journal of the mechanical behavior of biomedical materials 133 (2022) 105333

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Journal of the Mechanical Behavior of Biomedical Materials

journal homepage: www.elsevier.com/locate/jmbbm

Temporary materials used in prosthodontics: The effect of composition,

fabrication mode, and aging on mechanical properties
Edmara T.P. Bergamo a, b, *, Tiago M.B. Campos a, Mariana M.T. Piza a, Eliezer Gutierrez a,
Adolfo C.O. Lopes a, Lukasz Witek b, c, Paulo G. Coelho b, d, e, Marcos Celestrino f,
Laura F.de Carvalho a, Ernesto B. Benalcázar Jalkh a, Estevam A. Bonfante a
a
Department of Prosthodontics and Periodontology, University of Sao Paulo, Bauru School of Dentistry, Bauru, Brazil
b
Division of Biomaterials, Department of Molecular Pathobiology, New York University College of Dentistry, New York, NY, USA
c
Department of Biomedical Engineering, New York University Tandon School of Engineering, Brooklyn, NY, USA
d
Hansjörg Wyss Department of Plastic Surgery, NYU Langone Medical Center, New York, NY, USA
e
Department of Mechanical and Aerospace Engineering, New York University Tandon School of Engineering, Brooklyn, NY, USA
f
Aliança Dental Laboratory, São Paulo, SP, Brazil

A R T I C L E I N F O A B S T R A C T

Keywords: Purpose: To evaluate the effect of composition, fabrication mode, and thermal cycling on the mechanical prop­
Dental prosthesis erties of different polymeric systems used for temporary dental prostheses.
Temporary prosthesis Materials and methods: Standard bar-shaped specimens (25 × 2 × 2 mm) were fabricated of six polymeric systems
Polymers
of varying compositions and fabrication modes (n = 10/group): conventional PMMA (Alike, GC) – group CGC;
Mechanical properties
conventional PMMA (Dêncor, Clássico) – group CD; bis-acryl (Tempsmart, GC) – group BGC; bis-acryl (Yprov,
Yller) – group BY; milled PMMA (TelioCAD, Ivoclar) - group MI; 3D printed bis-acryl – (Cosmos Temp, Yller)
group PY. Half of the specimens were subjected to 5000 thermal cycles (5 ◦ C to 55 ◦ C). Three-point bending tests
were performed using a universal testing machine with a crosshead speed set to 0.5 mm/min. Flexural strength
and elastic modulus were calculated from the collected data. FTIR spectra were recorded pre and post curing and
after thermal cycling to evaluate material composition and degree of conversion. Energy-dispersive spectroscopy
(EDS) and scanning electron microscope (SEM) were utilized to examine the composition and micromorphology
of the systems, respectively. Data were analyzed using two-analysis of variance and Tukey tests (α = 0.05).
Results: FTIR spectra indicated that BGC, BY and PY groups corresponded to urethane dimethacrylate systems
(bis-acryl), while CGC, CD, and MI groups corresponded to monomethacrylate systems, polymethyl methacrylate
(PMMA). Bis-acryl BGC system yeilded the highest flexural strength (80 MPa), followed by the milled PMMA MI
system (71 MPa), both statistically significant different relative to other groups. Bis-acryl BY exhibited the lowest
flexural strength (27 MPa). Thermocycling significantly increased the flexural strength of all polymeric systems
(~10–15 MPa), except for the 3D-printed PY group. Bis-acryl BGC (1.89 GPa) and conventional PMMA CGC
(1.66 GPa) groups exhibited the highest elastic modulus, followed by milled PMMA MI group (1.51 GPa) and
conventional PMMA CD (1.45 GPa) systems, with significant difference detected between BGC group and MI and
CD groups. The 3D printed PY (0.78 GPa) and bis-acryl BY (0.47 GPa) systems presented the lowest elastic
modulus. Thermocycling did not have a significant influence on the elastic modulus. FTIR spectra indicate water
sorption and release of unreacted monomers as well as increased degree of conversion (~5–12%) after thermal
cycling.
Conclusion: Composition and fabrication mode and thermal cycling significantly affected the mechanical prop­
erties of polymeric systems used for temporary dental prostheses.

* Corresponding author. Department of Prosthodontics and Periodontology, University of Sao Paulo – Bauru School of Dentistry, 9-75 Octavio Pinheiro Brizolla,
17012-901, Bauru, SP, Brazil.
E-mail addresses: edmaratatiely@gmail.com, edmarabergamo@usp.br (E.T.P. Bergamo).

https://doi.org/10.1016/j.jmbbm.2022.105333
Received 17 April 2022; Received in revised form 19 June 2022; Accepted 20 June 2022
Available online 30 June 2022
1751-6161/© 2022 Elsevier Ltd. All rights reserved.
E.T.P. Bergamo et al.
1. Introduction
Oral rehabilitation is a complex treatment, and definitive prostheses
are usually not fabricated in a single appointment, requiring the use of
temporary prostheses to restore esthetic’s and function (Federick,
1975). Temporary prostheses have to fulfill important roles within the
mentioned timeframe in the mouth, including the protection of pulpal
and periodontal tissues (from chemical, thermal, and bacterial irritants),
evaluation of the prognosis of the remaining dental structure, teeth
preparation, maintenance of established occlusal vertical dimension,
phonetic, and masticatory function, as well as soft tissue conditioning
(Federick, 1975; Yao et al., 2014). It is also important to note their
current pivotal function in the assessment of the planned definitive
restoration. Ideally, to attain such requirements, temporary prostheses
should present a favorable fracture resistance, good polishing and
marginal adaptation, wear resistance, and low or ideally no change in
temperature during polymerization, as well as they should be easily
fabricated, repaired, and removed (Federick, 1975; Yao et al., 2014).
Several polymeric systems have been developed for temporary
prostheses, including the most popular monomethacrylate, polymethyl
methacrylate (PMMA), and dimethacrylates, bisphenol A-glycidyl
dimethacrylate – Bis-GMA, triethylene glycol dimethacrylate –
TEGDMA, and urethane dimethacrylate – UDMA (bis-acryl) (Astu­
dillo-Rubio et al., 2018; Yao et al., 2014). Such materials present
different compositions, fabrication methods, and polymerization tech­
niques, which impact their physical and mechanical properties as well as
clinical application (Alp et al., 2019; Astudillo-Rubio et al., 2018; Bal­
kenhol et al., 2008; KEβLER et al., 2021; Yao et al., 2014). The setting
reaction of PMMA systems is initiated chemically (self-curing), whereas
bis-acyl systems are available as self-curing or dual-curing systems
(chemical and light curing) (Balkenhol et al., 2008). PMMA is widely
used in dentistry due to its biocompatibility and satisfactory strength (σ
= 55–66 MPa) (Alp et al., 2019; Nejatidanesh et al., 2009), convenient
short term color stability, and simple use and repair by relining pro­
cedures (Yao et al., 2014). However, conventional PMMA consist of a
long-chain linear polymer, with scarce intermolecular crosslinking
(Anusavice et al., 2012; Yao et al., 2014). Such systems generate sig­
nificant heat due to exothermal reactions connected with polymeriza­
tion that might be associated with pulpal tissue damage and
polymerization shrinkage that deforms prosthesis’ contour, leading to
an inadequate marginal adaptation, and require additional clinical time
to relining (Angwarawong et al., 2020; Yao et al., 2014). Also, PMMA
provisionals crafted chairside usually contain more voids and unreacted
monomers and, consequently are highly susceptible to water sorption
that might influence their properties after a period in function (Ang­
warawong et al., 2020; Astudillo-Rubio et al., 2018).
Bis-acryl systems consist of functional monomers (Bis-GMA,
TEGDMA, and UDMA) that form a cross-linked polymer network as well
as inorganic fillers, potentially yielding improved strength (σ = 85–100
MPa) and toughness relative to conventional PMMA systems (Alp et al.,
2019; Astudillo-Rubio et al., 2018; Schwantz et al., 2017; Yao et al.,
2014). Bis-acryl systems are available with an automix delivery system
that simplifies the fabrication process and provides a consistent mixture
of base materials with decreased air incorporation, voids, and porosities,
improving the strength of temporary prostheses (Astudillo-Rubio et al.,
2018; Yao et al., 2014). In addition to a more cohesive polymer network,
bis-acryl systems present a low rise in temperature due to exothermic
polymerization, low polymerization shrinkage, good wear resistance,
improved polish ability and color stability (Alp et al., 2019; Astu­
dillo-Rubio et al., 2018). In contrast, such materials are more expensive
and less repairable (Singh and Garg, 2016).
Aside from chemical and structural modifications, a variety of indi­
rect manufacturing techniques are currently available to fabricate
polymeric temporary prostheses, which can also affect their physical
and mechanical properties (Alp et al., 2019; Angwarawong et al., 2020;
Hensel et al., 2021; KEβLER et al., 2021; Yao et al., 2014). The
2
Journal of the Mechanical Behavior of Biomedical Materials 133 (2022) 105333
availability of PMMA blocks/discs has gained interest in the prostho­
dontist community using computer-aided design/computer-aided
manufacturing (CAD/CAM) machinery to fabricate temporary prosthe­
ses (Alp et al., 2019; Angwarawong et al., 2020; Yao et al., 2014).
Temporary CAD/CAM polymeric systems are fabricated in an industrial
environment under controlled temperature, pressure and humidity,
which reduces bulk flaw population and improves mechanical strength
(s = 100–130 MPa for PMMA blocks) and precision (Alp et al., 2019;
Angwarawong et al., 2020; Yao et al., 2014). Likewise, they are pre­
polymerized at higher temperatures and for longer periods under
controlled conditions, increasing the degree of conversion and pre­
venting heat damage to oral tissues and restoration deformation due to
polymerization shrinkage (Alp et al., 2019; Angwarawong et al., 2020).
The more homogeneous structure of CAD/CAM PMMA systems may
overcome shortcomings of chairside handmade PMMA systems,
including excessive water sorption and residual monomer release,
increasing physical and mechanical properties stability (Yao et al.,
2014).
Along with CAD/CAM production, 3D-printing is currently available
to fabricate temporary prostheses (Kessler et al., 2020). Stereo­
lithography (SLA) and digital light processing (DLP) technology are the
two most common 3D-printing technologies used in dentistry for tem­
porary reconstructions, which are based on the principle that an object is
constructed by sequential thin layer deposition with the help of a
photopolymer resin (KEβLER et al., 2021; Kessler et al., 2020). While the
advantages of additive manufacturing include material savings, usually
lower costs of equipment and materials, production of complex geom­
etries, and possibility of combination of materials, the disadvantages lie
in the mechanical property anisotropy due to the layered fabrication and
low filler content of materials (KEβLER et al., 2021). Until the present
moment, 3D-printer technology including printing parameters, layer
thickness, postprocessing parameters, printing orientation, and slicing
of the object has shown to play a critical role on the physical and me­
chanical (s = 90–150 MPa) properties of the 3D-printed prosthesis, all
requiring extensive research (KEβLER et al., 2021; Osman et al., 2017;
Tahayeri et al., 2018).
The understanding of the mechanical properties of temporary ma­
terials is important in prosthodontics to select the appropriate system for
each clinical scenario; for instance, stronger materials should be selected
for long-span prostheses or extended treatment duration (Hensel et al.,
2021). Moreover, the oral environment have presented a detrimental
effect on temporary polymeric prostheses properties through softening
of polymer matrix, release of unreacted monomers, degradation of
products, and leaching of filler ions (Alp et al., 2019; Yao et al., 2014),
warranting extensive characterization. Therefore, this study evaluated
the effect of system composition, fabrication mode, and thermal cycling
on the mechanical properties of different polymeric systems used for
temporary dental prostheses. The postulated alternative hypotheses
were: (i) that composition and fabrication mode would affect the me­
chanical properties of polymeric systems used for temporary dental
prostheses and (ii) that thermal cycling would affect the mechanical
properties of polymeric systems used for temporary dental prostheses.
2. Materials and Methods
Six polymeric systems with different compositions and fabrication
modes were investigated: conventional PMMA GC (CGC) (Alike, GC
Corporation, Tokyo, Japan); conventional PMMA Dencôr (CD) (Dencôr,
Clássico, Campo Limpo Paulista, SP, Brazil); bis-acryl GC (BGC)
(Tempsmart, GC Corporation, Tokyo, Japan); bis-acryl Yller (BY) (Yller,
Pelotas, RS, Brazil); milled PMMA Ivoclar (MI) (TelioCAD, Ivoclar,
Schaan, Liechtenstein); 3D-printed PMMA Yller (PY) (Cosmos, Yller,
Pelotas, RS, Brazil) (Table 1).
Standard bar-shaped (25 × 2 × 2 mm) specimens were fabricated (n
= 10/group), following ISO 4049:2019 specifications. A metallic mold,
milled to comply with sample dimensions, was used for the fabrication
E.T.P. Bergamo et al. Journal of the Mechanical Behavior of Biomedical Materials 133 (2022) 105333

Table 1 model of a bar-shaped specimen was designed with the dimensions

Experimental groups description, according to the manufacturer information. required in the normative, exported as a stl. file, and used to either mill
GROUP Manufacturer Composition Fabrication samples from MI group (Ceramill motion 2, Amann Girbach, Curitiba,
Mode PR, Brazil) or 3D-print (Photon S, Anycubic, Shenzhen, China) speci­
CGC GC Coporation, Polymethyl methacrylate Conventional mens from PY group. 3D-printed specimens were fabricated in a hori­
Tokyo, Japan (PMMA) zontal position, with 50 μm layer thickness (Fig. 1).
CD Classico, Campo Polymethyl methacrylate Conventional All specimens were polished in an automatic polishing machine
Limpo Paulista, SP, (PMMA) (Automet 2000; Buehler, Lake Buff, IL) with 8-, 6-, 3- and 1-μm diamond
Brazil
BGC GC Coporation, Paste A: Urethane Automix
discs and diamond solutions under running water. After polishing, all
Tokyo, Japan Dimethacrylate (Bis-acryl) + System specimens were checked for their dimensions with a digital caliper and
Inorganic Silica Particles stored in a 37 ◦ C distilled water bath for 24 h prior to testing (Alp et al.,
Paste B: Urethane 2019).
Dimethacrylate (Bis-acryl) +
Photoinitiator + Inorganic
Silica Particles 2.1. Thermal cycling
BY Yller, Pelotas, RS, Paste A: Dimethacrylate (Bis- Automix
Brazil acryl) System
Half of the specimens were subjected to 5000 thermocycles in
Paste B: Dimethacrylate (Bis-
acryl) + Photoinitiator distilled water from 5 ◦ C to 55 ◦ C with a 30 s dwell time at each tem­
MI Ivoclar, Schaan, Polymethyl methacrylate Milled perature (Thermocycle, BioPDI, Red deer, AB, Canada) (Angwarawong
Liechtenstein (PMMA) et al., 2020). Such hydrothermal challenge was made in attempt to
PY Yller, Pelotas, RS, Dimethacrylate (Bis-acryl) + Printed simulate 6 months of use in the oral environment (Gale and Darvell,
Brazil Photoinitiator
1999).

of the specimens of conventional PMMA and automixed bis-acryl sys­
tems. The specimens of conventional PMMA systems (CGC and CD) were
fabricated by mixing the polymer and monomer according to the man­
ufacturers’ recommendations and pouring into the mold. The mold was
placed onto a transparent polyester film supported by a glass slab. After
pouring the material, a glass slide was placed on the top of the mold to
conform the desired bar dimensions. The specimens were maintained in
the mold for 15 min at room temperature prior to removal. The speci­
mens of bis-acryl systems were directly injected into the mold from the
cartridge using the automix dispenser system according to the manu­
facturers’ instructions, as previously described for the conventional
PMMA groups. The BGC group was photopolymerized for 5 s on each
surface (Valo, Ultradent, South Jordan, UT, USA), as recommended by
the manufacturer. Both bis-acryl groups were maintained in the mold for
15 min at room temperature and then removed from the mold. A CAD
2.2. Three-point bending test
Three-point bending flexural strength of the specimens was tested in
an all-electric dynamic test machine (ElectroPulsTM E3000, Instron,
Norwood, MA, UA) at a loading rate of 0.50 mm/min loading according
to ISO 4049:2019 requirements (Fig. 1). Specimens were placed on the
sample holder apparatus, which had a support span of 20 mm. The load
was applied at the center of the specimen by a 2-mm diameter rod. The
flexural strength (σ) was calculated (MPa) using the following formula:
σ = 3Fl/2bh2, where F is the maximum load at failure (N), l is the dis­
tance between support spans (mm), b is the width at the center of the
specimen (mm), and h is the height at the center of the specimen (mm).
Elastic modulus (E) was determined according to the following formula:
E = Fl3/4bh3γ, where F is the maximum load at failure (N), l is the
distance between support spans (mm), b is the width at the center of the

Fig. 1. Description of experimental groups (A). Specimens were fabricated manually using a metallic matrix (B1) or they were 3D-printed (B2) or milled (B3). All
specimens were polished and fabricated with similar dimensions (25 × 2 × 2 mm). Mechanical properties were evaluated by three-point bending testing following
ISO 4049:2019 requirements.

3
E.T.P. Bergamo et al.
specimen (mm), h is the height at the center of the specimen (mm), and γ
is the deflection at the end of the linear part of the force-deflection di­
agram (mm). Failed samples were first inspected using a polarized light
stereomicroscope (AxioZoom V16, Zeiss, Oberkochen, Germany) for
fractographic analysis.
2.3. Fourier transform infrared spectrometer (FTIR)
FTIR spectra of the polymeric systems before and after thermal
cycling were recorded on Frontier spectrometer (PerkinElmer Inc,
Waltham, MA, USA) equipped with a universal attenuated total reflec­
tion (UATR) accessory. Each spectrum was acquired in transmittance
mode by accumulation of 16 scans with a range of 4000–500 cm− 1.
Degree of conversion (%, C– – C) was determined before and after ther­
mal cycling. The percentage of unreacted C–– C bonds (%) was calculated
from the ratio of the absorbance peak area of aliphatic C– – C (cm− 1
wavelength) stretching vibrations against the aromatic C– C and C–
– –O
stretching vibrations (cm− 1 wavelength) in the uncured and cured
forms, as well as after thermal cycling. The DC was then calculated by
subtracting the percentage of the C–– C bonds from 100%, according to
the following formula: i) PMMA systems: DC (%) = 100*{1 – [(C– –C
aliphatic − 1637 cm− 1-/C–– O (1608 cm− 1) after)/(C–
– C aliphatic − 1637
cm− 1/C = 0 1608 cm− 1 before)]}; and i) Bis-acryl systems: DC (%) =
100*{1 – [(C– – C aliphatic − 1637 cm− 1-/C– – C aromatic (1730 cm− 1)
after)/(C– C aliphatic − 1637 cm /C– C aromatic 1730 cm− 1
– − 1 –
before)]}.
2.4. Scanning electron microscopy (SEM)
SEM was used to investigate the morphology of the polymeric sys­
tems before and after thermal cycling. Observation was performed and
micrographs from the surface were obtained with a scanning electron
microscope (VEGA3-TESCAN, Brno-Kohoutovice, Czech Republic).
Additionally, energy dispersive spectroscopy (EDS) was conducted to
analyze the elemental and chemical composition of the polymeric sys­
tems (INCA Energy EDS System, Oxford Instruments, Concord, MA, USA;
incorporated into the SEM).
2.5. Statistical analysis
Flexural strength, elastic modulus, and degree of conversion data
were tested for normal distribution using Shapiro-Wilk test. Descriptive
statistics including mean values and the corresponding 95% confidence
interval (CI) were calculated and data were compared using two-way
analysis of variance (fixed factors of group and aging) and Tukey tests.
Analyses were performed using SPSS with a significance level of 5%
(IBM SPSS 23, IBM Corporation, Armonk, NY, USA).
3. Results
Composition and fabrication mode significantly influenced the flex­
ural strength of the polymeric systems used for temporary prostheses (F
= 84/p < 0.001). Bis-acryl BGC system showed the highest flexural
strength (80 MPa) (p < 0.037), followed by the milled PMMA group, MI
(71 MPa) (p < 0.037). Conventional PMMA CGC (50 MPa) and CD (49
MPa) as well as 3D-printed PY (52 MPa) groups presented intermediate
values, with no significant difference between the groups (p > 0.544).
Bis-acryl BY showed the lowest flexural strength 27 (MPa) (p < 0.001).
Thermocycling significantly increased the flexural strength of all poly­
meric systems used for temporary prostheses (p < 0.047), except for PY
group (p = 0.717). After thermal cycling, bis-acryl BGC and milled
PMMA systems exhibited the highest flexural strength (89 MPa an 86
MPa, respectively) (p < 0.001). Conventional PMMA CGC (64 MPa) and
CD (57 MPa) systems presented intermediate values, followed by the PY
system (51 MPa), with significant difference between CGC and PY
groups (p = 0.005). Bis-acryl BY showed the lowest flexural strength (40
4
Journal of the Mechanical Behavior of Biomedical Materials 133 (2022) 105333
MPa) (p < 0.010) (Table 2).
Stereomicroscope images of representative fractured specimens are
shown in Figs. 2–4. The micrographs reveal rounded areas, voids/de­
fects, as the area of the fracture origin. Such flaws were more commonly
observed in the handmade PMMA samples (Fig. 2) compared to the bis-
acryl samples (Fig. 3) and indirect PMMA (Fig. 4) which can be asso­
ciated with difficulties of chairside handmade fabrication, including
mixing of monomer and powder and voids incorporation. Regarding
failure mode, groups with a highly structured network and high quantity
of inorganic fillers (especially BGC system) seemed to present a brittle
fracture, in which many of the fractographic marks were similar to those
observed in failed ceramic’s specimens subjected to flexure tests (i.e.
compression curl and hackle lines) (Quinn and Quinn, 2010). In the
monomethacrylates and dimethacrylates presenting limited inorganic
content, however, substantial plastic deformation was observed by the
plasticizing effect.
Composition and fabrication mode significantly influenced the
elastic modulus of the polymeric systems used for temporary prostheses
(F = 52/p < 0.001). Bis-acryl BGC (1.89 GPa) and conventional PMMA
CGC (1.66 GPa) groups showed the highest elastic modulus, followed by
milled PMMA group (1.51 GPa) and conventional PMMA CD (1.45 GPa)
systems, with significant difference between BGC group and MI and CD
groups (p < 0.015). The printed PY (0.78 GPa) and bis-acryl BY (0.47
GPa) systems showed the lowest elastic modulus (p < 0.001). Thermo­
cycling demonstrated no significant influence on the elastic modulus of
the polymeric systems used for temporary prostheses (p > 0.047).
Therefore, bis-acryl BGC (1.91 GPa) and conventional PMMA CGC (1.71
GPa) groups showed the highest elastic modulus after thermal cycling,
followed by milled PMMA MI group (1.49 GPa) and conventional PMMA
CD (1.31 GPa) systems, with significant difference between BGC group
and MI and CD groups (p < 0.009) as well as CGC and CD groups (p =
0.018). The PMMA 3D-printed PY (0.73 GPa) and bis-acryl BY (0.47
GPa) systems showed the lowest elastic modulus (p < 0.001) (Table 3).
The Fourier-transformed infrared spectrometer (FTIR) spectra of the
polymeric systems used for temporary prostheses indicated that con­
ventional CGC and CD and milled MI samples exhibited similar spectra,
where the bands correspond to PMMA spectra (Fig. 5) (Gengenbach and
Griesser, 1998; Ramesh et al., 2007). The bands in the wavelengths 1730
and 1438 cm− 1 correspond to stretching vibrations of the aliphatic ester
C–– O and deformation vibrations C–H bonds, corresponding to CH3
groups, respectively (Gengenbach and Griesser, 1998). The bands
located at 2900 cm− 1 correspond to the asymmetrical and symmetrical
stretching of the C–H bond (Ramesh et al., 2007). The large and poorly
defined band between 3200 and 3650 cm− 1 represents hydrogen
bonding that indicates the presence of OH groups in the polymer. The
band located at approximately 1485 cm− 1 is also related to the asym­
metrical deformation of the C–H bond, while the bands around 1157,
1190, and 1062 cm− 1 are related to the stretching vibrations of the C–O
bond of the ester group. The bands at 1271 and 1241 cm− 1 correspond to
C–H rocking vibrations (type wag). The bands at 988, 965, 910 and 841
cm− 1 refer to the balance vibrations (type wag) of the C–H bonds
Table 2
Flexural strength (MPa) with the corresponding 95% confidence interval of the
interim polymeric systems before and after thermal cycling.
GROUP FLEXURAL STRENGTH (MPa)
Immediate Aged
CGC 50 (5.8) aC 64 (6.5) bB
CD 49 (5.8) aC 57 (5.8) bBC
BGC 80 (5.8) aA 89 (5.8) bA
BY 27 (5.8) aD 40 (5.8) bD
MI 71 (5.8) aB 86 (5.8) bA
PY 52 (5.8) aC 51 (5.8) aC
*Different lowercase letter indicate statistically significant difference between
aging condition; Different uppercase letters indicate statistically significant
difference between materials.
E.T.P. Bergamo et al. Journal of the Mechanical Behavior of Biomedical Materials 133 (2022) 105333

Fig. 2. Stereomicroscope images of representative fractured specimens of the PMMA polymeric systems after three point bending testing. Asterisk indicates main
defects, arrows show the direction of crack propagation, and pointers depict voids related to direct handmade manufacturing.

Fig. 3. Stereomicroscope images of representative fractured specimens of the bis-acryl polymeric systems after three point bending testing. Asterisk indicates main
defects, arrows show the direction of crack propagation, letters exhibit main fractographic marks (CC, compression curl, and H, hackle lines), and pointers depict
voids/defects related to direct manufacturing.

(Ramesh et al., 2007). A band at 750 cm− 1, which is related to the vi­
brations of the long hydrocarbon chains, can be also observed in the
spectra (Gengenbach and Griesser, 1998).
The FTIR spectra of BGC, BY and PY samples correspond to dime­
thacrylate systems, bis-acryl. This system is composed of several
monomers: methyl methacrylate, which is the main component of
PMMA, as well as bisphenol A-glycidyl dimethacrylate (Bis-GMA), tri­
ethylene glycol dimethacrylate (TEGDMA), and urethane dimethacry­
late (UDMA) (Delgado and Young, 2021). These monomers, even with
different structures, are composed of bonds very similar to PMMA sys­
tems, presenting a set of bands in the FTIR that are very similar. The
main differences in the FTIR spectra are the bands corresponding to the
aromatic ring from Bis-GMA at 1600 cm− 1, corresponding to the double
bond present in the aromatic ring, and deformation of N–H at 3500 -
3070 cm − 1 present in UDMA (Delgado and Young, 2021).
Table 4 shows the degree of conversion (DC) values of the polymeric
systems used for temporary prostheses. Material type and thermal
cycling significantly influenced the degree of conversion of the poly­
meric systems used for temporary prostheses (F = 9.7/p = 0.014). For
immediate samples, conventional PMMA CGC (74.5%), bis-acryl BGC
(72.5%), and 3D-printed PY (66.5%) exhibited the highest percentage of
conversion, without significant difference between them (66.5%) (p >
0.249). Conventional PMMA CD (54.0%) and bis-acryl BY (49.5%)
showed the lowest DC, significantly different from conventional PMMA
CGC and bis-acryl BGC systems (p < 0.030). For aged samples, bis-acryl
BY group (56.0%) presented significantly lower DC relative to others (p
< 0.009). DC significantly increased for CD group before and after
thermal cycling (p = 0.003), with approximately 12% increase in the DC.
Although no significant difference was detected for CGG, BCG, BY, and
PY systems before and after thermal cycling (p > 0.082), all groups
presented at least 5% increase in the DC after thermal cycling. Pre­
polymerized CAD/CAM group showed no significant difference on the

5
E.T.P. Bergamo et al. Journal of the Mechanical Behavior of Biomedical Materials 133 (2022) 105333

Fig. 4. Stereomicroscope images of representative fractured specimens of the bis-acryl polymeric systems after three point bending testing. Asterisk indicates main
defects, arrows show the direction of crack propagation, letters exhibit main fractographic marks (CC, compression curl), and pointers depict voids/defects related to
manufacturing.

first postulated alternative hypothesis that composition and fabrication

Table 3
mode would affect the mechanical properties of polymeric systems used
Elastic modulus (GPa) with the corresponding 95% confidence interval of the
for temporary dental prostheses was accepted. Thermal cycling
interim polymeric systems before and after thermal cycling.
increased the flexural strength of all polymeric systems used for tem­
GROUP ELASTIC MODULUS (GPa)
porary prosthesis, except for the 3D-printed PY group. Thermal cycling
Immediate Aged exerted no significant influence on the elastic modulus. Hence, the
CGC 1.66 (0.22) aAB 1.71 (0.24) aAB second postulated alternative hypothesis that thermal cycling would
CD 1.45 (0.22) aB 1.31 (0.22) aC affect the mechanical properties of polymeric systems used for tempo­
BCG 1.89 (0.22) aA 1.91 (0.22) aA rary dental prostheses was also accepted.
BY 0.47 (0.22) aC 0.47 (0.22) aD
In the current study, conventional handmade PMMA systems, CGC
MI 1.51 (0.22) aB 1.49 (0.22) aBC
PY 0.78 (0.22) aC 0.73 (0.22) aD and CD, exhibited no significant difference regarding the flexural
strength (s = ~50 MPa) and elastic modulus (E = ~1.5 GPa). Previous
*Different lowercase letter indicates statistically significant difference between
studies evaluating the mechanical properties of conventional handmade
aging condition; Different uppercase letters indicate statistically significant
PMMA systems have exhibited a similar range of values (σ = 55–66
difference between materials.
MPa), which can be associated with their similar composition and
fabrication mode (Alp et al., 2019; Nejatidanesh et al., 2009). In
initial and thermal cycled samples’ spectra.
contrast, bis-acryl systems showed statistically significant difference
Scanning electron microscope images of representative specimens of
either in the flexural strength (σ = ~50 MPa difference) or in the elastic
the temporary polymeric systems before and after thermal cycling are
modulus (E = 1.42 GPa difference), with BGC group outperforming BY
shown in Figs. 6 and 7. Bis-acryl BGC and milled PMMA systems pre­
group. Given that both systems present similar monomers (chiefly MMA,
sented a smoother and more homogeneous surface relative to others,
TEGDMA, Bis-GMA, and UDMA) and inorganic particles (silica), the
while a higher presence of defects could be observed for conventional
rationale for such a difference may lie in the amount and size of the
handmade PMMA and 3D-printed PY systems. No differences in
inorganic content as well as polymerization method (Balkenhol et al.,
morphology were recognizable before and after thermal cycling. Results
2008; Schwantz et al., 2017; Yao et al., 2014). Bis-acryl BGC system
of the energy dispersive spectroscopy (EDS) analysis suggest that the
presents a higher content of micro and nanometric inorganic silica
inorganic phase of the temporary polymeric systems is composed by
particles (mentioned by the manufacturer and confirmed in the EDS
silica (Fig. 6).
analysis) along with a dual curing mode, which might increase the de­
gree of conversion and improve the strength of the system (Balkenhol
4. Discussion
et al., 2008; Ghavami-Lahiji et al., 2018). The bis-acryl BGC system also
demonstrated statistically significant higher flexural strength (σ = ~30
This study evaluated the effect of system composition, fabrication
MPa difference) and elastic modulus (E = 0.23–045 GPa difference)
mode, and thermal cycling on the mechanical properties of different
relative to both conventionally handmade PMMA systems, CGD and CD.
polymeric systems used for temporary dental prostheses, especially of
Parallel with the results presented in the current study, bis-acryl systems
recently developed nanostructured bis-acryl systems and 3D-printed and
have also shown more favorable mechanical properties when compared
CAD/CAM milled systems. The results indicated that the composition
to conventional PMMA systems (σ = ~20–40 MPa difference) (Alp et al.,
and fabrication mode significantly affected the mechanical properties of
2019; Nejatidanesh et al., 2009). The composition of bis-acryl systems,
the systems, with bis-acryl (dimethacrylates) BGC (Tempsmart, GC
dimethacrylates, supports their improved mechanical performance since
Corporation) and bis-acryl BY (Yller) systems presenting the highest and
they exhibit a rigid crosslinked network due to the presence of multi­
lowest flexural strength and elastic modulus, respectively. Milled PMMA
functional monomers as well as inorganic particles and dual polymeri­
(polymethyl methacrylate) MI (TelioCAD, Ivoclar) system exhibited
zation, as above mentioned (Astudillo-Rubio et al., 2018; Balkenhol
intermediate values of flexural strength, followed by conventional
et al., 2008; Nejatidanesh et al., 2009; Schwantz et al., 2017; Yao et al.,
PMMA CGC (Alike, GC Corporation) and CD (Dencôr, Clássico) as well as
2014). In contrast, handmade PMMA systems, monomethacrylates, are
3D-printed PY (Cosmos, Yller) groups. Similarly, conventional PMMA
composed of a monofunctional, low molecular weight and linear struc­
CGC and CD as well as milled PMMA group presented intermediate
ture, with low content or absence of inorganic particles, leading to lower
values of elastic modulus, followed by 3D-printed PY group. Thus, the

6
E.T.P. Bergamo et al. Journal of the Mechanical Behavior of Biomedical Materials 133 (2022) 105333

Fig. 5. FTIR spectra of the interim polymeric systems before and after thermal cycling.

et al., 2019; Yao et al., 2014). Despite improvements in the CAD/CAM

Table 4 PMMA structure, the flexural strength (σ = 9 MPa difference) and elastic
Degree of conversion with the corresponding 95% confidence interval of the
modulus (E = 0.38 GPa difference) was lower when compared to the
interim polymeric systems before and after thermal cycling.
bis-acryl BGC system, which may also lie in the highly cross-linked
GROUP DEGREE OF CONVERSION (%) polymer and reinforcement with inorganic particles of the latter (Alp
Immediate Aged et al., 2019; Astudillo-Rubio et al., 2018; Schwantz et al., 2017).
CGC 74.5 (11) aA 80 (7) aA 3D-printed PY system presented intermediate values of flexural
CD 54.0 (11) aBC 71.5 (7) bA strength (52 MPa), which was similar to conventional handmade PMMA
BCG 72.5 (11) aA 78.5 (7) aA and lower than milled PMMA (σ = 19 MPa difference) and bis-acryl BGC
BY 49.5 (11) aC 56.0 (7) aB (σ = 28 MPa difference). Also, a lower elastic modulus was observed for
PY 66.5 (11) aAB 73.5 (7) aA
3D-printed PY system relative to other systems (E = ~1.5 GPa differ­
*There was no alteration in the spectra of the MI group. *Different lowercase ence), except for bis-acryl BY system since both systems present similar
letter indicate statistically significant difference between aging condition; composition. Previous studies have exhibited a high range in the me­
Different uppercase letters indicate statistically significant difference between chanical properties of 3D-printed polymeric systems (σ = 90–150 MPa;
materials.
E = 2–5 GPa), which was associated with differences in the material’s
composition and printing parameters (KEβLER et al., 2021; Osman et al.,
rigidity and mechanical properties (Astudillo-Rubio et al., 2018; Bal­ 2017). Despite the advantages of 3D-printing concerning material sav­
kenhol et al., 2008; Nejatidanesh et al., 2009; Yao et al., 2014). ings, independence of the milling instrument, ability to produce com­
Compared to conventional handmade PMMA, CAD/CAM fabricated plex geometries, and combination of materials, the anisotropy of
specimens presented 20-MPa increase in the flexural strength (σ = 71 physical properties due to layer-by-layer fabrication as well as the low
MPa), with no significant difference on the elastic modulus (E = ~1.5 filler content (herein confirmed in the EDS analysis) to obtain a
GPa). Previous studies have also exhibited higher flexural strength for low-viscosity polymer and optimize the 3D printing process might have
CAD/CAM PMMA systems relative to conventional handmade PMMA affected the mechanical properties of the system evaluated (KEβLER
systems (at least 30 MPa increase) (Alp et al., 2019). Aside from the et al., 2021; Ligon et al., 2014). Printers current used in dentistry to
benefits of the industrial fabrication on the reduction of defect popula­ fabricate temporary prostheses, stereolithography (SLA) and digital
tion, resulting in a more homogeneous structure, CAD/CAM PMMA light processing (DLP) printers, require low-viscosity polymeric systems
systems are prepolymerized under optimized conditions of temperature, to provide a good coating of the liquid monomer in the vat on the
humidity, and pressure (Alp et al., 2019; Angwarawong et al., 2020). polymerized layer on the building platform, avoiding penetration of air
Such a processing method provides adequate time for and inclusion of voids (KEβLER et al., 2021; Ligon et al., 2014). In
post-polymerization processes and relaxation phenomena within the high-viscosity systems, gravity and surface tension has shown to favor
polymer network, toughening effect (Alt et al., 2011; Astudillo-Rubio void inclusion as well as incomplete polymerization, affecting surface
et al., 2018), improving the properties of CAD/CAM polymeric systems smoothness and prosthesis’ accuracy (KEβLER et al., 2021; Ligon et al.,
and making them a promising option for temporary prostheses (Alp 2014). Moreover, printing direction and layer thickness can influence

7
E.T.P. Bergamo et al. Journal of the Mechanical Behavior of Biomedical Materials 133 (2022) 105333

Fig. 6. Scanning electron microscope of the surface of interim polymeric systems using secondary electron mode at magnifications of 500x and 10,000x before
thermal cycling. Results of the energy-dispersive spectroscopy analyses (within boxes).

Fig. 7. Scanning electron microscope of the surface of interim polymeric systems using secondary electron mode at magnifications of 500x and 10,000x after
thermal cycling.

the degree of anisotropy, where, until the present moment, horizontal
parallel direction, as the samples fabricated in the current study, have
demonstrated an improved mechanical performance since each printed
layer acts as an impediment to fracture (interfacial shear loads are
shown to easily separate interlayers, originating fracture) (KEβLER
et al., 2021). Layer thickness has shown a larger impact on the flexural
strength of the object than the printing direction, where the risk of either
printing errors or voids inclusion can be reduced by printing with a
100-μm layer size instead of 50-μm, as set in the current study (KEβLER
et al., 2021; Tahayeri et al., 2018; Vaezi and Chua, 2011). Future studies
should investigate different printers, printing and postprocessing pa­
rameters, as well as printing orientation and slicing of the object to
optimize physical and mechanical properties of the prosthesis according
to force distribution of each unit.
Water uptake into the network is a characteristic of polymers, which
might affect the surface properties and increase interaction with
microorganisms as well as plasticize the polymer matrix, altering the
mechanical properties (Buergers et al., 2007). In the current study,
thermal cycling for 5.000 cycles from 5 ◦ C to 55 ◦ C, which would
simulate 6 months of intra-oral use (Gale and Darvell, 1999), signifi­
cantly increased the flexural strength of all polymeric systems used for
temporary prosthesis (s = ~10–15 MPa increase), but the 3D printed PY
group, while no significant influence was observed on the elastic
modulus. In previous studies, different results have been reported
regarding the effect of thermal cycling on the flexural strength of sys­
tems used for temporary reconstructions, which was also associated with
the lack of standardization on aging methods and protocols (Alp et al.,
2019; Angwarawong et al., 2020; Astudillo-Rubio et al., 2018; Yao et al.,
2014). In a similar protocol, Yao et al. (2014), reported a significant
reduction in the flexural strength of bis-acryl (σ = ~10–20 MPa
reduction) and milled PMMA (σ = ~20–30 MPa reduction) systems (Yao
et al., 2014). Similarly, in a more aggressive thermal cycling protocol,

8
E.T.P. Bergamo et al.
10.000 cycles, previous literature findings have also demonstrated a
detrimental effect on the flexural strength of conventional and milled
PMMA, bis-acryl, and 3D-printed (σ = ~10–20 MPa reduction) poly­
meric systems used for temporary prostheses (Alp et al., 2019; KEβLER
et al., 2021). In fact, the effect of hydrothermal aging on the physical
properties of polymers has shown to be influenced by the composition,
processing parameters, fabrication mode, and aging protocol (Alp et al.,
2019; Astudillo-Rubio et al., 2018; Ferracane et al., 1998; KEβLER et al.,
2021). At initial stages, the effect of water sorption in monomer hy­
drolysis is low or nonexistent, allowing the material a certain degree of
plastic deformation before breaking, known as ductile behavior; how­
ever, at later stages, water sorption might progressively degrade the
mechanical properties of polymers due to softening of the matrix (water
molecules penetrate the spaces between polymer chains and separate
them; and, by acting as a plasticizer, the polymer chains become more
mobile and weaken) and release of monomers and degradation products
(Alp et al., 2019; Astudillo-Rubio et al., 2018; Yao et al., 2014). FTIR
spectra support the assumption that mechanical properties change in the
current study after thermal cycling might be an effect of an initial pro­
cess of water sorption through a conformational change in the relative
intensities of the CH bands at around 2900 cm− 1. Also, almost all sys­
tems showed an increase in the relative intensity of the bands at
approximately 3400 cm− 1 over the CH bands (as shown in the magni­
fication next to the full spectrum), which is an indicative of water uptake
by the polymer (Sales et al., 2011). However, for the 3D printed PY
system, there was a reduction in the relative intensity of the band at
3400 cm− 1 compared to 2900 cm− 1, which may be associated with the
release of residual monomer (UDMA) since the N–H band is present in
this region, overlapping the OH band (NOMOTO and HIRASAWA,
1999). Such fact might explain the absence of significant difference in
the flexural strength only for this system, where monomer release
counterbalanced for the initial beneficial effect of water sorption.
Another factor that might have affected the mechanical properties of
the polymeric temporary composites is the higher degree of conversion
after thermal cycling (5–12% increase) for all polymeric systems, except
for the PMMA MI system that is prepolymerized under an industrial
environment. Previous studies have demonstrated similar findings after
thermal cycling polymeric systems, with approximately 7%-increase in
the degree of conversion in a similar aging method and protocol to the
adopted in the current study (Ghavami-Lahiji et al., 2018; Schwantz
et al., 2017). The higher the degree of conversion, the better the me­
chanical properties and the lower the susceptibility to water sorption
and monomer release (Balkenhol et al., 2008; Schwantz et al., 2017).
Theoretically, the minimum degree of conversion to guarantee the
clinical success of a tooth restoration is approximately 50%, percentage
reached for all polymeric systems investigated in the current study
(Barszczewska-Rybarek et al., 2020). The increase in the degree of
conversion after hydrothermal aging might be the result of either
increased temperature or swelling by diffusion reaction that can in­
crease the molecular mobility in the system, enabling entrapped
unreacted monomers, pendant carbon double bonds, and photoinitiators
to continue the polymerization process (Ghavami-Lahiji et al., 2018;
Leprince et al., 2010, 2013). Despite different compositions and fabri­
cation and polymerization modes, the increase rate in the degree of
conversion was similar for most of the temporary polymeric systems
evaluated, requiring further analysis regarding the effect of thermal
cycling on the degree of conversion using longer periods of aging.
Although the outcomes of this study cannot be directly extrapolated
to clinical practice, the present findings indicate a promising generation
of polymeric systems with improvements in the composition and fabri­
cation mode that might increase the reliability of short- and long-term
temporary reconstructions. However, there is no temporary polymeric
system that meets the optimal requirements for all clinical situations,
and clinicians’ choice should be based on each clinical scenario and
intended application. Moreover, flexural strength is an important tool to
evaluate the mechanical properties of restorative systems under
9
Journal of the Mechanical Behavior of Biomedical Materials 133 (2022) 105333
controlled conditions; however, the test does not adequately simulate
the oral environment (Alp et al., 2019; Karaokutan et al., 2015; KEβLER
et al., 2021; Yao et al., 2014). Storage medium, temperature, and
anatomic geometry might also influence the clinical performance of
such systems (Calheiros et al., 2013). Therefore, fatigue testing and
clinical trials are required to provide more realistic information
regarding their performance.
5. Conclusion
Composition and fabrication mode significantly affected the me­
chanical properties of polymeric systems used for temporary dental
prostheses, where the bis-acryl system with a potential higher content of
micro and nanostructured inorganic particles and milled PMMA system
mostly outperformed the conventional PMMA and printed systems.
Thermal cycling increased the flexural strength of all polymeric systems
used for temporary dental prostheses, except the 3D-printed system.
CRediT authorship contribution statement
Edmara T.P. Bergamo: Writing – original draft, Methodology,
Investigation, Formal analysis, Data curation, Conceptualization. Tiago
M.B. Campos: Writing – original draft, Methodology, Investigation,
Formal analysis, Data curation. Mariana M.T. Piza: Methodology,
Investigation, Formal analysis, Data curation. Eliezer Gutierrez:
Methodology, Investigation, Formal analysis, Data curation. Adolfo C.
O. Lopes: Methodology, Investigation, Formal analysis, Data curation.
Lukasz Witek: Writing – review & editing, Validation, Methodology,
Investigation, Formal analysis, Conceptualization. Paulo G. Coelho:
Writing – review & editing, Validation, Supervision, Formal analysis,
Data curation, Conceptualization. Marcos Celestrino: Software, Re­
sources, Methodology, Investigation. Laura F.de Carvalho: Methodol­
ogy, Investigation, Formal analysis, Data curation. Ernesto B.
Benalcázar Jalkh: Methodology, Investigation, Formal analysis, Data
curation. Estevam A. Bonfante: Writing – review & editing, Validation,
Supervision, Resources, Project administration, Funding acquisition,
Formal analysis, Data curation, Conceptualization.
Declaration of competing interest
The authors declare that they have no known competing financial
interests or personal relationships that could have appeared to influence
the work reported in this paper.
Data availability
Data will be made available on request.
Acknowledgements
To Fundação de Amparo a Pesquisa do Estado de São Paulo (FAPESP)
Young Investigators Award Grant Part II 2021/06730–7, EMU 2016/
18818–8, FAPESP 2019/08693-1 and BEPE 2021/08018–2, 2019/
14798–0, 2020/12874–9, 2020/16500–6, 2022/07157-1 and to Con­
selho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)
Grant # 307255/2021-2, and Capes Finance Code 001.
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