Dental Materials Journal 2013; 32(3): 468–475

Micro-shear bond strength of adhesive resins to enamel at different relative

humidity conditions
Andaç Barkın BAVBEK1, Erhan DEMIR1, Barış GOKTAS1, Betül OZCOPUR2, Benin BEHRAM1,
Gürcan ESKITASCIOGLU1 and Mutlu ÖZCAN3

1
Department of Prosthodontics, Faculty of Dentistry, University of Yüzüncü Yıl, 65080 Kampus, Van, Turkey
2
Department of Endodontics, Faculty of Dentistry, University of Yüzüncü Yıl, 65080 Kampus, Van, Turkey
3
Dental Materials Unit, Center for Dental and Oral Medicine, Clinic for Fixed and Removable Prosthodontics and Dental Materials Science, University
of Zürich, Plattenstrasse 11, CH-8032 Zürich, Switzerland
Corresponding author, Andaç Barkın BAVBEK; E-mail: bavbekab@yahoo.com

This study tested whether exhaled humid conditions would affect the adhesion of etch-and-rinse, two-step and one-step self-etch
adhesive resins to enamel. Enamel surfaces of human maxillary anterior teeth (N=240, n=20) were exposed to four humid conditions
(H1: 63–68%, H2: 73–78%, H3: 93–98%, H4: 36–45% RH) during bonding with Adper Single Bond 2 (SB2), Clearfil SE Bond (CSE)
and Adper Easy Bond (AEB). Specimens were stored in distilled water at 37ºC for 24 h and tested to failure using micro-shear bond
strength (μSBS) test. Data were analyzed using two-way ANOVA and Tukey’s test (p<0.05). The μSBS to enamel with SB2, CSE
and AEB was not significantly affected by humidity parameters. AEB resulted in significantly lower μSBS in all conditions. The
frequency of adhesive failures was the highest at H2, H3 for SB2, H3 for CSE and H1-4 for AEB indicating that humidity conditions
may decrease adhesion quality to enamel.

Keywords: Adhesion, Micro-shear bond strength, Relative humidity, Self-etch adhesive resin, Total-etch system

factor becomes an important issue8). While considering

INTRODUCTION
Various factors such as chemical composition of the
adhesive resin, polymerization protocol, oxygen and
moisture degree can influence the adhesion quality at
the resin-adhesive-tooth interface1). Wet enamel surfaces
are frequently encountered prior to the application of
bonding agents on demineralized surfaces. Presence of
humidity at the bonding area is one of the challenging
situations in adhesive dentistry. Previous studies
indicated that keeping saliva away from the bonding
surface or to obtain a dry enamel surface by eliminating
remnant water prior to adhesive application are crucial
precautions to to take for long-term bond durability2,3).
Several in vitro studies had investigated the bond
strength between resin-enamel interfaces and concluded
that by prevention of saliva on the enamel surface or
similar water contamination, ideal dry enamel surfaces
could be achieved4-6).
In vitro studies are very popular and beneficial
experimental designs that give the examiners the
opportunity to test different situations that cannot be
tested in vivo. Delong and Douglas7) summarized the
obligations to simulate an artificial oral environment.
According to their considerations, an artificial oral
environment may be set up, if the mastication
function, saliva secretion and temperature, aeration,
and humidity conditions were provided. Specifically,
when the percentage of relative humidity (RH) in oral
environment (about 78–94%) is taken into account, this
Color figures can be viewed in the online issue, which is avail-
able at J-STAGE.
Received Jul 31, 2012: Accepted Feb 21, 2013
doi:10.4012/dmj.2012-200 JOI JST.JSTAGE/dmj/2012-200
the source of the humidity in oral environment, air that is
exhaled through the mouth, had always been overlooked.
The amount of water saturated in the exhaled air is
reported to be about 27 mg/dm3 and its possible effects
on dental practice requires careful evaluation9). Although
rubber dam can be used in routine in order to isolate the
adhesive surface from the oral environment, its use could
be restricted during luting laminate veneers and crowns
with subgingival margins, operating in Class V lesions,
bonding brackets in the posterior area or in many other
chair-side conservative applications. In such situations,
bonding surfaces may be more prone to contaminate
with the exhaled air. Unfortunately, most of the in vitro
studies on bond strength tests were designed without
considering the effect of humidity and there is a common
consensus about the dissimilarity of the results of in
vivo and in vitro studies regarding to the bond strength
values10-12). Hajrassie and Khier11) showed that in vivo
bond strength of orthodontic brackets bonded to enamel
were significantly less than those measured in in vitro
conditions. Consequently, they argued that the accepted
experimental environment does not exactly simulate the
oral environment. The efforts of researchers to simulate
the in vivo conditions cannot be denied13-15). Yet, in many
studies, the possible effect of oral humidity on the bond
strength of the composite resin to tooth structure has
been neglected.
Considering the application steps, the adhesive
resin types in dentistry can be classified as etch-and-
rinse and self-etch systems. These systems were further
modified to shorten the chair-side time for the clinician
 Dent Mater J 2013; 32(3): 468–475 469

by introducing one-step and two-step self-etch adhesive under water.

systems to the market. Such adhesive resins require
either combined or separate application of the primer
and adhesive resin solutions, respectively16). Although
the technological improvements in adhesive resins ease
the clinical process in many ways, they should be applied
in dry conditions.
The objectives of this study therefore were to
evaluate the effect of oral humidity on micro-shear
bond strength (μSBS) of adhesive resins to enamel with
three different adhesive systems. The null hypothesis
tested was that increased percentage of RH conditions
simulating the oral environment would not affect the
bond strength of the adhesive resins to enamel.
MATERIALS AND METHODS
Specimen preparation —Establishment of humid
conditions
Sound human maxillary incisors, extracted due to
periodontal reasons (N=240) within 6-month period
were used in this study. After soft tissue remnants were
eliminated, teeth were stored in distilled water for 2
more weeks at room temperature. Roots were resected
1 mm above the cemento-enamel junction and crowns
were embedded in auto-polymerized acrylic resin
(Akribel, Atlas-Enta AS, İzmir, Turkey). The exposed
labial enamel surfaces localized on the acrylic resin
were flattened using a slow speed saw (IsoMet 1000,
Buehler Ltd, Lake Bluff, Illinois, USA) under water-
cooling. The enamel surfaces were further ground
finished using 600- and 800-grit silicone carbide papers
Humidity conditions were established in an
ultrasonic nebulizer (Medi-nem SDT-15, Medineks
Medical Education Materials Ltd., İstanbul, Turkey)
in a laminar flow chamber (LN090/120, Nuve, Ankara,
Turkey). The humid air was blown into the cabinet from
the mouthpiece of the nebulizer and a suction system
surrounded the inner walls collecting the humid air
continuously in order to maintain the humidity level
inside the cabinet. The humidity of the blown air was
quantified with a hygrometer (Trotec T200, Trotec
GmbH & Co. KG, Heinsberg, Germany) and inside the
cabinet the RH levels were changed by adjusting the
distance from the mouthpiece of nebulizer: the further
from the mouthpiece, the lower the RH. Three different
RH conditions were achieved namely, 63–68% (H1),
73–78% (H2), 93–98% (H3) to which the specimens
exposed8). The distances from the mouthpiece of the
nebulizer to the H1, H2 and H3 were; 34 cm, 30 cm and
25 cm, respectively (Fig. 1). While three of the humid
conditions were achieved in laminar flow chamber, one
group was treated in laboratory conditions (H4) serving
as the control group. The RH level of H4 was measured
between 36–45% by the hygrometer.
Specimens were randomly divided into four
groups (n=60 per humidity group). In each group, four
subgroups (n=20) were established depending on the
adhesive resins used. Materials used, their chemical
compositions, manufacturers and application procedures
are listed in Table 1.
Group SB2: After etching enamel surfaces with 36%
H3PO4, specimens were exposed to humidity conditions

Fig. 1 Schematic drawing of the laminar flow chamber where extended RH conditions
was established using a nebulizer at 30°C (Relative humidity of H1: 63–68%,
H2: 73–78%, H3: 93–98% and laboratory humidity condition, H4: 36–45%).
470 Dent Mater J 2013; 32(3): 468–475

Table 1 The type, brand, chemical composition, batch numbers and application protocols of the materials used for
the experiments

Manufacturer and
Type Brand, Abbreviation, Chemical Composition Application Protocol
Batch Numbers

One-bottle Adper Single Bond 2 (SB2) 3M ESPE, Applied two layers for 15 s.
Total-etch Bis-GMA, HEMA, dimethacrylates, polyalkenoic acid St. Paul, USA Gently air-thin each layer
adhesive copolymer, initiators, water and ethanol Batch no: 9XE for 5 s.

Clearfil SE Bond (CSE)

Apply primer for 20 s.
Primer: MDP, HEMA, Hydrophilic dimethacrylate,
Two-step Kuraray Noritake Dry with mild air blast
N,N-diethaol-p-toluidine, water, photoinitiator
self-etch Co, Ltd, Osaka, Japan for 5 s.
Bond: MDP, HEMA, hydrophobic dimethacrylate,
adhesive Batch no: 41728 Apply bond and air-thin
N,N-diethaol-p-toluidine, silanated colloidal silica,
gently for 3 s.
bisphenol-A-diglycidyl methacrylate, photoinitiator

Adper Easy Bond (AEB)

One-step HEMA, Bis-GMA, water, metahacrylated phosphoric 3M ESPE, Apply bonding for 20 s
self-etch esters, ethanol, silane treated silica, copolymer St Paul, USA and air-thin gently
adhesive of acrylic and itaconic acid, phosphine oxide, 1,6 Batch no: 441760 for 5 s.
hexanediol dimethacrylate

Bisco Inc, Apply incrementally,

Resin Reflexions
Schaumburg, USA photo-polymerize each
Composite Ethoxylated Bis-GMA, glass filler, amorphous silica
Batch no: 1100012550 increment 20 s

Dentsply De Trey Apply to the surface

De Trey Conditioner 36
Etching gel GmbH, Germany for 15 s. Rinse for 10 s,
36% H3PO4
Batch no: 0803001025 dry with air

Abbreviations: Bis-GMA: bisphenol-A-diglycidyl methacrylate, HEMA: 2-hydroxyethyl methacrylate

for 30 s. Then, an etch-and-rinse (total-etch) adhesive
resin (Adper Single Bond 2-SB2, 3M ESPE, St. Paul,
USA) was applied according to the manufacturer’s
instructions and photo-polymerized using a light-
emitting diode (LED) polymerization unit (Elipar S10,
3M ESPE) for 10 s.
Group CSE: In this group, enamel surfaces were
conditioned initially with the primer of the two-step
self-etch adhesive (Clearfil SE Bond-CSE, Kuraray
Noritake Co., Osaka, Japan). After exposure to humid
conditions for 30 s, bonding was applied according to the
manufacturer’s recommendations. The adhesive resin
was applied accordingly, and photo-polymerized for 10 s.
Group AEB: The enamel surfaces in this group were
exposed to humidity conditions for 30 s and treated with
one-step self-etch adhesive resin (Adper Easy Bond-
AEB, 3M ESPE) and photo-polymerized for 10 s.
After conditioning enamel surfaces with the
adhesive resins at different RH levels as described
before, resin composite (Reflexions, Bisco, Schaumburg,
USA) was condensed into translucent polyethylene
tubes (diameter: 1 mm; height: 2 mm) which positioned
on the enamel surfaces and polymerized using the LED
polymerization unit for 20 s.
After the composite resin was polymerized, all
specimens were stored at 37°C water for 24 h until the
tests.
Micro-shear bond strength (μSBS) testing
All specimens were tested to failure for μSBS using a
special testing machine (Bisco Inc, Schaumburg, IL,
USA) at a crosshead speed of 0.5 mm/min (Figs. 2a–b).
Maximum stresses in Newton (N) were obtained from
the screen of the machine. The quantitative values were
converted into megapascal (MPa) by dividing it by the
bonded area (mm2) of the relevant resin cements.
Failure analysis
The debonded areas of all specimens were examined
under stereomicroscope (Olympus SZ40, Tokyo, Japan)
at 30× magnification. Failure modes were assigned as
adhesive, cohesive or mixed. Representative specimens
were sputter coated using a gold alloy to evaluate the
debonded areas on enamel under Scanning Electron
Microscope (SEM) (LEO 440, Electron Microscopy Ltd,
Cambridge, UK) with an acceleration voltage of 20 keV.
Statistical analysis
Statistical analysis were made using SPSS for Windows,
version 15.0 (SPSS Inc., Chicago, IL, USA). The μSBS
values of specimens in different humid conditions were
not normally distributed (Kolmogorov-Smirnov and
Shapiro-Wilk, α=0.05). Thus, they were logarithmically
transformed before statistical analysis. Data (MPa)
were submitted to two-way analysis of variance (2-
 Dent Mater J 2013; 32(3): 468–475 471

Figs. 2a–b Photos of the a) testing machine used for determining μSBS tests, b) position of the
specimen in the jig in relation to the shearing blade of the testing machine.

Table 2 The mean μSBS values and standard variations of the resin composite to enamel bonded with SB2, CSE, AEB
adhesive resins at different humid conditions. Same capital superscript letters in the same row and same lower
case letters in the same column show no statistical difference (p<0.05). See Table 1 for group abbreviations

Mean (±SD) (MPa)

Groups
H1 H2 H3 H4

SB2 11.8±5.6A,a 8.5±5.4A,a 10.6±5A,a 9.9±4.3A,a

CSE 12.9±5B,a 11.2±4.9B,a 9.6±4B,a 12.3±1.8B,a

AEB 3.5±1.1C,b 3.4±1.4C,b 3.6±1.8C,b 5.8±3.9C,b

way ANOVA) with the bond strength as the dependent

variable and the RH (4 levels) and the adhesive resin
type (3 levels) as independent variables. Multiple
comparisons were made using Tukey’s post-hoc test. P
values less than 0.05 were considered to be statistically
significant in all tests.

RESULTS
While adhesive resin type significantly affected the
results (F=131.596, p=0.000), RH parameters did not
have a significant effect (F=2.406, p=0.068). Interaction
terms were significantly different (F=2.158, p=0.049).
The mean μSBS values to enamel with SB2, CSE
and AEB were shown in Table 2. Among all adhesive
resins, AEB resulted in significantly lower μSBS (3.4–
5.8 MPa) than those of SB2 (8.5–11.8 MPa) and CSE Fig. 3. The distribution of the failure types in percentage
(9.6–12.9 MPa) in all H1, H2, H3 and H4 conditions per experimental group at different relative
(p<0.05). SB2 and CSE showed no significant difference humidity conditions.
in terms of μSBS (p>0.05).
The frequency of adhesive failures was the highest
at H2, H3 for SB2, H3 for CSE and H1-4 for AEB
indicating that humidity conditions may decrease
adhesion quality to enamel (Fig. 3). Cohesive failures depending on the adhesive resin (Figs. 4a–d, 5a–d, 6a–
were more in common in CSE followed by SB2. d). With the increase in RH level, the amount of bonded
SEM images especially in H4 conditions showed resin on the enamel surface decreased.
cohesive failure of the resin composite at varying degrees
472 Dent Mater J 2013; 32(3): 468–475

Figs. 4a–d SEM images (×2,000) of enamel surface after debonding from specimens belonging to Group SB2.
a) bonded at H1. Note the large cohesive failure in the composite resin, b) bonded at H2, c) bonded at H3. Note the
very small amount of resin composite attached on the enamel surface compared to (adhesive failure), d) bonded
at H4. Note the large fragment of composite resin adhered on the enamel surface (mixed failure). The arrow in
all SEM images indicate the remnants of resin composite.

Figs. 5a–d SEM images (×2,000) of enamel surface after debonding from specimens belonging to Group CSE.
a) bonded at H1. Note the distributed resin composite remnants on the enamel (cohesive failure), b) bonded at
H2, c) bonded at H3. Note the very small amount of resin composite left adhered (adhesive failure), d) bonded
at H4. Note the resin composite layer throughout the debonded surface (cohesive failure). The arrow in all SEM
images indicate the remnants of resin composite.

Figs. 6a–d SEM images (×2,000) of enamel surface after debonding from specimens belonging to Group AEB.
a) bonded at H1, b) bonded at H2. Note the resin composite remnants on the enamel covering a small area (mixed
failure), c) bonded at H3. Note the absence of resin composite (adhesive failure), d) bonded at H4. Note the resin
composite layer very small remnants of composite particles (cohesive failure). The arrow in all SEM images
indicate the remnants of resin composite.

DISCUSSION
In this study, the μSBS of resin composite to enamel was
tested after conditioning the enamel surface with three
different adhesive systems applied at various humidity
conditions. Since humidity did not significantly influence
the mean μSBS results within one adhesive system,
the null hypothesis that increased percentage of RH
conditions simulating the oral environment would not
affect the bond strength of the adhesive resins to enamel,
was accepted.
In the experimental set-up, in an effort to simulate
the exhaled humidity conditions in the oral environment,
a humid air chamber was constructed and the humidity
was measured with the help of a digital hygrometer. To
the authors’ best knowledge, a similar methodology has
not been established for in vitro conditions to date. The
humid air has been warmed in the nebulizer up to 30oC
before it departed from the chamber. The idea for this
was to simulate the respiratory system that heats the
 Dent Mater J 2013; 32(3): 468–475
air exhalation.
Total etch adhesive and two-step self-etch adhesive
resin exhibited significantly higher μSBS than that
of one-step self-etch adhesive resin to enamel at all
humidity conditions. Previous in vitro studies did not
consider humidity conditions but assuming that they
were performed in laboratory conditions, their results
could be compared to our results obtained at 36–45%
RH (H4) conditions. Among many studies, where
adhesion of total-etch, two-step self-etch and one-step
self-etch adhesive systems to enamel was studied, Lopes
et al.17) emphasized the similarity of the bond strength
to enamel between total-etch system and two-step self-
etch system whereas some studies18,19) pointed out the
differences between SB2 and CSE on bond strength to
enamel. Our results were comparable with the third
preliminary study of Adebayo et al.20), regarding the
mean μSBS values of SB2 and CSE adhesives. On the
other hand, McLeod et al.21) observed that the total-etch
systems showed significantly higher shear bond strength
to enamel than those of self-etch systems where they
used CSE and AEB. Nazari et al.22) have put forward
the superiority of the bond strength of the total-etch
adhesive to one-step self-etch adhesive on both intact
and ground enamel surfaces. In particular, a study of
Mine et al.23) showed significantly lower bond strength of
AEB than CSE. It has to be noted that in these studies
either macroshear test17,21), or microtensile test18,23) was
used. In vitro studies are considerably influenced by
the testing parameters. Thus, our study can only be
compared in the real sense with those studies where also
microshear test was used18-20,22).
The quality of the bond strength of self-etch adhesive
systems is related to their acidity. The self-etch adhesive
systems are generally categorized as: strong (pH≤1),
mild (pH≈2) and ultra-mild (pH>2.5)16). The pH levels of
CSE and AEB self-etch systems used in our study were
about 2 and 2.4, respectively23). A well-structured and
rough enamel surface could not be accomplished by mild
adhesives22). Although both self-adhesives used in the
present study appear in the mild acidic category, CSE
presented significantly higher mean μSBS than AEB in
all conditions. This could be explained by the chemical
compositions of the adhesives. The 10-methacryloxydecyl
dihydrogen phosphate monomer (10-MDP) present in
the chemical composition of CSE is claimed to interact
with the hydroxyapatite of the enamel by ionic bond
to produce MDP-Ca salts24). On the other hand, both
adhesives contain cross-linking monomers that improve
the bonding performance to the substrate. McLeod
et al.21) stressed the amount of these monomers in the
one-step self-etch systems to be less than two-step ones.
This could be one reason for lower results with the AEB
group.
In the presence of four different humidity conditions,
mean μSBS of the composite resin to enamel with all
adhesive systems tested was not statistically significant
within each group. Furuse et al.25) applied five different
adhesive systems including SB2 and CSE and found no
statistical difference between μSBS of resin composite
473
to the wet and dry enamel surfaces. Similarly, Chuang
et al.26) reported that marginal quality was not affected
when SB2 was applied on dry and wet enamel. However,
in both studies wetness of the enamel surfaces were
constituted with water contamination. In this study,
interaction terms were significant indicating that
some resin types behaved differently in varying RH
conditions. This can be attributed to the distinction in
the chemical composition of adhesives used in the study.
If the chemical composition of the adhesive systems
were examined, HEMA monomer could be found in SB2,
CSE and AEB adhesive systems. Hydrophilic property
of HEMA monomer, which designated the bonding
performance of the adhesives, could be verified according
to their polymerized and unpolymerized states27). If the
water absorption takes place before polymerization, a
reduction in the polymerization degree might occur due
to the dilution of the monomer in the adhesive system.
As shown in the present study, the specimens were
prone to humid conditions prior to the application of
the adhesive. However, the hydrophilic adhesive system
was not affected from the existing humidity conditions
according to μSBS values in all groups. Unlike SB2
and AEB, CSE contains 10-MDP monomer, merging
both hydrophilic and hydrophobic functional groups28).
Apparently, here hydrophobic functional monomers in
CSE were not influenced from the humid conditions29).
This could be due to the hydrophilic monomer in CSE
that contributed to the water sorption capability of
HEMA29). In fact, SB2 contains not only HEMA but also
water, ethanol and 10% silica nanofillers by weight30).
Ethanol is added into the agent as solvent to accelerate
water elimination31). As mentioned above, if the ratio of
the water to solvent in the chemical composition
increases, the degree of polymerization is negatively
affected32,33). The humid conditions did not affect the bond
strength in Group AEB. It was reported that excess water
may influence the mechanical properties of adhesive
layer of the one-step self-etch adhesives by inhibiting
the optimal polymerization of the monomers32,33). Beside
a significant difference about μSBS values in Group
AEB from the other groups, an adequate bonding
quality of AEB could also not be observed in the SEM
findings. As previously detected by Mine et al.23), etching
capability of AEB on the enamel surface was not ideal
and bonded particles decreased in H2 compared to H1
and H4. Moreover, no resin remnant was found on the
debonded surface in Group AEB at H3. In accordance
with the mechanical superiority of CSE, less adhesive
failure types were observed in Group CSE than in
Group AEB. In Group CSE, quantity of the composite
resin remnants on debonded surface decreased and the
bonded resin amount on the enamel became sparse with
the increased humidity level indicating that humidity
level may indeed impair the adhesion quality.
Adhesive failure types were dominated in the
debonded areas in Group SB2 at H2 and H3 conditions.
These alterations were independent from the μSBS
values. Thus, not only the μSBS values but also the
failure types should be assessed when evaluating
474 Dent Mater J 2013; 32(3): 468–475
bond durability of adhesive resins and resin composite
assemblies. The discrepancy between bond results and
failure types could be as a consequence of different
hydrophilic characteristics of the adhesives as discussed
above. Chuang et al.26) observed more cohesive failures
in dry enamel and adhesive failures in wet enamel
specimens after the application of total-etch adhesive
system.
Dentin tubules constitute 20 to 39% of dentin and
the fluid inside these tubules constitutes approximately
22% of the whole dentin volume34). It is reported that
the regular pulp pressure causes the fluid inside these
tubules flow towards the dentin surface which then
becomes uniformly wet35). This kind of effect is not
present in enamel making the testing situation less
complex. For the future investigations, bond strengths
of the adhesives on dentin surfaces could be evaluated
taking the pulp pressure into consideration. Humidity
aspect is also important for direct restorations applied on
enamel or orthodontic applications where brackets are
bonded to enamel. Nevertheless, future studies should
consider not only bond strength results but also failure
types in assessing adhesion quality on both enamel and
dentin at different humidity levels. Also, clinical studies
should correlate survival of adhesive resins in relation
with the intraoral humidity level during application.
CONCLUSION
Based on the results of this study, the following
conclusions could be drawn:
1. The μSBS of the resin composite bonded with
etch-and-rinse (total-etch) (SB2), two-step self-
etch system (CSE) and one-step self-etch adhesive
system (AEB) to enamel were not affected from
the alteration in humid conditions.
2. The frequency of adhesive failures was the highest
at H2, H3 for SB2, H3 for CSE and H1-4 for AEB
indicating that humidity conditions may decrease
adhesion quality to enamel.
3. Cohesive failures in the resin composite were
more frequent in CSE followed by SB2, also
supported by SEM findings.
REFERENCES
1) Chaves CAL, de Melo RM, Passos SP, Camargo FP, Bottino
MA, Balducci I. Bond strength durability of self-etching
adhesives and resin cements to dentin. J Appl Oral Sci 2009;
17: 155-160.
2) Quaas AC, Yang B, Kern M. Panavia F 2.0 bonding to
contaminated zirconia ceramic after different cleaning
procedures. Dent Mater 2007; 23: 506-512.
3) Santos BM, Pithon MM, Ruellas AC, Sant’Anna EF. Shear
bond strength of brackets bonded with hydrophilic and
hydrophobic bond systems under contamination. Angle
Orthod 2010; 80: 963-967.
4) Matos AB, Tate WH, Powers JM. Influence of enamel surface
preparation on composite bond strength. Am J Dent 2003; 16:
37A-40A.
5) Senawongse P, Sattabanasuk V, Shimada Y, Otsuki M,
Tagami J. Bond strengths of current adhesive systems on
intact and ground enamel. J Esthet Restor Dent 2004; 16:
107-115.
6) Osorio R, Monticelli F, Moreira MA, Osorio E, Toledano M.
Enamel-resin bond durability of self-etch and etch & rinse
adhesives. Am J Dent 2009; 22: 371-375.
7) Delong R, Douglas WH. Artificial oral environment for testing
dental materials. IEEE Trans Biomed Eng 1991; 38: 339-
345.
8) Plasmans PJ, Reukers EA, Vollenbrock-Kuipers L,
Vollenbrock HR. Air humidity: a detrimental factor in dentine
adhesion. J Dent 1993; 21: 228-233.
9) Varene P, Ferrus L, Manier G, Gire J. Heat and water
respiratory exchanges: comparison between mouth and nose
breathing in humans. Clin Physiol 1986; 6: 405-414.
10) Pickett KL, Sadowsky PL, Jacobson A, Lacefield W.
Orthodontic in vivo bond strength: comparison with in vitro
results. Angle Orthod 2001; 71: 141-148.
11) Hajrassie MK, Khier SE. In-vivo and in-vitro comparison of
bond strengths of orthodontic brackets bonded to enamel and
debonded at various times. Am J Orthod Dentofacial Orthop
2007; 131: 384-390.
12) Nguyen TT, Miller A, Orellana MF. Characterization of the
porosity of human dental enamel and shear bond strength in
vitro after variable etch times: initial findings using the BET
method. Angle Orthod 2011; 81: 707-715.
13) Leibrock A, Degenhart M, Behr M, Rosentritt M, Handel G.
In vitro study of the effect of thermo- and load-cycling on the
bond strength of porcelain repair systems. J Oral Rehabil
1999; 26: 130-137.
14) Att W, Kurun S, Gerds T, Strub JR. Fracture resistance of
single-tooth implant-supported all-ceramic restorations: an
in vitro study. J Prosthet Dent 2006; 95: 111-116.
15) Vasanthan A, Satheesh K, Hoopes W, Lucaci P, Williams K,
Rapley J. Comparing suture strengths for clinical applications:
a novel in vitro study. J Periodontol 2009; 80: 618-624.
16) Van Meerbeek B, Yoshihara K, Yoshida Y, Mine A, De Munck
J, Van Landuyt KL. State of the art of self-etch adhesives.
Dent Mater 2011; 27: 17-28.
17) Lopes GC, Marson FC, Vieira LC, de Caldeira AM, Baratieri
LN. Composite bond strength to enamel with self-etching
primers. Oper Dent 2004; 29: 424-429.
18) El Zohairy AA, Saber MH, Abdalla AI, Feilzer AJ. Efficacy
of microtensile versus microshear bond testing for evaluation
of bond strength of dental adhesive systems to enamel. Dent
Mater 2010; 26: 848-854.
19) Nagayassu MP, Shintome LK, Arana-Chavez VE, Fava M.
Micro-shear bond strength of different adhesives to human
dental enamel. J Clin Pediatr Dent 2011; 35: 301-304.
20) Adebayo OA, Burrow MF, Tyas MJ. Bond strength test: role
of operator skill. Aust Dent J 2008; 53: 145-150.
21) McLeod ME, Price RB, Felix CM. Effect of configuration
factor on shear bond strengths of self-etch adhesive systems
to ground enamel and dentin. Oper Dent 2010; 35: 84-93.
22) Nazari A, Shimada Y, Sadr A, Tagami J. Pre-etching vs.
grinding in promotion of adhesion to intact enamel using self-
etch adhesives. Dent Mater J 2012; 31: 394-400.
23) Mine A, De Munck J, Cardoso MV, Van Landuyt KL, Poitevin
A, Kuboki T, Yoshida Y, Suzuki K, Lambrechts P, Van
Meerbeek B. Bonding effectiveness of two contemporary self-
etch adhesives to enamel and dentin. J Dent 2009; 37: 872-
883.
24) Li N, Nikaido T, Takagaki T, Sadr A, Makishi P, Chen J,
Tagami J. The role of functional monomers in bonding to
enamel: acid-base resistant zone and bonding performance. J
Dent 2010; 38: 722-730.
25) Furuse AY, Cunha LF, Moresca R, Paganeli G, Mondelli RF,
Mondelli J. Enamel wetness effects on bond strength using
different adhesive systems. Oper Dent 2011; 36: 274-280.
26) Chuang SF, Chang CH, Yaman P, Chang LT. Influence of
 Dent Mater J 2013; 32(3): 468–475
enamel wetness on resin composite restorations using various
dentine bonding agents: part I-effects on marginal quality
and enamel microcrack formation. J Dent 2006; 34: 343-351.
27) Silva e Souza MH Jr, Carneiro KG, Lobato MF, Silva e Souza
Pde A, de Góes MF. Adhesive systems: important aspects
related to their composition and clinical use. J Appl Oral Sci
2010; 18: 207-214.
28) Tanaka R, Fujishima A, Shibata Y, Manabe A, Miyazaki T.
Cooperation of phosphate monomer and silica modification on
zirconia. J Dent Res 2008; 87: 666-670.
29) Jacques P, Hebling J. Effect of dentin conditioners on the
microtensile bond strength of a conventional and a self-
etching primer adhesive system. Dent Mater 2005; 21: 103-
109.
30) Faria-E-Silva AL, Fabião MM, Sfalcin RA, de Souza Meneses
M, Santos-Filho PC, Soares PV, Martins LR. Bond strength
of one-step adhesives under different substrate moisture
conditions. Eur J Dent 2009; 3: 290-296.
475
31) Higashi C, Michel MD, Reis A, Loguercio AD, Gomes OM,
Gomes JC. Impact of adhesive application and moisture on the
mechanical properties of the adhesive interface determined
by the nano-indentation technique. Oper Dent 2009; 34: 51-
57.
32) Manuja N, Nagpal R, Chaudhary S. Bonding efficacy of 1-step
self-etch adhesives: effect of additional enamel etching and
hydrophobic layer application. J Dent Child 2012; 79: 3-8.
33) Vaz RR, Hipolito VD, D‘Alpino PH, Goes MF. Bond strength
and interfacial micromorphology of etch-and-rinse and self-
adhesive resin cements to dentin. J Prosthodont 2012; 21:
101-111.
34) Mjor IA, Nordahl I. The density and branching of dentinal
tubules in human teeth. Arch Oral Biol 1996; 41: 401-412.
35) Rosales-Leal JI, de la Torre-Moreno FJ, Bravo M. Effect of
pulp pressure on the micropermeability and sealing ability of
etch & rinse and self-etching adhesives. Oper Dent 2007; 32:
242-250.