polymers

Article
Influence of 3D Printing Conditions on Some
Physical–Mechanical and Technological Properties of PCL
Wood-Based Polymer Parts Manufactured by FDM
Irina Bes, liu-Băncescu 1, *, Ioan Tamas, ag 1, * and Laurent, iu Slătineanu 2

1 Faculty of Mechanical Engineering, Automotive and Robotics, “Stefan cel Mare” University,
720229 Suceava, Romania
2 Faculty of Machine Manufacturing and Industrial Management, “Gheorghe Asachi” Technical University of
Iasi, 700050 Ias, i, Romania; [email protected]
* Correspondence: [email protected] (I.B.-B.); [email protected] (I.T.); Tel.: +40-744322449 (I.B.-B.);
+40-741564971 (I.T.)

Abstract: The paper investigates the influence of some 3D printing conditions on some physical–
mechanical and technological properties of polycaprolactone (PCL) wood-based biopolymer parts
manufactured by FDM. Parts with 100% infill and the geometry according to ISO 527 Type 1B were
printed on a semiprofessional desktop FDM printer. A full factorial design with three independent
variables at three levels was considered. Some physical–mechanical properties (weight error, fracture
temperature, ultimate tensile strength) and technological properties (top and lateral surface roughness,
cutting machinability) were experimentally assessed. For the surface texture analysis, a white light
interferometer was used. Regression equations for some of the investigated parameters were obtained
and analysed. Higher printing speeds than those usually reported in the existing literature dealing
with wood-based polymers’ 3D printing had been tested. Overall, the highest level chosen for the
printing speed positively influenced the surface roughness and the ultimate tensile strength of the
3D-printed parts. The cutting machinability of the printed parts was investigated by means of cutting
Citation: Bes, liu-Băncescu, I.; force criteria. The results showed that the PCL wood-based polymer analysed in this study had lower
Tamas, ag, I.; Slătineanu, L. Influence machinability than natural wood.
of 3D Printing Conditions on Some
Physical–Mechanical and
Keywords: wood-based biopolymer; surface quality; tensile strength; machinability
Technological Properties of PCL
Wood-Based Polymer Parts
Manufactured by FDM. Polymers
2023, 15, 2305. https://doi.org/
1. Introduction
10.3390/polym15102305
The ability to quickly generate complex surfaces and structures at lower costs and sig-
Academic Editors: Cristina-Elisabeta
nificantly lower material losses in the case of traditional mechanical processing technologies
Pelin and Anton Ficai
recommend 3D printing technologies for many industrial applications. There are several
Received: 29 April 2023 types of 3D printing processes, such as selective laser sintering (SLS), stereolithography
Revised: 10 May 2023 (SLA), multi-jet fusion (MJF), digital light processing (DLP), digital light processing (DLP),
Accepted: 12 May 2023 fused deposition modelling (FDM), etc. FDM, also known as MEX (Material Extrusion) [1],
Published: 14 May 2023 is one of the most commonly used 3D printing processes because of the wide range of
materials that can be processed/manufactured. The FDM process input parameters, such
as the layer thickness, wall shell thickness, printing temperature, infill structure, infill
density percentage, and printing speeds, strongly influence the mechanical proprieties of
Copyright: © 2023 by the authors.
the printed products.
Licensee MDPI, Basel, Switzerland.
FDM is an emerging technology implemented in sectors such as the automotive,
This article is an open access article
aerospace, medical, architecture, fashion, and food industries [2]. The main drawbacks
distributed under the terms and
reported for these technologies are the anisotropic nature and poor mechanical properties
conditions of the Creative Commons
Attribution (CC BY) license (https://
of the 3D-printed parts [2]. The principle of this manufacturing technique is that the wire
creativecommons.org/licenses/by/
material is heated and deposited layer by layer into the desired part shape. The part
4.0/).
material must be pre-processed by hot melt extrusion to be transformed into filaments.

Polymers 2023, 15, 2305. https://doi.org/10.3390/polym15102305 https://www.mdpi.com/journal/polymers

Polymers 2023, 15, 2305 2 of 21

The literature provides multiple studies that analyse the influence of printing con-
ditions and parameters and post-processing methods on the mechanical properties of
3D-printed parts, especially FDM [3–11]. Several researchers have contributed with com-
prehensive reviews on these issues [12–14]. Furthermore, the subject continuously develops
due to the increasing interest in different industries, requiring more attention from the
scientific community.
Voids usually appear between the deposited filament layers in the FDM printing
process. These voids are believed to be one of the main causes of low tensile strength and
anisotropy [15] and may also affect the 3D-printed parts’ cutting machinability. In the case
of WPC (wood-based composite polymer) 3D-printed parts, it had been considered that
wood fibres might encourage void formation. Comparing unfilled printed specimens with
reinforced ones with natural fibres has shown a negative influence of the fibres on strength,
while stiffness either increases slightly or remains constant [16].
The use of wood is increasing due to the growth of the world population, the de-
velopment of new wood products, and the identification of new applications in various
fields. Wood is a renewable and carbon-storing resource [16] with excellent properties but is
limited to forest land. In recent decades, the wood demand increased significantly and over-
came disposable supplies. Sustainability targets and growing environmental concerns have
increased the demand for renewable and recyclable materials with compatible proprieties
and behaviour/performance. In recent years, wood-based composite polymers (WPCs)
have been gaining popularity [15,17–19]. These materials are composed of one or more
natural wood chips, fibres, or flours and one or a mixture of polymers, most commonly
thermoplastic polymers such as polyethene (PE), polylactide (PLA), or polypropylene (PP).
Compared to natural timber products, WPCs present higher resistance to weathering and
biological deterioration, thermal resistance, and expose sufficient strength for structural
applications [20]. WPCs are mainly used for outdoor and indoor furniture, window and
door frames, moulding, different construction purposes, and the automotive and marine
industries [15,18,21]. The main drawbacks are the slightly higher prices and lower thermal
resistance compared to natural wood.
The mechanical performance of WPCs is the main objective addressed by research
in this field. Most of the research dealing with wood-based polymers analyses some
mechanical proprieties for commercially available filaments [22,23] or develops and tests
new wood composite filaments by mixing different amounts and types of wood fibres,
polymers, additives, and fillers [15,16,24–29].
The most popular wood-based polymer type is obtained with a polylactic acid (PLA)
polymer matrix and different percentages of wood fibres, dust, or chips. The performance of
WPC material can be enhanced by using a proper combination of polymers and providing
different fillers and additives. The research carried out in this field showed that beech
sawdust can contribute to the reinforcement of flexural stress and tensile strength and
that sawdust also helps reduce WPC density [21]. Additionally, WPCs are often brittle.
Styrene and butadiene rubber (SBR), ethylene-propylene monomers leather (EPDM), or
plastic elastomers can be used for toughening purposes [18]. Because of their strong
flammability level, flame retardants, usually polyphosphate (APP), must be provided in
their composition [19]. The addition of lignocellulosic fibres to WPC filaments was reported
to lower the mechanical proprieties of the 3D-printed composites [27].
Hydrothermal degradation tests were performed [27] to establish its effect on the
mechanical properties. The results showed that adding natural fillers and different levels
of infilling resulted in a similar level of reduction in the properties. Additionally, the
addition of natural fillers resulted in a slightly lower drop than the lowered infilling rate
for tensile strength [27].
Results from another study [30] indicated that thickness swell, water uptake, mechani-
cal strength, and stiffness increased, and elongation at break and impact energy decreased
with an increasing wood fibre proportion.
Polymers 2023, 15, 2305 3 of 21

The influence of the shape of wood particles on the mechanical proprieties of WPCs
was also investigated. Huang et al. [29] showed that the shape and surface roughness of
the wood particles, rather than the wood species, play an essential role in determining the
properties of 3D-printed WPC products. Additionally, it was reported that wood particles
with more rounded shapes and smoother surfaces are more suitable for obtaining a denser
and stronger 3D-printed WPC product [29].
The machinability of wood–plastic composites has been approached by a relatively
small number of studies. Most of these studies were carried on parts generated by other
machining processes than 3D printing. Zhu et al. [31] explored the cutting performance of
wood–plastic composites based on cutting forces, cutting temperature, surface quality, chip
formation, and tool wear during peripheral milling experiments using cemented carbide
cutters. The wood–plastic composites tested were processed by extrusion, moulding, and
injection moulding. WPPC exhibited the highest cutting forces and cutting temperatures
under the same cutting conditions, followed by WPEC and WPVCC. Wu et al. [32] had
studied the helical milling performance of the WPC obtained by mixing poplar flour and
polyethylene followed by extrusion at high temperatures. They reported that in WPC
helical milling, the cutting force increases with increased spindle speed, cutting depth, and
tool helical angle.
Biopolymers have attracted increased attention in recent years mainly because of
their abundant and sustainable sources and versatile properties [2]. Biowood, produced
by Rosa3D, is a wood-based composite biopolymer. The main components of Biowood
filament are polycaprolactone (PCL), polyester, starch, lignin, natural resins, waxes and
oils, natural fatty acids, cellulose, and natural fibres [33]. Polycaprolactone (PCL) is a
biodegradable polyester with a low melting point of 60 ◦ C [25] that is usually blended
with other polymers. Studies [25] showed that natural fibres generally enhance poly-
caprolactone’s biodegradability and mechanical proprieties. Combining cellulose with
polycaprolactone increased the tensile modulus but decreased the tensile strength of the
composites [25]. Lignin is a natural polymer that binds cellulose fibres together, assuring
stiffness for the wood-based polymer composites. Starch is not only used for binding and
as a glue agent. The blending of starch with plastics has been reported to improve water
resistance, processing properties, and mechanical properties [27].
Zgodavová K. et al. [23] have tested different thermoplastic materials for printing
shield frames in terms of mechanical properties, geometric accuracy, weight, printing time,
filament price, and environmental sustainability. Among them, they tested PHABiowood
Rosa3D. The input parameters considered were the layer thickness, number of perimeters,
extrusion width, infill density, and nozzle temperature. The tensile stress of the PHA
Biowood varied from 10.8 MPa to 21.8 MPa, and the factors with significant influence over
the mechanical properties were the infill and the interaction between the layer height and
printing infill.
The aim of this paper was to highlight the results of some experimental studies dealing
with the influence of some specific factors that characterise the 3D printing conditions of
PCL wood-based polymer parts on some physical–mechanical and technological properties
of the material incorporated in those parts. As input factors of the 3D-printing process,
printing temperature, layer height, and printing speed were considered. Some physical–
mechanical properties (weight error, fracture temperature, ultimate tensile strength) and
technological properties (top and lateral surface roughness, cutting machinability) consti-
tuted output parameters that were subjected to the analysis. This study’s novelty consists
in analysing the influence of some printing parameters (printing temperature, layer height,
and printing speed) on some of the qualitative aspects and mechanical proprieties of the
Biowood Rosa3D wood-based biopolymer parts generated by FDM. The values selected for
the printing speed parameter were significantly superior to those usually tested in previous
research in this field or those recommended by the filament producer. Another novelty
aspect of this study is the slot milling machinability analysis by means of cutting force
levels of the FDM-printed parts.
 usually tested in previous research in this field or those recommended by the filament
producer. Another novelty aspect of this study is the slot milling machinability analysis
Polymers 2023, 15, 2305 4 of 21
by means of cutting force levels of the FDM-printed parts.
Even if complex shape parts can be generated by additive manufacturing, there are
several situations where 3D-printed parts may require future processing.
Even
The useif of
complex
cuttingshape parts can beprocessing
as a secondary generated operation
by additive manufacturing,
for 3D-printed partsthere
canaread-
several situations where 3D-printed parts may require future processing.
dress for parts with high functional and tolerance requirements. Usually, the FDM parts
The use of cutting as a secondary processing operation for 3D-printed parts can
achieved accuracies of ±0.5mm for desktop printers and ±0.2mm for industrial printers,
address for parts with high functional and tolerance requirements. Usually, the FDM parts
and with CNC machining, accuracies of ±0.05mm can be obtained.
achieved accuracies of ±0.5 mm for desktop printers and ±0.2 mm for industrial printers,
andAnother
with CNC reason for combining
machining, accuraciesthe
of ±two
0.05technologies is productivity. Even with the
mm can be obtained.
recentAnother
advancements
reason infor3D-printing technology,
combining the printingisspeed
two technologies is still a Even
productivity. majorwith
drawback
the
for considering these technologies for industrial applications. By considering
recent advancements in 3D-printing technology, printing speed is still a major draw- cutting tech-
nologies for some of the part features, the machining time of the parts can be
back for considering these technologies for industrial applications. By considering cut- significantly
improved.
ting technologies for some of the part features, the machining time of the parts can be
This study
significantly can be a starting point for other researchers that aim to establish the
improved.
properThis study conditions
printing can be a starting pointwood-based
for PCL for other researchers
polymers that aim
and fortoindustry
establish agents
the proper
inter-
printing conditions for PCL wood-based polymers
ested in developing biodegradable wood-like products. and for industry agents interested in
developing biodegradable wood-like products.
2. Experimental Setup
2. Experimental Setup
In Figure 1, a schematic representation of the experimental program used in the study
In Figure 1, a schematic representation of the experimental program used in the
isstudy
presented. The model offers information about the input parameters, equipment, pro-
is presented. The model offers information about the input parameters, equipment,
cedures,
procedures, and investigated
and the parameters
the investigated considered
parameters inin
considered the
thestudy.
study.

Figure
Figure1.1.Schematic
Schematicrepresentation of the
representation of the experimental
experimentalprogram.
program.
Polymers 2023, 15, 2305 5 of 21

The parts, in the form of test specimens with dimensions according to ISO 527-2 1B,
were manufactured using a BambuLab X1C 3D printer and then tested and analysed from
four perspectives:
1. Surface quality by obtaining values for surface roughness (Sq) using a Mahr CWM
100 profilometer;
2. Tensile strength, obtaining values for UTS but also for the temperature at the time of
specimen rupture;
3. Analysis of the density variation of the resulting parts in terms of weight;
4. Machinability of the parts, where the values for the components Fx, Fy, and Fz of the
cutting force were obtained using a Kistler type 9257B dynamometer.
A full factorial experiment was considered to achieve the desired research objectives.
The independent variable factors that were changed in the experimental procedure were
the following: the printing temperature Tp (◦ C), the layer height, hl (mm), and printing
speed, sp (mm/s). The values of the input factor levels selected in this study for each of
them are presented in Table 1.

Table 1. Values of the input factors corresponding to the full factorial design.

Input Parameters
Level Printing Layer Height hl Printing Speed sp
Temperature Tp (◦ C) (mm) (mm/s)
1 175 0.2 150
2 190 0.28 200
3 220 0.4 300

The results obtained under experimental conditions according to the DOE 33 factorial
design, were analysed to obtain variation plots, and then ANOVA was applied to determine
the factors with statistically significant influence.
As output interest parameters of the proposed study, the following parameters
were considered:
- Weight error (%);
- Arithmetical mean height, Sa (µm) of the top and lateral surfaces of the specimens;
- Ultimate tensile strength UTS (MPa);
- Fracture temperature T (◦ C);
- Cutting force components Fx (N), Fy (N), and Fz (N).
The advancements in 3D printing equipment have opened new opportunities in terms
of reducing the printing time. The producers of 3D printers have focused on addressing one
of the main drawbacks of additive manufacturing technologies, which is the printing time.
Printing time is directly proportional to the printing speed that can be achieved. Therefore,
in recent years, new 3D printers with higher printing speed facilities were produced. Even
if high printing speeds can be achieved by using these new 3D printers available in the
market, the testing of these capabilities is still limited. In this study, significantly higher
printing speeds than those usually reported in the scientific literature were considered.
The factor levels were chosen to preserve the randomness of the results. In the case of
temperature, the minimum level was chosen to be 175 ◦ C, the second level 190 ◦ C, which is
most often used in FDM 3D printing especially for biopolymers (such as PLA—polylactic
acid), and 220 ◦ C, 10 ◦ C more than the manufacturer’s recommendation.
In terms of layer height, level 1 of 0.2 mm was chosen because it is the most common
in the literature, 0.4 mm because the nozzle used has a diameter of 0.6 mm (dimensions
suggested by the filament manufacturer), and the layer height represents under 75% of the
nozzle diameter. The middle value of 0.28 mm was chosen to be able to observe inter-layer
overlap and part density variation when the levels did not have a multiple character.
In terms of printing speed, high random speeds in the range 150–300 mm/s were
chosen. These values were chosen because this range is less studied and the printer used,
Polymers 2023, 15, x FOR PEER REVIEW 6 of 21
Polymers 2023, 15, 2305 6 of 21

being core XY, allows printing at high speeds obtaining high qualities, comparable to 3D
being core
printing at XY,
lowallows
speeds.printing at high speeds obtaining high qualities, comparable to 3D
printing at low speeds.
The choice of level values was made in such a way that the midpoint was not close to
Thevalues,
the end choice thus
of level values the
avoiding waspossibility
made in such a way that the
of intercalation midpoint
of mean was not close to
effects.
the end values, thus avoiding the possibility of intercalation of mean effects.
2.1. Materials
2.1. Materials
Biowood is a raw polymer consisting of only renewable resources. The test samples
Biowood is a raw polymer consisting of only renewable resources. The test samples
used in
used in the
the experiments
experiments were were produced
produced by by Rosa3D
Rosa3D Filaments
Filaments (Poland).
(Poland). The
The main
main compo-
compo-
nents of this wooden thermoplastic polymer filament are the following:
nents of this wooden thermoplastic polymer filament are the following: polycaprolactone polycaprolactone
(PCL), polyester,
(PCL), polyester, starch,
starch,lignin,
lignin,natural
naturalresins, waxes
resins, waxes and oils,
and natural
oils, fatty
natural acids,
fatty cellulose,
acids, cellu-
and natural fibres [33]. The wood fibre content is considered to facilitate mechanical
lose, and natural fibres [33]. The wood fibre content is considered to facilitate mechanical pro-
cessing. In Table 2, the main physical properties of biowood polymer
processing. In Table 2, the main physical properties of biowood polymer are presented. are presented. Ac-
cording to to
According thethe
filament
filament producer,
producer,biowood
biowoodfilaments
filamentsrequire
requirelowlowextrusion
extrusiontemperatures,
temperatures,
between 170 and 210 ◦°C. Moreover, printing speeds in the range
between 170 and 210 C. Moreover, printing speeds in the range 60–80 mm/s and 60–80 mm/s and build
build
platform temperatures of 30–50 °C
◦ are recommended
platform temperatures of 30–50 C are recommended [33]. [33].

Table 2.
Table 2. Physical
Physical properties
properties of
of Biowood
Biowood [34].
[34].

Softening point (°C) 50

Softening point (◦ C) 50
Density
Density (kg/m
(kg/m3))
3
1260 1260
Elastic
Elasticmodulus (MPa)
modulus (MPa) 3200 3200
Tensile strength
Tensile strength (MPa)
(MPa) 36 36

2.2. Sample Preparation and Equipment

Experimental tests were conducted
conducted considering standardised tensile test specimens
specimens
ISO 527 Type
Type 1B.
1B. The
The probes
probes had
had the
the geometry
geometry and
and dimensions
dimensions presented
presented in
in Figure
Figure 2.
2. For
these studies, 100%
100% infill
infill specimens
specimens were
were considered.
considered.

Figure 2.
Figure 2. Tensile
Tensile testing
testing specimen
specimen ISO
ISO 527
527 Type
Type 1B.
1B.

Specimens were manufactured

Specimens manufactured on on an FDM Desktop enclosed printer type X1-Carbon
Combo produced
produced by by Bambu
BambuLab Lab(Austin,
(Austin,TX, TX,USA)
USA) (Figure
(Figure3). 3).
TheThe printer has has
printer a lidar res-
a lidar
olution of 7µm,
resolution 20 m/s²
of 7 µm, 20 m/s 2 acceleration,
acceleration, and and
a maximum
a maximum speed of 500
speed of m/s, and itand
500 m/s, works with
it works
with a Prusa-type
a Prusa-type slicer.
slicer. A hardened
A hardened steel
steel nozzle
nozzle of of
5050
HRCHRCwithwitha adiameter
diameterof of0.5
0.5 mm was
used. The weight of the specimens was determined using an analytical balance produced
by Kern (Balingen, Germany) type ADB 200-4 with a resolution resolution of of 0.0001
0.0001 g.
g. A 100% infill
for all
all the
thetested
testedsamples
sampleswas wasconsidered.
considered.The Thebuild platform
build platform temperature
temperature waswas set set
to 35to◦35
C.
°C. The theoretical part weight was determined by calculating the theoretical volume
basedTheon theoretical
the nominalpartdimensions
weight was of the ISO 527-2by
determined 1Bcalculating
specimen and the after multiplying
theoretical volume it
with the density provided by the producers of Rosa Biowood filaments
based on the nominal dimensions of the ISO 527-2 1B specimen and after multiplying it in the technical
data
with sheet. The estimated
the density provided theoretical weight was
by the producers of used
Rosa to determine
Biowood the weight
filaments error
in the for the
technical
3D-printed
data sheet. parts. The weight
The estimated error wasweight
theoretical calculated
was as the to
used difference
determine between the theoretical
the weight error for
and the measured
the 3D-printed weight
parts. The and divided
weight error bywasthe theoretical
calculated asweight as follows
the difference between the theo-
retical and the measured weight and divided by the theoretical weight as follows
( wt − w )
εw = · 100 [%]; (1)
wt
Polymers
Polymers2023,
2023,15,
15,x xFOR
FORPEER
PEERREVIEW
REVIEW 7 7ofof2121

Polymers 2023, 15, 2305 (( ))

7 of 21
𝜀𝜀 == ∙ ∙100
100[%];
[%]; (1)
(1)

Figure
Figure3. The
TheBambu
BambuLab
Lab3D
3DFDM
FDMprinter
printerused
usedin the
theexperiments.
Figure 3.3.The Bambu Lab 3D FDM printer used ininthe experiments.
experiments.

The
Thetensile
The tensilestrength
tensile strengthof
strength ofofthe specimens
thespecimens
the specimenswaswas
wasmeasured using
measuredusing
measured experimental
experimentalequipment
usingexperimental equipment
equipment
(Figure
(Figure 4)4) previously
previously designed
designed and
and executed
executed within
within the
the Faculty
Faculty ofofMechanical
Mechanical
(Figure 4) previously designed and executed within the Faculty of Mechanical Engineering, Engineer-
Engineer-
ing, Automotive,
ing, Automotive,
Automotive, and Robotics
and Robotics
and Robotics at the “Stefan
at theat“Stefan
the “Stefan cel Mare”
cel Mare”
cel Mare” University
University
University of Suceava,
of Suceava,
of Suceava, Romania.
Romania.
Romania. The
The
Thetensile
tensiletensile
strengthstrength
strength measuring
devicedevice
measuring
measuring device comprises
comprises
comprises specimenspecimen
specimen grips
gripsmounted
grips mounted mounted ononthe
thecross-
on the crossheads cross-
of
heads
heads
the ofofthe
tensile the tensile
tensile
testing testing
testing
device device
device
body. body.
The body. The
driveThedrive
drivesystem
system systemcontrols
controls the up the
controls the
or upuporormotion
down down
downmotion
motion
of the
ofofthe
themoving
moving moving crosshead.
crosshead.crosshead. Sensors
Sensors Sensors
measuremeasure
measure the
thespecific
specific
the specific elongation
and and
elongation
elongation andtraction
traction
traction force.
force.force.After
AfterAfter
the
the amplifier amplifies the signal, the measuring results are introduced
amplifier amplifies the signal, the measuring results are introduced to a computer viavia
the amplifier amplifies the signal, the measuring results are introduced to
toaacomputer
computer via
a
adata
adata
data acquisition
acquisition
acquisition device
device
device and
andand processed
processed
processed byby
byspecialised
specialised
specialised software.
software.
software.

Figure 4. The ultimate tensile strength measuring device.

Polymers 2023, 15, x FOR PEER REVIEW 8 of 21

Polymers 2023, 15, 2305 8 of 21

Figure 4. The ultimate tensile strength measuring device.

temperaturescan
Fracture temperatures canbebeused
used to to analyse
analyse the the energy
energy levels
levels absorbed
absorbed by thebyspec-
the
specimen
imen material
material andand
the the strain
strain developed
developed in in
thethe materialbefore
material beforethe
therupture.
rupture. The
The fracture
fracture
temperature was measured using a high-speed thermal camera produced by Flir type
X6540sc,
X6540sc, produced
producedby byTeledyne
TeledyneFLIRFLIR(Wilsonville,
(Wilsonville,OR, OR,USA)
USA)(Figure
(Figure5),5),
with anan
with accuracy of
accuracy
± 1 ◦ C/1%. The data provided by the camera were analysed and processed using Research
of ±1 °C/1%. The data provided by the camera were analysed and processed using Re-
IR specialized
search software.
IR specialized The maximum
software. temperature
The maximum before the
temperature rapture
before of the samples
the rapture was
of the sam-
retained
ples was and analysed
retained in this study.
and analysed in this study.

(a) (b)
Figure 5. Fracture temperature measurement: (a) Flir X6540sc thermal camera; (b) fracture temper-
Figure 5. Fracture temperature measurement: (a) Flir X6540sc thermal camera; (b) fracture
ature analysis.
temperature analysis.

Surface
Surface quality
quality was
was investigated
investigated by by the
the surface
surface area
area roughness
roughness parameter
parameter Sa Sa (arith-
(arith-
metical mean height). According to ISO 25178, this parameter expresses
metical mean height). According to ISO 25178, this parameter expresses the arithmetic the arithmetic
mean
mean ofof the
theheight’s
height’sabsolute
absolutevalue
valuefrom
fromthe the surface’s
surface’s mean
mean plane
plane [35].
[35]. It isItknown
is knownthatthat
the
the most frequently used parameter for characterising the surface texture
most frequently used parameter for characterising the surface texture in a section through in a section
through the machined
the machined surface ofsurface
a partofisa the
partaverage
is the average
arithmeticarithmetic deviation
deviation Ra of Ra theofevaluated
the eval-
uated profile.
profile. In many In situations,
many situations, only for
only values values for the roughness
the roughness parameter parameter Ra are pre-
Ra are prescribed in
scribed in part technical drawings. It is appreciated that, in relation to
part technical drawings. It is appreciated that, in relation to other roughness parameters, other roughness
parameters, the Raprovides
the Ra parameter parameterthe provides the most regarding
most information information theregarding the future
future operating operat-
behaviour
ing behaviour of the surface it characterises. When the question arises
of the surface it characterises. When the question arises of evaluating the roughness of of evaluating thea
roughness of a specific
specific surface, surface,
the roughness the roughness
parameter Sa has parameter Sa has aand
a similar meaning similar meaning
importance and
to that
importance to thatparameter
of the roughness of the roughness
Ra in the parameter Ra profile
case of the in the case
of a of the profile
surface of a surface
in a certain sectionin
athrough
certain the
section through the workpiece.
workpiece.
Because of the specific way the FDM printing processes are carried out, the printed
parts’ top surface and lateral surfaces will expose different different surface textures. These textures
are a result of how how the
the melted
melted material
material layers
layers are
are deposited.
deposited. That is why both surfaces
were considered. The measurements were carried out on three different different surface areas, and
the average value was determined and used in the study. study.
Sa surface roughness values values were
were obtained
obtained using
using the
the Mahr
Mahr CWM
CWM 100 100 confocal
confocal mi-mi-
croscope and white light interferometer, produced by Mahr GmbH, Gottingen, Germany
(Figure 6a), and surface topography (Figure 6b) was analysed using the related Mahrsurf
MfM software Version 7.4.8676.
In Figure 7, the end milling setup for the cutting machinability testing is presented.
The machining tests were carried out on a Diy CNC router. The cutting forces’ magnitude
was measured using a Kistler dynamometer (produced by Kistler Group, Austria) type
9257B. The cutting parameters used for the machining tests were the following: cutting
 speed—150 m/min, cutting feed—800 mm/min, and depth of cut—ap = 1.5 mm. The cut-
ting tool used was a two-flute end mill with a diameter of 3.17 mm made of ultrafine car-
Polymers 2023, 15, 2305
bide Co10%, produced by Jiangsu Weixiang Tools Manufacturing Co.,Ltd , Jiangsu,9 of 21
China
(Figure 7b). The obtained graphs for the cutting forces were processed and analysed in the
related specialised software Dynoware version 3.3.1.0.

Polymers 2023, 15, x FOR PEER REVIEW 9 of 21

speed—150 m/min, cutting feed—800 mm/min, and depth of cut—ap = 1.5 mm. The cut-
ting tool used was a two-flute end mill with a diameter of 3.17 mm made of ultrafine car-
bide Co10%, produced by Jiangsu Weixiang Tools Manufacturing Co.,Ltd , Jiangsu, China
(Figure 7b). The obtained graphs for the cutting forces were processed and analysed in the
related specialised software Dynoware version 3.3.1.0.

(a) (b)
Figure 6. Surface
Figure 6. Surfaceroughness
roughnessmeasuring
measuring procedure:
procedure: (a) Mahr
(a) Mahr CWM CWM 100 interferometer;
100 interferometer; (b) top(b)
andtop and
lateral surface analysis.
lateral surface analysis.

In Figure 7, the end milling setup for the cutting machinability testing is presented.
The machining tests were carried out on a Diy CNC router. The cutting forces’ magnitude
was measured using a Kistler dynamometer (produced by Kistler Group, Wien, Austria)
type 9257B. The cutting parameters used for the machining tests were the following: cutting
speed—150 m/min, cutting feed—800 mm/min, and depth of cut—ap = 1.5 mm. The
cutting tool used was a two-flute end mill with a diameter of 3.17 mm made of ultrafine
(a)
carbide Co10%, produced by Jiangsu Weixiang (b) Tools Manufacturing Co., Ltd., Zhenjiang,
China (Figure 7b). The obtained graphs for the cutting
Figure 6. Surface roughness measuring procedure: (a) Mahr forces
CWMwere processed and(b)
100 interferometer; analysed
top and
in the related specialised
lateral surface analysis. software Dynoware version 3.3.1.0.

(a) (b)
Figure 7. Slot milling tests setup: (a) cutting force measurement; (b) the end-milling tool.

The experimental data obtained were analysed using a trial version of the DOE sta-
tistical software Minitab.

3. Results
The experimental results of the main output parameters investigated in this study
are presented in Table 3. (a) (b)
Figure7.7.Slot
Figure Slotmilling
millingtests
testssetup:
setup:(a)
(a)cutting
cuttingforce
forcemeasurement;
measurement;(b)
(b)the
theend-milling
end-millingtool.
tool.
Table 3. Testing conditions and experimental results.
The experimental
The experimental data
data obtained
obtained were
wereanalysed
analysedusing
usinga trial version
a trial of the
version DOE
of the sta-
DOE
Top Surface Lateral Surface Ultimate Tensile
tistical
Printing Temperature Layer Height software
Printing
statistical SpeedMinitab.
softwareWeight Error
Minitab. Fracture Temperature
Roughness, Sa Roughness Sal Strength, UTM
Tp (°C) hl (mm) sp (mm/s) εw (%) T (°C)
(µm) (µm) (MPa)
3.3.Results
Results
1 150 7.100% 14.995 38.161 7.5000 28.1
175 0.2 The
2 Theexperimental
experimental
200 results
resultsofof
6.971% the main
the output
main
14.549 parameters
output investigated
parameters
35.6655 13.1250 in this
investigated study
in this are
study
26.7
presented in Table
are presented 3. 3.
in Table

Table 3. Testing conditions and experimental results.

Top Surface Lateral Surface Ultimate Tensile
Printing Temperature Layer Height Printing Speed Weight Error Fracture Temperature
Roughness, Sa Roughness Sal Strength, UTM
Tp (°C) hl (mm) sp (mm/s) εw (%) T (°C)
(µm) (µm) (MPa)
1 150 7.100% 14.995 38.161 7.5000 28.1
Polymers 2023, 15, 2305 10 of 21

Table 3. Testing conditions and experimental results.

Printing Lateral Ultimate Fracture

Layer Printing Weight Top Surface
Tempera- Surface Tensile Tempera-
15, x FOR PEERHeight
Polymers 2023, ture REVIEW Speed Error Roughness,
Roughness Strength, ture10 of 21
hl (mm) sp (mm/s) εw (%) Sa (µm)
Tp (◦ C) Sal (µm) UTM (MPa) T (◦ C)
1 150 7.100% 14.995 38.161 7.5000 28.1
32 0.2 200
300 6.971%
6.948% 14.549
14.441 35.6655
35.343 13.1250
13.2787 26.7
29.6
43 300
150 6.948%
6.071% 14.441
13.845 35.343
40.418 13.2787
10.0000 29.6
27.3
54 0.28 150
200 6.071%
6.108% 13.845
16.238 40.418
33.848 10.0000
11.4062 27.3
27.5
65 175 0.28 200
300 6.108%
6.056% 16.238
14.034 33.848
37.807 11.4062
12.4992 27.5
28.1
76 300
150 6.056%
7.328% 14.034
55.260 37.807
46.174 12.4992
12.5000 28.1
27.2
87 0.4 200
150 7.403%
7.328% 59.768
55.260 48.912
46.174 12.7840
12.5000 28.7
27.2
98 0.4 300
200 7.509%
7.403% 58.225
59.768 37.840
48.912 11.7187
12.7840 26.9
28.7
109 150
300 7.262%
7.509% 14.9585
58.225 45.719
37.840 9.2160
11.7187 26.7
26.9
11 0.2 200 7.286% 16.599 36.305 12.3437 29.2
10 150 7.262% 14.9585 45.719 9.2160 26.7
12 300 7.130% 15.560 36.400 15.3125 27.1
11 0.2 200 7.286% 16.599 36.305 12.3437 29.2
13 150 6.379% 62.972 44.391 13.1250 28.2
12 300 7.130% 15.560 36.400 15.3125 27.1
14 190 0.28 200 6.413% 67.723 35.031 15.7824 27.9
13
15 150
300 6.379%
6.388% 62.972
67.476 44.391
31.971 13.1250
15.4688 28.2
28.9
14
16 190 0.28 200
150 6.413%
7.619% 67.723
113.845 35.031
36.211 15.7824
9.0624 27.9
27.3
15
17 0.4 300
200 6.388%
7.608% 67.476
118.236 31.971
43.638 15.4688
11.5625 28.9
27.6
18
16 300
150 7.605%
7.619% 109.852
113.845 52.905
36.211 11.8750
9.0624 29.3
27.3
19
17 0.4 150
200 7.260%
7.608% 64.635
118.236 38.328
43.638 12.0313
11.5625 28
27.6
20
18 0.2 200
300 7.117%
7.605% 64.556
109.852 42.606
52.905 11.4062
11.8750 28.4
29.3
21 300 7.119% 82.446 43.400 10.7812 29.4
19 150 7.260% 64.635 38.328 12.0313 28
22
20 150
200 5.906%
7.117% 106.59
64.556 36.131
42.606 12.0313
11.4062 27.7
28.4
0.2
23
21 220 0.28 200
300 6.004%
7.119% 112.97
82.446 54.213
43.400 13.2800
10.7812 28.5
29.4
24 300 6.049% 72.425 36.364 13.4375 29
22 150 5.906% 106.59 36.131 12.0313 27.7
25 300 7.098% 131.640 44.051 14.2188 27.8
23 220 0.28 200 6.004% 112.97 54.213 13.2800 28.5
26 0.4 150 7.045% 122.390 57.922 17.1872 28.8
24 300 6.049% 72.425 36.364 13.4375 29
27 200 7.164% 149.720 39.632 19.0624 27.9
25 300 7.098% 131.640 44.051 14.2188 27.8
26 150
0.4 3.1. Part Weight 7.045% 122.390 57.922 17.1872 28.8
and Weight Error
27 200 7.164% 149.720 39.632 19.0624 27.9
Figure 8 presents the main effects and interaction plots obtained for the part weight.
The results show that the specimens printed with layer heights of 0.28 mm have a
3.1. Part Weight and Weight Error
significantly higher weight and a smaller weight error than those with layer heights of 0.2
mmFigure 8 presents
and 0.4 mm. the main effects and interaction plots obtained for the part weight.

(a) (b)
Figure 8. The influence of the selected input parameters on specimen weight: (a) the main effects
Figure 8. The influence of the selected input parameters on specimen weight: (a) the main effects
plots; (b) interaction plots.
plots; (b) interaction plots.

An explanation could be that this is caused by how the Prusa slicer determines the
extrusion width and, more precisely, the overlapping between the extrusion lines when
the height of the part is not an integer multiple of the layer height value. The overlap factor
greatly impacts the FDM parts’ voids’ volume, conducting denser structures and lower
Polymers 2023, 15, 2305 11 of 21

Polymers 2023, 15, x FOR PEER REVIEW The results show that the specimens printed with layer heights of 0.28 mm11have of 21a

significantly higher weight and a smaller weight error than those with layer heights of
0.2 mm and 0.4 mm.
An explanation
hardness, and tensilecould be thatExperimental
properties. this is caused by how
results thea Prusa
show minimumslicerweight
determines the
error for
extrusion
the parts width
printedand, withmore precisely, the
a temperature overlapping
of 220 °C whichbetween extrusion
exceeds the range lines when by
recommended the
height of the part is not an integer multiple of the layer height value.
the Biowood filament producers. At lower printing temperatures, the material does reach The overlap factor
greatly impacts
the proper the and
fluidity FDMcauses
parts’bad
voids’ volume,
adhesion andconducting denser
voids between thestructures
extrusion and
lineslower
and
weight
layers. error for the FDM-printed parts. Besides the layer height, the printing temperature
is another
Tableimportant
4 presentsfactor strongly
the analysis of influencing the partcarried
variance (ANOVA) weightoutandtoweight
analyseerror.
how This
the
parameter influences
selected input the printed
factors affect material’s values
the experimental thermal expansion,
obtained fluidity,
for the layer adhesion,
part weights. The test
hardness,
shows that and tensile
with a 95% properties.
confidenceExperimental
interval, noneresults
of the show
inputsaare
minimum weight
statistically error for
significant.
the parts printed with a temperature of 220 ◦ C which exceeds the range recommended
Table
by the4.Biowood
Analysis of Varianceproducers.
filament for weight best
At fit regression.
lower printing temperatures, the material does
reach the proper fluidity and causes bad adhesion and voids between the extrusion lines
Source DF Adj SS Adj MS F-Value p-Value
and layers.
Regression
Table 4 presents the analysis of 3variance 0.008754
(ANOVA)0.002918
carried out to 0.77
analyse how 0.521
the
printing temp (°C) 1 0.001036 0.001036
selected input factors affect the experimental values obtained for the part weights. The 0.27 0.605
test
layer
shows height
that with(mm)
a 95% confidence interval, 1 0.007717 0.007717
none of the inputs 2.04 significant.
are statistically 0.166
printing speed (m/s) 1 0.000001 0.000001 0.00 0.986
Error4. Analysis of Variance for weight23
Table best fit0.086840
regression. 0.003776
Total
Source DF
26 0.095594
Adj SS Adj MS F-Value p-Value
Regression 3 0.008754 0.002918 0.77 0.521
3.2. Sa Surface Roughness
◦ Parameter
printing temp ( C) 1 0.001036 0.001036 0.27 0.605
3.2.1.layer
Roughness of the Top Surface1of the 0.007717
height (mm) Specimens 0.007717 2.04 0.166
printing
Figure 9speed (m/s)
presents the influence 1exerted0.000001
by the selected0.000001 0.00on Sa surface
input parameters 0.986
Error 23 0.086840 0.003776
roughness of the top surface of the specimens. As it can be observed the printing temper-
Total 26 0.095594
ature and layer height have a strong influence on the Sa surface roughness parameter var-
iations.
3.2. SaFigure
Surface
10Roughness Parameter
presents the isometric images of the surface topography of the top surfaces
3.2.1.
of theRoughness
3D-printedofparts
the Top Surface
obtained of the
using the Specimens
Mahr CWM 100 white light interferometer and
confocal microscope.
Figure 9 presentsItthe
caninfluence
be seen that higherbyprinting
exerted temperatures
the selected result in better
input parameters on Salayer
sur-
adhesion and fewer pores. Additionally, when higher temperatures and higher
face roughness of the top surface of the specimens. As it can be observed the print- layer
heights
ing are used,and
temperature the upper top surfaces
layer height have aofstrong
the specimen expose
influence significantly
on the Sa surfacehigher sur-
roughness
face asperities
parameter that result from over-extrusion and signalise a bad material flow.
variations.

(a) (b)
Figure 9. The influence exerted by the selected input parameters on Sa surface roughness of the top
Figure 9. The influence exerted by the selected input parameters on Sa surface roughness of the top
surface of the specimens: (a) the main effects plots; (b) interaction plots.
surface of the specimens: (a) the main effects plots; (b) interaction plots.
Polymers 2023, 15, 2305 12 of 21

Figure 10 presents the isometric images of the surface topography of the top surfaces
of the 3D-printed parts obtained using the Mahr CWM 100 white light interferometer
and confocal microscope. It can be seen that higher printing temperatures result in better
layer adhesion and fewer pores. Additionally, when higher temperatures and higher
Polymers 2023, 15, x FOR PEER REVIEW 12 layer
of 21
heights are used, the upper top surfaces of the specimen expose significantly higher surface
asperities that result from over-extrusion and signalise a bad material flow.
µm µm µm

250
900

800
200 150
700

600
150
100 500

400
100
300
50
200
50
100

0 0 0

Tp = 175 °C, hl = 0.2 mm, v = 150 mm/s Tp = 190 °C, hl = 0.2 mm, v = 150 mm/s Tp = 200 °C, hl = 0.2 mm, v = 150 mm/s
µm µm µm

250 200
400

350
200
150
300

150 250

100 200
100
150

50 100
50
50

0 0 0

Tp = 175 °C, hl = 0.2 mm, v = 150 mm/s Tp = 175 °C, hl = 0.28 mm, v = 150 mm/s Tp = 175 °C, hl = 0.4 mm, v= 150 mm/s

Figure 10. Isometric images top surface topography of the printed specimens.
Figure 10. Isometric images top surface topography of the printed specimens.

The ANOVA
ANOVA test carried out for the the top
top surface
surface Sa
Sa roughness
roughness parameter is presented
presented
in Table
Table 5.
5. The
Thetest
testresult
resultindicates
indicatesthat
thatallall
thethe input
input parameters
parameters investigated
investigated are are statisti-
statistically
cally significant,
significant, with awith a reliability
reliability coefficient
coefficient of 0.95.of 0.95.

Table 5. Analysis of Variance for Sa top best fit regression.

Source
Source DF
DF Adj
Adj SSSS Adj
AdjMSMS F-Value
F-Value p-Value
p-Value
Regression
Regression 33 43847.9
43,847.9 14616.0
14,616.0 62.55
62.55 0.000
0.000
printing temp ( ◦ C) 1 22,324.0 22,324.0 95.53 0.000
printing temp (°C) 1 22324.0 22324.0 95.53 0.000
layer height (mm) 1 21,523.4 21,523.4 92.11 0.000
layer height (mm) 1 21523.4 21523.4 92.11 0.000
printing speed (m/s) 1 0.5 0.5 0.00 0.964
printing speed (m/s)
Error 231 0.5
5374.7 0.5
233.7 0.00 0.964
Error
Total 23
26 5374.7
49,222.6 233.7
Total 26 49222.6
3.2.2. Roughness of the Lateral Surface of the Specimens
3.2.2.Even
Roughness
if in theofscientific
the Lateral Surface
literature of it
[16] the is Specimens
stipulated that increasing the printing speed
is chosen
Even at the
if in theexpense
scientificof literature
lower surface[16] itquality, in thisthat
is stipulated study, for thethe
increasing PCL wood-based
printing speed
biopolymer investigated, the results show contrary aspects (Figures
is chosen at the expense of lower surface quality, in this study, for the PCL wood-based 9 and 11). The printing
speed exhibits
biopolymer a relatively the
investigated, lowresults
influenceshowover the Sa surface
contrary aspectsroughness
(Figures 9parameter measured
and 11). The print-
for the top surface of the tested samples. Lower surface roughness
ing speed exhibits a relatively low influence over the Sa surface roughness parameter values for the lateral
surfaces offor
measured thethesamples were obtained
top surface for the
of the tested parts printed
samples. Lower with
surfacetheroughness
highest level chosen
values for
for the
the printing
lateral surfacesspeed of sp
the= samples
300 mm/s. were Theobtained
arithmetical mean
for the height
parts roughness
printed parameter
with the highest
increases
level with
chosen forthe
theincrease
printinginspeedprinting
sp = speed
300 mm/s.but tends to decreasemean
The arithmetical after aheight
certain value.
roughness
parameter increases with the increase in printing speed but tends to decrease after a cer-
tain value.
Polymers 2023, 15, x 2023,
Polymers FOR 15,
PEER REVIEW
2305 13 of 13
21of 21
Polymers 2023, 15, x FOR PEER REVIEW 13 of 21

(a) (a) (b) (b)

FigureFigure
11. Main
11. effects plots plots
Main effects for Saforroughness
Sa roughnessparameter measured
parameter on on
measured thethe
lateral surface
lateral of of
surface thethe
Figure 11. Main effects plots for Sa roughness parameter measured on the lateral surface of the
specimens : (a) effects
: (a) main
specimens main effects
plots plots for(b)
for Sa; Sa;Pareto
(b) Pareto chart.
chart.
specimens: (a) main effects plots for Sa; (b) Pareto chart.

FigureFigure
Figure 1212presents
12 presents presentsisometric
isometric images
isometric images ofofthe
of the
images thelateral
lateral surface
surface
lateral texture
texture
surface of of
texture ofthe
the specimens
specimens
the specimens
printed
printedprinted with
with a with a printing
printing temperature
temperature
a printing of
of Tp of
temperature Tp =
= 190 190
Tp =°C 190°C◦ and
andCwith with a layer
a layer
and with height
height
a layer of
of 0.4
height of0.4
0.4mm
mm atatat
mm
different
different differentprinting
printingprinting speeds.
speeds. speeds. The arithmetic
The arithmetic
The arithmetic meansmeans
means indicate
indicate
indicate that
thatthat the
thethe height
height
height of
of of
the the
the asperities
asperities is
asperities
is significantly
significantly lower
lower when
when the
the highest
highest level
level of
of the
the printing
printing speed
speed
is significantly lower when the highest level of the printing speed is adopted. isis adopted.
adopted.

µm µm µm
µm µm µm

450
550
400 550
450 500
400
400
350 500
400 450
350 350 450
400
350 300
300 400
300 350
300 250
250 350 300
250
250 200 300 250
200

200 200 250 200

150 150
200 150
150 100 150
100
150 100
100 50 100
50 100 50
50 0
50 50 0
0
0 0
0
Tp = 190 °C, hl = 0.4 mm, sp = 150 m/s Tp = 190 °C, hl = 0.4 mm, sp = 200 m/s Tp = 190 °C, hl = 0.4 mm, sp = 300 m/s
Tp = 190 °C, hl = 0.4 mm, sp = 150 m/s Tp = 190 °C, hl = 0.4 mm, sp = 200 m/s Tp = 190 °C, hl = 0.4 mm, sp = 300 m/s
Figure 12. Isometric images of lateral surface topography of the printed specimens.
Figure 12. Isometric images of lateral surface topography of the printed specimens.
Figure 12. Isometric images of lateral surface topography of the printed specimens.
These
Thesecould
couldbebea aresult
resultofofthe
therapid
rapidcooling
coolingofofthe themelted
melteddeposit
depositlayers
layersdueduetotothethe
ventilation
These effect
could be
ventilation associated
a result
effect with
of thewith
associated the
rapid high
thecooling velocity of the
of theofmelted
high velocity nozzle.
deposit layers due to the
the nozzle.
ventilationTheTheANOVA
effect test
associated
ANOVA testcarried
with out
the
carried for
high
out forthe
theSaSaroughness
velocity parameter
parametermeasured
of the nozzle.
roughness measuredfor forthe
thelateral
lateral
surfaces
Thesurfaces
ANOVA (Table
test6)carried
(Table of of
6) thethe
3D-printed
for theparts
3D-printed
out indicates
Sa parts that
indicates
roughness the layer
that
parameter height
themeasured
layer is for
heightstatistically
is sig-
thestatistically
lateral
nificant with a reliability coefficient of 0.95 (α = 0.05). This is also sustained
surfaces (Table 6) of the 3D-printed parts indicates that the layer height is statistically sig- the
significant with a reliability coefficient of 0.95 (α = 0.05). This is also by the
sustained Pareto
by
graph
nificant with(Figure
Pareto agraph 11b),
(Figure
reliability which
11b),indicates
coefficientwhich of 0.95that(α the
indicates interest
= that the
0.05). parameter
interest
This Sa variation
parameter
is also sustained Sa by is likely
variation
the at-
is likely
Pareto
tributable
graph (Figure to
attributable the layer
11b),towhich height
the layer parameter
height parameter
indicates variation.
variation.
that the interest parameter Sa variation is likely at-
tributable to the layer height parameter variation.
Table
Table6.6.Analysis
AnalysisofofVariance
Variancefor
forSa.
Sa.
Table 6.Source
Analysis
Source of Variance for Sa. DF
DF Adj SSSS Adj MS
Adj Adj MS F-Value
F-Value p-Value
p-Value
Regression 33 313.20 104.40 2.95 0.054
Source Regression DF Adj SS313.20Adj MS 104.40 F-Value 2.95 p-Value0.054
printing temp
printing (°C)(◦ C)
temp 11 89.57
89.57 89.5789.57 2.53
2.53 0.125
0.125
Regression layer height (mm) 3 313.20192.69 104.40 192.69 2.95 5.44 0.054
layer height (mm) 11 192.69 192.69 5.44 0.029
0.029
printing temp (°C)speed (m/s)
printing 1 1 89.57 30.95 89.57 30.95 2.53 0.87 0.125
0.360
printing
Error speed (m/s) 123 30.95
814.71 30.9535.42 0.87 0.360
layer height (mm) 1 192.69 192.69 5.44 0.029
Error
Total 2326 814.71
1127.91 35.42
printing speed (m/s) 1 30.95 30.95 0.87 0.360
Total 26 1127.91
Error 23 814.71 35.42
Total 26 1127.91
Polymers 2023,
Polymers 2023, 15,
15, 2305
x FOR PEER REVIEW 1414of
of 21
21

3.3. Ultimate Tensile Strength

Figure 13 presents images of the fracture surfaces obtained in the tensile strength
tests. The fracture appearance presents different
different proportions of brittle or ductile failure
modes. It could be observed that the specimens obtained at higher printing temperatures
exposed higher percentages of ductile fracture. This means that by using higher printing
temperatures, the
the parts
parts will
will have
have more
more toughness.
toughness.

Figure 13.
Figure 13. Fracture
Fracture surfaces of the specimens after the tensile strength tests:
tests: (a) specimen printed at
Tp = 175 °C
◦ with hl = 0.4 mm and sp = 200 mm/s; (b) specimen printed
Tp = 175 C with hl = 0.4 mm and sp = 200 mm/s; (b) specimen printed at Tp at=Tp
190= 190 °C with
◦ C with hl =mm
hl = 0.4 0.4
mm and sp = 200 mm/s; (c) specimen printed at Tp =◦ 220 °C with hl = 0.4 mm and sp
and sp = 200 mm/s; (c) specimen printed at Tp = 220 C with hl = 0.4 mm and sp = 200 mm/s. = 200 mm/s.

This was
This was also
also reflected
reflected in
in the
the ultimate
ultimate tensile
tensile strength
strength values
values obtained
obtained in in the
the tensile
tensile
strength tests that were carried out. The printing temperature exposed a
tests that were carried out. The printing temperature exposed a significant significant influ-
in-
fluence on ultimate tensile strength values. In the Pareto chart (Figure 14b), the levelsig-
ence on ultimate tensile strength values. In the Pareto chart (Figure 14b), the level of of
nificance of each
significance input
of each factor
input chosen
factor for this
chosen study
for this can can
study be analysed. The The
be analysed. results showshow
results that
among
that the studied
among factors,
the studied thethe
factors, printing
printingspeed
speedand
andthe
theinteraction
interactionbetween
between the
the printing
temperature andand layer
layer height are statistically
height are statistically significant
significant at
at the
the 0.05
0.05 level.
level.

(a) (b)
Figure 14. The influence of the selected input parameters over the ultimate tensile strength: (a) the
Figure 14. The influence of the selected input parameters over the ultimate tensile strength: (a) the
main effects plots; (b) Pareto chart for the significance of the studied input parameters.
main effects plots; (b) Pareto chart for the significance of the studied input parameters.
This result
This result isisalso
alsosustained
sustainedby bythetheanalysis
analysisofofvariance
variance carried
carried outout (Table
(Table 7).7). Accord-
According
ing to the ANOVA test, the printing speed is statistically significant for
to the ANOVA test, the printing speed is statistically significant for the ultimate tensile the ultimate tensile
strength variation with a reliability coefficient
strength variation with a reliability coefficient of 0.95. of 0.95.
In this
In this study,
study,significantly
significantlyhigherhigherprinting
printingspeeds
speedsthanthan those
those usually
usually reported
reported as as be-
being
ing studied
studied in the
in the scientific
scientific literature
literature (range
(range 15–170
15–170 m/s)[1,3]
m/s) [1,3]were
wereused.
used. Higher
Higher printing
printing
speeds can prevent the alteration of biocomponents of the filaments due
speeds can prevent the alteration of biocomponents of the filaments due to intense exposure to intense expo-
sure to high temperatures. Even if it is a general belief that higher printing
to high temperatures. Even if it is a general belief that higher printing speeds conduct speeds conduct
weaker structures
weaker structures due duetotoinsufficient
insufficientcooling
cooling time
timebetween
between layers andand
layers badbad
layer adhesion,
layer adhe-
the results obtained in this study indicate that a higher printing speed
sion, the results obtained in this study indicate that a higher printing speed significantly significantly in-
creases thethe
increases ultimate
ultimatetensile
tensilestrength
strength andand
the the
fracture temperature
fracture temperature of the
ofprinted partsparts
the printed (Fig-
ures 14 and
(Figures 15). 15).
14 and
Polymers 2023, 15, 2305 15 of 21

Table 7. Analysis of Variance for UTS (MPa).

Source DF Adj SS Adj MS F-Value p-Value

Regression 3 56.29 18.763 4.19 0.017
printing temp (◦ C) 1 18.75 18.748 4.19 0.052
layer height (mm) 1 11.32 11.321 2.53 0.125
printing speed (m/s) 1 26.22 26.220 5.86 0.024
Error
Polymers 2023, 15, x FOR PEER REVIEW 23 102.95 4.476 15 of 21
Total 26 159.24

Figure 15. The main effects plots for the fracture temperature.
Figure 15. The main effects plots for the fracture temperature.

Table
3.4. 7. Analysis
3D-printed of Variance
Parts for UTS (MPa).
Machinability
SourceThe cutting machinability ofDF Biowood
Adj Rosa3D
SS printed
Adj MS parts was also investigated.
F-Value p-Value Slot
milling tests were carried out, and the cutting force values obtained were compared with
Regression 3 56.29 18.763 4.19 0.017
the ones achieved by machining in identical condition pinewood and beech wood samples.
printing temp (°C) 1 18.75 18.748 4.19 0.052
Pine and beech wood were selected as representatives for the soft and hard wood categories.
Alayer height (mm)
measurement 1 components
of the cutting force 11.32 11.321
for slot 2.53
milling operations 0.125samples
of some
printing speed (m/s) 1 26.22 26.220 5.86
from three distinct wooden materials was carried out, one of which was the biowood. The 0.024
Error
tests 23
were carried out on a three-axis 102.95 4.476
DIY milling router-type machine tool, using a two-
flute
Total tungsten carbide end mill type
26 10113117
159.24 produced by Weix tools, China. The geometry
of the active zone of the end mill is typical for wood bits. As for cutting conditions, the
following values
3.4. 3D-printed were
Parts chosen: ap = 1.5 mm for depth of cut, f = 800 mm/min for cutting
Machinability
feed, and vc = 150 m/min for cutting speed.
The cutting machinability of Biowood Rosa3D printed parts was also investigated.
By machining the samples obtained by FDM 3D printing of Biowood Rosa filaments,
Slot milling tests were carried out, and the cutting force values obtained were compared
significantly higher cutting forces were obtained (Figure 16). The average cutting forces
with the ones achieved by machining in identical condition pinewood and beech wood
generated by machining Biowood Rosa samples were up to 10× higher than those obtained
samples. Pine and beech wood were selected as representatives for the soft and hard wood
by end-milling softwood samples and up to 2.5× higher than those obtained for the
categories. A measurement of the cutting force components for slot milling operations of
hardwood samples.
some samples from three distinct wooden materials was carried out, one of which was the
Figure 17 presents the main influence of the 3D printing input parameters analysed in
biowood. The tests were carried out on a three-axis DIY milling router-type machine tool,
the study over the cutting force components. The printing temperature and layer height
using a two-flute tungsten carbide end mill type 10113117 produced by Weix tools, China.
positively affect the cutting force components’ magnitude. Printing speed negatively
The geometry
influences of the active of
the machinability zone of the Rosa
Biowood end mill
partsisaccording
typical fortowood bits. As forcriteria.
the force-cutting cutting
conditions, the following values were chosen: ap= 1.5 mm for depth of cut,
Even if the material becomes more ductile because of the exposure to high temperatures f = 800 mm/min
for cutting
and feed,
therefore and vchigher
requires = 150 efforts
m/min to
forbecutting speed.
machined, at high printing temperatures, over-
By machining the samples obtained by
extrusion phenomena could be observed by analysing FDM 3D printing
the topof Biowood
surface Rosa filaments,
topography of the
significantly higher cutting forces were obtained (Figure 16). The
specimens. This phenomenon can lead to weak structural bonds and is conducive average cutting forces
to lower
generated
values by machining
for the Biowood Rosa samples were up to 10× higher than those obtained
cutting forces.
by end-milling softwood samples and up to 2.5× higher than those obtained for the hard-
wood samples.
 5

Cutting force [N]

4
pinewood
3
Polymers 2023, 15, 2305
Polymers 2023, 15, x FOR PEER REVIEW
beech wood 16
16 of 21
of 21
2
biowood
1

06
Fx [N] Fy [N] Fz [N]
5

Cutting force [N]

Figure 16.
4 Cutting force components comparison between pinewood, beech wood, and Biowood
parts generated during slot milling with cutting speeds of 150 m/min, cutting feeds ofpinewood
800 mm/min,
3 depth of 1.5 mm.
and cutting
beech wood
2
Figure 17 presents the main influence of the 3D printing input parameters biowood
analysed
in the study
1 over the cutting force components. The printing temperature and layer height
positively affect the cutting force components’ magnitude. Printing speed negatively in-
fluences0 the machinability of Biowood Rosa parts according to the force-cutting criteria.
Even if the material Fx becomes
[N] Fy [N]because of the Fz
more ductile [N]
exposure to high temperatures
and therefore requires higher efforts to be machined, at high printing temperatures, over-
Figure16.
extrusion
Figure 16.phenomena
Cuttingforce
Cutting forcecould
components comparison
be observed
components betweenthe
by analysing
comparison between pinewood, beech
top surface
pinewood, beech wood,and
topography
wood, andBiowood
ofBiowood
the
parts generated during slot milling with cutting speeds of 150 m/min, cutting feeds of 800 mm/min,
specimens. Thisduring
parts generated phenomenon canwith
slot milling lead to weak
cutting structural
speeds bonds and
of 150 m/min, is conducive
cutting feeds of 800tomm/min,
lower
and cutting depth of 1.5 mm.
values for the
and cutting cutting
depth of 1.5forces.
mm.

Figure 17 presents the main influence of the 3D printing input parameters analysed
4.4 Fx [N] 5.9
in the study over the cuttingFy [N]components. The 2.4
force Fz [N]and layer height
printing temperature
4.3 5.8
positively affect the cutting force components’ magnitude.
2.35 Printing speed negatively in-
fluences the5.7machinability of Biowood Rosa parts according to the force-cutting criteria.
4.2
Even if the material becomes more ductile because2.3 of the exposure to high temperatures
MEAN

MEAN

5.6
4.1 and therefore requires higher efforts to be machined, MEAN
2.25at high printing temperatures, over-
5.5
extrusion phenomena could be observed by analysing the top surface
printingtopography
temp [°C] of the
4 printing temp [°C] printing temp [°C] 2.2
specimens. 5.4
This phenomenon can lead to weak structural bonds and is conducive to lower
layer height [mm] layer height [mm]
3.9 values for the layer height [mm]
cutting forces.
5.3 2.15
printing speed [mm/s] printing speed [mm/s] printing speed [mm/s]
3.8 5.2 2.12.4
4.4 Fx 2[N] 5.9 Fy Fz2 [N]
1 3 1 2 [N] 3 1 3
4.3 5.8 2.35
(a) (b) (c)
5.7
4.2 Figure 17. Mean effects plots for the cutting forces’ components. 2.3 (a) main effect plot for Fx [N]; (b)
Figure 17. Mean effects plots for the cutting forces’ components. (a) main effect plot for Fx [N];
main effect plot5.6for Fy[N; (c)main effect plot for Fz[N]
MEAN

MEAN

MEAN

4.1 (b) main effect plot for Fy[N]; (c) main effect plot for Fz[N].2.25
5.5
3.5. Nonlinear printing temp [°C]
4 printing temp NonlinearRegression
3.5.[°C] RegressionAnalysis
Analysis
printing temp [°C] 2.2
5.4
Through
Through the
the mathematical processing of the experimental results, itit became
became possible to
height [mm]of the experimental results,layer
mathematical height possible
[mm]
3.9 layer height [mm] layer processing
to determine some
5.3 empirical power, function-type 2.15
mathematical models. With these em-
determine
printing speed [mm/s] some empirical power, function-type mathematical models.printing With these
speed empirical
[mm/s]
pirical mathematical printing
models, speedinformation
additional [mm/s] was obtained regarding the order of
3.8 mathematical5.2 models, additional information was obtained 2.1 regarding the order of influence
1 2 influence
and and the intensity
3 the intensity of the 2influence
of the1 influence exerted byexerted
3 some by someon
factors factors on theparameters
the1 output output
2
param-
of
3 the
eters of the investigated process.
investigated process. Microsoft Microsoft
Excel Excel
software software
was used was
for used
the for the mathematical
mathematical processing
(a) (b) (c)
processing of the experimental
of the experimental results. Inresults. In this
this way, theway, the following
following empiricalempirical mathematical
mathematical models
Figure
models 17. Mean effects
were obtained: plots for the cutting forces’ components. (a) main effect plot for Fx [N]; (b)
were obtained:
main effect plot for Fy[N; (c)main effect plot for Fz[N]
-- For
Forthe
thelateral
lateralsurface
surfaceroughness
roughness(standard
(standarderror
errorofofthe
theregression S =S 6.0487,
regression correla-
= 6.0487, correla-
tion coefficient
tion coefficientR = 0.5039):
R = 0.5039):
3.5. Nonlinear Regression Analysis
Through the mathematical processing of the experimental results, it became possible
0.4558 0.2210 −0.0747
to determine some empiricalSa = 7.3154 · Tp
power, hl
function-type sp [µm]; models. With these em-
mathematical (2)
-pirical
Formathematical models,
the ultimate tensile additional
strength information
(standard error ofwas obtained regarding
the regression S = 2.076, the order of
correlation
influence and the
coefficient R =intensity
0.6140): of the influence exerted by some factors on the output param-
eters of the investigated process. Microsoft Excel software was used for the mathematical
processing of the experimental results. 0.7137In this0.1974
way, the following empirical mathematical
UTS = 0.08885 T hl sp0.2708 [MPa]; (3)
models were obtained:
-- For
Forthe
thepart weight
lateral (standard
surface error(standard
roughness of the regression
error of Sthe= 0.0629, correlation
regression coefficient
S = 6.0487, correla-
Rtion
= 0.2167):
coefficient R = 0.5039):
Polymers 2023, 15, 2305 17 of 21

W = 9.5844 · T0.06157 hl−0.004079 sp0.000083 [g]; (4)

Figure 18 shows normally distributed data for the regression equations determined
for the lateral surface roughness of the printed parts and the ultimate tensile strength
interest parameters. Additionally, the distances between the residuals versus their expected
values for the regressions are relatively small. The parameter estimation errors are pre-
Polymers 2023, 15, x FOR PEER REVIEW 18 of 21
sented in Tables 8–10. The small values of the coefficient standard error (SE) indicate a
precise estimation.

(a) (b)
Figure 18. Normal probability plots for the nonlinear regressions (a) for the Sa roughness parameter
Figure 18. Normal probability plots for the nonlinear regressions (a) for the Sa roughness parameter
measured on the lateral surfaces of the printed part and (b) for the ultimate tensile strength.
measured on the lateral surfaces of the printed part and (b) for the ultimate tensile strength.

By examining the mathematical model corresponding to the lateral surface, Sa rough-

Table 8. The parameter estimation errors for Equation (2).
ness parameter, it could be seen that these parameters will register an increase when the
printing
Parametertemperature TP and layer height hl increase and decrease with the increase
Estimate in the
SE Estimate
printing speed sp. The printing temperature Tp exerts the most substantial influence on
×1 7.31547 12.0722
the
×2Sa parameter, which, in the empirical mathematical model, corresponds to the highest
0.45580 0.2951
value
×3 of the corresponding exponent compared to the values of the exponents attached
0.22107 0.1002to
the
×4rest of the analysed process input factors. −0.07472 0.0998
It should be noted that increasing the value of any of the three factors considered will
increase the ultimate tensile strength UTS because the values of all exponents are positive.
Table 9. The parameter estimation errors for Equation (3).
The printing temperature Tp is also the input factor with the strongest influence in the
ultimate
Parameter tensile strength UTS because, in this case,Estimate
the value of the exponentSE attached
Estimateto
this
×1 factor also has the maximum value of the values of
0.088580the exponents of the other input
0.161801
factors
×2 studied. An explanation of the increase in the value
0.713767 of the UTS parameter when
0.326272
increasing
×3 the printing temperature Tp could result0.197467
from better adhesion of the deposited
0.111027
×4 due to the higher values of the printing temperature.
layers 0.270825 0.109504
The three input factors have a relatively small influence on the weight output param-
TableThis
eter. finding
10. The is based
parameter on theerrors
estimation very for
lowEquation
values of
(4).the exponents obtained for the input
factors in the empirical mathematical model corresponding to the parameter W. However,
itParameter Estimate also seems to be exerted
can be observed that in this case, the strongest influence SE Estimate
by the
printing
×1 temperature Tp, whose exponent has the maximum 9.58440 value. 0.686965
×2 0.00615 0.012852
4.×Discussion
3 −0.00408 0.004299
×4 0.00008 0.004279
Even when 100% infill was set as the printing condition for the specimen manufac-
turing process, the resulting parts’ weight was smaller than the theoretical weight (deter-
minedByby
examining the mathematical
the theoretical volume andmodel corresponding
the material to theprovided
density value lateral surface,
by theSa rough-
filament
ness
producers). The weight error calculated for the specimens ranged between 5.9–7.6%. the
parameter, it could be seen that these parameters will register an increase when
printing
Thetemperature TP andparameter
surface roughness layer height
Sa hl increase on
measured andthe
decrease with the
top surfaces increase
of the in the
3D-printed
samples ranged between 13.8 and 149.7 (µm). For this output parameter, all of the consid-
ered input factors were reported as statistically significant according to the ANOVA test
carried out. Even if the printing temperature levels tested in this study did not exceed the
temperature range recommended by the filament producer, the area surface roughness
parameter Sa of the top surfaces of the samples printed at 190 °C recorded an average
Polymers 2023, 15, 2305 18 of 21

printing speed sp. The printing temperature Tp exerts the most substantial influence on
the Sa parameter, which, in the empirical mathematical model, corresponds to the highest
value of the corresponding exponent compared to the values of the exponents attached to
the rest of the analysed process input factors.
It should be noted that increasing the value of any of the three factors considered will
increase the ultimate tensile strength UTS because the values of all exponents are positive.
The printing temperature Tp is also the input factor with the strongest influence in the
ultimate tensile strength UTS because, in this case, the value of the exponent attached to
this factor also has the maximum value of the values of the exponents of the other input
factors studied. An explanation of the increase in the value of the UTS parameter when
increasing the printing temperature Tp could result from better adhesion of the deposited
layers due to the higher values of the printing temperature.
The three input factors have a relatively small influence on the weight output parame-
ter. This finding is based on the very low values of the exponents obtained for the input
factors in the empirical mathematical model corresponding to the parameter W. However,
it can be observed that in this case, the strongest influence also seems to be exerted by the
printing temperature Tp, whose exponent has the maximum value.

4. Discussion
Even when 100% infill was set as the printing condition for the specimen manufactur-
ing process, the resulting parts’ weight was smaller than the theoretical weight (determined
by the theoretical volume and the material density value provided by the filament produc-
ers). The weight error calculated for the specimens ranged between 5.9–7.6%.
The surface roughness parameter Sa measured on the top surfaces of the 3D-printed
samples ranged between 13.8 and 149.7 (µm). For this output parameter, all of the consid-
ered input factors were reported as statistically significant according to the ANOVA test
carried out. Even if the printing temperature levels tested in this study did not exceed the
temperature range recommended by the filament producer, the area surface roughness
parameter Sa of the top surfaces of the samples printed at 190 ◦ C recorded an average
increase of 152%, and those printed at 220 ◦ C showed an average increase of 347% com-
pared with those printed with a temperature of 175 ◦ C. The layer height parameter also
exposed a similar influence on the Sa roughness of the top surfaces of the printed parts.
The roughness parameter had an average increase of 176% when the layer height was set
at 0.28 mm and an average increase of 303% when a layer height of 0.4 mm was adopted
compared with that resulting from parts printed with a layer height of 0.2 mm. These
variations result due to over-extrusion caused by inefficient flow rates.
The surface roughness parameter Sa values measured on the lateral surfaces of the
printed specimens ranged between 35.34 and 57.92 (µm). According to the main effect plots
(Figure 11a), the printing conditions that assured a better surface roughness were the lowest
◦
value of the printing temperature (175 ), the layer height of 0.28 mm, and the maximum
value of the printing speed (300 m/s). Among the input factors investigated, only the layer
height tested as statistically significant according to the ANOVA test (Table 6).
The ultimate tensile strength values obtained were in the range of 7.5–19.06 MPa.
Significant correlations were found between printing speed, mechanical strength (ultimate
tensile strength), printing temperature–layer height interaction, and mechanical strength.
The machinability was investigated using cutting forces criteria. Machinability is
rated relative to the results achieved for a representative/reference material. To evaluate
the machinability of Biowood printed parts, machining tests were carried out in similar
conditions for pinewood and beech wood as representatives of softwood and hardwood
materials. The average cutting forces generated by machining Biowood Rosa samples were
up to 10× higher than those obtained by end-milling softwood samples and up to 2.5×
higher than those obtained for the hardwood samples. The printing temperature and layer
height tend to positively affect the cutting force components’ magnitude, while printing
speed negatively influences the machinability of Biowood Rosa printed parts.
Polymers 2023, 15, 2305 19 of 21

5. Conclusions
Biopolymers are a natural alternative to synthetic polymers that exhibit reduced carbon
dioxide emissions in their synthesis. In recent decades, more and more emphasis has been
placed on using biopolymers for various medical, food, and industrial applications.
Few studies have been carried out on testing the capabilities of wood biopolymer
composites. Most of these studies usually address only the mechanical properties of WPC.
The present research explores the effect of printing temperature, layer height, and printing
speed on surface quality, tensile performance, and cutting machinability of parts obtained
by FDM printing of Rosa3D Biowood filament. Biowood produced by Rosa3D is a wood-
based composite biopolymer obtained by amalgamating wood fibres in a polycaprolactone
PCL and polyester polymeric matrix and adding fillers (starch, lignin) and additives
(natural resins, waxes, and oils, natural fatty acids) to the mix.
The novelty of this study consists in exploring some of the qualitative aspects and
mechanical proprieties of the PCL wood-based biopolymer parts generated by FDM with
different printing conditions. The printing parameters varied in the experimental study
were the printing temperature, the layer height, and the printing speed. The printing speed
levels selected for the experiment were significantly superior to those usually tested in
previous research in this field or those recommended by the filament producer.
The surface roughness of the parts was investigated. Higher Sa (arithmetical mean
height) values were obtained when high printing temperatures and layer height were used.
The surface texture obtained for these specific printing conditions exhibits signs of over-
extrusion. Overall, the highest level chosen for the printing speed positively influenced the
surface roughness.
Another novelty aspect of this study is the cutting machinability as a secondary
machining operation of the FDM-printed wood-based composite biopolymer. Machinability
is the property that characterizes the ease with which a material can be machined with
a cutting tool. The machinability testing criteria used in this study was the cutting force
components’ magnitude. The Biowood Rosa3D printed parts exhibit poor machinability
in reference to natural wood parts (pinewood and beech wood). Therefore, lower cutting
forces and better cutting machinability were obtained for the parts printed at higher printing
temperatures and layer heights and with lower printing speeds.
Testing the capabilities of newly developed polymer composites, especially biopolymer
composites, should be a constant concern for researchers to achieve competitive products
for the industry. Many drawbacks of FDM 3D printing of wood-based biopolymers could
be overcome by carefully choosing the processing parameters.

Author Contributions: Conceptualization I.B.-B.; methodology, I.B.-B. and I.T.; software I.B.-B.;
formal analysis, I.B.-B., I.T. and L.S.; investigation, I.B.-B. and I.T.; writing—original draft preparation,
I.B.-B., I.T. and L.S.; writing—review and editing, I.B.-B. and L.S.; supervision, L.S. All authors have
read and agreed to the published version of the manuscript.
Funding: This research received no external funding.
Institutional Review Board Statement: Not applicable.
Data Availability Statement: Some or all data, models, or code generated or used during the study
are available from the corresponding author by request.
Acknowledgments: The work of the author Ioan Tamas, ag was supported by the project “PROIN-
VENT”, Contract no. 62487/03.06.2022-POCU/993/6/13-Code 153299, financed by The Human
Capital Operational Programme 2014–2020 (POCU), Romania.
Conflicts of Interest: The authors declare no conflict of interest.
Polymers 2023, 15, 2305 20 of 21

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