506 Effect of resin coating in Class Ⅱ Dental

cavities Materials Journal 26

（4）
: 506－513, 2007

Effect of Resin Coating on Dentin Bonding of Resin Cement in Class II Cavities

Shamim SULTANA1, Toru NIKAIDO1, Khairul MATIN1,2, Miwako OGATA1, Richard M. FOXTON3 and Junji
TAGAMI1,2
1
Cariology and Operative Dentistry, Department of Restorative Sciences, Graduate School, Tokyo Medical and Dental
University, 5-45 Yushima 1-chome, Bunkyo-ku, Tokyo 113-8549, Japan
2
Center of Excellence Program for Frontier Research on Molecular Destruction and Reconstruction of Tooth and Bone,
Tokyo Medical and Dental University, 5-45 Yushima 1-chome, Bunkyo-ku, Tokyo 113-8549, Japan
3
King’s College London Dental Institute at Guy’s, King’s College and St. Thomas’ Hospitals, London, UK
Corresponding author, Toru NIKAIDO; E-mail: nikaido.ope@tmd.ac.jp

Received August 18, 2006/Accepted February 24, 2007

This study was designed to evaluate the efficacy of resin coating on the regional microtensile bond strength (MTBS) of a
resin cement to the dentin walls of Class II cavities. Twenty mesio-occlusal cavities were prepared in human molars. In 10
cavities, a resin coating consisting of a self-etching primer bonding system, Clearfil SE Bond, and a low-viscosity microfilled
resin, Protect Liner F, was applied. The other 10 teeth served as a non-coating group. After impression taking and
temporization, they were kept in water for one day. Composite inlays were then cemented with a dual-cure resin cement,
Panavia F 2.0, and stored in water for one day. Thereafter, MTBSs were measured. Two-way ANOVA (p＝0.05) revealed
that the MTBS of resin cement to dentin was influenced by resin coating, but not by regional difference. In conclusion,
application of a resin coating to the dentin surface significantly improved the MTBS in indirect restorations.

Keywords: Regional bond strength, Indirect restoration, Dual-cure resin cement

Dentin moisture, as well as regional difference,

INTRODUCTION
The indirect fabrication of composites is widely used
not only for the esthetic treatment of posterior and
anterior teeth, but also to conserve tooth structure
in the case of large defects. Direct composite
restorations are preferred to indirect composite
restorations because they require only minimal
intervention during cavity preparation ― even in
posterior restorations1) . However, polymerization
shrinkage of direct composites under confined
conditions generates stress at the tooth-restoration
interface, which may lead to gap formation,
postoperative sensitivity, and secondary caries2) .
Unfortunately, current resin cements do not always
provide good bonding performance to dentin
compared with dentin bonding systems for direct
resin composites3).
To overcome the lackluster bonding performance
to dentin, a resin coating technique was developed in
the early 1990s. In this technique, a hybrid layer
and a tight sealing film are produced on the dentin
surface with a dentin bonding system and a low-
viscosity microfilled resin3-5). It enables coverage and
protection of the prepared dentin immediately after
cavity preparation. Therefore, this technique has
the potential to minimize pulp irritation and
postoperative sensitivity6,7) . Further, a resin coating
can provide a resin cement with high dentin bond
strength3-5,8) and good interfacial adaptation of
composite inlays9). Therefore, the resin coating
technique is a key to achieving minimal intervention
with indirect resin composites10).
are important factors that may affect dentin
bonding11,12) . The bond strength of the cavity floor
dentin of Class I13,14) and Class II15) restorations have
been evaluated in direct composite restorations.
There have also been some studies on the relationship
between resin coating and resin cement bond
strength3,8,16-18). However, there is little information on
the regional bond strength of resin cement to resin-
coated dentin. Therefore, the purpose of this study
was to evaluate the efficacy of a resin coating on the
regional (i.e., occlusal and proximal) microtensile
bond strength (MTBS) of a resin cement to the
dentin walls of Class II (MO) cavities.
MATERIALS AND METHODS
Specimen preparation
Specimen preparation is illustrated in Fig. 1. Twenty
non-carious human third molars were used for this
study. Mesio-occlusal (MO) cavities with slightly
rounded internal line angles were prepared using a
regular-grit diamond bur (207CR, Shofu, Kyoto,
Japan), and cavity surfaces were finished with a
superfine diamond bur (SF 207 CR, Shofu) mounted
in an air turbine handpiece under water coolant.
Dimensions of the occlusal cavities were approxi-
mately 4 mm wide and 2.5 mm high. The mesial
gingival margin of the proximal cavity was located
1.5 mm above the cementoenamel junction. Height of
the proximal cavities depended on the crown height.
The prepared teeth were randomly divided into
two groups. For one group, the cavities were coated
 SULTANA et al. 507

Fig. 1 Specimen preparation for microtensile bond strength test.

Table 1 Materials, batch numbers, and compositions

Material Batch No. Components
Dentin bonding system
Clearfil SE Bond 00565B Primer: MDP, HEMA, hydrophilic dimethacrylates,
water, photoinitiator
Bond: MDP, HEMA, Bis-GMA, photoinitiator,
microfiller, functional monomer

Low-viscosity microfilled resin

Protect Liner F 0060A Bis-GMA, TEGDMA, microfillers, photoinitiator

Indirect resin composite

Estenia (DA3) 00239A Hydrophobic methacrylates, 92 wt％ (82 vol％) fillers.
Ultra-fine fillers (0.02 μm particle size) loaded into a
microfilled (2 μm particle size) resin matrix.

Resin cement
Panavia F 2.0 011120 ED primer II:
Primer A ― MDP, HEMA, chemical initiator, water,
5-NMSA
Primer B ― 5-NMSA, chemical initiator, water

Panavia F 2.0:
A Paste ― Quartz glass, microfiller, MDP,
methacrylate, photoinitiator
B Paste ― Barium glass, NaF, methacrylates,
chemical initiator
All materials were manufactured by Kuraray Medical Inc., Tokyo, Japan.
MDP＝10-methacryloxydecyl dihydrogen phosphate; HEMA＝2-hydroxyethyl methacrylate; Bis-GMA＝bisphenol
A diglycidymethacrylate; TEGDMA＝triethylene glycol dimethacrylate; 5-NMSA＝N-methacryloyl 5-aminosalicylic
acid; NaF＝Sodium fluoride
508 Effect of resin coating in Class Ⅱ cavities
with a combination of a self-etching primer bonding
system, Clearfil SE Bond (Kuraray Medical, Tokyo,
Japan), and a low-viscosity microfilled resin, Protect
Liner F (Kuraray Medical). Table 1 lists the batch
numbers and compositions of the materials used.
According to the manufacturer’s instructions, SE
Primer was first applied to the cavity for 20 seconds
and gently air-dried. SE Bond was then applied,
mildly air-dried, and light-cured for 10 seconds using
a conventional halogen light curing unit (XL 3000,
3M ESPE, Seefeld, Germany). Thereafter, Protect
Liner F was placed on the cured adhesive surface
using a brush-on technique and light-cured for 20
seconds. The other 10 cavities remained as a Non-
Coated group. After cavity preparation, the roots of
all the teeth were embedded in a silicon impression
material (Exafine Putty Type, GC, Tokyo, Japan).
Impression of each cavity was taken using a
combination of an agar (Aromaloid, GC) and an
irreversible hydrocolloid (Aroma Fine DFII, GC). The
impression was then cast in a Type III stone (Zo
Gypsum, GC). After impression taking, the cavities
were temporized with a water-setting temporary
filling material (Cavit-G, 3M ESPE) and stored in
water at 37℃ for 24 hours. Composite inlays were
fabricated on the working casts using an indirect
resin composite (Estenia, Kuraray Medical) according
to the manufacturer’s instructions. The inlays were
polymerized with a halogen light curing unit (Alpha
Light II, J. Morita, Kyoto, Japan) for three minutes,
and then heat-cured at 110 ℃ in an oven (KL-100,
Kuraray Medical) for 15 minutes.
The temporary filling material was removed with
a spoon excavator, and the cavity cleaned with an
alcohol-soaked cotton pellet for 10 seconds.
Following this, trial insertion of the composite inlays
prior to cementation was performed to check their
fit. An etchant of 37％ phosphoric acid gel (K-
etchant, Kuraray Medical) was applied to the fitting
surface of the inlay for 10 seconds, rinsed, and
gently air-dried. The inlay was then silanized using
a mixture of Clearfil SE Bond Primer and Porcelain
Bond Activator (Kuraray Medical) applied to the
surface of the inlay for five seconds and mildly
air-dried. Before cementation, the cavity surface of
the non-coating group was treated with ED Primer
II (Kuraray Medical) for 30 seconds and gently
air-dried.
Next, the resin-coated surface was treated with
37％ phosphoric acid gel (K-etchant) for 10 seconds,
rinsed, and dried to remove any debris on the
surface. A mixture of ED Primer II was then
applied for five seconds and gently air-dried.
To simulate the interproximal contact area, an
adjacent tooth was used during light curing. For
cementation, equal amounts of the two pastes of a
dual-cure resin cement (Panavia F 2.0, Kuraray
Medical) were mixed together and placed on the
fitting surface of the inlays. The inlays were seated
in the cavities using hand pressure. After removal
of any excess cement, the cement was exposed to
light (XL 3000, 3M ESPE) from the occlusal, buccal,
and lingual directions for 20 seconds each. After
cementation, the margins of the restorations were
finished with a superfine diamond bur (SF207CR,
Shofu) and then stored in water at 37℃ for 24 hours.
Microtensile bond strength test
The occlusal and proximal surfaces of each specimen
were ground with a carborundum point (2 HP, Shofu)
for additional resin composite build-up. Ground
surface of the inlay was treated with 37％ phosphoric
acid gel (K-etchant) for 10 seconds, rinsed, and gently
air-dried. A mixture of SE Primer and Porcelain
Bond Activator was then applied for five seconds and
mildly air-dried. SE Bond was then applied, gently
air-dried, and light-cured for 10 seconds. A resin
composite (Clearfil AP-X, Kuraray Medical) was built
up to a height of 3 mm in two increments. Each
increment was light-cured for 20 seconds (XL 3000).
Each specimen was sectioned perpendicular to the
bonded interface occlusally or proximally to obtain
a thickness of 0.7 mm. Occlusal and proximal slabs
were obtained from different restorations.
Eventually, 4−5 occlusal slabs or 3−4 proximal slabs
were obtained from one specimen. Each slab was
trimmed and shaped along the adhesive interface
with a superfine diamond bur (V16ff, GC) to obtain
an hourglass shape. The proximal box was discarded
to get the occlusal slab, while the first cut slab was
discarded due to its irregular shape. The narrowest
portion at the adhesive interface was then trimmed
to approximately 1 mm2 for the MTBS test. Width
and thickness were then measured with digital
calipers to calculate the bonded surface area.
Each specimen was attached to a Bencor Multi-
Testing apparatus (Danville Engineering, San Ramon,
CA, USA) with cyanoacrylate adhesive (Zapit, Dental
Ventures of America, Corona, CA, USA) and placed
in a benchtop material tester (EZ Test, Shimadzu,
Kyoto, Japan) for MTBS test at a crosshead speed of
1.0 mm/min. Number of samples in each group was
11. Data were statistically analyzed using two-way
ANOVA at a 5％ level of significance.
Scanning electron microscopic (SEM) observation
After MTBS testing, the fractured specimens were
fixed in 10％ neutral buffer formalin. Both the
dentin and composite sides of the fractured samples
were desiccated, gold sputter-coated, and observed
with a SEM (JSM-5310LV, JEOL, Tokyo, Japan) to
confirm the fracture mode.
Fracture mode was classified into one of the
following four categories ― A: Partial adhesive
 SULTANA et al. 509

failure, where remnants of resin cement remained on Table 2 Microtensile bond strengths (MPa) to human
the dentin surface; B: Cohesive failure within resin dentin and modes of fracture
cement; C: Complete and partial adhesive failure Occlusal Proximal
including cohesive failure of the resin cement at resin
Non-coating 17.9 (3.1)a 16.7 (3.7)a
coating-resin cement interface; D: Partial adhesive
failure at resin coating-resin cement interface where AB AB
b b
remnants of resin cement remained on the coating Resin coating 25.7 (5.2) 24.8 (6.7)
surface. BCD BCD
To examine the dentin-composite interface, three Number of specimens＝11.
bonded specimens were prepared for each group in Four modes of fracture ― A: partial adhesive failure,
the same manner as described in the sample where remnants of resin cement remained on the
preparation for MTBS testing. The specimens were dentin surface; B: cohesive failure within resin cement;
stored in water at 37℃ for 24 hours. Bonded C: complete and partial adhesive failure including
assemblies were then sectioned into two halves using cohesive failure of the resin coating-resin cement
a low-speed diamond saw microtome (Isomet, interface; D: partial adhesive failure at resin coating-
resin cement interface where remnants of resin cement
Buehler, Lake Bluff, IL, USA) and embedded in a remained on the coating surface.
self-curing epoxy resin (Epon 815, Nissin EM, Tokyo, Same superscript letters among MTBS values repre-
Japan). The specimens were subsequently polished sent no significant differences (p>0.05.).
with silicon carbide papers under running water, and
polished to high gloss with abrasive disks and
diamond pastes of decreasing abrasiveness down to
0.25 μm. At each step, the specimens were cleaned
ultrasonically. Polished specimens were subjected to
argon ion beam etching (EIS-1E, Elionix, Tokyo,
Japan) for five minutes at 0.2 mA and 1 kV to
disclose the interfacial structure, and then gold
sputter-coated.

RESULTS
Microtensile bond strengths and fracture modes
Microtensile bond strengths and their fracture modes
are summarized in Table 2. Two-way ANOVA
revealed that the MTBSs of resin cement to the
dentin walls of Class II cavities were influenced by
resin coating (F＝29.22, p＝.0001), but not by dentin
region (F＝0.467, p＝0.499). There was no interaction
between resin coating and dentin region (F＝0.009,
p＝0.927). Indeed, the resin coating group provided
statistically higher MTBSs to dentin than those of
the non-coating group (p<0.05). Some specimens
debonded during trimming for MTBS testing in the
non-coating group, which were discarded from the
calculation. However, no specimens debonded in the
resin coating group.
Figure 2 shows the SEM views of typical frac-
ture modes for the coating and non-coating groups.
For the non-coating group, the fracture mode was
mainly partial adhesive failure (category A). In the
resin coating group, the key fracture mode was
Fig. 2 Representative scanning electron micrographs of
complete and partial adhesive failure including the fractured surface on the dentin side after
cohesive failure of the resin cement at the resin microtensile bond strength test. (a) Non-coating
coating-resin cement interface (category C). group: Partial adhesive failure where remnants of
resin cement (CE) remained on the dentin (D) sur-
SEM observation of the interface face. (b) Resin-coating group: Complete and par-
tial adhesive failure including cohesive failure of
Figure 3 shows the SEM views of the dentin-
the resin cement remaining at the resin coating
composite interface. The SEM pictures revealed good (RC)-resin cement interface.
510 Effect of resin coating in Class Ⅱ cavities

Fig. 3 Scanning electron micrographs of the interface between the indirect composite and dentin with and
without resin coating (RC: Resin coating, CE: Resin cement, D: Dentin, H: Hybrid layer). In the resin
coating group, good bonding was observed at the interface between the indirect composite and resin-
coated dentin. Thickness of the hybrid layer was approximately 0.5 μm on both occlusal surface (a)
and proximal surface (b).
In the non-coating group, thickness of the hybrid layer was approximately 0.5 μm on both occlusal
surface (c) and proximal surface (d).

bonding at the interface between indirect resin
composite and dentin in both the resin-coated and
non-coated specimens. However, in some non-coated
specimens, some gaps were observed at the interface ―
probably due to poor bonding.
The hybrid layer was observed at the interface in
every specimen. Thickness of the hybrid layer in
resin-coated dentin was approximately 0.5 μm on
both the occlusal (a) and proximal (b) sides. In the
non-coating group, thickness of the hybrid layer was
also 0.5 μm on both the occlusal (c) and proximal (d)
sides.
DISCUSSION
When pitted against conventional cements, resin
cements wield some advantages ― such as
micromechanical bonding to tooth structure, low
solubility19), and better wear resistance20). Successful
adhesion of the resin cement is very important for
the longevity of indirect restorations 21). However, the
bond strength of resin cements is still lower than
that of adhesive systems for direct composites2,16) .
With indirect restorations, contamination of the
prepared dentin surfaces with temporary filling
materials22), blood, and saliva may also further
deteriorate dentin bonding capacity23,24).
Previous studies have shown that the bond
strength of resin cements to dentin could be
successfully improved by a resin coating technique
using a combination of an adhesive system and a
low-viscosity microfilled resin16,17). This technique can
also protect the pulp and reduce postoperative
sensitivity 6,7) in vital teeth, as well as reduce coronal
leakage in endodontically treated teeth 25). To improve
the bond strength of resin cements to dentin, careful
and discerning selection of resin coating material and
adhesive system is very important. On this account,
 SULTANA et al.
low-viscosity microfilled resin seems to be an
expedient choice on two fronts. It can protect the
underlying adhesive, and at the same time promote
polymerization of the adhesive because of two-
pronged effects: double-cure action of the adhesive as
well as air inhibition on top of the adhesive, thereby
resulting in increased bond strength5) . It has been
shown that if the correct combination of adhesive
and low-viscosity microfilled resin were selected, good
bonding of the resin cement to dentin can be
obtained for indirect restorations17) ― to the extent of
being almost identical to the bond strength of direct
composite restorations. A two-step self-etching
primer bonding system, Clearfil SE Bond, and a low-
viscosity microfilled resin, Protect Liner F, were used
in this study. This combination was selected because
it demonstrated the highest bond strength in a
previous study 17).
It is difficult to evaluate regional bond strength
in Class II cavities by conventional testing methods,
chiefly because of the relatively large adhesive area
needed. However, microtensile bond strength test26)
enables us to evaluate regional bond strengths in the
same tooth. Previous studies have demonstrated that
microtensile bond strength is influenced by several
clinical factors, such as bonding technique27) , cavity
configuration factor (C-factor)13) , remaining dentin
thickness, dentin permeability, and also the age and
depth of dentin28). Contamination from saliva, blood,
temporary filling materials, and impression materials
also affects the adhesion of indirect restorations.
Smear layers produced with a regular diamond
bur were found to be more acid-resistant than those
produced by superfine diamond burs, thereby
influencing the dentin bonding of a two-step self-
etching primer bonding system29) . In light of this
finding29) , cavities in the present study were finished
with a superfine diamond bur.
From our results, it was shown that the bond
strength of resin cement to dentin was influenced by
the material, but not by region. Similarly, Zheng et
al.30) reported that the bond strengths of different
regions (pulp horn, center, and periphery) to dentin
were influenced by the material and pulpal pressure,
but not by region. In a study by Bouillaguet
et al. 15), they compared the regional (occlusal, axial,
gingival) resin-dentin bond strengths to MOD cavities
versus the same surfaces isolated by cutting away all
but the test surface. They reported that the mean
bond strengths in the cavity bonding group were
significantly lower than those of the flat bonding
surface group. However, there were no significant,
consistent differences among the various regions
within either group. On the other hand, it was also
reported that regional differences were found in
resin-dentin bond strengths, which were probably
related more to operator variability than to material
511
differences31) . Bond strength varies across a dentin
surface, and the magnitude of variability can be
influenced by the bonding technique15).
The C-factor is the ratio of bonded surface area
to unbonded or free surface area32) . Since the C-
factor of a complex MO cavity is higher than that of
a flat bonding surface 13), high polymerization stress
maybe present during cementation. The resin coat-
ing could have thus acted as a stress absorber33) and
reduced the polymerization shrinkage stress at the
interface.
Materials for temporization and impression
taking influence the bond strength of resin cements
to the surface of resin-coated cavities. Previous
studies have demonstrated that a water-setting
material, such as Cavit-G (3M ESPE, Seefeld,
Germany), was an optimal material for temporiza-
tion, while resin-based temporary filling materials
reduced bond strength due to contamination of the
coating surface18,22) . As for impression taking of
resin-coated surfaces, hydrocolloid impression materi-
als are recommended. When addition-cured silicon
impression materials are used for resin-coated
surfaces, the air-inhibited unpolymerized surface
layer should be removed with an alcohol-soaked
cotton pellet prior to impression taking34).
Hybridization of the intertubular dentin is an
essential mechanism of dentin bonding 35). In the case
of directly placed resin composites, adhesion to
dentin occurs by the formation of a hybrid layer35) ―
the same as with indirect restorations36). As for the
thickness of the hybrid layer with resin coating, it
depends on the adhesive system used in combination
with the resin cement17) . SE Primer contains an
acidic monomer, MDP, which solubilizes the smear
layer and demineralizes the underlying dentin, as a
result of mild surface etching9) . ED Primer II also
contains MDP, which plays the same role as in SE
Primer. In the present study, thickness of the
hybrid layer in both resin coating and non-coating
groups was approximately 0.5 μm ― which was due
to mild surface etching. With these self-etching
primer systems, smear plugs partially remain on the
treated dentin as a result of incomplete formation of
resin tags in the dentinal tubules.
This study showed that the resin coating
technique evidently improved the microtensile bond
strength of resin cement to the walls of Class II
cavities. This achievement is essential for the
prevention of microleakage and secondary caries. A
gap-free interface between the restoration and cavity
wall is undisputedly necessary for good clinical
longevity of restorations. On this note, application
of a resin coating on prepared cavities can reduce
interfacial gap formation between composite inlays
and the cavity surface22). At this juncture, it should
be highlighted that resin coating has been shown to
512 Effect of resin coating in Class Ⅱ cavities
improve dentin bonding of resin cements, whereas no
effect was observed on enamel bonding37) . With the
enamel surface, no significant statistical differences
in bond strength were observed with or without the
use of a low-viscosity microfilled resin. Further, the
bonding performance of indirect restorations to
enamel was clinically acceptable, which was almost
identical to that achieved with direct resin composite
restorations.
In view of the current, vigorous promotion of
minimal intervention dentistry, the resin coating
technique can indeed achieve this objective when an
indirect restoration is indicated. However, complete
and partial adhesive failure including cohesive failure
of the resin cement at the resin coating-resin cement
interface (category C) was the key fracture mode
observed in the resin coating group. This finding
suggested that the joint interface was the weak link
in indirect composite restorations. In light of this
finding, there is an imperative need for better,
enhanced bond strength at the interface.
Nonetheless, this need can currently be met by the
resin coating technique, whereby the resin coating
material can protect the prepared dentin from
chemical, physical, and biological insults38).
CONCLUSIONS
Within the limitations of the present study, the fol-
lowing conclusions were drawn:
1. Application of a resin coating ― using a combi-
nation of Clearfil SE Bond and Protect Liner F
― to the dentin surface following cavity prepa-
ration significantly improved the microtensile
bond strength of Panavia F to dentin in indirect
Class II restorations.
2. No regional differences in microtensile bond
strength between the occlusal and proximal
dentin surfaces were observed.
ACKNOWLEDGEMENTS
The authors are grateful to Dr Md. Asafujjoha for
his co-operation in this study, and to Mr. Ikeda for
the statistical consultation sessions. This work was
supported by the Center of Excellence (COE) Program
for Frontier Research on Molecular Destruction and
Reconstruction of Tooth and Bone at Tokyo Medical
and Dental University, Tokyo, Japan.
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