Dental Materials 19 (2003) 758–767

www.elsevier.com/locate/dental

The influence of the dentin smear layer on adhesion: a self-etching

primer vs. a total-etch system
Sofia S.A. Oliveiraa, Megan K. Pugacha, Joan F. Hiltonb, Larry G. Watanabea,
Sally J. Marshalla, Grayson W. Marshall Jr.a,*
a
Department of Preventive and Restorative Dental Sciences, University of California, 707 Parnassus Avenue D2246, San Francisco, CA 94143 0758, USA
b
Department of Epidemiology and Biostatistics, University of California, San Francisco, CA, USA

Abstract
Objective. To determine the effect of dentin smear layers created by various abrasives on the adhesion of a self-etching primer (SE) and
total-etch (SB) bonding systems.
Methods. Polished human dentin disks were further abraded with 0.05 mm alumina slurry, 240-, 320- or 600-grit abrasive papers, # 245
carbide, # 250.9 F diamond or # 250.9 C diamond burs. Shear bond strength (SBS) was evaluated by single-plane lap shear, after bonding
with SE or SB and with a restorative composite. Smear layers were characterized by thickness, using SEM; surface roughness using AFM;
and reaction to the conditioners, based on the percentage of open tubules, using SEM.
Results. Overall, SBS was lower when SB was used than when SE was used. SBS decreased with increasing coarseness of the abrasive in
the SE group. Among burs, the carbide group had the highest SBS, and 320- and 240-grit papers had SBS close to the carbide group. Surface
roughness and smear layer thickness varied strongly with coarseness. After conditioning with SE primer, the tubule openness of specimens
abraded by carbide bur did not differ from 240- or 320-grit paper, but did differ from the 600-grit.
Significance. Even though affected by different surface preparation methods, SE yielded higher SBS than SB. The higher SBS and thin
smear layer of the carbide bur group, suggests its use when self-etching materials are used in vivo. Overall, the 320-grit abrasive paper
surface finish yielded results closer to that of the carbide bur and its use is recommended in vitro as a clinical simulator when using the SE
material.
2003 Academy of Dental Materials. Published by Elsevier Ltd. All rights reserved.
Keywords: Self-etching primers; Smear layer; Burs; Abrasive papers; Dentin adhesion

1. Introduction
The smear layer has been defined as a layer of debris on
the surface of dental tissues created by cutting a tooth [1]. It
varies in thickness, roughness, density and degree of
attachment to the underlying tooth structure according to
the surface preparation [2 – 8].
As part of restorative procedures required by adhesive
dentistry, the smear layer must be removed, modified or
impregnated by the resin to allow for bonding between the
tooth and the restorative material [9 – 11]. The poor
performance of early dentin adhesive systems was thought
to occur because the smear layer was not removed, resulting
in bonding of the adhesive to the surface of the smeared
debris [12], and not to the underlying dentin [1]. As a result,
an acidic conditioner was introduced to dissolve and remove
* Corresponding author. Tel.: þ1-415-476-9119; fax: þ 1-415-476-0858.
E-mail address: graymar@itsa.ucsf.edu (G.W. Marshall Jr.).
0109-5641/$ - see front matter 2003 Academy of Dental Materials. Published by Elsevier Ltd. All rights reserved.
doi:10.1016/S0109-5641(03)00023-X
this layer, allowing the direct contact of the resin with
partially demineralized dentin.
Some studies [7,13,14], show no difference in bond
strength of total-etch adhesive systems to different dentin
smear layers, probably because these systems completely
remove smeared debris from the surface. Nevertheless, the
topography of the dentin surface after removal of the smear
layer would reflect the coarseness of the abrasive and
coarser abrasives would have increased surface area. It
would be reasonable to assume that this roughness
influences the bond strength of the adhesive agents [4,15].
The introduction of self-etching materials in which the
acid conditioning step is eliminated by use of a primer
containing an acidic monomer raises new questions. It has
been stated that the self-etching primers, most likely due to
their intrinsic acidity, have the ability to permeate dentin
smears and impregnate the underlying dentin [16]. The
smear layer components are probably incorporated within
the bonding layers [17], since the dissolved matter is not
 S.S.A. Oliveira et al. / Dental Materials 19 (2003) 758–767
rinsed away. Koibuchi et al. [18] demonstrated that this
hybridized smear layer has an effect on the bond strength of
the self-etching materials and Ogata et al. [19] showed that
different smear layers had different effects on the bond
strength of a self-etching primer to dentin.
Several studies have evaluated the importance of surface
preparation method on bond strength. [13,20] and have
attempted to define the most clinically relevant smear layer
preparation for use in in vitro tests. The preparation of the
sample’s surface with a bur in vitro is complex and time
consuming and may be difficult to standardize. [3,5 – 7]
Most in vitro bond strength studies prepare dentin surfaces
with a 600-grit abrasive paper, even though they do not
indicate the clinical relevance of that surfacing procedure.
[21 – 26] Others treat tooth surfaces with 400-grit, [27,28]
320-grit, [29,30] or even 60-grit, [6] abrasive paper in vitro.
In order to perform clinically relevant research in dentin
adhesive systems in vitro, an increased understanding of the
smear layer is important so that relevant standards for
various approaches to dentin bonding can be developed.
The first objective of this study was to establish a
standard in vitro method to create a smear layer that most
closely mimics those produced by clinical burs. Secondly,
we tested the hypotheses that, when a total-etch adhesive
system is used, shear bond strength does not depend on the
surface preparation method (specifically, the type or
coarseness of the abrasive used to create a smear layer),
but when a self-etching primer is used shear bond strength
does depend on these factors. Finally, we hope to better
understand how the self-etching materials interact with the
smear layer.
2. Materials and methods
The specimens used in this study were prepared from
randomly selected human non-carious third molars. All the
teeth were recently extracted (less than three months) from
patients needing extractions as part of their dental treatment
and as approved by the UCSF Committee on Human
Research. They were gamma irradiated and refrigerated in
Hank’s balanced salt solution prior to use. For shear bond
strength tests, teeth were sagittally sectioned into 2
segments with a low-speed diamond saw (Buehler, Lake
Bluff IL, USA) and proximal surfaces were abraded to
remove the enamel and expose the superficial dentin
surface. For characterization of smear layers, dentin disks
were sectioned from approximately the same depth
(occlusal surface , 2 mm above the pulp horns) and a
smear layer on the occlusal side of each disk was prepared.
Smear layers were prepared with seven different surface
preparation methods: # 250.9 F fine diamond bur and #250.9
C coarse diamond bur (Premier Dental Products Co,
Canada- batch numbers 166 and 176, respectively), #245
carbide plain fissure bur (Midwest-Des Plaines, IL- batch
number 0086) all operated in a highspeed handpiece,
759
0.05 mm alumina powder slurry (Buehler Micropolish,
Buehler, Lake Bluff, IL), 600-, 320- and 240-grit SiO2
abrasive papers (Carbimet Buehler-met, Buehler, Lake
Bluff, IL). These preparation methods were classified by
type and coarseness (0.05 mm alumina powder slurry -
lowest coarseness; burs: carbide , fine diamond , coarse
diamond; SiO2 papers: 600-grit , 320-grit , 240-grit).
Before surface preparation, all samples were polished
through 0.05 mm alumina powder slurry (Buehler Micro-
polish, Buehler, Lake Bluff, IL) to create a baseline surface
finish. All the surface preparations were performed with
water flow (25 ml/min).
The smear layers created by the burs were prepared in a
device developed in our laboratory that firmly holds the bur
in a high-speed hand piece while moving the sample with a
constant load of 150 g. This load was found to be the mean
pressure exerted by most clinicians at the tip of the bur. [31]
Each bur was used under constant water spray, to prepare a
maximum of 5 surfaces. Each sample prepared with paper
was abraded with one of the different grits, for 5 s with a
weight , 150 g, measured on a digital scale (Mettler PC-
2000- Mettler Instruments Corp, NJ). Since it was difficult
with the rougher abrasive papers to maintain constant
weight an effort was made to keep it between 100 and 300 g.
The adhesive and restorative materials used in this study
are listed in Table 1 along with the manufacturers
compositions, batch numbers and codes. All were used
following manufacturers directions.
Four outcome variables were analyzed in two phases. We
examined the distribution of each outcome prior to analysis;
all were analyzed on the natural scale. In phase A, we
analyzed the shear bond strength associated with different
surface preparation methods when bonded with Clearfil SE
bond (SE; Kuraray America, Inc. New York, NY) or Single
Bond Adhesive system (SB; 3M ESPE, St Paul, MN). We
then identified the best clinical abrasive (bur) when the SE is
used (i.e. that associated with the highest shear bond
strength), and compared the paper abrasives with this bur to
identify the best in vitro abrasive (paper). In phase B, we
characterized the surface preparation methods according to
the smear layers’ roughness, thickness, and reaction to
conditioners (Fig. 1). We theorized that the paper abra-
sive(s) with the shear bond strength closest to that of the best
bur also would be closest with respect to characteristics of
the smear layer, indirectly explaining the variation in shear
bond strength. Specifically, we hypothesized that shear bond
strength for the SE should be enhanced by a rough dentin
surface, a thin smear layer, and increased tubule openness
after application of the acidic primer.
2.1. Bond strength
Following smear layer preparation, each specimen was
mounted in a single-plane lap shear device as described by
Watanabe et al, 1996; 1999. [30,32] A Mylar mask with a 3-
mm diameter hole was placed on each prepared surface to
760 S.S.A. Oliveira et al. / Dental Materials 19 (2003) 758–767

Table 1
Restorative and adhesive materials

Material Code Composition Batch # Function

Single Bond Adhesive
system—3M St Paul, MN
Clearfil SE Bond—Kuraray
America, USA
Z-100—3M St Paul, MN
35% phosphoric
acid—Fisher Scientific, USA
SB 35% phosphoric acid Bisphenol A diglycidyl ether dimethacrylate, OEU Adhesive system
HEMA, dimethacrylate, solvent, water.
SE Primer- 10-MDP, HEMA, hydrophilic dimethacrylate, Primer-00101A Adhesive system
dl-Camphorquinone, N, N-diethanol-p-toluidine, water
Resin-10-MDP, Bis-GMA, HEMA, hydrophilic dimethacrylate, dl- Adhesive-00103A
Camphorquinone, N, N-diethanol-p-toluidine, Silanated colloidal silica.
Z100 Bisphenol A diglycidyl ether dimethacrylate; Silanated zirconium silica OKA Restorative material
synthetic mineral.
PA 35% phosphoric acid diluted from 85% phosphoric acid 933812 Acid conditioner

standardize the bonded area. One group, consisting of seven
different surface treatments (n ¼ 12 per treatment), was
tested with SE and an analogous group with SB. The
adhesive systems were applied following manufacturers’
instructions and the composite was applied in 1 mm
increments. The intensity of the curing light was monitored
periodically with a curing radiometer (acceptable range of
500 –600 mw/cm2) (Model 100, Demetron Research Cor-
poration, Danbury, CT, USA). Samples were stored for 24 h
at 37 8C and 100% humidity before testing. Shear bond
strength was evaluated at a crosshead speed of 5 mm/min,
using a universal testing machine (Instron model 1122,
Instron Corp., Canton, MA, USA).
For each conditioner, we obtained the mean (standard
deviation) shear bond strength by coarseness level (high,
medium, low, extra low) and abrasive type (bur or paper,
slurry), and used ANOVA and Tukey’s studentized range
test to compare the means as a function of these two factors.
The findings based on Tukey’s statistic were described via
letters identifying mean differences that were statistically
significant based on two-sided 0.05- level tests.
Failed samples were examined in the SEM at 25 £
magnification on the bonded surface, followed by 1000 –
2000 £ on the cross-section of the failed bonded area to
determine mode of failure.
layers formed by the different abrasives and to determine the
dependence of roughness on abrasive type and coarseness
level. Smear layer thickness and reaction to conditioners
were analyzed in the same manner as smear layer roughness.
(1) Smear layer roughness (Root Mean Square rough-
ness, Rq) was measured using an atomic force microscope
(AFM—Digital Instruments—Nanoscope III, Santa Bar-
bara, CA, USA). All measurements were made in water to
prevent sample dehydration. One 50 mm £ 50 mm image
was taken of each segment and the whole image was
measured for surface roughness, using the roughness
analysis option from the AFM software (Nanoscope III,
version 5.12r2. Digital Instruments. Santa Barbara, CA,
USA).
(2) Smear layer thickness was evaluated using a scanning
electron microscope (SEM; ISI ABT SX-40A wet SEM,
Topcon Instruments, Pleasanton, CA, USA). Immediately
after surface preparation and prior to segmentation, disks

2.2. Smear layer characteristics

After surface preparation, each dentin disk was cross-

fractured into 3 segments by applying a shearing force into
pre-cut grooves on the pulp side of the disk (Fig. 1).
Separate segments were evaluated for roughness (9
segments per treatment), thickness (6 segments per treat-
ment), and reaction to the conditioners (for each condi-
tioner, 9 segments per treatment), as described below.
Prior to analyzing the smear layer characteristics, we
used mixed-effects models to estimate the correlation
among segments within teeth (and among tubules within
segments). If the correlation was less than 0.10, we used
segments as the units of analysis; otherwise we conducted
the analysis at the disk level. We then used these models to
estimate and compare the mean roughness of the smear
Fig. 1. Sample preparation for smear layer classification. Different samples
were used for each classification method. The occlusal surface of each
dentin disk was prepared with the abrasive, and the samples were fractured
by applying a shearing force in pre-cut grooves on the pulp side. Smear
layer roughness was measured using software from the AFM in images
from the surface of the dentin segments. Smear layer thickness was
measured on the cross section of the dentin segments. Smear layer removal
was evaluated by SEM imaging of the sample surface following smear layer
preparation by each abrasive and conditioning with either the primer of
Clearfil SE Bond or a 35% aqueous phosphoric acid.
 S.S.A. Oliveira et al. / Dental Materials 19 (2003) 758–767 761

were treated for SEM analysis. They were fixed in 2.5% 3. Results
glutaraldehyde in a 0.1 M sodium cacodylate buffer
(pH ¼ 7.4) for 12 h at 4 8C, rinsed with 0.2 M sodium 3.1. Bond strength test
cacodylate for one hour in three different baths, and rinsed
for one minute with deionized water. The disks were then Overall, shear bond strength was greater when SE was
dehydrated in ascending grades of ethanol to 100%, used (35.5 ^ 8.8 MPa) than when SB was used
transferred to HMDS and allowed to air-dry for 10 min. (21.8 ^ 7.3 MPa; P , 0:001). In the SB group, when
[33] Finally the disks were segmented and sputter-coated specimens abraded with 0.05 mm alumina slurry were
with 200 nm gold/palladium in a sputtering system included in the model, shear bond strength varied by both
(Hummer VII, Anatech Ltd, Alexandria, VA). One coarseness level ðP ¼ 0:039Þ and abrasive type ðP ¼
SEM image at 5000 £ was taken of the cross-section of 0:029Þ; however, when these specimens were excluded,
each segment, and the smear layer thickness was measured shear bond strength did not vary with either factor (model,
at ten equally spaced points along the smear layer surface, P ¼ 0:53).
using image analysis software (Ultrascan 2.1.1, Soft In the SE group, the mean shear bond strength (standard
Imaging Software, Kevex Sigma, Noran Instruments, Inc., deviation) was 35.5 (8.8) MPa. When specimens abraded
Madison, WI). Each segment was tilted 208 in each direction with 0.05 mm alumina slurry were included in the model,
to ensure that the smear layer width was measured shear bond strength varied by both coarseness level ðP ¼
accurately. 0:053Þ and abrasive type ðP ¼ 0:043Þ: When these speci-
(3) Smear layers’ reactions to the conditioners were mens were excluded, the statistical significance of both
analyzed on the SEM micrographs of the segment factors increased (P ¼ 0:005 and P ¼ 0:003; respectively).
surfaces. After surface abrasion and prior to segmenta- Regardless of abrasive type, shear bond strength decreased
tion, each conditioner was applied to 3 disk surfaces with increasing coarseness of the abrasive (Table 2) and was
(Fig. 1). The primer from SE was applied for 20 s and significantly lower when the coarsest abrasives were used
then air-dried with a gentle stream of air, following the (coarse diamond bur or 240-grit paper), according to
manufacturer’s instructions. These disks were immedi- Tukey’s test. Among the bur abrasives, the carbide bur
ately placed in 100% ethanol for 5 min to dissolve the yielded higher bond strength than either the fine diamond
monomer of the SE primer, and then soaked in de- bur [by 2.1 (95% CI, 2 2.9 –7.1) MPa] or the coarse
ionized water for 5 min to reverse any dehydration from diamond bur [by 7.3 MPa (95% CI, 2.2– 12.4) MPa]. Thus it
the ethanol. A prior study showed that this procedure was selected as the standard against which the paper
removed the monomer and reversed the effect of the abrasives were then compared. Although no paper abrasive
ethanol dehydration. [34] Phosphoric acid liquid was differed significantly from the carbide bur ðP ¼ 0:15Þ; the
applied to 3 other disks for 15 s with a brush and rinsed 320-grit paper and the 240-grit paper yielded shear bond
with deionized water for 10 s. The 35% phosphoric acid strengths within 0.5 MPa of the shear bond strength of the
used for this procedure was prepared by diluting 85% carbide bur (Table 2). Thus they appeared to offer better
phosphoric acid (Fisher Scientific, USA) with de-ionized simulations of the clinical bur than the 600-grit paper.
water, since the conditioner from the SB contains a silica Examination of the surfaces fractured during the shear
thickener, which leaves a precipitate that interfered with bond strength test showed a common cohesive failure
the surface analysis. The same ethanol and de-ionized through the adhesive layer for all abrasives except for the
water treatments were applied to these disks as were coarsest when used in conjunction with SE. In the latter
used after the SE treatment. All 6 disks were then treated cases (coarse diamond bur and 240-grit paper), residual
for SEM evaluation (as described above) and segmented smear layer appeared to remain on the de-bonded surfaces
before sputtering.
One 5000 £ SEM micrograph was taken per segment. Table 2
The numbers of tubules that were open, partially open, Abrasive and adhesive influence on shear bond strength (MPa)
plugged with smear layer or closed, were determined by
visual evaluation of the SEM micrographs for each surface Abrasive Mean shear bond strength
(std. dev.)a
treatment. Tubules were considered closed when the
structure of the peritubular dentin was not visible, whereas Type Coarseness Clearfil SE Single bond
plugged tubules were clogged below the surface, with the
Alumina slurry 0.05 mm Extra low 35.1 (13.8)A,B 17.0 (6.6)A
tubule structure and peritubular dentin visible. The extent of
Abrasive paper 600-grit Low 42.0 (7.5)A 25.4 (6.8)A
openness was coded as follows: 100% ¼ completely open, Abrasive paper 320-grit Medium 36.6 (7.6)A,B 21.7 (6.6)A
66% ¼ partially open, 33% ¼ plugged, 0% ¼ fully closed. Abrasive paper 240-grit High 35.7 (8.7)A,B 22.4 (9.0)A
In order to perform a segment-level analysis, the mean Bur Carbide Low 36.2 (5.3)A,B 22.0 (6.8)A
openness per segment was calculated (on average, there Bur Fine diamond Medium 34.1 (5.8)A,B 20.4 (7.9)A
Bur Coarse diamond High 28.9 (7.0)B 23.6 (6.2)A
were 9 tubules per segment) and analyzed using mixed-
effects models, as described above. a
The outcomes are significantly different if the superscript letters differ.
762 S.S.A. Oliveira et al. / Dental Materials 19 (2003) 758–767

Fig. 2. Fractured surfaces from shear bond strength samples from the Clearfil SE bond group. (a) 25 £ magnification SEM micrograph of the 600-grit abrasive
paper subgroup sample shows almost all the surface covered with adhesive (x), which suggests a mainly cohesive failure within the adhesive layer. (b) SEM
micrographs (25 £ magnification) of the coarse diamond bur subgroup sample show some areas (z) where there is no adhesive and failure appears to have
occurred below it. From the similarity with the surface around the bonded area, we can see that striations are the same in the area that was conditioned and the
dentin surface around it. These areas (z) appear not to have been conditioned and look just like the smear layer around it. Therefore we would consider this
failure to be cohesive within the smear layer.

(Fig. 2). Although demarcation between the bonded and
unbonded areas was clear, it was apparent that the striations
and smear layer are continuous across the bonded and
unbonded areas.
3.2. Smear layer characteristics
We compared the smear layers created by three paper
abrasives with the carbide bur with respect to three
characteristics of the smear layer: roughness of the dentin
surface, thickness of the smear layer, and reaction to the
conditioner (by means of tubule openness).
Surface roughness. AFM measurements made of the
surface roughness (Rq) for disks abraded with a coarse
diamond bur exceeded 1000 nm, which was too large to
measure; hence no data were available for analysis. In disks
abraded with 0.05 mm alumina slurry, surface roughness
ranged from 16.8 –28.6 nm, whereas for other abrasives it
was 220 nm or higher (Table 3). Because the effect of
0.05 mm alumina slurry on surface roughness was very
different from the effects of other abrasives and this skewed
the overall distribution; these samples were excluded from
further analysis. The correlation among segments within
disks was low (0.05), enabling us to use segments as the
units of analysis of surface roughness (n ¼ 45 segments; 9
per abrasive).
Surface roughness varied strongly by coarseness level
(median (range): Low, 347 (220 – 618) nm; Medium, 769
(479 – 1232) nm; and High, 726 (541 – 1389) nm;
P , 0:001) but not by abrasive type (P ¼ 0:20). Of the
SiO2 papers, the 600-grit paper produced a surface rough-
ness most similar to that of the carbide bur (difference,
158 ^ 91 nm; the 320-grit paper differed by
280 ^ 113 nm).
Thickness of the smear layer. Smear layer thickness
measurements for each segment were made by SEM
analysis of the fractured segments (Fig. 1). Specimens
treated with 0.05 mm alumina slurry were not analyzed
because smear layers were too thin to measure. Since the
correlation among segments within a given tooth was low
(0.09) but the correlation among measurements per segment
was high (0.58), we averaged over the measurements within
each segment and used segments as the units of analysis of
smear layer thickness (n ¼ 36 segments; 9 per abrasive).

Table 3
Smear layer characteristics produced by different abrasives

Abrasive Smear layer characteristics [mean (std. dev.)]a

Type Coarseness Roughness (nm)a Thickness (mm) Smear layer reaction to the SE
primer.b (Tubule Openness; %)

Alumina slurry 0.05 mm Extra low 21.7 (3.3) N/A 66.0 (14.4)A
Abrasive paper 600-grit Low 267.7 (27.0)A 1.4 (0.2)A 48.8 (11.8)A,B
Abrasive paper 320-grit Medium 757.5 (80.3)B 2.0 (0.4)A,B 33.4 (17.2)C,B
Abrasive paper 240-grit High 821.2 (225.6)B 3.0 (0.7)C 16.4 (13.9)C
Bur Carbide Low 425.9 (94.6)A 1.8 (0.1)A,B 22.2 (17.8)C
Bur Fine diamond Medium 909.7 (92.2)B 2.0 (0.2)A,B 18.5 (13.0)C
Bur Coarse diamond High .1000 2.4 (1.1)C,B 15.5 (16.1)C
a
The outcomes are significantly different if the superscript letters differ. Abrasives without letters were excluded from the analysis.
b
The SB system had tubule openness of 100% for all abrasives.
 S.S.A. Oliveira et al. / Dental Materials 19 (2003) 758–767 763

As was true for surface roughness, the thickness of the
smear layer increased significantly with the coarseness of
the abrasive [median (range): Low, 1.6 (1.2 – 1.9) mm;
Medium, 2.0 (1.5 – 2.6) mm; and High, 2.8 (1.6 – 4.5) mm.
P , 0:001)] but did not differ significantly by abrasive type
(burs vs. papers; P ¼ 0:68). The thickness produced by the
carbide bur (1.76 ^ 0.13 mm; Table 3) was slightly more
than that of the 600-grit paper, by 0.36 ^ 0.17 mm, and
slightly less that of the 320-grit SiO 3 paper, by
0.22 ^ 0.32 mm.
Tubule openness. SEM micrographs of all smear layers
treated with 35% phosphoric acid showed the tubules 100%
opened so that further analysis with this conditioner was not
needed. Typical SEM micrographs for the effect of the SE
primer on smear layers created with various abrasives are
shown in Fig. 3. When tubule openness (varying from 0% to
100% open) was analyzed, low correlation among measure-
ments within segments (0.0006) would have enabled us to
use tubules as the units of analysis. However, we averaged
the data within segments to make these the units of analysis
(n ¼ 63 segments; 9 per abrasive), to approximate this
analysis with the others in sample size and power. Overall,
the mean tubule openness for SE was 33 ^ 36%; 10% were
completely open, 21% were partially open, 30% were
mostly closed, and 39% were fully closed. After reducing
the data to segment-specific means, the overall mean tubule
openness was 32 ^ 23%.
Tubule openness decreased with increasing coarseness
level and was lower among burs than among paper abrasives
(both, P , 0:001; Table 2 and Fig. 4). The tubule openness
of specimens abraded with a carbide bur (22 ^ 18%) did not
differ from those abraded with 240-grit or 320-grit paper,
but did differ from the level of 600-grit specimens (Table 3).
4. Discussion
The self-etching materials were introduced to the dental
market at a time when dentists desired easier and less
technique-sensitive adhesive materials. Although these
qualities can be very appealing to clinicians, care should
be taken to evaluate how these new materials interact with
the dentin surface. Since the current self-etching materials
have higher pH values than the acids used with total-etch
adhesive systems, and the self-etching materials are not
rinsed away, the smear layer or its components are
incorporated into the bonded layers.
With the methods used in this study we found that the
total-etch system (SB) completely removed the smear layer,
regardless of the abrasive used and that shear bond strength

Fig. 3. SEM micrographs of the reaction of the smear layer to the Clearfil SE primer treatment. (a) 600-grit smear layer; (b) 320-grit smear layer; (c) carbide bur
smear layer; (d) coarse diamond bur smear layer. Open tubules (O), partially opened tubules (PO), plugged tubules (P) and closed tubules (C), are indicated in
the images.
764 S.S.A. Oliveira et al. / Dental Materials 19 (2003) 758–767
Fig. 4. Reaction of the smear layers, by surface preparation method, to the primer of Clearfil SE Bond. Tubule openness decreased with increased coarseness
level and was lower among burs than paper abrasives (both, P , 0:001). The tubule openness was similar for specimens abraded with carbide bur, 240-grit or
320-grit paper.
for the SB system was not sensitive to the method used to
create the smear layer. This was not true for the SE system
and the results confirmed the hypothesis that the method
used to produce the smear layer affects the bond strength of
this system.
The evaluation of the smear layer modification by the
primer showed a significant inverse association between
coarseness level and the tubule openness (Figs. 3 and 4).
Thicker smear layers resulted in increased number of closed
tubules after SE treatment.
To determine if the rinsing step influenced the retention
of the smear layer on the dentin surface, an additional
experiment was performed (Fig. 5) where dentin samples
with a smear layer created by a 240-grit abrasive paper
(which gave the thickest smear layer; Table 3) were acid
etched with SE primer for 20 s (Fig. 5 – a) and air dried for
5 s. These were compared with those etched with different
concentrations of phosphoric acid [0.13%, pH ¼ 2 (same as
SE), Fig. 5b; 20%, pH ¼ 0.21, Fig. 5c; and 35%,
pH ¼ 2 0.28,Fig. 5d] for 15 s and rinsed with de-ionized
water for 10 s. The smear layer was successfully rinsed
away after being etched with the acid only when 35 %
phosphoric acid was used (Fig. 5d). This suggests that more
diluted acids were not strong enough to etch through the
whole thickness of the 240-grit smear layers and that even
after rinsing part of the smear layer was still attached to the
dentin surface. Pashley and Carvalho. [11] suggested that
the dentin smear layer interferes with the self-etching
primer adhesion. Our results support this suggestion.
Additionally, the decreased bond strength and increased
smear layer thickness with the coarseness of the abrasive
when the SE was used (Tables 2 and 3), and the presence of
smear layer on the de-bonded samples from the coarser
abrasives in the SE group (Fig. 2), further support this
hypothesis. Nonetheless, the shear bond strength results of
SE were, overall, significantly higher than those bonded
with SB. This was true despite the fact that SE was less
effective in completely removing the smear layer. This
challenges the general consensus that it is necessary to
remove the smear layer in order to achieve high bond
strengths. [9] Preliminary work in our lab evaluated the
hybrid layer for the self-etching primer and total etch system
studied in this work. We found that the hybrid layer had a
substantially higher modulus for the self-etching system and
this may offer a possible explanation for the higher bond
strengths found in this investigation. We hope a more
complete evaluation will confirm these findings in the near
future. On the other hand, it was reported [35] that the
phosphoric acid used in these concentrations causes the
denaturation of the top layer of collagen, which could
explain its lower bond strength.
When SE was used, the carbide bur gave the thinnest
smear layer of all the burs (Table 3), and it produced the
highest bond strength among the bur groups (Table 2).
This finding emphasizes the importance of using, clinically, a
bur that creates a thin smear layer when applying the current
SE materials as an adhesive system for bonded restorations.
In order to generate relevant data, laboratory testing
should be performed on surfaces that closely resemble those
created under clinical conditions. According to our results
on the smear layer characteristics, the carbide bur group
yielded smear layer thickness between those of 320- and
600-grit papers, and its roughness was closer to the 600-grit
paper. But when the adhesive system was used (shear bond
strength and reaction to the conditioner), the smear layer
created by the carbide bur gave results that were similar to
the 320-grit smear layer or were in between those of the
320- and 240-grit papers.
 S.S.A. Oliveira et al. / Dental Materials 19 (2003) 758–767 765

Fig. 5. 240-grit abrasive paper smear layer samples etched with (a)—Clearfil SE primer (SE), and different concentrations of phosphoric acid: (b)—0.13%
(pH ¼ 2; similar to SE primer), (c)—20% (pH ¼ 0.21), and (d)—35% (pH ¼ 20.28). Only in (d) the smear layer was successfully rinsed away after being etched
with the acid. These pictures represent the inability of an acid with higher pH to etch through the thick smear layer created by the 240-grit abrasive paper.

An explanation for this difference could rely on the explained by our observation that although the 35%
difference between the two abrasive methods. Using a bur phosphoric acid removes the whole smear layer, the striated
may produce a denser smear layer than that produced by topography created by the dentin surface preparation
abrasive papers, which may affect the primer’s ability to remained intact (Fig. 6). It is reasonable to assume that by
etch through the smear layer. We found that, on average, the
thickness of smear layer did not vary by abrasive type, but
burs tended to have more closed tubules than the papers.
Thus openness may be more closely related to denseness of
smear layer. The suggestion that burs may leave a thinner
but denser smear layer than the sandpaper was discussed by
Tao et al. [14] If the 320-grit abrasive paper creates a less
compact smear layer than the carbide bur, this might
compensate for its slightly higher thickness, so that both
react similarly to the self-etching primer, as seen in the
results from the shear bond strength and reaction to the
conditioners. Regardless, within the limitations of our study,
the 320-grit paper yielded reactions to the conditioners
(shear bond strength and openness of tubules) that were
similar to those produced by the carbide bur. Thus the 320-
grit abrasive paper would be the most clinically relevant
SiO2 paper of the three we studied.
Even though in a previous study there was a similar result,
[36] it is still perplexing that in the shear bond strength tests
the lowest values were found for the 0.05 mm alumina group Fig. 6. Fine diamond bur smear layer treated with 35% aqueous phosphoric
with either SB or SE, even though it presented the thinnest acid. Although the surface is clean of smear, the striations due to the
smear layer with the most open tubules. This might be preparation were still evident.
766 S.S.A. Oliveira et al. / Dental Materials 19 (2003) 758–767
increasing the surface area, the bond strength would be
higher, since it would increase the true area of the surface
bonded by the resin. [37] Thus the lower surface area
resulting from the 0.05 mm alumina slurry would probably
give lower bond strengths in the SB group. For the SE group
however, the smear layer thickness seems to play a major role
in the bond strength, as discussed above, so a balance
between roughness and thickness should be achieved in order
to produce higher bond strengths. Another, possible
explanation for the low bond strength of the 0.05 mm
alumina group is that by highly polishing with an alumina
powder slurry, we modify the surface in some way that
interferes with bonding. Finally it should be noted that the
polished surfaces are of theoretical interest but are not
relevant to clinical settings.
The finding that the self-etching primer did not totally
remove the smear layer or open all the tubules for the bur-
abraded samples may be important from the clinical
standpoint. As noted by Pashley, [38] the combination of
the smear layer and smear plugs reduce dentin permeability.
Removing this barrier would increase dentin permeability,
[12] producing an outward dentinal fluid movement from the
pulp, which could interfere with dentin adhesion [39] and
dilute the adhesive agents. [11] Also, since some resin
components are hypertonic, they can osmotically increase
dentinal fluid flow toward the dentin surface, resulting in a
displacement of the odontoblasts. [38] and post-operative
pain. Since the self-etching materials do not completely
remove the smear plugs, they may have the potential to
promote less post-operative sensitivity and be less disturbed
by moisture changes of the dentin substrate, [40] without
sacrificing shear bond strength.
Another concern is that the bacteria present in the smear
layer might be retained with it and affect the pulp. However,
if the restoration is well sealed, this may not be a concern
because it would prevent the bacteria from subsisting. Even
though high bond strength and low microleakage may not
always be correlated, high bond strengths are necessary to
overcome curing stresses and prevent the formation of gaps
between the restoration and tooth substrate. However, it is
possible that retaining part of the smear layer or its
components could affect the long-term bond strength by
degrading over time. In this study, the smear layer has been
shown to be important in the adhesion of self-etching
primers. Research on long-term effects is needed to more
fully understand its implications.
In conclusion, shear bond strength of the SB system was
not sensitive to the abrasive used except for the very smooth
surfaces produced by the 0.05 mm alumina slurry. In general
thick smear layers seemed to interfere with the adhesion
capabilities of the self-etching primer studied, although this
system still showed higher bond strengths than the etch-and-
rinse adhesive system. This suggests that self-etching
primers should be used in vivo with a surface preparation
method that creates a thin smear layer. In this study we
found that, compared with those produced by the two
diamond burs, the carbide bur yielded the highest shear
bond strength and the thinnest smear layer. Therefore,
surface preparation for in vitro tests of this SE system
should consider the use of an abrasive paper that creates a
smear layer with similar characteristics to the carbide bur,
which we believe to be the 320-grit SiO2 paper.
Acknowledgements
Sofia Oliveira is supported by a PhD fellowship from the
Portuguese Ministry for Science and Technology, Praxis
XXI program. This study was supported by NIH/NIDCR
Grant P0.1 DE09859.
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