Australian Dental Journal

The official journal of the Australian Dental Association

Australian Dental Journal 2011; 56:(1 Suppl): 31–44

doi: 10.1111/j.1834-7819.2011.01294.x

Current aspects on bonding effectiveness and stability in

adhesive dentistry
MV Cardoso,* A de Almeida Neves,* A Mine,* E Coutinho,* K Van Landuyt,* J De Munck,*
B Van Meerbeek*
*Catholic University of Leuven, School of Dentistry, Oral Pathology and Maxillo-facial Surgery, Department of Conservative Dentistry, Leuven
BIOMAT Research Cluster, Leuven, Belgium.

ABSTRACT
Improved dental adhesive technology has extensively influenced modern concepts in restorative dentistry. In light of
minimal-invasive dentistry, this new approach promotes a more conservative cavity design, which basically relies on the
effectiveness of current enamel-dentine adhesives. Nowadays, the interaction of adhesives with the dental substrate is based
on two different strategies, commonly described as an etch-and-rinse and a self-etch approach. In an attempt to simplify the
bonding technique, manufacturers have decreased the number of steps necessary for the accomplishment of the bonding
procedure. As a consequence, two-step etch-and-rinse and one-step (self-etch) adhesives were introduced and gained rapid
popularity in the dental market due to their claimed user-friendliness and lower technique sensitivity. However, many
concerns have been raised on the bonding effectiveness of these simplified adhesives, especially in terms of durability,
although this tends to be very material dependent. In order to blend all the adhesive components into one single solution,
one-step adhesives were made more acidic and hydrophilic. Unfortunately, these properties induce a wide variety of
seemingly unrelated problems that may jeopardize the effectiveness and stability of adhesion to the dental substrate. Being
more susceptible to water sorption and thus nanoleakage, these adhesives are more prone to bond degradation and tend to
fail prematurely as compared to their multi-step counterparts. Incidentally, another factor that may interfere with the
bonding effectiveness of adhesives is the technique used for caries removal and cavity preparation. Several tools are on the
market today to effectively remove carious tissue, thereby respecting the current trend of minimum intervention. Despite
their promising performance, such techniques modify the tooth substrate in different aspects, possibly affecting bonding
effectiveness. Altogether, we may conclude that not only the adhesive formulation, but also substrate nature must be taken
into account to achieve a stable bonding interface, rendering the restorative treatment more predictable in terms of clinical
performance. In this review, we analyse the current theoretical and clinical aspects of adhesion to enamel and dentine, and
discuss the diverse possibilities to overcome problems which nowadays still challenge clinicians in their achievement of a
more stable and effective bond to tooth enamel and dentine.
Keywords: Adhesion, bond strength, cavity preparation, caries removal, dental adhesive, dentine, enamel.

dental structure for additional mechanical retention.

INTRODUCTION
Although these restorations tend to fulfil the main
Improvements in dental adhesive technology have requirements of a more conservative and aesthetic
extensively influenced modern restorative dentistry. treatment, their clinical longevity is still a topical issue,
Nowadays, the surgical approach of ‘extension for mainly due to the degradation of the adhesive interface
prevention’ proposed by GV Black1 in 1917 is no longer over time.3 Clinically, the main cause of failure of
justifiable, and has been replaced by the concept of composite fillings is related to the occurrence of
‘minimally-invasive dentistry’.2 This modern approach marginal leakage, which eventually leads to marginal
focuses on the achievement of a more conservative discolouration, secondary caries, and subsequent loss of
cavity design, basically providing sufficient access for retention.4,5 This forces dentists to replace composite
the complete removal of the carious tissue. The restorations in relatively short intervals. In this context,
subsequent restorative procedure relies on the bonding several aspects should be considered with regard to the
effectiveness of adhesive materials such as resin com- bond strength and durability of adhesion to dental hard
posites, which do not require the removal of sound tissues. These include the heterogeneity of tooth
ª 2011 Australian Dental Association 31
MV Cardoso et al.

structure and composition, the hydrophilicity of the outcome involved the complete removal of the smear
exposed dentine surface, the features of the dental layer by a ‘total-etch’ and now better termed ‘etch-and-
substrate after cavity preparation6–8 and the character- rinse’ approach.6 In order to deal with the organic
istics of the adhesive itself, such as its physicochemical collagen mesh exposed following acid-etching dentine,
properties and its strategy of interaction with enamel these ‘adhesive systems’ provide a separate adhesion
and dentine.3,9 The present literature review deals with promotor or ‘primer’ that contains hydrophilic func-
modern concepts in adhesive dentistry, discussing issues tional monomers dissolved in an organic solvent.10 In a
that still challenge the achievement of an optimal third step, a hydrophobic resin is applied and penetrates
interaction between adhesives and dental substrates. the collagen network exposed by the acid-etching
For this purpose, a parallel is drawn among the procedure. These multi-step dental adhesives have been
currently available adhesive strategies and the main marketed since the early 1990s and can still today be
factors that interfere with their interaction with enamel considered as the ‘gold-standard’ adhesives. On the
and dentine. other hand, the market-driven demand for simplified
adhesive procedures has rapidly led to the introduction
of the alternative ‘self-etch’ approach. This bond
Interaction with dental hard tissues
strategy only dissolves the smear layer (but does not
The fundamental mechanism of bonding to enamel and remove it, as there is no rinse phase) and embeds the
dentine is essentially based on an exchange process in dissolved products within the interfacial transition
which minerals removed from the dental hard tissues zone.18
are replaced by resin monomers that upon polymeriza- Despite the major difference in the manner of etching
tion become micromechanically interlocked in the between etch-and-rinse and self-etch adhesives, the
created porosities.6,10 other fundamental steps for adhesion, namely the
Dissolution of superficial dental hard tissue is con- ‘priming’ and actual ‘bonding’ phase, can be either
ventionally achieved by phosphoric-acid etching, one of separate or combined.19 Etch-and-rinse adhesives
the major breakthroughs in adhesive dentistry intro- require either two or three steps depending on whether
duced by Buonocore more than 50 years ago.11 On the primer and bonding agent are separated or com-
enamel, acid-etching selectively dissolves the enamel bined in a single bottle. Similarly, self-etch adhesives
rods, creating microporosities which are readily pene- can be either one- or two-step systems depending on
trated, even by ordinary hydrophobic bonding agents, whether the self-etching ⁄ primer solution is separated
by capillary attraction.12 Upon polymerization, this from the bonding agent or combined with it. The latter
micromechanical interlocking of tiny resin tags within enables a single application procedure of a so-called
the acid-etched enamel surface still provides the best ‘all-in-one’ adhesive. Figure 1 shows the most recent
achievable bond to the dental substrate.6 It not only and accepted classification of adhesives currently avail-
effectively seals the restoration margins in the long able in the market according to Van Meerbeek et al.19
term, but also protects the more vulnerable bond to
dentine against degradation.13
Etch-and-rinse approach
Despite the reliability of adhesion to enamel, bonding
to dentine has been considered more difficult and less Etch-and-rinse adhesives are characterized by an initial
predictable. The main hindrance is the heterogeneous etching step, followed by a compulsory rinsing proce-
nature of dentine, with hydroxyapatite deposited on a dure which is responsible for the complete removal of
mesh of collagen fibres.10 In addition, dentine is smear layer and smear plugs. Concurrently, acid-
intimately connected with pulpal tissue by means of etching promotes dentine demineralization over a depth
numerous fluid-filled tubules, which traverse through of 3–5 lm, thereby exposing a scaffold of collagen
dentine from the pulp to the dentino-enamel junction. fibrils that is nearly totally depleted of hydroxyapa-
Once under constant outward pressure, this fluid tite.20,21 The following step consists of the application
renders the exposed dentine surface naturally moist of a primer containing specific monomers with
and thus intrinsically hydrophilic.15,16 This hydrophi- hydrophilic properties, such as 2-Hydroxy ethyl meth-
licity definitely represents one of the major challenges acrylate (HEMA), dissolved in organic solvents like
for the interaction of modern adhesives with dentine. It acetone, ethanol or water. While HEMA is responsible
has in essence led to the different bond strategies for improving the wettability and promoting the
currently available. re-expansion of the collagen network, the solvents are
The presence of cutting debris on instrumented able to displace water from the dentine surface, thus
dental surfaces in the form of smear layer and smear preparing the collagen network for the subsequent
plugs that obstruct the dentine tubules is also a primary adhesive resin infiltration.22,23 In the bonding step, a
co-factor that may not be underestimated.16,17 The first solvent-free adhesive resin is applied on the prepared
bonding protocol that revealed a clinically acceptable surface, leading to the penetration of hydrophobic
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 Bonding effectiveness and stability in adhesive dentistry

located beneath and ⁄ or within the hybrid layer, leaving

exposed collagen unprotected and thus more suscepti-
ble to degradation over time.27,28 Such nanometre-sized
voids can be depicted by infiltration of silver traces
in vitro, which has been referred to as nanoleakage
(Fig 3).29 Although occurring even in the absence of
interfacial gaps, nanoleakage seems to play a negative
role in bonding, especially in terms of durability.30,31 It
is noteworthy, however, that even the so-called gold-
standard adhesives seem to be incapable of preventing
nanoleakage,32 despite their satisfactory long-term
clinical performance.33
The technique sensitivity of etch-and-rinse adhesives
is mostly related to the etching step itself and to the
ostensibly antagonistic role of water in the bonding
protocol. It has been widely said that the demineralized
collagen network must be kept loosely arranged during
Fig 1. Classification of contemporary adhesives according to Van
Meerbeek et al.19 Adhesives within the same classification may vary adhesive procedures in order to allow proper resin
considerably in terms of composition and proportional amount of monomer infiltration.34 Actually, a certain amount of
ingredients. Two-step etch and rinse adhesives are also referred to as water is crucial to prevent the collagen network from
‘one-bottle’ systems, while one-step self-etch adhesives are often
referred to as ‘all-in-one’ systems. Note that each component, either collapsing,35 while an excessively wet surface may
primer or bonding or even self-etching adhesive can be presented in contribute negatively towards effective bonding to
two separate bottles that need to be mixed prior to application. dentine.36 In ‘over-wet’ conditions, excess water that
Therefore, one-step self-etch adhesives may be subdivided in one- and
two-component systems. is incompletely removed from the dentine surface seems
to cause phase separation between the hydrophobic and
hydrophilic components of the adhesive, resulting in the
monomers not only into the interfibrilar spaces of the formation of blister- and globule-like voids at the resin-
collagen network but also into dentine tubules. After dentine interface.37 Furthermore, excessive moisture on
infiltration, these monomers are polymerized in situ, the adherent substrate is also responsible for a lower
resulting in the formation of a hybrid layer, which in degree of resin monomer conversion, reducing the
combination with the presence of resin tags inside mechanical properties of the adhesive layer.38
dentine tubules provides micromechanical retention to Adhesive systems containing hydrophilic primers
the composite restoration (Fig 2).24 dissolved in acetone were found to produce higher
From the traditional three-step etch-and-rinse adhe- bond strengths when acid-conditioned dentine was left
sives, simplified two-step adhesives have been developed visibly moist prior to bonding, a protocol commonly
that combine the primer and the adhesive resin into one referred to as the ‘wet bonding technique’.39 However,
single solution. Despite presenting a more friendly determining how moist the dentine should be left
technique, these simplified adhesives tend to perform in during the adhesive procedure remains a major concern
an inferior manner when compared to their three-step and a clinical protocol that is difficult to standardize.
counterparts. By blending primer and bonding compo- Achieving a ‘window of opportunity’ between over-dry
nents in a single solution, simplified etch-and-rinse and over-wet conditions is still a challenge, since not
adhesives present a reduced ability to infiltrate the only extrinsic, but also intrinsic sources of humidity
demineralized dentine substrate, thereby producing must be considered when an adhesive procedure is
suboptimal hybridization.25 Moreover, the hydrophilic clinically performed. Self-evidently, over-drying by
nature of such adhesives render them more prone to which the acid-etched dentine surface is severely
water sorption and consequently more susceptible to the dehydrated should be avoided at any time during the
effects of hydrolytic degradation. The solvent present in clinical application procedure. Therefore, the surface
such adhesives is also more difficult to evaporate, should be gently dried until the etched enamel presents
frequently remaining entrapped within the adhesive its white-frosted appearance and dentine loses its shine
layer after polymerization.26 and turns dull.34
Classification aside, the infiltration of both two- and Interestingly, water-based primers have shown a
three-step etch-and-rinse adhesives into etched dentine potential self-rewetting effect on air-dried dentine.
has been shown to be only partially effective. There- Their water content seems to be sufficient to rehydrate
fore, complete replacement of the superficial mineral or re-wet the air-dried and then collapsed collagen
content, lost due to acid etching, remains practically network, transforming it into a loosely arranged
unattainable. As a result, voids are formed that may be structure that allows the hydrophilic primer monomers
ª 2011 Australian Dental Association 33
MV Cardoso et al.

Fig 2. Electron photo micrographs illustrating the interface of different adhesives bonded to dentine. (a) SEM image of the two-step etch-and-rinse
adhesive Single Bond (3M ESPE) bonded to dentine. Dentine was demineralized and deproteinized to expose the resin tags formed inside dentine
tubules. Thick hybrid layer (Hy) and long resin tags can be observed as a result of the etching step with a 30–40% phosphoric acid. On the other
hand, short resin tags and a barely visible hybrid layer can be observed in image (b) as a consequence of the interaction of dentine with a ‘mild’ two-
step self-etch adhesive (Clearfil SE Bond, Kuraray). (c) TEM image of the interface between the three-step etch-and-rinse adhesive Adper
Scotchbond Multi Purpose (3M ESPE) and dentine. A deeply demineralized hybrid layer of approximately 4 lm can be clearly visualized.
Conversely, the adhesive-dentine interaction showed in image (d) is characterized by a relatively thinner hybrid layer (about 1.0 lm), in which only a
partial demineralization has occurred as a consequence of the mild self-etch approach of Clearfil SE Bond. Note that the collagen fibrils remained
protected by hydroxyapatite, especially at the bottom half of the hybrid layer. A: adhesive; D: dentine.

as the wetness of the acid-etched dentine is con-

cerned.34
However, it must be emphasized that any remaining
solvent should be evaporated from the dentine surface
by air-drying the applied primer ⁄ adhesive.40 Non-
evaporated solvent may jeopardize polymerization of
resin monomers, creating undesirable voids in the
adhesive interface.38 Nevertheless, complete evapora-
tion of the solvent is difficult to achieve, especially in
water-based adhesives. To facilitate the evaporation of
the solvent in water-based adhesives, ethanol and
acetone can be used in conjunction with water as co-
solvents, resulting in an azeotropic mixture.9,42 This
implies the formation of hydrogen bonds between
Fig 3. TEM photomicrograph of the interface between dentine and water and ethanol ⁄ acetone molecules, resulting in a
the three-step etch-and-rinse adhesive CMF Adhesive System (Sare- more easily evaporated solvent.9
mco, St Galler, Switzerland) after infiltration with silver nitrate. Silver
deposition showed a typical spot-like distribution within the hybrid More recently, a new solvent named tert-butanol has
layer (Hy) and a localized cluster-like deposition at the bottom of the been introduced for the production of an innovative
hybrid layer (hand-pointer). Even multi-step adhesives have been two-step etch-and-rinse adhesive, XP Bond (Dentsply,
reported to present similar types of nano-leakage, by which the
relevance of such phenomena is still unclear. Konstanz, Germany). The results obtained so far seem
to be promising as this solvent presents an ethanol-like
vapour pressure, with better stability towards chemical
to interdiffuse.34 Therefore, in contrast with adhesives reaction with monomers.42 However, additional re-
containing acetone, water-based adhesives appear to be search and clinical trials are necessary to confirm the
less sensitive to variations in the bonding protocol as far advantages of tert-butanol-based adhesives.
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 Bonding effectiveness and stability in adhesive dentistry

to chemically bond to the mineral content of the

Self-etch approach
partially demineralized dentine.45
Differently from their etch-and-rinse counterparts, self- The desirable chemical bonding presented by some
etch adhesives do not require a separate etching step, as self-etch adhesives is related to the presence of specific
they contain acidic monomers that simultaneously etch functional monomers in their composition, such as 10-
and prime the dental substrate. Due to such acidic MDP, 4-META and phenyl-P. These monomers contain
characteristics, self-etch adhesives are able to dissolve carboxylic and phosphate groups that are able to
the smear layer and demineralize the underlying ionically bond with calcium in hydroxyapatite.49 How-
dentine ⁄ enamel.43 Consequently, this approach has ever, it has been shown that the chemical bonding
been claimed to be more user-friendly and less promoted by 10-MDP is not only more effective but
technique-sensitive, thereby resulting in a clinically also more stable in an aqueous environment than that
reliable performance.33 Nowadays, however, many provided by 4-MET and phenyl-P.45,50 Clearfil SE Bond
concerns have been raised about the bonding effective- (Kuraray) is a 10-MDP-based two-step self-etch adhe-
ness of self-etch systems, especially in terms of dura- sive and has been proven to yield reliable results in
bility, although it may be material dependent.3 Indeed, terms of bonding effectiveness and durability when
some of them have proved to perform satisfactorily, compared to other commercially available self-etch
both clinically and in the laboratory.33 adhesives.33 Other adhesives from the same manufac-
The morphological features of the hybrid layer turer, such as Clearfil S3 Bond, Clearfil Protect Bond,
produced by self-etch adhesives depend to a great and Clearfil Liner Bond, also contain the 10-MDP
extent on the ability of their functional monomers to monomer in their composition.
demineralize the dental substrate. Therefore, according Generally, the bonding effectiveness of self-etch
to their acidity or etching aggressiveness, self-etch adhesives has been attributed to their ability to
adhesives can be classified as strong (pH £ 1), demineralize and infiltrate the dentine surface simulta-
intermediate (pH » 1.5) and mild (pH ‡ 2).44 Strong neously to the same depth, theoretically preventing
self-etch adhesives, such as Adper Prompt-L Pop incomplete penetration of the adhesive into the exposed
(3M ESPE), produce rather deep demineralization collagen network.51 However, traces of nano-leakage
effects in both enamel and dentine. The interfacial have been reported along the resin ⁄ dentine interfaces
ultramorphological features promoted by these adhe- produced by some of these self-etch adhesives, thereby
sives on dental substrates resemble those of etch-and- challenging the original concept of a highly effective
rinse systems, despite the fact that the products sealing ability.52 It has been suggested that acidic
originated from demineralization are not rinsed away. monomers of some self-etch adhesives (in particular the
On the other hand, mild self-etch adhesives deminer- simplified one-step versions) are gradually buffered by
alize dentine only partially, leaving a substantial the mineral content of the substrate. At this stage, such
amount of hydroxyapatite crystals around the collagen weakened monomers are only able to partially etch
fibrils. This remains available for possible additional dentine.52 As a consequence, zones of partially demin-
chemical interaction (Fig 2d).44 This twofold bonding eralized but non-infiltrated dentine may be formed
mechanism (i.e. micromechanical and chemical adhe- beneath the hybrid layer, defeating the conventional
sion) is believed to be advantageous in terms of wisdom that such adhesives do not exhibit discrepan-
bonding effectiveness and durability.45 The hybrid cies between the depth of demineralization and the
layer formed by such adhesives is no deeper than 1 lm depth of resin infiltration. This phenomenon, however,
and resin tags are hardly observed (Fig 2b).44 Never- is not common to all self-etch systems and seems to be
theless, neither the thickness of hybrid layer, nor the material dependent, although affecting both one- and
length of resin tags seem to be important for the two-step self-etch adhesives.52
achievement of bonding effectiveness and stability.46,47 Another factor that may interfere with the bonding
A more recent adhesive presents a relatively low effectiveness of a self-etch adhesive is the type of
acidity (pH2.7) and, consequently, a considerably smear layer produced on the dental substrate.17,53
reduced ability to dissolve the smear layer and Depending on the technique and instrument used for
demineralize the underlying dentine surface. Being cavity preparation, the smear layer can vary in
referred to as an ultra-mild self-etch adhesive, Clearfil thickness, density and degree of attachment to the
S3 Bond (Kuraray) can only very superficially expose underlying tooth structure (Fig 4).54 As self-etch
collagen on dentine, creating a characteristic nanome- adhesives interact with the smear layer rather than
tre-sized hybrid layer, which has been termed a eliminating it, their acidic potential may be buffered
nano-interdiffusion zone.48 However, the key factor by the mineral content of a thick and dense smear
in this ultra-mild adhesive is related to the presence of layer.55 This may hence result in a poor interaction
10-MDP in its composition and its consequent ability with the underlying substrate.53 Obviously, the less

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MV Cardoso et al.

Fig 4. Feg-SEM photomicrographs of fractured dentine (a) and dentine surfaces prepared with different cavity preparation techniques (b–f): (a)
fractured dentine resulted in a rather flat and smear-free surface, exposing the typical structure of a sound dentine tissue; (b) bur-cut dentine shows a
surface entirely covered by a smear layer. The irregularities of the diamond bur produced a scratched dentine surface, with well-defined tops and
valleys. Note that the smear layer is thicker at the tops (left side) as compared to the valleys (right side), where the entrances of the dentine tubules are
barely apparent; (c) diamond tip used in ultrasound produced a relatively regular surface covered by a rather thin smear layer. Not only plugged, but
also opened dentine tubules may be observed; (d) irradiated dentine using an Er:YAG laser (31.5 J ⁄ cm2, 200 mJ, 10 Hz, 100 ls) resulted in a smear-
free surface with open dentine tubules and prominent peritubular dentine. Note the irregular and rugged aspect of the surface and its typical
undulating pattern; (e) dentine substrate after chemo-mechanical caries exaction with Carisolv shows open dentine tubules and visible intertubular
dentine with a certain amount of exposed collagen fibrils (caries-affected dentine); (f) sono-abrasion with a diamond tip resulted in a flat surface
covered by a relatively thick smear layer and plugged dentine tubules.

acidic the adhesive, the more the smear layer may purpose, these adhesives have been made more acidic
interfere with bonding.17 Therefore, techniques and and more hydrophilic than their two-step counterparts.
instruments that produce thinner and less compact These properties may, however, lead to a wide variety
smear layers should be preferred during cavity prep- of seemingly unrelated problems that may jeopardize
aration. Finishing the cavity walls with an extra-fine the effectiveness and stability of adhesion to a dental
diamond bur results in thinner smear layers, which substrate.58 Actually, none of the contemporary all-in-
consequently may promote a better interaction one adhesives can compete with the more traditional
between mild and ultra-mild self-etch adhesives and multi-step systems in terms of bond effectiveness and
the dental substrate.17 durability.3,44,47,59,60
Regarding adhesion to enamel, it has been reported One of the main disadvantages of one-step self-etch
that some self-etch adhesives bond reasonably well to adhesives is related to their excessive hydrophilicity that
ground enamel, but there are general concerns nowa- makes the adhesive layer more prone to attract water
days about the adhesion of such adhesives to unground from the intrinsically moist substrate.58 Due to such
aprismatic enamel where micromechanical retention is increased water affinity, these adhesives have been
hardly achieved.56,57 Thus, preparing bevelled cavosur- reported to act as semi-permeable membranes, even
face margins is helpful for improving the bonding after polymerization, allowing water movement from
effectiveness of self-etch adhesives in cavities whose the substrate throughout the adhesive layer.61 As a
margins are placed in enamel.57 consequence, small droplets can be found at the
transition between the adhesive layer and the lining
composite, especially when polymerization of the latter
Concerns about one-step self-etch adhesives
is delayed (Fig 5a). Besides promoting a decrease in
Attempting to provide faster and thus more user- bond strength between composite and substrate,62 such
friendly adhesives, manufacturers have introduced permeability of the adhesive layer seems to contribute
one-step self-etch adhesives which etch, prime and to the hydrolysis of resin polymers and the consequent
bond the dental substrate simultaneously. For this degradation of tooth-resin bond over time.13,63,64
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 Bonding effectiveness and stability in adhesive dentistry

In this context, the presence and concentration of step self-etch adhesive (G-Bond, GC) in comparison to
HEMA in the adhesive’s composition must be ad- a HEMA-containing adhesive of the same category
dressed. HEMA is a water-soluble methacrylate mono- (Clearfil S3 Bond, Kuraray). Up to two years of clinical
mer frequently present in the composition of dental service, a satisfactory performance was observed for
adhesives to increase their wettability and hydrophilic- both adhesives (Fig 6).70 Obviously, longer-term clin-
ity.22,66 Moreover, when incorporated in relatively high ical evaluation is needed in respect to bond durability.
concentration, it improves the miscibility of hydropho-
bic and hydrophilic components in an adhesive solu-
Adhesion to carious tissue
tion.62 However, disadvantages have also been related
to the presence of HEMA, especially when it is The most convenient substrate to test the bonding
incorporated in high amounts (HEMA-rich adhesives). performance of dental adhesives in laboratory studies is
Besides the potential allergenic effects of its uncured sound (‘normal’) dentine. However, this standard
monomer,67 HEMA may increase the water sorption of ‘laboratory’ dentine differs from the kind of dentine
adhesives, adversely influencing the mechanical prop- that clinically remains after carious tissue was removed.
erties and stability of the adhesive interface.13,68 These Caries excavation frequently results in a complex
drawbacks have led to the introduction of HEMA-free substrate involving areas of caries-infected, caries-
mild one-step self-etch adhesives in an attempt to create affected, sclerotic, eroded and sound dentine (Fig 7).
a less hydrophilic adhesive that could promote a more Following a more conservative cavity-preparation con-
durable bond to dental substrates.69 However, it must cept, the current aim of caries excavation is limited to
be considered that the absence of HEMA makes the removal of the outer highly infected and denatur-
the adhesive more prone to the occurrence of the ated dentine,8,71 preserving the inner layer of caries-
so-called phenomenon of phase separation. In this affected dentine that still possesses a high potential to
process, once ethanol ⁄ acetone starts to evaporate, the remineralize.72 However, clinically distinguishing be-
solvent-monomer balance is broken, with water tween caries-affected and caries-infected dentine is
separating from the other adhesive ingredients.69 When definitely not straightforward (Fig 8). Depending on
the adhesive is cured, these water blisters become the clinical perception of the operator and the technique
entrapped in the adhesive layer (Fig 5b), probably used for caries removal, caries-infected dentine may
jeopardizing the bonding effectiveness.62 To prevent remain in the cavity and also needs to be bonded as
phase-separation droplets from being embedded in the effectively as possible. Obviously, such ‘abnormal’
polymerized adhesive, a strong, prolonged air-blowing substrates are characterized by structural variations
should be performed before polymerization so as to that may represent a challenge to achieve optimal
remove them from the adhesive layer. How successful adhesion.73
this technique can be performed clinically remains a In general, the presence of carious dentine results in a
concern.69 Meanwhile, a controlled amount of HEMA thicker hybrid layer and lower bond strength.72,74–76
should be preferred that strikes the right balance The bonding effectiveness of adhesives to carious
between HEMA-free and HEMA-rich self-etch dentine has been reported to be inversely proportional
adhesives. to the degree of caries progression, with caries-infected
One of our most recent clinical Class V studies dentine yielding the lowest bond-strength results.72,76
evaluates the clinical performance of a HEMA-free one- This sort of substrate is characterized by an extremely

Fig 5. Electron micrographs illustrating the occurrence of droplets at the resin-dentine interface. (a) Failure analysis of a specimen of composite
bonded to dentine using the one-step self-etch adhesive Clearfil S3 Bond (Kuraray) after fracture under micro-tensile bond strength testing. The
insert shows the Feg-SEM image of the fracture plan of the composite side of the specimen. These voids have been formed as a consequence of water
flow from the substrate through the semi-permeable adhesive layer, due to osmosis. (b) TEM photomicrograph of the interface between dentine and
the HEMA-free one-step self-etch adhesive G-Bond (GC). Note the presence of droplets entrapped at the bottom of the adhesive layer due to the
phase-separation phenomenon and thus an insufficiently air-blown adhesive.
ª 2011 Australian Dental Association 37
MV Cardoso et al.

Fig 6. Graphs showing the retention rate (%) and overall success rate of 2 one-step self-etch adhesives in Class V restorations up to 2 years of clinical
service. G-Bond is a HEMA-free adhesive while Clearfil S3 Bond does contain HEMA in its composition. Observe the satisfactory performance of
both adhesives after a 2-year follow-up. Overall clinical success includes the evaluation of retention rate, caries recurrence, marginal integrity and
discolouration. Note that the Y-axes start at 80%.

Fig 7. Different residual dentine substrates left for further adhesive procedures after caries removal with a chemo-mechanical method (Carisolv),
ranging from lightly (a), to mixed (b) and darkly stained residual dentine (c).

low cohesive strength, which should be attributed to its organic components.78 This results in a substrate of
high degree of demineralization and disorganized inferior mechanical properties74,79 and increased sus-
collagen matrix. Considering that resin-monomer infil- ceptibility to the effects of acid etching.71,72,80,81
tration is incomplete at caries-infected dentine, a Although enabling a thicker hybrid layer to be formed,
compromised bonding effectiveness can be ex- this highly permeable substrate also results in a
pected.72,76 Therefore, caries-infected dentine should disproportional penetration of resin monomers. They
best be removed as much as possible. Occasionally, an are not able to completely fill the voids of such a thick
exception can be made to prevent further progression of
the disease in the case of uncooperative patients, while
working on behaviour control and ⁄ or planning other
treatment strategies.
The issue of bonding to caries-affected dentine has
been considered more controversial. Normally, in light
of the concept of minimal-invasive dentistry, one could
bond to caries-infected dentine provided that the cavity
margins are placed in sound dentine or enamel.8,77
Nevertheless, one should not neglect that this modified
substrate may result in a lower bonding effectiveness
and sealing when compared to sound dentine.74,75
These less favourable outcomes are basically related to
important alterations that normally occur in dentine as
a consequence of caries progression. Besides presenting Fig 8. A typical cavitated occlusal caries lesion seen on a mesio-distal
a significant reduction in its mineral content, caries- stereomicroscopic section is delimited by the full black lines.
affected dentine undergoes an important loss in the Transparent blue area corresponds to caries-unaffected dentine
reactions. The different shades of dashed lines indicate possible
crystallinity of its remaining mineral phase, as well as morphological endpoints for caries removal, illustrating some of the
considerable changes in the secondary structure of its variability to which this parameter is exposed.
38 ª 2011 Australian Dental Association
 Bonding effectiveness and stability in adhesive dentistry

mineral-depleted zone,82 rendering the adhesive inter-

Relation between caries-removal techniques and
face more prone to water degradation over time.80,83
adhesion
In contrast to the high intertubular dentine perme-
ability mentioned above, the penetration of resin As an alternative to the use of diamond and carbide
monomers into the dentine tubules of caries-affected rotatary instruments, several techniques for caries
dentine is usually impaired due to the presence of removal and cavity preparation, thereby employing
acid-resistant mineral casts, like those formed by different concepts and technologies, have been intro-
b-tricalcium phosphates.74,81,84 Such structures, also duced to the market. The one common aspect of all
called ‘whitlockite’, are deposited into the dentine these techniques is the promotion of a more conserva-
tubules during the early phases of dentine reaction tive cavity-preparation approach, aiming to minimally
against further caries progression.80,85 Besides hinder- remove sound tissue. Subsequently, a filling material is
ing intratubular penetration and, consequently, required that can bond to the dental substrate without
resin-tag formation, such enhanced impermeability the need of additional mechanical retention. Therefore,
impairs also the sideways diffusion of resin monomers the influence of the resulting substrate on the bonding
via the dentine tubules to the deepest demineralized effectiveness of dental adhesives is an issue that deserves
dentine.85 This poorly infiltrated substrate, along with further attention.
the low mechanical properties of the caries-affected The use of erbium-laser devices for cavity prepara-
dentine, has been pointed out as the most logical tion, for example, has gained popularity as a technique
explanation for the lower bond strengths obtained to that provides the patient with more comfort during
such a substrate as compared with that to sound treatment. The substrate that results from laser ablation
dentine.72 shows a particular undulating surface pattern with
As described so far, the type of substrate on which complete absence of surface smear (Figs 4d and 9a).
the adhesive is applied strongly influences its bonding This could improve the bonding effectiveness of adhe-
effectiveness. From another standpoint, particular sives, especially that of mild and ultra-mild self-etch
characteristics of the adhesive selected should also be adhesives.17 However, despite some minor disagree-
considered, such as its specific approach and composi- ments in the literature, there is a certain consensus
tion.83 In general terms, there is no ‘ideal’ adhesive to among researchers that laser-irradiated dentine nega-
bond to caries-affected dentine. Alternatively, the tively affects the bonding effectiveness of resin-based
alleged fluoride-releasing properties of some adhesives adhesives.7,90–92 These disappointing results are related
such as the Optibond adhesives (Kerr), One-up Bond F not only to the presence of subsurface micro-cracks that
Plus (Tokuyama, Tokyo, Japan) and Clearfil Protect are induced during irradiation (Fig 9b),7,91 but also to
Bond (Kuraray) could be beneficial for inhibiting the occurrence of alterations in the chemical composi-
development of secondary caries and for promoting tion of dentine and especially its organic matrix.93
remineralization of caries-affected dentine.86,87 It is, Some other cavity-preparation techniques, such as
however, unclear whether the amount of fluoride ultrasono-abrasion, and air-abrasion have also been
released by such adhesives is sufficient to promote reported as alternative techniques for cavity prepara-
remineralization and prevent demineralization. tion, although their effectiveness in removing carious
This still remains a controversial issue. Some adhesives tissue remains debateable.8 Both techniques produce a
that contain antibacterial monomers have also discrete smear layer but no noticeable damage to the
been reported to inhibit caries progression underneath substrate (Fig 4c), which may result in a more effective
adhesive restorations thanks to their strong bactericidal interaction of even mild self-etch adhesives with
activity.88 For example, Clearfil Protect Bond (Kuraray) dentine, and thus a better bond.6 However, the use of
incorporates the monomer 12-methacryloyloxydo- sono-abrasion seems to less effectively remove surface
decylpyridinium bromide (MDPB), and was shown to smear than ultra-sono abrasion (Figs 4c and d). Obvi-
possess a significant antibacterial effect in the labora- ously, surface smear hardly interferes with the bonding
tory, even after polymerization.89 Unfortunately, there potential of etch-and-rinse adhesives, since the phos-
is still a need for further investigation, especially to phoric acid readily dissolves and removes all smear
provide evidence that such antibacterial property upon rinsing.6
clinically also results in longer-lasting composite resto- The use of chemo-mechanical excavation has also
rations.9 Irrespective of fluoride release and antibacte- received new interest as a less-invasive method for
rial properties, the adhesive that performs most favour- caries removal. This procedure consists of the use of a
ably on sound dentine will probably also be the best gel based on a mixture of sodium hypochlorite, amino
option to bond to caries-affected dentine. As reported acids and water (Carisolv, MediTeam Dental, Säveda-
for normal dentine, etch-and-rinse adhesives tend to lem, Sweden). Its working principle is based on
result in higher bond strengths to both sound and cleavage of exposed and denatured collagen of carious
caries-affected dentine than self-etch systems.74,83 dentine, thereby facilitating its removal manually using
ª 2011 Australian Dental Association 39
MV Cardoso et al.

an excavator with rounded edges. Using Carisolv, caries trials remain the ultimate way to collect scientific
is excavated to the same extent as corresponding to the evidence on the clinical effectiveness of a restorative
auto-fluorescent signature of carious tissue, when treatment.101 The popularity of laboratory studies in
evaluated using confocal microscopy.94 The chemical the field of adhesive dentistry may in part be ascribed to
composition and microstructure of sound dentine does the rapid evolution of dental adhesive technology and
not seem to be significantly altered by the use of the resultant high turnover of adhesive systems. This
Carisolv.95,96 Its chloride is not able to interact with often tempts manufacturers to release a successor
collagen fibrils that are protected by the mineral content product on the market even before its precursor has
of sound dentine.97 Therefore, it has been reported that been clinically evaluated, at least in the long term. By
the use of this technique does not affect the bonding carrying out in vivo studies, all possible ageing factors
effectiveness of dental adhesives, provided that the are concurrently evaluated. Retention, marginal integ-
carious tissue is completely removed (Fig 4e).97,98 rity and clinical microleakage are usually the key
With the purpose of providing clinicians a rotating parameters recorded to judge upon clinical perfor-
instrument that could selectively remove carious den- mance of adhesives.
tine, polymeric burs have recently been introduced to The best clinical performance with regard to
the market (SmartPrep, SS-White Burs; Lakewood, NJ, retention (the most objective criterion to judge
USA). These burs are made of a polymer (PEKK, upon clinical effectiveness) has so far been achieved by
polyether-ketone-ketone) with a particular hardness of glass-ionomers.33,100 Their low annual failure rates can
50 KHN, which is higher than the hardness of carious be ascribed to their unique self-adhesiveness, based on
dentine (0 to 30 KHN), but lower than that of sound the twofold micromechanical and chemical bonding
dentine (70 to 90 KHN).99 Therefore, it is not mechanism.19,45 Nevertheless, despite their excellent
surprising that both the cutting efficiency and efficacy clinical performance in terms of retention, glass-iono-
of these burs decreases early as soon as sound dentine is mers are commonly associated to poorer aesthetic and
touched. This obviously compromises the effectiveness mechanical properties when compared to resin-based
of these burs.100 Adhesion to dentine remaining after restorative materials.103,104 Besides glass-ionomers,
the use of these polymeric burs has been reported to be three-step etch-and-rinse adhesives have exhibited a
negatively affected by the fact that residual caries reasonably good clinical effectiveness.33,105 Some of
commonly remains after excavation.99,100 A new ver- these adhesives, such as Optibond FL (Kerr) and its
sion of these burs have recently been marketed (Smart- predecessor Optibond Dual Cure, have been related to
Burs, SS-White Burs; Lakewood, NJ, USA), although an excellent performance with 94% and 93% of
further studies are still necessary. Actually, any kind of retention rates being registered after 13 and 12 years
cavity preparation that is not successful in completely of clinical follow-up, respectively.101,105 The durability
eliminating carious tissue may represent a challenge for of three-step etch-and-rinse adhesives confirms their
currently available adhesives to bond effectively. generally superior laboratory results, being currently
considered as ‘gold-standard’ among other adhesive
approaches.101
Clinical performance
According to the same standard, mild two-step self-
Despite the importance of laboratory studies attempt- etch adhesives tend to approach three-step etch-and-
ing to predict the performance of biomaterials, clinical rinse adhesives in terms of low annual failure rates.33 In

Fig 9. Electron photo micrographs illustrating the morphological aspects of dentine after laser irradiation (4.0 W, 20 Hz, 71.4 J ⁄ cm2 and 140 ls)
with an Er,Cr: YSSG laser (Waterlase, Biolase Technology, San Clemente, CA, USA). (a) Feg-SEM photomicrograph of a cross-section of dentine
surface after laser treatment. Note the irregularities produced by laser ablation, resulting in an imbricate patterned surface. (b) Non-demineralized
and non-stained TEM photomicrograph of the interface between Clearfil SE Bond and laser-irradiated dentine (D). Despite the clear interaction
between adhesive (A) and substrate, microcracks (arrows) can be observed at the dentine subsurface as a result of laser ablation. Hy: hybrid layer.
40 ª 2011 Australian Dental Association
 Bonding effectiveness and stability in adhesive dentistry

this context, Clearfil SE Bond has been the most tested When bonding to enamel, an etch-and-rinse ap-
adhesive and is frequently employed as a control group proach is definitely preferred, indicating that simple
due to its satisfactory performance clinically.101,106 Its micromechanical interaction appears sufficient to
ability to provide a shallow but uniform hybrid layer, achieve a durable bond to enamel. On the other hand,
along with its capability to chemically bond to the the mild self-etch approach seems to provide superior
dentine substrate seems to play an important role to performance when bonding to dentine, as it addition-
resist long-term hydrolytic degradation. Commonly, ally chemically interacts with residual hydroxyapatite,
the clinical performance of such self-etch adhesives does which definitely contributes to bond durability.
not vary substantially from one study to another, which Altogether, when bonding to both enamel and
is indicative of their rather low technique-sensitivity. dentine, selective etching of enamel followed by the
Altogether, it is not surprising that such adhesives are application of the self-etch adhesive to both (etched)
usually related to very low levels of postoperative enamel and (non-etched) dentine may represent the
sensitivity.107 best option to effectively and durably bond to the
In general, two-step etch-and-rinse adhesives have dental substrate. Moreover, the quality of the substrate
performed less favourably than the conventional to which the adhesive is applied is of paramount
three-step version, sometimes not even meeting the importance to achieve effective and durable bonding.
previous American Dental Associaton full acceptance In this context, many variables should be taken into
guidelines.33,108 Laboratory studies have corroborated account such as the technique used for cavity prepa-
these results, ascribing their poorer performance to ration and the approach employed during caries
their higher hydrophilicity and reduced hybridization removal. Despite the current trend towards more
potential. It is noteworthy that irrespective of the conservative intervention, one must be aware that
number of application steps, acetone-based etch-and- adhesion to carious tissue reduces the bonding effec-
rinse adhesives have performed less satisfactorily tiveness and bond durability.
than their water ⁄ ethanol-based alternatives.33,108 The Along with the fast evolution of multi-step adhesives
above-mentioned high technique-sensitivity of acetone- towards one-step adhesives, luting composites to bond
based adhesives must be the reason for their compro- indirect ceramic restorations underwent a similar
mised long-term clinical results. evolution towards simple-to-use and less technique-
At this point in time, the clinical performance of one- sensitive one-step luting agents. Hence, these so-called
step adhesives has been shown to be less predictable. self-adhesive luting composites do not need any kind of
Widely varying retention scores have been recorded, pre-treatment of the tooth substrate, thereby bringing
indicating their higher technique sensitivity despite the development of self-adhesive composites closer to
them being more user-friendly.33,109,110 Such lower reality.
bonding performance must be ascribed to the many
concerns advanced earlier. Interestingly, Clearfil S3
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2010;26:e100–121. Dr B Van Meerbeek
102. van Dijken JW, Pallesen U. Long-term dentin retention of etch- Catholic University of Leuven
and-rinse and self-etch adhesives and a resin-modified glass io- Department of Conservative Dentistry
nomer cement in non-carious cervical lesions. Dent Mater
2008;24:915–922.
Leuven BIOMAT Research Cluster
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Kapucijnenvoer 7
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zation methods, and a resin-modified glass ionomer in non-car- Belgium
ious cervical lesions. J Contemp Dent Pract 2006;7:42–53.
Email: bart.vanmeerbeek@med.kuleuven.be

44 ª 2011 Australian Dental Association