion process temperature, printing speed, and cooling cycle [66]. Fig. 14e (at the 0◦ layer) and 14 g (at the 45◦ layer) show a large area
These cavities and propagated cracks were found in [0]5 (Fig. 13c), of micro-hills on the fracture surface. These micro-hills shows that the
[90]5 (Fig. 13e), [45]5 (Fig. 13d), [- 45/45]5 (Fig. 13a) and [0/90]5 layers are removed by pulling out, not by separating from the adjacent
(Fig. 13b) specimens. layer. Fig. 14h also shows a large area of delamination and roughness on
From Fig. 12e, the interlayer adhesion, of [90]5 was weaker than [0]5 the fracture surface, indicating that the sample underwent simultaneous
(Fig. 12a) lay-up mode, and the main failure mechanism also depended fracture inter-layer and intra-layer mode [61].
on the adhesion between adjacent checkered layers [36]. As observed
from Fig. 12b and e, the interlayer adhesion of [0/90]5 was lower than
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S.A. Sajjadi et al. Additive Manufacturing 59 (2022) 103191
Fig. 12. SEM photography of porosity and fracture surface of DENT for different lay-ups: a) [0]5, b) [0/90]5, c) [0/45]5, d) [90/45]5, e) [90]5, f) [− 45/45]5, g)
[45]5 and f) molded HIPS. Blue arrows indicate triangular air gaps.
13
S.A. Sajjadi et al. Additive Manufacturing 59 (2022) 103191
Fig. 13. SEM photography of fracture surface of DENT for different lay-ups: a) [− 45/45]5, b) [0/90]5, c) [0]5, d) [45]5, and e) [90]5. Yellow arrows indicate intera-
layer cavities and green arrows are Interlayer adhesion.
14
S.A. Sajjadi et al. Additive Manufacturing 59 (2022) 103191
Fig. 14. SEM photography of fracture mechanisms for different lay-ups: a) [0]5, b) [45]5, c) [− 45/45]5, d) [90/45]5, e) [0]5, f) [90/0]5, g) [0/45]5, and h) [− 45/
45]5. Green arrows indicates interlayer adhesion.
5. Conclusions • Results show that [0]5 and [0/90]5 lay-ups had the highest
(23.9598 MPa) and the lowest (15.8924 MPa) strength, respectively.
In this study, the essential work of fracture (EWF) approach was • Measurements for we show that the maximum and minimum value of
utilized to examine the fracture behavior of high impact polystyrene essential work of fracture belonged to [− 45/45]5 and [0]5 lay-ups
(HIPS) processed by additive manufacturing, specifically by the material with values of 10.855 and 1.6338 KJ.m− 2, respectively.
extrusion technique to characterize fracture properties. The influence of • Measurements for βwp show that the highest and lowest value of non-
different raster angles and lay-up modes on the essential and non- essential work of fracture belongs to [0]5 and [0/90]5 lay-ups with
essential work of fracture parameters was investigated. 3D printed values of 2.4357 and 0.4371 KJ.m− 3, respectively.
DENT specimens were produced with eight different infill orientations • By SEM imaging of the fracture surface of the specimens, we found
cases. The main conclusions derived from this research are: that the highest interlayer porosity (triangular air gaps) was for [0]5
lay-up, which also had the lowest value of we. The lowest interlayer
• Self-similarity on the load-displacement curves and confirming the porosity was for [− 45/45]5 and [45]5 ones, which subsequently had
plane stress condition by Sai Hill’s method indicated that the EWF the highest value of we.
procedure was applicable.
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S.A. Sajjadi et al. Additive Manufacturing 59 (2022) 103191
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