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Operative Dentistry, 2003, 28-5, 647-660

Microtensile Bond Strengths of


an Etch&Rinse and
Self-Etch Adhesive to
Enamel and Dentin as a

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Function of Surface Treatment
B Van Meerbeek • J De Munck • D Mattar
K Van Landuyt • P Lambrechts

Clinical Relevance
Cavity preparation methods, such as diamond sonoabrasion, laser irradiation and air abra-
sion, may affect bonding performance of etch&rinse and self-etch adhesives to enamel and
dentin. Irrespective of the cavity preparation technique, separate acid-etching as part of an
etch&rinse approach remains recommended to achieve adequate bonding to enamel.

SUMMARY This study investigated whether diamond


In light of the current trend towards “minimal sonoabrasion (SonicSys Micro, Kavo), air abra-
invasive” dentistry, diverse cavity preparation sion (Prep Start, Danville) and Er:YAG laser irra-
techniques have been introduced as an alterna- diation (Fidelis) produce surfaces at
tive or addition to common bur instrumentation. enamel/dentin that are equally receptive to
bonding as traditional mid-grit diamond-bur
*Bart Van Meerbeek, DDS, PhD, professor, Leuven BIOMAT (Komet) and 600-grit SiC-paper prepared sur-
Research Cluster, Department of Conservative Dentistry, School faces, of which the latter two served as controls.
of Dentistry, Oral Pathology and Maxillo-Facial Surgery, An etch&rinse adhesive (OptiBond FL, Kerr)
Leuven, Belgium applied with and without prior acid-etching and
Jan De Munck, DDS, PhD-student, Leuven BIOMAT Research a self-etch adhesive (Clearfil SE, Kuraray) were
Cluster, Department of Conservative Dentistry, School of employed to bond the restorative composite
Dentistry, Oral Pathology and Maxillo-Facial Surgery, Leuven, (Z100, 3M ESPE) to the diversely prepared enamel
Belgium
and dentin surfaces. The microtensile bond
Daniela Mattar, DDS, MS, visiting research associate, Leuven strength (µTBS) was determined after 24 hours
BIOMAT Research Cluster, Department of Conservative of storage in water at 37°C. The results indicated
Dentistry, School of Dentistry, Oral Pathology and Maxillo-
Facial Surgery, Leuven, Belgium
that the manner of preparation of enamel and
dentin prior to bonding procedures significantly
Kirsten Van Landuyt, DDS, PhD-student, Leuven BIOMAT
influenced the bonding effectiveness of both the
Research Cluster, Department of Conservative Dentistry, School
of Dentistry, Oral Pathology and Maxillo-Facial Surgery, etch&rinse and the self-etch adhesive. Using an
Leuven, Belgium etch&rinse adhesive, separate acid-etching of
air-abraded and Er:YAG-irradiated enamel and
Paul Lambrechts, DDS, PhD, full professor and head, Leuven
BIOMAT Research Cluster, Department of Conservative dentin surfaces remains mandatory. Bonding to
Dentistry, School of Dentistry, Oral Pathology and Maxillo- diamond-sonoabraded and air-abraded enamel
Facial Surgery, Leuven, Belgium and dentin was, in general, not different from
Reprint request: Kapucijnenvoer 7, B-3000 Leuven, Belgium; bonding to conventional diamond-bur prepared
e-mail: bart.vanmeerbeek@med.kuleuven.ac.be surfaces, whereas, bonding to Er:YAG-irradiated
648 Operative Dentistry

enamel and dentin surfaces in general resulted in and noise, as these are commonly experienced during
a significantly lower bonding effectiveness com- mechanical preparation of teeth when rotating burs are
pared to bonding to diamond-bur prepared sur- used (Roeder & others, 1995).
faces. Recently, the use of laser technology has also been
introduced as an alternative to traditional mechanical
INTRODUCTION
rotating instruments for cavity preparation (Hibst,
Tooth cavities are commonly prepared by means of Keller & Stainer, 1988). In particular, the Erbium:YAG
rotary instruments equipped with either diamond or laser with an ultra-short square pulse technology has
tungsten carbide burs. While prepared relatively fast, been advocated to prepare micro-cavities. Thanks to an
bur-prepared cavities are often, however, larger than ablation process that involves micro-explosions, hard

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dictated by the extent of the actual caries. In addition, tooth substrate can be effectively removed, while
beveling of margins for adhesive purposes in critical cooling with water prevents cracking or melting of
approximal regions using burs is often not feasible. enamel and dentin, thereby, protecting the underlying
Also, iatrogenic bur damage of healthy adjacent teeth pulp tissue.
has been reported to be responsible for a substantial
This laboratory study determined the microtensile
amount of new caries lesions (Moopnar & Faulkner,
bond strength (µTBS) of two representative adhesives
1991; Qvist, Johannessen & Bruun, 1992; Lussi, 1995;
to diamond sonoabraded, air-abraded and laser-irradi-
Lussi & Gygax, 1998; Wicht & others, 2002). All these
ated enamel and dentin, as compared to their µTBS to
drawbacks, associated with conventional rotary cavity
bur-cut and SiC-paper prepared enamel and dentin
preparation techniques, along with the current trend
(controls). The hypothesis tested was that diamond
toward “minimal invasive” (Degrange & Roulet, 1997)
sonoabrasion, air abrasion and laser irradiation are
or “minimum intervention” dentistry (Tyas, Anusavice
equally effective to pre-treat enamel and dentin for
& Frencken, 2000), have lately led to the introduction of
bonding as traditional acid etching of bur-cut tooth sur-
new tools or the revival of already existing techniques
faces.
that, until recently, were considered somewhat less
practical. These techniques intend to facilitate the METHODS AND MATERIALS
preparation of micro-cavities with minimal sacrifice to
sound tooth substrate. Ninety non-carious molars were stored in 0.5% chlo-
ramine solution at 4°C and used within one month after
One such new cavity preparation method involves extraction for µTBS determination. The molars were
using a modified sonic air-scaler handpiece equipped randomly divided into 18 experimental (nine enamel
with a diamond-coated working tip activated through and nine dentin experimental groups) and 12 control
ultrasonic frequency oscillations. These diamond tips groups (six enamel and six dentin control groups)
exist in different forms, enabling direct occlusal or lat- (Figure 1). All teeth selected were first mounted in gyp-
eral access to the initial caries lesion through sonoabra- sum blocks to ease sample manipulation. The µTBS to
sion. The tips are only coated with diamonds at one enamel and dentin was determined using one of the
side. The highly polished, non-active side allows the tip protocols described by Pashley and others (1999). A rep-
to be supported on the approximal site of the neighbor- resentative etch&rinse adhesive, Optibond FL (Kerr,
ing tooth without damaging it. Diamond sonoabrasion Orange, CA, USA) and a self-etch adhesive, Clearfil SE
is, therefore, particularly recommended for minimal (Kuraray, Osaka, Japan) were applied to successively
cavity preparations of proximal lesions in anterior and diamond sonoabraded, air-abraded, laser-irradiated,
posterior teeth (Hugo, 1999a,b; Yip & Samaranayake, bur-cut and SiC-paper-prepared enamel and dentin
1998). In addition, they are very handy to bevel enamel/ (Table 1 and Figure 1). The etch&rinse adhesive
dentin margins at difficult accessible areas, such as the OptiBond FL was used with (AE) and without (NAE)
approximal cervical and lateral box margins. 37.5% phosphoric acid conditioning. At each moment
Air abrasion is a cavity preparation technique first during specimen processing, care was taken to prevent
introduced in the 1940s by Dr Robert Black (Goldstein dehydration of the samples.
& Parkins, 1994) that lately has re-gained interest. Its Enamel Specimen Preparation
reappearance must largely be attributed to signifi-
cantly improved air abrasion units released on the mar- Lingual and/or buccal enamel of the human third
ket (Manhart & others, 1999). The major benefit of this molars was flattened using a high-speed, medium-grit
technique is that kinetic energy, generated by a high- (100 µm) diamond bur (842, Komet, Lemgo, Germany)
velocity stream of aluminum oxide particles, can be uti- mounted in the MicroSpecimen Former (University of
lized to prepare hard tissue (dentin/enamel), while hav- Iowa, Iowa City, IA, USA). The exposed enamel surface
ing little effect on soft materials such as gingival tis- served as the bur-cut control. For the SiC-paper pre-
sues. In addition, this abrasive technique increases pared samples (control), a standard smear layer was
patient comfort by reducing pressure, heat, vibration also produced by wet-sanding the enamel surface with
Van Meerbeek & Others: Bond Strength to Variously Prepared Enamel and Dentin 649

600-grit silicon carbide sandpaper for 60 seconds. For face was build up with Z100 (3M ESPE, St Paul, MN,
the diamond-sonoabraded specimens (SonicSys Micro, USA) in three-to-four layers to a height of 5-6 mm.
Kavo Dental, Biberach, Germany), a new “space shut- Dentin Specimen Preparation
tle”-shaped diamond tip of the SonicSys system was
applied to the SiC-paper prepared enamel surface for The occlusal third of the molars was removed using an
one minute in as uniform a manner as possible. For the Isomet slow-speed diamond saw (Isomet 1000, Buehler,
air-abrasion samples, the surface received a standard Lake Bluff, IL, USA). The dentin surfaces were con-
SiC-paper smear layer prior to uniform abrading for 10 trolled for the absence of enamel and/or pulp tissue
seconds following three different directions by means of using a light microscope (Wild M5A, Heerbrugg,
Prep Start (Danville, San Ramon, CA, USA) with 27 Switzerland). For the bur-cut samples (control), the

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µm aluminum oxide particles at 6.5 psi air pressure. teeth were mounted in a chuck and a standard smear
The distance of the nozzle tip to the dentin surface was layer was produced by removing a thin layer of the sur-
kept constant to about 2 mm, with the nozzle held at face with a high-speed diamond bur (842, Komet) using
45° to the enamel surface. After air abrasion, the spec- the MicroSpecimen Former. For all other experimental
imens were thoroughly rinsed with a vigorous water and controls groups, the respective dentin surfaces
spray for 15 seconds to remove residual aluminum par- were prepared as described above for the enamel spec-
ticles from the surfaces. For laser-irradiated surfaces, a imens. Subsequently, the adhesive and composite were
standard SiC-paper prepared smear layer was first pro- applied again, strictly following the manufacturers’
duced prior to being uniformly irradiated using a com- instructions (Table 1). Settings for the laser “condition-
mercially available
Er:YAG laser (Fidelis,
Fotona Medical Lasers, µTBS to
Ljubljana, Slovenia)
with a sapphire tip in ENAMEL - DENTIN
constant slight con-
tact with the surface.
The settings for
enamel “conditioning”
were 10 Hz, 120 mJ
and short pulse mode
(pulse length is 250
µs). Subsequently, the
adhesives were applied
on the diversely pre-
pared enamel sur-
faces strictly following
the manufacturers’
instructions (Table 1).
After curing the adhe-
sive using an Optilux
500 (Demetron/Kerr,
Danbury, CT, USA)
device with a light
output not less than
550 mW/cm2, the sur- Figure 1. Flow diagram presenting the experimental set-up. AE = Acid-etch; NAE = No acid-etch.

Table 1: List of Adhesives Investigated


Code Product Name Adhesive Component Application Procedure Batch #
C-SE Clearfil SE Bond Primer Applied for 20 seconds; Gently air blown. [00125C]
Kuraray, Osaka, Japan Bond Applied and light cured for 10 seconds. [00069A]
O-FL OptiBond FL Kerr Gel Etchant Applied for 15 seconds, rinsed for 15 [104634]
Kerr, Orange, CA, USA seconds and gently air dried for five seconds.
OptiBond Primer Applied for 30 seconds with continuous [103962]
scrubbing, gently air dried and light cured
for 20 seconds.
OptiBond Adhesive Applied in a thin, even layer. [104369]
650 Operative Dentistry

ing” of dentin were 10 Hz, 80 mJ and short pulse mode Twenty additional human third molars were used for
(pulse length was 250 µs). examination using Fe-SEM of unbonded enamel and
µTBS Testing dentin surfaces prepared following the three experi-
mental and two control conditions. The specimen sur-
After bonding procedures, all specimens were stored for faces were prepared in exactly the same way that the
24 hours at 37°C in tap water. The teeth were then sec- µTBS was determined and were further processed for
tioned perpendicular to the bonding surface using the SEM following the methodology described above.
Isomet saw to obtain rectangular samples about 2x2
mm wide and 8-9 mm long. These specimens were RESULTS
mounted in the pin-chuck of the MicroSpecimen The mean µTBS and standard deviations are summa-
Former and trimmed at the biomaterial-tooth interface

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rized per experimental group in Table 2 and graph-
to a cylindrical hour-glass shape with a diameter of ically presented in Figures 2-3, respectively, for Clearfil
about 1.2 mm using a cylindrical extra-fine grit (15 µm) SE and Optibond FL, when bonded respectively to
diamond bur (835KREF, Komet) in a high-speed hand- enamel and dentin. The p-values comparing the effects
piece under air/water spray coolant. The specimens of acid-etching (solely OptiBond FL) and the adhesive
were then fixed to a Ciucchi’s device with cyanoacrylate (Clearfil SE versus OptiBond FL AE) are mentioned in
glue (Model Repair II Blue, Sankin Kogyo, Otahara, Table 3. The results from failure analysis are summa-
Japan) and stressed at a crosshead speed of 1 rized in Tables 4 and 5, respectively, for Clearfil SE and
mm/minute until failure in an LRX testing device (LRX, Optibond FL.
Lloyd, Hampshire, UK) using a load cell of 100N. The
µTBS was expressed in MPa as derived from dividing When bonded to enamel, the µTBS ranged from on
the imposed force (in N) at the time of fracture by the average 10.0 MPa for OptiBond FL bonded to non-
bond area (in mm2). When the specimens failed prior to etched, Er:YAG-irradiated enamel to an average 37.8
actual testing, the mean µTBS was determined from MPa for OptiBond FL bonded to etched, air-abraded
the specimens that survived specimen processing with enamel (Table 2, and Figures 2 and 3). Clearfil SE
an explicit note of the number of pre-testing failures bonded equally effectively irrespective of experimental
(ptf). The mode of failure was determined at a magnifi- or control conditions (Table 2 and Figure 2). Separate
cation of 50x using the stereomicroscope. acid-etching of enamel prior to applying OptiBond FL
significantly increased (p<0.01) the µTBS in all experi-
Pairwise Kruskal-Wallis analysis and Dwass-Steel- mental and control groups with the exception of bond-
Chritchlow-Fligner multiple comparisons were used to ing to etched versus non-etched, air-abraded enamel,
determine statistical differences in µTBS between the which was only nearly significantly different (Tables 2
experimental and control groups for each adhesive and 3, and Figure 3). Following acid-etching (AE), the
group separately (C-SE, O-FL AE, O-FL NAE) at a sig- µTBS of OptiBond FL bonded to laser-irradiated enamel
nificance level of 0.05. Furthermore, the effect of acid- was significantly lower than that obtained when
etching using OptiBond FL and the adhesive (Clearfil OptiBond FL was bonded to all other experimental and
SE versus OptiBond FL AE) were pair-wise assessed control enamel surfaces (Table 2). Among the latter
using two-sided Mann-Whitney U tests for the diversely groups, no significant differences were found. When
prepared enamel and dentin surfaces. In order to com- enamel was not separately acid-etched (NAE), again,
pensate for multiple testing, the significance level α for the µTBS of OptiBond FL bonded to Er:YAG-irradiated
the latter statistical analysis was adjusted to 0.01 fol- enamel was significantly lower than OptiBond FL
lowing a Bonferroni correction. bonded following all other experimental and control
Fe-SEM Evaluation conditions with the exception of sonoabrasion (Table 2),
Selected µTBS samples of each experimental and con- which, however, was not significantly different from all
trol group that exhibited a representative failure mode other experimental and control conditions. Pre-testing
and a µTBS close to the average value were processed failures only occurred for OptiBond FL bonded to non-
for Fe-SEM. The authors employed common procedures etched, sonoabraded enamel (Table 2), indicating that
for SEM specimen preparation, including fixation in a when these failures would have been taken into account
2.5% glutaraldehyde in cacodylate buffer solution, (µTBS=0 MPa), bonding to non-etched, sonoabraded
dehydradation in ascending concentrations of ethanol enamel and non-etched, laser-irradiated enamel should
and chemical drying using HMDS (the protocol has be considered significantly less effective than the
been described in detail by Perdigão & others, 1995). remaining three conditions.
After mounting on aluminum stubs, the specimens When bonded to enamel, failure analysis revealed the
were coated with a thin gold layer using a gold sputter- highest amount of adhesive failures when Clearfil SE
ing device (Sputtering device 07 120, Balzers Union, was bonded to bur-cut enamel (Table 4). This was also
Liechtenstein) prior to examination in the Philips XL- characteristic of the relatively high amount of mixed
30 Fe-SEM (Eindhoven, The Netherlands). failures (including enamel) when Clearfil SE was bonded
Van Meerbeek & Others: Bond Strength to Variously Prepared Enamel and Dentin 651

to laser-irradiated enamel (Table


4). For OptiBond FL, the rela-
tively high amount of adhesive
failures when bonded to acid-
etched, laser-irradiated and bur-
cut enamel is noteworthy (Table
5). Also, when Optibond FL was
bonded to unetched enamel sur-
faces, the amount of adhesive
failures significantly increased,

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confirming the less optimal bond-
ing effectiveness when no sepa-
rate acid-etching was carried out.
Finally, all samples of OptiBond
FL bonded to non-etched,
Er:YAG-irradiated enamel were
recorded as mixed failures, includ-
ing enamel (Table 5).
Figure 2. Bar plot (+95% confidence interval) of µTBS results for Clearfil SE. Black bars represent results
When bonded to dentin, the to enamel, white bars to dentin.
µTBS means ranged from 6.9
MPa for Optibond FL when
applied to non-etched, laser-irra-
diated dentin to 59.6 MPa for
Optibond FL when applied to
etched, bur-cut dentin (Table 2).
Clearfil SE bonded least effec-
tively to laser-irradiated dentin
that was significantly different
from all other experimental and
control conditions (Table 2 and
Figure 2). The µTBS of Clearfil
SE to air-abraded dentin was sig-
nificantly higher than all other
experimental and control condi-
tions except when bonded to SiC-
paper prepared dentin and bur-
cut enamel (nearly significantly
different). Bonding of Clearfil SE
to diamond-sonoabraded dentin Figure 3. Bar plot (+95% confidence interval) of µTBS results for Optibond FL. Black bars represent results
to enamel, white bars to dentin.
was equally effective as when
Table 2: µTBS to Enamel and Dentin
ENAMEL SonicSys Air Abrasion Er:YAG Laser Diamond Bur SiC-Paper
Clearfil SE µTBS (MPa) ± SD 22.0 ± 7.0a 26.3 ± 11.1a 19.2 ± 4.7a 22.4 ± 6.8a 24.5 ± 11.4a
ptf/n 0/12 0/9 0/12 0/12 0/9
OptiBond FL (AE) µTBS (MPa) ± SD 30.3 ± 7.5A 37.8 ± 12.9A 20.3 ± 4.0B 36.9 ± 9.8A 36.2 ± 11.5A
ptf/n 0/12 0/11 0/12 0/17 0/10
OptiBond FL (NAE) µTBS (MPa) ± SD 15.1 ± 10.7a,b 25.6 ± 7.2b 10.0 ± 3.2a 20.1 ± 8.1b 24.9 ± 7.3b
ptf/n 2/12 0/11 0/11 0/11 0/13
DENTIN SonicSys Air Abrasion Er:YAG Laser Diamond Bur SiC-Paper
Clearfil SE µTBS (MPa) ± SD 30.4 ± 10.7a 54.1 ± 13.0b 12.7 ± 6.9c 37.7 ± 10.5a 45.5 ± 16.6a,b
ptf/n 0/12 0/10 0/11 0/8 0/10
OptiBond FL (AE) µTBS (MPa) ± SD 39.9 ± 13.4A 54.9 ± 16.3A,B 18.6 ± 5.5C 59.6 ± 16.8B 51.6 ± 19.6A,B
ptf/n 0/10 0/10 0/9 0/21 0/12
OptiBond FL (NAE) µTBS (MPa) ± SD 41.9 ± 16.7a 24.6 ± 17.6a,b 6.9 ± 1.2b 27.3 ± 13.6a,b 41.8 ± 21.2a
ptf/n 0/11 3/11 5/9 0/11 0/11
SD = Standard deviation; ptf = pre-testing failures; n = total number of specimens measured; Data marked with same superscript are not significantly different from one another.
652 Operative Dentistry

bonded to bur-cut and SiC-paper prepared dentin, but when the high number of pre-testing failures of
significantly less effective than bonding to air-abraded Optibond FL to Er:YAG irradiated dentin (five out of
dentin. Separate acid-etching significantly increased nine specimens) would have been included (µTBS=0
the µTBS of Optibond FL when bonded to air-abraded MPa), bonding of Optibond FL to non-etched, Er:YAG
dentin, Er:YAG-irradiated and bur-cut dentin, but not irradiated dentin would be significantly worse com-
to sonoabraded and SiC-paper prepared dentin (Tables pared to all other experimental and control groups with
2, 3 and Figure 3). Following acid-etching (AE), the exception of bonding to non-etched, air- abraded
OptiBond FL had the least effective bond to laser-irra- dentin. Also, for the latter, three out of 11 specimens
diated dentin, while bonding to air-abraded dentin was failed prior to being measured.
not significantly different from both control conditions. When bonding to dentin, the failure analysis of

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The use of sonoabrasion resulted in a µTBS of Optibond Clearfil SE revealed that (as when bonded to enamel)
FL to dentin that was only significantly lower than
Optibond FL bonded to dia-
mond-bur cut dentin (Table 2, Table 3: p-Values Comparing OptiBond FL Applied with (AE) and without Acid-Etching
and Figure 3). When enamel (NAE) and Clearfil SE Versus OptiBond FL (AE) (Mann-Whitney U Test)
was not separately acid-etched AE vs NAE C-SE vs O-FL
(NAE), bonding of Optibond FL Enamel Dentin Enamel Dentin
to Er-YAG irradiated dentin SonicSys 0.0026 0.9177 0.0068 0.1072
was least effective, although Air Abrasion 0.0192 0.0031 0.0562 0.8534
its µTBS was only significant- Er:YAG <0.0001 0.0028 0.7987 0.0674
ly different from Optibond FL Diamond bur 0.0001 <0.0001 0.0002 0.0008
bonded to diamond-sonoabrad-
SiC-paper 0.0099 0.2351 0.0350 0.3136
ed and SiC-paper prepared The significance level _ was set at 0.01 to correct for multiple comparison testing (Bonferroni correction); p-values underlined are
dentin (Table 2). However, smaller than 0.01 and thus indicate significant difference; p-values underlined with a dashed line indicate nearly significant difference.

Table 4: Failure Analysis of Clearfil SE


ENAMEL SonicSys Air Abrasion Er:YAG Laser Diamond Bur SiC-Paper
Adhesive failure 0 0 2 4 0
Mixed failure including enamel 0 2 8 1 3
Mixed failure including resin 12 7 2 7 6
DENTIN SonicSys Air Abrasion Er:YAG Laser Diamond Bur SiC-Paper
Adhesive failure 2 0 5* 1 0
Mixed failure including dentin 1 5 3 5 5
Mixed failure including resin 9 5 3 2 5
*Micro-cohesive in dentin

Table 5: Failure Analysis of OptiBond FL


ENAMEL-Acid Etch SonicSys Air Abrasion Er:YAG Laser Diamond Bur SiC-Paper
Adhesive failure 0 0 11 9 2
Mixed failure including enamel 3 2 1 0 2
Mixed failure including resin 9 9 0 8 6
ENAMEL-No Acid Etch SonicSys Air Abrasion Er:YAG Laser Diamond Bur SiC-Paper
Adhesive failure 8 2 0 5 4
Mixed failure including enamel 0 3 11 4 0
Mixed failure including resin 2 6 0 2 9
DENTIN-Acid Etch SonicSys Air Abrasion Er:YAG Laser Diamond Bur SiC-Paper
Adhesive failure 2 0 6* 3 0
Mixed failure including dentin 6 5 0 7 6
Mixed failure including resin 2 5 3 11 6
DENTIN-No Acid Etch SonicSys Air Abrasion Er:YAG Laser Diamond Bur SiC-Paper
Adhesive failure 1 3 4* 9 2
Mixed failure including dentin 6 1 0 1 7
Mixed failure including resin 4 4 0 1 2
*Micro-cohesive in dentin
Van Meerbeek & Others: Bond Strength to Variously Prepared Enamel and Dentin 653

characteristic of all adhesive groups is the relatively were selected (Table 1; Van Meerbeek & others, 2001;
high amount of adhesive and mixed failures, including 2003). Both adhesives have repeatedly been documented
dentin (Table 4). Again, when Optibond FL was bonded to consistently provide high bond strengths to enamel
without acid etching, the number of adhesive failures and dentin (Tay & others, 2000a; Armstrong, Keller &
increased with the exception of the sonoabrasion group Boyer, 2001; Inoue & others, 2001b). Special attention
(Table 5). was given to correct application procedures, in particu-
Comparing the bonding effectiveness to enamel of the lar, to apply both adhesives to tooth substrates that
two-step self-etch adhesive Clearfil SE with that of the were prepared in a standardized way, as previously
three-step etch&rinse adhesive OptiBond FL described in detail (De Munck & others, 2002b). As a
(including acid-etching), Clearfil SE bonded significantly tool to prepare specimens for µTBS testing, the authors

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worse (p<0.01) to diamond sonoabraded and diamond- used the MicroSpecimen Former developed at the
bur prepared enamel than OptiBond FL (Table 3). No University of Iowa (Armstrong & others, 2001). This
significant difference in bonding of Clearfil SE and device greatly reduces the technique sensitivity of spec-
OptiBond FL was found when applied to Er:YAG-irra- imen preparation since any hand manipulation is
diated enamel, with bonding to air-abraded and SiC- excluded (De Munck & others, 2002a). It also enables
paper prepared enamel approaching significant differ- the preparation of cylindrical µTBS specimens that opti-
ence. At dentin (Table 3), Optibond FL bonded only sig- mally distribute internal stress and cause them to fail at
nificantly better to diamond-bur prepared dentin than the interface itself (Armstrong & others, 2001). In order
Clearfil SE. In all other experimental and control con- to prepare a relatively flat surface using the SonicSys
ditions, Clearfil system, the air-abrasion unit and the Er:YAG laser, flat
SE did not bond
significantly dif-
ferently from
OptiBond FL.
Representative
examples of fail-
ure modes imaged
by Fe-SEM are
shown in Figures
4-8. Fe-SEM pho-
tomicrographs of
enamel and dentin
subjected to the
three experimen-
tal and two con-
trol tooth tissue Figure 4. Fe-SEM photomicrographs of a fractured dentin-adhesive interface with the dentin side in (a) and the composite side
in (b) when Clearfil SE was bonded to diamond sonoabraded dentin. The specimen failed mixed adhesively (A) at the inter-
preparation tools face and cohesively within the adhesive resin (CA).
are shown in
Figures 9-13.

DISCUSSION
In order to meas-
ure the bonding
effectiveness to
diversely pre-
pared enamel and
dentin surfaces,
two commercially
available adhe-
sives that repre-
sent a three-step
etch&rinse
(OptiBond FL)
and a two-step Figure 5. Fe-SEM photomicrographs of a fractured dentin-adhesive interface with the dentin side in (a) and the composite side
self-etch (Clearfil in (b) when Clearfil SE was bonded to air-abraded dentin. The interface failed mixed adhesively (A) at the interface and cohe-
SE) approach sively within the adhesive resin (CA) and within the resin composite (CC).
654 Operative Dentistry

vations). The rather thin


smear layer produced by
sonoabrasion and wet
sanding with 600-grit
SiC-paper did not
obstruct the formation of
a hybrid layer. As the
thickness of the hybrid
layer has been shown not
to influence bond

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strength (Inoue S & oth-
ers, 2001b), the mild self-
etch effect of the
OptiBond FL primer that
resulted in hybrid-layer
formation most likely
explains that separate
acid-etching of dentin did
not result in a significant-
ly higher µTBS in the
case where OptiBond FL
was applied to sonoabrad-
ed or SiC-paper-prepared
dentin.
Comparing the bonding
effectiveness of the con-
ventional three-step
Figure 6. Fe-SEM photomicrographs of a fractured dentin-adhesive interface with the dentin side in (a) and (b), and
the composite side in (c) and (d) when Clearfil SE was bonded to Er:YAG-irradiated dentin. The interface failed uni- etch&rinse adhesive
formly cohesively within dentin (CD). OptiBond FL to the two-
step, self-etch adhesive
enamel and dentin surfaces were initially prepared Clearfil SE to enamel
using the diamond saw and/or wet sanding with 600-grit (Table 3), the µTBS of Optibond FL exceeded Clearfil SE
SiC-paper. Only a small layer was subsequently in all groups except Er:YAG-irradiated enamel, to which
removed through respective diamond sonoabrasion, air both adhesives bonded equally effectively. Due to the
abrasion and Er:YAG-laser irradiation. In this way, the Bonferroni correction applied because of multiple com-
authors expect to have prevented surface enlargement parison testing, significant differences were only found
by irregularities and, thus, to have avoided a false-posi- for sonoabrasion and diamond-bur preparation at the
tive increase of bond strength. The Fe-SEM images con- level of p<0.01 (Table 3). However, the p-values for air
firmed that the enamel and dentin surfaces were uni- abrasion and SiC-paper preparation approached statis-
formly prepared following the three experimental and tically significant differences. All together, the authors
two control conditions (Figures 9-13). can, therefore, conclude that the “etch&rinse” approach
using phosphoric acid remains the more reliable bond-
The results obtained in this study clearly demonstrate ing technique for enamel, though the difference between
that separate acid etching prior to applying an the etch&rinse and self-etch approach becomes smaller
etch&rinse adhesive is indispensable for enamel and (Inoue & others, 2000; Van Meerbeek & others, 2001,
dentin, by which the hypothesis advanced was rejected 2003; De Munck & others, 2002a). At dentin, only the
(Table 3). The only exceptions were the bonding of diamond-bur preparation appeared to have hindered
Optibond FL to diamond sonoabraded and to SiC-paper adequate micromechanical bonding through hybridiza-
prepared dentin. A plausible explanation for the latter is tion. This is not unexpected considering the regular-grit
that sonoabrasion and the use of 600-grit SiC paper pro- diamond the authors applied results in a relatively thick
duces a relatively thin smear layer (Figures 9 and 13). smear layer (Figure 12), as compared to the superficial
The primer of OptiBond FL is acidic (pH=1.78, meas- smearing effect resulting from the other tissue prepara-
ured using Inolab pH Level 2, WTW, Welheim, tion techniques and 600-grit SiC-paper, in particular.
Germany) (De Munck & others, 2002a). Consequently, Such bur-dependent bonding effectiveness has repeat-
due to a self-etch effect induced by the primer, itself, a edly been reported for so-called “mild” self-etch adhe-
thin, submicron hybrid layer is produced on a 600-grit sives (Inoue & others, 2000; Tay & others, 2000b; Inoue
SiC-paper prepared dentin surface (unpublished obser- & others, 2001a; Van Meerbeek & others, 2001; De
Van Meerbeek & Others: Bond Strength to Variously Prepared Enamel and Dentin 655

Munck & others, 2002a),


while the “strong” self-
etch and etch&rinse
adhesives, thanks to their
higher etching aggres-
siveness, are rather
insensitive to the tooth
surface preparation
mode.
Diamond Sonoabra-

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sion (SonicSys)
Except for OptiBond FL
bonded to acid-etched
dentin, diamond-sonoabra-
sion resulted in tooth sur-
faces that are equally
receptive to bonding com-
pared to conventional dia-
mond-bur prepared sur-
faces.
No data with regard to
bond strength of adhesives
to diamond sonoabraded
enamel and dentin are
available in the litera-
ture. In a study by Setien
and others (2001), Figure 7. Fe-SEM photomicrographs of a fractured enamel-adhesive interface with the enamel side in (a) and (b),
and the composite side in (c) and (d) when OptiBond FL was bonded to acid-etched, Er:YAG-irradiated enamel. The
SonicSys Approx (Kavo) interface failed cohesively within enamel (CE) and within the particle-filled adhesive (C ).
A
was investigated among
other cavity preparation
devices. The authors of that study concluded that the acid etching. Laurell, Lord and Beck (1993) reported no
way the cavity was prepared did not affect the sensi- significant difference in shear bond strength to enamel
tivity of the composite restoration for microleakage at between an acid-etched and solely air-abraded surface.
the (acid-etched) enamel and dentin margins. Since Likewise, Keen, von Fraunhofer and Parkins (1994)
SonicSys Approx only differs from SonicSys Micro with obtained similar shear bond strengths to air-abraded
regard to the shape of the instruments’ active end, the and acid-etched (35% phosphoric acid) enamel, and even
authors of this study believe that the latter data can be higher bond strengths to dentin obtained with air abra-
extrapolated to the SonicSys Micro tested in this study. sion compared with acid etching. Also, Doty and others
Consequently, this latter study substantiates the bond (1994) concluded that air abrasion technology had the
strength data gathered in this study using diamond potential to prepare enamel bonding surfaces equal to
sonoabrasion. those obtained from acid etching.
Air Abrasion However, many papers reported the contrary. Roeder
and others (1995) reported that acid etching of enamel
Bonding to air-abraded enamel and dentin was not sig- and the priming of dentin was necessary to achieve
nificantly different from bonding to conventional dia- maximum bond strengths to air abraded tissues. In
mond-bur prepared tooth surfaces for either adhesive addition, according to a study by Berry and Ward (1995),
tested. Moreover, as mentioned above, the mild self-etch tensile bond strengths of resin composite to acid-etched,
adhesive Clearfil SE bonded even significantly better to air-abraded enamel were significantly greater than
air-abraded dentin than to the coarse, thick, smear those of unetched, air-abraded enamel. Also, a shear
layer produced by the diamond bur. bond strength study by Bae and others (1996) showed
In the literature, great controversy exists regarding that “air abrasion” conditioning was less effective than
whether air abrasion produces a micro-retentive surface conventional acid etching. Canay, Kocadereli and Akça
that is sufficiently receptive to bonding so that acid etch- (2000) found that enamel preparation through solely
ing is no longer needed. Several studies showed that air sandblasting using a micro-etcher resulted in a signifi-
abrasion alone yielded results equal to or superior to cantly lower bond strength than conventional acid-etch-
656 Operative Dentistry

ing and, therefore, should


not be advocated for clini-
cal use as an enamel con-
ditioner. Finally, Valentino
and Nathanson (1996) con-
cluded that air abrasion
could be effective for
dentin bonding when used
in conjunction with acid
etching but should not be

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used as a sole surface
treatment prior to bonding
composite to enamel or
dentin. All the latter stud-
ies agree with the present
results, suggesting that it
remains mandatory to sep-
arately acid-etch air-
abraded enamel and
dentin when applying an
etch&rinse adhesive.
Er:YAG Laser
Thanks to the ablation
process that involves
micro-explosions of tooth
Figure 8. Fe-SEM photomicrographs of a fractured enamel-adhesive interface with the enamel side in (a) and (b),
substrate and the greater
and the composite side in (c) and (d) when Clearfil SE was bonded to SiC-paper prepared enamel. The interface volatilization of intertubu-
failed mixed adhesively at the interface (A), cohesively within the adhesive (CA) and cohesively within the resin lar compared to peritubu-
composite (CC). lar dentin (Armengol &
others, 1999a), the Er:YAG
laser exposes a typical
imbricate patterned sur-
face (Kameyama & others,
2001) with open dentin
tubuli (Figure 11). More-
over, this ablation process
leaves no hydroxyapatite-
depleted collagen on the
surface. Consequently, when
the laser-conditioned tis-
sue is not separately acid-
etched, collagen is not
exposed and, consequently,
no hybrid layer can be
formed (Kataumi & oth-
ers, 1998), also eliminating
the need for an hydrophilic
dentin primer to penetrate
within the organic tissue
(Armengol & others,
1999b). Despite this differ-
ent approach, laser manu-
facturers commonly argue
that at low-energy settings
Figure 9. Fe-SEM photomicrographs of diamond sonoabraded enamel in (a) and (b), and of diamond sonoabrad- enamel and dentin can be
ed dentin in (c) and (d). Note the clear marks at the enamel surface resulting from sonoabrasion. At the dentin sur- conditioned with the
face, sonoabrasion resulted in a relatively thin smear layer with the dentin tubules almost completely closed.
Van Meerbeek & Others: Bond Strength to Variously Prepared Enamel and Dentin 657

Er:YAG laser when replac-


ing conventional acid-etch-
ing as pretreatment for
adhesive procedures. How-
ever, bond strengths to
Er:YAG-irradiated tooth
substrate reported in the
literature are often confus-
ing and even contradictory.
Kataumi and others,

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(1998) observed resin-
dentin interfaces and
found microcracks below
the hybrid layer, indicat-
ing that subsurface dam-
age was caused by Er:YAG
irradiation. These findings
confirm the authors’ previ-
ous study that demon-
strated using Fe-SEM
resulted in significantly
more microcracks at laser-
irradiated rather than at
fractured dentin surfaces
(De Munck & others,
2002b). Very conclusive
Figure 10. Fe-SEM photomicrographs of air-abraded enamel in (a) and (b), and of air-abraded dentin in (c) and (d).
evidence of deficient hybrid-
Note at dentin that air abrasion resulted in an irregular surface without any patent tubules.
ization to Er:YAG lased
dentin was provided in a
recent study using trans-
mission electron micro-
scopy by Ceballo and oth-
ers (2002). The results
showed a 3-4 µm severely
altered dentin subsurface
beneath which collagen
fibrils appeared to have
lost cross-banding and
were fused together, elimi-
nating interfibrillar spaces
and, thus, impeding
hybridization.
This subsurface damage
caused by laser irradiation
can also exceed the thick-
ness of the hybrid layer,
leaving a weakened sub-
strate without resin rein-
forcement underneath.
This, in particular, could
explain the cohesive frac-
tures of dentin and enamel
frequently observed in this Figure 11. Fe-SEM photomicrographs of Er:YAG-irradiated enamel in (a) and (b), and of Er:YAG-irradiated dentin
and in other studies in (c) and (d). (a,b) The surface is very rough and irregular. The enamel prisms are clearly visible, but appear to
have been partially melted at their exposed ends. Micro-cracks in between enamel prisms can be observed. (c,d)
(Martinez-Insua & others,
Dentinal tubules are clearly visible and are not covered by a smear layer. The surface is very rough and irregular
2000; Kameyama & oth- with a typical imbricate patterned topography. Also a lot of microcracks can be observed.
658 Operative Dentistry

and dentin surfaces, in gen-


eral, results in significantly
lower bonding effectiveness
as compared to bonding to
diamond-bur prepared sur-
faces. Subsurface damage
initiated by Er:YAG abla-
tion is most likely the major
reason for the decrease in
µTBS and, thus, might

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compromise clinical bond-
ing on the long-term.

Figure 12. Fe-SEM photomicrographs of diamond-bur prepared dentin. Note the rather coarse scratches across Acknowledgements
dentin as part of a rather thick smear layer produced by the diamond bur. All dentin tubules are closed.
The authors thank the manufac-
turers of the respective instru-
ments and materials used in
this study. A special thanks goes
to High Tech Laser (Herzele,
Belgium) for putting the Er:YAG
laser at our disposal and to Mr P
Verheyen, who, as an expert
user of the Er:YAG laser, pre-
pared all laser-irradiated sur-
faces. This study was conducted
in part thanks to the support
offered by the Toshio Nakao
Chair for Adhesive Dentistry
inaugurated at the Catholic
University of Leuven with G
Vanherle awarded as Chairholder.
Figure 13. Fe-SEM photomicrographs of SiC-paper prepared dentin. Note the scratches produced by wet-sand-
ing dentin with SiC paper. The scratches are less irregular and deep than those produced by the diamond bur in
Figure 12. All dentin tubules are closed.

ers, 2000). A tensile bond strength study of Clearfil SE (Received 24 September 2002)
applied to Er:YAG irradiated bovine enamel and dentin
revealed that treatment with phosphoric acid, air-scaler,
ultrasonic scaler and air-abrasion after Er:YAG irradia- References
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