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Effect of air-drying dentin surfaces on dentin bond strength of a solvent-free


one-step adhesive

Article  in  Dental Materials Journal · July 2012


DOI: 10.4012/dmj.2012-034 · Source: PubMed

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Dental Materials Journal 2012; 31(4): 558–563

Effect of air-drying dentin surfaces on dentin bond strength of a solvent-free


one-step adhesive
Tomoyuki TAKAI 1, Keiichi HOSAKA 1, Keisuke KAMBARA 1, Suppason THITTHAWEERAT 1, Naoko MATSUI 1,
Masahiro TAKAHASHI 1, Ryuzo KISHIKAWA 1, Masatoshi NAKAJIMA 1, Masayuki OTSUKI 1, Richard M. FOXTON 2
and Junji TAGAMI 3
1
Cariology and Operative Dentistry, Oral Restitution Department, Graduate School of Medical and Dental Sciences, Tokyo Medical and Dental
University, 1-5-45 Yushima, Bunkyo-ku, Tokyo 113-8549, Japan
2
Department of Conservative Dentistry, King’s College London Dental Institute at Guy’s, King’s and St Thomas’ Hospitals, King’s College London,
London Bridge, London, SE1-9RT, UK
3
Cariology and Operative Dentistry, Oral Restitution Department, Graduate School of Medical and Dental Sciences, Tokyo Medical and Dental
University, Tokyo, Japan and Global Center of Excellence Program; International Research Center for Molecular Science in Tooth and Bone
Diseases, Tokyo Medical and Dental University
Corresponding author, Keiichi HOSAKA; E-mail: hosaka.ope@tmd.ac.jp

The purpose was to evaluate the effect of air-drying dentin surfaces on the microtensile bond strength (μTBS) of a solvent-free one-
step adhesive (Bond 1 SF). Twelve human molars were ground with 600-grit SiC paper. Before applying bonding agent, the dentin
surface was rinsed with distilled water and blot-dried with tissue paper, followed by air-drying for 0, 3, 30, and 60 s using with a
dental air syringe. After applying and curing Bond 1 SF, resin composite was incrementally built up. Specimens were then stored
in distilled water for 24 h and then μTBSs were measured at a cross-head speed of 1 mm/min. Higher μTBS were observed when
the dentin surface was air-dried for 3 s (33.2±6.8MPa)>0 s (26.7±4.5MPa)>30 s (22.6±5.5MPa)=60 s (20.4±5.0MPa). The results
suggested that prolonged air-drying of the dentin surface removed water and decreased the bond strengths of Bond 1 SF.

Keywords: Solvent-free, One-step self-etch adhesive, Microtensile bond strength, Dentin bonding, Air-drying

solvents in adhesives must be explained by their wide


INTRODUCTION
availability and good biocompativility1).
Dentin bonding systems for resin composite restorations Ideally, all solvents should be completely removed
have been widely used over the past few decades. The from the dentin surface prior to polymerization. One
latest advancement in adhesion technology is the clinical approach to obtaining stable dentin bonding
one-step self-etch adhesive system. One-step self- and relatively higher bond strengths is to employ warm
etch adhesive systems combine etching, priming, and air-drying of the adhesives4,5). However, complete
bonding into single procedure. Generally, one-step self- evaporation using with dental air syringe in clinical
etch adhesives consist of ionic resin monomers with situations is difficult to achieve and is dependent on the
phosphate or carboxylic functional groups, hydrophilic properties of the solvents6). As the solvents evaporates,
monomers (ex. HEMA), hydrophobic monomers (ex. Bis- the concentration of non-volatile monomers increases,
GMA, UDMA), solvents (water and organic solvents like which, in turn, decrease the vapor pressure of the
ethanol or acetone), fillers, and initiators. remaining solvents, making it impossible to evaporate
In adhesives, water, ethanol and acetone are the all the solvents under clinically relevant conditions7,8).
most commonly used as solvents. Water is an essential The residual contents of the solvents in the adhesives
solvent of one-step self-etch adhesives, which allows become a critically important factor in predicting the
them to generate the hydrogen ions required for effective bond integrity or the longevity of adhesive resins9-15),
dissolution and demineralization of tooth substrates. because residual solvents produce localized areas
The etching effect of a self-etch adhesive is related to of incomplete monomer polymerization, generating
the acidic functional monomers that interact with the porosities within the bonded interfaces that, in turn, may
mineral component of the tooth substrate, followed by permit inward diffusion of oral fluids11,16-18), lower the
simultaneous demineralization and resin penetration. conversion of monomers into polymers8) and increase the
A limited potential to dissolve the smear layer could water sorption, resulting in lower mechanical properties
impair the infiltration of functional monomers into of the adhesive polymers19) and hydrolysis of resin and
the underlying dentin, which would lead to a ‘weak’ collagen fibrils20, 21). Less stiff resin might lead to weaker
link in the adhesion mechanism to dentin1). In order bonding to dentin22).
to keep water in solution with other resin monomers, Current one-step self-etch adhesives contain HEMA
hydrophilic and hydrophobic resin monomers of one-step (2-hydroxyethyl methacrylate), which is a well-known
self-etch adhesives were dissolved in a relatively high co-monomer that prevents phase separation because
concentration of organic solvents2,3). The use of organic of its solvent-like nature23). Since HEMA acts as a

Received Jan 30, 2012: Accepted Mar 21, 2012


doi:10.4012/dmj.2012-034 JOI JST.JSTAGE/dmj/2012-034
Dent Mater J 2012; 31(4): 558–563 559

wetting agent for hydrophilic dentin24) and a diffusion curing unit (XL3000, 3M ESPE, Minnesota, USA) for
promoter for resin into the exposed collagen23,25), one- 10 s with a light output>600 mWcm-2. After curing the
step adhesives can achieve immediate bond strengths adhesive, a resin composite, Clearfil AP-X (Shade-A2,
to dentin, which are as high as those for two-step self- Kuraray Medical Corp., Tokyo, Japan) was built up
etch adhesives26), however, HEMA retains water in incrementally to a height of 5.0 mm to ensure sufficient
hydrogels, which is difficult to remove water by air- bulk for the microtensile bond test. Each increment was
drying. Moreover, the existence of HEMA contained light-cured for 20 s. The specimens were then stored
in one-step self-etch adhesives also makes it difficult to in distilled water at 37oC for 24 h. Following this, five
evaporate the solvents because HEMA lowers the vapor slices (0.7±0.1 mm thick) from each specimen were cut
pressure of solvents. perpendicular to the bonded interface using a low-speed
A unique one-step adhesive system, Bond 1 SF diamond saw (Isomet, Buehler Ltd., Illinois, US) under
(Pentron Clinical, California, USA) has been developed, water spray coolant. The adhesive-dentin interface was
which contains neither water nor organic solvents in trimmed into an hour-glass shape with a 1 mm2 cross-
the ingredients in order to eliminate technical issues sectional area (0.7 mm×1.4 mm), using a fine diamond
in terms of evaporation of solvents and concerns for bur (SF114, Shofu Inc., Kyoto, Japan) mounted in a
the durability of resin-dentin bond. The application of high-speed turbine handpiece under copious air-water
this “solvent-free” adhesive system does not require air- spray. The specimens were individually bonded to a jig
blowing with a dental air syringe and takes fewer steps. using a cyanoacrylate adhesive (Zapit, Dental Ventures
However, there is little information on its bonding of America, California, USA) mounted in a tabletop
performance. testing machine (EZ Test, Shimadzu Co., Kyoto, Japan)
The purpose of this study was to evaluate the effects and subjected to the microtensile bond strength (μTBS)
of air-drying of the dentin surfaces on the microtensile test at a crosshead speed of 1.0 mm/min according to the
bond strength (μTBS) of a solvent-free one-step adhesive method described by Sano et al.27). Fifteen slices obtained
system, Bond 1 SF, to dentin. The null hypothesis tested from the three bonded specimens in each test group
was that the duration of air-drying of the dentin surfaces were measured, and all data of μTBS were statistically
does not affect the bond strength of Bond 1 SF. analyzed by a one-way ANOVA to determine if there
were any statistically significant differences among
MATERIALS AND METHODS the air-drying groups. The Dunnett’s T3 test was used
for post-hoc multiple comparisons at the 95% level of
A solvent-free one-step adhesive system, Bond 1 SF confidence. After the microtensile bond test, the dentin
(Pentron Clinical, California, USA), was used in the sides of fractured specimens in each group were observed
current study. It is a one-bottle adhesive system, which using a stereomicroscope (Nikon SMZ 1000, Nikon Corp.,
consists of urethane dimethacrylate (UDMA), triethylene Kanagawa, Japan) at 120× magnification for failure
glycol dimethacrylate (TEGDMA), 2-hydroxyethyl mode characterization. Failure modes were classified
methacrylate (HEMA), 4-methacryloxyethyl trimellitic into four categories as follows: Cohesive failure in dentin
acid (4-MET), silane-treated bariumborosilicate glasses, (80–100% of the failure occurred in the underlying
silica with initiators, stabilizers and UV absorber, dentin); Interfacial failure (80–100% failure occurred
organic and/or inorganic pigments, opacifiers (Table 1). between resin and dentin); Cohesive failure in resin
This bonding system contains neither water nor any (80–100% of the failure occurred in the adhesive resin
organic solvents. and/or overlying composite); Mixed failure (interfacial
failure and cohesive failure in the adhesive resin and/or
Specimen preparation for the microtensile bond strength dentin). Failure modes were analyzed for statistically
(μTBS) test significant differences by the non-parametric Pearson
Twelve freshly extracted caries-free human molars were Chi-square test at the 95% level of confidence.
used in this study, according to the protocol approved by
the Human Research Ethics Committee, Tokyo Medical SEM observation of the treated surface
and Dental University, Japan. The occlusal enamel was The dentin surfaces treated with Bond 1 SF were
removed perpendicularly to the long axis of the tooth observed after the dentin surface was air-dried for each
by means of a model trimmer under running water to time interval. Flat dentin discs, approximately 1.5 mm
obtain superficial or mid-coronal dentin. The dentin thick, were cut perpendicular to the long axis of the
surfaces were abraded with 600-grit SiC paper. The teeth by means of a low-speed diamond saw (Isomet)
specimens were then divided into four groups (three from the mid-coronal part of human third molars. The
teeth for each group). Before applying the bonding dentin surfaces were prepared using a 600-grit SiC
agent, the dentin surface was rinsed with distilled water paper, and conditioned using the same procedure as
and blot-dried with tissue paper (Kimwipe, Kimberly- for μTBS measurement as described above. After each
Clark, Texas, USA), followed by air-drying for 0, 3, 30, drying method and application of the adhesive, the
60 s using a dental air syringe at a distance of 15 cm adhesive components were removed with a 50% acetone/
at air pressure of 3.8 kgf/cm2. The adhesive system water solution. All the specimens were then dehydrated
was applied to the dentin surfaces according to the in a series of solutions containing ascending grades of
manufacturer’s instructions and irradiated with a light- acetone (50%, 75%, 95%, and 100% for 30 min each),
560 Dent Mater J 2012; 31(4): 558–563

Table 1 Adhesive system tested in this study

Material Compositions Procedures Lot number

UDMA, TEGDMA, HEMA, 4-MET, silane-treated


Bond 1 SF Apply and spread evenly
bariumborosilicate glasses, silica with initiators,
(Pentron Clinical, and rub for 20 s/Light 3563739
stabilizers, ultraviolet light absorber, organic and/or
California, USA) cure for 10 s
inorganic pigments, opacifiers

Abbreviations: UDMA: Urethane Dimethacrylate; TEGDMA: Triethylene glycol dimethacrylate; HEMA: 2-hydroxyethyl
methacrylate; 4-MET: 4-methacryloxyethyl trimellitic acid.

Table 2 Microtensile bond strength of Bond 1 SF to dentin

Duration of air-drying 0 s (blot-dry) 3s 30 s 60 s

μTBS 26.7±4.5a 33.2±6.8b 22.6±5.5c 20.4±5.0c

Failure mode [0/5/2/8] [2/3/0/10] [0/8/0/7] [0/9/0/6]

Values are mean±SD in MPa. Different superscript letters indicate statistically significant differences (p<0.05). N=15 in
each group.
Failure mode: [cohesive failure in dentin/Interfacial failure/cohesive failure in resin/mix failure].
Cohesive failure in dentin=80–100% of the failure occurred in the underlying dentin. Interfacial failure=80–100% failure
occurred between resin and dentin. Mixed=interfacial failure and cohesive failure in the adhesive resin and/or dentin.
Cohesive failure in resin=80–100% of the failure occurred in the adhesive resin and/or overlying composite.

followed by immersion in hexamethyldisilazane, (CH3)3 removed after 3 s air-drying (Fig 1(b)), and that the
SiNHSi (CH3)3 (HMDS, Pierce, Rockford, Illinois, US) for smear layer partially remained on the dentin surfaces
10 min. After which time, the specimens were placed on after 30 s and 60 s air-drying (Figs. 1(c)–(d)).
a filter paper inside a covered glass vial and air-dried at
room temperature. They were then gold sputter-coated DISCUSSION
and observed with a scanning electron microscope (SEM,
JSM-5310LV, JEOL, Tokyo, Japan). Generally, one-step self-etch adhesives contain solvents
to act as transport media and modifiers of liquid
viscosity to allow resin monomer infiltration into the
RESULTS
demineralized dentin surfaces. The one-step self-etch
The results of the μTBS test are shown in Table 2. adhesives have been reported to exhibit relatively
One-way ANOVA indicated that the duration of air- low degrees of conversion28,29). Moreover, an excessive
drying the dentin surfaces affected the μTBS of Bond 1 SF solvent concentration in an adhesive can inhibit self-
(p<0.05). The higher bond strength was observed when polymerization30). One of the methods currently used to
dentin surface was air-dried for 3 s (33.2±6.8MPa)>0 evaporate solvents from adhesives has been air-drying
s (26.7±4.5 MPa)>30 s (22.6±5.5 MPa)=60 s (20.4±5.0 prior to light irradiation6,31,32). However, it is difficult to
MPa). There was no significant difference in μTBS completely evaporate the solvents.
between the 30 s and 60 s groups. In the 0 s air-drying The solvent-free one-step self-etch adhesive system,
group, all failures were observed except cohesive failure Bond 1 SF, has a unique concept. Since bond 1 SF
in dentin. The predominant failure mode in the 3 s air- does not require air-blowing procedure, it has fewer
drying group was a mixed failure, while the predominant application steps and may eliminate technical sensitivity
mode of failure in 30 s and 60 s air-drying groups was in terms of evaporation of the solvents.
interfacial failure. However, there were no significant This leads to the speculation on how does the
differences in failure modes between the experimental solvent-free one-step self-etch adhesive remove the
groups (p=0.052). The SEM observations of the treated smear layer and demineralize the dentin surface. Since
dentin surfaces are shown in Figs. 1(a)–(d). The treated Bond 1 SF does not contain water, some amount of water
surfaces showed that the smear layers were clearly (moisture) on the dentin surface must play an important
removed from the dentin surfaces after 0 s air-drying role. Thus, the effect of air-drying the dentin surfaces
(blot-dry) (Fig. 1(a)), that the smear layer was almost on the dentin bond strength of a solvent-free one-step
Dent Mater J 2012; 31(4): 558–563 561

(a) (b)

(c) (d)
Fig. 1 Representative SEM photographs of treated dentin surfaces after the application of Bond 1 SF with various dentin
air-drying conditions (×5,000).
(a) 0 s air-drying with dental air syringe (blot-drying); smear layer and smear plugs were completely removed off.
(b) 3 s air-drying with a dental air syringe; smear layer and plugs were almost removed.
(c) 30 s air-drying with a dental air syringe; smear layer and plugs partially remained.
(d) 60 s air-drying with a dental air syringe; smear layer and plugs partially remained.

adhesive was evaluated in this study. 3 s before applying Bond 1 SF, μTBS was significantly
The results of this study do not support the null higher than the 30 s or 60 s air-drying groups. According
hypothesis that the duration of air-drying the dentin to the SEM observations of the treated dentin surfaces,
surfaces does not affect the bond strength of Bond 1 SF. the smear layer was almost removed after 3 s air-drying,
The behavior of Bond 1 SF investigated in the present while the smear layer partially remained on the dentin
study varied when the duration of air-drying was surfaces after 30 s and 60 s air-drying. Since 30 s or 60
altered. Higher bond strengths were observed in the 3 s s air-drying removes water (moisture) from the dentin
group (33.2±6.8 MPa)>0 s (26.7±4.5 MPa)>30 s (22.6±5.5 surfaces, functional monomers would not be able to
MPa)=60 s (20.4±5.0 MPa). generate enough protons for the etching effect. However,
In this study, when the dentin surface was dried for 3 s air-drying could leave some water remaining on
562 Dent Mater J 2012; 31(4): 558–563

the dentin surface, resulting in removal of most of the one-step self-etch adhesives37). Further research on
smear layers. Functional monomers would be able to the effect of HEMA on durability of resin-dentin bond
generate protons and therefore an etching effect in the created by solvent-free one-step adhesive is therefore
3 s air-drying group. It is known that the amount of indicated.
smear layer removal is related to the pH value of acidic We propose that the procedure of drying the dentin
conditioners used6,22,25). Umino et al. reported that water surfaces is very important for optimum performance
is essential for one-step self-etch adhesives otherwise of the solvent-free one-step self-etch adhesive and is
the adhesive would not be able to remove the smear potentially technique sensitive. Based on the findings
layer effectively33). Regarding the failure mode, the of this study, it was clearly indicated that the presence
predominant failure mode in the 3 s air-drying group of moisture on the dentin surface was essential when a
was a mixed failure, while the predominant failure in 30 solvent-free one-step adhesive was applied. Therefore
s and 60 s air-drying groups was interfacial failure. Poor over-drying of dentin surface should be avoided. If there
penetration of bonding resin into the underlying dentin is insufficient moisture on the surface, the adhesive
may lead to poor hybrid layer formation in 30 s and 60 will not be able to remove the smear layer effectively.
s air-drying groups. From these results, it is speculated There would be poor penetration of the bonding resin
that over-drying the dentin surfaces should be avoided into the underlying dentin, which will result in poor
when using Bond 1 SF in order to etch dentin with water hybrid layer formation. Clinically, it is necessary to
present on the surface. maintain a wet dentin surface when this adhesive is
For the 0 s air-drying (blot-drying) group, the bond used. However, excessive water may interfere with
strength was significantly lower than that of 3 s air- polymerization of bonding resin, thereby resulting in
drying group although SEM observation revealed that poor bond strength34,35,38). Future studies will explore
the etching effect in the 0 s air-drying group was higher the long-term durability of resin-dentin bond created by
than in the 3 s air-drying group. SEM observation of solvent-free one-step self-etch adhesives.
the treated dentin surface showed that the 0 s air-drying Within the present study, the following conclusion
(blot-drying) group exhibited more complete removal of can be drawn: the duration of air-drying affected
the smear layer compared to other groups. However, microtensile bond strength of a solvent-free one-step
the presence of excessive water during polymerization of self-etch adhesive, Bond 1 SF; the results suggested
the adhesive has a detrimental effect on the hybrid layer that prolonged air-drying of the dentin surface removed
formation, since it lowers the mechanical properties water and decreased the bond strengths.
of the bonding resin20,21,34,35). Moreover, failure mode
analysis revealed that some specimens of 0 s air-drying ACKNOWLEDGMENT
group exhibited cohesive failure in resin.
Since Bond 1 SF does not require an air-blowing This study was supported by the grant from Ministry
step, the adhesive layer of Bond 1 SF would be relatively of Education, Culture, Sports, Science and Technology
thicker than other solvent-containing one-step self-etch of Japan, Global Center of Excellence (GCOE) Program,
adhesives which require air blowing. In general, solvent- “International Research Center for Molecular Science in
containing one-step adhesives should be thoroughly air- Tooth and Bone Diseases” and Grant-in-Aid for Young
blown to enable evaporation of the solvents, which makes Scientists (B) (#23792165) from Ministry of Education,
the bonding layer thinner. Thinner adhesive layers Culture, Sports, Science and Technology of Japan. We
may suffer from incomplete polymerization due to the thank Pentron Japan Inc. for providing the commercial
existence of oxygen36). Oxygen inhibits the free radical adhesive.
polymerization, resulting in a layer of not or partially
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