VOLUME 44 NUMBEP 1 JANUAPY 2013 9

QUI NTESSENCE I NTERNATI ONAL

RESTORATIVE DENTISTRY
dental substrates has been extensively
studied to develop materials that provide
greater durability, better esthetics, and
superior ease of use.
2,3
In dentistry, adhesion or bond may be
dened as the process by which restorative
materials are united to dental substrates.
4

Adhesion to enamel may be considered an
efcient and predictable clinical procedure,
whereas bond to dentin has been inconsis-
tent, mainly due to the structural and chem-
ical instability of this biologic composite,
which affects the bond mechanism of
restorative material.
5,6
The adhesion pro-
cess involves two stages. The rst consists
of the removal of calcium phosphates from
the enamel and dentin, with the subsequent
Esthetic dentistry has been increasingly
applied to restorative procedures. Since the
use of acid etching was recommended by
Buonoooro,
1
adhesive material bonding to
1
Associate Professor, Biomaterials Division, Faculty of Dentistry
of Uberaba, University of Uberaba, Uberaba, MG, Brazil.
2
Postgraduate student, Biomaterials Division, Faculty of
Dentistry of Uberaba, University of Uberaba, Uberaba, MG,
Brazil.
3
Associate Professor, Department of Restorative Dentistry,
Araraquara School of Dentistry UNESP, Araraquara, SP, Brazil.
Correspondence: Prof Dr Fernando Carlos Hueb de Menezes,
Departamento de Materiais Odontolgicos, Faculdade de
Odontologia da Universidade de Uberaba (UNIUBE), Av Nen
Sabino, 1801, 38055-500, Uberaba, MG, Brasil. Email: fernando.
menezes@uniube.br
Evaluation of bond strength and thickness
of adhesive layer according to the techniques
of applying adhesives in composite resin
restorations
Fernando Carlos Hueb de Menezes, PhD
1
/Stella Borges da Silva, DDS
2
/
Thiago Assuno Valentino, PhD
1
/Maria Anglica Hueb de Menezes
Oliveira, PhD
1
/Alessandra Nara de Souza Rastelli, PhD
3
/Luciano de
Souza Conalves, PhD
1
Adhesive restorations have increasingly been used in dentistry, and the adhesive system
application technique may determine the success of the restorative procedure. The aim
of this study was to evaluate the inuence of the application technique of two adhesive
systoms (Cloarhl SE Bond and Adpor Sootonbond MultiPurposo) on tno bond strongtn and
adhesive layer of composite resin restorations. Eight human third molars were selected
and prepared with Class I occlusal cavities. The teeth were restored with composite using
various application techniques for both adhesives, according to the following groups
(n = 10): group 1 (oontrol), systoms woro appliod and adnosivo was immodiatoly lignt aoti-
vated for 20 seconds without removing excesses; group 2, excess adhesive was removed
with a gentle jet of air for 5 seconds; group 3, excess was removed with a dry microbrush-
type device; and group 4, a gentle jet of air was applied after the microbrush and then
light activation was performed. After this, the teeth were submitted to microtensile testing.
For the two systems tested, no statistical differences were observed between groups 1
and 2. Groups 3 and 4 presented higher bond strength values compared with the other
studied groups, allowing the conclusion that excess adhesive removal with a dry micro-
brusn oould improvo bond strongtn in oomposito rostorations. Prodominanoo o adnosivo
fracture and thicker adhesive layer were observed via scanning electron microscopy
(SEM) in groups 1 and 2. For groups 3 and 4, a mixod ailuro pattorn and tninnor adno-
sive layer were veried. Clinicians should be aware that excess adhesive may negatively
affect bond strength, whereas a thin, uniform adhesive layer appears to be favorable.
(Quintessence Int 2013;44:915)
Key words: adhesive system, bond strength, composite resin
10 VOLUME 44 NUMBEP 1 JANUAPY 2013
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Menezes et al
formation of microporosities in both sub-
strates. The second stage involves inltra-
tion and later in situ polymerization of the
adhesive system, creating the so-called
hybrid layer.
7
The micromechanical reten-
tion is based on a mechanism of diffusion,
7

which is commonly referred to as hybridiza-
tion.
810
Basod on tno aoromontionod adno-
sive strategy, the adhesive systems cur-
rontly availablo involvo two approaonos:
one with previous acid etching (wet tech-
niquo) and tno otnor witn sol-otoning adno-
sivos (dry toonniquo).
10,11
Adhesive systems are combinations of
hydrophilic and hydrophobic resin mono-
mers of different molecular weights and
viscosities. Hydrophilic monomers allow the
adhesive to be compatible with the natural
humidity of dentin, but absorb water and
are therefore less stable. Hydrophobic
monomers present a higher molecular
weight, are more viscous, and provide the
system with higher mechanical strength
and stability.
5
In spite of having interesting
features, hydrophobic monomers are
unable to penetrate the porosities created
on the dental tissues. Therefore, hydrophilic
resin diluents and solvents are added to the
composition.
24

Uniform inltration of hydrophilic mono-
mers throughout the entire portion of demin-
eralized dentin to protect and reinforce the
collagen ber network is therefore essential
while carrying out the adhesive technique.
An excessive thickness of the adhesive
layer may be harmful to the bond strength
and lead to staining and postoperative sen-
sitivity.
1214
This makes it important to control
the clinical conditions of the restorative
technique to obtain the best bond results.
However, most manufacturers do not pres-
ent clear information about the application
of the adhesive systems, especially accord-
ing to excess adhesive removal. The tech-
nique and devices to promote excess
removal are usually not detailed, and some
manufacturers only recommend applying a
gentle air blast. However, the effect of tech-
niques for excess adhesive removal on
bond strength remains unclear.
Therefore, the aim of this study was to
evaluate the inuence of the application
technique of two adhesive systems on the
bond strength and adhesive layer of com-
posite resin restorations. The null hypothesis
of the study was that there was no inuence
of the techniques for excess adhesive
removal on the bond strength of restorations.
METHOD AND MATERIALS
Tooth selection and preparation
This study was approved by the Ethics
Committee of the University of Uberaba,
Uboraba, Brazil (CAE: 004.0.227.000-10).
Eighty recently extracted human third
molars, obtained from the Human Tooth
Bank o tno Univorsity o Uboraba, woro
cleaned with periodontal curettes and
stored in a 0.9% saline solution with 0.1%
thymol. Afterward, the tooth roots were
embedded in acrylic resin in a polyvinyl
chloride tube 25 mm in diameter and 15 mm
high, so that the crowns remained com-
pletely exposed in the direction of the long
axis of the teeth. A diamond tip no. 1095
(K.G. Soronson) was usod at nign spood
under abundant cooling to prepare Class I
type occlusal cavities, 6 mm in the distome-
sial direction, 1 mm in the vestibulolingual
direction, and 2 mm deep, standardized by
using a machine adapted for creating tooth
preparations.
Adhesive system application
techniques
The teeth were restored with composite
rosin (Filtok Z350, 3M ESPE) using two
types of adhesive systems, one self-etching
(Cloarhl SE Bond, Kuraray) and ono oon-
vontional (Adpor Sootonbond MultiPurposo,
3M ESPE), witn tno applioation toonniquos
varying aooording to tno groups (Tablo 1).
The composite was applied by means of
oblique increments at a maximum of 1 mm
thickness according to the incremental
technique. After this, the roots of the
restored teeth were removed with a dia-
mond disk.
Sample preparation for
microtensile testing
The test specimens were xed in an acrylic
support with low-melting point wax (Exata,
DFL) and woro adaptod to prooision outtor
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Menezes et al
Table 1 Adhesive systems, groups, and respective application techniques
Adhesive system Group Application techniques
CL1 Cavity drying + acidic primer + rubbing for 20 s + adhesive application + light
activation for 20 s
CL2 Cavity drying + acidic primer + rubbing for 20 s + gentle jet of air for 5 s + adhe-
sive application + gentle jet of air for 5 s + activation for 20 s
Cloarhl SE Bond CL3 Cavity drying + acidic primer + rubbing for 20 s + gentle jet of air for 5 s + adhe-
sive application + remove excess with a dry microbrush + activation for 20 s
CL4 Cavity drying + acidic primer + rubbing for 20 s + gentle jet of air for 5 s + adhe-
sive application + excess was removed with a dry microbrush + gentle jet of air
for 5 s + activation for 20 s
SB1 Cavity drying + acid etching for 15 s + washing for 15 s + drying with absorbent
paper + primer application for 20 s with agitation + adhesive application + gentle
activation for 20 s
SB2 Cavity drying + acid etching for 15 s + washing for 15 s + drying with absorbent
paper + primer application for 20 s with agitation + adhesive application + gentle
jet of air for 5 s + activation for 20 s
Adper
Scotchbond
MultiPurposo
SB3 Cavity drying + acid etching for 15 s + washing for 15 s + drying with absorbent
paper + primer application for 20 s with agitation + adhesive application +
remove excess with a dry microbrush + activation for 20 s
SB4 Cavity drying + acid etching for 15 s + washing for 15 s + drying with absorbent
paper + primer application for 20 s with agitation + adhesive application + excess
was removed with a dry microbrush + gentle jet of air for 5 s + activation for 20 s
soMot 1000 (Buonlor). Undor oonstant irri-
gation, the teeth were sectioned perpen-
dicularly to the bond surface, thus obtaining
ve sections in the pulp wall region. The
interface was sectioned at a thickness of
1 mm in the vestibulolingual direction into
hourglass-shaped specimens. Afterward,
the samples were taken to the machine for
microtensile tests.
The areas of specimens selected for the
microtensile test were measured with a digi-
tal paonymotor (Digimatio Calipor), witn
0.01-mm precision, and measurements were
recorded. After this, the specimens were
individually picked up with the aid of forceps
and xed to the device by their extremities
using instant cyanoacrylate-based adhesive
(Zapit, DvA), witn tno bond aroa plaood por-
pendicularly to the long axis of the microten-
sile force to perform the microtensile test.
The mechanical microtensile test was per-
formed in a Universal Test Machine DL 2000
(EMC 2003), proviously ad|ustod or tonsilo
forces, with a load cell of 50 Kgf capacity, at
a speed of 1 mm/min. At the time of fracture,
movement was immediately stopped, and
the data were collected. The nal adhesive
bond strength values were calculated by
dividing the rupture load values obtained in
Nowton (N), by tno oross sootions o tno
hourglass-shaped specimens, obtained in
mm
2
, tnus boing oxprossod in MPa.
Afterward, statistical analysis of the results
was performed (analysis of variance
|ANOvA] and oomplomontary Tukoy tost). n
addition, the specimens were analyzed by
SEM to observe fracture patterns and the
adhesive layer of the restorations.
RESULTS
Booauso tno rosults prosontod a normal
and homogenous curve, adoption of the
ANOvA paramotrio tost was allowod
(P < .001). For vorihoation o signihoanoo, it
was necessary to apply the Tukey comple-
mentary test, at a level of 5% signicance
(Tablo 2). No statistioal dioronoo was
observed between groups 1 and 2. For
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Table 2 Bond strength (MPa) and standard SD of composite resin restorations
according to the adhesive system application technique
Groups
Bond strength (MPa) (SD)
Clearfl SE Bond Adper Scotchbond MultiPurpose
1 12.98 (1.31)
Bb
12.85 (2.11)
Bb
2 13.88 (1.55)
Bb
14.34 (2.37)
Bb
3 20.53 (1.80)
Ab
22.09 (1.49)
Aa
4 19.74 (1.97)
Ab
20.63 (2.75)
Ab
SD, standard deviation. Distinct letters indicate statistical difference in the bond strength values among groups,
with capital letters used for comparison in columns and lowercase letters for comparison in lines.
Fig 1 SEM illustrating the fracture patterns. (a) Adhesive fracture. (b) Mixed fracture.
a b
groups 3 and 4, higher bond strength val-
ues were found for the two adhesive sys-
tems tested in comparison with the other
studied groups.
By SEM, tno prodominanoo o adnosivo
raoturo was obsorvod (Fig 1a), as woll as
greater thickness of the adhesive layer for
groups 1 and 2 (Figs 2a, 2b, 3a, and 3b).
For groups 3 and 4, predominance of the
mixod ailuro pattorn was vorihod (Fig 1b),
as was a thinner adhesive layer for both
studiod adnosivos (Figs 2o, 2d, 3o, and 3d).
DISCUSSION
The null hypothesis of the present study
was rejected. The adhesive system applica-
tion techniques inuenced the results, inter-
fering in the bond strength values in the
groups studied for the two tested adhesive
systems.
Adhesive restorations have been widely
used for esthetic and functional restoration
of teeth. At present, composites have
acquired a prominent place among materi-
als used in direct techniques. Their consid-
erable esthetic possibilities have made
them preferable for various therapeutic indi-
cations. These materials conserve dental
structure, since they are retained by adhe-
sive methods and do not require additional
moonanioal rotontion. Novortnoloss, tnoy
are highly technique sensitive.
15
In spite of the technological advance-
ment of these materials, there are still con-
troversies regarding the efcacy of adhe-
sive restorations. Adhesive systems must
be used with awareness of their limitations.
This fact leads to the understanding that
this advancement applied to adhesive sys-
tems does not necessarily correspond to an
improvement in the quality of the product,
but to efcacy during their use.
4
There are different application techniques
according to the type of composition of the
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Menezes et al
Fig 2 SEM illustrating the adhesive layer thicknesses for the Clearfl groups. (a) Group 1, (b) group 2, (c)
group 3, and (d) group 4.
Fig 3 SEM illustrating the adhesive layer thicknesses for the Scotchbond groups. (a) Group 1, (b) group 2, (c)
group 3, and (d) group 4.
b a
c
a b
d c
d
66,1m
164m
4,53m
98,1m
102m
104m
48m
73,6m
73,7m
91,5m
5,33m
5,87m
8,73m
7,20m
7,53m
6,73m 6,20m
3,87m
9,19m
10,1m
10,1m
14 VOLUME 44 NUMBEP 1 JANUAPY 2013
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Menezes et al
adhesive system used.
1619
However, the
manufacturers of these products do not pres-
ent clear information about the techniques for
use, mainly with reference to application of
the adhesive. In the present study, the self-
otoning adnosivo systom Cloarhl SE Bond
and conventional Adper Scotchbond
MultiPurposo woro onoson, booauso tnoy aro
products widely used by professionals in the
adhesive dentistry eld and because they do
not have explanatory instructions about the
adhesive application technique.
There has been a great deal of discus-
sion about treatment of the dentin substrate
and application of primers with different
solvents and mechanisms of action.
2022

However, there has not been a great deal of
concern with regard to application of the
adhesive, particularly regarding the thick-
ness of the lm and removal of excess
material. Some studies have shown evi-
dence that a thick layer of adhesive may
diminish the bond strength of adhesive
restorations, compromising their longevi-
ty.
1214
Clinically, the adhesive must be
applied carefully. Very thick layers may be
deposited, particularly in the internal angles
of a cavity, determining a signicant reduc-
tion in bond quality.
4

Some companies do not approach the
subject of removing adhesive excesses of
their systems and instruct that light activa-
tion be performed immediately after they
have been applied. However, in the present
study, it was observed that immediate
polymerization of both adhesives caused a
reduction in bond strength, which may be
observed from the values obtained and by
the predominance of adhesive failures (see
Fig 1a), in wnion tno matorial dobondod
from the dentinal substrate. In addition, a
thicker adhesive layer was observed at the
intoraoo (soo Figs 2a and 3a). n tnis oon-
text, Carvalho
4
warned that polymerizing the
adhesive immediately after its application
caused serious harm. The material is not
adequately polymerized, thus compromising
bond strength, with resultant degradation of
the interface and postoperative sensitivity.
4

Other companies have suggested that
the component should be applied in a sin-
gle layer and that excess should be
removed with a gentle jet of air, without any
standardization. In the present study, the
application of a gentle jet of air after appli-
cation of the adhesive did not interfere
positively in the results, and there was no
statistical difference for groups CL1 and
SB1, witn prodominanoo o tno adnosivo
failure pattern, as well. Moreover, the adhe-
sive layer veried was also shown to be
vory tniok (soo Figs 2b and 3b). Studios
have shown that the jet of air may nega-
tively inuence the bond of the restoration.
Incorporation of oxygen into the matrix and
disorderly spreading of the lm may inter-
fere in the bond quality and longevity of the
restoration, in addition to causing staining
at the interface.
17,23
The results of the pres-
ent study are in agreement with those
obtained by Hilton and Schwartz,
23
who
observed that with the jet of air, there is no
control over spreading of the adhesive. This
could result in an adhesive layer without
uniformity, negatively inuencing the bond
strength of the restoration.
In this context, careful removal of excess
may provide a more effective bond. In the
other groups, in which a dry, microbrush
type device was used for removing the
excess adhesive, statistically higher results
were observed, resulting in higher bond
strongtn valuos (Tablo 2). Tnis was also
proved by the predominance of mixed fail-
uro, (soo Fig 1b) and a tninnor adnosivo
layor (soo Figs 2o, 2d, 3o, and 3d). Tno
application of gentle jets of air after remov-
ing the excesses with the microbrush
(groups CL4 and SB4) also nad no inhu-
ence on the results. This could be justied
by the good absorption capacity of the
device, preventing the adhesive from sim-
ply being displaced to other regions of the
tooth, and providing a thinner and more
uniform adhesive layer. This may have
determined the higher bond strength found,
in agroomont witn Potio ot al,
13
who veried
that a thick or heterogeneous layer of adhe-
sive could harm the bond interface and
promote a reduction in adhesiveness of the
restorative material.
Therefore, manufacturers could be more
clear with regard to the clinical methods of
application of their products. However, the
majority present information with very little
detail, which could lead to errors. Thus, it is
the professionals responsibility to research
and know about the mechanisms of adhe-
VOLUME 44 NUMBEP 1 JANUAPY 2013 15
QUI NTESSENCE I NTERNATI ONAL
Menezes et al
sion to apply adhesive systems in the best
possible manner, with the purpose of avoid-
ing possible postrestorative failures and
increasing the longevity of restorations.
Clinicians should be aware that excess
adhesive may negatively affect bond
strength and that a uniform and thin adhe-
sive layer appears to be favorable.
CONCLUSION
Adhesive systems should be carefully
applied. Some aspects should be seen
mainly on the thickness of the adhesive
layer. The effective methods for removal of
excess adhesive have a positive inuence
on the bond strength. The use of a gentle jet
of air, often recommended by the manufac-
turer, does not allow the formation of a thin,
uniform layer. The application of a dry
microbrush is effective in the standardiza-
tion of the adhesive lm and can be safely
used to remove the excess.
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