biomedicines

Article
Statistical Comparison of the Mechanical Properties of
3D-Printed Resin through Triple-Jetting Technology
and Conventional PMMA in Orthodontic Occlusal
Splint Manufacturing
Ioan Barbur 1,† , Horia Opris 1, *,† , Bogdan Crisan 1 , Stanca Cuc 2 , Horatiu Alexandru Colosi 3, * ,
Mihaela Baciut 1 , Daiana Opris 1 , Doina Prodan 2 , Marioara Moldovan 2 , Liana Crisan 1 , Cristian Dinu 1
and Grigore Baciut 1

Citation: Barbur, I.; Opris, H.; Crisan,
B.; Cuc, S.; Colosi, H.A.; Baciut, M.;
Opris, D.; Prodan, D.; Moldovan, M.;
Crisan, L.; et al. Statistical
Comparison of the Mechanical
Properties of 3D-Printed Resin
through Triple-Jetting Technology
and Conventional PMMA in
Orthodontic Occlusal Splint
Manufacturing. Biomedicines 2023, 11,
2155. https://doi.org/10.3390/
biomedicines11082155
Academic Editors: Angelo Michele
Inchingolo, Gianna Dipalma,
Assunta Patano, Alessio Danilo
Inchingolo, Giuseppina Malcangi
and Francesco Inchingolo
Received: 28 June 2023
Revised: 25 July 2023
Accepted: 28 July 2023
Published: 31 July 2023
1 Department of Maxillofacial Surgery and Implantology, Iuliu Hatieganu University of Medicine and
Pharmacy, 400012 Cluj-Napoca, Romania; drbarur@gmail.com (I.B.); crisan.bogdan@umfcluj.ro (B.C.);
mbaciut@umfcluj.ro (M.B.); daiana.opris@umfcluj.ro (D.O.); lcrisan@umfcluj.ro (L.C.);
cristian.dinu@umfcluj.ro (C.D.); gbaciut@umfcluj.ro (G.B.)
2 Department of Polymer Composites, Institute of Chemistry Raluca Ripan, Babes-Bolyai University,
400294 Cluj-Napoca, Romania; stanca.boboia@ubbcluj.ro (S.C.); doina.prodan@ubbcluj.ro (D.P.);
marioara.moldovan@ubbcluj.ro (M.M.)
3 Department of Medical Education, Division of Medical Informatics and Biostatistics,
Iuliu Hatieganu University of Medicine and Pharmacy, 400012 Cluj-Napoca, Romania
* Correspondence: horia.opris@umfcluj.ro (H.O.); hcolosi@umfcluj.ro (H.A.C.)
† These authors contributed equally to this work.
Abstract: Dental 3D-printing technologies, including stereolithography (SLA), polyjet (triple-jetting
technology), and fusion deposition modeling, have revolutionized the field of orthodontic occlusal
splint manufacturing. Three-dimensional printing is now currently used in many dental fields,
such as restorative dentistry, prosthodontics, implantology, and orthodontics. This study aimed to
assess the mechanical properties of 3D-printed materials and compare them with the conventional
polymethylmethacrylate (PMMA). Compression, flexural, and tensile properties were evaluated
and compared between PMMA samples (n = 20) created using the “salt and pepper” technique and
digitally designed 3D-printed samples (n = 20). The samples were subjected to scanning electron
microscope analysis. Statistical analysis revealed that the control material (PMMA) exhibited a
significantly higher Young’s modulus of compression and tensile strength (p < 0.05). In the flexural
tests, the control samples demonstrated superior load at break results (p < 0.05). However, the
3D-printed samples exhibited significantly higher maximum bending stress at maximum load (MPa)
(p < 0.05). Young’s modulus of tensile testing (MPa) was statistically significant higher for the control
samples, while the 3D-printed samples demonstrated significantly higher values for elongation at
break (p < 0.05). These findings indicate that 3D-printed materials are a promising alternative that
can be effectively utilized in clinical practice, potentially replacing traditional heat-cured resin in
various applications.
Keywords: polymethylmethacrylate (PMMA); 3D printing; polyjet; mechanical properties; occlusal
splint; scanning electron microscopy (SEM)

Copyright: © 2023 by the authors.

Licensee MDPI, Basel, Switzerland. 1. Introduction
This article is an open access article
The use of occlusal devices is regarded as an evidence-based therapeutic option for
distributed under the terms and
the management of temporomandibular disorder symptoms [1]. Bruxism, myalgia of the
conditions of the Creative Commons
temporomandibular muscles, and arthralgia of the temporomandibular joints are among
Attribution (CC BY) license (https://
the indications for using occlusal splints. The materials used to make such devices should
creativecommons.org/licenses/by/
4.0/).
be strong enough to bear significant occlusal forces [2]. Typically, acrylic resin that has

Biomedicines 2023, 11, 2155. https://doi.org/10.3390/biomedicines11082155 https://www.mdpi.com/journal/biomedicines

Biomedicines 2023, 11, 2155 2 of 15

been auto-, heat-, or light-polymerized is used to make conventional occlusal devices [3].
Recently, additive (3D-printing) techniques have been made possible by manufacturing
methods assisted by CAD-CAM technology [4].
Dental 3D printers employ stereolithography (SLA), polyjet (triple-jetting technol-
ogy), fusion deposition modeling printing, digital light processing, and selective laser
sintering [4,5]. SLA printing uses ultraviolet lasers to sculpt resin. In this method, the
printing plate travels down in small increments, and the liquid polymer is subjected to an
ultraviolet laser that cures a cross section layer by layer. This process is repeated until a
dental model is produced [6].
Polyjet 3D printing is comparable to inkjet printing, except that the printer sprays
layers of curable liquid photopolymer onto a construction platform [7]. More material is
placed immediately on the preceding layer when the construction platform goes down one
layer. This is repeated until the form is printed [8]. Triple-jetting technology allows 3D
printing of complex things with different materials. Triple jetting uses three printheads
to extrude various materials simultaneously, unlike single-nozzle 3D printing. This new
method deposits model, support, and contrasting materials precisely and simultaneously.
The printheads layer materials to generate intricate shapes and geometries. This approach
is useful for prototyping, functioning pieces, and designs that require a mix of materials
for mechanical, aesthetic, or functional features. The triple-jetting method allows for more
flexibility and efficiency in 3D printing personalized goods [9].
A powerful laser is used in the additive manufacturing technique known as SLS
(Selective Laser Sintering) to selectively fuse powdered materials, layer by layer, to produce
three-dimensional things out of a variety of materials, including plastics, metals, and
ceramics [5].
Recent mechanical property studies of printable denture-based resins have been
helpful. The PMMA samples had the highest mean surface roughness, Vickers hardness
number, and flexural strength but the lowest contact angle. The samples printed using the
ASIGA resin had the highest average contact angle and smoothest average surface, while
the Dentona 3D printer had the highest mean impact force. NextDent materials had the
highest mean bending modulus and the lowest mean Vickers hardness number, flexural
strength, and impact strength [10].
In a separate study on 3D-printed materials, the printed group had the lowest rough-
ness before polishing, the lowest bacterial adherence after 90 min, and superior flexural
qualities except for strength. Polished PMMAs had similar surface roughness and microbial
adherence [11].
Flexural testing showed that neither the IvoBase printed group nor Vertex Ther-
moSens specimens fractured under load, while other groups had flexural strength ratings of
71.7 ± 7.4 MPa to 111.9 ± 4.3 MPa. Flexural strength and surface hardness varied from
67.13 ± 10.64 MPa to 145.66 ± 2.22 MPa, indicating significant differences between the
tested materials. CAD/CAM and polyamide had the highest flexural strength, while a
third group and polyamide had the lowest. Flexural strength was lowest in 3D-printed
materials [12].
Antibacterial 3D-printed materials have been enhanced using various methods.
Stereolithography-printed aluminum nitride composites had good dispersion and antibac-
terial properties, reducing colony-forming units by 70%. Aluminum nitride-reinforced
PMMA resins also had good mechanical properties, with a 12 percent loss of ultimate
strength for ceramic fractions of 15 percent and the potential for further strengthening
through conventional post-curing [13].
Three-dimensional-printed materials may have lower mechanical properties than
heat-cured PMMA, according to some studies. ZrO2 NPs in 3D-printed resins increased
flexure strength, impact strength, and hardness (p < 0.05) but not surface roughness or
elastic modulus. Three-dimensional-printed resins with ZrO2 NPs had better mechanical
properties than heat-polymerized acrylic resin. The new nano-composite denture-based
resins may be clinically applicable [14].
Biomedicines 2023, 11, 2155 3 of 15

Considering these advancements, the present study aimed to investigate the mechan-
ical properties of 3D-printing materials and compare them with the conventional poly-
methylmethacrylate. Specifically, we evaluated and compared the compression, flexural,
and tensile properties of samples manufactured using these two approaches. Additionally,
scanning electron microscopy was employed to examine the surface characteristics of the
investigated samples. By elucidating the mechanical performance of 3D-printed occlusal
splints, this research contributes to our understanding of their potential applications in
clinical practice.

2. Materials and Methods

2.1. Manufacturing of Experimental Samples
2.1.1. PMMA
For each mechanical trial, 20 samples were created using polymethylmethacrylate
(Orthocryl® —Dentaurum, Ispringen, Germany) and the “salt and pepper” technique in
accordance with the manufacturer’s instructions.
According to the manufacturer’s instructions, the salt-and-pepper method begins by
first combining salt and pepper. Applying a coating of powder (polymer), followed by
a layer of liquid (monomer), and then applying alternating layers of powder and liquid
with tiny pendulum motions. Apply only as much liquid as the powder can absorb. The
substance must not run off. To prevent air pockets from forming under the screws, a slightly
larger amount of fluid at the outset can be applied so that the acrylic can spread under
the screws. Powder must be used to complete the application. Sufficient powder must be
applied to dry the top layer.
The samples were placed for curing in the pressure vessel containing water at be-
tween 40 and 46 ◦ C/104 and 115 ◦ F and a pressure of 2.2 bars (30 p.s.i.) for 20 min.
The samples included flat samples for tensile testing, parallelepipedal prisms for flexing
(2 mm × 2 mm × 25 mm), and standard cylinders (4 mm diameter × 8 mm length)
for compression.

2.1.2. 3-D Printed

Using dental CAD software program (Exocad; Exocad GmbH, Darmstadt, Germany),
the samples were digitally designed, and with the help of the 3D printer (Stratasys Ltd.,
Eden Prairie, MN, USA), the samples were printed from biocompatible clear resin MED610
(Stratasys Ltd., Eden Prairie, MN, USA) according to specifications of the manufacturer.
Twenty pieces were produced with the same dimensions as the control samples, which
were manufactured from PMMA.

2.2. Evaluation of Mechanical Properties

For the mechanical evaluation, the samples were produced in conformity with ISO
4049:2019 [6]. Throughout the preparation process, silicone molds were used to lessen the
formation of cracks and flaws within the material.
A universal testing device (LR5K Plus, Lloyd Instruments Ltd., West Sussex, UK) with
a maximum allowable capacity of 5 KN was used to test the mechanical characteristics
at room temperature of 23 ◦ C. Data processing was carried out using Nexygen software
(version 4.0) [15]. According to ISO 4049:2019 [6], the samples (n = 20) were polymerized at
dimensions under the manufacturer’s conditions.
Three various mechanical tests were conducted:
1. The compressive strength test (Figure 1), which gauges the material’s stiffness and
determines the breaking point and compressive strength curve. The Nexygen software
generated test results while each compression sample was being tested at a speed of
0.5 mm/min and a force of 50 N/s. The samples used for this test were cylindrical in
form, measuring 6 mm in height and 4 mm in diameter.
 Biomedicines 2023, 11, x FOR PEER REVIEW 4 of 1
Biomedicines 2023,
Biomedicines 11,11,
2023, x FOR
2155 PEER REVIEW 4 of 15 4 of 15

Figure 1. Testing the compressive strength on PMMA cylindric samples (PMMA and 3D-printed
Figure
Figure 1. Testing
1.
sample). Testingthethe compressive
compressive strength
strength on PMMAon cylindric
PMMAsamples
cylindric samples
(PMMA (PMMA and
and 3D-printed 3D-printed
sample).
sample).
2. The three-point bending test was used to conduct the bending resistance test
2. (Figure
The three-point bending
2), whichbending
measured
test was used to conduct the bending resistance test (Figure
2. The 2), three-point
which measured testbending
bending was resistance
used
resistance toand and the
conduct Young’s
Young’s
modulus.
bending
modulus.
The sam-
resistance
The testwere
samples (Figure
rec
ples were rectangular prisms with dimensions of 25 mm in length, 2 mm in height,
2), which
tangular measured bending resistance and Young’s modulus. The samples were rec-
and 2 mm prisms with
in width. dimensions
With of N/min,
a force of 50 25 mm in thelength,
arm was 2 mm in height,
lowered and
at a pace of 2 mm in
tangular prisms withofdimensions of 25 mm in lowered
length, 2atmm in height, and 2 mm in
1width.
mm/min. With a force 50 N/min, the arm was a pace of 1 mm/min.
width. With a force of 50 N/min, the arm was lowered at a pace of 1 mm/min.

Figure2.2.Prior
Figure Priortoto and
and throughout
throughout the evaluation,
the evaluation, rectangular
rectangular PMMAPMMA prisms
prisms were were
used used to measur
to measure
Figure 2. Prior bending
thethree-point
the three-point tobending
and throughout the evaluation, rectangular PMMA prisms were used to measure
resistance.
resistance.
the three-point bending resistance.
3.
3. To Todetermine
determine thethe
tensile strength
tensile (Figure
strength 3), a test
(Figure 3),piece
a testwas subjected
piece to an increasing
was subjected to an increas
3. To axial force, typically
determine until itstrength
thetypically
tensile broke, while the accompanying changes in the test piece’s
ing axial force, until it (Figure 3), a test
broke, while the piece was subjected
accompanying to aninincreas-
changes the tes
length
ing axialwere recorded.
force, Based
typically untilon it
thebroke,
ASTM-D638
while reference
the standard [16],
accompanying measure-
changes in the test
piece’swere
ments length were recorded.
performed using a load Based
force on5 the
of N ASTM-D638
and a stress of reference
1000 N/mm standard
2 . The [16]
piece’s length were
measurements were recorded.
performed Based
using on
a the force
load ASTM-D638
of 5 N reference
and a stress standard
of 1000 [16],2
N/mm
test pieces utilized for the tensile test were flat rectangular shapes with dimensions of
measurements were performed using a test
loadwere
forceflat
of 5rectangular
N and a stress of 1000
withN/mm
dimen.
2
2The
mmtestthick,pieces
6 mmutilized
wide, and for40the
mmtensile
long. They provided shapes
the testing equipment with
The
asions
testofpieces
calibrated 2 mm utilized
part thick,
and two
for
6 mm the
wide,
gripping
tensile
and
ends
test
(2 40
mm
were
mm × 10
flat
long. rectangular
mm They provided
× 10 mm).
shapes with dimen-
the testing equip
sions
mentofwith
2 mm thick, 6 mm
a calibrated partwide, and gripping
and two 40 mm long.
endsThey provided
(2 mm × 10 mmthe testing
× 10 mm).equip-
ment with
2.3. Scanning a calibrated
Electron part and two gripping ends (2 mm × 10 mm × 10 mm).
Microscopy
Scanning electron microscopy was performed on the fillers and the samples using
an FEI Inspect microscope (SEM-Inspect S, FEI Company, Hillsboro, OR, USA), S model,
functional in high-vacuum and low-vacuum, with an accelerating voltage between 200 V
and 30 kV (discs). The microscope had a 4096 × 3536 pixel image-processing capability
CCD-IR infrared inspection camera in addition to a backscatter electron detector. The
images were typically taken at magnifications of 500–1000 times.
Biomedicines 2023, 11, x FOR PEER REVIEW 5
Biomedicines 2023, 11, 2155 5 of 15

Figure3.3. Specimens
Figure Specimensthat
thatwere
wereutilized
utilizedto to evaluate
evaluate thethe tensile
tensile strength
strength prior
prior to and
to and during the
during
uation.
the evaluation.

2.4. Statistical Analysis

2.3. Scanning Electron Microscopy
JASP Version 0.16.3 (JASP Team, University of Amsterdam, Amsterdam, The Nether-
lands)Scanning
[17] has electron
been used microscopy was performed
to statistically on the
describe and fillers and
analyze the the samples usin
measured
FEI Inspect
mechanical microscope (SEM-Inspect S, FEI Company, Hillsboro, OR, USA), S mo
characteristics.
Shapiro–Wilk tests and Q–Q
functional in high-vacuum and plots have been used
low-vacuum, withtoanassess the normality
accelerating of data
voltage between 2
distributions resulting from the measured characteristics.
and 30 kV (discs). The microscope had a 4096 × 3536 pixel image-processing capab
Descriptive statistics have been computed and reported. Median values and interquar-
CCD-IR infrared inspection camera in addition to a backscatter electron detector. The
tile ranges (IQR) were considered reliable measures of central tendency and data spread,
ages were typically
respectively, regardlesstaken
of the at magnifications
symmetrical of 500–1000
or skewed times.
distribution of the described data.
Mean values and standard deviations (SD) were also reported as indicators of central
2.4. Statistical
tendency Analysis
and data spread, with a higher reliability in the case of normally distributed data
(p > 0.05 following the Shapiro–Wilk test).
JASP Version 0.16.3 (JASP Team, University of Amsterdam, Amsterdam, The N
Independent samples t-test was used to evaluate the degree of significance between
erlands)
the [17]
samples. has
The been
level used to statistically
of statistical describe
significance was chosenand
to beanalyze thecomparisons.
0.05 for all measured mecha
characteristics.
The mechanical characteristics of the examined materials were graphically presented
Shapiro–Wilk
and contrasted tests and
using boxplots, Q–Q plots
raincloud plots, have been
and plots forused
meanstoandassess the normality
their 95% CI. of
distributions resulting from the measured characteristics.
3. Results
Descriptive statistics have been computed and reported. Median values and i
3.1. Compression
quartile ranges (IQR) were considered reliable measures of central tendency and
In Table 1, the results of the Young’s modulus of compression and tensile strength are
spread, respectively, regardless of the symmetrical or skewed distribution of the descr
represented. Only valid registrations of the tested samples have been used in this analysis.
data.
The Mean
values forvalues and standard
the Young’s modulus of deviations
compression(SD)
for were also reported
both printed as indicators
and control samples of ce
tendency and data spread, with a higher reliability in the case of normally
have a normal distribution (p < 0.05). The tensile strength for printed samples also has distributed
a
normal
(p > 0.05distribution
following (p the
< 0.05), and the control
Shapiro–Wilk has a non-normal distribution.
test).
InIndependent
Figure 4, the aspect
samples of the samples
t-test after the
was used mechanical
to evaluate compression
the degree of test can be
significance betw
observed with the macroscopic structural modification accordingly.
the samples. The level of statistical significance was chosen to be 0.05 for all comparis
In Figure 5, the raincloud plots for the Young’s modulus of compression and tensile
strengthThecanmechanical
be observed.characteristics
The 3D-printedof the examined
material has lowermaterials wereforgraphically
median values both tests. prese
Itand
can contrasted using
also be observed boxplots,
that raincloud
the 3D-printed plots,
material has aand plots
smaller for means
interquartile and their
distance and 95% CI
a smaller variability in the samples tested.
3. Results
3.1. Compression
In Table 1, the results of the Young’s modulus of compression and tensile stre
are represented. Only valid registrations of the tested samples have been used in this a
ysis. The values for the Young’s modulus of compression for both printed and co
samples have a normal distribution (p < 0.05). The tensile strength for printed samples
 Young’s Modulus of Compres-
Tensile Strength (MPa)
sion (MPa)
Table 1. Young’s modulus of compressionControl
Printed and tensile strength:
Printeddescriptive statistics
Control for PM
(control) and 3D-printed materials in the compression test (SD—standard deviation; IQR—in
Valid N 13 16 13 16
Biomedicines 2023, 11, 2155 quartile range). 6 of 15
Shapiro–Wilk p-
0.007 <0.001 0.017 0.586
value Young’s Modulus of Compres-
Tensile Strength (MPa)
TableMedian
1. Young’s modulus 1011.4 1468.61
and tensile strength: 50.5
sion (MPa)
of compression 76.85
descriptive statistics for
Mean 960.7
PMMA (control) and 3D-printed Printed 1326.18
materials in the Control 46.5 75.51
Printed deviation;
compression test (SD—standard Control
SD
IQR—interquartile
Valid N range). 84.8 13 331.97 16 6.3 13 7.49 16
IQR
Shapiro–Wilk p- 167.7 307.19
Young’s Modulus of 11.5 10.4
Minimum 853.40.007
Compression589.36
<0.001
(MPa)
Tensile 0.017
37.1 Strength (MPa) 63.12 0.586
value
Maximum
Median 1055.7Printed
1011.4 1598.58
Control
1468.61 52.9 50.5 Control
Printed 86.89 76.85
Valid N
Mean 13
960.7 16
1326.18 13 46.5 16 75.51
In Figure 4,
Shapiro–Wilk the aspect
p-value of the
0.007samples after the
<0.001 mechanical
0.017 compression 0.586 test can be
SD 84.8 331.97 6.3 7.49
observed with the macroscopic1011.4
Median
structural modification
1468.61
accordingly.
50.5 76.85
IQR 167.7 307.19 11.5 10.4
Mean 960.7 1326.18 46.5 75.51
Minimum 853.4 589.36 37.1 63.12
SD 84.8 331.97 6.3 7.49
Maximum 1055.7 1598.58 52.9 86.89
IQR 167.7 307.19 11.5 10.4
Minimum4, the aspect 853.4
In Figure 589.36
of the samples 37.1
after the mechanical 63.12
compression test can
Maximum 1055.7 1598.58 52.9
observed with the macroscopic structural modification accordingly. 86.89

Figure 4. The aspect of the samples after the compression test (left—PMMA control, right—3D
printed).

In Figure 5, the raincloud plots for the Young’s modulus of compression and tensile
strength can be observed. The 3D-printed material has lower median values for both tests.
It can also be observed that the 3D-printed material has a smaller interquartile distance
and a smaller variability in the samples tested.
Figure 4.4.The
Figure Theaspect of theof
aspect samples after the compression
the samples test (left—PMMA
after the compression control,
test right—3D printed).
(left—PMMA control, right—
printed).

In Figure 5, the raincloud plots for the Young’s modulus of compression and ten
strength can be observed. The 3D-printed material has lower median values for both te
It can also be observed that the 3D-printed material has a smaller interquartile dista
and a smaller variability in the samples tested.

Figure
Figure 5. 5. Young’smodulus
Young’s modulus ofof compression
compression and
andtensile strength
tensile rainrain
strength cloud charts
cloud and descriptive
charts and descriptive
plots for PMMA (control) and 3D-printed materials.
plots for PMMA (control) and 3D-printed materials.
In Table 2, the results of the independent samples t-test for Young’s modulus of
compression and tensile strength can be observed with statistically significant values for
both tests p < 0.05. This results in the rejection of the null hypothesis that there is no
significant difference between the samples tested, meaning that there is a statistically
significant difference in the compression test between the 3D-printed material and the
standard PMMA.
Figure 5. Young’s modulus of compression and tensile strength rain cloud charts and descrip
plots for PMMA (control) and 3D-printed materials.
 In Table 2, the results of the independent samples t-test for Young’s modulus of com
pression and tensile strength can be observed with statistically significant values for both
Biomedicines 2023, 11, 2155
tests p < 0.05. This results in the rejection of the null hypothesis that there is no significan
7 of 15
difference between the samples tested, meaning that there is a statistically significant dif
ference in the compression test between the 3D-printed material and the standard PMMA
Table 2. Young’s modulus of compression and tensile strength comparison of the materials under
Table 2. Young’s
investigation modulus
(PMMA of and
as control compression and tensile strength comparison of the materials unde
3D printed).
investigation (PMMA as control and 3D printed).
Young’s Modulus of
Young’s Modulus of Compression Tensile Strength (MPa) (MPa)
Compression (MPa)(MPa) Tensile Strength
Independent Samples
Independent t-test
Samples t-test
PMMA control vs. 3D printed
PMMA control vs. 3D printed 0.001 0.001 0.001 0.001

3.2. Bending/Flexural
3.2. Bending/Flexural
InFigure
In Figure6, 6,thethe aspect
aspect after
after the the flexural
flexural mechanical
mechanical test
test can becan be observed
observed with thewith the
maximum
maximumbendbend forforthethe
tested sample.
tested sample.

Figure6.6.Aspect
Figure Aspect after
after thethe bending/flexural
bending/flexural testing
testing of theofsamples.
the samples.

In
InTable
Table3, 3,
thethe
descriptive statistics
descriptive can becan
statistics observed for the mechanical
be observed bending/flexural
for the mechanical bending/flex
tests: Young’s modulus of bending, load at break, maximum bending stress
ural tests: Young’s modulus of bending, load at break, maximum bending stress at maxi at maximum
load, and stiffness of the investigated materials (control PMMA and 3D printed). The
mum load, and stiffness of the investigated materials (control PMMA and 3D printed)
number of valid tests can be observed. There is normal distribution (p < 0.05) for the
The number
Young’s modulusof valid tests can
of bending (PMMA be observed. There
and printed) and is
fornormal
stiffnessdistribution (p < 0.05) for the
(both samples).
Young’s modulus of bending (PMMA and printed) and for stiffness (both samples).
Table 3. Young’s modulus of bending, load at break, maximum bending stress at maximum load,
Table
and 3. Young’s
stiffness modulus ofmaterials
of the investigated bending, load at
(control break,
PMMA maximum
and bending
3D printed). stress at
SD—standard maximum load
deviation;
and stiffness of the investigated
IQR—interquartile range. materials (control PMMA and 3D printed). SD—standard deviation
IQR—interquartile range.
Young’s Modulus of Maximum Bending Stress
Young’s Modulus Load at Break (N) Stiffness (N/m)
Bending (MPa) of Maximum Bending
at Maximum Stress
Load at
(MPa)
Load at Break (N) Stiffness (N/m)
Bending
Printed (MPa)
Control Printed Control Maximum
PrintedLoad (MPa)
Control Printed Control
Valid N Printed 19 Control
23 Printed
19 Control23 Printed 19 Control
23 Printed
19 23 Control
Valid N
Shapiro–Wilk 19 23 19 23 19 23 19 23
0.002 <0.001 0.64 0.174 0.99 0.833 0.002 <0.001
Shapiro–Wilk
p-value
0.002 <0.001 0.64 0.174 0.99 0.833 0.002 <0.001
p-value
Median 1287.91 7092.49 36.55 21.91 68.1 103.81 53,358 41,222.01
MedianMean 1287.91
1443.3 7092.49
50,237.74 36.55
36.95 21.9124.88 68.1 68.11 103.81
108.04 53,358
60,982.5 41,222.01
330,098.91
Mean SD 1443.3
410.7 50,237.74
144,037.9 36.951.8 24.88 7.4 68.11 2.72 108.04
29.96 60,982.5
17,286.6 330,098.91
991,464.4
SDIQR 410.7
409.77 144,037.9
7143.04 1.81.7 7.4 11.01 2.72 3 29.96
44.77 17,286.6
17,372.5 991,464.4
25,595.48
IQR
Minimum 409.77
1017.5 7143.04
4115.9 1.7
33.6 11.0114.04 3 62.3 44.77
53.94 17,372.5
43,137 25,595.48
25,276.75
Minimum
Maximum 1017.5
2394.5 4115.9
668,077.42 33.6
40.9 14.04 44.1 62.3 74 53.94
164.11 43,137
101,510 25,276.75
4,575,000
Maximum 2394.5 668,077.42 40.9 44.1 74 164.11 101,510 4,575,000
 Biomedicines 2023, 11, x FOR PEER REVIEW 8 of 15

Biomedicines 2023, 11, 2155 8 of 15

23, 11, x FOR PEER REVIEW 8 of 15
In Figure 7, the raincloud plots for the bending mechanical test can be observed. For
the Young’s modulus of bending, we can observe that there are a few outliers for the con-
In Figure 7, the raincloud plots for the bending mechanical test can be observed. For
trolYoung’s
the (PMMA). The load
modulus at break median
of the
bending, we can is higher
observe forthere
that the printed material with the
a lower
In Figure 7, the raincloud
interquartile plots for
distance and a bending
lower mechanical
variability. The test can beare
maximum
a few
observed.
bending
outliers
For atfor
stress maximum
control (PMMA). The load at break median is higher for the printed material with a lower
the Young’s modulus load of bending,
is lower we3D-printed
for the can observe that there are a few interquartile
outliers for the con- The stiffness
interquartile distance and a lowermaterial with
variability. The a tighter
maximum distance.
bending stress at maximum
trol (PMMA). Theraincloud
load at break median is higher for the
is aprinted material
variance with a lower
load is lowerplot shows
for the us
3D-printed that there
material with atighter
highinterquartile in the
distance.PMMA samples.
The stiffness
interquartile distance and plot
raincloud a lower
showsvariability. The
us that there is amaximum bending
high variance in the stress
PMMAatsamples.
maximum
load is lower for the 3D-printed material with a tighter interquartile distance. The stiffness
raincloud plot shows us that there is a high variance in the PMMA samples.

Figure 7. Young’s modulus of bending, load at break, maximum bending stress at maximum load,
Figure 7. Young’s modulus of bending, load at break, maximum bending stress at maximum load,
and stiffness for PMMA (control) and 3D printing, presented as rain cloud plots.
and stiffness for PMMA (control) and 3D printing, presented as rain cloud plots.

Table44presents
Table presentsthe
the independent
independent samples
samples t-test
t-test for for
the the mechanical
mechanical bending
bending tests tests
for for
Figure 7. Young’s modulus of bending, load at break, maximum bending stress at maximum load,
thePMMA
the PMMAand and3D-printed
3D-printedmaterial.
material.The
The3D-printed
3D-printedmaterial
material has
has higher
higher load
load at at break (p
break
and stiffness for PMMA (control) and 3D printing, presented as rain cloud plots.
<<
(p 0.001), and
0.001), andthe
thePMMA
PMMAhas hasa ahigher
highermaximum
maximumbending
bending stress
stress at
at maximum load (p <
maximum load
0.001).
(p < 0.001).
Table 4 presents the independent samples t-test for the mechanical bending tests for
the PMMA and 3D-printed
Table material.
Results
Table4.4. Results of the
of The 3D-printed
the independent
independent t-test material
t-test for
forthe has higher
theYoung’s
Young’s load
modulus
modulus at break
ofofbending,
bending, (p atatbreak,
load
load break,maxi-
< 0.001), and themaximum
PMMA has a
bendinghigher
stress maximum
at maximum bending
load stress
and at
stiffnessmaximum
between load
PMMA
mum bending stress at maximum load and stiffness between PMMA (control) and 3D-printed (p <
(control) and ma-
0.001). terial.
3D-printed material.

Young’s Modulus of Maximum Bending Stress

Table 4. ResultsYoung’s Modulus of t-test for the Young’s modulus
of the independent Load
Load at Break
at Break (N) (N)
Maximum Bendingload
of bending, Stress
at break, maxi-
Stiffness
Stiffness (N/m)(N/m)
Bending (MPa)
Bending (MPa) at Maximum
at Maximum LoadLoad
(Mpa)(Mpa)
mum bending stress at maximum load and stiffness between PMMA (control) and 3D-printed ma-
Applied
Applied Test
Test
terial. Independent
Independent Samples
Samples t-test t-test
p-values
p-values
3D Young’s
printed vs. Modulus of
Control 0.1 Maximum
<0.001 Bending Stress <0.001
3D printed vs. Control Load at Break (N) <0.001
0.1 <0.001 Stiffness (N/m) 0.2 0.2
Bending (MPa) at Maximum Load (Mpa)
lied Test 3.3.Tensile
3.3.
Independent Samples t-test
TensileTesting
Testing
InFigure
In Figure8,8,the p-values
theaspect
aspect after
after thethe mechanical
mechanical tensile
tensile test test
can can be observed.
be observed.
d vs. Control 0.1 <0.001 <0.001 0.2

3.3. Tensile Testing

In Figure 8, the aspect after the mechanical tensile test can be observed.

Figure8.8.Aspect
Figure Aspectafter
after the
the mechanical
mechanical tensile
tensile testtest of the
of the samples.
samples.
23, 11, x FOR PEER REVIEW 9 of 15
Biomedicines 2023, 11, 2155 9 of 15

Table 5 presents the descriptive

Table 5 presents statistics for the
the descriptive mechanical
statistics for thetensile test for
mechanical 3D printed
tensile test for 3D printed
and the control PMMA Young’s modulus of tensile testing and elongation
and the control PMMA Young’s modulus of tensile testing and elongation at break with
at break with
the valid samples.the
The Young’s
valid modulus
samples. of tensile
The Young’s testingofhas
modulus a normal
tensile testingdistribution
has a normal (p distribution
<
(p < 0.05)
0.05) for both samples, andforthe
both
3Dsamples,
printedandhasthe 3D printed
a normal has a normal
distribution fordistribution for the
the elongation atelongation
break (p < 0.05). at break (p < 0.05).
Table 5.of Young’s
Table 5. Young’s modulus modulus
tensile testing andofelongation
tensile testing anddescriptive
at break: elongation statistics
at break: for
descriptive
PMMA statistics
for PMMA
(control) and 3D-printed (control)
material in theand 3D-printed
bending material in thedeviation;
test. SD—standard bending test. SD—standard deviation;
IQR—interquartile
range. IQR—interquartile range.

Young’sYoung’s
ModulusModulus of Tensile
of Tensile Elongation at Break (mm)
Testing (MPa) Elongation at Break (mm)
Testing (MPa)
Printed Control Printed Control
Printed Control Printed Control
Valid N 19 22 19 22
Valid N 19 22 19 22
Shapiro–Wilk
Shapiro–Wilk p-value
p-value 0.035 0.035 0.046 0.046 0.031 0.031 0.397 0.397
Median Median 1496.31496.3 2081.062081.06 4.26 4.26 1.23 1.23
Mean Mean 1528 1528 2126.85 2126.85 4.24 4.24 1.21 1.21
SD SD 130.7 130.7 279.89 279.89 0.78 0.78 0.37 0.37
IQR IQR
166.1 166.1
353.65 353.65
0.99 0.99
0.28 0.28
Minimum Minimum 1383.21383.2 1795.761795.76 1.9 1.9
0.55 0.55
Maximum Maximum 1879.11879.1 2817.362817.36 5.5 5.5
1.96 1.96

In Figure 9, the raincloud plots for the mechanical tensile testing can be observed.
In Figure 9, the raincloud plots for the mechanical tensile testing can be observed. The
The median for Young’s modulus of tensile testing is lower for the 3D printed, and the
median for Young’s modulus of tensile testing is lower for the 3D printed, and the control
control has a lower
haselongation at break.
a lower elongation at These
break. values have ahave
These values significant statistical
a significant differ-
statistical difference, as
ence, as shown inshown
Table in
6. Table 6.

Figure 9. Comparative rain

Figure plots for 3D-printed
9. Comparative rain plotsmaterial and PMMA
for 3D-printed material(control)
and PMMAregarding
(control)Young’s
regarding Young’s
modulus of tensile testing
modulusand elongation
of tensile testingatand
break.
elongation at break.

Table 6. ComparisonTable
of 6. Comparison
Young’s modulus of Young’s modulus
of tensile of and
testing tensile testing and
elongation atelongation at break
break between thebetween the
investigated
investigated materials materials
(3D printed (3D printed
and control and control PMMA).
PMMA).

Young’s Modulus ofYoung’s Modulus

Tensile Test- of Tensile Elongation at Break (mm)
Elongation at Break (mm)
Testing (MPa)
ing (MPa)
Independent Samples t-test
Independent Samples t-test
3D printed vs. Control <0.001 <0.001
3D printed vs. Control <0.001 <0.001
Biomedicines 2023, 11, x FOR PEER REVIEW 10 of 15
Biomedicines 2023, 11, 2155 10 of 15

3.4. SEM Analysis

3.4. SEM Analysis
Scanning Electron Microscopy (SEM) (Figures 10 and 11) was used to analyze the
Scanning Electron Microscopy (SEM) (Figures 10 and 11) was used to analyze the
morphology
morphology ofof
the samples,
the samples,with
withlow
lowmagnification
magnification being
being used for the
used for the observation
observationofof ma-
jormajor
morphologic
morphologic features and a microstructure overview, medium magnification beingbeing
features and a microstructure overview, medium magnification
used forfor
used precise morphological
precise morphologicalfeatures,
features,and high
and magnification
high magnificationbeing
beingused
usedforfor
micro-
structural details.details.
microstructural

Figure 10.10.
Figure SEMSEMimaging
imagingof
of the
the PMMA (control)sample
PMMA (control) sample before
before andand
afterafter flexural
flexural strength
strength tests. tests.

In Figure 10, the PMMA sample in this study has a compact microstructure generated
by PMMA particles diffusing toward one another, forming strong connection necks due
to the photopolymerization process. At 500× magnification, many polyhedral pores are
visible, indicating the effectiveness of the consolidation process. The material diffusion
from left to right is evident in the upper left side, with a tendency for pores to form. SEM
microscopy was used to analyze the fracture microstructure following the flexural
strength test, showing complex solicitations such as lateral compression and extension.
The failure of the PMMA sample is evident on the lower side, with interior pore rupture
and PMMA neck failure close to the surface.

Figure 11. SEM imaging of the 3D-printed sample before and after flexural strength tests.

In Figure 10, the PMMA sample in this study has a compact microstructure generated
by PMMA particles diffusing toward one another, forming strong connection necks due
to the photopolymerization process. At 500× magnification, many polyhedral pores are
visible, indicating the effectiveness of the consolidation process. The material diffusion
from left to right is evident in the upper left side, with a tendency for pores to form. SEM

Figure 11. SEM imaging of the 3D-printed sample before and after flexural strength tests.
Biomedicines 2023, 11, 2155 11 of 15

microscopy was used to analyze the fracture microstructure following the flexural strength
test, showing complex solicitations such as lateral compression and extension. The failure
of the PMMA sample is evident on the lower side, with interior pore rupture and PMMA
neck failure close to the surface.
The compression determines the densification of the material; the holes decrease,
increasing overall resistance. The failure spreads through the material until it reaches the
dense layer, which breaks the sample. The printed PMMA (Figure 11) sample was generated
layer by layer, with a mean layer thickness of 350 µm and a transition zone of 50 µm. The
flexural strength of the material was tested perpendicular to the inter-layer transition
zones, and the fracture aspect is complex depending on microstructural aspects. The
compressed area on the lower side of the image shows good preservation of microstructural
aspects due to compression effort, and failure occurs simultaneously in both layers and
transition zones.

4. Discussion
Regarding the compression, our results concluded that the control material (PMMA)
has a statistically significant higher Young’s modulus of compression and tensile strength
(p < 0.05). Concerning the flexural tests, statistically significant and higher results were
shown to be better for the control samples (PMMA) for load at break. Maximum bending
stress at maximum load (MPa) is statistically more significant for the 3D-printed samples.
Young’s modulus of tensile testing (MPa) is statistically significant for the control samples.
The 3D-printed samples had statistically significant values for elongation at break.
The results of our study cannot clearly conclude which of the material behaves better,
as the control behaves better in some conditions and the 3D printed using the polyjet
technique in other conditions. The polyjet technique has brought some improvements in
the splint quality, and it also inherently has other advantages, such as reproducibility of
the technique, fast learning curve for the technician, scalability, less residual material and
lower toxicity, uniformity of the product, and mechanical proprieties that are the same in
all the thicknesses of the splint.
A review of the literature has shown similar results regarding the mechanical features
of the polyjet materials having better flexural strength [18].
To summarize the results of our study, PMMA shows better compression results with
higher values, whereas the 3D-printed polyjet material presents better tensile and flexural
mechanical results. This anisotropy is in accordance with other studies, which find that
modifying the force direction majorly influences the outcome of the mechanical testing [19].
Additionally, considering the technical aspect of the 3D-printing polyjet technique,
the mechanical proprieties differ due to the placement and orientation on the XYZ on
the printing tray, according to some studies [20]. Some papers suggest that the tensile
proprieties of the material, when printed along the Z-axis, are improved [21].
Other parameters, such as printing mode and type of finish, can be modified in the
printing process to enhance some proprieties, such as the tensile strength [22]. Additionally,
postprocessing of polishing can also significantly modify the results of the mechanical
testing [23].
Figure 10 shows a compact microstructure generated by PMMA particles diffusing
toward one another to form strong connection necks because of the photopolymerization
process in the PMMA sample prior to the flexural test. However, at 500× magnification,
many pores are seen that are polyhedral in shape and range in size from 80 to 200 nm.
In Figure 10, a pore detail shown at 1000× magnification shows the strong bonding of
the photopolymerized PMMA particles. The formation of tiny PMMA filaments on the
pores’ surface is evidence of the consolidation process’ effectiveness. The neck between
two previous PMMA particles can be seen in the middle-lower half of the image at a high
magnification level of 5000×, demonstrating the material diffusion from left to right. The
image’s upper left side demonstrates a tendency for pores to form. Because of the energy
Biomedicines 2023, 11, 2155 12 of 15

being dissipated through the pore walls, which enhances the material tenacity, this complex
structure may be exceedingly resilient.
SEM microscopy was also used to analyze the fracture microstructure following
the flexural strength test. The results are shown in Figure 10. Complex solicitations,
such as lateral compression on the upper side and extension on the lower side of the
testing specimen, take place. The energy is lost through the pores and produces intricate
micro solicitations over the PMMA necks inside the substance. Due to the breaking line’s
progressive elongation observable at low magnification, the failure first manifests itself
on the lower side. Average magnification demonstrates interior pore rupture and PMMA
neck failure close to the surface. It happens when necks elongate past the point of greatest
resistance, as seen at extreme magnification (5000×). On the middle-lower side of the
image, a broken neck can be seen, with the fracture margin looking like a “bent plastic
sheet” due to the intense elongation effort.
On the plus side, the compression determines the densification of material, and
the holes decrease, increasing the overall resistance. The failure, which started on the
specimen’s lower side, gradually spreads through the material until it reaches the dense
layer, which suddenly becomes exposed during the elongation effort and completely breaks
the sample, as seen in the right side of the SEM image at low magnification in Figure 10.
As a result, the PMMA sample’s overall behavior shows good tenacity but just average
flexural strength. The addition of a modest amount of micro-sized filler material may help
the situation.
The printed PMMA sample was generated layer-by-layer by adding material that
was locally photopolymerized. Thus, the SEM image at low magnification (100×) in
Figure 11 presents a mean layer thickness of about 350 µm. Successive layers are bonded
together by a transition zone of about 50 µm. Moderate magnification (×500) reveals a
compact structure of the PMMA inside of the printed layers having a relative dendritic
aspect and a low number of pores. Only a few rounded pores are observed ranging from
10 to 30 µm in diameter. This compact structure inside of the printed layers assures good
cohesion of the material. Unfortunately, the high magnification SEM images (1000× and
5000×) in Figure 11 indicate a fine-grained structure of the layer transition zone, which is a
sign of a lower cohesion due to the partial lack of photopolymerization. The presence of
small, rounded PMMA grains of about 5 µm might be sensitive to certain effort dissipation
through the material.
The flexural strength of the material was tested perpendicular to the inter-layer transi-
tion zones, as observed at low magnification (100×) in Figure 11, and the fracture aspect is
complex depending on the microstructural aspects. Therefore, the average magnification
(500×) in Figure 11 reveals the lower part of the sample that supports the elongation effort
in the upper side of the image. The transition zones are very tensioned and elongated,
proving their behavior as failure promoters, circumstances better observed at higher mag-
nifications (1000× and 5000×). Since they disintegrated, the failure is further propagated
into the printed layers. The compressed area situated on the lower side of the image reveals
good preservation of the microstructural aspects due to the compression effort, and the
failure occurs simultaneously in both layers and transition zones.
SEM investigation proves that lower values obtained for the flexural strength of printed
PMMA compared to the bulk samples are generated by the behavior of the transition zones
between printed layers. There might be an improvement in the quality of the material with
more control of the parameters allowing a better adhesion between printed layers.

Limitations
This study was conducted with some constraints regarding the sample size and the
number of products to be compared. Ideally, without any space and physical constraints,
more samples in different forms should be used.
Only one type of printing direction was used, and this can be a limitation due to the
increased anisotropy of the mechanical proprieties in such cases. Additionally, no tweaking
Biomedicines 2023, 11, 2155 13 of 15

of other proprieties of the printing process was performed, such as surface finish or speed
of printing.
Assessing materials with the purpose of dental use must consider the oral environment,
which is complex. Aging the materials modifies the proprieties and can drastically change
the proprieties and the behavior for the foreseen period of use of the appliance [24].
Only one type of printer and one type of material were used.
Some studies suggest that there is no statistical significance in different 3D-printed ma-
terials using another type of printing method (low-force stereolithography) when assessing
mechanical proprieties [25,26].
Further studies should, therefore, be performed to investigate whether triple-jetting
technology could be suitable for occlusal retainers after conventional [27], lingual [28], or
aligner-based orthodontic treatments [29]. Additionally, adding different nanofillers [30] to
the compound could enhance some proprieties, as seen in previous studies [10–14,31,32].

5. Conclusions
The findings of this study demonstrate that 3D-printed materials, particularly those
produced using triple-jetting technology, offer a promising and viable solution for clinical
applications. Our research revealed favorable mechanical properties of the 3D-printed
material, indicating its potential to replace the conventional heat-cured resin (PMMA) in
various applications.
However, further exploration and understanding of 3D-printing protocols and pro-
cesses are warranted to enhance the mechanical properties of the printed materials. Im-
provements in these areas will contribute to the optimization of 3D-printed occlusal splints
for clinical use.
Additionally, while polyjet technology is still under development, future research
endeavors can expand its capabilities and explore its potential in the field of orthodontic
occlusal splint manufacturing. The ease of use and comparable mechanical properties of
polyjet technology make it an appealing avenue for further investigation.
In conclusion, the present study highlights the significant potential of 3D-printed
materials in clinical practice. PMMA showed better compression results with higher values,
whereas the 3D-printed polyjet material presented better tensile and flexural mechani-
cal results. However, ongoing research and advancements in 3D-printing protocols and
technologies are crucial to unlocking the full range of benefits and improving the me-
chanical properties of these materials. By capitalizing on these developments, the field of
orthodontics can continue to progress towards more effective and efficient occlusal splint
manufacturing techniques.

Author Contributions: Conceptualization, I.B. and M.M.; methodology, M.B.; software, B.C.; vali-
dation, L.C.; formal analysis, D.O.; investigation, S.C. and D.P.; resources, G.B.; data curation, C.D.;
writing—original draft preparation, H.O.; writing—review and editing, H.A.C.; visualization, M.M.;
supervision, I.B.; project administration, G.B.; funding acquisition, I.B. 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.
Informed Consent Statement: Not applicable.
Data Availability Statement: Not applicable.
Conflicts of Interest: The authors declare no conflict of interest.

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