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Procedia Manufacturing 48 (2020) 755–762

48th SME North American Manufacturing Research Conference, NAMRC 48, Ohio, USA
48th SME North American Manufacturing Research Conference, NAMRC 48, Ohio, USA
48th SME48th SME
North North American
Fused Filament
American Manufacturing
Research Research
Fabrication
Manufacturing Conference,
of Biodegradable
Conference, NAMRC 48 NAMRC 48, Ohio,
PLA/316L
(Cancelled due toUSA
COVID-19)
Fused Filament Fabrication of Biodegradable PLA/316L
Composite
Fused Scaffolds:
Filament Effects
Fabrication of of Metal Particle
Biodegradable Content
PLA/316L
Composite Scaffolds: Effects of Metal Particle Content
Composite Scaffolds: Effects of Metal Particle Content
Dayue Jiang, Fuda Ning*
Dayue Jiang, Fuda Ning*
Dayue Jiang,
Department of Systems Science and Industrial Engineering, FudaofNing*
State University New York at Binghamton, Binghamton, New York 13902
Department of Systems Science and Industrial Engineering, State University of New York at Binghamton, Binghamton, New York 13902
Department
* Corresponding of Systems
author. Tel.: Science and E-mail
+1 607-777-4793. Industrial Engineering,
address: State University of New York at Binghamton, Binghamton, New York 13902
fning@binghamton.edu
* Corresponding author. Tel.: +1 607-777-4793. E-mail address: fning@binghamton.edu
* Corresponding author. Tel.: +1 607-777-4793. E-mail address: fning@binghamton.edu

Abstract
Abstract
Polylactic acid (PLA) is a biodegradable polymer suitable for fabricating porous scaffolds in bone tissue engineering. Fillers are often added into
Abstract
Polylactic
PLA matrix acid
to (PLA) is acomposite
fabricate biodegradable polymer
scaffolds suitable
in order for fabricating
to improve porous scaffolds
the performance of pureinPLA.
boneIn tissue engineering.
the present study,Fillers are often PLA/316L
we fabricated added into
PLA matrix
composite
Polylactic to (PLA)
acid fabricate
scaffolds is acomposite
with stainless scaffolds
steel
biodegradable in contents
particle
polymer order to from
suitable improve the performance
5 vol% to 15
for fabricating of pure
vol%scaffolds
porous using inPLA.
fused In
filament
bone thefabrication
tissue present study,
(FFF)
engineering. weprocess.
Fillersfabricated
ThePLA/316L
are often effectsinto
added on
composite
PLA matrixscaffolds
dimensions of
topore with
and
fabricate stainless
strut,
composite steel
surface particle
roughness,
scaffolds in contents
as welltoasfrom
order 5 vol%
thermal,
improve to 15 vol%
mechanical,
the performance using
and of fused
in-vitro
pure filament
In thefabrication
degradation
PLA. properties
present (FFF) weprocess.
of the
study, scaffolds The
fabricated effects
were on
studied.
PLA/316L
dimensions
The
composite of pore and
resultsscaffolds
showed that
withstrut,
the surface
dimensional
stainless roughness,
steel accuracy
particle as well
contents asfrom
thermal,
was improved, mechanical,
and
5 vol% tothe and
15surface
vol% in-vitro
roughness
using fused degradation
was tailored
filament properties of the process.
by the addition
fabrication (FFF) scaffolds were
of steelThe studied.
powders
effectsthat
on
The results
were
dimensions showed
dispersedly
of pore thatstrut,
and the dimensional
distributed on the strut
surface accuracy
surface.
roughness, was
asInwell improved,
addition, and
PLA/316L
as thermal, the surface
androughness
composite
mechanical, scaffolds was tailored
exhibited
in-vitro degradation by the
aproperties
lower addition
coefficient of thermal
steel were
of the scaffolds powders that
expansion
studied.
were
The dispersedly
than results
pure PLA,
showeddistributed
while glass
that on the strut
the transition
dimensional surface.
accuracyInand
temperature addition,
was PLA/316L
crystalline
improved, phase
and the composite
transition scaffolds exhibited
temperature
surface roughness waswere nota lower
tailored coefficient
significantly
by the of thermal
affected
addition expansion
by steel
steel powder.
powders that
than
were pure
Moreover, PLA,
dispersedly while
compressive glass
distributed transition
strength
on the temperature
andstrut
elastic Inand
modulus
surface. crystalline
were
addition, enhancedphase
PLA/316L when transition
powder temperature
composite loading
scaffoldswas were
set atnot
exhibited 10 significantly
vol% or
a lower affected
15 vol%.
coefficient by steel
ofIn-vitro
thermal powder.
degradation
expansion
Moreover,
tests pure
than showed compressive
PLA,no while strength
significant
glass and elastic
differences
transition modulus
on degradation
temperature andwere
rates enhanced
between
crystalline when
PLA
phase powder
and loadingcomposite
PLA/316L
transition temperature was were
set atscaffolds.
10 significantly
not vol% or 15 vol%. In-vitro
affected degradation
by steel powder.
tests showed
Moreover, no significant
compressive differences
strength on degradation
and elastic modulus were ratesenhanced
between PLA
whenand PLA/316L
powder loadingcomposite
was set atscaffolds.
10 vol% or 15 vol%. In-vitro degradation
© 2019
© 2020
tests TheAuthors,
The
showed Authors.
no Published
Published
significant by on
Elsevier
by Elsevier
differences B.V. B.V. rates between PLA and PLA/316L composite scaffolds.
degradation
This
© 2019
Peer is The
an open
review access
Authors,
under articleby
the Published
responsibility under thescientific
Elsevier
of the CC
B.V.BY-NC-ND
committeelicense (http://creativecommons.org/licenses/by-nc-nd/4.0/)
of NAMRI/SME
Peer-review
Peer review under
under theresponsibility
responsibility
© 2019 The Authors, Published by Elsevier B.V.of
of the
the Scientific
scientific Committee
committee of of the NAMRI/SME.
NAMRI/SME
Keywords:
Peer reviewPLA scaffolds;
under Metal particle;ofFused
the responsibility filament fabrication;
the scientific committeeBiodegradable
of NAMRI/SME material
Keywords: PLA scaffolds; Metal particle; Fused filament fabrication; Biodegradable material
Keywords: PLA scaffolds; Metal particle; Fused filament fabrication; Biodegradable material

1. Introduction PLA matrix due to the great osteogenesis effect and

1. Introduction PLA matrix due[6,7].
biodegradability to The the great osteogenesis
disadvantage effect and
of ceramic-based
1. Introduction
Polylactide (PLA) is a thermoplastic aliphatic polyester that PLA
fillers, matrix
biodegradability due[6,7].
is the uneven todistribution
the great
The osteogenesis
disadvantage
of ceramic of effect
ceramic-based
powders and
induced
hasPolylactide (PLA) studied
been extensively is a thermoplastic
as a type of aliphatic polyester
bioplastic. that
Recently, biodegradability
fillers,
by the tendency of[6,7].
is the uneven The disadvantage
distribution
agglomeration, of ceramicinof
resulting ceramic-based
powders
poor induced
mechanical
has been extensively
Polylactide
PLA-made (PLA) studied
biodegradable as a type of
is a thermoplastic
scaffolds bioplastic.
aliphatic
have Recently,
polyester
attracted that
much fillers,
by is the
the tendency
properties uneven distribution
of agglomeration,
especially of ceramic[10].
resulting
decreased ductility inpowders induced
poorFurthermore,
mechanical
PLA-made
has been extensively
attention bone studied
inbiodegradable as a type of
tissue scaffolds
engineering bioplastic.
have to Recently,
dueattracted its much
high by the tendency
properties
distorted of
oragglomeration,
especially
shapes decreased
inaccurate resulting
ductility
pore in poor
[10].
dimensions mechanical
Furthermore,
can always be
attention
PLA-made inbiodegradable
processability, bone tissue elastic
suitable engineering
scaffolds havedueattracted
modulus, toandits much
high
great distorted
presentedshapes
properties or inaccurate
inespecially decreased
the ceramic-filled pore
PLA dimensions
ductility [10].
scaffolds, can always
should be
Furthermore,
which
processability,
attention in bone suitable
tissue elastic
biodegradability/bioactivity engineering
[1-3]. modulus,
However, duethetoand its great
high
mechanical distorted
precisely shapes
presented in or inaccurate
the ceramic-filled
controlled pore dimensions
PLA
[7,8]. Given scaffolds, can always
which should be
these disadvantages of
biodegradability/bioactivity
processability, suitable elastic
strength and biocompatibility [1-3]. modulus,
of pureHowever,
PLA needtheto beand great
mechanical
improved presented
precisely
polymer and in the ceramic-filled
controlled
ceramic PLA
[7,8]. inGiven
fillers scaffolds,
these PLA
reinforcing which shouldthe
disadvantages
scaffolds, be
of
strength
in order and biocompatibility
biodegradability/bioactivity
to meet of pureHowever,
[1-3].
the harsh requirements PLAfor need to bemechanical
the
medical improved
implants. polymer
precisely and ceramic
controlled
metallic particle becomesfillers
[7,8]. inGiven
reinforcing
a promising these PLA scaffolds,
because itthe
disadvantages
alternative of
is
in order
strength to
and meet the
biocompatibility
harsh of pure
requirements PLA need
for
Efforts have been attempted to improve the performance to
medicalbe improved
implants.of polymer
metallic and ceramic
particle becomesfillers
a in reinforcing
promising PLA
alternative
more ductile and can be homogeneously distributed in the PLA scaffolds,
because itthe
is
Efforts
in
PLAorder have
to meet
scaffolds been
theattempted
by adding to improve
harsh requirements
fillers, suchfor themedical
as performance
implants.
high-performing of metallic
more particle
matrixductile
[11-13].and becomes a promising alternative
can be homogeneously distributedbecause it is
in the PLA
PLA
Effortsscaffolds
polymers have
[4,5], by attempted
been adding
ceramic fillers,
particles such
to [6-8],
improve etc.as
the high-performing
performance of moreIn ductile
matrix [11-13].
recent and cana be
years, homogeneously
variety distributed
of manufacturing in the have
methods PLA
polymers
PLA [4,5], ceramic
scaffolds
Specifically, by adding particles
polycaprolactone [6-8],
fillers, such
(PCL) etc.asbeen
has high-performing
selected as a matrix
been [11-13].
In utilized
recent years, a variety
to fabricate the of manufacturing
PLA-based methods
composite have
scaffolds,
polymers
potential [4,5], ceramic
Specifically,
polymer particles
polycaprolactone
filler owing [6-8],
(PCL)
to its etc.
great has been selected as
biocompatibility anda beenIn utilized
recent
including years, a variety
to fabricate
molding [14], ofcasting
manufacturing
the PLA-based
solvent methods
composite
[15,16], have
scaffolds,
extrusion [17],
Specifically,
potential polymer
biodegradability polycaprolactone
filler
but theowing
mechanical (PCL)
to its great has been selected
biocompatibility
strength of the PLA/PCLas
anda been utilized
including to[18],
molding
polymerization fabricate
[14], the PLA-based
andsolvent
additive casting composite
[15,16],
manufacturing (AM)scaffolds,
extrusion [17],
[19-21].
biodegradability
potential
composites polymer but theowing
filler
is sacrificed mechanical
[9]. Ceramic strength
to its great
fillers, of the PLA/PCL
biocompatibility
especially and
calcium polymerization
including
AM buildsmolding [18], andsolvent
[14], additivecasting
a three-dimensional manufacturing
object [15,16],
from (AM) [19-21].
extrusion [17],
a computer-aided
biodegradability
composites
phosphate (CaP) but
basedthe[9].
is sacrificed mechanical
Ceramic
fillers, strength
fillers,
are also of the PLA/PCL
especially
incorporated calcium
into the polymerization
AM
designbuilds
model by[18], and theadditive
a three-dimensional
joining manufacturing
object
materials (AM)Due
frombya layer.
layer [19-21].
computer-aided
to its
composites(CaP)
phosphate is sacrificed
based [9]. Ceramic
fillers, fillers,
are also especially into
incorporated calcium
the AM builds
design model a three-dimensional
by joining the materials objectlayer
frombya layer.
computer-aided
Due to its
phosphate (CaP) based fillers, are also incorporated into the design model by joining the materials layer by layer. Due to its
2351-9789 © 2019 The Authors, Published by Elsevier B.V.
2351-9789 ©2019
2351-9789
2020
Peer review©under the
The Authors.
Theresponsibility
Published
of the scientific
Authors, Published
by Elsevier B.V.
committee
by Elsevier B.V. of NAMRI/SME
Thisreview
Peer
is an under
openthe
access article under
responsibility of the
the CCcommittee
scientific
BY-NC-ND license (http://creativecommons.org/licenses/by-nc-nd/4.0/)
of NAMRI/SME
2351-9789
Peer-review© 2019
underTheresponsibility
Authors, Published by Elsevier
of the B.V.Committee
Scientific of the NAMRI/SME.
Peer review under the responsibility of the scientific committee of NAMRI/SME
10.1016/j.promfg.2020.05.110
756 Dayue Jiang et al. / Procedia Manufacturing 48 (2020) 755–762
2 Author name / Procedia Manufacturing 00 (2020) 000–000
benefits in processing geometrically complex structures, AM is
a favorable approach to fabricate scaffolds with desired pore
structures for cell penetration and inhabitation in tissue
engineering applications. Fused filament fabrication (FFF)
advances in its ability to produce complex pore structures at
higher material utilization rate and lower energy cost compared
with other AM technologies such as stereolithography (SLA)
and selective laser sintering (SLS) [22,23]. During the FFF
process, the thermoplastic-based feeding filament is extruded
from a heated nozzle with the beads solidified on the printing
bed, which is desirable for the PLA-based composite scaffolds
fabrication [22]. However, very limited studies have focused on
the FFF of PLA/metal composite scaffolds [12,24].
In the recent work of [12], PLA/Ti composite scaffolds with
a dispersive titanium powder distribution were additively
manufactured using FFF technique. The scaffolds exhibited
enhanced mechanical strength and improved cytocompatibility
due to a higher cell proliferation rate, indicating the
considerable functions of biocompatible metallic-based fillers.
However, this literature did not investigate the biodegradation
behavior of PLA/metal composite scaffolds, and the effects of
different metallic powder contents on their physical properties
such as surface roughness and dimensional accuracy remained
unknown. Compared with titanium, 316L stainless steel also
possesses high strength and good cytocompatibility to allow for
their wide applications in medical scaffolds [25,26]. Because of
the biodegradability of iron-based alloys, fabricating a totally
biodegradable scaffold by adding 316L fillers could be of
greater significance. In addition, the daily tolerance in the
human body for iron is higher than that for Ti [27,28]. However,
few studies have been conducted on the FFF fabrication of
PLA/316L composites [29], wherein the effects of 316L
powder contents on the performance of the PLA-based
composites have not been explored.
In this work, we provide a feasibility study on the fabrication
of biodegradable PLA/316L composite scaffolds with different
steel particle contents using FFF process. The physical
properties including pore size, strut width, and surface
roughness are analyzed to evaluate the dimensional accuracy
and surface quality of the printed scaffolds. The structure,
thermal properties, compressive performance, and corrosion
behavior are also investigated to comprehensively evaluate the
in-vitro performance of the PLA/316L scaffolds. The
completion of this study provides valuable insights into
understanding the effects of steel particle filler contents on the
product performance of the PLA-based composite scaffolds for
potential practical applications.
2. Experimental conditions
2.1. Filament preparation
PLA pellets (4043D, IngeoTM Biopolymer) and 316L
stainless steel powder (EOS, Munich, Germany) (meeting with
ASTM standard F138-12 [30] with a particle size between 20
μm and 50 μm) were mixed in a lab roll ball mill (YLK-Q-5,
Yonglekang Equipment Co., Ltd, Changsha, China) at room
temperature for three hours. Based on the volume ratio of 316L
to PLA, samples were divided into four groups: pure PLA,
PLA5, PLA10, and PLA15, as the number represented the
volume percentage of 316L. After mixing, the powder mixture
was fed into a single-screw extruder (EX2, FilaBot Corp.,
Barre, VT, USA) to fabricate filaments. The extrusion
temperature was 185 ℃, and the screw rotation speed was
dynamically adjusted around 30 RPM to yield a suitable flow
rate. Fan airpath was also applied to provide forced convection
to cool filament for a uniform filament diameter of 2.85±0.15
mm.
2.2. Scaffold fabrication
The FFF process was conducted on a desktop 3D printer
(TAZ 6, Lulzbot Corp., Colorado, USA) with a single extruder
tool head. Fig. 1 illustrates the 3D printer and designed three-
dimensional porous scaffold to be fabricated in this work.
Specifically, the extrusion nozzle initially deposited a group of
eight parallel struts with a four-layer height. Each strut owns
both width and height of 0.8 mm. After that, the printing
orientation was alternated by 90° followed by layering another
eight struts. Thus, a total of 60 layers were deposited to create
a cube with a side length of 12 mm, and an interconnected pore
dimension of 0.8×0.8×0.8 mm. The main process parameters
for this sample fabrication are listed in Table 1.
(a)
(b)
Filament
Motor
Cooling fan
Printing bed
Cooling fan Nozzle
Fig. 1. (a) Lulzbot TAZ 6 3D printer; (b) 3D structure of PLA-based
scaffolds. (D1 = D2 = 0.8 mm, L = W = H = 12 mm)
Table 1. FFF process parameters for PLA-based scaffolds fabrication.
Parameters Value
Nozzle Temperature 205 ℃
Bed Temperature 70 ℃
Printing Speed 60 mm/s
Filament Diameter 2.85±0.15 mm
Layer Height 0.2 mm
Infill Density 50 %
Nozzle Size 0.5 mm
2.3. Geometrical and structural characterizations
Dimensions and surface roughness of the struts were
measured using a 3D structural light profilometer (VR-3000,
Keyence Corp., Itasca, USA). A graphical description of the
measuring methodology is presented in Fig. 2. The pore size
was determined by measuring its length and width (D1) in the
side view and the strut width (D2) was measured in the top view,
as shown in Figs. 2(a) and 2(b), respectively. The side view
allowed for higher accuracy in measuring the pore size because
struts were built in the same plane. The parameter Sa was used
 Dayue Jiang et al. / Procedia Manufacturing 48 (2020) 755–762 757
Author name / Procedia Manufacturing 00 (2020) 000–000 3

to evaluate the areal surface roughness of the strut in the top
view. Three samples were measured and a total number of 24,
120, and 12 statistical data were collected in each group for
strut width, pore size, and surface roughness, respectively.
Then the results were analyzed by the ANOVA methodology
using the Minitab 19 software, with Tukey’s methods
incorporated to compare between each two groups. The surface
morphologies of the prepared filament and fabricated scaffold
were observed by a scanning electron microscopy (SEM)
(Supra 55VP, ZEISS Corp., Oberkochen, Germany). Prior to
the observation, carbon coating was conducted on the sample
surface to increase conductivity.
(a)
0.959
0.797
with the ramping rate of 5 ℃ per minute. The result data was
processed by the software of TA Universal Analysis.
2.5. Mechanical property testing
The compression test was conducted on a universal tester
(Instron 3334, INSTRON Corp., Norwood, USA) in
accordance with the ASTM D1621 standard [31] to evaluate
the compressive properties of the as-built scaffold. Five
samples for each group were compressed to at least 20%
deformation with a rate of 0.1 mm per second. Compressive
strength and modulus were calculated from the plotted stress-
strain diagram. The surface morphology of the sample after the
compression test was also observed by SEM.

2.6. In-vitro biodegradation testing

0.936 Biodegradation properties were evaluated by an immersion

test at 37±0.5 ℃ in phosphate-buffered saline (PBS)
0.843

(ThermoFisher Scientific, Waltham, USA) following the

Units: mm
standard of ASTM NACE/G31 [32]. The initial pH value of the
PBS solution was 7.4. Three samples for each group were
(b)
immersed for 7 days, and another three samples in the same
group were immersed for one month. Before and after the
immersion test, samples were completely dried in a 50 ℃
incubator for 12 hours, and the weights were measured
0.736 0.736 0.717 0.787 0.762 accordingly. Structural and surface morphology after the
immersion was also characterized by SEM.

3. Results and discussion

Units: mm 3.1. Dimensions and surface roughness

Fig. 2. Illustration of dimensional measurements for the PLA scaffolds: (a)
side view of pure PLA; (b) top view of pure PLA
2.4. Thermal property analysis
Thermal gravimetric analysis (TGA) (Q50, TA Inc., New
Castle, USA) was conducted on the filament to evaluate the
thermal stability and actual composition of different samples.
The temperature ranged from room temperature to 500 ℃, with
a ramping rate of 10 ℃ per minute. The glass transition
temperature Tg, crystalline phase transition temperature Tc, and
the coefficient of thermal expansion (CTE) were determined by
thermal-mechanical analysis (Q400, TA Inc., New Castle, USA)
Fig. 3 shows the boxplots for pore size, strut width, and
surface roughness Sa consisting of maximum, mean, median,
upper quartile, lower quartile, and minimum values. The
related statistical results are listed in Table 2. In Fig. 3(a), the
mean pore size within the pure PLA scaffold is 0.88 mm, which
is larger than the designed value of 0.8 mm. For the PLA/316L
composite scaffolds, the mean pore size significantly decreases,
which is closer to the designed one. Under different 316L
powder contents, the mean pore size follows the order in PLA5 >
PLA15 > PLA10. On the other hand, PLA/316L scaffolds show
a larger mean strut width than pure PLA in Fig. 3(b), and
PLA10 group exhibits the largest value compared with other
groups. The mean pore size and mean strut width could be

Table 2. Statistical results of pore size, strut width, and surface roughness (For Tukey’s comparison method, means that do not share a letter are significantly
different, α = 0.05)
Category Pore size / mm Strut width / mm Surface roughness / μm
Vol % of 316L 0 5 10 15 0 5 10 15 0 5 10 15
Mean 0.88 0.80 0.78 0.80 0.72 0.81 0.91 0.84 0.09 0.03 0.04 0.009
StDev 0.07 0.07 0.05 0.04 0.07 0.09 0.06 0.07 0.03 0.02 0.02 0.003
P-value < 0.0001 < 0.001 < 0.001
Tukey’s Grouping A B C B/C A B C B/C A B B C
758 Dayue Jiang et al. / Procedia Manufacturing 48 (2020) 755–762
4 Author name / Procedia Manufacturing 00 (2020) 000–000
inversely linked because a wider strut would narrow the pore
space, which is consistent with our experimental results.
The measured results of surface roughness are provided in
Fig. 3(c). The average surface roughness Sa of pure PLA
scaffold is 0.09 mm. After adding the steel powders at 5 vol%
and 10 vol%, the surface roughness is tailored to 0.03 mm and
0.04 mm, respectively, but no statistical difference is found
between these two groups. As the steel powder load further
increases to 15 vol%, a significantly lower average surface
roughness of 0.009 mm with a standard deviation of 0.003 mm
is obtained.
(a)
Pore size (mm)
(b)
Strut width (mm)
(c)
Sa (mm)
Fig. 3. Effects of 316L particle content on (a) pore size, (b) strut width, and
(c) surface roughness in the PLA-based scaffold built by FFF.
PLA/316L scaffolds show better dimensional accuracy and
lower surface roughness than pure PLA. The pore size and strut
width could be influenced by various important factors during
the printing process. The results indicate that the addition of
316L powders significantly changes the physical properties of
pure PLA. Generally, pore size is one of the most important
characteristics in bone tissue scaffolds, which can not only
determine the loading capability and modulus matching but the
mass transfer and cell growth accommodation [22]. A good
average pore size lies in the range of 300 to 900 μm, and it is
better to fabricate the pore with less standard deviation.
Homogenous distribution of pores could facilitate continuous
tissue growth and prevent clogging in some regions of the
scaffolds, thus accelerating the healing process. For the surface
roughness, it is found in the literature that a rougher surface
could assist cell adhesion and growth because a higher surface
fluctuation could provide more space for tissue spreading and
remodeling, thus promoting a better cytocompatibility for the
scaffolds [33,34]. However, another result shows that the cell
adhesion could not be solely determined by surface roughness,
but more by the surface energy, as evidenced by the optimal
cell adhesion is obtained in small roughness ratios [35].
3.2. Structural characterization
Fig. 4(a) illustrates the SEM morphology of PLA5 filament.
It is notable that the texture on the PLA5 filament surface is
elongated because of the extrusion and several small cracks are
observed. Those cracks may be induced due to the friction
between the nozzle and filament. Another reason for cracking
might be the unstable fan cooling during the extrusion process,
leading to stress concentration in some areas on the surface and
producing cracks. Those cracks would reduce the elongation of
the filament, which ultimately affects the printing
processability of the filament. Generally, the surface of PLA5
filament is smooth but a better cooling strategy should be
considered.
(a) (b)
Cracks
316L
10 μm 100 μm
(c) (d)
Gaps
Voids
Voids
Agglomeration
100μm 100μm
Fig. 4. Surface morphologies of (a) PLA5 filament; (b) PLA5 scaffold; (c)
PLA10 scaffold with voids observed; and (d) PLA15 scaffold with voids and
gaps observed.
Figs. 4(b) to 4(d) represent the SEM images of PLA/316L
scaffolds with different powder contents. Dispersed steel
powders (marked in Fig. 4(b)) could be observed on the surface
of struts. As seen in Fig. 4(b), the steel powders are fully
covered by PLA and no considerable agglomeration is
discovered, indicating a homogeneous distribution of PLA and
316L steel powders at 5% volume fraction. However, when the
steel powder load increased to 10 vol%, voids are found in
 Dayue Jiang et al. / Procedia Manufacturing 48 (2020) 755–762 759
Author name / Procedia Manufacturing 00 (2020) 000–000 5

some regions within a single layer. After the powder loading volume of shrinkage could be obtained in PLA5 and PLA15,
increases to 15 vol%, agglomeration of powders and large gaps so the mean strut width of PLA5 or PLA15 is smaller than that
are observed between layers as shown in Fig. 4(d). The of PLA 10. However, it can be considered that the detachment
generation of voids is associated with the entrapment of steel of PLA/316L composite layers contributes more to increasing
powders into the flow of the melting PLA polymer. Steel the mean strut width to the level that the volume shrinkage can
powders are thermodynamically stable at printing temperature be ignored.
around 205 ℃, thus impeding the polymer movement or even
cutting the melting PLA matrix during the printing process. (a)
This phenomenon is not remarkable during the filament
extrusion because the filament has a relatively large dimension
(2.85 mm). In the printing process, however, the one-layer
depositing height is only 0.2 mm which is much closer to the
diameter of steel powders, resulting in a larger portion of voids
when the powder loading was 10 vol% or 15 vol%. Large gaps
between layers are found in PLA15, which might be caused by
the contact of steel powders between layer surfaces. Those
contact could weaken the surface adhesion so that the adjacent
layer could be detached to generate large gaps.
The existence of steel powders significantly contributes to
changes in the dimensions and surface roughness of the
scaffolds. According to the SEM images, gaps are generated
between layers, which could be the main cause in the increase (b)
of mean strut width that narrows down the mean pore size.
Tc
However, within the PLA/316L groups, PLA10 composite
scaffolds exhibit the highest mean strut width. This could be
explained by the varied thermal properties that will be
discussed later. On the other hand, because of the entrapment
effect of steel powders, the melting flow PLA matrix is
inhibited and smaller surface roughness of PLA/316L struts is
thus obtained.

Tg
3.3. Thermal properties

Fig. 5 depicts the TGA and TMA curves of PLA/316L

composites with different 316L contents. As shown in TGA
curves, the actual powder composition is close to the nominal Fig. 5. (a) TGA curves and (b) TMA curves of PLA-based scaffolds with
value, and a higher starting decomposition temperature is found different 316L contents.
in pure PLA sample. Table 3 lists the glass transition
Table 3. Thermal properties of PLA-based scaffolds
temperature (Tg), crystalline phase transition temperature (Tc),
and the coefficient of thermal expansion (CTE) measured from Category PLA PLA5 PLA10 PLA15
TMA curves. Tg and Tc points are marked in Fig. 5(b) and the Tg / ℃ 65.29 63.29 63.3 63.68
CTE is measured from the largest tangent slope in the
Tc / ℃ 101.12 98.89 98.2 99.28
temperature range from Tg to Tc for each curve. It can be noted
CTE / μm/(mm×℃) 13.0 8.3 5.0 6.8
that Tg and Tc of PLA are not significantly affected by the
addition of steel powders because of their thermodynamic
stability within the temperature range. However, the CTE of 3.4. Compressive properties
the PLA/316L composites was decreased due to the impeding
effect of the metallic powders against the expansion of the PLA Representative compression strain-stress curves of the FFF-
matrix. Such an effect is the strongest in the PLA10 composite built scaffolds are shown in Fig. 6. The compressive modulus
scaffolds and gets weakened when adding 15 vol% 316L and compressive strength are listed in Table 4. From the strain-
powders. This could be caused due to the agglomeration of stress curves, the initial elastic deformation stage could be
316L particles at 15 vol% that results in a non-uniform thermal determined for all samples, but the yield points for PLA and
expansion. It should be noted that the strut width for pure PLA PLA5 could not be clearly identified. Following the instruction
scaffold is less than 0.8 mm, which could stem from the highest of ASTM D1621, the compressive strengths for all samples are
volume shrinkage of PLA under the cooling process. With a measured in the stress at 10% strain. Both compressive
higher CTE, the volume change of material per Celsius could modulus and strength are enhanced for PLA scaffolds by
be larger during heating or cooling process. On the other hand, adding 316L powder fillers. Within the group of PLA/316L
for the FFF-built PLA/316L composite scaffolds, a larger composites, the highest elastic modulus is obtained in PLA10
760 Dayue Jiang et al. / Procedia Manufacturing 48 (2020) 755–762
6 Author name / Procedia Manufacturing 00 (2020) 000–000

which is approximately six times higher than pure PLA5. This (a) (b)
result shows that adding stainless-steel powder could increase
the stiffness of PLA, and the effect is more significant when the 200 μm 200 μm
volume percentage of steel powder exceeds 10%. But for the
group of PLA15, more voids are generated in the matrix
resulting in a decline of modulus. As for compressive strength,
600 μm
higher strength is also obtained in the group of PLA10, whereas 600 μm

the PLA5 exhibits a similar plastic deformation behavior with (c) (d)
PLA. PLA15 exhibits slightly lower compression strength than
PLA10, which also could be ascribed to the existence of voids 100 μm
100 μm

and agglomeration of powders. However, the yield points for

PLA10 and PLA15 are achieved at a lower strain, suggesting a
smaller compressive elongation for these groups.
600 μm 600 μm

Fig. 7. SEM images of (a) PLA; (b) PLA5; (c) PLA10; and (d) PLA15
scaffolds after compression test.

3.5. In-vitro degradation properties

In order to evaluate the biodegradation properties of

PLA/316L scaffolds, in vitro immersion tests were conducted
in PBS solution at 37±0.5 ℃. After one-month immersion, the
results of pH value and sample weight change are listed in
Table 5. There is not much difference that can be detected by
the results of pH value and weight change between groups.
PLA naturally degrades in simulated body fluid by hydrolysis
where the reaction is:

Fig. 6. Strain-stress curve from compression test of PLA-based scaffolds. - COO + H 2O → −COOH + −OH

Table 4. Compressive properties of PLA-based scaffolds

Generally, the degradation of PLA causes the pH value to drop
Groups Modulus / GPa Compressive strength / MPa but in PBS solution, the pH value remains stable [36]. No large
PLA 0.22±0.03 15.73±2.13
weight change of samples is observed after immersion for one
PLA5 0.28±0.05 21.35±3.54
month, which might be due to the low degradation rate of 316L
PLA10 1.51±0.04 39.08±4.32
in the PBS solution. Three of the four groups exhibit larger
PLA15 0.77±0.07 30.91±6.05
weight after immersion because the degradation products on
the scaffold surface and inside the pores could be hardly
eliminated, so well as the oxide product of 316L powder.
Fig. 7 illustrates the structures of different scaffolds after
compression tests. Because of low modulus, bending and Table 5. Change of pH value and weight after immersion in PBS for one
fracture occur in PLA struts, as shown in Fig. 7(a). Compared month
with pure PLA scaffold, the PLA/316L composites are more Groups pH value Weight/g
resilient to compressive force. The bending of struts is also Before After Before After
found in the group PLA5, suggesting similar deformation PLA 7.4 7.0 0.71 0.80
behavior with PLA and is consistent with the results of strain- PLA5 7.4 7.2 1.29 1.35
stress curves. No obvious bending or cracking is observed for PLA10 7.4 7.0 1.41 1.45
PLA10 and PLA15 because of higher compressive strength. It PLA15 7.4 7.0 1.50 1.55
should be noted that gaps in the composite scaffolds may not
influence the compressive strength because those gaps are Fig. 8 shows the morphologies of the PLA and PLA10
eliminated during the compressive displacement. As shown in scaffolds after immersion for one week and one month. As for
the high-magnification image in Fig. 7(c), the gaps are filled by PLA, the delamination of struts and layers could be observed
compression with several bulges observed. Those bulges could after one-week immersion as a result of the weak inter-layer
be related to the agglomeration of steel powders, which connection [9] that hastens the degradation in additively
promote the generation of extra resistance against the manufactured scaffolds. The modulus and strength may drop
compressive force. In the high-magnification image of PLA15, rapidly because of those disconnections. After immersed in
more voids are formed because of the exfoliation of steel PBS for one month, swelling occurs due to the penetration of
powder. Thus, compressive strength for PLA15 is lower than PBS solution between the layers. It also can be seen that the
that of PLA10. corrosion product is accumulated between layers rather than on
the layer surfaces. On the other hand, PLA/316L composite
 Dayue Jiang et al. / Procedia Manufacturing 48 (2020) 755–762
Author name / Procedia Manufacturing 00 (2020) 000–000
scaffolds exhibit no fracture or disconnection in the one-week
immersed sample, whereas swelling is still observed given the
voids formed during the printing. For the PLA10 sample
immersed in PBS for one month in Fig. 8(d), delamination is
presented, which could be generated by the gaps, while the
316L powders remain intact suggesting a high corrosion
resistance. Based on the results of pH value, weight change,
and corrosion morphology, no significant effects could be
found on the degradation rate and the corrosion behavior after
adding 316L into the PLA matrix.
Fig. 8. SEM images of PLA-based scaffolds immersed in PBS for different
immersion times.
4. Conclusions
This work studied PLA/316L composite scaffolds with
different metal contents fabricated by fused filament
fabrication. The physical properties, meso-structure and their
thermal, mechanical, and in-vitro degradation properties of the
scaffolds were investigated. The detailed conclusions are
drawn as follows:
• The higher dimensional accuracy based on the mean pore
size and mean strut width was obtained by PLA/316L
composite scaffolds, and the addition of 316L powder also
decreased the surface roughness. The lowest surface
roughness was obtained when the steel powder loading was
at 15 vol%.
• 316L powders were dispersedly distributed in the struts
when the volume fraction was under 10%. For steel powder
loading higher than 10 vol%, voids within a layer, gaps
between two layers and powder agglomeration were
observed.
• The addition of 316L powder decreased the coefficient of
thermal expansion of the PLA composite scaffolds, leading
to the higher dimension accuracy and lower surface
roughness. The adding of 316L in 10 vol% most effectively
enhanced the compressive modulus and strength of the
scaffolds.
• Swelling and delamination of the layers were found in PLA
and PLA/316L scaffolds in the immersion test for one
month, but no considerable differences were discovered in
the effects of 316L powder on the degradation behavior of
the PLA/316L scaffolds.
761
7
Acknowledgments
This work has been supported by the start-up funds from
Thomas J. Watson School of Engineering and Applied Science
at State University of New York at Binghamton, USA. The
authors also would like to acknowledge the support (Grant#
ADLG196) from the Small Scale Systems Integration and
Packaging (S3IP) Center of Excellence, funded by New York
Empire State Development’s Division of Science, Technology
and Innovation.
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