Additive Effects of Touchactivated Polymerization and
Additive Effects of Touchactivated Polymerization and
Additive Effects of Touchactivated Polymerization and
Supported by the Ministry of Education, Culture, Sports, Science and Technology of Japan (Grant Numbers 17K17125, 18K09571 and 19K10106) and by the Cooperation
Program between TMDU and Sony IP&S, Inc scholarship to W.S.D.
a
Graduate student, Department of Cariology and Operative Dentistry, Graduate School of Medical and Dental Sciences, Tokyo Medical and Dental University, Tokyo, Japan;
and Lecturer, Department of Conservative Dentistry, Faculty of Dentistry, Hasanuddin University, Makassar, South Sulawesi, Indonesia.
b
Graduate student, Department of Cariology and Operative Dentistry, Graduate School of Medical and Dental Sciences, Tokyo Medical and Dental University, Tokyo, Japan;
and Lecturer, Biomaterials Department, Faculty of Oral and Dental Medicine, Modern University for Technology and Information, Mokatam, Cairo, Egypt.
c
Graduate student, Department of Cariology and Operative Dentistry, Graduate School of Medical and Dental Sciences, Tokyo Medical and Dental University, Tokyo, Japan;
and Graduate student, Institute of Dental Medicine, First Faculty of Medicine of the Charles University and General University Hospital in Prague, Prague, Czech Republic.
d
Clinical Fellow, Operative Dentistry Clinic, Tokyo Medical and Dental University Dental Hospital, Tokyo, Japan.
e
Senior Lecturer, Department of Oral Prosthetic Engineering, Graduate School of Medical and Dental Sciences, Tokyo Medical and Dental University, Tokyo, Japan.
f
Assistant Professor, Department of Cariology and Operative Dentistry, Graduate School of Medical and Dental Sciences, Tokyo Medical and Dental University, Tokyo, Japan.
g
Professor, Department of Cariology and Operative Dentistry, Graduate School of Medical and Dental Sciences, Tokyo Medical and Dental University, Tokyo, Japan.
h
Junior Associate Professor, Department of Cariology and Operative Dentistry, Graduate School of Medical and Dental Sciences, Tokyo Medical and Dental University, Tokyo,
Japan.
10-MDP, 10-Methacryloyloxydecyl dihydrogen phosphate; BHT, Butylated hydroxytoluene; Bis-GMA, Bisphenol A-glycidyl methacrylate; CQ, Camphorquinone; DCA, Clearfil DC Activator;
EBPADMA, Ethoxylated bisphenol A dimethacrylate; HEMA, Hydroxyethylmethacrylate; PBU, Prime&Bond Universal; PENTA, Dipentaerythritol penta-acrylate phosphate; s, seconds; SCA, Self
Cure Activator; SEB, Clearfil SE Bond 2; TEGDMA, Triethylene glycol dimethacrylate; UBQ, Universal Bond Quick ER; UDMA, Urethane dimethacrylate.
and PBU+SCA; and Clearfil DC Core Automix ONE Each beam was then subjected to a tensile force at a
(Kuraray Noritake Dental Inc) for SEB, SEB+DCA, crosshead speed of 1 mm/min until fracture on a table-
and UBQ, followed by light-irradiation for 60 seconds. top testing machine (EZ-SX; Shimadzu Co), and the
The bonding procedures are illustrated in Figure 1. force at bond failure was converted to mTBS value in
After being stored in water at 37 C for 24 hours, each MPa. The mTBS testing procedure is summarized in
bonded specimen was sectioned mesiodistally at the Figure 1.
center of the post cavity with a low-speed precision cutter The resin and dentin fragments were mounted on
(Isomet; Buehler) to create a 0.6-mm-thick slab. The slab brass holders and sputter-coated with gold (Quick Auto
was sectioned perpendicular to the bonded interface to Coater SC-701AT; ELIONIX Inc). Using a scanning
produce eight 0.6×0.6-mm-thick beams.22 Four coronal electron microscope (JSM IT-100; JEOL Ltd), failure
beams represented the coronal region of the post cavity, modes were classified into 1 of 4 categories: adhesive
corresponding to the coronal third of the root canal, and failure (A: >70% of the failure area was at the interface
4 apical beams represented the apical region of the post between the resin and the dentin), cohesive failure
cavity, corresponding to the middle third of the root ca- within dentin (CD: >70% of the failure area was within
nal. The interface to be tested was selected, and the the dentin), cohesive failure within resin core (CR: >70%
beams were carefully glued to a testing jig with cyano- of the failure area was within the resin), or mixed failure
acrylate resin (Model Repair II Blue; Dentsply Sirona). (M: combination of both cohesive and adhesive failure).21
Figure 1. Schematic illustration of bonding procedures and microtensile bond strength testing. DCA, Clearfil DC Activator; PBU, Prime&Bond Universal;
s, seconds; SCA, Self Cure Activator; SEB, Clearfil SE Bond 2; UBQ, Universal Bond Quick ER.
The Kolmogorov-Smirnov test indicated that mTBS Table 2. Results of repeated measures ANOVA showing effects of
data were normally distributed. A repeated measures bonding systems, dentin region, and light-irradiation time on
analysis of variance (ANOVA) was performed to evaluate microtensile bond strength
the effect of 2 between-subject variables (bonding systems Source SS df MS F P
and light-irradiation time) and 1 within-subject variable Regiona 19070.165 1 19070.165 963.098 <.001
Region×Bonding systema 2834.236 4 708.559 35.784 <.001
(dentin region). To analyze the effect of touch-
Region×Light-irradiation timea 52.541 1 52.541 2.653 .111
polymerization activators, a 3-way ANOVA was per-
Region×Bonding system×Light- 113.007 4 28.252 1.427 .243
formed for each region with the following factors: adhe- irradiation timea
sives (PBU and SEB), touch-polymerization activator (with Bonding systemb 5549.767 4 1387.442 9.624 <.001
or without), and light-irradiation time (10 seconds or 20 Light-irradiation timeb 2071.330 1 2071.330 14.368 <.001
seconds). The Bonferroni correction was performed for Bonding system×light-irradiation timeb 863.046 4 215.762 1.497 .221
multiple comparisons of all analyses. The failure modes DCA, Clearfil DC Activator; PBU, Prime&Bond Universal; SCA, Self Cure Activator; SEB,
were analyzed with the Kruskal-Wallis test to compare the Clearfil SE Bond 2; UBQ, Universal Bond Quick ER. Bonding systems (PBU, PBU+SCA,
SEB, SEB+DCA, and UBQ); region (coronal and apical); and light-irradiation time (10 or
bonding systems and light-irradiation times within each 20 seconds). aTest of within-subject effect. bTest of between-subject effect.
region of the root, followed by pairwise comparisons with
the Dunn-Bonferroni correction (a=.05). A statistical
software program (IBM SPSS Statistics for Windows, v23;
the dentin region were also significantly different (P<.001),
IBM Corp) was used for the analyses.
whereas the interaction between light-irradiation time and
both dentin region (P=.111) and bonding system (P=.221)
RESULTS
were not. Moreover, the interaction among the 3 factors was
The repeated measures ANOVA (Table 2) revealed that the also statistically similar (P=.234). The 3-way ANOVAs
effects of dentin region, bonding system, and light- (Tables 3 and 4) revealed that the touch-polymerization
irradiation time were statistically significantly different activator significantly affected mTBS in the coronal (P=.015)
(P<.001). The interactions between the bonding systems and and apical regions (P=.001). The effect of adhesives was
Table 3. Results of 3-way ANOVA showing effects of adhesives, touch- Table 4. Results of 3-way ANOVA showing effects of adhesives, touch-
polymerization activator, and light-irradiation time in coronal region polymerization activator, and light-irradiation time in apical region
Variables SS df MS F P Variables SS df MS F P
Adhesives 4146.014 1 4146.014 35.327 <.001 Adhesives 101.194 1 101.194 2.23 .145
Touch-polymerization activator 774.088 1 774.088 6.596 .015 Touch-polymerization activator 664.251 1 664.251 14.641 .001
Light-irradiation time 358.31 1 358.31 3.053 .090 Light-irradiation time 1163.336 1 1163.336 25.642 <.001
Adhesives×Touch-polymerization activator 27.192 1 27.192 0.232 .634 Adhesives×Touch-polymerization activator 3.136 1 3.136 0.069 .794
Adhesives×Light-irradiation time 4.199 1 4.199 0.036 .851 Adhesives×Light-irradiation time 12.442 1 12.442 0.274 .604
Touch-polymerization activator×Light- 93.25 1 93.25 0.795 .379 Touch-polymerization activator×Light- 33.686 1 33.686 0.743 .395
irradiation time irradiation time
Adhesives×Touch-polymerization 247.415 1 247.415 2.108 .156 Adhesives×Touch-polymerization 443.421 1 443.421 9.774 .004
activator×Light-irradiation time activator×Light-irradiation time
DCA, Clearfil DC Activator; PBU, Prime&Bond Universal; SCA, Self Cure Activator; SEB, DCA, Clearfil DC Activator; PBU, Prime&Bond Universal; SCA, Self Cure Activator; SEB,
Clearfil SE Bond 2; UBQ, Universal Bond Quick ER. Adhesives (PBU and SEB); touch- Clearfil SE Bond 2; UBQ, Universal Bond Quick ER. Adhesives (PBU and SEB); touch-
polymerizeation activator (with or without); and light-irradiation time (10 or 20 seconds). polymerization activator (with or without); and light-irradiation time (10 or 20 seconds).
Table 5. Microtensile bond strength to root canal dentin for each 100
bonding system, light-irradiation time, and root region (mean ±standard
deviation) 80
Bonding System Irradiation Time Coronal Apical P
μTBS (MPa)
PBU 10 s 52.8a ±9.1 34.3a ±5.0 .002
60
a b
20 s 66.1 ±4.2 52.5 ±5.8 .020
40
PBU+SCA 10 s 67.9a ±10.4 51.5b ±7.6 .005
20 s 65.2a ±9.9 52.7b ±6.8 .032
20
SEB 10 s 75.8a ±11.9 37.3a ±7.4 <.001
20 s 80.5ab ±10.4 44.3ab ±3.9 <.001 0
PBU
PBU+SCA
SEB
SEB+DCA
UBQ
PBU
PBU+SCA
SEB
SEB+DCA
UBQ
PBU
PBU+SCA
SEB
SEB+DCA
UBQ
PBU
PBU+SCA
SEB
SEB+DCA
UBQ
ab
SEB+DCA 10 s 84.3 ±16.4 40.0a ±8.6 <.001
20 s 92.9b ±10.6 56.7b ±7.6 <.001
UBQ 10 s 54.7a ±12.8 27.0a ±5.9 <.001
20 s 69.0b ±5.4 36.7a ±10.4 <.001
10 s 20 s 10 s 20 s
DCA, Clearfil DC Activator; PBU, Prime&Bond Universal; s, seconds; SCA, Self Cure
Activator; SEB, Clearfil SE Bond 2; UBQ, Universal Bond Quick ER. For each individual
Apical Coronal
adhesive (PBU, SEB, UBQ), different letter within each column indicates significant
Figure 2. Microtensile bond strengths of dentin region, bonding system,
difference (P<.05). P values refer to difference between coronal and apical regions.
and light-irradiation time. Horizontal bars between columns indicate
significant difference (P<.05). DCA, Clearfil DC Activator; PBU,
Prime&Bond Universal; s, Seconds; SCA, Self Cure Activator; SEB, Clearfil
significant only in the coronal region (P<.001), while light- SE Bond 2; UBQ, Universal Bond Quick ER.
irradiation time was a significant factor only in the apical
region (P<.001). Interactions between pairs of factors were
not significant in either of the dentin regions (P>.05); mTBS of UBQ (10 seconds) was significantly lower than
however, the interaction among the 3 factors was significant that of UBQ (20 seconds) in the coronal region (P=.014),
in the apical region (P=.004). but not in the apical region (P>.05).
The mTBS of the tested groups are presented in Table 5 Failure mode distributions are presented in Table 6. In
and Figure 2. The coronal region demonstrated significantly the coronal region, there was no significant difference in
higher mTBS than the apical region in all tested groups failure mode among the tested groups (P=.099). In
(P<.05). In the coronal region, there was no significant contrast, in the apical region, the PBU (10 seconds) group
difference between groups bonded with PBU and exhibited a significantly higher incidence of adhesive
PBU+SCA. In the apical region, the mTBS of PBU (10 sec- failures (85%, P=.002) than the other groups. Addition-
onds) was significantly lower than that of PBU (20 seconds) ally, the adhesive layers in the apical region contained
(P=.013), PBU+SCA (10 seconds) (P=.022), and PBU+SCA numerous voids, whereas no such voids were observed in
(20 seconds) (P=.001). SEB (10 seconds) exhibited a the coronal region (Fig. 3). No pretesting failures
significantly lower mTBS than SEB+DCA (20 seconds) in the occurred during specimen preparation.
coronal (P=.023) and apical (P=.007) regions. The addition
of DCA or the extension of light-irradiation time alone did DISCUSSION
not significantly increase the mTBS of SEB (P>.05) in either
of the regions except for the mTBS of SEB+DCA (20 sec- The results of this study revealed that the addition of a
onds), which was significantly higher than that of touch-polymerization activator to light-activated adhe-
SEB+DCA (10 seconds) in the apical region (P<.05). The sives SEB and PBU significantly improved their mTBS to
Table 6. Failure mode percentages The mTBS of SEB and PBU were significantly lower
Region Adhesive Irradiation Time A C/D C/R M in the apical region than in the coronal region. In the
Coronal PBU 10 s 30 0 0 70 case of SEB, whose polymerization is initiated by
20 s 30 0 20 50 camphorquinone,24 the apical mTBS was almost half of
PBU+SCA 10 s 15 0 20 65
the coronal mTBS, on which the extension of the light-
20 s 50 0 15 35
irradiation time had no significant effect. In contrast,
SEB 10 s 45 5 5 45
PBU, which uses a phosphine oxide photoinitiator,
20 s 40 5 35 20
exhibited significantly higher mTBS in the apical region
SEB+DCA 10 s 25 10 15 50
20 s 20 25 10 45
if light-irradiation time was extended to 20 seconds
UBQ 10 s 30 25 10 35
and the difference between regions decreased. The
20 s 15 5 20 60 apical mTBS was significantly lower than the coronal
Apical PBU 10 s 85 0 0 15 mTBS even if touch-polymerization activators were
20 s 35 5 0 60 added (SCA to PBU and DCA to SEB). This indicated
PBU+SCA 10 s 25 0 10 65 that light energy delivered to the adhesives affected the
20 s 35 0 20 45 bonding performance of dual-activated adhesives,
SEB 10 s 40 5 0 55 regardless of touch-polymerization.
20 s 50 0 15 35 Extending the light-irradiation time slightly
SEB+DCA 10 s 55 0 20 25 increased the mTBS of SEB in both regions, but its effect
20 s 35 25 5 35 was more pronounced with SEB+DCA, leading to a
UBQ 10 s 65 0 10 25
significant increase in mTBS in the apical region. The
20 s 45 5 5 45
SEB+DCA (20 seconds) group exhibited the highest
A, Adhesive failure; CD, Cohesive failure within dentin; CR, Cohesive failure within resin
core; DCA, Clearfil DC Activator; M, Mixed failure; PBU, Prime&Bond Universal; s,
mTBS among SEB groups in both regions, indicating a
Seconds; SCA, Self Cure Activator; SEB, Clearfil SE Bond 2; UBQ, Universal Bond Quick combined effect of the DCA addition and extended
ER. light-irradiation time on the mTBS of SEB. Presumably,
the addition of DCA promoted the light-activated
root canal dentin. Hence, the first null hypothesis was polymerization of SEB.
rejected. The effect of extended light-irradiation time was In the case of PBU, the apical mTBS was significantly
significant according to the repeated measures ANOVA, increased with SCA. SCA contains tetraphenylborate
but the 3-way ANOVA for SEB and PBU indicated that (TPB) salts, which are derivatives of aryl borate salts. The
the extension significantly affected the bond strengths reaction between the TPB ion and the proton from acidic
only in the apical region. Therefore, the second null hy- monomer produces triphenyl boron, which later de-
pothesis was partially rejected. composes to a phenyl free radical that initiates chemical
UBQ is a type of 1-SEA that contains a touch- polymerization.25 This mechanism is similar to that of
polymerization activator. Consequently, it can poly- DCA, which contains aryl sulfinic acid sodium salt. How-
merize chemically when used in combination with a ever, in contrast with DCA, the combination of SCA with
specific chemical initiator in a dual-polymerizing resin extended light-irradiation time did not further increase the
core material such as in Clearfil DC Core Automix ONE. mTBS of PBU. The phosphine oxide photoinitiator in SCA
The mTBS of UBQ in the apical region was lower than could produce more free radicals, thus enabling optimal
that in the coronal region, irrespective of light-irradiation polymerization even at a shorter light-irradiation time.
time. The lower bond strengths in the apical region may Therefore, touch-polymerization activators may affect the
be attributed to insufficient solvent evaporation from the mTBS of light-activated adhesives not only by using an
1-SEA in the post cavity,21,23 resulting in the increased accelerator of chemical polymerization but also by incor-
incidence of adhesive failure because of the formation of porating an additional photoinitiator.
multiple voids in the adhesive layer in the apical region The 3-way ANOVA revealed no significant inter-
(Fig. 3). The extension of light-irradiation time improved action between adhesives, touch-polymerization ac-
the mTBS of UBQ significantly in the coronal region, tivators, and light-irradiation time in the coronal
indicating that chemical polymerization initiated solely region. Conversely, the interaction was significant in
by the touch-polymerization system may not fully replace the apical region, presumably because light energy
light-activation and that optimal polymerization is ob- was attenuated. Since no significant interaction was
tained if the 2 activation methods are combined, because observed between pairs of the factors, this indicated
additional radicals are formed by photoinitiators upon that the combined effect of touch-polymerization
light-irradiation.14 These results are consistent with those activators and extended light-irradiation time was
of previous reports on touch-polymerization systems15 dependent on the adhesive used: the apical mTBS of
and dual-activated materials.3,4,23 SEB was improved but that of PBU was not.
Figure 3. Representative scanning electron microscope images of adhesive and/or mixed failures in coronal and apical regions of post cavities. Original
magnification ×500. A, PBU coronal region. B, PBU apical region. C, PBU+SCA coronal region. D, PBU+SCA apical region. E, SEB coronal region. F, SEB
apical region.
Figure 3. (Continued) G, SEB+DCA coronal region. H, SEB+DCA apical region. I, UBQ coronal region. J, UBQ apical region. DCA, Clearfil DC Activator;
PBU, Prime&Bond Universal; SCA, Self Cure Activator; SEB, Clearfil SE Bond 2; UBQ, Universal Bond Quick ER.
2. Their effect may be additive, especially in the apical 8. Feitosa V, Watson T, Vitti R, Bacchi A, Correr-Sobrinho L, Correr A, et al.
Prolonged curing time reduces the effects of simulated pulpal pressure on
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9. Catelan A, Soares GP, Bedran-Russo AK, Lima DANL, Marchi GM,
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