Effect of Smear Layer Thickness on Bond

Strength Mediated by Three All-in-One

Self-etching Priming Adhesives
Chihiro Tania/Werner J. Fingerb

Purpose: The aim of this study was to investigate the effect of dentin smear-layer thickness on the bond
strength of three all-in-one adhesives of different acidity.
Materials and Methods: Peripheral dentin was prepared by wet grinding on SiC papers (80-, 180-, 240-,
320-, 400-, 600-, 4000-grit), and by turbine cutting with supercoarse, coarse, medium, fine, or extrafine
diamond burs. The smear layer thickness (SLT) was measured microscopically. The relationship between
SLT and average grain size of the abrasives used to prepare the dentin surface was described by regres-
sion analysis. Shear bond strength (SBS) was determined for the following adhesives: AC Bond, pH 2.1
(experimental, Heraeus); AQ Bond, pH 2.5 (Sun Medical); and Prompt L-Pop, pH 1.1 (3M-Espe). Six spec-
imens were tested for each adhesive on dentin ground with each of the seven SiC grit sizes. The mode
of failure was inspected by SEM. SBS data were analyzed by one-way ANOVA and Fisher’s PLSD test at
p < 0.05.
Results: A logarithmic relationship between SLT and grain size of the abrasives was established. The
coefficient of determination R2 for the regression line was 0.803. Shear bond strengths for the individual
adhesives did not differ significantly by SiC grit size. SBS of AC Bond (18.3 MPa) was greater than the
SBS of AQ Bond and Prompt L-Pop (16.9 MPa). Cohesive failures were consistently found in resin com-
posite or adhesive.
Conclusion: Smear layer thickness increased with decreasing SiC grit numbers and increasing diamond
bur roughness. In spite of the widely differing acidity, all three adhesives tested were equally effective
over the range of SLT from 2.6 µm through 0.9 µm.

J Adhes Dent 2002; 4: 283–289. Submitted for publication: 24.05.02; accepted for publication: 26.08.02.

entin smear layers are produced during me-
D chanical cavity preparation. It has been report-
ed that thick smear layers could compromise the
a Instructor, Department of Operative Dentistry, Showa University,
School of Dentistry, Tokyo, Japan.
b
Professor, Dental Materials and Technology, School of Dental Med-
icine, Department of Preclinical Dentistry, University of Cologne,
Cologne, Germany.
Reprint requests: Prof. Dr. Werner J. Finger, Department of Preclinical
Dentistry, School of Dental Medicine, University of Cologne, Kerpen-
erstr. 32, D-50931 Cologne, Germany. Tel: +49-2133-514996, Fax:
+49-2133-513410. e-mail: wjfinger@aol.com
efficiency of moderately acidic self-etching primer
adhesives, since early neutralization of the adhe-
sive by dissolution of the smear layer might hamper
superficial demineralization of solid dentin, which
is required for collagen exposure and thus effective
hybridization upon penetration and polymerization
of the adhesive resin.1 Smear layers of differing
thickness result from dentin preparation with abra-
sive papers of differing roughness.2,7 Koibuchi et
al2 found that the smear layer thickness decreased
with decreasing particle size of the abrasive paper.
Watanabe et al7 investigated the effect of the
smear layer thickness prepared with abrasive pa-
per of different grit numbers on dentin bonding with
an experimental self-etching dentin primer, an
aqueous solution of 20% 2-methacryloxyethyl phe-

Vol 4, No 4, 2002 283

Tani/Finger
nyl hydrogen phosphate (Phenyl-P), and 30% 2-hy-
droxyethylmethacrylate (HEMA), covered with a
light-curing bonding agent containing 5% Phenyl-P in
triethyleneglycol dimethacrylate (TEG-DMA). The
tensile bond strength on dentin was high when the
dentin smear layer was produced with SiC papers ≥
grit #600, and significantly lower when dentin was
prepared on SiC paper ≤ grit #400. Following dentin
preparation on 80- and 180-grit SiC papers, mostly
cohesive failures were found in the hybridized
smear layer. However, in the 400- and 600-grit
groups, mostly cohesive debonding was observed
in the adhesive layer. Inoue et al1 and Ogata et al3
investigated the effect of dentin preparation with
different bur types and coarseness on microtensile
bond strength. Ogata et al3 reported that the bond
strengths to diamond bur cut dentin was signifi-
cantly lower than to dentin prepared either on
600-grit SiC paper or with steel burs. The authors
hypothesized that the differences in bond strength
found were related to differences in smear layer
thickness. Diamond bur preparation produced thick
smear layers and rough surfaces, whereas dentin
prepared with steel burs was smoother and cov-
ered with a thinner smear layer. They concluded
therefore that the ability of self-etching adhesive
monomers to simultaneously demineralize and
penetrate into the dentin surface was related to the
smear layer thickness and the surface roughness.
Inoue et al1 reported that microtensile bond
strength to dentin prepared with superfine diamond
cutting instruments was higher than with regular
grit diamond burs.
The purpose of this study was to investigate the
effect of dentin smear-layer thickness on the bond
strength of three all-in-one adhesives possessing
different levels of acidity. The null hypothesis to be
tested was: the bonding efficiency of self-etching
primer adhesives to dentin covered with smear lay-
ers of different thicknesses is independent of pH
variations between 1.1 and 2.5.
MATERIALS AND METHODS
Two commercial dentin bonding systems and one
experimental adhesive were used in this study
(Table 1). Extracted human teeth stored in 1%
chloramine solution for a maximum of 6 months
and possessing at least one sound labial or oral
surface were selected for the study. The teeth were
embedded in slow-curing epoxy resin with the target
284
surface facing the bottom of cylindrical rubber
molds and ground flat on wet 80-grit SiC paper until
peripheral dentin was exposed.
Determination of Smear Layer Thickness
Dentin smear layer thickness produced on wet
SiC paper
Two dentin surfaces each were prepared by wet
grinding on 80-, 180-, 240-, 320-, 400-, 600-, or
4000-grit SiC paper (Table 2). The specimens were
hand ground (60 strokes for each consecutive grit
number) under gentle pressure in one direction
only. Following the final grinding step, the dentin
surfaces were coated with a thin layer of the com-
mercial hydrophobic resin Gluma Solid Bond S
(Heraeus Kulzer, Hanau, Germany) and light acti-
vated for 60 s with the tungsten halogen light-cur-
ing unit Translux CU (Heraeus Kulzer) at
600 mW/cm2 output. The specimens were then re-
placed in the cylindrical rubber molds and covered
with an approximately 5-mm-thick layer of the
self-curing methylmethacrylate base resin Techno-
vit 4004 (Heraeus Kulzer). After 15 min curing time
at ambient temperature, the specimens were re-
moved from the rubber mold, sectioned perpendic-
ularly through the flat dentin interface with the
Isomet low-speed diamond saw (Buehler, Lake
Bluff, IL, USA) under water cooling, and hand pol-
ished on wet 4000-grit SiC paper. The thickness of
the dentin smear layers was measured in an inci-
dent light microscope fitted with an ocular screw
micrometer at 1000X magnification, giving a read-
ing accuracy of 0.096 µm. For each of the SiC grits
used, two specimens, ie, four sections were in-
spected. On each of the sections, the smear layer
thickness was determined at seven neighboring
sites approximately 100 µm apart, starting from
the enamel-dentin junction.
Dentin smear layer thickness produced by dia-
mond burs
Following dentin exposure with wet 80-grit SiC pa-
per as above, two specimens were prepared with
each of the five diamond bur types (Table 2) in a tur-
bine handpiece under water cooling. The dentin sur-
faces were prepared (30 strokes for each consecu-
tive grit) under very gentle pressure in one direction
only. The final specimen preparation followed the
procedure described above. The relationship be-
tween the smear layer thickness and the average
The Journal of Adhesive Dentistry
 Tani/Finger

Table 1 Materials tested

Code Materials pH* Manufacturer Lot No. Composition of adhesive

ACB AC Bond** 2.1 Heraeus Kulzer, VP050901Ge1 UDMA, 4-META, acetone, water
Hanau, Germany

Adhesives AQB AQ Bond 2.5 Sun Medical, EG1 MMA, 4-META, UDMA, HEMA, ace-
Shiga, Japan tone, water, coinitiator impregnated
application pellet

PLP Prompt L-Pop 1.1 3M-ESPE, 110490 Methacrylated phosphoric acid es-
Seefeld, Germany ters, phosphine oxide, stabilizer,
fluoride complex, parabenes, water

Resin Composite – Charisma A2 – Heraeus Kulzer, 100053 –

Hanau, Germany

* Values from manufacturers. ** Experimental adhesive.

Table 2 Grinding papers and diamond burs used for dentin

Grit # Grain size (µm) ISO No.

80 200
180 76
240 58
SiC papers 320 46
400 35
600 26
4000 5

Diamond burs Super Coarse 150 806314141504014

Coarse 125 806314141514014
Medium 100 806314141524014
Fine 30 806314141534014
Extra Fine 15 806314141544014

SiC paper: Buehler, Lake Bluff, IL, USA; Diamond Bur: Komet, Germany.

grain size of the abrasives was analyzed by least
square distance regression analysis.
Shear Bond Strength Measurement
Flat peripheral dentin surfaces were produced by
grinding the embedded teeth on wet 80-grit SiC pa-
per, until a sufficiently large dentin area was ex-
posed for bonding of a 3.5-mm-wide resin compos-
ite cylinder. Dentin smear layers were prepared by
wet grinding on 80-, 180-, 240-, 320-, 400-, 600-,
and 4000-grit SiC paper as described above. The
two commercial dentin bonding systems were ap-
plied strictly according to the manufacturer’s in-
structions. The experimental adhesive AC Bond
(Heraeus-Kulzer) was dispensed in a mixing well
and applied to the rinsed and gently air-dried dentin
surface with a saturated brush in three consecutive
coats. The adhesive was left undisturbed for 30 s

Vol 4, No 4, 2002 285

Tani/Finger

each SBS test was sputter coated with gold to ex-

Table 3 Dentin smear layer thickness amine the failure type with the SEM (Quanta 400,
Fei, Kassel, Germany).
Smear layer thickness
(µm)

SiC papers by 80 2.6 ± 0.6

grit size 180 2.7 ± 0.7 RESULTS
240 2.1 ± 0.8
320 1.9 ± 0.6
400 1.4 ± 0.5
Smear Layer Thickness
600 1.3 ± 0.5
4000 0.9 ± 0.3 The smear layer thicknesses resulting from SiC pa-
per grinding and diamond bur cutting are listed in
Diamond burs Super Coarse 2.8 ± 0.5
Coarse 2.4 ± 0.4 Table 3.
Medium 2.2 ± 0.5
Fine 1.2 ± 0.3 Smear layer thickness on dentin produced by
Extra Fine 1.0 ± 0.3
grinding with SiC paper
n=28 from n=4 specimens, mean ± SD The maximal thickness found was 2.7 ± 0.7 µm
when dentin was ground on 180-grit SiC paper, and
the minimal thickness was 0.9 ± 0.3 µm after grind-
ing with 4000-grit SiC paper.

Smear layer thickness on dentin produced by di-

dwell time, followed by 5 s of gentle air drying to vol-
atilize the solvent and light activation for 30 s with
a tungsten halogen curing unit at 600 mW/cm2 out-
put. A split Teflon mold, 3.5 mm in diameter and
2 mm high, mounted on the dentin specimen and
clamped in a stand, was bulk filled with the hy-
brid-type resin composite material Charisma A2
(Heraeus Kulzer), covered with a Mylar strip, and
light activated for 60 s with the halogen light curing
unit Translux CU (Heraeus Kulzer). The specimens
were stored in deionized water at 37°C for 24 h prior
to shear loading in a universal testing machine
(Model 1474, Zwick, Ulm, Germany) with a steel rod
at a crosshead speed of 1 mm/min until rupture oc-
curred. For each bonding system and for each of the
seven dentin preparation modes, six specimens
were produced.
All specimen preparation, processing, and test-
ing was performed at ambient laboratory atmo-
sphere (23 ± 2°C and 50 ± 5% RH).
The results were statistically analyzed by one-way
ANOVA and Fisher’s PLSD test (p < 0.05).
Scanning Electron Microscopy
From each of the materials and each dentin prepa-
ration group, one representative specimen from
amond bur cutting
In the diamond-bur preparation group, the maximal
thickness found was 2.8 ± 0.5 µm produced by the
supercoarse diamond bur, and the minimal thick-
ness was 1.0 ± 0.3 µm, produced by the extrafine
diamond bur.
Figure 1 illustrates the relationship between the
average grain size of SiC papers and diamond burs
used for dentin surface preparation and the result-
ing smear layer thickness. The equation for the
best fit of the regression line by least square dis-
tance is: smear layer thickness = 0.537 ln(grain
size) - 0.147; the coefficient of determination R2 is
0.803.
Shear Bond Strength
Table 4 shows the shear bond strength data for
dentin prepared on SiC papers. When tested by
ANOVA, the shear bond strengths of the individual
adhesives did not differ significantly by SiC grit
(ACB, p = 0.3490; AQB, p = 0.2606; PLP, p =
0.4454). Therefore, the individual means by SiC
grit number were pooled for each of the three adhe-
sives. One-way ANOVA showed significant differenc-
es between the adhesives (p = 0.0011). Post-hoc
testing by Fisher’s PLSD (p < 0.05) revealed that
ACB mediated higher shear bond strength than
AQB and PLP, which were not significantly different.

286 The Journal of Adhesive Dentistry

 Tani/Finger

Fig 1 Logarithmic regres-

sion line indicating a likely
relation between the grain
size of the SiC and diamond
abrasives used and the re-
sulting smear layer thick-
ness.

Table 4 Shear bond strength on dentin prepared on different SiC

papers

Grit size ACB AQB PLP

80 16.4 ± 2.4 16.0 ± 2.9 15.6 ± 1.5

180 17.3 ± 2.0 15.7 ± 2.7 17.3 ± 1.3
240 18.8 ± 1.6 16.8 ± 1.1 17.7 ± 2.8
320 18.5 ± 2.2 16.2 ± 1.1 17.1 ± 1.8
400 19.3 ± 2.4 16.6 ± 2.2 17.1 ± 2.4
600 18.6 ± 1.9 18.7 ± 1.6 18.2 ± 1.5
4000 18.7 ± 2.0 16.7 ± 1.9 17.3 ± 1.9

N=6, mean ± SD (MPa)

In a second statistical approach, all shear bond DISCUSSION

strengths from the three adhesives and the seven
SiC grit numbers were compared by one-way ANOVA
(p = 0.262).
Scanning Electron Microscopy
SEM inspection of the 21 samples proved that the
failure site after shear debonding was consistently
located in the adhesive resin or in resin composite.
Figure 2 shows representative examples of the co-
hesive failure morphology found with ACB, prepared
on SiC paper grits 600 and 80, after debonding from
dentin.
The quality and thickness of smear layers resulting
from mechanical dentin preparation depend on the
cutting instruments used. As a rule, the smear lay-
er thickness will increase with increasing grain size
of the abrasive, independent from the type of abra-
sive (SiC or diamond). This study showed that the
smear layer produced using very fine to very coarse
abrasives was from 0.9 to 2.8 µm thick. Often, in
vitro studies on the bonding efficiency of dentin ad-
hesives are performed on dentin prepared on wet
600-grit SiC paper, closely matching the smear
thickness produced with a fine-grained diamond
bur. It is suggested to instead use 180-grit SiC pa-

Vol 4, No 4, 2002 287

Tani/Finger
Fig 2 Scanning electron micrographs showing the mor-
phology of ACB specimens after debonding by shear loading.
The respective dentin bonding surfaces were ground on 80-
and 600-grit SiC paper. In both cases, cohesive failure oc-
curred in resin close to the bonding interface.
per, since the smear layer produced is more similar
to medium or coarse diamonds, which are often se-
lected as preparation instruments. Under such con-
ditions, the smear layer thickness is approximately
2.6 µm, as found in the present investigation.
When evaluating the efficiency of moderately
acidic self-etching primer adhesives, the potential
of a product can be more relevantly described when
applied on a thick smear layer. It might be speculat-
ed that self-etching primer compounds with higher
pH are less effective in solubilizing a thick smear
layer and demineralizing the underlying solid dentin
surface for hybridization than adhesives with a low
pH. The fact that adhesives produce adequate
288
bonding even when applied on dentin covered with
almost the thickest smear layer possible proves
that such products will be effective under all com-
mon clinical preparation conditions that produce
thinner smear layers.
The rationale for using dentin surfaces prepared
with SiC paper for bond strength evaluation is relat-
ed to the macro shear bond strength test used,
where reasonable testing requires a flat bonding in-
terface. This condition cannot, however, be guaran-
teed by diamond bur cutting.
The dentin smear layer may be considered a nat-
ural barrier to penetration of self-etching adhesives
and for demineralization of the underlying intact
dentin. Superficial dentin demineralization is, how-
ever, an indispensable condition for hybridization
and reliable dentin sealing and bonding.4-6 Tay et al5
investigated the effect of self-etching primers on
resin composite bonding to dentin covered with a
thick smear layer, ie, following grinding on 60- and
80-grit SiC paper. They reported that the smear lay-
er was transformed into a kind of hybridized layer,
and that the thickness of this hybridized smear var-
ied with the smear layer thickness. In contrast, the
thickness of the underlying collagen-adhesive hy-
brid layer remained unaffected. Since these two
types of hybrid layers are supposed to function to-
gether as a unit without separation during the mi-
crotensile bond strength test, the authors suggest-
ed that the bonding efficiency of self-etching primer
adhesives would be similar on smear layer-free den-
tin and on dentin covered with a thick smear layer.
Self-etching primer systems include different
acidic monomers. Most self-etching primers are
moderately acidic, with pH values between 1.8 and
2.5, whereas only a few products on the market
may be classified as strongly acidic with a pH
around 1.0.5 In the present investigation, apart
from determining the smear layer thickness, no at-
tempt was made to characterize the quality of the
smear produced, which might have an essential ef-
fect on the penetrability of or dissolution in the ad-
hesives applied.
The thickest smear layer found was 2.8 µm, fol-
lowing preparation with a super coarse diamond
bur. This figure is comparable to the smear layer
thickness produced after grinding on 80- to 240-grit
SiC paper or cutting with coarse or medium-grained
diamond burs, but thicker than the smear coatings
resulting from all other abrasives tested. Neverthe-
less, the shear bond strengths mediated with each
of the three adhesives did not differ significantly
The Journal of Adhesive Dentistry
 Tani/Finger

over the range of smear layers produced with 80- to

4000-grit SiC paper, proving that, in spite of their
widely differing acidity, the three adhesives are uni-
versally applicable and compatible with any com-
mon preparation method. Scanning electron mi-
croscopy of the dentin sites of debonded speci-
mens showed consistently cohesive failures in res-
in close to the bonding interface. It is therefore as-
sumed that the bonding efficiency is mainly related
to the adhesives’ mechanical characteristics, which
is a function of their individual composition and de-
gree of polymerization.

CONCLUSION

In conclusion, the null hypothesis is accepted,

since the differences in pH of the three adhesives
tested had no effect on the shear bond strengths
mediated to dentin surfaces covered with smear lay-
ers between and 0.9 µm and 2.7 µm in thickness.

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3. Ogata M, Harada N, Yamaguchi S, Nakajima M, Tagami J. Ef-
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5. Tay FR, Carvalho R, Sano H, Pashley DH. Effect of smear lay-
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