RESEARCH AND EDUCATION

The shear bond strength of self-adhesive resin cements to

dentin and enamel: An in vitro study
Raphaela F. Rodrigues, MSc, PhD,a Carla M. Ramos, MSc, PhD,b Paulo A. S. Francisconi, DDS, MSc, PhD,c and
Ana Flávia. S. Borges, DDS, MSc, PhDd

The clinical success of indirect ABSTRACT

restorative procedures depends Statement of problem. Clinicians continue to search for ways to simplify bonding procedures
partly on the cement used to without compromising clinical efficacy.
bond indirect restorations on
Purpose. The purpose of this study was to evaluate the shear strength of self-adhesive cements
the teeth.1-4 Dental cements
RelyX U100 and RelyX U200, and conventional resin cement RelyX ARC to enamel and dentin
promote the required retention after different surface treatments.
of indirect restorations to the
remaining dental surface and Material and methods. The crowns of 120 bovine incisor teeth were separated from the roots and
embedded in epoxy resin in polyvinyl chloride tubes. In each tooth, the area to be cemented was
seal tooth margins. Resin ce-
delimited with central holed adhesive tape. The teeth were distributed into 12 groups (n=10)
ments are the most used according to the substrate; etched or not with 37% phosphoric acid; and cement type of enamel-
materials for the cementation U100, enamel-phosphoric acid-U100, enamel-U200, enamel-phosphoric acid-U200, enamel-ARC,
of indirect restorations.5,6 Self- enamel-phosphoric acid-ARC, dentin-U100, dentin-phosphoric acid-U100, dentin-U200, dentin-
adhesive resin cements can phosphoric acid-U200, dentin-ARC, and dentin-phosphoric acid-ARC. After 7 days of storage in
provide a single-step cemen- artificial saliva, shear strength tests were performed by using a universal testing machine (0.5
tation technique2,7-10 because mm/min). The data were analyzed with 3-way ANOVA and the Tukey test (a=.05). Fracture
analysis was performed with a light microscope. Two specimens from each group were analyzed
the dental substrate does not
with a scanning electron microscope.
need to be etched or have
an adhesive applied. 1,2,11-14 Results. In enamel, ARC (9.96 MPa) had higher shear strength (P=.038) than U100 (5.14 MPa);
however, after surface etching, U100 (17.81 MPa) and U200 (17.52 MPa) had higher shear strength
Self-adhesive resin cements
(P<.001). With dentin, no significant differences were observed (P=.999), except for dentin-ARC (0.34
eliminate the chemical in- MPa) (P=.001). Most fractures were of the adhesive type.
compatibility observed when
simplified adhesive systems Conclusions. U200 self-adhesive cement had similar bond strength to the ARC in enamel, but the
combination with phosphoric acid had the best bond strength. For dentin, self-adhesive resin
are used with chemical or dual-
15 cements are equally effective alternatives to conventional resin cement. (J Prosthet Dent
polymerized resin cements. 2015;113:220-227)
Furthermore, self-adhesives
tolerate moisture and fluoride
release, and do not trigger postoperative sensitivity.1,16,17 The demineralization pattern for both enamel and
The combination of technical simplification and lower dentin, however, is different from that of resin cements
patient sensitivity provided by self-adhesive resin ce- that require acid etching. In enamel, the demineralization
ments has attracted considerable interest from manu- pattern is based on multifunctional monomers with
facturers and clinicians.2,18-20 phosphoric acid groups simultaneously demineralizing

This study was supported by the Coordination for the Improvement of Higher Education Personnel (CAPES) and the National Council for Scientific and
Technological Development (CNPq).
a
Graduate student, Department of Dentistry, Endodontic and Dental Materials, Bauru School of Dentistry, University of São Paulo, Bauru, São Paulo, Brazil.
b
Graduate student, Department of Dentistry, Endodontic and Dental Materials, Bauru School of Dentistry, University of São Paulo, Bauru, São Paulo, Brazil.
c
Associate Professor, Department of Dentistry, Endodontic and Dental Materials, Bauru School of Dentistry, University of São Paulo, Bauru, São Paulo, Brazil.
d
Professor, Department of Dentistry, Endodontic and Dental Materials, Bauru School of Dentistry, University of São Paulo, Bauru, São Paulo, Brazil.

220 THE JOURNAL OF PROSTHETIC DENTISTRY

March 2015 221

self-adhesive resin cements to bovine enamel and

Clinical Implications
The dental profession has been searching to
simplify bonding procedures without compromising
clinical efficacy, and self-adhesive resin cements can
be a practical alternative to conventional resin
cements in tooth restoration procedures.
and infiltrating the enamel.1,21-24 By contrast, a porous
surface, which can be infiltrated by resin, must be acid
etched to enable a strong micromechanical bond.25
In dentin, self-adhesive cements produce a superficial
interface without demineralizing the smear layer or
forming a hybrid layer.21,24 Even total etching determines
other patterns of demineralization and dissolution of
minerals, which allows micromechanical interlocking
and/or entrapment of the resin with the tissue sub-
strate.26-29 In spite of the superficial interface, a chemical
interaction seems to occur between the monomers
of self-adhesive resin cements and the calcium hy-
droxyapatite; this interaction provides micromechanical
retention.1,20,23
Detailed information about the composition and ad-
hesive properties of self-adhesive cements is still limited.
Different results have been reported for the bond
strength of self-adhesive and conventional resin cements
in enamel and dentin, with or without prior etching
of the tooth surfaces. Most reports indicate that self-
adhesive cements produce a lower bond strength in
enamel and in dentin than conventional resin cement,
even though manufacturers’ instructions indicate no acid
etching.5,11,18,21,30-35
Although self-adhesive cements provide reasonable
adhesion to dentin,3,35,36 its adhesion in enamel is still a
concern.22 However, the adhesion effectiveness of newly
launched and improved self-adhesive cements has not
been fully investigated in either enamel or dentin.
This in vitro study aims to evaluate the bond strength of
dentin, with and without phosphoric acid etching. The
null hypotheses tested were that the resin cements
would not exhibit different bond strengths in enamel
and dentin or with and without prior phosphoric acid
etching.
MATERIAL AND METHODS
The composition, batch, and manufacturer of the mate-
rials are listed in Table 1. One hundred and twenty
bovine incisor teeth were selected, cleaned, and stored in
0.1% thymol supersaturated solution at 4
C before
preparation. The first step was to section the roots from
the crowns with a cutting machine (Isomet 1000TM;
Buehler). Each crown was embedded in polyvinyl chlo-
ride (PVC) cylinders (15.0 mm in height and 25.0 mm in
diameter) with epoxy resin (MX-6921; Redelease). The
buccal surfaces of the crowns were ground in a water-
cooled mechanical grinder and polisher (ER-27000;
Erios) at a speed of 300 rpm to expose the flat enamel or
dentin. To expose the enamel, 320-grit and 600-grit
silicon carbide paper (Sandpaper; Extec) were used;
each grit was used for 5 minutes. To expose the dentin,
120-grit abrasive paper was used until initial exposure,
and 320-grit and 600-grit abrasive papers were used
thereafter. The ground dentin surfaces were observed
under a stereomicroscope (Plus AM-313T; Dino-Lite)
at ×25 magnification to verify complete enamel removal.
All the crowns were cleaned with pumice (Pumice;
Maquira) and water. To standardize the bonding area of
all the specimens, a central holed adhesive tape, 3.0 mm
in diameter was placed on the surface of the enamel and
the dentin. Before cementing, the crowns received sur-
face treatment in the bonding areas, according to the
substrate, group, and manufacturer’s instructions (Fig. 1).
The enamel-ARC and dentin-ARC groups were consid-
ered negative controls, whereas the enamel-phosphoric
acid-ARC and the dentin-phosphoric acid-ARC were
positive controls.

Table 1. Composition, batch number, and manufacturer of materials used

Material Composition Batch No. Manufacturer
RelyX U100 Base paste: fiberglass, phosphoric acid esters methacrylate, triethylene glycol dimethacrylate, 459579 3M ESPE
silica treated silane, and sodium persulfate; catalyst paste: fiberglass, substitute dimethacrylate,
silane treated silica, p-toluenesulfonate sodium, and calcium hydroxide
RelyX U200 Base paste: glass powder treated with silane, 2-propenoic acid, 2-methyl 1,10 -(1-[hydroxymetil]-1,2-ethanodlyl) 481248 3M ESPE
ester dimethacrylate, triethylene glycol dimethacrylate (TEGDMA), silica treated silane, glass fiber, sodium
persulfate and per-3,5,5-trimethyl hexanoate t-butyl; catalyst paste: glass powder treated with silane,
substitute dimethacrylate, silica-treated silane, sodium p-toluenesulfonate, 1-benzyl-5-phenyl-acid barium,
calcium, 1,12-dodecane dimethacrylate, calcium hydroxide, and titanium dioxide
RelyX ARC Paste A: bisphenol-A-glycidyl dimethacrylate (BisGMA), TEGDMA, zirconia silica, pigments, amines and N331951 3M ESPE
photoinitiator system; paste B: BisGMA, TEGDMA, zirconia silica, benzoyl peroxide
Phosphoric acid Phosphoric acid 37%, colloidal silica, surfactant, and colorant 525532D Dentsply Intl
Adper Scotchbond Primer 2-hydroxyethyl-methacrylate and polyalkenoic acid N239896 3M ESPE
Adper Scotchbond Bismethacrylate (1-methylethylidene) bis (4,1-phenylenoxy [2-hydroxy-3,1-propanediyl]) and N251381 3M ESPE
Adhesive 2-hydroxyethyl methacrylate

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222 Volume 113 Issue 3

SUBSTRATE CEMENTS SURFACE GROUPS

TREATMENT

..... E-U100
RelyX U100
Phosphoric acid (P) E-P-U100

..... E-U200
Enamel (E) RelyX U200
Phosphoric acid (P) E-P-U200

Adhesive E-ARC
RelyX ARC
Phosphoric acid (P) +
E-P-ARC
adhesive

..... D-U100
RelyX U100
Phosphoric acid (P) D-P-U100

..... D-U200
Dentin (D) RelyX U200
Phosphoric acid (P) D-P-U200

Primer + Adhesive D-ARC

RelyX ARC
Phosphoric acid (P) +
D-P-ARC
primer + adhesive

Figure 1. Experimental groups according to substrate, cement, and surface treatment.

The crowns were secured in a metal device (Fig. 2) Basis for coupling Teflon mold
for the cement application and were mounted inside a
split polytetrafluoroethene mold (Teflon; Dupont) mold Teflon mold
(Fig. 2) with a central orifice (3.0 mm in diameter and Screw to secure the Teflon mold
2.0 mm in height). The cements were inserted into the
PVC + tooth
Teflon mold, and standardized pressure was applied by
using the largest Gilmore needle (454 g). Photoactivation Cement
was performed with a light emitting diode (Optilight LD 3.0 mm
Max; Gnatus) with a power density of 500 mW/cm2,
which was verified before use with a radiometer. The time
for cement mixing, photoactivation, and setting was ac-
Screw to secure the PVC 2.0 mm
cording to the manufacturers’ instructions. For the U100, PVC + tooth
the mixture time was 20 seconds plus 20 seconds of
photactivation and 5 minutes of setting. For the U200, the Metallic device Teflon mold Specimen
mixture time was 20 seconds plus 20 seconds of pho-
tactivation and 6 minutes of setting. For the ARC, the Figure 2. Schematic representation of metal device to clamp polyvinyl
mixture time was 10 seconds plus 40 seconds of pho- chloride (PVC) cylinder plus tooth and Teflon mold to cementation;
tactivation and 10 minutes of setting. The cement and Teflon mold with central orifice (diameter, 3.0 mm; height, 2.0 mm)
adhesive tape excesses were removed with a scalpel blade. and specimen after cementation.
The specimens (Fig. 2) were stored for 7 days at 37
C in
artificial saliva with an electrolyte composition similar to

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March 2015 223

e e
17.81 17.52
18 Enamel
Dentin
16

Shear Bond Strength (MPa)

14

12 e
9.96
10
a,c
8 a,c
7.34
a,b a,b,c a,b,c 6.74
a,b,d a,b,d
6 5.14 5.29 5.47
4.62 4.85
4 b,d
2 1.64 d
0.34
0
00

00

00

00

00

00

00

C
10

AR

AR

AR

AR
U1

U2

U2

U1

U1

U2

U2
U

P-
E-

D-

P-
E-

P-

E-

P-

D-

P-

D-

P-
E-

D-
E-

E-

D-

D-
Group
Figure 3. Mean of shear bond strength values (MPa) of different resin cements for enamel and dentin, with and without acid etching; means with
different letters are significantly different (P<.05).

Table 2. Three-way ANOVA (P<.05)

Source of
Variation df Sum of Squares
S 1 653.007
C 1 358.420
T 2 1451.509
S×C 2 118.153
S×T 1 509.356
C×T 2 10.165
S×C×T 2 179.932
S, substrate; C, cement; T, treatment.
that of human saliva. The artificial saliva consisted of a 0.02
M Tris buffer, pH 7.0, which contained 1.5 mM calcium
nitrate, 0.9 mM dibasic sodium phosphate dehydrate, 0.15
M potassium chloride, and 0.05 ppm sodium fluoride.
Shear bond strength (SBS) tests were performed in
a universal testing machine (0.5 mm/min) (Emic DL 500
DF; LTDA) with a cell load of 50 kg. The shear load was
applied through a steel wire around the cement cylinder
and the tooth surface. The SBS values were recorded in
newtons (N) and converted into megapascals (MPa).
Fracture analysis was performed on all specimens with a
portable digital microscope (Plus AM-313T; Dino-Lite).
Fractures were classified as adhesive, cohesive in enamel,
cohesive in dentin, cohesive in cement, or mixed. Two
specimens from each group were selected for scanning
electron microscope (SEM) analysis in a scanning elec-
tron microscope (JSM-T220A; Jeol) with ×1000 magnifi-
cation. The specimens were attached to metal stubs,
vacuum dried, and sputter coated with gold (Desk IY;
Denton Vacuum). The data were analyzed with 3-way
ANOVA followed by the post hoc Tukey test (a=.05).
RESULTS
Mean Squares F P
The median SBS values of the tested resin cements are
653.007 66.180 <.001
179.210 18.162 <.001
listed in Figure 3. The results of the 3-way ANOVA of
1451.509 147.105 <.001
SBS data are listed in Table 2. Results of statistical
59.077 5.987 .003 analysis indicated that the type of substrate, type of resin
509.356 51.621 <.001 cement, and phosphoric acid etching affected the bond
5.083 0.515 .060 strength values (P<.001). A significant substrate and
89.966 9.118 <.001 treatment interaction occurred (P<.001), and the phos-
phoric acid etching increased the SBS values, except for
the U100 (P=.998) and the U200 (P>.05) cements in
dentin. In enamel, the self-adhesive cements had similar
SBS values when compared with each other (P>.05).
When comparing enamel-U100 (5.14 ±1.15 MPa),
enamel-U200 (5.29 ±1.20 MPa), and enamel-phosphoric
acid-ARC (9.96 ±3.79 MPa), all the groups were used
as recommended by the manufacturers, and similar
SBS values (mean ±SD) were observed between ARC
and U200 (P=.052), but the U100 had lower SBS values
compared with ARC (P=.038). When phosphoric acid
etching was applied to the enamel before placement
of the self-adhesive resin cements (enamel-phosphoric
acid-U100: 17.81 ±4.08 MPa and enamel-phosphoric
acid -U200: 17.52 ±7.37 MPa) higher SBS values were
observed for the conventional resin cement (enamel-
phosphoric acid-ARC: 9.96 ±3.79 MPa) (P<.001).
No difference (P>.05) was observed in dentin be-
tween RelyX U100, RelyX U200, and RelyX ARC, with or
without phosphoric acid etching before the application of
the cements, except for the dentin-ARC negative control
group (0.34 ±0.48 MPa) (P=.001). The majority of frac-
tures (68.3%) produced during the SBS tests were of
the adhesive mode (Fig. 4). Results of the SEM analysis

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224 Volume 113 Issue 3

100%

90%

80%

70%

Fractures
60%

50%

40%

30%

20%

10%

0%

C
E- 00
00

E- 00
00

E- C

D- 00

D- 0
D- 00

00

D- C
L G ARC

S
UP
0
AR
AR

AR
U1

U1

U2

U2

U1

U1

U2

U2

RO
E-

P-

D-

P -
E-

P-

E-

P-

D-

P-

P-

AL
Group

Mixed Cohesive in cement Cohesive in dentin

Cohesive in enamel Adhesive

Figure 4. Fracture modes of tested cements.

indicates minimal micromechanical retention between
the self-adhesive cements and enamel (Figs. 5A, B, and
6A, B). As indicated in Figure 7A (enamel-phosphoric
acid-ARC), micromechanical retention is more evident
between the conventional resin cement and enamel
in relation to Figures 5A, B, and Figures 6A, B. The
photomicrographs of dentinal surfaces show structures
that are suggestive of a smear layer combined with ce-
ments, which partially covered the dentin surface, and
indicated micromechanical retention between the cement
and dentin (Figs. 5C and 6C). More mechanical interac-
tion (smear layer combined with cements) between the
cement and dentin are shown in Figures 5D, 6D, and 7B,
which suggests that the self-adhesive cement deminer-
alized and penetrated the dentinal tubules, similar to
what is observed with conventional resin cement.
DISCUSSION
This study investigated the SBS values of self-adhesive
(U100 and U200) and conventional (ARC) resin ce-
ments to bovine enamel and dentin with and without
prior phosphoric acid etching. The SBS results found
that the null hypotheses of the study were rejected
because significant differences in bond strength values
were observed between U100 and ARC in enamel,
and phosphoric acid etching improved the SBS values
between enamel-phosphoric acid-U100 and enamel-
phosphoric acid-U200 in enamel. The bond strength
values observed for the enamel were similar between
the self-adhesive cements (RelyX U100 and RelyX U200)
(P>.05). The same trend reported in the literature that
conventional resin cements present higher bond strength
to enamel compared with self-adhesive resin ce-
ments5,21,30,33,35 was found between ARC (enamel-
phosphoric acid-ARC, 9.96 ±3.79 MPa, positive control
group) and U100 (enamel-U100, 5.14 ±1.15 MPa) ce-
ments (P=.038). However, RelyX U200 (enamel-U200:
5.29 ±1.20 MPa) had similar bond strength results to
those of RelyX ARC (enamel- phosphoric acid-ARC, 9.96
±3.79 MPa) (P=.052), perhaps because of the additional
monomer, new rheology, and optimization of the filler
particle processing according to the manufacturer.
Furthermore, self-adhesive cements initially have a low
pH,11 and the acid groups connect with calcium hy-
droxyapatite to form a stable bond between the meth-
acrylate network and the tooth.21-24 Sodium, calcium,
fluoride, and silicate ions that are released by alkaline
particles neutralize the remaining acid groups,1,22 and the
presence of calcium hydroxide seems to accelerate the
neutralization.22 Both self-adhesive cements tested in
this study have calcium hydroxide in their composition.
Although not recommended by the manufacturer,
phosphoric acid etching improved the SBS values (P<.001)
of self-adhesive resin cements in enamel. The findings can
be explained by the increased microscopic irregularities
produced by the use of 37% phosphoric acid21 and the
pressure used. However, according to Goracci et al,32 the
pressure contributes to a reduction in the thickness and
porosity of the cement, and improves adaptation to the

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March 2015 225

Figure 5. Scanning electron microscope image (×1000 magnification) of specimens with U100 self-adhesive resin cement in enamel and dentin after shear
bond strength test. A, Group enamel-U100; note that micromechanical retention is not evident. B, Group enamel-phosphoric acid-U100; note that, in spite
of prior acid etching, it is not possible to see micromechanical retention. C, Group dentin-U100, mechanical interaction between cement and dentin was
not observed. D, Group dentin-phosphoric acid-U100; note that acid etching increased micromechanical retention between cement and dentinal tubules.

cavity walls21 but does not influence the bond strength to
the enamel.32 Similar results also were reported by Duarte
et al,5 and other investigators observed bond strength in
self-adhesive cements similar to that of conventional resin
cements33 after phosphoric acid etching.
Results of the SEM analysis indicated more micro-
mechanical retention between the enamel and cement
in the enamel-phosphoric acid-ARC group than in the
other enamel groups. These findings are contradictory,
because they show increased bond strength in the
enamel-phosphoric acid-U100 and enamel-phosphoric
acid-U200 groups when compared with the enamel-
phosphoric acid-ARC group. In dentin, the self-adhesive
cements show similar bond strength to conventional
resin cement in the dentin (P>.05), which corroborates the
results from several studies,6,21,30,32,33,35,36 except for the
dentin-ARC negative control group (0.34 ±0.48 MPa)
(P=.001). However, there is literature that indicates that
results are variable and dependent on the cement used
compared with conventional resin cements.6,7,22,31
In contrast, no improvement in SBS values (P>.05)
was observed when phosphoric acid etching was used on
the dentin surface, and these results do not corroborate
the findings of De Munck et al21 and Hikita et al,33 who
claimed that prior conditioning decreases the bond
strength of the self-adhesive resin cement (RelyX Uni-
cem; 3M ESPE) because of its high viscosity, which
prevents penetration on the collagen matrix and leads to
the formation of a weak union between the cement and
tooth surface. Conversely, Barcellos et al14 found that
pretreatment of dentin with phosphoric acid and adhe-
sive increased the bond strength of 2 self-adhesive resin
cements (Bifix [Voco]) (RelyX Unicem [3M ESPE]).
Results of the SEM analysis indicates improved
micromechanical retention of dentin substrates with resin
in the groups that received surface treatment (dentin-
phosphoric acid-U100, dentin-phosphoric acid-U200, and
the dentin-phosphoric acid-ARC); however, similar SBS
values were observed among all dentin groups. Most of
the observed fractures were of the adhesive type, similar to
what was reported in other studies33,34 and thus indicate
valid values for the SBS results obtained.
Results of some studies indicate that the interface
between the tooth surface and self-adhesive cements is

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226 Volume 113 Issue 3

Figure 6. Scanning electron microscope image (×1000 magnification) of specimens with U200 self-adhesive resin cement in enamel and dentin after
shear bond strength test. A, Group enamel-U200; note that micromechanical retention is not evident. B, Group enamel-phosphoric acid-U200; note
that, in spite of prior acid etching, it was not possible to see micromechanical retention. C, Group dentin-U200, mechanical interaction between cement
and dentin was not observed. D, Group dentin-phosphoric acid-U200; note that acid etching increased micromechanical retention between cement
and dentinal tubules.

Figure 7. Scanning electron microscope image (×1000 magnification) of specimens with ARC conventional resin cement in enamel and dentin after
shear bond strength test. A, Group enamel-phosphoric acid-ARC; note that micromechanical retention was evident between enamel and cement. B,
Group dentin-phosphoric acid-ARC; note micromechanical retention between cement and dentinal tubules.

superficial and highly irregular, without demineralization formation is likely an irregular layer of interaction be-
of the smear layer and formation of a real hybrid layer, tween the cement and the substrate. However, the in-
and possibly without resin tags.21,24 Therefore, this dications from the photoelectron spectroscopy

THE JOURNAL OF PROSTHETIC DENTISTRY Rodrigues et al

March 2015
radiograph analysis of the relevant chemical interaction
with calcium hydroxyapatite indicate that this approach
provides micromechanical retention, even without infil-
tration of more than 1 mm in the surface of the dentin.20
The adhesion mechanisms are dependent on the
micromechanical retention and chemical interaction
between the monomer and the hydroxyapatite acidic
groups.1,23 Some cements form weak micromechanical
interactions and weak chemical bonds with the calcium
in teeth, depending on the type of acid monomer and
neutralization mechanism used.11 In line with several
studies, the self-adhesive cementing ability of RelyX
Unicem relies on the action of the phosphoric acid
methacrylate, also present in RelyX U100 and RelyX
U200, which demineralizes and infiltrates the tooth
surface and provides micromechanical retention.23,30
Usually, self-adhesive cements provide satisfactory re-
sults regarding the bond strength in enamel and dentin
in in vitro studies. However, long-term clinical studies are
needed to confirm self-adhesives cement effectiveness.
CONCLUSIONS
The U200 self-adhesive cement had similar bond
strength to the ARC in the enamel, but the combination
with phosphoric acid had the best bond strength. In
dentin, self-adhesive and conventional resin cements
had similar bond strength values, so both cements can be
used with the same adhesion effectiveness. In relation to
the failure mode, most of the failures were with the ad-
hesive mode for all groups, except for the enamel-
phosphoric acid-U200 group (mixed mode).
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Corresponding author:
Dr Ana Flávia Sanches Borges
Al. Octávio Pinheiro Brisola, 9-75
Bauru-SP 17012-901
BRAZIL
Email: afborges@fob.usp.br
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