RESEARCH AND EDUCATION

Comparative evaluation of the effect of thermocycling on the

mechanical properties of conventionally polymerized, CAD-CAM
milled, and 3D-printed interim materials
Simge Taşın, DDSa and Artur Ismatullaev, DDSb

The properties of materials ABSTRACT

used for interim fixed pros- Statement of problem. Studies on the energy absorption characteristics by means of elastic and
theses are important for the plastic material deformation of interim materials are lacking.
success of definitive restora-
Purpose. The purpose of this in vitro study was to compare the effect of different thermocycling
tions. The interim materials
periods on the flexural strength (sfs), resilience (Ur), and toughness (UT) of conventionally
should possess certain bio- polymerized, computer-aided design and computer-aided manufacturing (CAD-CAM) milled, and
logical, esthetic, and mechan- 3-dimensionally (3D) printed interim materials.
ical properties, including color
Material and methods. Rectangular specimens (n=30 for each material) were fabricated from
and dimensional stability and autopolymerized polymethyl methacrylate (PMMA), bis-acryl resin (Bis-acryl), CAD-CAM
adequate resistance to func- polymethyl methacrylate-based polymer (CAD-CAM/Milled), and 3D-printed composite resin (3D-
tional loads.1,2 These re- Printed). Each material was divided into 3 groups (n=10) according to the applied thermocycling
quirements are particularly (5  C to 55  C) procedure: control (0 cycles), 2500, and 10 000 cycles. Parameters of the materials
important when the treatment such as sfs, Ur, and UT were tested in a 3-point bend test according to International Organization
time is extended.3,4 for Standardization (ISO) 10477. Data were statistically analyzed with the Shapiro-Wilk test
Interim restorations are followed by Kruskal-Wallis test, the Mann-Whitney U test, the Friedman test, and Wilcoxon
signed-rank test (a=.05).
subjected to temperature fluc-
tuation and functional loading Results. The tested material and thermocycling had a statistically significant influence on the sfs, Ur,
during their clinical service. and UT values (P<.05). PMMA showed the lowest mean sfs, Ur, and UT values (P<.05), and CAD-CAM/
Milled showed sfs values similar to those of 3D-Printed at all thermocycling periods. CAD-CAM/
Residual stresses resulting
Milled showed the highest Ur values at 10 000 cycles and the highest UT values at all
from these dynamic changes thermocycles. No significant differences were found in the mean change of sfs and Ur of CAD-
may cause deformation,5,6 CAM/Milled among different thermocycling periods.
ranging from reversible elastic
Conclusions. The results suggested that digitally fabricated interim materials had better
deformation to irreversible
mechanical properties than conventionally polymerized materials and that milled materials had
plastic deformation and to the highest stability in maintaining their initial capacity to absorb energy. (J Prosthet Dent
fracture. Therefore, the me- 2022;127:173.e1-e8)
chanical properties of interim
materials are of particular importance, as they might in- particularly for long-span interim restorations, which are
fluence the integrity of interim restorations during required to resist failure from bending.8,9
functional load. Flexural strength (sfs) is a mechanical
7
Resilience (Ur) and toughness (UT) are 2 other
parameter that has been widely used to evaluate the essential mechanical parameters. Ur is a measure of the
strength of dental materials and is a critical property, capacity of a material to absorb energy per unit volume

a
Assistant Professor, Department of Prosthodontics, Faculty of Dentistry, Cyprus Health and Social Sciences University, Mersin, Turkey.
b
Assistant Professor, Department of Prosthodontics, Faculty of Dentistry, University of Kyrenia, Mersin, Turkey.

THE JOURNAL OF PROSTHETIC DENTISTRY 173.e1

173.e2
Clinical Implications
The 3D-printing resin tested could be a more
promising material for clinical application than the
conventionally polymerized materials because of its
improved mechanical properties, whereas CAD-
CAM milled polymethyl methacrylate-based resin
tested is more suitable for long-term treatments
because of its high potential to dissipate destructive
fracture energy.
without displaying permanent deformation and is related
to the pure elastic properties of material.10 UT is defined
as the amount of energy required to completely fracture a
material and is characterized by both the elastic and
plastic properties.10 A good understanding of these 2
properties may be important in material selection
because the resilience and toughness provide informa-
tion on the behavior of a material at lower stress levels
rather than at the fracture level.11
Interim fixed prostheses are commonly fabricated
from conventional materials including polymethyl
methacrylate and bis-acryl composite resins because of
their easy accessibility and relatively low cost. How-
ever, the conventional materials exhibit drawbacks that
limit their application.12,13 With advancements in
digital technology, the computer-aided design and
computer-aided manufacturing (CAD-CAM) of interim
restorations is gaining acceptance.14 Millable poly-
methyl methacrylate-based interim materials have
highly cross-linked structures.15 These structural
properties provide decreased residual monomer,
increased strength, and durability depending on their
chemical composition when compared with conven-
tional materials.14,16,17
Despite improved mechanical performance, there is
still concern about the limitations of the milling proced-
ure, and the high cost of this method limits its use.18-20
The 3D-printing method is an alternative way of digi-
tally fabricating interim restorations and offers compar-
ative advantages. This method allows mass production
with little material waste and reduces fabrication time,
and low-cost 3D-printers provide easy access to 3D-
printed materials.18 Although acceptable surface and
optical properties have been reported,21-23 investigations
on the mechanical properties of 3D-printed interim res-
torations are lacking.
The effect of aging on the sfs of the interim materials
fabricated by conventional and milling methods has been
relatively well documented,15,19,24,25 but information
regarding the effect of thermocycling on elastic and
plastic properties is sparse.26-28 Studies of 3D-printed
THE JOURNAL OF PROSTHETIC DENTISTRY
Volume 127 Issue 1
interim materials have investigated sfs29-32 and modulus
of elasticity33 but have not included an examination of
the influence of thermocycling. Additionally, the authors
are unaware of a study that focused on the evaluation of
the effect of thermocycles on the Ur and UT of 3D-printed
interim materials. Therefore, the purpose of the present
study was to compare the strength, resilience, and
toughness properties of conventionally polymerized,
milled, and printed interim materials after different pe-
riods of thermocycling by calculating sfs, Ur, and UT from
the stress-strain curve in a 3-point bend test. The null
hypotheses were that no difference would be found in sfs,
Ur, and UT among the tested interim materials and
that these parameters would not be influenced by
thermocycling.
MATERIAL AND METHODS
Autopolymerized polymethyl methacrylate (PMMA) and
bis-acryl composite resin (Bis-acryl), CAD-CAM poly-
methyl methacrylate-based polymers (CAD-CAM/Milled),
and 3D-printed composite resin (3D-Printed) interim
materials were evaluated in this study (Table 1). The
sample size was determined by using a statistical power
analysis software program (G*Power 3.1.9.3; Heinrich-
Heine-Universität Düsseldorf). The effect size was hy-
pothesized to be 0.57. Accordingly, with 0.05 significance
level and 0.8 power, the projected sample size needed was
10 specimens per group.
A split stainless-steel mold with slots of dimension
25×2×2 mm was produced to obtain PMMA (Temdent
Classic; Schütz Dental GmbH) and Bis-acryl (Protemp
4; 3M ESPE) specimens in accordance with the Inter-
national Organization for Standardization (ISO)
10477.34 The PMMA was mixed manually as per the
manufacturer’s recommendations. The mixture was
packed into the mold with a spatula. A glass slab loaded
with 14.7 N was placed on the surface of the mold to
remove excess resin material, and the specimens were
removed from the mold after 15 minutes. The Bis-acryl
resin was mixed in an automixing cartridge and injected
into the mold.
A rectangular plate (25×2×2 mm) was designed by
an experienced dental laboratory technician in the
system software program (Nauta XFAB Edition; DWS -
VAT) and saved as a standard tessellation language
(STL) file. The same rectangular plate design was
used to mill (Yenadent DS15; Yenadent Inc) the CAD-
CAM/Milled specimens from CAD-CAM polymethyl
methacrylate-based polymer blocks (Duo Cad; FSM
Dental) and to print 3D-Printed specimens from a com-
posite resin material (Temporis; DWS - VAT) in a
stereolithography-based 3D printer (XFAB 2500PD;
DWS) at a 90-degree build orientation. The thickness of
Taşın and Ismatullaev
January 2022 173.e3

Table 1. Materials used System 2007; NCSS Statistical Software). Descriptive

Product
Name Manufacturer Abbreviation Lot Number Type
Temdent Schütz-Dental PMMA 2017000568 Methyl
Classic methacrylate
Protemp 4 3M ESPE Bis-acryl 4108503 Bis-acrylate
composite resin
Duo Cad FSMDENTAL CAD-CAM/ 118 CAD-CAM
Milled polymethyl
methacrylate-
based polymer
Temporis DWS 3D-Printed 1921741 Composite resin
each layer was 60 mm, and the laser scanning speed
was 5000 mm/s. The 3D-Printed specimens were then
rinsed with isopropyl alcohol in an ultrasonic bath for 1
minute, and postpolymerization procedures were
completed in an ultraviolet polymerization unit (S2; DWS)
for 30 minutes.
The final dimensions of the specimens were adjusted
by using silicon carbide abrasive papers with decreasing
grit (360, 600) under constant water irrigation and
controlled with digital calipers (Digimatic CD-15DCX;
Mitutoyo). After storage in distilled water at 37  C for
24 hours, the specimens from each material were divided
into 3 groups (n=10) based on different thermocycling
(MTE-101; Mod dental, Esetron Smart Robot-
echnologies): control (0 cycles), 2500 cycles, and 10 000
cycles, which simulated 1 year of clinical aging.35 The
distilled water baths of the thermocycler were set to 5  C
and 55  C with a transport time of 15 seconds and a dwell
time of 30 seconds.
The flexural properties of each specimen were
determined in a 3-point bend test on a newly calibrated
universal testing machine (EZ 50; Lloyd Instruments
Ltd) with a 0.5-kN load cell. The distance between the
supports was 20 mm, and the crosshead speed was 1
mm/min. The applied force and the crosshead
displacement were recorded by using the software
program of the testing machine (Nexygen; Lloyd In-
struments Ltd). Flexural strength9 (MPa), modulus of
elasticity9 (MPa), and resilience10 (MJ/m3) were calcu-
lated by using the following formulas: sfs = 3F2bhmax L
2 , E=
Flin L3 s 2
Ur = 2Ey , where Fmax (N) is the maximum load, L
4dlin bh3
, Friedman test showed that the thermocycling
(mm) is the distance between supports, b (mm) and h
(mm) are the width and height of the specimen, E is
the modulus elasticity, Flin (N) is the chosen force in the
linear part of the stress-strain curve, dlin (mm) is the
deflection at Flin, and sy is the 0.2% yield strength
(MPa). The area under the stress-strain curve was used
to measure the toughness36,37 (MJ/m3) from UT = bhL 9A
, (P=.074).
where A (J) is the total area under the stress-strain curve
procured with the software program.
Statistical analyses were performed by using a
software program (Number Cruncher Statistical
statistical methods (mean, standard deviation, median,
minimum, maximum) and the distribution of data were
evaluated by the Shapiro-Wilk test. All data were
determined as nonnormally distributed; therefore, the
Kruskal-Wallis and Mann-Whitney U tests were used
to compare the groups. The Friedman test was used for
the comparisons of 3 thermocycling periods for each
parameter, and the Wilcoxon test was used to deter-
mine the differences among thermocycling periods
(a=.05).
RESULTS
The values of the calculated parameters for each group
and thermocycling period combinations are presented in
Figure 1 and Table 2. The Kruskal-Wallis test showed
significant differences in the sfs results among groups at
each evaluated thermocycling period (P<.05). The Mann-
Whitney U test revealed the lowest mean sfs values for
PMMA (P=.001), followed by Bis-acryl (P=.001) speci-
mens, at all thermocycling periods. When the differences
between mean sfs values of the CAD-CAM/Milled and
3D-Printed were compared, there were no significant
differences between groups at any thermocycling period.
The Friedman test showed that the thermocycling pe-
riods had a statistically significant influence on sfs results
for each evaluated group (P<.05). As per the Wilcoxon
test, the 10 000 thermocycles led to a significant decrease
in the mean values of sfs for PMMA (P=.005), Bis-acryl
(P=.013), and 3D-Printed (P=.005), but not for CAD-
CAM/Milled (P=.093) compared with that of the control
group.
The Kruskal-Wallis test showed significant differ-
ences in the Ur results among groups at each evaluated
thermocycling period (P<.05). The Mann-Whitney U
test revealed the lowest mean Ur values for PMMA
(P=.001), followed by Bis-acryl (P=.001), at all thermo-
cycling periods (P). When the differences between mean
Ur values of the CAD-CAM/Milled and 3D-Printed
were compared, there were no significant differences
between groups at any thermocycling period. The
period had a statistically significant influence on Ur re-
sults for each evaluated group (P<.05). As per the Wil-
coxon test, compared with the control group, the 10 000
thermocycles led to a significant decrease in the mean
values of Ur for PMMA (P=.005), Bis-acryl (P=.028), and
3D-Printed (P=.005), but not for CAD-CAM/Milled
The Kruskal-Wallis test showed significant differ-
ences in the UT results among groups at each evaluated
thermocycling period (P<.05). The Mann-Whitney U
test revealed the highest mean UT values for the

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173.e4 Volume 127 Issue 1

140
Ca Ca Ca
Ca
Ba Ca Cb
Ba 122 125
Bb 127 125
120 117 116
113
Flexural Strength (MPa)

108

100 99

Aa
Aa
80

68 Ab
62
60
49

40

20
PMMA Bis-acryl CAD-CAM/Milled 3D-printed
Material A

BCa Ca
1.20
Ca
Ca
Ca 1.12
Ba 1.04 1.03
1.00 Aa Ba Bb
0.98 0.93 Cb
Aa
Resilience (MJ/m3)

Ab 0.85
0.81
.80 0.77
0.74
0.72

0.64
.60
0.53

.40

.20
PMMA Bis-acryl CAD-CAM/milled 3D-printed
Material B
Control 2500 cycles 10K cycles

Figure 1. Box plot for values of tested groups. Group codes as shown in Table 1. Different uppercase letters denote statistical difference among groups of
same cycles. Different lowercase letters denote statistical difference among cycles of same group (P<.05). A, Flexural strength. B, Resilience.

CAD-CAM/Milled, followed by 3D-Printed, Bis-acryl, results for each evaluated group (P<.05). As per
and PMMA at all thermocycling periods (P=.001). the Wilcoxon test, the mean values of UT were sig-
The Friedman test showed that the thermocycling pe- nificantly decreased after 10 000 thermocycles for
riods had a statistically significant influence on UT PMMA (P=.005), Bis-acryl (P=.037), CAD-CAM/Milled

THE JOURNAL OF PROSTHETIC DENTISTRY Taşın and Ismatullaev

January 2022
6.00
5.00
Toughness (MJ/m3)
4.00
Ba
3.00
2.47
Aa
2.00 1.82
Ab
1.31 Ac
1.00 0.96
.00
PMMA
Figure 1. Continued. C, Toughness.
(P=.005), and 3D-Printed (P=.005) compared with that
of the control group.
DISCUSSION
Both null hypotheses were rejected, as all investigated
mechanical properties were dependent on the tested
materials and these properties varied after thermocycling.
Although the flexural strength test may not completely
replicate the dynamic oral environment, its advantages in
comparing the mechanical properties of dental materials
under controlled conditions have been demonstrated.8,10
Therefore, the flexural strength test was used in the
present study to evaluate the mechanical parameters of
materials.
Thermocycling can be applied as a method of artificial
aging, which mainly consists of water immersion and
temperature change under standardized laboratory con-
ditions.35 The received results were consistent with those
of previously reported findings,5,6,19,26 where most of the
parameters of interim materials showed considerable
degradation with thermocycling. In the present study,
PMMA showed a significantly lower sfs and the highest
degradation of sfs (23.3%) during thermocycling. These
results are consistent with those of previous studies,24,28
which demonstrated that the mean sfs values of
conventionally polymerized methacrylate resins were
lower than those of bis-acryl resins. The increased
strength of the bis-acryl resins could be related to
Taşın and Ismatullaev
173.e5
Ca
Ca
4.93
4.59
Cb Da
3.70
3.63 Da
3.09
Ba
Db
2.47
Bb 2.20
1.54
Bis-acryl CAD-CAM milled 3D-printed
Material
Control 2500 cycles 10K cycles C
multifactorial monomers capable of cross-linking with
other monomers.7 Additionally, they contain inorganic
fillers, which may dissipate destructive load energy and
inhibit the formation of microcracks.25 Moreover, the
cartridge delivery system, instead of hand mixing, with
adequate mixing in accurate proportions24 may improve
mechanical properties.
A higher sfs for milled interim materials than for
conventional materials has been reported3,5,6,14,17
because of their highly cross-linked structure and
polymerization process under optimized pressure and
temperature. Consistent with these previous studies,
the present study found higher sfs values for CAD-
CAM/Milled than for PMMA and Bis-acryl. However,
some previous studies19,20 compared the sfs of bis-acryl
resins with that of milled-PMMA interim materials and
reported inconsistent results, where different milled
resins showed similar, lower, or higher sfs values. The
results of the present study are consistent with those of
previous studies,14,19 where the sfs of CAD-CAM/
Milled were less affected by thermocycling than those
produced by conventional polymerization. Lower
polymerization of conventional materials may lead to
higher water absorption, which may induce a plasti-
cizing effect on polymer networks, resulting in lower
strength.13
Scotti et al32 compared the sfs of 3D-printed and bis-
acryl resin materials after storage in a water bath for 24
hours. Consistent with the results of the present study,
THE JOURNAL OF PROSTHETIC DENTISTRY
173.e6 Volume 127 Issue 1

Table 2. Mean ±standard deviation (SD), median, minimum, and maximum of modulus of elasticity and yield strength values for tested materials
Property Group Thermocycles Mean ±SD Median Minimum Maximum
Modulus of elasticity (MPa) PMMA Control 2284 ±676 2155 1334 3761
2500 2045 ±524 1926 1365 3034
10K 1810 ±161 1769 1600 2070
Bis-acryl Control 3464 ±166 3467 3114 3758
2500 3247 ±383 3074 2840 3928
10K 2606 ±511 2553 1779 3321
CAD-CAM/Milled Control 3107 ±422 3173 2624 3978
2500 3039 ±254 2897 2761 3440
10K 2829 ±387 2701 2184 3726
3D-Printed Control 3357 ±282 3333 3109 4083
2500 3214 ±192 3238 2973 3494
10K 2937 ±194 2989 2567 3128
Yield strength (MPa) PMMA Control 57 ±3 58 51 62
2500 52 ±8 50 41 63
10K 44 ±5 44 35 51
Bis-acryl Control 78 ±10 83 64 92
2500 72 ±6 73 59 81
10K 60 ±6 59 50 71
CAD-CAM/Milled Control 79 ±7 78 69 92
2500 75 ±7 76 64 84
10K 70 ±10 70 58 89
3D-Printed Control 85 ±1 86 84 87
2500 80 ±2 81 75 83
10K 66 ±3 66 62 71

3D-printed materials showed higher sfs than bis-acryl
resins. Prpic et al30 compared the sfs of milled-PMMA
and 3D-printed interim materials in a water bath for 50
hours and reported higher sfs for milled resins. Suralik
et al31 also evaluated the sfs of milled-PMMA and 3D-
printed 3-unit interim fixed prostheses, reporting higher
sfs for 3D-printed specimens than that for milled ones.
However, in the present study, the sfs in the CAD-CAM/
Milled and 3D-Printed groups were not significantly
different (P=.571). These differences suggest that the
fabrication method is not the only factor affecting the
mechanical properties of materials, which might also be
related to the different fabricating parameters, chemical
composition, specimen design, and testing proto-
col.16,17,33 In the present investigation, no significant
differences were found between the sfs of CAD-CAM/
Milled and 3D-Printed after 10 000 thermocycles, but
3D-Printed (7.5%) showed higher degradation than
CAD-CAM/Milled (6.6%) during aging. This could be
attributed to the residual stress from water uptake and
temperature change causing debonding between the
layers in 3D-Printed, which may provoke crack formation
and result in long-term structural failure.33
High resilience is essential for the long-term integrity
of restorations, as higher resilience increases the ab-
sorption of functional forces without plastic deformation
of the material. In the present study, 3D-Printed (1.10
±0.09 MJ/m3) showed the highest mean Ur values at
control, followed by CAD-CAM/Milled (1.04 ±0.24 MJ/
m3), Bis-acryl (0.90 ±0.22 MJ/m3), and PMMA (0.78 ±0.25
MJ/m3). Previous studies5,27,28 investigated the influence
of the degree of conversion on the resilience of conven-
tional interim materials and reported higher mean Ur
values than those in the present study because of
confusion with yield strength and sfs in the respective
formulas. The mean Ur values of CAD-CAM/Milled in
the present study were consistent with those reported by
Niem et al37 who compared the resilience and toughness
behavior of milled interim restorative materials by using a
similar formula.
The primary cause of damage requiring replacement
of the interim restoration is fracture2; therefore, tough-
ness defines the ability to absorb fracture energy, which
is important for the evaluation of the applicability of
long-term restorative materials. In the present investi-
gation, CAD-CAM/Milled had substantially higher UT
values than other materials; therefore, this material has
comparatively ductile characteristics, which was further
verified by its proportionally lower Ur and modulus of
elasticity values. This effect may be caused by the high
plastic energy-consuming property of the milled mate-
rials with longer polymer chains.37
In the results of the present study, CAD-CAM/Milled
showed Ur similar to that of 3D-Printed and Bis-acryl as
the control, but they showed distinct decreases in mean
Ur values (3D-Printed 31.8%, Bis-acryl 23%) after 10 000

THE JOURNAL OF PROSTHETIC DENTISTRY Taşın and Ismatullaev

January 2022
thermocycles. Although thermocycling reduced the me-
chanical properties of CAD-CAM/Milled in the present
study, these were lowest for Ur (10.6%) and UT (25%)
after 10 000 thermocycles. These findings showed that
CAD-CAM/Milled appeared less prone to hydrolytic
degradation processes than conventionally polymerized
and printed materials because of its denser cross-linked
and homogeneous structure, which decreased water
immersion and plasticizing effects as has been previously
discussed.15
Balanced plastic deformation of the material seems an
advantage for sealing flaws effectively. However, in
clinical applications, repeated extensive plastic deforma-
tion of a restoration might cause problems such as misfit,
resulting in the penetration of oral fluids,3 degradation of
the interim cement,11 and stress formation around the
abutment-implant junction.4 Nevertheless, resistance to
plastic deformation may increase the resistance to mar-
ginal gap formation, restoration fracture, and surface
wear. Therefore, resilience may be a more important
selection criterion than toughness. Although questions
remain regarding the clinical significance of these pa-
rameters and clinical investigations are sparse, according
to the results of the present study, 3D-Printed could be a
promising material for clinical application because of its
higher sfs and Ur, whereas CAD-CAM/Milled is more
suitable for long-term treatments because of its higher
potential to maintain its initial capacity for elastic and
plastic deformation.
The materials were tested under static loads, and re-
sults may be different when dynamic loads are used.
Further studies by using different materials with various
aging processes to simulate intraoral conditions are rec-
ommended to better understand material behavior.
Although in vitro studies allow clinicians to compare the
performance of materials under standardized conditions,
long-term clinical studies are required for the better
understanding of behavior of different interim materials.
CONCLUSIONS
Based on the findings of this in vitro study, the following
conclusions were drawn:
1. All investigated properties were affected by the type
of tested interim material and thermocycling
periods.
2. CAD-CAM/Milled and 3D-Printed have the highest
mean values for flexural strength at control, 2500,
and 10 000 thermocycles.
3. The lowest mean resilience values were observed
in PMMA at control, 2500, and 10 000 thermo-
cycles, and the highest mean resilience values
were observed in CAD-CAM/Milled at 10 000
thermocycles.
Taşın and Ismatullaev
173.e7
4. The lowest mean toughness values were found in
PMMA, followed by those of Bis-acryl, 3D-Printed,
and CAD-CAM/Milled at control, 2500, and 10 000
thermocycles.
5. CAD-CAM/Milled showed the highest stability in
maintaining its initial capacity for elastic and plastic
deformation during aging.
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Corresponding author:
Dr Simge Taşın
Faculty of Dentistry
Cyprus Health and Social Sciences University
Güzelyurt, Mersin 10
TURKEY
Email: simgetasin@gmail.com
Copyright © 2021 by the Editorial Council for The Journal of Prosthetic Dentistry.
https://doi.org/10.1016/j.prosdent.2021.09.020
Taşın and Ismatullaev