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Available online at www.sciencedirect.com

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journal homepage: www.intl.elsevierhealth.com/journals/dema

New bulk-fill composite system with high

irradiance light polymerization: Integrity and
degree of conversion

Juri Hayashi a,b , Junji Tagami b , Daniel Chan a , Alireza Sadr a,∗
a Department of Restorative Dentistry, Biomimetics Biomaterials Biophotonics Biomechanics & Technology
Laboratory, School of Dentistry, University of Washington, 1959 NE Pacific Street, Seattle, WA 98195-7456, USA
b Cariology and Operative Dentistry, Department of Restorative Sciences, Graduate School of Medical and Dental

Sciences, Tokyo Medical and Dental University, 1-5-45, Yushima, Bunkyo-ku, Tokyo 113-8549, Japan

a r t i c l e i n f o a b s t r a c t

Article history: Objective. The study used optical coherence tomography (OCT) and micro Raman microscopy
Available online xxx (mRM) to investigate internal defect (ID) and degree of conversion (DC) of two bulk-fill
composite systems with high-irradiance or conventional light polymerization settings.
Keywords: Methods. The ID and DC of the new bulk-fill composites; Tetric PowerFill (PwrPst) and Tetric
Polymerization PowerFlow (PwrFlw) were compared with the predecessor bulk-fill composites; Tetric Evo-
Dental restoration failure Ceram Bulkfill (EvoPst) and Tetric EvoFlow Bulkfill (EvoFlw), using LED light curing unit in
Optical coherence tomography two settings; normal (LED-Nrm: 1000 mW/cm2 , 10-s) or PowerCure (LED-Pwr: 3000 mW/cm2 ,
Bulk-fill 3-s). ID formation was observed in bonded cylindrical composite cavities (4-mm depth, 3-
Shrinkage stress mm diameter) using Yoshida Dental OCT. From the vertically projected 2D image, ID area
Gap percentage (ID-A%) was calculated. DC at the top and bottom and bottom/top DC ratio (DC-
Cracks R%) of 4-mm thick discs was calculated using mRM. All data were statistically analyzed at
Interfacial integrity significance level of ˛ = 0.05.
Kinetics Results. Flowable composites in LED-Pwr showed smaller ID frequencies than other groups
(PwrFlw: 0/8, EvoFlw: 2/8) (p < 0.05). Composite type significantly affected ID-A%, DC and
DC-R% (p < 0.001), while light settings significantly affected ID-A% but not DC and DC-R% (p
> 0.05). In both light settings, EvoPst showed the lowest DC-R% (<80%).
Significance. Internal defect and degree of conversion of bulk-fill composites were affected by
their composition and light settings. There was a tendency for less defects and better poly-
merization for the flowable bulk-fills. The new flowable bulk-fill composite with 3-seconds
high irradiance light curing showed no defect formation.
© 2020 The Academy of Dental Materials. Published by Elsevier Inc. All rights reserved.

∗
Corresponding author at: Department of Restorative Dentistry, University of Washington, 1959 NE Pacific Street Box 357456, Seattle, WA
98195-7456, USA.
E-mail address: [email protected] (A. Sadr).
https://doi.org/10.1016/j.dental.2020.10.012
0109-5641/© 2020 The Academy of Dental Materials. Published by Elsevier Inc. All rights reserved.

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Liechtenstein). The system is compositionally mainly similar

1. Introduction to its predecessors, but features a 3-seconds curing setting at
3000 mW/cm2 .
Resin composites have become reliable materials for direct
According to the exposure reciprocity law, the total radi-
restorations, thanks to the development of the mechanical
ant exposure (J/cm2 ) is the product of irradiance (W/cm2 ) and
properties and adhesive technology [1]. In order to meet the
exposure time (s). However, studies have reported that the
demands for application in various clinical situations particu-
degree of conversion (DC) and the kinetics of the composite
larly extensive restorations, incremental layering techniques
polymerization depended on the many parameters and did
were introduced [2]. The rationale behind the technique was to
not necessarily conform to this law and total radiant exposure
guarantee the penetration of the curing light deeply enough to
[20,21]. Furthermore, the high irradiance might be associated
initiate and complete curing, besides the minimization of the
with negative effects on stress generation [10,22]. In spite
shrinkage and shrinkage-induced stress associated with the
of these concerns, clinical evaluations with up to 10 years
polymerization [3]. The time consuming nature of the place-
follow-up suggested that bulk-fill composites were compara-
ment and light irradiation in multiple increments along with
ble in performance with incremental composite restorations
the risks of void formation and oral fluid contamination [4]
[23]. The adverse events of bulk-fill composite restorations
have promoted the development of bulk-fill resin composites,
were mainly associated with physical defects, loss of marginal
which have been commercially introduced for placement as a
integrity and tooth/restoration fractures [24,25]. Given the
single increment up to 4- or 5-mm depth [5].
importance of the material integrity, a meaningful investiga-
Polymerization shrinkage of methacrylate-based dental
tion of a newly introduced bulk-fill materials should consider
resin composites is unavoidable, due to the fact that monomer
internal defect (ID) formation [26].
molecules are converted into a polymer network and, there-
Optical coherence tomography (OCT) has been introduced
fore, exchanging van der Waals spaces in covalent bond spaces
for non-invasive real-time observation of ID formation and
[6]. Contraction stress is the result of polymerization shrink-
3D quantification in resin composites. The infrared beam of
age taking place under confinement caused by bonding to
high-speed swept-source OCT is far in wavelength from the
cavity walls [7]. The stress magnitude is affected by the vol-
absorption spectrums of any photo-initiators. In addition, fast
ume of each increment and cavity configuration (C-factor) [8],
digital to analogue (DAC) technology and powerful image pro-
which are relatively larger in bulk-fill materials applications.
cessing [26,27] have facilitated 3D real-time observation of the
Therefore, the stress control has been one of the main sub-
polymerization phenomenon.
jects in the material development. Various approaches have
The objective of this study was to observe and quantify ID
been employed in the formulation of bulk-fill composites to
formation during light polymerization of the new fast-curing
reduce the stress, adjust the stress generation kinetics and
bulk-fill composite by OCT followed by DC analysis using micro
improve depth of cure. Those include changes in filler con-
Raman microscophy. The null hypothesis was that there was
tent and shape [9], modified monomer molecular weight and
no significant difference in ID and DC among the new and
structure [10], addition of stress relievers and polymerization
the predecessor bulk-fill materials and in combination with
modulators [11,12], increase of polymerization inhibitors [10],
different light curing settings.
new combinations of photoinitiators [13], enhanced mate-
rial translucency and dual-cured polymerization mechanisms
[14].
2. Materials and methods
In addition to the resin composite material deveropments,
the dental light curing units (LCUs) have been evolving in the
2.1. Specimen preparation
paradigm shift. Light emitting diodes (LEDs) have intensively
been used as light source for LCUs due to the advantages
Procedures of specimen preparation and OCT real-time mon-
over quartz–tungsten–halogen units (QHTs) in terms of lower
itoring followed a previous study [26]. Cylindrical cavities
heat emission, maintenance cost, and the higher durability
(3 mm in diameter, 4 mm in depth, C-factor = 4.98) were
[15]. Compared to the wide range wavelength output of QHTs,
prepared in resin composite blocks using a diamond bur
LEDs have a narrower maximum peak of light emission [16].
(SF101CR, Shofu, Kyoto, Japan) with a high-speed handpiece
In order to achieve the maximum polymerization efficiency of
under water coolant. A silicone impression of the prepara-
each composite, various LED-LCUs have been developed with
tion was made (EXA’lence extra light body; GC America, IL,
adjustment the emission peaks and combination of differ-
USA), form which 64 standardized molds were fabricated with
ent LEDs that match the absorption spectrum of the targeted
a light-curing flowable resin composite (Estelite Flow Quick
photoinitiators [17]. However, these technological develop-
shade A2; Tokuyama Dental, Tokyo, Japan). The flowable resin
ments have set some restrictions on the selection of LCUs to
composite was inserted and polymerized in 4 increments with
match the photo-polymerization requirements of the compos-
40 s using a halogen light curing unit with 500 mW/cm2 light
ites [18].
irradiance (Coltolux 75; Coltene/Whaledent Inc., Cuyahoga
Manufacturers have introduced high irradiance LED-
Falls, OH, USA) for each increment. Each resulting mold was
LCUs, anticipating an improved polymerization efficiency and
stored in 37 ◦ C for 1 week to complete polymerization. In order
shortened clinical procedure time [19]. Recently, a bulk-fill
to provide sufficient bonding, the inner surfaces of the molds
composite system including high and low viscosity light-cured
were sandblasted with 50 ␮m alumina particles (MicroEtcher
bulk-fill composites and a high irradiance light curing unit has
II; Danville Materials, Carlsbad, CA, USA) at 0.4 MPa for 15
been developed (3 s PowerCure, Ivoclar Vivadent AG, Schaan,
s, followed by ultrasonic cleaning for 10 min (Model US 102;

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Table 1 – Tested composites, specimen preparation and surface treatment materials and tested light curing units and the
settings used in the study.
Tested composites

Material/shade (code/lot no). Recommended light activation Viscosity Composition (filler wt% &
manufacturer time and irradiance vol%)
Tetric EvoCeram Bulk fill/IVA 20 s (≥500 mW/cm2 ), 10 s (≥1000 High Monomers; Bis-GMA, Bis-EMA,
(EvoPst/W33026) Ivoclar Vivadent mW/cm2 ) UDMA Fillers; Barium aluminium
AG, Schaan, Liechtenstein silicate glass, Ytterbium,
Trifluoride, Prepolymer, Mixed
Oxide (77 wt%, 55 vol%)
Tetric EvoFlow Bulk fill/IVA 20 s (≥500 mW/cm2 ), 10 s (≥1000 Low Monomers; Bis-GMA, Bis-EMA,
(EvoFlw/V30889) Ivoclar Vivadent mW/cm2 ) UDMA Fillers; Barium aluminium
AG, Schaan, Liechtenstein silicate glass, Ytterbium,
Trifluoride, Prepolymer, Mixed
Oxide (68.2 wt%, 46.4 vol%)
Tetric PowerFill/IVA 20 s (500–900 mW/cm2 ), 10 s High Monomers; Bis-GMA, Bis-EMA,
(PwrPst/W11515) Ivoclar Vivadent (900–1400 mW/cm2 ) 5 s (1800–2200 UDMA, Bis-PMA, DCP, D3MA.
AG, Schaan, Liechtenstein mW/cm2 ), 3 s (2700–3300 mW/cm2 ) Fillers; Barium glass, Ytterbium,
Trifluoride, Copolymer, Mixed
Oxide (SiO2 /ZrO2 ) (79 wt%, 53–54
vol%)
Tetric PowerFlow/IVA 20 s (500–900 mW/cm2 ), 10 s Low Monomers; Bis-GMA, Bis-EMA,
(PwrFlw/WM1175) Ivoclar Vivadent (900–1400 mW/cm2 ) 5 s (1800–2200 UDMA, CMP-1E, DCP, D3MA.
AG, Schaan, Liechtenstein mW/cm2 ), 3 s (2700–3300 mW/cm2 ) Fillers; Barium glass, Ytterbium,
Trifluoride, Copolymer, Mixed
Oxide (SiO2 /ZrO2 ) (71 wt%, 46–47
vol%)

Specimen preparation and surface treatment materials

Materials lot no. Manufacturer Composition Application

Estelite Flow Quick shade A2 JO651 Tokuyama Dental, Tokyo, Japan Monomers; Bis-MPEPP, Dispense in layers up to 2 mm in
TEGDMA, UDMA, Fillers; thickness; light cure for 20 s.
Silica-zirconia filler,
silica-titania fillers (71 wt%,
53 vol%)
K-etchant gel 3D0042 Kuraray Noritake Dental, Tokyo, 35–45% phosphoric acid, Apply onto the adherent surface
Japan colloidal silica, water and leave for 5 s; Thoroughly wash
and dry.
Clearfil Ceramic Primer Plus Kuraray Noritake Dental, Tokyo, Methacryloxypropil Apply to the adherent surface; dry
A50030 Japan trimethoxy silane, MDP, the entire adherent surface
Ethanol sufficiently using mild, oil-free air
blow.
Adhese Universal W83530 Ivoclar Vivadent AG, Schaan, MDP, Bis-GMA, HEMA, CQ, Apply onto the adherent surface
Liechtenstein MCAP, D3MA, ethanol, and mild air blow; Light cure for 10
water, highly dispersed s.
silicon dioxide
Bis-EMA, bisphenol-A polyethylene glycol diether dimethacrylate; Bis-GMA, bisphenol-A diglycidyl ether dimethacrylate; UDMA,
urethane dimethacrylate; Bis-PMA, Propoxylated bisphenol A-dimethacrylate; DCP, tricyclodecane dimethanol dimethacrylate;
D3MA, decandiol dimethacrylate; CMP-1E, p-cumylphenoxyethylene glycol methacrylate; Bis-MPEPP, bisphenol A polyethoxy
methacrylate; TEGDMA, triethylene glycol dimethacrylate; MDP, 10-methacryloyloxydecyl dihydrogen phosphate; CQ,
camphorquinone; HEMA, 2-hydroxyethyl methacrylate; MCAP, Methacrylated carboxylic acid polymer

The light curing unit

Equipment, manufacturer Light source and wavelength Curing setting (code), irradiance &
time (total exposure)
Bluephase PowerCure Experimental #8 3 blue and 1 violet light LEDs Spectral Normal setting (LED-Nrm); 1200 mW/cm2 ,
Ivoclar Vivadent AG, Schaan, peaks; 410 nm and 460 nm (>385 nm, <515 10 s (=12 J/cm2 ) Power setting (LED-Pwr);
Liechtenstein nm) 3400 mW/cm2 , 3 s (=10.2 J/cm2 )

SND, Nagano, Japan), phosphoric acid cleaning (K-etchant gel; in accordance with the manufacturer’s instructions as listed
Kuraray Noritake Dental, Tokyo, Japan), silanization (Clearfil in Table 1.
Ceramic Primer Plus; Kuraray Noritake Dental, Tokyo, Japan), Four types of light-cured resin composites (two high-
and adhesive (Adhese Universal; Ivoclar Vivadent AG, Schaan, viscous and two low-viscous resin composites) recommended
Liechtenstein). All surface conditioning steps were performed for bulk placement in 4 mm depth were evaluated (Table 1);

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two new bulk-fill composites; Tetric PowerFill (PwrPst, paste- (ID-A%) values were calculated considering the area propor-
type) and Tetric PowerFlow (PwrFlw, flowable) and their two tion of the binarized pixel clusters over total floor area in each
predecessor bulk-fill composites; Tetric EvoCeram Bulkfill MIP image.
(EvoPst, paste-type) and Tetric EvoFlow Bulkfill (EvoFlw, flow-
able) (Ivoclar Vivadent AG, Schaan, Liechtenstein). 2.3. Degree of conversion (DC)
The resin composites were placed in the mold in bulk, and
the free surface was covered by a plastic matrix (Hawe Trans- Discs from each the 4 experimental composites were placed
parent Striproll, Kerr, Orange, CA, USA) to flatten the surface and polymerized using each of the two light curing settings
and isolation without disturbing the light delivery. High vis- as described earlier in a silicone mold (3 mm in diameter, 5
cous composites (EvoPst and PwrPst) were placed using a hand mm in height). After 24 h storage in deionized water at 37
instrument as a single increment. Low viscous composites ◦ C, the discs were axially sectioned at the center with low-

(EvoFlw and PwrFlw) were directly dispensed from the syringe speed diamond saw (Isomet, Buehler, Lake Bluff, IL, USA) in a
using the provided tips. dark room. Raman microscopy (LabRAM HR Evolution, Horiba,
The tested composites were polymerized by a LED light Kyoto, Japan) with power output of 5 mW was used to collect
curing unit (Bluephase PowerCure premarket prototype test 633 nm wavelength laser spectrum along a Z-axis line at the
sample #8, Ivoclar Vivadent AG, Schaan, Liechtenstein) with center of the cross-section at 500 ␮m intervals (n = 3). Unpoly-
two light settings similar in nominal total exposure; normal merized resin composite specimens (3 mm in diameter, 1 mm
setting (LED-Nrm; 1000 mW/cm2 , 10 s) and power setting in height) were also measured under the same Raman settings
(LED-Pwr; 3000 mW/cm2 , 3 s). The radiant exitance of each at the center as a reference. From the obtained spectrums,
mode was confirmed prior to the experiment using a handheld the degree of conversion (DC) of the polymerized specimen
radiometer (Bluephase Meter II, Ivoclar Vivadent AG, Schaan, was calculated using the aliphatic CC peak at 1640 cm−1 as an
Liechtenstein). The values recorded from 3 measurements immutable reference and the aromatic CC peak at 1610 cm−1
were consistently 1200 mW/cm2 and 3400 mW/cm2 , respec- as a reaction peak as follows:
tively. During photo polymerization, the LCU guide tip was set  
aliphatic C=C
perpendicularly as close as possible over the plastic matrix on aromatic C=C
the top surface of the resin composite. DC = 1 −   polymerised
aliphatic C=C
aromatic C=C
unpolymerised
2.2. Optical observation of internal defect formation
and quantitative 3D analysis To exclude the effect of oxygen inhibition of the polymer-
ized specimens, DC at the top region (DCtop) was calculated by
A prototype OCT system (Yoshida Dental OCT, Yoshida Mfg., the spectrum obtained at 0.5 mm from the top surface. DC at
Tokyo, Japan) with 12.13 mW output power at sample, a cen- the bottom region (DCbottom) was calculated by the spectrum
ter wavelength was 1310 nm (bandwidth 140 nm) and 50-kHz obtained at 4 mm from the top surface. The bottom-to-top
sweep rate was used for evaluation of the internal defect DC ratio (DC-R%) which indicates the extent of polymeriza-
formation in the placements of composites. The optical reso- tion decrement through depth was calculated according to the
lution is 40 ␮m transversally and 11 ␮m axially in air (7–8 ␮m formula:
in tissues with a refractive index around 1.5) [28]. During poly- DCbottom
DC − R (%) = × 100
merization of the resin composites, the OCT probe was placed DCtop
beneath the mold specimen so that formation of the internal
defect at deeper regions of the restoration adjacent to the cav-
2.4. Statistical analysis
ity floor could be imaged through the 0.5-mm thick mold. The
XZ cross-sectional views (B-scans) at the center of the mold
ID Frequencies were statistically analyzed using Pearson Chi-
and en-face views were recorded continuously in real time as
Square test followed by residual analysis using adjusted
a windows media video file at a resolution of 800 × 600 pixels
residual values. The effects of factors composite type and light
and 20 frames per second. 3D scans were obtained immedi-
curing settings and their interaction on the variables ID-A%
ately after light-curing at 400 × 400 × 1024 pixels over an XYZ
and DC-R% were statistically analyzed using two-way ANOVA.
volume of 6 × 6 × 8 mm3 . Immediately after the scanning,
DC values were analyzed by repeated-measure ANOVA which
OCT was applied from top of the cavities so that the integrity
treated depth (top vs. bottom) as a within subject factor. Bon-
at the middle-top regions of the placements of all specimens
ferroni correction was used for pairwise comparisons among
was confirmed.
groups. All the analyses were performed using the Statistical
ID frequency was recorded as the specimens with any
Package for Social Science (SPSS, Chicago, IL, USA) with the
defect formation during polymerization in each group. Amira
significance level set at ˛ = 0.05.
software (version 5.5.0, FEI Visualization Sciences Group, Ore-
gon, USA) was then used for quantitative analysis of OCT data.
For ID quantification, a volume of interest (VOI) of 3 × 3 × 3. Results
1 mm3 , covering the whole cavity floor area was selected on
each scan. A binary image was created by averaging XY slices The representative OCT real-time observation video clips of
over 1000-␮m thick region at the floor using the maximum each composites edited in Windows Movie Maker (Microsoft,
intensity projection (MIP) in the VOI, according to a previously Bellevue, WA) are presented in Videos A–D. The still images
established method [26,27]. Internal defect area percentage are shown in Fig. 1a–d. Real-time OCT recordings could show

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Fig. 1 – Representative OCT XZ cross-section at horizontal line on the XY en-face frames from the real-time video clips
during the light curing procedure from each specimen (a–d).
The high signal intensities (a–c, white, black and bold arrows) which indicate ID appeared in the materials during light
irradiation, while all PwrFlw/LED-Pwr specimens showed no defect formation (d). In paste-type composites (EvoPst and
PwrPst), voids and air bubbles that tended to entrap showed enlargement during the light polymerization (a, c, black
arrows). Also crack-like defects initiated during light curing (a–c bold arrows). Immediately after finishing light curing, 3D
OCT scan was applied and from the data presence and the location of the defect in any XZ, YZ and XY cross-sections was
confirmed (e, white arrows). The OCT data set was imported and processed in Amira software (f–i). The 3D image was
reconstructed by a series of OCT XZ data (f), and the 3D volume were selected for analysis over 1-mm thick region of interest
at the floor (g). The selected region was projected on Z axis using the MIP method (h), and the ID area percentage (ID-A%;
white arrow) in whole cavity area (broken circle) was finally calculated (i).

internal defects initiation within the bulk of the composite

and its vertical and horizontal developments. IDs were indi-
cated by high signal intensities in the XZ cross-sectional views
(Fig. 1a–c) and XY en-face views (Fig. 1a–c). In EvoPst and
PwrPst, voids and air bubbles that tended to entrap in resin
composites during the placement showed enlargement dur-
ing the light polymerization (Fig. 1a, c). In some specimens,
crack-like defects initiated during light curing (Fig. 1a–c). The
scanned OCT dataset could be explored in the system for
visualization of any XZ, YZ, and XY cross-sections (Video E,
Fig. 1e). After the light curing, the majority of the defects were
observed in the deepest areas of the cavity within 1 mm of the
cavity floor (Fig. 1e, g). Under LED-Nrm setting, all specimens
Fig. 2 – Internal defect (ID) frequency in each group. ID
(8/8) showed some defect formation regardless of the compos-
frequencies were statistically analyzed using Pearson
ite. In LED-Pwr, the two flowable composites polymerized had
Chi-Square test followed by residual analysis using
significantly smaller ID frequencies (EvoFlw: 2/8, PwrFlw 0/8)
adjusted residual values indicate significant difference
than the two paste-type composites (EvoPst: 7/8, PwrPst 5/8)
among groups (p < 0.05).
(p < 0.001, Fig. 2).
Mean values of ID-A% calculated from MIP images (Fig. 3)
were shown in Table 2. ID-A% was significantly affected by
both factors of composite type (p < 0.001) and light setting (p nificantly affected by factors of measured location (top vs.
< 0.001), and their interaction was significant (p < 0.001). In bottom), composite type and their interaction (p < 0.001), but
both light settings, there was a significant difference among not light settings (p = 0.99). All composites showed a signifi-
all composites; PwrFlw showed the smallest ID-A% followed cantly higher DC at the Top compared with the Bottom (p <
by EvoFlw and PwrPst (p < 0.05). Within composites, LED- 0.05) (Table 3). The DC-R% ranged between 75.6% and 96.1%
Pwr setting resulted in significantly smaller defect formation for different groups. While there was a significant effect of
(p < 0.05) for all composites, except for EvoPst. DC was sig- composite as a factor (p < 0.001), the light settings did not

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Table 2 – Mean (standard deviation) values of ID-A% in each group. Two-way ANOVA followed by pairwise comparison
with Bonferroni was performed. There was a significant difference among all groups in each row (p < 0.05). Same
uppercase letters in each column indicate no significant difference (p > 0.05).
Composite/light curing settings EvoPst EvoFlw PwrPst PwrFlw
LED-Nrm 22.1 (4.7)A 8.3 (3.4) 14.4 (2.7) 3.1 (1.8)
LED-Pwr 17.1 (3.6)A 0.84 (1.3) 4.0 (1.2) 0 (0)

Table 3 – Mean (standard deviation) of DC percentage values of each group. Repeated-measure ANOVA followed by
pairwise comparisons with Bonferroni corrections was performed. Similar lowercase letters in each row indicate no
significant difference between groups (p > 0.05). (A) Similar uppercase letters with a group indicate no significant
difference between top and bottom locations (p > 0.05). (*) Light curing setting was not a significant factor (p > 0.05).
Composite/light curing setting*/location EvoPst EvoFlw PwrPst PwrFlw
LED- Top 57.1 (4.3) 65.5 (1.7)b 51.2 (1.5) 66.5 (1.7)b
Nrm Bottom 43.0 (2.0)a 58.7 (1.9)c 42.4 (2.6)a 60.1 (2.1)c
LED- Top 56.5 (3.1) 63.8 (1.9)d 51.7 (4.3) 61.6 (2.0)d,A
Pwr Bottom 42.7 (1.9) 57.4 (1.8)e 45.3 (2.3) 59.1 (2.1)e,A

Table 4 – Mean (standard deviation) of DC-R% values of each group. Two-way ANOVA followed by pairwise comparison
with Bonferroni correction was performed. Different lowercase letters in each row indicate significant difference between
composites (p < 0.05). (*) Light curing setting was not a significant factor (p > 0.05).
Composite/light curing settings* EvoPst EvoFlw PwrPst PwrFlw
a b a,b
LED-Nrm 75.6 (6.9) 89.7 (1.2) 82.8 (4.6) 90.4 (5.3)b
LED-Pwr 75.8 (6.0)c 90.1 (5.0)d 87.9 (6.9)d 96.1 (4.6)d

fill resin composite at the deep cavity floor in a composite

mold [26]. A noteworthy innovation in the new prototype OCT
system in this study was the usage of micro electro mechani-
cal systems (MEMS) in the laser source. The MEMS-controlled
system allowed great increase of scan speed and decrease
of motion artifacts [30,31], resulting in a real-time 3D inner
structural monitoring. The 2D cross-section scan and data
processing rate is 390 fps which produces 3 volumes per sec-
ond (vps) of the 3D dataset. The compact intraoral probe in
this system provides a field of view of 10 mm × 10 mm, opti-
Fig. 3 – Representative reconstructed XY plane MIP images mized to capture the whole surface of a single tooth in one
of the lower cavity area (3 × 3 × 1 mm3 ) from OCT 3D data volume. In addition to 2D cross-sectional and 3D previews,
just after light curing. White areas and bright pixel clusters the backscattered signal intensity is processed and projected
indicate internal defects. in a whole-volume enface preview window, allowing real-time
visualization of the formation, deformation and lateral prop-
agation of the internal and interfacial defects (Fig. 1).
show a significant effect on DC-R% (p = 0.08), and there was Shrinkage stress of the light-cured resin composite restora-
no significant interaction (p = 0.36). EvoPst showed the low- tions in a tooth can result in cusp displacement, interfacial gap
est DC-R% values (<80%), which were significantly lower than formation or tooth/restoration fracture [32,33]. Timing, mag-
all other composites (p < 0.005). PwrPst showed significantly nitude and distribution of these outcomes would be affected
lower DC-R% than PwrFlw (p < 0.05), while there was no differ- by external factors such as the configuration (C-factor), vol-
ence between the two flowables EvoFlw and PwrFlw (p = 0.99) ume, fracture toughness, compliance and adhesive quality of
(Table 4). the cavity substrates, besides the factors in the restorative
materials [22,34,35]. The current study approach simplified
comparison among tested resin composites and light curing
4. Discussion settings using a standard composite mold. Nevertheless, it
should be emphasized that these visual observations do not
A newly established nondestructive real-time internal visual- necessarily correspond to the results in the clinical situations.
ization and analysis method using OCT has been applied for The development and distribution of polymerization stress
interfacial adaptation evaluation in resin composite restora- depends on the system compliance and interfacial gap for-
tions [26,27]. Considering the limited OCT imaging depth due mation [26]. The flowable resin composite used to fabricate the
to near infrared light attenuation through anisotropic struc- simulated cavities in this study was chosen due to its favorable
ture of human dentin [29], in the current report, a modified scattering characteristics for OCT imaging of the cavity floor
OCT technique was applied for the internal evaluation of bulk-

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[26,36]. However, this type of composite has lower modulus of bulk-fill composites, rather than interfacial gaps or separation
elasticity compared to enamel and dentin, and would deflect from cavity walls. It appears that high intensity light deliv-
under the stress that could affect defect formation compared ery at the initial stage resulted in copolymerization between
to a preparation in human tooth [26,35,36]. the bulk-fill composite and the adhesive at the cavity floor
The null hypothesis was rejected since ID-A%, DC and interface, which resisted against separation during polymer-
DC-R% were different among groups. As shown in previous ization [37,48]. However, defect formation within the deepest
studies [37,38], mechanical properties and shrinkage strain of 1-mm of the composite suggest that the stress developed in
the light-initiated composites distribute non-uniformly due to the post-gel phase resulted in composite defect, and crack
the attenuation of light energy through depth. Because of the formation and propagation, particularly in the high viscosity
long light pathway of light through deep bulk-fill composites, composite group. In the post-gel phase, the composite loses
mechanical properties develop at different rates at various its viscous-elastic flow since the cross-linking of the poly-
depths. This discrepancy results in localized stress concen- mer chains within the resin composite increases modulus of
tration and development of internal fractures. In this regard, a elasticity and brittleness [49]. A previous report demonstrated
clear inverse trend was observed in this study between ID-A% faster increase of DC with higher irradiance at very early stage
and DC-R%, where the composite with the highest bottom/top of the light activation [21], which can be explained by the very
polymerization ratio showed the lowest internal defects and high generation rate of radicals and the initial decrease in
vice versa. In addition, polymerization with the power light viscosity with the temperature increases [50,51].
(LED-Pwr) at a higher rate tended to decrease the ID-A% to One concern for bulk-filled composite is light attenuation
some extent for all composites. through depth and insufficient DC at the depth. A previous
The paste-type conventional bulk-fill composite showed report demonstrated the lowest DC at 4 mm when high irradi-
the lowest DC-R% in this study. Regarding polymerization ance light (>2000 mW/cm2 ) and short exposure time (3 s) were
efficiency, the current results was consistent with previous employed, compared with other irradiance-exposure combi-
studies, which showed that the low-viscous bulk-fill compos- nations. [52]. The current study demonstrated that DC profiles
ites performed better than high-viscous bulk-fill composites within each composite was not significantly affected by the
[3]. The negative effects of high filler contents on DC could be light settings. This may result from the optimized wavelength
explained by increased attenuation by scattering [19], in addi- of the light source, photo-initiators composition and translu-
tion to the restricted mobility of the resin matrix. Formation cency of the used composites, which were provided by the
of localized nanogel particles in flowable composites prior to same manufacturer [53].
complete cross-linking is thought to be the reason for their There have been several approaches to delay the gel point
higher conversion rate [39,40]. Higher filler loaded composites by controlling free radical polymerization [54]. ␤-Allyl sulfone
have smaller interparticle spacing, which limits the gener- addition-fragmentation chain transfer (AFCT) has been intro-
ation of the nanogel particles [41]. In addition, these fillers duced as an effective agent for a change from the radical
obstruct mobility of reactive species the like monomers, short chain growth mechanism toward a step growth-like system
chain-segments and the nanogel particles [42]. [55,56]. In the presence of AFCT, the growing radical chain
The current study results showed enlargement of preex- is modified by forming an intermediate radical that under-
isting internal voids/micro-porosities during polymerization, goes fragmentation and forms a sulfonyl radical and a new
as suggested previously [43]. Larger ID-A% of both high vis- double bond, which results in shorter chain formation lead-
cous composites might be attributed to these voids, which ing to delayed gel point [53,55]. The expected AFCT function
were entrapped during the composite placements. The larger could have contributed the similar or larger DCbottom of the
ID-A% of paste-type composites can be explained by their PwrPst compared to EvoPst. In general, an incomplete con-
higher filler content. A previous study demonstrated that the version could decrease contraction stress [26]. The observed
stress level surrounding the filler particles increased in higher smaller DCtop in the PwrPst composite compared to EvoPst
filler fraction composites [44]. Coupling of the filler particles could potentially explain the smaller ID-A% in PwrPst. It was
and the matrix typically is mediated by covalent bonding of a suggested that the AFCT modulates the polymerization rate
silane molecule [7]. For well-bonded particles, the developed and results in a milder shrinkage stress development [12,55],
stress can be transferred to the particles from the matrix. How- this assumption is closely in line with the observations for the
ever, for poorly bonded filler particles, the increased stress PwrPst group in the current study. This also would contribute
can result in separation of the filler-matrix interface [45,46]. to slower loss of fracture toughness, which associate to crack
Such separation was described as a concern leading to loss propagation [57]. A recent study reported that the 3 s fast cur-
of mechanical properties such as wear resistance or stiffness, ing approach in the PwrPst induced comparable properties to
facilitating crack growth through the matrix [44,47]. the EvoPst, which is cured via free radical polymerization and
The current results suggest that the increased stress during has comparable chemical composition [58].
light polymerization in paste-type bulk-fill composites could The OCT method promotes visual and quantitative assess-
lead to internal crack development (Supplemental video). This ment of various factors, and reveals new clinically relevant
is an interesting finding in the new 3D imaging approach, information, which could not be noted by individual property
and in contrast to previous reports. Previous studies showed evaluation. Nevertheless, further data from various experi-
only interfacial gaps at the same configuration cavity floors ments including standard mechanical properties and bonding
in all tested light-cured bulk-fill materials polymerized by 40- tests are necessary to investigate the potential clinical benefits
seconds light at 600 mW/cm2 [26]. In the current study, the of these new products.
majority of IDs were observed as porosities or cracks in the

Please cite this article in press as: Hayashi J, et al. New bulk-fill composite system with high irradiance light polymerization: Integrity and degree
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