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journal of dentistry 42 (2014) 800–807

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Bonding performance of universal adhesives in


different etching modes

Andrea Wagner a, Michael Wendler a,b, Anselm Petschelt a, Renan Belli a,


Ulrich Lohbauer a,*
a
Laboratory for Biomaterials Research, Dental Clinic 1 – Operative Dentistry and Periodontology,
University of Erlangen-Nuernberg, Erlangen, Germany
b
Department of Restorative Dentistry, Faculty of Dentistry, University of Concepción, Concepción, Chile

article info abstract

Article history: Objectives: The aim of this study was to compare the microtensile bond strength (mTBS) and
Received 7 March 2014 resin penetration into dentine of three universal adhesives (UAs) applied in two different
Received in revised form etching modes (i.e. self-etch or etch-and-rinse). The effect of thermocycling on the mTBS was
11 April 2014 also evaluated.
Accepted 28 April 2014 Methods: The occlusal third of sound human molars was removed and the exposed surfaces
were treated with three UAs (Futurabond Universal, Scotchbond Universal Adhesive and
All-Bond Universal) in self-etch or etch-and-rinse mode. Two one-step self-etch adhesives
Keywords: (Futurabond DC and Futurabond M) were applied on additional teeth as reference. After
Adhesion composite build up, the specimens were stored for 24 h in distilled water at 37 8C
Universal adhesives or thermocycled for 5000 cycles. Composite/dentine beams were prepared (1 mm2) and
Self-etch mTBS test was performed. Data was analyzed using three-way ANOVA and Tukey’s test
Etch-and-rinse (a = 0.05). One additional tooth was prepared for each group for evaluation of infiltration
Dentine bonding ability into dentine by dyeing the adhesives with a fluorochrome (Rhodamine B). After
longitudinal sectioning, the generated interfaces were examined under confocal laser
scanning microscopy.
Results: The addition of an etching step did not significantly affect the mTBS of none of the
UAs, when compared to their self-etch application mode. All pre-etched specimens showed
considerably longer resin tags and thicker hybrid layers. Thermocycling had no significant
effect on the mTBS of the UAs.
Conclusions: Application of an etching step prior to UAs improves their dentine penetration,
but does not affect their bond strength to dentine after 24 h or after thermocycling for 5000
cycles.
Clinical significance: Similar bond strength values were observed for the UAs regardless
of application mode, which makes them reliable for working under different clinical
conditions.
# 2014 Elsevier Ltd. All rights reserved.

* Corresponding author at: Dental Clinic 1 – Operative Dentistry and Periodontology, Glueckstr. 11, D-91054 Erlangen, Germany.
Tel.: +49 9131 854 3740; fax: +49 9131 853 3603.
E-mail addresses: ulrich.lohbauer@fau.de, lohbauer@dent.uni-erlangen.de (U. Lohbauer).
http://dx.doi.org/10.1016/j.jdent.2014.04.012
0300-5712/# 2014 Elsevier Ltd. All rights reserved.
journal of dentistry 42 (2014) 800–807 801

mode,7,22 although bond strength degradation has been


1. Introduction observed after ageing for pre-etched samples.23 The aim of
the present study was to compare the bond strength and resin
Current dental adhesive systems and adhesive approaches penetration pattern into dentine of three commercial UAs
seek to provide long-term bonding, while ensuring simplifica- applied in two different etching modes (i.e. SE or ER). Two 1-
tion of the technique. Self-etch adhesives (SEAs) were SEAs were compared as reference. The effect of thermocycling
introduced with the goal of eliminating the highly sensitive on mTBS was also evaluated. The null hypotheses were that (i)
technique step of acid etching, as their acidic monomers the application mode of the UAs did not affect their mTBS, (ii)
simultaneously etch and infiltrate the dental substrate,1 nor their resin penetration pattern into dentine; and (iii) that
thereby minimizing the discrepancies between hybridized the bond strength is not affected by thermocycling.
and etched zones in the substrate.2 Among them, ‘‘all-in-one’’
or ‘‘one step self-etch adhesives’’ (1-SEAs) go even further, as
they intend to combine all-steps in only one application. While 2. Materials and methods
their bonding ability to dentine has been progressively
improved with respect to the first 1-SEAs by means of better 2.1. Bonding procedures, specimen fabrication and mTBS
chemical interaction,3 adhesion to enamel still remains testing
unsatisfactory. Therefore, application of selective acid etching
on enamel before SEA application has been recommended, Sound human third molars were stored in 0.5% chloramine
especially when the use of mild-pH SEAs is intended.4 solution and used within 3 months of extraction. The occlusal
However, inadvertent pre-etching of dentine is a clinical risk, third was removed using a low-speed diamond saw (IsoMet;
which can negatively affect bonding efficacy.5,6 Aiming to Buehler Ltd., USA) under water irrigation and flat surfaces
eliminate complications and providing a single product for all were prepared in mid-coronal dentine with a remaining
situations, ‘‘universal adhesives’’ (UAs) that might be indis- thickness in the range of 2.5  0.2 mm. The dentine surface
tinctly applied, either in self-etch (SE) or etch-and-rinse (E&R) was ground with a 600-grit SiC paper for 60 s in order to
mode,7,8 have been recently introduced. produce a clinical relevant smear layer. Twelve teeth were
One of the keys of success with self-etching adhesives is assigned randomly to each of the three experimental groups
the chemical bonding capability of their functional monomers and the UAs Futurabond U (FbU) (Voco, Cuxhaven, Germany),
to hydroxyapatite (HAp),1 as described by the ‘‘adhesion/ Scotchbond Universal Adhesive (SbU) (3M ESPE, Seefeld,
decalcification concept’’.9,10 Among the currently used func- Germany) and All-Bond Universal (AbU) (Bisco, Schaumburg,
tional monomers, 10-methacryloyloxydecyl dihydrogenpho- USA) were applied either in self-etch (SE) or etch-and-rinse
sphate (MDP) has demonstrated a very effective and durable (E&R) mode. Two self-etching adhesives, Futurabond M (FbM)
bond to dentine,11,12 due to the low solubility of the calcium and Futurabond DC (FbDC) (Voco, Cuxhaven, Germany), were
salt that forms on the hydroxyapatite surface.12 On the other used for comparison and only applied in the SE mode (each on
hand, micromechanical interlocking by means of good six teeth). Composition and manufacturer’s instructions are
dentine hybridization (i.e. resin tags and hybrid layer), has described in Table 1.
been proposed to improve the bond strength of SEAs.13 For the SE mode, the dentine surface was left slightly wet
Phosphoric acid etching of dentine prior to application of and the adhesives were applied following manufacturer’s
SEAs significantly improves the interface infiltration morphol- instructions and light-cured for 20 s under a halogen light-
ogy, by generating thicker hybrid layers14,15 and longer resin curing unit (EliparTrilight, 3M ESPE, USA) with an output
tags.16 Removal of the smear layer and smear plugs by this pre- intensity of 750 mW/cm2. For the E&R mode, before adhesive
treatment17 facilitates the adhesive penetration, especially in application, Scotchbond Etchant (35% H3PO4, 3M ESPE, USA)
mild SEAs. Nevertheless, a clear correlation to higher bond was applied on the dentine surface for 15 s, rinsed for 30 s and
strengths by these enhanced interfaces has not been estab- left slightly wet.
lished.18 Resin composite crowns (GrandioSO; Voco, Germany)
According to their ability to demineralize dentine, SEAs were incrementally build-up in 1 mm increments up to 5 mm
have been classified into strong (pH 1), intermediately strong under the same curing conditions as described above. Three
(pH between 1 and 2), mild (pH  2) and ultra-mild (pH >2.5).1 teeth in each group were stored in distilled water for 24 h at
This ‘‘etching aggressiveness’’ is strongly related with their 37 8C, whereas the other three were thermo-cycled (Willytec
interaction depth in dentine,19 which varies from few V2.8; Willytec/SD Mechatronik, Germany) for 5000 cycles
nanometers in ultra-mild SEAs20 to several micrometres, in (cyclic immersion for 30 s at 5.5 8C/55 8C each, 7 s dwelling
the strong SEAs.1 Thus, hybrid layers of mild SEAs are much time).
thinner than those generated by stronger SEAs or etch-and- All specimens were then longitudinally sectioned in both
rinse adhesives, although hybrid layer thickness may not be of ‘x’ and ‘y’ directions across the bonded interface with a low-
major importance to bonding efficacy.2 By demineralizing speed diamond saw under sustained water-cooling (IsoMet
dentine only incompletely, mild SEAs leave HAp partially low speed saw with a Buehler 10.2 cm  0.3 mm diamond
attached to collagen, so it is available for chemical interac- wafering blade, No. 11-4244), following a non-trimming
tion12 and protective nanolayering.21 microtensile technique.24 Each beam dimensions were con-
At present, there is only sparse literature reporting on the trolled with a digital calliper to ensure a cross-sectional area of
efficacy of UAs. Similar adhesive performance has been 1  0.05 mm2. Only beams from the central region of each
observed for these adhesives regardless of their application tooth were used. After sectioning, the specimens were fixed to
802 journal of dentistry 42 (2014) 800–807

Table 1 – Adhesive composition and application procedure (information supplied in the safety data sheets and material
instructions).
Material Composition Application procedure
Futurabond U Liquid 1: 1. Mix and stir thoroughly both liquids with the
(FbU) Acidic adhesive monomer Single Tim applicator.
HEMA 2. Apply the adhesive homogenously to the surface
Voco BISGMA, HEDMA, UDMA and rub for 20 s using the Single Tim.
Cuxhaven, Germany Catalyst 3. Dry off the adhesive layer with dry, oil-free air for
at least 5 s.
Liquid 2: 4. Light cure the adhesive layer for 10 s.
Ethanol
Initiator, catalyst

Scotchbond Universal 10-MDP phosphate monomer, 1. Apply the adhesive with the applicator to the
Adhesive Vitrebond Copolymer entire tooth surface and rub for 20 s.
(SbU) HEMA 2. Dry gently for about 5 s until it no longer moves
BISGMA, dimethacrylate resins and the solvent has evaporated completely.
3M ESPE Filler, silane, initiators 3. Harden the adhesive with a curing light for 10 s.
Seefeld, Germany Ethanol, water

All-Bond Universal 10-MDP phosphate monomer 1. Dispense 1–2 drops of ABU into a clean well.
(ABU) HEMA 2. Apply two separate coats, scrubbing the
BISGMA preparation with a microbrush for 10–15 s per coat.
Bisco Ethanol 3. Evaporate excess solvent by thoroughly air-drying
Schaumburg, USA for at least 10 s. Surface should have a uniform
glossy appearance.
4. Light cure for 10 s.

Futurabond M Acidic adhesive monomer 1. Dispense 1 drop of FbM onto mixing palette.
(FbM) HEMA 2. Apply a moderately thin layer of the adhesive to
UDMA the enamel/dentine with a suitable applicator and
Voco Ethanol, catalyst allow it to act for 20 s.
Cuxhaven, Germany 3. Dry the adhesive layer for at least 5 s.
4. Polymerize with blue light for 10 s.

Futurabond DC Liquid 1: 1. Mix one drop of Liquids 1 and 2 on a mixing


(FbDC) Acidic adhesive monomer palette for approximately 2 s.
HEMA 2. Apply the adhesive in a medium thickness layer
Voco BISGMA and rub into the tooth surface for 20 s.
Cuxhaven, Germany 3. Dry the adhesive layer for at least 5 s.
Liquid 2: 4. Light cure for 10 s.
Ethanol NOTE: FbDC is dual-curing and therefore must be
Initiator applied immediately after mixing.

Geraldeli’s testing jigs25 with cyanoacrylate glue (Loctite 401, of the substrates). The cohesive failures in dentine or
Henkel, Germany) and stressed in tension until failure using a composite were not included in the mean mTBS calculation.
universal testing machine (Z2.5, Zwick, Germany) with a 100 N
load cell travelling at a crosshead speed of 0.5 mm/min. The 2.3. Semi-quantitative analysis of penetration depth into
imposed force (in Newton) at the time of fracture was divided dentine by confocal laser scanning microscopy (CLSM)
by the calculated bonded area (in mm2) to obtain the mTBS in
MPa. The Kolmogorov–Smirnov test at a = 0.05 was applied to Following the same adhesive protocols described above, one
confirm the normal distribution of the results. The obtained specimen per group was prepared for observation under
data was analyzed using a three-way ANOVA and Tukey’s post CLSM.26 The fluorochrome Rhodamine B Isothiocyanate (Merck,
hoc test at a = 0.05 (IBM SPSS Statistics 21.0 software, IBM Germany) was compounded into the respective adhesives at a
Chicago, IL, USA). Samples broken cohesively in dentine or concentration of 0.008wt% directly before application on the
with glue covering the adhesive layer as well as pre-testing dentine surface. Only one composite increment was placed over
failure (PTF) samples were excluded from the statistics. the adhesive resin. The teeth were then cut longitudinally into
two halves and both new generated surfaces were polished for
2.2. Analysis of failure mode by light microscope one minute with SiC paper in sequence (Grit 800/1200/2000/
4000) under permanent water cooling.
The failure modes were evaluated for each sample using a The samples were examined in 1000-fold magnification
light microscope (SV 6, Zeiss, Germany) at 50 magnification under a CLSM (TCS SL, Leica, Germany) at a 514-nm excitation
and classified as ‘cohesive’ (entirely within dentine substrate line of argon ion laser. The emissions were detected using a DD
or resin composite), ‘adhesive’ (at the dentine-resin interface) 458/514 band pass filter. A semi-quantitative analysis of the
or ‘mixed’ (at dentine-resin interface including failure into one penetration depth of the adhesive resin into the dentine
journal of dentistry 42 (2014) 800–807 803

Table 2 – Microtensile bond strength (MPa), number of valid samples and number of pre-testing failures (n/PTF).
Adhesive Self-etch mode Etch-and-rinse mode

24-h After thermo-cycling 24-h After thermo-cycling


b,c,d b,c,d b,c,d
Futurabond U 37.9  14.0 (104/5) 36.6  18.7 (41/39) 41.2  10.7 (66/2) 46.0  12.9a,b,c (21/0)
All Bond Universal 52.6  12.7 a (35/0) 44.7  12.7a,b,c (30/0) 44.8  10.8a,b (26/1) 54.6  11.7 a (25/0)
Scotchbond Universal 44.0  21.9a,b,c (35/0) 48.3  13.85a,b,c (18/0) 49.1  11.1a,b,c (48/0) 46.8  15.1a,b,c (65/1)
Futurabond M 36.7  14.5c,d,e (33/4) 26.1  9.7 e (34/13)
Futurabond DC 38.5  14.8b,c,d (28/7) 25.2  9.2d,e (22/11)
Means followed by the same superscript letters are not statistically different (at p < 0.05). Valid samples number (n) corresponds to those
samples included in the statistical analysis; i.e. excluding the PTF samples and those broken within dentine or with glue covering the binding
site.

substrate and the hybrid layer formed was performed utilizing the SE mode (Fig. 1A–C). In contrast, a mean HL of 2–4 mm was
the ‘Leica Confocal software’ (Version 2.61, Leica, Germany). identified in the E&R mode and deep penetration of the UAs
into dentine was discernible by formation of resin tags. FbU
produced 18–30 mm long resin tags (Fig. 1D), while ABU (Fig. 1E)
3. Results and SbU (Fig. 1F) showed a slightly deeper penetration (Table
3). FbM showed only a slight penetration (less than 0.5 mm)
3.1. Microtensile bond strength and fracture mode into dentine (Fig. 2A), while FbDC (Fig. 2B) produced a HL
analysis comparable to that of the UAs in the E&R mode (about 2.3 mm)
and resin tags of 9–30 mm length. This analysis, however,
The mTBS values of the adhesives after the different applica- reflects only a semi-quantitative assessment of the described
tion and ageing protocols are presented in Table 2. The mean parameters.
bond strength values of the UAs were similar or higher than
the results of the two 1-SEAs, before as well as after
thermocycling. 4. Discussion
The highest mTBS value after 24-h water storage was
obtained for the ABU under SE mode, being statistically higher Universal adhesives represent the last generation of adhesives
than FbU ( p = 0.000), FbM ( p = 0.000) and FbDC ( p = 0.006). in the market. They are designed under the ‘‘all-in-one’’
Although there were no significant differences in mTBS concept of already existing one-step self-etch adhesives, but
between the SE and the E&R mode for all UAs, FbU and SbU incorporating the versatility of adapting them to the clinical
performed slightly better in the E&R mode, contrary to ABU, situation, by application under different etching modes. In the
which showed a reverse trend. ABU and SbU showed no PTF, present study, the use of three of these UAs to dentine
while FbU had 3.1% (in SE mode) and 1.8% (in E&R mode) following a self-etch or an etch-and-rinse protocol did not
specimen pre-test failure rates. FbM and FbDC showed higher affect significantly their mTBS, but showed a very different
PTF percentages (7.7% and 13.5% respectively). dentine infiltration behaviour. They performed better than the
There were no significant differences between the mTBS two 1-SEAs used here regardless of the application mode.
results under SE and E&R mode after thermocycling of the The presence of MDP in the composition of SbU and ABU
three UAs utilized, namely FbU ( p = 0.819), ABU ( p = 0.388) and (Table 1), may well explain the higher mTBS of this groups in
SbU ( p = 1.000). Except for FbU, all other UAs showed the SE mode, before and after thermocycling. SbU also
significantly higher mTBS values than FbM and FbDC. There contains the polyalkenoic acid copolymer (the so called
were almost no PTF after thermocycling when specimens were Vitrebond Copolymer), which in combination with MDP has
treated with ABU, FbU (E&R mode) or SbU (0.75% in the E&R shown contradictory results in the literature. Perdigão et al.
mode), while there was an important increase in PTF for FbM reported higher mTBS to dentine of SbU when compared to
(22.8% vs. 7.7%) and FbDC (32% vs. 13.5%) and even more for Clearfil SE Bond, which has only the MDP monomer,7 while
FbU in the SE mode (43% vs. 3.1%).
Fractographic analysis under light microscope revealed a
predominance of failures in the adhesive layer for all groups. Table 3 – Penetration depth (mm) and hybrid layer
Nevertheless, most of the fractures occurred cohesively inside thickness (mm).
the adhesive, especially when treated with FbM and FbDC. The
Group Penetration depth Hybrid layer
thermocycling ageing did not alter this adhesive failure mode thickness
tendency.
SE E&R SE E&R
3.2. Penetration depth into dentine FbU 0 18–30 0 4
ABU 0 30–50 0 2.3
SbU 0 30–46 0 2.3
Table 3 summarizes the mean penetration depth values and
FbM 2–4 – 0 –
hybrid layer (HL) thicknesses for the different adhesives and FbDC 10–30 – 2.3 –
application modes. Neither penetration into dentine nor
SE, self-etch mode; E&R, etch-and-rinse mode.
hybrid layer formation was detectable for all UAs tested in
804 journal of dentistry 42 (2014) 800–807

Fig. 1 – CLSM images of the universal adhesives interfaces: (A–C) correspond respectively to FbU, ABU and SbU in SE mode.
(D–F) correspond to the same adhesives but in E&R mode. AL: adhesive layer; D: dentine; C: composite; OIL: oxygen
inhibition layer; T: resin tags; HL: hybrid layer.

Muñoz et al. observed a lower mTBS of SbU when compared to less, in this study SbU (SE mode) did not show a statistically
the same adhesive.22 The polyalkenoic acid copolymer may significant difference in mean mTBS when compared to ABU
compete with the MDP monomer for Ca-bonding sites in HAp 3 (which only contains MDP). In the Futurabond adhesives (FbU,
and due to its high molecular weight, could even prevent FbM and FbDC), the manufacturer describes its functional
monomer approximation during polymerization.22 Neverthe- monomer only as a phosphate monomethacrylate. When

Fig. 2 – CLSM images of the self-etch adhesives interfaces: (A) corresponds to FbM and (B) corresponds to FbDC. AL: adhesive
layer; D: dentine; C: composite; OIL: oxygen inhibition layer; T: resin tags; HL: hybrid layer.
journal of dentistry 42 (2014) 800–807 805

looking at the inferior bond strength results of the Futurabond hand, despite the fact that the application of the etching step
family, the absence of MDP in their formulation may be a prior to self-etch adhesives has shown to improve the hybrid
reasonable speculation, since its presence is not disclosed in layer thickness and resin tag formation, these interfaces
the product information sheet. showed significantly decreased bond strengths, with an
Following the acidity classification of self-etch adhesives, increased number of adhesive failures.5,14,37 The lower bond
the bonding agents tested in this study can be considered strength has been attributed to an incomplete infiltration of
ultra-mild (ABU, SbU), mild (FbU, FbM) or strong (FbDC). When the demineralized collagen network by the bonding resin.38
looking at the generated interface, none of the UAs applied in This shortcoming has been overcome in UAs through the
the SE mode modified the smear layer and penetrated into the addition of low viscosity monomers like HEMA, that increase
dentine tubules (Fig. 1A–C), which could be explained by their the affinity to the hydrophilic wet collagen network, as has
mild (or ultra-mild) acidity.19,27 The hybrid layer formed was been done earlier for one-step etch-and-rinse adhesives.
therefore very thin or inexistent (Table 3), resembling the Considering the ‘‘universal application’’ concept behind
results obtained by other studies with self-etch adhesives.28,29 these new adhesives, bond strength should not be compro-
FbDC, on the other hand, in concordance with its lower pH mised by the application mode used. In the present study, SbU
(1.5), infiltrated dentine up to a depth of 30 mm (Fig. 2B), and FbU slightly improved their mTBS after pre-etching, while
approaching penetration depths of conventional etch-and- ABU showed a slight reduction. However, none of these
rinse adhesives.16 differences were statistically significant. The first null hypoth-
Dentine smear layer is a barrier for some SEAs if contact to esis therefore has to be accepted. It is important to highlight,
intact dentine is desired.30 Indeed, milder self-etch adhesives that the non-inclusion of PTF in this study could have
show a lower penetration capacity of thick smear layers,29 generated overestimated strength bond values, especially in
when compared with stronger ones. In this study, a thin the SE-mode groups. The bond strength results of the same
artificial smear layer was created by means of grinding with UAs in the literature tend to agree with our findings. Marchesi
600-grit SiC paper, which can be matched to clinical smear layer et al. observed no significant differences in mTBS after 24 h of
thicknesses (1.3  0.5 mm) produced by fine-grained diamond artificial saliva storage of SbU when applied in SE (35.5 MPa) or
burs.17,30 As shown by FbDC, strong SEAs have demonstrated a E&R (34.8 MPa) mode.23 Nevertheless, after six months and
better ability to remove the smear layer19,29 and create thicker especially after 1 year storage, there was a significant drop in
hybrid layers.31,32 Nevertheless, higher aggressiveness of SEAs mTBS for the E&R treated groups. When compared to a
is usually not related to higher bond strengths.15,17,31,32 The conventional 2-SEA, SbU showed statistically better bonding
results of the present study are in agreement with these performance in every application mode (SE and E&R with dry
findings, since the lowest bond strengths were obtained by the or wet dentine), while no differences between its application
strong and intermediately strong SEAs (FbM and FbDC), while with or without the etching step were found.7 Muñoz et al.
the ultra-milder ones showed significantly higher values. This compared the effect of application mode on SbU and ABU.22
difference increased after thermocycling. It has been proposed, They found no statistical differences in bond strength between
that due to water presence in the dentinal tubules, some of the the SE and E&R modes for SbU (32.4 MPa and 35.1 MPa
acidic monomers of the strong SEAs retain their acidity and respectively), while there was an important drop in mTBS
continue etching, as a consequence of an incomplete polymer- for ABU when applied in the SE mode (13.4 MPa vs. 39.3 MPa in
ization.33,34 On the other hand, the MDP monomer (present in the E&R mode). Lee et al. observed a similar trend for ABU
the milder UAs tested here) has shown not only to chemically when applied in SE mode (8.1 MPa) in comparison to E&R mode
bond to HAp, but also to self-assemble into nanolayers,35 which (21.1 MPa),39 which has also been observed for other 1-SEAs
has strong hydrophobic properties that protect the formed under similar test designs.8,40 The application mode of ABU,
hybrid layer from hydrolytic degradation.3 without active brushing, was suggested as a possible cause for
The etching step ensures a deeper penetration of the self- the diminished mTBS in SE mode.22 In the present study,
etch adhesives into the dentine substrate, generating longer however, ABU was applied scrubbing the preparation surface,
resin tags,16,36 as well as thicker hybrid layers.14,15 When acid which could explain its similar mTBS in SE mode compared to
etching was applied prior to the adhesive (E&R mode), all UAs E&R mode. Higher mTBS values for these adhesives have been
showed deeper penetration into dentine (Fig. 1D–F) with reported when a second layer of the adhesive is applied,41
formation of long resin tags (up to 50 mm) and thicker hybrid which was associated with thicker and more resistant
layers (2–4 mm). The second null hypothesis therefore has to be adhesive interfaces. While ABU has shown decreased bond
rejected. Removal of smear layer and smear plugs by strength when applied in one layer,39 SbU adhesive perfor-
phosphoric acid,17 increased adhesive infiltration15,16 and mance was not affected by the second layer.41 This variable
facilitated the penetration of the UAs into the dentine tubules, seems to have no influence in the present study, since there
thus improving the tag length and morphology when were no significant differences in mTBS values between ABU
compared to their respective SE counterparts. Although there (applied in two layers) and SbU (only one layer).
was a better interface morphology after acid etching, its Thermocycling is a widely used technique to induce artificial
correlation to better mTBS values in self-etch adhesives has ageing by accelerated chemical degradation42 and contraction/
been brought into question.18 In one study, the use of expansion stresses due to the coefficient of thermal expansion
phosphoric acid prior to self-etch application in dentine mismatch between tooth substrates and the restorative
created well impregnated hybrid layers, which were associat- materials.43 The application of a thermocycling regime led to
ed to significantly improved mTBS values when compared to no significant mean bond strength variations among any of the
conventional application of the same 1-SEAs.13 On the other adhesives tested when compared to the 24-h water storage
806 journal of dentistry 42 (2014) 800–807

specimens. Notwithstanding, there were significant incre-


ments in pre-test failures for the Futurabond adhesives (SE Acknowledgements
mode) after thermocycling (Table 2), indicating a deleterious
effect of the ageing procedure on the bond interface of these This study was supported by Voco (Germany). Materials were
adhesives. This could be related to an insufficient chemical kindly donated by Bisco, 3M ESPE and Voco. We kindly thank E.
interaction to dentine, since FbU had no pre-test failures when Scheuermeyer, M. Schachtner and G. Stein for technical
additional micromechanical retention was generated (E&R assistance with the microtensile test and CLSM images.
mode). The third null hypothesis has to be partially rejected.
Despite the limited number of cycles (5000), which is regarded
to correspond to 6 month of in vivo functioning,42 may not seem references
enough for mimicking long-term bonding efficacy, other
studies on SEAs with longer cycling obtained similar
results.14,44 The efficacy of the thermocycling test in evaluating 1. Van Meerbeek B, Yoshihara K, Yoshida Y, Mine A, De Munck
bond strength has been questioned42 and highly conditioned to J, Van Landuyt KL. State of the art of self-etch adhesives.
specific test set-ups.43 The presence of surrounding dentine Dental Materials 2011;27:17–28.
2. Van Meerbeek B, De Munck J, Yoshida Y, Inoue S, Vargas M,
and composite could have avoided direct water contact with the
Vijay P, et al. Buonocore memorial lecture. Adhesion to
specimens, protecting them from accelerated hydrolysis,44
enamel and dentin: current status and future challenges.
while the low C-factor of the specimens could have diminished Operative Dentistry 2003;28:215–35.
the expansion/contraction stress effect.18 3. Yoshida Y, Yoshihara K, Nagaoka N, Hayakawa S, Torii Y,
Considering the short time elapsed since these new Ogawa T, et al. Self-assembled nano-layering at the adhesive
universal adhesives appeared in the market, only little clinical interface. Journal of Dental Research 2012;91:376–81.
outcomes are available in the literature. A clinical evaluation of 4. Peumans M, De Munck J, Van Landuyt KL, Poitevin A,
Lambrechts P, Van Meerbeek B. Eight-year clinical
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