polymers

Article
Impact of CAD/CAM Material Thickness and Translucency on
the Polymerization of Dual-Cure Resin Cement in Endocrowns
Soshi Ikemoto 1,2 , Yuya Komagata 1 , Shinji Yoshii 3 , Chihiro Masaki 2 , Ryuji Hosokawa 2 and Hiroshi Ikeda 1, *

1 Division of Biomaterials, Kyushu Dental University, Kitakyushu 803-8580, Japan;

r19ikemoto@fa.kyu-dent.ac.jp (S.I.); pty_pty_kjm@yahoo.co.jp (Y.K.)
2 Division of Oral Reconstruction and Rehabilitation, Kyushu Dental University, Kitakyushu 803-8580, Japan;
masaki@kyu-dent.ac.jp (C.M.)
3 Division of Promoting Learning Design Education, Kyushu Dental University, Kitakyushu 803-8580, Japan
* Correspondence: r16ikeda@fa.kyu-dent.ac.jp

Abstract: The objective of this study is to evaluate the impact of the thickness and translucency
of various computer-aided design/computer-aided manufacturing (CAD/CAM) materials on the
polymerization of dual-cure resin cement in endocrown restorations. Three commercially available
CAD/CAM materials—lithium disilicate glass (e.max CAD), resin composite (CERASMART), and a
polymer-infiltrated ceramic network (ENAMIC)—were cut into plates with five different thicknesses
(1.5, 3.5, 5.5, 7.5, and 9.5 mm) in both high-translucency (HT) and low-translucency (LT) grades.
Panavia V5, a commercial dual-cure resin cement, was polymerized through each plate by light
irradiation. Post-polymerization treatment was performed by aging at 37 ◦ C for 24 h under light-
shielding conditions. The degree of conversion and Vickers hardness measurements were used to
characterize the polymerization of the cement. The findings revealed a significant decrease in both the
degree of conversion and Vickers hardness with increasing thickness across all CAD/CAM materials.
Notably, while the differences in the degree of conversion and Vickers hardness between the HT and
LT grades of each material were significant immediately after photoirradiation, these differences
became smaller after post-polymerization treatment. Significant differences were observed between
samples with a 1.5 mm thickness (conventional crowns) and those with a 5.5 mm or greater thickness
Citation: Ikemoto, S.; Komagata, Y.;
(endocrowns), even after post-polymerization treatment. These results suggest that dual-cure resin
Yoshii, S.; Masaki, C.; Hosokawa, R.;
Ikeda, H. Impact of CAD/CAM
cement in endocrown restorations undergoes insufficient polymerization.
Material Thickness and Translucency
on the Polymerization of Dual-Cure Keywords: dental materials; luting agent; endocrown; CAD/CAM; ceramic; polymer-infiltrated
Resin Cement in Endocrowns. ceramic network; resin composite; polymerization
Polymers 2024, 16, 661. https://
doi.org/10.3390/polym16050661

Academic Editor: Daniel

1. Introduction
Torres-Lagares
An endocrown is a specialized dental restoration primarily utilized in dentistry for
Received: 23 January 2024 teeth that have experienced substantial damage, typically due to decay, following root
Revised: 18 February 2024
canal treatment [1]. Unlike conventional crowns that envelope the entire visible portion of
Accepted: 27 February 2024
a tooth, endocrowns are custom-designed for molars and premolars, offering a modern and
Published: 29 February 2024
less-invasive alternative in restorative dentistry [2]. Endocrowns are inserted into the pulp
chamber previously occupied by the pulp of the removed tooth and cover the occlusal sur-
face of the tooth [3]. Unlike conventional crowns that often require additional dental posts,
Copyright: © 2024 by the authors.
endocrowns bond directly to the tooth cavity, resulting in minimal removal of the natural
Licensee MDPI, Basel, Switzerland. tooth structure. A primary benefit of this conservative approach to restoration is that it
This article is an open access article dispenses with the need for extensive tooth reshaping, often required for conventional
distributed under the terms and crown fitting, thereby conserving more of the natural tooth structure than conventional
conditions of the Creative Commons crowns [4]. The conservation of tooth is advantageous for the long-term health and struc-
Attribution (CC BY) license (https:// tural integrity of the tooth. Additionally, the procedure for placing an endocrown tends to
creativecommons.org/licenses/by/ be simpler and more expedient than that for placing a conventional crown [5]. Endocrowns
4.0/). exhibit excellent mechanical strength and durability, particularly those fabricated from

Polymers 2024, 16, 661. https://doi.org/10.3390/polym16050661 https://www.mdpi.com/journal/polymers

Polymers 2024, 16, 661 2 of 12

advanced ceramic materials and resin composites [6], which makes them notably effective
in restoring the function and aesthetics of damaged molars and premolars.
The history of endocrowns as a dentistry concept is relatively recent compared to that
of other dental restorations, such as fillings or conventional crowns. Their development
and popularity are closely linked to the advancements in dental materials and adhesive
technologies [6,7]. The late 20th century saw notable progress in adhesive dentistry, en-
abling more conservative restorations that effectively bonded to tooth structures [8]. During
the period of emergence, this concept was not initially defined as the endocrown. The
term “endocrown” and its unique approach gained prominence in the 1990s, aided by the
introduction of high-strength ceramic materials and improved adhesive techniques [9]. The
“monoblock technique”, proposed by Pissis in 1995 [10], was a precursor to endocrown
restoration. A significant milestone was a 1999 publication in which Bindle and Mör-
mann [11] introduced the “endocrown” as a monolithic ceramic restoration, made from
computer-aided design/computer-aided manufacturing (CAD/CAM) ceramic, for post-
root canal treatment. In the 2000–2010s [1,12,13], the use of endocrowns expanded, sup-
ported by further enhancements in luting agents, ceramic materials, and CAD/CAM
technology, leading to more precise and aesthetically pleasing restorations. Recently,
endocrowns have become the favored choice for restoring endodontically treated teeth,
particularly in cases of substantial tooth structure loss [3].
The clinical outcomes of endocrowns, as reported by various studies, have generally
been positive, demonstrating their efficacy as a restorative option for endodontically treated
teeth. Many studies have reported high survival rates for endocrowns, often comparable
to conventional crowns, typically exceeding 90% over five years [14]. The clinical failure
of an endocrown, particularly debonding, is an important consideration in restorative
dentistry [14,15]. Factors contributing to the debonding failure of endocrowns include
tooth design and preparation. If the endocrown fits poorly or errors occur during tooth
preparation (e.g., undercuts or insufficient decay removal), then it can result in weak bond-
ing and failure. The success of endocrowns also relies heavily on the correct application
of adhesive techniques. The inappropriate use of luting agents, improper etching, or con-
tamination of the bonding surface (such as by saliva or blood) during the procedure can
compromise the bond strength. In addition, luting agents play a crucial role in bonding
endocrowns to the remaining tooth structure [16,17]. Among the luting agents, resin-based
cements are considered the optimal choice for endocrowns due to their superior bonding
strength and durability [18]. Dual-cure resin cements, in particular, are favored for their
versatility and reliable performance, making them highly suitable for bonding endocrowns.
Their broad acceptance among dentists stems from their ability to cure through both light
and chemical means, accommodating a variety of clinical scenarios. However, the poly-
merization behavior of dual-cure resin cements in endocrown restorations remains to be
fully understood. Given the increased thickness of endocrowns compared to conventional
crowns, the penetration of light into the dual-cure resin cement poses a challenge, leading
to concerns regarding the efficiency of photopolymerization.
Several in vitro studies have explored the polymerization behavior of light-cure and
dual-cure resin cements, as well as restorative resin composites, in endocrown restora-
tions. Gregor et al. assessed the degree of polymerization of a light-cure restorative resin
composite and dual-cure resin cement under 7.5 mm-thick endocrowns made from resin
composite or ceramic using Vickers hardness measurements. Their findings indicated that
the Vickers hardness values of both the dual-cure resin cement and the light-cure resin
composite, when irradiated for 3 × 90 s at high irradiance, reached at least 80% of the
control values [19]. Daher et al. evaluated the minimal irradiation time required to achieve
sufficient polymerization of a light-cure restorative resin composite under 9.5 mm-thick
endocrowns [20]. The study concluded that 40 s light curing per site (buccal, palatal,
and occlusal) achieved a hardness of up to 80% of the positive control sample, indicating
adequate polymerization. Kuijper et al. investigated the effects of ceramic translucency
and restoration type (onlays and endocrowns) on the polymerization efficiency of dual-
Polymers 2024, 16, 661 3 of 12

cure resin cement and a restorative resin composite using a high-power light device [21].
Their results demonstrated that material translucency influenced the polymerization of the
resin composite under endocrowns, while the polymerization of the resin cement was not
significantly affected by either translucency or restoration type.
While previous studies offer valuable insights into the use of dual-cure resin cements
for bonding endocrowns, questions persist regarding the impacts of material type, thickness,
and translucency on dual-cure resin cement polymerization. Therefore, this study aims to
elucidate the impact of the thickness and translucency of aesthetic CAD/CAM materials on
dual-cure resin cement polymerization. The first null hypothesis posits that the thickness
of CAD/CAM materials does not affect dual-cure resin cement polymerization, while
the second null hypothesis suggests that material translucency has no impact on the
polymerization process. The materials chosen for endocrown fabrication include lithium
disilicate glass, polymer-infiltrated ceramics, and resin composites. Both high-translucency
(HT) and low-translucency (LT) grades of each material were selected to evaluate their
respective influences on the polymerization process.

2. Materials and Methods

2.1. Materials
Table 1 lists CAD/CAM materials. This study used three types of commercially avail-
able aesthetic CAD/CAM materials: lithium disilicate glass (e.max CAD), resin composite
(CERASMART), and polymer-infiltrated ceramic network (ENAMIC). Both HT and LT
grades were used for each material, which makes a total of six types of CAD/CAM materi-
als. Each CAD/CAM material block was cut into plates of different thicknesses (1.5, 3.5, 5.5,
7.5, and 9.5 mm) using a diamond wheel saw (MINICUT 40, SCAN-DIA GmbH & CO. KG,
Hagen, Germany) under water cooling. The surface of each plate was polished using emery
papers in the order of #400, #800, and #1500. To ensure that the specified thickness was
within ±0.1 mm, the resultant plate thickness was measured using a digital vernier caliper
(Mitutoyo CD-15CPX, Mitutoyo Corp., Kawasaki, Japan). The polished plates were then
cleaned via ultrasonication in distilled water for 5 min to eliminate debris. The resultant
plates were used for the polymerization experiment of the dual-cure resin cement. Figure 1
illustrates the CAD/CAM material plates, showcasing variations in thickness along with
the HT and LT grades.
Polymers 2024, 16, x FOR PEER REVIEW Panavia V5 (Kuraray Noritake Dental, Inc., Tokyo, Japan) was used as the dual-cure
4 of 13

resin cement.

Figure 1.1. Photograph

Figure Photograph of of CAD/CAM
CAD/CAMmaterial
materialplates showcasing
plates varying
showcasing thicknesses
varying withwith
thicknesses high-high-
translucency (HT) and low-translucency (LT) grades. Illumination from beneath the samples high-
translucency (HT) and low-translucency (LT) grades. Illumination from beneath the samples high-
lights the distinctions in thickness and translucency between the grades of each material.
lights the distinctions in thickness and translucency between the grades of each material.
2.2. Photopolymerization of Dual-Cure Resin Cement and Post-Polymerization Treatment by
Aging
Photopolymerization of the dual-cure resin cement was conducted by light irradia-
tion through a CAD/CAM material plate, as depicted in Figure 2. In the experimental
Polymers 2024, 16, 661 4 of 12

Table 1. CAD/CAM material blocks used in this study. The material composition is based on the
information published by the manufacturer.

Material Type Product Name Product Company Composition

Ivoclar Vivadent, Schaan, SiO2 , Li2 O, K2 O, P2 O5 , ZrO2 , ZnO, Al2 O3 , MgO,
Lithium disilicate glass IPS e.max CAD
Liechtenstein Coloring oxide
SiO2 , Barium glass, urethane dimethacrylate, 2,2-
Resin composite CERASMART300 GC Corp., Tokyo, Japan
bis(4-methacryloxypolyethoxyphenyl)propane
Figure 1. Photograph of CAD/CAM material plates showcasing varying thicknesses with high-
Polymer-infiltrated translucency VITA Zahnfabrik, SiO2 , Al2 O3 , Polymer, Na2 O, Kthe
2 O,samples
B2 O3 , ZrO2,
VITA ENAMIC(HT) and low-translucency (LT) grades. Illumination from beneath high-
ceramic network lights the distinctions Nabertherm, Germany
in thickness and translucency between the grades CaOof each material.

2.2.
2.2.Photopolymerization
PhotopolymerizationofofDual-Cure
Dual-CureResin
ResinCement
Cementand
andPost-Polymerization
Post-PolymerizationTreatment
Treatmentby
Aging
by Aging
Photopolymerization
Photopolymerizationofofthe thedual-cure
dual-cure resin cement
cement waswas conducted
conductedby bylight
lightirradiation
irradia-
through
tion through a CAD/CAM
a CAD/CAM material
materialplate, as depicted
plate, as depictedin Figure 2. In2.the
in Figure Inexperimental
the experimental setup,
the dual-cure
setup, the dual-cureresinresin
cement waswas
cement placed
placedbetween
between twotwo 2525µm µmpolyester
polyesterfilms
films(Lumirror
(Lumir-
film
ror filmT60,
T60, Toray
Toray Industries,
Industries, Inc., Tokyo,
Inc., Tokyo, Japan)
Japan) that served
that served asasthe top
the topandandbase
baselayers.
layers.To
Toensure
ensure a standardized
a standardized thickness
thickness of of
thethe
dual-cure
dual-cure resin
resincement,
cement, a 1amm-thick
1 mm-thick spacer was
spacer
positioned adjacent to the resin cement. This assembly was placed
was positioned adjacent to the resin cement. This assembly was placed on a glass plate on a glass plate and
a CAD/CAM material plate was mounted on the sandwiched
and a CAD/CAM material plate was mounted on the sandwiched cement. Light irradia- cement. Light irradiation
waswas
tion performed
performed using
usinga handheld
a handheld light-curing
light-curing unit (VALO
unit (VALO GRAND;
GRAND; Ultradent
Ultradent Products
Prod-
Inc.,Inc.,
ucts South Jordan,
South UT, UT,
Jordan, USA) placed
USA) in direct
placed contact
in direct withwith
contact the CAD/CAM
the CAD/CAM material plate.
material
Continuous lightlight
irradiation waswasperformed for for
90 s90
atsaattemperature of 25 ◦
plate. Continuous irradiation performed a temperature of 25C,°C,
using the
using
light-curing unit in high-power-plus mode (1600 w/cm 2 ). The dual-cure resin cement
the light-curing unit in high-power-plus mode (1600 w/cm ). The dual-cure resin cement
2

wasthen
was thenimmediately
immediatelyevaluated
evaluatedpost-irradiation,
post-irradiation,with withthis
thiscondition
conditiondesignated
designatedasasthe the
“Immediate group”. Subsequently, the photopolymerized dual-cure
“Immediate group”. Subsequently, the photopolymerized dual-cure resin cement was resin cement was aged
in aninincubator
aged an incubatorat 37 ◦at
C for 24 hfor
37 °C under
24 hlight
undershielding, referred toreferred
light shielding, as the “Aging
to as thegroup”. The
“Aging
resulting dual-cure resin cements were characterized based on
group”. The resulting dual-cure resin cements were characterized based on their degreetheir degree of conversion
ofand Vickers hardness
conversion and Vickers in subsequent
hardness inexperiments.
subsequent experiments.

Light curing unit

CAD/CAM material plate

(1.5, 3.5, 5.5, 7.5, or 9.5 mm) Alminium foil

Spacer
Polyester films
Dual-cure resin cement

Glass plate

Figure 2.2.
Figure Schematic view
Schematic ofof
view experimental setup
experimental forfor
setup photopolymerization ofof
photopolymerization dual-cure resin
dual-cure cement
resin cement
through CAD/CAM material plate.
through CAD/CAM material plate.

2.3. Fourier Transform Infrared (FTIR) Spectroscopy

The polymerization of the dual-cure resin cements for each experimental group was
characterized by degree of conversion, which was estimated using FTIR spectroscopy. FTIR
measurements were performed using an FTIR spectrometer (IRSpirit; Shimadzu Corp.,
Kyoto, Japan) equipped with an attenuated total reflectance unit (QATR-S; Shimadzu Corp.).
In the FTIR spectra, two characteristic bands at 1638 cm−1 (C=C stretch vibration) and
1720 cm−1 (C=O stretch vibration) before and after polymerization of the dual-cure resin
cement were used to calculate the degree of conversion using the following equation [22,23]:
!
[ A(C = C )/A(C = O)]be f ore polymerization
Degree o f conversion (%) = 1 − × 100 (1)
[ A(C = C )/A(C = O)] a f ter polymerization
 madzu Corp.). In the FTIR spectra, two characteristic bands at 1638 cm (C=C stretch vi-
bration) and 1720 cm−1 (C=O stretch vibration) before and after polymerization of the dual-
cure resin cement were used to calculate the degree of conversion using the following
equation [22,23]:
Polymers 2024, 16, 661 𝐴(𝐶 = 𝐶)/𝐴(𝐶 = 𝑂) 5 of 12
𝐷𝑒𝑔𝑟𝑒𝑒 𝑜𝑓 𝑐𝑜𝑛𝑣𝑒𝑟𝑠𝑖𝑜𝑛 (%) = 1 − × 100 (1)
𝐴(𝐶 = 𝐶)/𝐴(𝐶 = 𝑂)
where A(C=C)
where A(C=C)and A(C=O)
and A(C=O)areare
thethe
absorbance
absorbance values. Five
values. samples
Five sampleswere used
were to measure
used to measure
thethe
degree of conversion in each group (n = 5). Figure 3 illustrates an example
degree of conversion in each group (n = 5). Figure 3 illustrates an example of the FTIR
of the
spectra
FTIR for the dual-cure
spectra resin cements,
for the dual-cure illustrating
resin cements, the changes
illustrating the before and
changes after and
before photo-
after
polymerization.
photopolymerization.

0.3

Before polymerization
C=O
After polymerization

0.2
Absorbance

0.1

C=C

0
1720 1670 1620
Wavenumber (cm−1)
Figure 3. Typical FTIR spectra of the dual-cure resin cements before and after polymerization.
Figure 3. Typical FTIR spectra of the dual-cure resin cements before and after polymerization.
2.4. Microhardness Test
2.4. Microhardness Test
After the FTIR measurements, the samples were subjected to Vickers microhardness
After
tests the FTIR measurements,
to determine the mechanical the samples
properties ofwere subjected
the cement to Vickers
in each microhardness
experimental group. For
tests to determine the mechanical properties of the cement in each
each group, a microhardness test was performed using a Vickers hardness tester experimental group.
(HMV-
ForG21ST,
each group,
Shimadzu a microhardness
Corp., Kyoto, test waswith
Japan) performed
a load ofusing
50–200 a Vickers hardness
g and a dwell timetester
of 15 s.
(HMV-G21ST,
Five samplesShimadzu
were usedCorp., Kyoto,the
to measure Japan) withhardness
Vickers a load offor 50–200
each g and a(ndwell
group = 5). time of
15 s. Five samples were used to measure the Vickers hardness for each group (n = 5).
2.5. Statistical Analysis
2.5. Statistical Analysisdata were analyzed using a statistical software program (EZR version
The obtained
1.62,
TheSaitama
obtained Medical
data wereCenter, Jichi Medical
analyzed University,
using a statistical Saitama,
software Japan),(EZR
program withversion
one-way
variance
1.62, Saitama (ANOVA)
Medical followed by Tukey’s
Center, Jichi Medicalpost-hoc test,Saitama,
University, to compare statistical
Japan), differences
with one-way
between
variance the groups.
(ANOVA) Statistical
followed significance
by Tukey’s post-hocwas settotocompare
test, (p) < 0.05 for all analyses.
statistical differences The
independent samples Student’s t-test was used to compare the values
between the groups. Statistical significance was set (p) < 0.05 for all analyses. The inde-of the immediate
and aged
pendent samples
samples for eacht-test
Student’s group.
was used to compare the values of the immediate and
aged samples for each group.
3. Results
3.1. Degree of Conversion
Figure 4 shows the degree of conversion of dual-cure resin cement in the immediate
group. In the case of lithium disilicate glass (Figure 4a), the degree of conversion decreased
with increasing material thickness. For thicknesses of 1.5, 7.5, and 9.5 mm, the degree
of conversion in the HT group was statistically higher than that in the LT group. For
the resin composite (Figure 4b), a similar trend of decreasing degree of conversion with
increasing plate thickness was observed. There were statistically significant differences
between the degree of conversion for the HT and LT groups at plate thicknesses of 5.5,
7.5, and 9.5 mm. For the polymer-infiltrated ceramic network (Figure 4c), the degree of
conversion also diminished with increasing plate thickness. When comparing the HT and
LT groups, no significant differences were found in the degree of conversion across various
plate thicknesses.
 and LT groups,
For the no significant
resin composite (Figuredifferences weretrend
4b), a similar foundofindecreasing
the degreedegree
of conversion across
of conversion
various plate thicknesses.
with increasing plate thickness was observed. There were statistically significant differ-
encesFigure
between5 shows the degree
the degree of conversion
of conversion for theofHTtheand
dual-cure resin
LT groups at cement in the aging
plate thicknesses of
groups. Across
5.5, 7.5, and 9.5 all
mm. CAD/CAM materials, the degree
For the polymer-infiltrated of conversion
ceramic decreased
network (Figure 4c),as the
the plate
degree
Polymers 2024, 16, 661 thickness increased.
of conversion In this instance,
also diminished no statistical
with increasing platedifference
thickness.was
Whenobserved between
comparing the
6 of
the HT12
HT and LT groups across plate thicknesses for each CAD/CAM material.
and LT groups, no significant differences were found in the degree of conversion across
various plate thicknesses.
Figure 5 shows the degree of conversion of the dual-cure resin cement in the aging
groups. Across all CAD/CAM materials, the degree of conversion decreased as the plate
thickness increased. In this instance, no statistical difference was observed between the
HT and LT groups across plate thicknesses for each CAD/CAM material.

Figure 4. Mean and standard deviation for degree of conversion (%) for the dual-cure resin cements
in immediategroups,
in immediate groups,photopolymerized
photopolymerized through
through different
different thicknesses
thicknesses of CAD/CAM
of CAD/CAM materialmaterial
plates;
plates;
(a) (a) lithium
lithium disilicate
disilicate glass,
glass, (b) (b)composite,
resin resin composite,
and (c)and (c) polymer-infiltrated
polymer-infiltrated ceramic
ceramic networknetwork
with
with high-translucency (HT) and low-translucency (LT) grades. The samples that did not cure at all
high-translucency (HT) and low-translucency (LT) grades. The samples that did not cure at all
are indicated with “×” symbols. Different uppercase and lowercase letters represent statistically sig-
are indicated with “×” symbols. Different uppercase and lowercase letters represent statistically
nificant differences among different plate thicknesses within HT or LT groups, respectively. An as-
significant
Figure
terisk differences
4. Mean
indicates and amongsignificant
standard
a statistically different for
deviation plate thicknesses
degree
difference of within
conversion
between the HT HTand
(%) or LT
for LTgroups,
the groups respectively.
dual-cure resinthe
within An
cements
same
asterisk
in indicates
immediate
plate a statistically significant difference between the HT and
thickness.groups, photopolymerized through different thicknesses of CAD/CAM material LT groups within the same
plates;thickness.
plate (a) lithium disilicate glass, (b) resin composite, and (c) polymer-infiltrated ceramic network
(a) with high-translucency
(b) (HT) and low-translucency (LT) grades. (c) The samples that did not cure at all
100 Figure 5with
are indicated shows
100 “×” the degree
symbols. of conversion
Different uppercase of
andthe dual-cure
lowercase
100 resin
letters cement
represent in the aging
statistically sig-
groups.
nificant
HT
Across
differences all CAD/CAM
among different materials,
plate the degree
thicknesses
HT
withinof conversion
HT or LT decreased
groups, as the
respectively. plate
An
HT
as-
thickness increased. In this instance, no statistical difference was observed between the HT
Degree of conversion (%)

Degree of conversion (%)

Degree of conversion (%)

80 teriskLT
indicates a
80statistically
A significant differenceLT
between the
80 HT and LT groups within the same
LT
A a a a
AB plate
and LT groups across plateathicknesses for each CAD/CAMA material.
thickness. ab
60 ab 60 AB B 60 B
ab B B
BC bc
CD
(a) D (b) b
(c) C CDbc c
40 bc 40 b 40
100 100 100 D
c
b
HT HT HT
20 20 20
Degree of conversion (%)

Degree of conversion (%)

Degree of conversion (%)

80 80 A 80
A a LT a LT LT
AB A a
0 0 a 0 ab
60 ab 60 AB B 60 B
1.5 mm 3.5 mm 5.5 B mm
ab BCmm 7.5 mm 9.5 mm 1.5 mm 3.5 mm 5.5 7.5 mm 9.5
B mm 1.5 mm 3.5 mm 5.5 mm
bc 7.5 mm 9.5 mm
CD D
b
C CDbc c
40 bc
Figurec5. Mean and40 b
standard deviation for degree 40 (%) for the dual-cure resin cements
of conversion D
b
in aging groups, photopolymerized through different thicknesses of CAD/CAM material plates; (a)
20 20
lithium disilicate20glass, (b) resin composite, and (c) polymer-infiltrated ceramic network with high-
translucency and low-translucency grades. Different uppercase and lowercase letters represent
0 0 0
1.5 mm 3.5 mm 5.5 mm 7.5 mm 9.5 mm 1.5 mm 3.5 mm 5.5 mm 7.5 mm 9.5 mm 1.5 mm 3.5 mm 5.5 mm 7.5 mm 9.5 mm

Figure 5.5. Mean

Meanandandstandard
standarddeviation
deviation forfor
degree of conversion
degree (%) for
of conversion (%)the
fordual-cure resin resin
the dual-cure cements
ce-
in aging
ments ingroups, photopolymerized
aging groups, throughthrough
photopolymerized differentdifferent
thicknesses of CAD/CAM
thicknesses material plates;
of CAD/CAM (a)
material
lithium(a)
plates; disilicate
lithiumglass, (b) resin
disilicate glass,composite, and (c) polymer-infiltrated
(b) resin composite, ceramic network
and (c) polymer-infiltrated ceramicwith high-
network
translucency and low-translucency grades. Different uppercase and lowercase letters represent
with high-translucency and low-translucency grades. Different uppercase and lowercase letters
represent statistically significant differences among different plate thicknesses within HT or LT
groups, respectively.

3.2. Vickers Hardness

Figure 6 shows the Vickers hardness of the dual-cure resin cements in the immediate
group. For the lithium disilicate glass (Figure 6a), the Vickers hardness decreased with
increasing plate thickness. At thicknesses of 5.5 and 7.5 mm, the Vickers hardness could
not be measured as the dual-cure resin cement was too soft, falling below the lower
measurement limit. At a 9.5 mm thickness in the LT group, the dual-cure resin cement
could not be cured at all. In the case of the resin composite (Figure 6b), a similar trend
was observed with a decrease in the Vickers hardness as the plate thickness increased.
For thicknesses of 5.5, 7.5, and 9.5 mm, Vickers hardness measurements were not possible
because of the excessive softness of the dual-cure resin cement. For the polymer-infiltrated
ceramic network (Figure 6c), the Vickers hardness decreased with increasing plate thickness.
 could not be measured because the dual-cure resin cement was not sufficiently cured to
allow measurement.
Figure 7 shows the Vickers hardness of the dual-cure resin cements in the aging
groups. Across all CAD/CAM materials, a decrease in the Vickers hardness was observed
Polymers 2024, 16, 661 with increasing cement thickness. Unlike the immediate groups, all aging samples 7were of 12
sufficiently cured, allowing their Vickers hardness to be measured. Statistical differences
were observed between the HT and LT groups for the 1.5 and 3.5 mm thicknesses for the
lithium to
Similar disilicate glass;
the resin for the 3.5,
composite, the5.5, and 7.5
Vickers mm thicknesses
hardness for the resinofcomposite;
for the thicknesses for
5.5, 7.5, and
the 3.5, 5.5, and 9.5 mm thicknesses for the polymer-infiltrated ceramic network,
9.5 mm could not be measured because the dual-cure resin cement was not sufficiently respec-
tively.to allow measurement.
cured

Figure 6. Mean
Meanand andstandard
standarddeviation
deviationforfor
Vickers
Vickers hardness
hardness forfor
thethe
dual-cure resin
dual-cure cements
resin in im-
cements in
mediate groups,
immediate groups,photopolymerized
photopolymerized through
throughdifferent
differentthicknesses
thicknessesof of
CAD/CAM
CAD/CAM material plates;
material (a)
plates;
lithium
(a) disilicate
lithium glass,
disilicate (b)(b)
glass, resin composite,
resin composite,andand(c)(c)polymer-infiltrated
polymer-infiltratedceramic
ceramicnetwork
networkwith
with high-
high-
translucency (HT) and low-translucency (LT) grades. In the figures, the cement samples that were
translucency (HT) and low-translucency (LT) grades. In the figures, the cement samples that were
cured but remained too soft for Vickers hardness measurement are denoted with “△” symbols. The
cured but remained too soft for Vickers hardness measurement are denoted with “△” symbols. The
samples that did not cure at all are indicated with “×” symbols. Different uppercase and lowercase
samples that did statistically
letters represent not cure at all are indicated
significant with “×
differences ” symbols.
among Different
different plate uppercase
thicknessesand lowercase
within HT or
letters represent statistically significant differences among different plate thicknesses
LT groups, respectively. An asterisk indicates a statistically significant difference between within HTtheorHT
LT
groups, respectively.
and LT groups withinAntheasterisk indicates
same plate a statistically significant difference between the HT and LT
thickness.
groups within the same plate thickness.

Figure 7 shows the Vickers hardness of the dual-cure resin cements in the aging groups.
Across all CAD/CAM materials, a decrease in the Vickers hardness was observed with
increasing cement thickness. Unlike the immediate groups, all aging samples were suffi-
ciently cured, allowing their Vickers hardness to be measured. Statistical differences were
observed between the HT and LT groups for the 1.5 and 3.5 mm thicknesses for the lithium
Polymers 2024, 16, x FOR PEER REVIEW 8 of 13
disilicate glass; for the 3.5, 5.5, and 7.5 mm thicknesses for the resin composite; for the 3.5,
5.5, and 9.5 mm thicknesses for the polymer-infiltrated ceramic network, respectively.

Figure 7.
Figure 7. Mean
Mean and
andstandard
standarddeviation for Vickers
deviation hardness
for Vickers for thefor
hardness dual-cure resin cements
the dual-cure in aging
resin cements
groups,
in aging photopolymerized through different
groups, photopolymerized through thicknesses of CAD/CAM
different thicknesses material plates;
of CAD/CAM (a) lithium
material plates;
disilicate
(a) lithiumglass, (b) resin
disilicate composite,
glass, (b) resin and (c) polymer-infiltrated
composite, ceramic network
and (c) polymer-infiltrated withnetwork
ceramic high-translu-
with
cency (HT) and low-translucency (LT) grades. Different uppercase and lowercase letters represent
high-translucency (HT) and low-translucency (LT) grades. Different uppercase and lowercase let-
statistically significant differences among different plate thicknesses within HT or LT groups, re-
ters represent statistically significant differences among different plate thicknesses within HT or LT
spectively. An asterisk indicates a statistically significant difference between the HT and LT groups
groups, respectively.
within the same plateAn asterisk indicates a statistically significant difference between the HT and LT
thickness.
groups within the same plate thickness.
4. Discussion
The objective of this study was to elucidate the effects of the CAD/CAM material
thickness and translucency grade (high- or low-translucency) on the polymerization pro-
cess of dual-cure resin cement. The polymerization of dual-cure resin cements, both im-
mediately after light irradiation and after aging for 24 h in addition to light irradiation,
was characterized by the degree of conversion and Vickers hardness. The findings re-
vealed that both the degree of conversion and Vickers hardness decreased as the thickness
Polymers 2024, 16, 661 8 of 12

4. Discussion
The objective of this study was to elucidate the effects of the CAD/CAM material
thickness and translucency grade (high- or low-translucency) on the polymerization process
of dual-cure resin cement. The polymerization of dual-cure resin cements, both immedi-
ately after light irradiation and after aging for 24 h in addition to light irradiation, was
characterized by the degree of conversion and Vickers hardness. The findings revealed that
both the degree of conversion and Vickers hardness decreased as the thickness increased
for all the examined CAD/CAM materials, namely, lithium disilicate glass, resin composite,
and polymer-infiltrated ceramic networks. Consequently, the first null hypothesis, which
posited that the thickness of the CAD/CAM materials does not influence the polymeriza-
tion of the dual-cure resin cement, is rejected. Moreover, the results demonstrated that the
translucency grade of each CAD/CAM material affected both the degree of conversion
and Vickers hardness in the immediate groups, whereas it had no effect on the degree of
conversion and little effect on the Vickers hardness in the aging groups. Therefore, the
second null hypothesis, which stated that the translucency grades of CAD/CAM materials
do not affect the polymerization of dual-cure resin cement, is partially rejected.
In this study, two methods were employed to characterize the polymerization behavior
of dual-cure resin cement: degree of conversion and Vickers hardness. The results, as
estimated by both degree of conversion and Vickers hardness, exhibited a consistent trend:
an increase in the material thickness led to a decrease in both the Vickers hardness and
degree of conversion. These methods effectively verified the polymerization behavior of
dual-cure resin cement. Previous studies on the polymerization of resin-based materials
have shown that polymerization behavior can be similarly estimated using the degree
of conversion and/or hardness measurements [24–26]. The degree of conversion can be
determined using FTIR spectroscopy [27] and Raman spectroscopy [28,29]. Several methods
exist for measuring the hardness of resin-based materials, including the Vickers [30,31],
Knoop [24,29], and Martens hardnesses [32,33]. However, it is important to note that
hardness measurements may not always be feasible, particularly if the dual-cure resin
cement is too soft. In some instances, the dual-cure resin cement appeared to have solidified;
however, its hardness could not be measured. In contrast, the degree of conversion was
obtainable for such samples. Therefore, it is advisable to use both the hardness and degree of
conversion assessments, rather than evaluating only one, to corroborate each set of results.
For endocrown restorations, CAD/CAM materials are favored because of their durabil-
ity, aesthetic qualities, and adhesive bonding abilities [1,34,35]. Ceramics are the preferred
materials for endocrowns, with clinical reports citing the use of lithium disilicate glass [4],
zirconia [36], leucite-reinforced ceramic [37], and feldspar porcelain [38]. Among these,
lithium disilicate glass is often considered the most suitable for endocrowns because of
its excellent bonding ability and mechanical durability [34]. In addition to ceramics, resin
composites are utilized for endocrown fabrication [39]. Their lower brittleness compared
to traditional ceramics makes them a viable choice for endocrowns, particularly in pa-
tients with bruxism or in those requiring restoration to withstand heavier occlusal forces.
Polymer-infiltrated ceramic networks represent a unique category of hybrid materials that
combine the advantages of ceramics and polymers. This material has mechanical properties
that are highly compatible with human teeth [40]. Owing to their balanced mechanical
and physicochemical properties, polymer-infiltrated ceramic networks are increasingly
being recognized as a suitable choice for endocrown applications [41]. These CAD/CAM
materials for endocrowns are available in HT and LT grades and offer different levels of
optical translucency to achieve aesthetically pleasing tooth restorations. Previous studies
have investigated the impact of ceramic translucency on the polymerization of resin-based
cements by the light irradiation of ceramic [21,42,43]. Kuijper et al. [21] examined the influ-
ence of lithium disilicate translucency at thicknesses of 4.0 mm and 7.5 mm on the degree
of conversion of dual-cure resin cement. Their findings suggested that the translucency
grade of the lithium disilicate glass did not affect the degree of conversion. Similarly, Chen
et al. [42] explored the effect of lithium disilicate glass translucency on the polymerization
Polymers 2024, 16, 661 9 of 12

of dual-cure resin cement through 1 mm- and 2 mm-thick samples, finding no signifi-
cant effect on the microhardness or degree of conversion. In line with these findings, the
present study revealed that differences in the translucency of all the examined CAD/CAM
materials affected the polymerization of the dual-cure resin cement immediately after
light irradiation, with little or no influence on polymerization after aging. Based on the
results of these studies, the translucency grade of the material has little influence on the
polymerization of dual-cure resin cement in endocrown restorations.
The experimental results of this study demonstrate that the polymerization of dual-
cure resin cement diminishes with increasing material thickness. These findings are partic-
ularly relevant when comparing endocrowns with conventional crowns. For conventional
crowns, a material thickness of 1–2 mm is typical [44,45]. In contrast, endocrowns are
characterized by greater thicknesses, generally exceeding 4.0 mm [46–49]. This is due to the
large combined thickness of the crown (at least 2.0 mm) and pulp chamber extension (over
2 mm), with the overall thickness exceeding 4.0 mm for endocrowns. In this study, distinct
differences were observed in the degree of conversion and Vickers hardness between the
groups with 1.5 mm thickness (conventional crowns) and those with 5.5 mm or greater
thickness (endocrown).
Dual-cure resin cement is an adhesive widely used in various dental restorative
procedures. The term “dual-cure” reflects its dual mechanism of hardening or setting:
through light curing and self-curing. Light curing of the cement occurs immediately
upon exposure to light irradiation, whereas self-curing occurs gradually when the two
components of the cement are mixed. This dual mechanism is particularly beneficial in
areas where light cannot adequately penetrate. Given the substantial thickness of the
endocrowns, light penetration into the cement is often limited, thereby diminishing the
efficacy of light curing. In such scenarios, the self-curing property of dual-cure resin cement
becomes crucial. The findings of this study reveal a notable observation: the degree of
polymerization and Vickers hardness were significantly higher in samples with HT grade
compared to those with LT grade in the initial group. However, this difference diminished
in the aging group, highlighting the crucial influence of the self-curing properties of the
dual-cure resin cement. This phenomenon underscores the adaptability of dual-cure resin
cements in dental restorations, especially for applications involving substantial material
thickness or complex geometries that hinder light accessibility. The self-curing mechanism
ensures a dependable setting process throughout the material, compensating for areas not
reached by light. It emphasizes the importance of considering both curing methods when
assessing the performance and long-term stability of dental restorations.
Our experiments revealed that cement polymerization was insufficient with light irra-
diation alone. Meanwhile, post-polymerization occurred over time, leading to an increase
in both the degree of conversion and Vickers hardness. Despite post-polymerization involv-
ing aging, the degree of conversion and Vickers hardness for a material thickness of 5.5 mm
were not as high as those observed for a thickness of 1.5 mm. Consequently, the polymer-
ization of dual-cure resin cement in endocrowns is less efficient than that in conventional
crowns, even after considering the post-polymerization effects of self-curing. This result
suggests that the polymerization of dual-cure resin cement in endocrown restorations may
be inferior to that in conventional crown restorations. Consequently, when using dual-cure
resin cement to bond endocrowns to abutment teeth, there is a potential risk of insufficient
polymerization of the dual-cure resin cement, which could lead to clinical failures such as
debonding or fracture. Clinical reports on endocrowns have indicated a higher incidence
of debonding failures, particularly in cases where dual-cure or light-cure resin cements are
used as adhesives [11,50]. The choice of Panavia V5 as the dual-cure resin cement for this
study leverages its well-documented success in bonding CAD/CAM materials [51], making
it a representative candidate for examining the effectiveness of dual-cure resin cements in
such applications. Nevertheless, it is crucial to acknowledge the diversity of polymerization
behaviors among the various dual-cure resin cements available commercially [52]. This
Polymers 2024, 16, 661 10 of 12

variability suggests that the performance of endocrown bonding could be significantly

influenced by the distinct properties inherent to each brand of resin cement.
Although informative, this study has several limitations and does not entirely replicate
the clinical application of endocrowns. One significant limitation was the use of material in
plate form, which failed to accurately mimic the complex tooth shape typical of endocrowns.
Additionally, the specific orientation of the light irradiation through the endocrown to the
dual-cure resin cement was not considered in this experimental setup. The intensity and
duration of light irradiation are known to significantly influence cement polymerization.
In our experiment, we employed a relatively high irradiation intensity and extended the
irradiation time to ensure effective curing of the cement. However, the dependence of
polymerization on the irradiation intensity and duration warrants further investigation. In
addition, this study did not utilize human teeth, opting instead for a simplified experimental
approach. To bridge the gap between experimental settings and clinical practice, future
studies should include experiments that consider these critical factors. This includes both
in vitro and in vivo studies designed to closely align with the complexities and variables
encountered in dental treatments.

5. Conclusions
This study aimed to elucidate the polymerization behavior of dual-cure resin cement
in endocrowns by examining the degree of conversion and Vickers hardness after curing
with varying thicknesses of CAD/CAM materials (lithium disilicate glass, resin composite,
and polymer-infiltrated ceramic network), in both high- and low-translucency grades.
Considering the limitations of this study, the following conclusions were drawn.
• Polymerization of the dual-cure resin cement decreased with increasing CAD/CAM
material thickness, suggesting that thicker materials impeded the curing process.
• Significant differences in polymerization were observed between samples with a
1.5 mm thickness (conventional crowns) and those with a thickness of 5.5 mm or
greater (endocrowns).
• The translucency grades influenced the polymerization of the dual-cure resin cement
immediately after light irradiation. However, these differences were either eliminated
or substantially reduced after post-polymerization treatment by aging.
These findings suggest that when dual-cure resin cements are employed in endocrowns,
the degree of polymerization and Vickers hardness may be insufficient compared with conven-
tional crowns, irrespective of the translucency grade and thickness of the CAD/CAM material.

Author Contributions: Conceptualization, H.I. and Y.K.; data curation, S.I. and Y.K.; formal analysis,
C.M.; funding acquisition, S.Y., C.M. and H.I.; investigation, S.I., Y.K. and S.Y.; methodology, Y.K.
and H.I.; project administration, R.H. and H.I.; resources, H.I.; supervision, H.I.; validation, R.H.;
visualization, S.I. and C.M.; writing—original draft, S.I., Y.K., S.Y. and C.M.; writing—review and
editing, R.H. and H.I. All authors have read and agreed to the published version of the manuscript.
Funding: This research was funded by JSPS KAKENHI (grant number 23K09236).
Institutional Review Board Statement: Not applicable.
Data Availability Statement: Data are contained within article.
Conflicts of Interest: The authors declare no conflict of interest.

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