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334 PERDIGAO
Silane
Dental adhesive
Dental adhesive
Etched enamel
Fig. 1. Adhesive joint formed between enamel and etched porcelain. HF, hydrouoric acid.
forms a uniform coating on enamel and dentin and plugs the entrance of the
dentinal tubules, reducing the permeability of dentin (Fig. 2). The smear
layer is porous and permeable as a result of submicron channels that allow
the dentinal uid to pass through [4]. The basic composition of the smear
layer is hydroxyapatite and altered collagen with an external surface formed
by gellike denatured collagen [7]. The morphology of the smear layer is de-
termined to a large extent by the type of instrument that creates it and by the
site of dentin where it is formed [8,9].
Fig. 2. Field emission scanning electron micrograph of dentin smear layer and smear plug.
DENTAL ADHESION 335
Etch-and-rinse strategy
With the etch-and-rinse strategy, dentin and enamel are treated with an
acid gel (commonly phosphoric acid) to remove the smear layer and demin-
eralize the most supercial hydroxyapatite crystals (Fig. 7). Following this
chemical etching, a mixture of resin monomers (primer/adhesive) dissolved
in an organic solvent is applied to inltrate etched dentin [10]. The resin
monomers permeate the water-lled spaces between adjacent dentin colla-
gen bers that used to be occupied by hydroxyapatite crystals. This inltra-
tion results in a hybrid tissue composed of collagen, resin, residual
hydroxyapatite, and traces of water (see Fig. 3) known as the resindentin
interdiusion zone, rst described in 1982 as the hybrid layer [11]. This in-
timate micromechanical entanglement of resin monomers with etched dentin
Self-etch strategy
The latest development in dental adhesion is based on simplication and
reduced application time. These self-etch (nonrinsing) adhesives do not
require a separate acid-etch step as they condition and prime enamel and
dentin simultaneously by inltrating and partially dissolving the smear layer
Fig. 7. Field emission scanning electron micrograph of dentin etched with 40% phosphoric acid
for 15 seconds. Note the collagen bers deprived from hydroxyapatite crystals as a result of acid
demineralization. The more intense decalcication around the peritubular area may be a result
of both the high mineral content of the peritubular region and the easier penetration of the acid
through the tubular lumen.
338 PERDIGAO
Fig. 8. Field emission scanning electron micrograph of a resindentin interface formed with
Clearl S3 Bond (Kuraray). The neck of the resin tag contains residual smear layer particles.
Ad, adhesive; D, dentin; RT, resin tag; SP, resin-impregnated smear plug.
DENTAL ADHESION 339
Table 1
pHa of self-etch adhesives
Adhesive (manufacturer) pH
AdheSE (Ivoclar Vivadent) 1.7
Adper Prompt L-Pop (3M ESPE) 0.91.0
Clearl S3 Bond (Kuraray) 2.4
Clearl SE Bond (Kuraray) 1.8
iBond (Heraeus Kulzer) 2.2
Xeno IV (Dentsply Caulk) 2.5
a
pH of 35% silica-thickened phosphoric-acid gel 00.4.
Data from Refs. [1922].
Fig. 10. Transmission electron micrograph of resindentin interface formed with Clearl S3
Bond (Kuraray). Deposits of silver grains may correspond to areas of residual water. D, dentin;
H, hybrid layer.
DENTAL ADHESION 341
inltration into the hybrid layer [38]. One manufacturer recommends rub-
bing the adhesive continuously for 15 seconds, followed by the application
of a second coat after gentle air-drying and curing the rst coat. This second
coat prevents the formation of dry spots on the dentin surface and may
result in better impregnation of the monomers into the hybrid layer, as
observed in Figs. 11 and 12.
Low enamel and dentin bond strengths have been reported when acetone-
based all-in-one adhesives are applied as per manufacturers directions
[33,37]. These adhesives result in severe enamel microleakage following ther-
mal stresses [39,40]. When applied to one-surface occlusal preparations, one
of the most popular acetone-based all-in-one adhesives is not able to with-
stand polymerization shrinkage stresses nor thermocycling, resulting in
a high percentage of pretesting debonds [33]. Several mechanisms may ac-
count for this poor performance as compared with adhesives with dierent
solvents. The magnitude of dentin bond strengths depends on the degree
of inltration of the resin monomers into the collagen pretreated with an
acidic conditioner or with phosphoric acid [41]. The authors electron mi-
croscopy analyses (Figs. 13 and 14) have demonstrated that acetone-based
all-in-one adhesives result in a hybrid layer 0.2 to 0.5 mm thick, interfacial
gaps, and limited resin penetration into the dentinal tubules. It is known
that hybrid layers are particularly susceptible to degradation when the
cavo-surface margins are not in enamel [42]. The degradation of the dentin
bonding interface is caused by the availability of exposed collagen brils at
the base of hybrid layer [43] or by hydrolytic degradation of resin compo-
nents in the hybrid layer [28,4345]. Water can also inltrate and plasticize
Fig. 11. Field emission scanning electron micrograph of the dentin hybridization formed upon
application of two coats of Adper Prompt L-Pop. Note the inltration of the material into the
dentin tubules and the absence of interfacial gaps. When Adper Prompt L-Pop is applied in one
coat, a separation gap forms between the adhesive and the hybrid layer (not shown). Ad, adhe-
sive; Comp, composite restoration; D, dentin; H, hybrid layer.
342 PERDIGAO
Fig. 12. Transmission electron micrograph of the dentin hybridization formed upon appli-
cation of two coats of Adper Prompt L-Pop (3M ESPE). Note the reticular morphology of
the hybrid layer corresponding to the resin embedding of the collagen bers. Ad, adhesive;
C, composite particle; D, dentin; H, hybrid layer.
the resin matrix, which decreases the mechanical properties of the polymer
[46].
Other factors may play a role in the weak bonding performance of ace-
tone-containing all-in-one adhesives. Porosities (or blisters) occur at the
enamel and dentin bonding interfaces because most all-in-one adhesives
behave as semipermeable membranes [31,33,4749]. These porosities may
be a result of water accumulation either caused by an osmotic gradient or
by monomersolvent phase separation upon evaporation of the acetone
[21,49]. The number and size of these blisters may also depend on the inten-
sity of the air-drying step [47].
High hydrophilicity, and consequent higher water sorption, has been re-
ported associated with another acetone-based all-in-one adhesive containing
Fig. 13. Field emission scanning electron micrograph of a resindentin interface formed with
G-Bond (GC America). Ad, adhesive; Comp, composite restoration; D, dentin.
DENTAL ADHESION 343
Fig. 14. Transmission electron micrograph of a resindentin interface formed with G-Bond
(GC America) Asterisks indicate residual smear particles. Ad, adhesive; D, dentin; H, hybrid
layer; SP, smear plug; T, resin tag.
PERDIGAO
5. Light cure for 10s.
Adper Prompt 3M ESPE HEMA phosphates, HEMA, 1. Activate the L-Pop Unit Dose All-in-one self-etch,
L-Pop bis-GMA, modied Dispenser to mix the adhesive. but requires mixing
polyalkenoic acid, water, 2. Apply mixed adhesive to entire
photo-initiator surface, rubbing in the solution
with moderate nger pressure for
15s.
3. Use a gentle stream of air to
thoroughly dry the adhesive into
a thin lm.
4. Rewet the brush tip with adhesive
and apply a second coat of adhesive
to the tooth surface. The second
coat does not require rubbing.
5. Use a gentle stream of air to
thoroughly dry the adhesive into
a thin lm.
6. Light cure for 10s.
Adper Single Bond Plus 3M ESPE HEMA, bis-GMA, DMAs, 1. Apply Scotchbond Etchant (35% Two-step etch and rinse
methacrylate functional copolymer silica-thickened phosphoric acid
of polyacrylic and polyitaconic gel) to tooth surface for 15s.
acids, water, ethanol, nanoller, 2. Rinse thoroughly for 10s.
photo-initiator 3. Blot excess water using a cotton
pellet or mini-sponge. Do not air
dry.
4. Apply 23 consecutive coats of
adhesive for 15s with gentle
agitation using a fully saturated
applicator.
5. Gently air-thin for 5s to evaporate
solvent.
6. Light cure for 10s.
DENTAL ADHESION
Clearl S3 Bond Kuraray America 10-MDP, HEMA, bis-GMA, water, 1. Thoroughly wet brush tip with All-in-one self-etch
ethanol, silanated colloidal silica, Bond. Apply Bond to the tooth
camphorquinone surface and leave in place for 20s.
2. Dry the entire surface suciently by
blowing high-pressure air for more
than 5s while spreading the bond
layer thinly.
3. Light cure for 10s.
(continued on next page)
345
346
Table 2 (continued )
Adhesives and
manufacturers Composition Instructions for use Type
Clearl SE Bond Kuraray America Primer: 10-MDP, HEMA, hydrophilic 1. Thoroughly wet brush tip with Two-step self-etch
DMA, tertiary amine, water, primer. Apply primer to the tooth
photo-initiator surface and leave in place for 20s.
Bonding: 10-MDP, HEMA, 2. Dry with a mild air stream to
bis-GMA, hydrophilic DMA, evaporate the volatile ingredients.
tertiary amine, silanated colloidal 3. Dispense the necessary amount of
silica, photo-initiator Bond into second mix well.
PERDIGAO
4. Apply Bond to the tooth surface.
5. After applying Bond, create
a uniform lm using a gentle air
stream.
6. Light cure for 10s.
G-Bond GC America 4-MET, UDMA, phosphate 1. Before dispensing, shake the bottle All-in-one self-etch
monomer, DMA component, fumed of G-Bond thoroughly. Replace
silica ller, acetone, water, bottle cap immediately after use.
photo-initiator 2. Immediately apply to the prepared
enamel and dentin surfaces using
the microtip applicator.
3. Leave undisturbed for 10s.
4. After application, dry thoroughly
using oil free air under maximum
air pressure for 5s, in the presence
of vacuum suction to prevent
splatter of the adhesive.
5. Light cure 10s.
iBond Heraeus Kulzer UDMA, 4-MET, glutaraldehyde, 1. iBond is applied in three All-in-one self-etch
acetone, water, stabilizer, consecutive layers and massaged
photo-initiator into the prepared hard-tooth
structure for 30s.
2. Following that, the solution is
blown away with a gentle air
stream.
3. Polymerize for 20s.
Xeno IV Dentsply Caulk UDMA, PENTA, acetone, 1. Using the supplied disposable All-in-one self-etch
polymerizeable trimethacrylate microbrush applicator tip,
resin, and two polymerizeable DMA immediately apply and scrub
resins, photo-initiator. surfaces with generous amounts of
Xeno IV adhesive to thoroughly
wet all the tooth surfaces for 15s.
DENTAL ADHESION
2. Apply a second application of Xeno
IV adhesive with the microbrush as
above, scrubbing for 15s (20s for
larger restorations).
3. Remove excess solvent by gently
drying with clean, dry air from
a dental syringe for at least 5s.
4. Cure Xeno IV adhesive for 10s.
(continued on next page)
347
348
Table 2 (continued )
Adhesives and
manufacturers Composition Instructions for use Type
XP Bond Dentsply DeTrey Carboxylic acid modied 1. Etch enamel for at least 15s and Two-step etch and
dimethacrylate (TCB resin), dentine for 15s or less with 36% rinse
PENTA, UDMA, TEGDMA, phosphoric acid.
HEMA, butylated 2. Wet all cavity surfaces uniformly
benzenediol (stabilizer), with XP Bond in a disposable
ethyl-4-dimethylaminobenzoate, brush. Avoid pooling.
camphorquinone, functionalized 3. Leave the surface undisturbed for
amorphous silica, t-butanol 20s.
PERDIGAO
4. Evaporate solvent by thoroughly
blowing with air from an air syringe
for at least 5s. The cavity surface
should have a uniform, glossy
appearance. Otherwise repeat steps
2 and 4.
5. Light-cure for a minimum of 10s.
Ensure uniform exposure of all
cavity surfaces.
6. Immediately place the restorative
material over cured XP Bond.
Abbreviations: bis-GMA, bisphenol glycidyl methacrylate; DMA, dimethacrylate; HEMA, 2-hydroxyethyl methacrylate; 10-MDP, 10-methacryloyloxy
decyl dihydrogenphosphate; 4-MET, 4-methacryloxyethyl trimellitic acid; PENTA, dipentaerythritol penta-acrylate phosphate; TEGDMA, triethyleneglycol
dimethacrylate; UDMA, urethane dimethacrylate.
DENTAL ADHESION 349
Fig. 15. (A) Field emission scanning electron micrograph of enamel treated with iBond (Her-
aeus Kulzer) after roughening the enamel with a diamond bur for 5 seconds. The adhesive
was removed with acetone. (B) Enamel etched with 38% phosphoric acid (Pulpdent) for 15
seconds.
350 PERDIGAO
Fig. 16. Tooth #30 (left) preoperatively and (right) 1 year after being restored with the etch-
and-rinse adhesive One-Step Plus (Bisco Inc.).
DENTAL ADHESION 351
Fig. 17. Tooth #19 (left) preoperatively and (right) 1 year after being restored with the all-in-
one self-etch adhesive iBond (Heraeus Kulzer) (same patient as in Fig. 15).
with Prompt L-Pop, the predecessor of Adper Prompt, in cervical lesions re-
sulted in a high failure rate [68,69]. The most crucial dierence between the
two versions is the presence of the polyalkenoic-acid copolymer in the latest
versions (Adper Prompt and Adper Prompt L-Pop). This polyalkenoate-
based component was rst introduced in a resin-modied glass ionomer ma-
terial (Vitrebond, 3M ESPE) and subsequently used in other formulations,
including the adhesive systems (Scotchbond Multi-Purpose Primer and Sin-
gle Bond). The polyalkenoate salt has been claimed to provide water stabil-
ity to the adhesive system by a dynamic potential of breaking and renewing
the bonding between the carboxyl groups and calcium, forming a stress-
relaxation zone at the bonded interface [70].
Summary
Numerous simplied adhesives have been introduced to the dental mar-
ket within the last few years, sometimes without comprehensive testing to
validate the performance claimed by the respective manufacturers. Mild
self-etch adhesives are unable to etch enamel to provide adequate retention
for bonded restorations. Although high early resindentin bond strength
values can be achieved with some self-etch adhesives, their resistance to ther-
mal and mechanical stresses over time is disappointing. In light of the cur-
rent drawbacks attributed to all-in-one self-etch adhesives, etch-and-rinse
adhesives are still the benchmark for dental adhesion in routine clinical use.
Acknowledgments
The author gives special thanks to Drs. S. Duarte, G. Gomes, and
M. Lopes for help preparing the scanning electron microscopy and trans-
mission electron microscopy specimens.
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DENTAL ADHESION 355
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356 PERDIGAO
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