Ó
Operative Dentistry, 2011, 36-5, 512-520
Effect of Dentin-cleaning
Techniques on the Shear
Bond Strength of Selfadhesive Resin Luting
Cement to Dentin
MJMC Santos H Bapoo AS Rizkalla
GC Santos Jr
Clinical Relevance
This in vitro study showed that sandblasting dentin with aluminum oxide is the most
effective method to enhance bonding of an indirect restoration to the tooth surface when a
self-adhesive resin luting cement is used.
SUMMARY
Objective: This in vitro study evaluated the
influence of different cleansing techniques on
the bond strength of self-adhesive cement to
dentin.
*Maria Jacinta MC Santos, DDS, MSc, PhD, Restorative
Dentistry, The University of Western Ontario, Schulich
School of Medicine & Dentistry, London, Ontario, Canada
Hussein Bapoo, undergraduate student, The University of
Western Ontario, Schulich School of Medicine & Dentistry,
London, Ontario, Canada
Amin S. Rizkalla, PhD, Biomaterials Science, The University
of Western Ontario, Schulich School of Medicine & Dentistry,
London, Ontario, Canada
Gildo Coelho Santos Jr, DDS, MSc, PhD, Restorative
Dentistry, The University of Western Ontario, Schulich
School of Medicine & Dentistry, London, Ontario, Canada
*Corresponding author: Schulich School of Medicine &
Dentistry, DSB Room 0149, London, Ontario N6A 5C1
Canada; e-mail: jacinta.santos@schulich.uwo.ca
DOI: 10.2341/10-392-L
Methods and Materials: A total of 33 noncarious human molars were sectioned mesiodistally and embedded in chemically cured resin
with the buccal or lingual surfaces facing
upward. Superficial dentin was exposed and
resin disk provisional restorations were cemented to the dentin surfaces with noneugenol
provisional cement and were stored in distilled water at 378C. After seven days, the
provisional restorations were removed and 13
specimens were randomly assigned to each of
the five groups (n¼13), according to the following cleansing treatments: G1—excavator (control); G2—0.12% chlorhexidine digluconate;
G3—40% polyacrylic acid; G4—mixture of flour
pumice and water; and G5—sandblasting with
50 lm aluminum oxide particles at a pressure
of 87 psi. Resin composite disks (Filtek Supreme Plus, 3M ESPE Dental Products, St
Paul, MN, USA) 4.7 (60.1) mm in diameter and
3.0 (60.5) mm in height were cemented with
self-adhesive cement (RelyX Unicem, 3M
Santos & Others: Effect of Dentin-Cleaning Techniques on Bond Strength to Dentin
ESPE), photocured, and stored in distilled
water at 378C for 24 hours. Shear bond strength
testing was conducted using a universal test
machine at a crosshead speed of 0.5 mm/min
until failure.
Results: Data were analyzed using analysis of
variance (ANOVA) and the Tukey-B rank order
test. Sandblasting with aluminum oxide (11.32
6 1.70 MPa) produced significantly higher
shear bond strength values compared with
any other treatment groups (p,0.05). No significant differences were found between G1control (7.74 6 1.72 MPa), G2-chlorhexidine
(6.37 6 1.47 MPa), and G4-pumice (7.33 6 2.85
MPa) (p,0.05).
INTRODUCTION
The performance and longevity of indirect restorations can be affected by several factors, such as
preparation design/coarseness, provisional luting
agent, cleansing protocol, fit of the definitive restoration, and type of the definitive luting agent.1,2 The
main objective of restorative procedures is to obtain
an adaptation as close as possible between the
restorative material and the tooth structure to avoid
the presence of gaps and consequent microleakage.3
Resin-based dental luting cements can infiltrate into
the dentinal tubules and exposed collagen network
to promote a micromechanical interlock.4,5 Also,
because of the tooth-colored appearance, minimal
solubility, biocompatibility, and strengthening effects to the remaining dental structure provided by
resin luting materials, their use has been increasing
over the past decade.6
Despite the positive aspects of resin luting cements, the main disadvantage of the adhesive
cementation technique is the number of steps
involved in the luting protocol. For longer than 20
years, conventional resin cements have been used in
conjunction with dentin bonding agents; this has
resulted in a multistep application technique that is
considered time-consuming and technique-sensitive.7 Also, the discrepancy between the depth of
acid etching and resin infiltration can lead to
postoperative sensitivity and hydrolytic degradation
because of the large area of collagen fibrils exposed
but not encapsulated by the bonding resin.8 A resin
cement that combines pretreatment of dental tissues
and resin infiltration in a single application would be
advantageous because it may overcome some of the
limitations associated with a multistep technique.3
The introduction of self-adhesive resin cements was
a major advance in dental adhesive cementation
513
early in the decade, because they do not require
additional steps of etching, priming, or bonding;
instead, their application is accomplished through a
single clinical step, which allows the clinician to use
a cementation protocol very similar to that used with
conventional zinc-phosphate and polycarboxylate
cements. Self-adhesive cements are based on multifunctional phosphoric acid methacrylates, which
demineralize and infiltrate the tooth structure,
resulting in micromechanical retention.6
Regardless of the luting protocol of resin cements,
the bonding technique can be adversely affected by
the presence of remnants of provisional restorative
materials. Removal of provisional cement debris is
desirable to promote contact between the dentin and
the adhesive system, which will result in higher
bond strengths.1,2,9,10 Some studies have shown that
mechanical removal of provisional cement by excavators is not adequate in that cement remnants can
still be observed microscopically on dentin surfaces
that appear to be macroscopically clean.10,11
Furthermore, the presence of a smear layer is a
factor that can compromise the clinical bonding
effectiveness of a final restoration.12 For self-adhesive cements, no pretreatment is recommended to
remove the smear layer. However, several studies
have proposed the use of different agents to enhance
the interaction between resin cement and dental
tissues, thereby increasing the bond strength.4,13,14
The related literature reports a great number of
cleaning agents for the dentinal surface, some of
which are based on mechanical methods; others use
chemical agents. The most common techniques for
mechanical cleansing include the use of rotary
instrumentation with pumice and sandblasting with
aluminum oxide particles; chemical cleansing techniques include the use of chlorhexidine digluconate,
sodium hypochlorite, hydrogen peroxide, and polyacrylic acid. Application of different cleaning treatments to the dentin surface has shown different
results on the smear layer and on the removal of
provisional cement. Their effects range from simple
removal of contaminants such as blood and debris to
total or partial removal of the smear layer, promoting demineralization that can facilitate interaction
between the resin and the collagen network on the
dentin surface.2,3,6
Although some studies have reported that selfadhesive cements promote adequate bond strength
to dentin,4,13,15 others have verified lower bond
strength values when compared with conventional
resin cements.5,16,17 These studies have observed
that self-adhesive cements might interact superfi-
Operative Dentistry
514
cially with dentin, leading to partial demineralization of the smear layer, which would result in a weak
bonding mechanism.18 Because bond strength is
considered a relevant factor in the longevity of
indirect restorations, this study aims to verify the
influence of different cleansing techniques on bond
strength values of self-adhesive cement. It was
hypothesized that shear bond strength values would
differ significantly among the different cleansing
techniques.
MATERIALS AND METHODS
Tooth Preparation
Thirty-three freshly extracted human molars free of
cracks, caries, or restorations were selected for this
study. After they were cleaned for calculus deposits
and soft tissues, teeth were stored in 0.1% thymol
solution for a maximum of 6 months until use. Before
bonding experiments were begun, the teeth were
retrieved from the disinfectant solution and were
stored in distilled water, with daily changes of the
latter for two weeks to remove the disinfectant.
Approval to use human teeth was obtained from the
Research Ethics Committee at the University of
Western Ontario.
The teeth were sectioned mesiodistally at the
central groove and the roots removed using a slowspeed saw (Isomet, Buehler Ltd, Lake Bluff, IL,
USA) under water cooling. Sectioned teeth were
embedded in chemically cured acrylic resin (Dentsply Caulk Orthodontic Resin, Milford, DE, USA) in
cylindrical rings, with the buccal or lingual surface
facing upward. Each tooth had its proximal enamel
and superficial dentin removed with the use of a
series of SiC-papers on a polisher (Polimet, Buehler
Ltd, Lake Bluff, IL, USA), under water cooling,
ending with 600 grit to obtain a flat dentin surface
1.5 to 2.0 mm from the pulp.
Provisional Composite Specimen Preparation
Sixty-five disk specimens were prepared by loading a
composite temporization material (Protemp Plus, 3M
ESPE Dental Products, St Paul, MN, USA) into
translucent polyethylene cylindrical molds with an
inner diameter of 3 mm and a height of 4 mm to
fabricate the provisional restorations. These restorations were cemented to the center of dentin
surfaces with non–eugenol-containing provisional
cement (Temp Bond NE, Kerr Corp, Orange, CA,
USA) and were held in place with a 500 g load for one
minute. Teeth with provisional restorations were
stored in distilled water at 378C for seven days, after
which time the provisional restorations and the
cement were mechanically removed with a carving
instrument until the dentin surface appeared macroscopically clean.
Resin-Based Composite (RBC) Specimen
Preparation
A visible light–activated RBC (Filtek Supreme Plus,
3M ESPE), shade A3, was used to prepare disk
specimens by loading the composite resin into a
translucent polyethylene cylindrical mold with an
inner diameter of 3 mm and a height of 4 mm. The
RBC was placed in the mold in increments of about 2
mm. Each layer was individually light-cured for 40
seconds (Dentsply QHL75, with 600 mW/cm2 output). Polymerization was completed in an oven
(Dentacolor XS, Kulzer, Irvine, CA) at 1208C for
seven minutes. RBC surfaces were sandblasted with
50 lm Al2O3 for 10 seconds, using an intraoral air
abrasion device at a pressure of 87 psi (Optiblast,
Buffalo Dental Mfg Inc, New York, NY, USA). All
specimens were cleaned with 35% phosphoric acid
gel for 5 seconds (Scotchbond Etchand, 3M ESPE)
and were washed and dried.
Group Classification and Bonding Procedure
Specimens were randomly assigned to five groups of
13 specimens each, according to the cleansing
protocols listed in Table 1. The materials employed
are summarized in Table 2. The self-adhesive resin
luting cement (Rely-X Unicem Clicker, 3M ESPE)
was mixed for 20 seconds, according to the manufacturer’s instructions; it was then applied over the
restoration and placed in the center of the tooth
surface. The cement was initially light-cured for 10
seconds (Dentsply QHL75, with a 600 mW/cm2
output) to allow removal of cement excess at the
dentin restoration margin; then light-curing was
performed at the lateral surfaces of the bonded RBC
(20 seconds on each of the four surfaces, totaling 90
seconds of light activation). During the cementation
procedure, a load of 500 g was used over the indirect
restoration to standardize the pressure during
cementation. Before shear bond strength measurement, the specimens were stored at 378C in distilled
water for 24 hours.
Shear Bond Strength Test
Each specimen was mounted in a Bencor Multi-T
device to keep it stable and parallel to the base when
positioned in a universal testing machine (Instron,
Model 5585H, Instron Corp, Canton, MA, USA), and
loading was applied with a flattened rod at a
Santos & Others: Effect of Dentin-Cleaning Techniques on Bond Strength to Dentin
Table 1:
515
Experimental Groups With Cleansing Treatments
Dentin-Cleansing Technique
Group
Treatment
G1
Hand instrument (control)
Excavator was used for 10 seconds; dentin was rinsed and excess water removed
with absorbent papera
G2
0.12% chlorhexidine digluconate
Scrubbed over dentin for 10 seconds using a disposable applicator and gently
dried with absorbent papera
G3
40% polyacrylic acid
Scrubbed over dentin for 10 seconds using an applicator. Then rinsed off for 10
seconds and excess water removed with absorbent papera
G4
Pumice flour þ water
Pumice slurry was used with a prophy cup in a slow-speed rotary instrument for 10
seconds and rinsed for 10 seconds; excess water was removed with absorbent
papera
G5
Aluminum oxide, 50 lm Al2O3
Dentin was sandblasted for 10 seconds at 87 psi at a distance of 2 cm. Then
rinsed for 10 seconds and excess water removed with absorbent papera
a
To avoid dehydration of the dentin.
crosshead speed of 0.5 mm/min. Each specimen was
tightened and stabilized to ensure that the edge of
the shearing rod was positioned as close to the
restoration-tooth interface as possible. Shear bond
strength in megapascals (MPa) was calculated from
the maximum stress at failure divided by the
specimen surface area. Means and standard devia-
Table 2:
tions were recorded for each group tested. One-way
analysis of variance (ANOVA) was performed to
assess the significance of differences in interfacial
strength among the five treatments. Post hoc
multiple comparisons were achieved using the Tukey
test. P-values lower than 0.05 were considered to be
statistically significant in all tests.
Product Names, Batch Numbers, and Manufacturers
Material
Product Name
Batch No.
Manufacturer
Provisional cement
Rely X Temp NE
355430
3M/ESPE, St Paul, MN, USA
Provisional restorative
material
Protemp Plus
348072
3M/ESPE, St Paul, MN, USA
Luting cement
Rely X Unicem, Self-Adhesive
Universal Cement
356321
3M/ESPE, St Paul, MN, USA
Restorative material
Filtek Supreme Plus
8RB
3M/ESPE, St Paul, MN, USA
Dentin-cleansing agents
Chlorhexidine digluconate
Consepsis Scrub, Ultradent, South Jordan,
Utah, USA
Durelon (polyacrylic acid)
358558
3M/ESPE, St Paul, MN, USA
Pumice flour
M01771
Quadra Chemicals Ltd, Vaudreuil-Dorion, QC, CA
Aluminum oxide
Opiblast, Buffalo Dental Mfg Inc, New York, NY, USA
Operative Dentistry
516
Table 3:
Group
Mean of Bond Strength Values (MPa) of Different Dentin Surface Treatments
Dentin-Cleansing
Technique
No. of
Specimens
Mean Shear Bond Strength,
MPa* (mean 6 SD)**
G1
Hand instrument (control)
13
7.74 6 1.72ab
G2
0.12% chlorhexidine digluconate
13
6.37 6 1.47a
G3
40% polyacrylic acid
13
9.14 6 2.11b
G4
Pumice flour þ water
13
7.33 6 2.85ab
G5
Aluminum oxide, 50 lm Al2O3
13
11.3 6 1.70c
* Mean MPa with the same letters indicate groups that were not statistically different (p.0.05).
** Data analysis was done using ANOVA and the Tukey-B rank order test.
RESULTS
Mean shear bond strengths and standard deviations
for each treatment group are presented in Table 3
and Figure 1. Data analysis with ANOVA revealed
that specimens sandblasted with aluminum oxide
produced the highest mean shear bond strength
values (11.3 6 1.70), and those cleaned with 0.12%
chlorhexidine digluconate resulted in the lowest
shear bond strength values (6.37 6 1.47). The mean
shear bond strength of the aluminum oxide group
was significantly higher than that of any other
treatment group (p,0.05). Results also showed that
the mean shear bond strength of specimens cleaned
with chlorhexidine digluconate was significantly
lower than those of the polyacrylic acid and aluminum oxide groups (p,0.05). When all dentin-cleaning agents were compared, no significant differences
were found between the control (excavator), chlorhexidine digluconate, and pumice groups (p.0.05),
or between the chlorhexidine, pumice, and polyacrylic acid groups (p.0.05).
nient method of accessing the bond strength of luting
materials.20
It was hypothesized that different dentin-cleansing techniques would yield statistically significant
differences in shear bond strength values of a selfadhesive resin cement to dentin. Results of this
DISCUSSION
The use of dentin-cleaning techniques to avoid any
contaminants along the dentin-cement interface to
improve the bond strength of self-adhesive luting
systems to the dentin surface seems to be a desirable
procedure. In the present study, chemical and
mechanical cleansing protocols were tested using
shear forces, because shear stress tends to provide a
better representation of the forces capable of displacing crowns in the oral environment when
compared with tensile stress.19 Furthermore, the
shear bond test is considered a reliable and conve-
Figure 1. SEM micrograph of dentin surface after cleansing
treatment: G1—excavator (control).
Santos & Others: Effect of Dentin-Cleaning Techniques on Bond Strength to Dentin
517
Figure 2. SEM micrograph of dentin surface after cleansing
treatment: G2—0.12% chlorhexidine digluconate.
Figure 3. SEM micrograph of dentin surface after cleansing
treatment: G3—40% polyacrylic acid.
study partially support the hypothesis, in that a
significant difference in shear bond strength was
observed between group 5 (aluminum oxide) and all
other groups. The use of aluminum oxide particles
significantly improved the bond strength of a selfadhesive cement to dentin (p,0.05). Particle abrasion using aluminum oxide particles is a dentin
cleansing technique that has only recently regained
attention in operative dentistry. It is a relatively old
technique that is widely used by prosthodontists and
dental technicians to increase surface roughness and
enhance adhesion.10 Specimens abraded with aluminum oxide showed the highest shear bond strength
values compared with any other cleansing technique. This result is consistent with a previous
study21 showing significantly higher bond strength
when aluminum oxide particles were used for dentin
surface treatment before indirect restorations were
cemented with a self-adhesive resin luting cement,
compared with pumice and hand instruments. In
their study, tooth surfaces were treated with 50 and
27 lm aluminum oxide particles. Investigators
observed that although the smaller particles promoted a more retentive pattern, particle size did not
significantly influence bond strength. In the present
study, 50 lm aluminum oxide particles were used
and presented significantly higher bond strength
compared with all other groups. Representative
areas of the dentin surfaces treated with different
cleaning procedures are shown in Figures 1-5.
The high shear bond strength observed in this
group can be attributed to the fact that particle
abrasion using aluminum oxide creates rough,
irregular surfaces that increase the bonding surface
area, as visualized on scanning electron micrographs. This, in turn, has been reported to increase
the bond strength of restorations to both enamel and
dentin.22 It is important to mention that the use of
rubber dam isolation and of a high-volume evacuation system is recommended, to avoid inhalation of
alumina particles during clinical procedures.
In contrast to aluminum oxide, dentin treatment
with slurry of pumice resulted in significantly lower
shear bond strengths and no significant differences
compared with other tested groups. The use of
pumice flour to remove plaque and/or surface debris
is a well-known procedure that has been used in
dentistry for many years. It has been used as an
abrasive or polishing agent to clean teeth and
518
Operative Dentistry
Figure 4. SEM micrograph of dentin surface after cleansing
treatment: G4—pumice slurry.
Figure 5. SEM micrograph of dentin surface after cleansing
treatment: G5—sandblasting with alumina oxide 50 lm.
remove plaque and debris from the area to be
bonded. Investigators have attained variable results
regarding the use of pumice to improve bond
strength. Some support the use of pumice for
cleaning provisional cement3,23 on dentin; others
have reported otherwise.20,24 The latter study
showed that pumice is not effective as a dentincleansing agent, as indicated by the low shear bond
strength values achieved. A previous study similarly
observed that use of pumice on a flat tooth surface
produces a surface covered by pumice residues
condensed by the rubber cup, which negatively
interferes with adhesion.25 Sealed dentinal tubule
openings can prevent the impregnation of resin and
can reduce effective bonding.
dentin surface, thereby yielding low shear bond
strength values for pumice as compared with
aluminum oxide.
In another study, Saraç and others6 observed by
SEM that when a rotary instrument was used to
apply cleaning agents to dentin, dentinal tubules
were plugged with provisional cement by the force of
rotation, reducing the surface area for micromechanical interlocking. In the present study, pumice slurry
was applied using a prophy cup in a rotary
instrument. The rotary instrument could have
smeared the remnants of provisional cement on the
Chlorhexidine is a chemical agent that has been
indicated for tooth surface cleaning because of its
antibacterial action, and also because of its effect as
a matrix metalloproteinase (MMP) inhibitor.26 Recently, chlorhexidine has been shown to provide
structural integrity to hybrid layers through its
inhibitory effect on endogenous collagenolytic activity in dentin, preventing collagen degradation and
disintegration of the bonding interface over time.27
However, besides the potential advantages of using
this substance for dentin pretreatment, previous
studies have reported conflicting results, such as
reduced bond strength, with its use6,28; others
observed no difference in bonding strength values.29,30
In the present study, no statistically significant
differences were found between the control (excavator), chlorhexidine digluconate, and pumice groups
(p.0.05). The similarity in effects of chlorhexidine
digluconate and a hand instrument on dentin
cleaning has been documented in other studies.
Santos & Others: Effect of Dentin-Cleaning Techniques on Bond Strength to Dentin
Grasso and others2 reported no statistical difference
when 0.12% chlorhexidine digluconate, an explorer,
and air-water spray were used to remove provisional
cement from the dentin surface. In another study by
Saraç and others,6 no significant difference was
observed between shear bond strengths of specimens
cleaned with a hand instrument and a cavity
cleanser (2% chlorhexidine digluconate).
The low shear bond strength values obtained with
the use of chlorhexidine solution indicate that this
cleaning agent is not effective when used to clean
provisional cement off dentin before self-adhesive
cement is applied. This finding is in agreement with
data from a recent study31 demonstrating that the
use of chlorhexidine solution reduced the bond
strength of self-etch resin cement systems, because
this substance is not effective in removing the smear
layer. Also, because of its affinity for phosphate
groups (cationic properties), the bonding of chlorhexidine to these loose apatite remnants within the
smear layer could have interfered with the functions
of acidic monomers of self-adhesive resin cements. In
the same study, no detrimental effect on bonding
efficacy was observed when chlorhexidine was
applied to acid-etched dentin, followed by application
of total-etch adhesive systems.
According to the information available on selfadhesive cement, the presence of water, phosphoric
acid, and methacrylate monomer will demineralize
the smear layer and the underlying dentin, while
simultaneously infiltrating the porous dentin surface, as a result of its hydrophilic properties and the
neutralization of acid that occurs as polymerization
progresses21; however, insufficient demineralization
and limited resin infiltration have been observed.5,14,18,31 In the present study, 40% polyacrylic
acid was used to verify whether this weak acid would
provide further demineralization to enhance bonding. The beneficial effect of polyacrylic acid on bond
strength to dentin lies in the removal of the smear
layer and the shallow demineralization of the tooth
tissue.32 Although results of this study show that the
polyacrylic acid group was superior to the chlorhexidine digluconate group, the use of polyacrylic acid
did not improve shear bond strength compared with
the control group. This finding is consistent with
data from other studies.3,14
Although polyacrylic acid increases surface roughness and exposes dentinal tubules, limited diffusion
of the viscus-filled self-adhesive resin cement was
observed in a recent study.14 A previous study3
reported that when 40% polyacrylic acid (Durelon
liquid) was used to clean a normal dentin surface,
519
dentinal tubule openings were clearly visible and the
smear layer of dentin was significantly reduced.
However, in that study, it was shown that when this
acid was used to clean provisional cement, the effect
was significantly decreased. The explanation relies
on the presence of a provisional cement layer that
reduces the action of Durelon liquid. This finding
also helps to clarify the poor effects of polyacrylic
acid on bond strength, as observed in the present
study. In addition, the absence of a low-viscosity
agent to facilitate diffusion into the demineralized
dentin may contribute to the lower bond strength.14
This in vitro study used a predetermined protocol
with each cleaning agent; this was a limitation of the
study. Several factors can alter the effectiveness of
dentin-cleaning agents used in this study. Some of
these include time of application, application protocol, and concentration of solutions. Varying previously mentioned conditions can alter the
performance of these cleaning agents. This is an
area that needs further research to specify the
conditions under which each dentin-cleaning agent
will have an optimal effect on the provisional cement
and the smear layer. Results may more closely
reflect the reality of clinical practice.
CONCLUSIONS
Within the limitations of this in vitro study, the
highest mean shear bond strength values of a selfadhesive resin luting cement were achieved when
dentin was sandblasted with aluminum oxide.
On the contrary, the use of chlorhexidine digluconate as a dentin-cleaning agent resulted in the
lowest shear bond strength values with no significant difference from the control group (excavator).
Acknowledgement
The authors gratefully acknowledge the support of the
manufacturers through the donation of materials.
(Accepted 21 February 2011)
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