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Effect of Oxygen Inhibition of Self-etching Adhesives
se n
Enamel-Dentin Polymer Bond
Tatsuo Endoa/Takayuki Osadab/Werner J. Fingerc/Marcus Hoffmannd/Masafumi Kanehirae/
Masashi Komatsuf

Purpose: To determine effects of light curing of self-etching adhesives under ambient air or nitrogen on inhibition depths,
enamel and dentin bond strengths, and marginal adaptation in dentin cavities.
Materials and Methods: The adhesives investigated were: AQ Bond (AQB, Sun Medical; Kyoto, Japan), iBond (IBO, Heraeus Kulzer; Hanau, Germany), One-Up Bond F II (OUB, Tokuyama; Tokyo, Japan), and Prompt L-Pop (PLP, 3M/ESPE;
Seefeld, Germany). Inhibition layer thickness (ILT) was microscopically measured on 3 disk-shaped specimens each.
Shear bond strengths (SBS) on enamel and dentin (n = 8) were determined after 10 min and 24 h water storage of bonded composite specimens (Venus, Heraeus Kulzer). The marginal adaptation of bonded Venus restorations in cylindrical
dentin cavities was microscopically evaluated after 10 min of specimen storage (n = 8) in water. The data were statistically analyzed using parametric and nonparametric ANOVA and post-hoc tests at p < 0.05.
Results: Adhesive curing under air revealed significant ILT (m) differences: IBO (4) < AQB (8) < PLP (12) < OUB (23). Upon curing in nitrogen atmosphere, no inhibition occurred with AQB, IBO, and PLP, and < 3 m for OUB. SBSs on enamel
after 10 min or 24 h did not differ according to curing atmospheres (p > 0.05). On dentin, SBSs were higher after curing
under N2 (p < 0.05). Irrespective of the curing atmosphere, marginal adaptation was good for AQB and IBO and poor for
PLP; OUB revealed significantly smaller gaps under N2 than under air curing.
Conclusion: Oxygen inhibition of the four self-etching adhesives investigated had no or only moderate effects on bonding efficacy to enamel and dentin.
Keywords: self-etching adhesives, oxygen inhibition, enamel-dentin bonding, cavity marginal adaptation.
J Adhes Dent 2007; 9: 33-38.

xygen inhibits free-radical polymerization of light- or

chemically cured dental adhesives and resin composites, yielding an uncured surface layer.1,21 Oxygen dissolved
in the resin is in equilibrium with the surrounding atmosphere. Oxygen is consumed upon curing, while simultaneous

a Lecturer, Graduate School of Dentistry, Department of Restorative Dentistry,

Division of Operative Dentistry, Tohoku University, Sendai, Japan.

b Assistant Professor, Department of Prosthetic Dentistry, School of Dentistry,

Showa University, Tokyo, Japan.

c Professor, Department of Preclinical Dentistry, School of Dental Medicine,

University of Cologne, Cologne, Germany.

d Chemist, Research and Development, Heraeus Kulzer, Wehrheim, Germany.
e Assistant Professor, Graduate School of Dentistry, Department of Restorative

Dentistry, Division of Operative Dentistry, Tohoku University, Sendai, Japan.

f Professor, Graduate School of Dentistry, Department of Restorative Dentistry,

Head of the Division of Operative Dentistry, Tohoku University, Sendai, Japan.

Reprint requests: Werner J. Finger, Department of Preclinical Dentistry, School
of Dental Medicine, University of Cologne, Kerpener Strasse 32, D-50931
Cologne, Germany. Tel: +49-2133-514996; Fax: +49-2133-513410. e-mail:
wjfinger@aol.com

Vol 9, No 1, 2007

Submitted for publication: 31.01.06; accepted for publication: 03.04.06.

oxygen diffusion from the ambient air re-establishes the

equilibrium. This is a particular concern when thin resin layers, eg, adhesives or sealants, are to be cured.3,10 The effect
of such nonpolymerized layers on bonding and copolymerizatious with subsequently applied portions of resin is a contentous issue in the dental literature. Some research articles
emphasize the positive and desirable effect of such liquid
films as a means to improve interfacial bonding.8,19,20 Other reports conclude that oxygen-inhibited layers are not necessary for safe bonding at the interface.4,7,13 Recently published data13 confirm the conclusions of previous studies
that the presence of a non-cured surface film might adversely affect bonding to overlying resin.2,9 The monomer
composition of the inhibited zone has the same composition
as the non-cured adhesive monomer. The crucial difference
is, however, that the photoinitiating system is partially consumed after initial curing. The half-life of camphorquinone
depends strongly on irradiation time and intensity.13
With the increasing acceptance of self-etching bonding
agents, oxygen inhibition of acidic adhesive monomers has
become a relevant subject. In combination with redox-cured
33

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Table 1 Materials used

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Manufacturer
Lot

Composition

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Adhesive

Code

AQ Bond

IBO

Sun Medical, Japan

Base: GE2
Brush: GF1

Base: UDAMA, 4-META, HEMA, MMA

acetone, water, PI
Brush Impregnated with co-initiator

iBond

IBO

Heraeus Kulzer, Germany

10042

UDMA, 4-META, acetone, water, GA, PI

One-Up Bond F II
(exprimental)

OUB

Tokuyama, Japan
MS-07

A: Phosphate monomer, MAC-10

multifunctional MAs, co-initiator
B: HEMA, water, glass filler, PI,
dyesensitizer

Promt L-Pop

PLP

3M/ESPE, Germany
151246

Methacrylated phosphoric acid esters,

phosphine oxide, stabilizer, fluoride
complex, parabenes, water

UDMA urethane dimethacrylate; 4-META, 4-methacryloyloxyethyl trimellitic anhydride; HEMA, 2-hydroxyethyl methacrylate; MMA, methyl methacrylate;
PI, photoinitiator; GA glutardialdehyde; MAC-10, 11-methacryloxy-1, 1-undecan dicarboxylic acid; MA, methacrylate

Table 2 Application of adhesives

Adhesive

Code

Application

AQ Bond

IBO

2 drops of adhesive + 1 impregnated sponge,

2 coats, 20 s dwell time, 10 s air-drying,
10 s l. a., 1 additional coat, 10 air-dry, 20 s l.a.

iBond

IBO

3 coats, 30 s undisturbed dwell time,

20 s air-dry, 20 s l.a.

One-Up Bond F II
(experimental)

OUB

1 drop each of A and B mixed, 1 coat,

10 s agitated dwell time, 10s l.a.

Promt L-Pop

PLP

1 coat, 15 s agitated dwell time,

20 s air-dry, 10 s l.a.

l.a.: light activation (Translux Energy, Heraeus Kulzer; 850 mW/cm2 output)

and dual-cured resin composites, weak bonding strengths

were reported for self-etching adhesives as a result of the interaction between the acidic monomers from the inhibited
surface layer and the tertiary amines of the chemically cured
resin composite which are neutralized and thus lose their
ability to generate free radicals.5,6,11,12,14 Another mechanism to explain the incompatibility reaction between acidic
adhesive monomers and chemically or dual-curing composites is permeability for water across the polymerized adhesives water-filled channels via osmosis up to the overlying
coupling site with the restorative resin, where water accu34

mulates as blisters, jeopardizing the interfacial bond.16-18 A

similar adverse effect on bonding was found between acidic
self-etching adhesives and delayed activation of light-cured
resin composites.15
The purpose of this study was threefold: 1) to measure
the thickness of the surface inhibition layer of 4 self-etching
adhesives when cured under ambient air or nitrogen, 2) to
evaluate their shear bond strengths to enamel and dentin
depending on the curing atmosphere, and 3) to determine
the marginal adaptation of bonded cylindrical resin composite restorations in butt-joint dentin cavities with or withThe Journal of Adhesive Dentistry

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out oxygen access during light activation of the adhesives.

The null hypothesis tested was that there is no difference in
bonding performance of self-etching adhesives when cured
in ambient atmosphere or nitrogen.

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Cover Glasses

Adhesive
(solvent-free)

MATERIALS AND METHODS

se nz

Glass Slide
Light Activation

Table 1 shows the four all-in-one adhesives investigated and

their compositions, and Table 2 summarizes their application procedures. AQ Bond (AQB) is applied with a sponge impregnated with p-toluene sulfinate as a co-initiator that is
dipped and agitated in the base liquid. iBond (IBO) is an allin-one self-etching adhesive that is applied to the tooth surface with a disposable brush-stick in three consecutive
coats. One Up Bond F II (OUB) and Prompt L-Pop (PLP) are
two-component products that are mixed prior to application
either in a well or by lollipop folding. All adhesives were applied in strict accordance with the respective manufacturers
instructions for use.
Determining Oxygen Inhibition Layer
For determination of the inhibition layer thickness (ILT), an
appropriate volume of adhesive was dispensed in a mixing
well. Six droplets of AQB Base liquid were slightly stirred with
two immersed AQB sponges, from IBO six droplets were dispensed, three drops each of components A and B of OUB
were mixed, and the content of six PLP units was dispensed.
The AQB, IBO, and PLP liquids were thoroughly air dried in
dimmed-light surroundings under a gentle air stream for
several minutes in an attempt to remove the solvent/water.
OUB was not air dried since the manufacturers instructions
do not request air drying of the applied adhesive prior to light
activation. As shown in Fig 1, a small droplet of the solventfree adhesives was placed on a glass microscope slide between two spacer plates, 0.15 mm thick, under a coverglass plate supported by the spacers to produce a uniformly thick disk-shaped specimen. The specimens between the
glass plates were light activated (Translux Energy [Heraeus
Kulzer; Hanau, Germany], 850 mW/cm2, curing output controlled with built-in radiometer) either at ambient atmosphere or under a gentle continuous stream of nitrogen (60
l/h) passing the space between the glass plates from 10 s
before until 10 s after light activation. The depth of oxygen
inhibition was determined on three disks of each of the adhesives following the manufacturers light activation times.
The widths of the non-cured peripheral layers, discernable
from the central polymer portion by difference in refractive
index, were measured microscopially at 500X magnification
at four sites, 90 degrees apart. Data were statistically analyzed by nonparametric ANOVA and Mann-Whitney post-hoc
testing at p < 0.05.
Shear Bond Strength Testing
Shear bond strength (SBS) was determined on enamel and
dentin of extracted human maxillary incisors or molars that
were immersed immediately after extraction in 1% chloramine solution for 3 to 6 months prior to use. The teeth were
embedded in slow-curing epoxy resin (Lekutherm, Bayer AG;
Leverkusen, Germany) with their sound facial or proximal tarVol 9, No 1, 2007

Nitrogen Flow

Fig 1 Preparation of specimens for determination of depth of oxygen inhibition.

get sites facing the bottom of a 30-mm-wide and 20-mm-high

rubber mold. Flat peripheral enamel or dentin surfaces were
exposed by grinding on wet SiC paper, grits 180 through 600,
rinsed with tap water, and air dried prior to bonding according to instructions. Activation with the tungsten-halogen curing unit Translux Energy took place either at ambient atmosphere or under a continuous stream of nitrogen (60 l/h). A
split Teflon mold with a 3.5-mm-wide and 2-mm-high cylindrical hole was clamped in a stand on the pretreated teeth,
bulk-filled with the hybrid type resin composite Venus (Shade
A2, Heraeus Kulzer; Hanau, Germany), covered with a transparent matrix strip, and light activated for 60 s with the
Translux Energy lamp. Immediately after curing, the specimens were either immersed for 10 min in 23C water or for
24 h in 37C water prior to shear loading of the resin cylinder
in a universal testing machine (Zwick 1474; Ulm, Germany)
via a steel rod, parallel and close to the bonding interface, at
a rate of 1 mm/min until fracture occurred. For each adhesive, storage time, and curing mode, 8 specimens each were
prepared on enamel and dentin. Bond strength data were
statistically analyzed by one- and three-way ANOVA and Duncans post-hoc test at p < 0.05. The modes of failure were analyzed on the tooth side of specimens under a stereomicroscope (Zeiss, STEMI SV; Oberkochen, Germany) at 20X magnification and classified as adhesive, cohesive in resin or
tooth, or mixed adhesive-cohesive failures.
Measuring Marginal Gap
To evaluate the marginal gap width (MGW) of the adhesively bonded restorations, proximal, peripheral dentin of extracted human molars was exposed by wet grinding on SiC
paper, grits 180 through 600, until a sufficiently large area
was exposed for preparation of cylindrical butt-joint cavities,
approximately 4 mm in diameter and 1.5 mm in depth. The
cavities were cut with a medium-grained diamond bur under
copious water spray. For each material, 8 cavities were produced. The cavities were treated with the adhesives according to instructions, light cured either under ambient laboratory atmosphere (23C, 50% relative humidity) or under
a continuous stream of nitrogen (60 l/h), and bulk filled with
the hybrid-type resin composite Venus (A2) delivered from
preloaded tubes. The free composite surface was covered
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with a transparent matrix strip, pressed flush with the pelte
n
ripheral dentin surface, and light activated with the poly- n

ILT (m)
30

Air

N2

Air

N2

Air

N2

Air

N2

25
20
15
10
5
0

AQB

IBO

OUB

MPa

Enamel

30
25
20
15
10
5
0

AQB

MPa

35

IBO

OUB

PLP

Dentin

30
25
20
15
10
5
0

AQB

IBO

OUB

PLP

Fig 3 Shear bond strength (SBS, means and 95% confidence intervals) on enamel and dentin, after 10 min (circular symbols) storage in 23C water or 24 h (rhombic symbols) storage in 37C water
(n = 8). Open symbols denote adhesive curing under ambient air,
closed symbols under nitrogen.

36

RESULTS

PLP

Fig 2 Inhibition layer thickness (ILT) of adhesives, light activated

in ambient atmosphere or under protective nitrogen stream. Three
specimens with 4 measuring sites each. Same lowercase letters
denote not significantly different data subsets (Mann-Whitney pairwise comparison at p < 0.05).

35

essthe
z
merization lamp (Translux Energy) in contact with
e ncovering strip for 60 s. Immediately after polymerization, the teeth
were immersed in 23C water for 10 min prior to removal of
the restorative resin excess using SiC paper, grits 600 and
4000, until the entire cavity margin was exposed for immediate inspection at 500X magnification under an incidentlight microscope.
When a gap was detected, the maximum width was measured with an ocular screw micrometer. The data were analyzed using Kruskal-Wallis ANOVA and Mann-Whitneys posthoc test at p < 0.05.

Figure 2 shows the oxygen-inhibited layer thickness of the 4

adhesives cured under air and nitrogen. When cured at ambient atmosphere, IBO showed the thinnest inhibition zone,
approximately 4 m, and OUB the thickest layer, 23 m. Under the protective nitrogen atmosphere, no inhibited zone
was detected for AQB, IBO, or PLP, whereas the free surface
of OUB was covered with a 2- to 3-m-wide nonpolymerized
film.
Figure 3 shows the mean shear bond strengths (SBS) on
enamel and dentin together with the 95% confidence intervals, by storage time and curing atmosphere of the adhesives. Same uppercase and lowercase letters in Table 3
denote in increasing order homogeneous data subsets,
ie, SBSs on enamel and dentin that are not significantly different. On enamel, PLP showed a tendency towards slightly
higher SBS in early testing than the alternative adhesives;
after 24 h, no significant differences were noted between
the adhesives and curing conditions. On dentin, a tendency
towards higher SBS was seen with adhesives cured under
nitrogen, irrespective of the testing time.
Three-way ANOVA of shear bond strength to enamel and
dentin showed significant differences between adhesives
and storage times (p < 0.05). SBSs to enamel did not differ
by curing atmosphere (p > 0.05), whereas the bond
strengths on dentin were higher after curing under the protective nitrogen atmosphere (p = 0.013).
Table 4 summarizes the failure patterns of the debonded specimens. No adhesive or mixed adhesive-cohesive failures were noted. Testing after 10 min storage revealed mostly cohesive failures in resin close to the bonding site. The
128 specimens debonded after 24-h storage showed 59 cohesive failures in resin and 69 cohesive failures in enamel
or dentin, mostly visible as cracks in the tooth substance under the coupling site.
The box-and-whisker plots in Fig 4 with medians and interquartile distances describe the results of the marginal
adaptation test. Figures on top of the diagram give the numbers of gap-free restorations for each testing group. Same
lowercase letters denote groups not significantly different
according to pair-wise Mann-Whitney comparisons. Curing
of the adhesives under nitrogen resulted in significantly improved marginal adaptation for OUB, and in a tendency towards better adaptation for the three other adhesives. After
The Journal of Adhesive Dentistry

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Table 3 Shear bond strength data on enamel and dentin

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Adhesive

AQB

IBO

Substrate

OUB

PLP

se nz

E D

Air

ab

AB

ab

AB

bc

N2

abc

AB

abc

AB

cd

AB

abc

Air

def

fg

de

def

N2

def

ef

def

10 min

24 h

Same uppercase and lowercase letters denote groups on enamel aand dentin, respectively, that are not significantly different (p > 0.05). E: enamel;
D: dentin.

Table 4 Failure patterns after shear debonding from enamel and dentin (n = 8)
Location

Tooth, cohesive

Storage time

10 min

Substrate

Resin, cohesive
24 h

10 mn

24 h

Curing atmosphere

AQB

IBO

OUB

PLP

E: enamel; D: Dentin; A: ambient air: N: nitrogen

activation under nitrogen, AQB and IBO showed 7 and 8 gapfree cavity margins of the 8 cavities in the groups and OUB
only 2, whereas all PLP restorations showed marginal gaps
with an average maximum width around 5 to 6 m.

m 10

Air

N2

Air

N2

Air

N2

Air

N2

DISCUSSION
The depths of oxygen inhibition found after curing at ambient atmosphere were largely different for the four adhesives
tested, whereas curing under a protective nitrogen atmosphere completely prevented inhibition in three of the four
adhesives. For OUB, a thin inhibited layer persisted even after activation under nitrogen. According to the manufacturers application instructions, the adhesive should not be air
dried after the 10-s agitated dwell time. Thus, the water included for ionization of the functional acidic monomer,
probably 5%, remains. The water is saturated with oxygen
in equilibrium with the surrounding atmosphere before activation, and may therefore inhibit the polymerization of
OUB.
Vol 9, No 1, 2007

AQB

IBO

OUB

PLP

Fig 4 Maximum marginal gap width (m) of cylindrical restorations

in dentin cavities by curing atmosphere (n = 8). Same lowercase letters denote not significantly different data subsets (Mann-Whitney
pair-wise comparison at p < 0.05). The numbers on top of the diagram are the numbers of gap-free restorations in each group.

37

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CONCLUSION

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According to previously published data, differences in

bond strength and marginal adaptation were expected, especially when adhesives with very little or pronounced inhibition of polymerization are compared.9 When a relatively
thick layer of unpolymerized monomer on the adhesive surface is coated with resin composite, there might be insufficient diffusion of the photoinitiator into the oxygen-inhibited
layer. This might lead to a reduced degree of conversion of
double bonds and thus a lower degree of polymerization.
Comparison of the bond strength data on enamel with IBO
and OUB, showing 4 and 23 m inhibition depth respectively, revealed no significant difference, either after 10 min
or after 24 h of specimen storage time. This indicates sufficient initiator interdiffusion and/or adhesive and composite
monomer mixture, even into the thick inhibition layer. Bonding of light-cured resin composite to adhesives, cured under
nitrogen, had no adverse effect on enamel SBS when compared with bonding of the adhesives cured under ambient
laboratory atmosphere. This finding is in agreement with
previous reports, concluding that inhibited resin surfaces
are not necessary for good bonding at the interface.4,7,13
Presumably, the resin composite monomer is able to soften
and penetrate into the cured adhesive surface where an interpenetrating bonding zone is produced.
The bond strength data of adhesives cured on dentin under a protective atmosphere of nitrogen showed higher SBSs when compared with adhesive curing under atmospheric air. In contrast to enamel, dentin is a porous substrate.
Oxygen is dissolved in the tubular liquid and may inhibit polymerization of the adjacent adhesive. After activation under
nitrogen coverage or coating of the free adhesive surface
with resin composite, continuous oxygen diffusion from this
peripheral site is excluded; however, the oxygen source on
the dentin site remains active. This might offer a tentative
explanation for the trend towards increased dentin SBS after activation under nitrogen.
The marginal dentin cavity adaptation figures showed a
clear, albeit not statistically significant, tendency towards
improved bonding when the two moderately oxygen-inhibited adhesives AQB and IBO were activated under nitrogen.
Speculatively, these results might be explained with the high
initiator concentration in these products. With OUB, a significant improvement of marginal adaptation was achieved
after curing under nitrogen, however, still 6 of the 8 restorations placed showed minor marginal gaps. The poor marginal adaptation found for PLP bonded restorations, even after curing under nitrogen, cannot be attributed to oxygen inhibition, but rather to a low degree of polymerization and/or
low network density, since the product does not contain
crosslinking monomers.
Thus, the null hypothesis tested is accepted for adhesive
bonding to enamel and partially rejected for bonding to cut
dentin surfaces.

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sseofnzoxyThe results of this investigation show that the depth

gen inhibition of the four self-etching adhesives has no or little effect on bonding performance to enamel and dentin.
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11. Sanares AME, Itthagarun A, King NM, Tay FR, Pashley DH. Adverse surface
interactions between one-bottle light-cured adhesives and chemical-cured
composites. Dent Mater 2001;17:542-556.
12. Suh BI, Feng L, Pashley DH, Tay FR. Factors contributing to the incompatibility between simplified-step adhesives and chemically-cured or dual-cured
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2003;5:267-282.
13. Suh BI. Oxygen-inhibited layer in adhesive dentistry. J Esthet Restor Dent
2004;16:316-323.
14. Swift EJ, Perdigao J, Combe EC, Simpson CH, Nunes MF. Effects of restorative and adhesive curing methods on dentin bond strengths. Am J Dent
2001;14:137-140.
15. Tay FR, King NM, Suh BI, Pashley DH. Effect of delayed activation of lightcured resin composites on bonding of all-in-one adhesives. J Adhes Dent
2001;3:207-225.
16. Tay FR, Pashley DH, Suh BI, Carvalho RM, Itthagarun A. Single-step adhesives
are permeable membranes J Dent 2002;30:371-382.
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Clinical relevance: From a clinical perspective, the depth

of oxygen inhibition of polymerization of the four self-etching adhesives investigated has only a moderate effect on
enamel and dentin bonding performance.

38

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