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
Bauru School of Dentistry, University of São Paulo, Bauru,
São Paulo, Brazil
Statement of problem. Clinicians continue to search for ways to simplify bonding procedures without compromising clinical
efficacy.

Purpose. The purpose of this study was to evaluate the shear strength of self-adhesive cements RelyX U100 and RelyX U200,
and conventional resin cement RelyX ARC to enamel and dentin after different surface treatments.

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 delimited with central holed adhesive tape. The teeth
were distributed into 12 groups (n¼10) according to the substrate; etched or not with 37% phosphoric acid; and cement type
of enamel-U100, enamel-phosphoric acid-U100, enamel-U200, enamel-phosphoric acid-U200, enamel-ARC, enamel-
phosphoric acid-ARC, dentin-U100, dentin-phosphoric acid-U100, dentin-U200, dentin-phosphoric acid-U200, dentin-ARC,
and dentin-phosphoric acid-ARC. After 7 days of storage in artificial saliva, shear strength tests were performed by using a
universal testing machine (0.5 mm/min). The data were analyzed with 3-way ANOVA and the Tukey test (a¼.05). Fracture
analysis was performed with a light microscope. Two specimens from each group were analyzed with a scanning electron
microscope.

Results. In enamel, ARC (9.96 MPa) had higher shear strength (P¼.038) than U100 (5.14 MPa); however, after surface
etching, U100 (17.81 MPa) and U200 (17.52 MPa) had higher shear strength (P<.001). With dentin, no significant dif-
ferences were observed (P¼.999), except for dentin-ARC (0.34 MPa) (P¼.001). Most fractures were of the adhesive type.

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 cements are equally effective alternatives to
conventional resin cement. (J Prosthet Dent 2014;-:---)

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.

The clinical success of indirect restorations on the teeth.1-4 Dental ce- dental surface and seal tooth margins.
restorative procedures depends partly ments promote the required retention Resin cements are the most used ma-
on the cement used to bond indirect of indirect restorations to the remaining terials for the cementation of indirect

This study was supported by the Coordination for the Improvement of Higher Education Personnel and the National Council for
Scientific and Technological Development.
a
Graduate student, Department of Dentistry, Endodontic and Dental Materials.
b
Graduate student, Department of Dentistry, Endodontic and Dental Materials.
c
Associate Professor, Department of Dentistry, Endodontic and Dental Materials.
d
Professor, Department of Dentistry, Endodontic and Dental Materials.

Rodrigues et al
2 Volume - Issue -

restorations.5,6 Self-adhesive resin cements
can provide a single-step cementation
technique2,7-10 because the dental sub-
strate does not need to be etched or
have an adhesive applied.1,2,11-14 Self-
adhesive resin cements eliminate the
chemical incompatibility observed when
simplified adhesive systems are used
with chemical or dual-polymerized resin
cements.15 Furthermore, self-adhesives
tolerate moisture and fluoride release,
and do not trigger postoperative sen-
sitivity.1,16,17 The combination of tech-
nical simplification and lower patient
sensitivity provided by self-adhesive resin
cements has attracted considerable in-
terest from manufacturers and clini-
cians.2,18-20
The demineralization pattern for
both enamel and dentin, however, is
different from that of resin cements that
require acid etching. In enamel, the
demineralization pattern is based on
multifunctional monomers with phos-
phoric acid groups simultaneously
demineralizing and infiltrating the
enamel.1,21-24 By contrast, a porous
surface, which can be infiltrated by re-
sin, must be acid etched to enable a
strong micromechanical bond.25 In
dentin, self-adhesive cements produce a
superficial interface without demineraliz-
ing 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
substrate.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
hydroxyapatite; this interaction provides
micromechanical retention.1,20,23
Detailed information about the
composition and adhesive 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 ce-
ments produce a lower bond strength in
enamel and in dentin than conventional
resin cement, even though manufac-
turers’ instructions indicate no acid
etching.5,11,18,21,30-35
Although self-adhesive cements pro-
vide 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 self-adhesive resin ce-
ments to bovine enamel and 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 man-
ufacturer of the materials are listed in
Table I. 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 sec-
tion the roots from the crowns with
a cutting machine (Isomet 1000TM;
Buehler). Each crown was embedded in
polyvinyl chloride (PVC) cylinders (15.0
mm in height and 25.0 mm in diam-
eter) with epoxy resin (MX-6921;

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

Material Composition Batch No. Manufacturer

RelyX U100 Base paste: fiberglass, phosphoric acid esters methacrylate, triethylene 459579 3M ESPE
glycol dimethacrylate, 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, 481248 3M ESPE
2-methyl 1,10 -(1-[hydroxymetil]-1,2-ethanodlyl) 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, N331951 3M ESPE

zirconia silica, pigments, amines and 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 Adhesive Bismethacrylate (1-methylethylidene) bis (4,1-phenylenoxy N251381 3M ESPE

[2-hydroxy-3,1-propanediyl]) and 2-hydroxyethyl methacrylate

The Journal of Prosthetic Dentistry Rodrigues et al

- 2014 3
thereafter. The ground dentin surfaces
SUBSTRATE CEMENTS SURFACE GROUPS
TREATMENT
were observed under a stereomicro-
scope (Plus AM-313T; Dino-Lite) at
..... 25 magnification to verify complete
E-U100
enamel removal.
RelyX U100
Phosphoric acid (P) E-P-U100 All the crowns were cleaned with
pumice (Pumice; Maquira) and water.
..... E-U200 To standardize the bonding area of all
Enamel (E) RelyX U200 the specimens, a central holed adhesive
Phosphoric acid (P) E-P-U200 tape, 3.0 mm in diameter was placed
on the surface of the enamel and the
Adhesive E-ARC dentin. Before cementing, the crowns
RelyX ARC received surface treatment in the
Phosphoric acid (P) + bonding areas, according to the
E-P-ARC
adhesive
substrate, group, and manufacturer’s
instructions (Fig. 1). The enamel-ARC
..... D-U100 and dentin-ARC groups were con-
RelyX U100 sidered negative controls, whereas
Phosphoric acid (P) D-P-U100
the enamel-phosphoric acid-ARC and
the dentin-phosphoric acid-ARC were
..... D-U200 positive controls.
Dentin (D) RelyX U200
Phosphoric acid (P) D-P-U200 The crowns were secured in a metal
device (Fig. 2) for the cement applica-
tion and were mounted inside a split
Primer + Adhesive D-ARC
polytetrafluoroethene mold (Teflon;
RelyX ARC
Phosphoric acid (P) + Dupont) mold (Fig. 2) with a central
D-P-ARC
primer + adhesive orifice (3.0 mm in diameter and 2.0
1 Experimental groups according to substrate, cement, and surface treatment. mm in height). The cements were
inserted into the Teflon mold, and
standardized pressure was applied by
Basis for coupling Teflon mold using the largest Gilmore needle (454
g). Photoactivation was performed
Teflon mold
with a light emitting diode (Optilight
Screw to secure the Teflon mold LD Max; Gnatus) with a power density
PVC + tooth of 500 mW/cm2, which was verified
before use with a radiometer. The time
Cement for cement mixing, photoactivation,
3.0 mm
and setting was according to the man-
ufacturers’ instructions. For the U100,
the mixture time was 20 seconds plus
Screw to secure the PVC 20 seconds of photactivation and 5
2.0 mm
PVC + tooth minutes of setting. For the U200, the
mixture time was 20 seconds plus 20
Metallic device Teflon mold Specimen seconds of photactivation and 6 mi-
2 Schematic representation of metal device to clamp nutes of setting. For the ARC, the
polyvinyl chloride (PVC) cylinder plus tooth and Teflon mold mixture time was 10 seconds plus 40
to cementation; Teflon mold with central orifice (diameter, seconds of photactivation and 10 mi-
3.0 mm; height, 2.0 mm) and specimen after cementation. nutes of setting. The cement and ad-
hesive tape excesses were removed with
Redelease). The buccal surfaces of the grit silicon carbide paper (Sandpaper; a scalpel blade.
crowns were ground in a water-cooled Extec) were used; each grit was used for The specimens (Fig. 2) were stored
mechanical grinder and polisher (ER- 5 minutes. To expose the dentin, 120- for 7 days at 37 C in artificial saliva
27000; Erios) at a speed of 300 rpm to grit abrasive paper was used until with an electrolyte composition similar
expose the flat enamel or dentin. To initial exposure, and 320-grit and 600- to that of human saliva. The artificial
expose the enamel, 320-grit and 600- grit abrasive papers were used saliva consisted of a 0.02 M Tris buffer,
Rodrigues et al
4 Volume - Issue -

e e
results of the 3-way ANOVA of SBS
18 17.81 17.52 Enamel data are listed in Table II. Results of
Dentin statistical analysis indicated that the
Shear Bond Strength (MPa)

16
type of substrate, type of resin cement,
14 and phosphoric acid etching affected
12 the bond strength values (P<.001). A
e
9.96 significant substrate and treatment in-
10 teraction occurred (P<.001), and the
a,c a,c
8 7.34 phosphoric acid etching increased the
a,b a,b,c a,b,c 6.74
5.47 a,b,d a,b,d SBS values, except for the U100
6 5.14 5.29 4.62 4.85 (P¼.998) and the U200 (P>.05) ce-
4 b,d ments in dentin. In enamel, the
2 1.64 d self-adhesive cements had similar
0.34 SBS values when compared with each
0
other (P>.05). When comparing
0

00

00

00

RC

RC
0

10

10

20

20
AR

AR

enamel-U100 (5.14 1.15 MPa),

U1

U1

U2

U2

-A

-A
-U

-U

-U

-U
E-

P-

-P
E-

P-

E-

P-

-P

-P
E-

enamel-U200 (5.29 1.20 MPa), and

D
E-

E-

D
Group
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 II. Three-way ANOVA (P<.05)
Source of Sum of
Variation df Squares
S 1 653.007
C 1 358.420
T 2 1451.509
S3C 2 118.153
S3T 1 509.356
C3T 2 10.165
S3C3T 2 179.932
S, substrate; C, cement; T, treatment.
pH 7.0, which contained 1.5 mM cal-
cium nitrate, 0.9 mM dibasic sodium
phosphate dehydrate, 0.15 M potas-
sium 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 mi-
croscope (Plus AM-313T; Dino-Lite).
Fractures were classified as adhesive,
The Journal of Prosthetic Dentistry
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
(P¼.052), but the U100 had lower SBS
Mean values compared with ARC (P¼.038).
Squares F P When phosphoric acid etching was
applied to the enamel before placement
653.007 66.180 <.001 of the self-adhesive resin cements
179.210 18.162 <.001 (enamel-phosphoric acid-U100: 17.81
4.08 MPa and enamel-phosphoric
1451.509 147.105 <.001
acid -U200: 17.52 7.37 MPa) higher
59.077 5.987 .003
SBS values were observed for the con-
509.356 51.621 <.001 ventional resin cement (enamel-phos-
5.083 0.515 .060 phoric acid-ARC: 9.96 3.79 MPa)
89.966 9.118 <.001 (P<.001).
No difference (P>.05) was observed
in dentin between RelyX U100, RelyX
U200, and RelyX ARC, with or without
cohesive in enamel, cohesive in dentin, phosphoric acid etching before the
cohesive in cement, or mixed. Two application of the cements, except for
specimens from each group were the dentin-ARC negative control group
selected for scanning electron micro- (0.34 0.48 MPa) (P¼.001). The ma-
scope (SEM) analysis in a scanning jority of fractures (68.3%) produced
electron microscope (JSM-T220A; Jeol) during the SBS tests were of the adhe-
with 1000 magnification. The speci- sive mode (Fig. 4). Results of the
mens were attached to metal stubs, SEM analysis indicates minimal micro-
vacuum dried, and sputter coated with mechanical retention between the
gold (Desk IY; Denton Vacuum). The self-adhesive cements and enamel
data were analyzed with 3-way ANOVA (Figs. 5A, B, and 6A, B). As indicated in
followed by the post hoc Tukey test Figure 7A (enamel-phosphoric acid-
(a¼.05). ARC), micromechanical retention is
more evident between the conventional
RESULTS resin cement and enamel in relation
to Figures 5A, B, and Figures 6A, B. The
The median SBS values of the tested photomicrographs of dentinal surfaces
resin cements are listed in Figure 3. The show structures that are suggestive of a
Rodrigues et al
- 2014 5

100% hydroxyapatite to form a stable bond

between the methacrylate network and
90% the tooth.21-24 Sodium, calcium, fluo-
ride, and silicate ions that are released
80%
by alkaline particles neutralize the
70% remaining acid groups,1,22 and the
presence of calcium hydroxide seems to
60% accelerate the neutralization.22 Both
Fractures

self-adhesive cements tested in this

50%
study have calcium hydroxide in their
40% composition.
Although not recommended by the
30% manufacturer, phosphoric acid etching
improved the SBS values (P<.001) of
20% self-adhesive resin cements in enamel.
10%
The findings can be explained by
the increased microscopic irregularities
0% produced by the use of 37% phosphoric
00

00

00

00

RC

RC

S
acid21 and the pressure used. However,

UP
10

10

20

20
AR

AR
U1

U1

U2

U2

-A

-A
-U

-U

-U

-U

O
E-

P-

according to Goracci et al,32 the pressure

D

-P
E-

P-

E-

P-

GR
D

-P

-P
E-

D
E-

E-

L
contributes to a reduction in the thick-

Mixed
Cohesive in enamel
4 Fracture modes of tested cements.
smear layer combined with cements,
which partially covered the dentin sur-
face, and indicated micromechanical
retention between the cement and
dentin (Figs. 5C and 6C). More me-
chanical interaction (smear layer com-
bined 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 tu-
bules, similar to what is observed with
conventional resin cement.
DISCUSSION
This study investigated the SBS val-
ues of self-adhesive (U100 and U200)
and conventional (ARC) resin cements
to bovine enamel and dentin with
and without prior phosphoric acid
etching. The SBS results found that the
null hypotheses of the study were rejec-
ted because significant differences in
bond strength values were observed
between U100 and ARC in enamel,
and phosphoric acid etching improved
Rodrigues et al
AL
Group
Cohesive in cement Cohesive in dentin
Adhesive
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 conven-
tional resin cements present higher
bond strength to enamel compared with
self-adhesive resin cements5,21,30,33,35
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 (P¼.038). 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) (P¼.052),
perhaps because of the additional
monomer, new rheology, and optimi-
zation of the filler particle process-
ing according to the manufacturer.
Furthermore, self-adhesive cements in-
itially have a low pH,11 and the acid
groups connect with calcium
ness and porosity of the cement, and
improves adaptation to the 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 ce-
ments33 after phosphoric acid etching.
Results of the SEM analysis indi-
cated more micromechanical 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) (P¼.001). However,
there is literature that indicates that
results are variable and dependent on
the cement used compared with con-
ventional resin cements.6,7,22,31
In contrast, no improvement in SBS
values (P>.05) was observed when
phosphoric acid etching was used on
6 Volume - Issue -

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 micro-
mechanical 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.

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 de-
creases the bond strength of the self-
adhesive resin cement (RelyX Unicem;
3M ESPE) because of its high viscosity,
which prevents penetration on the
collagen matrix and leads to the for-
mation of a weak union between the
cement and tooth surface. Conversely,
Barcellos et al14 found that pre-
treatment of dentin with phosphoric
acid and adhesive increased the
bond strength of 2 self-adhesive resin
cements (Bifix [Voco]) (RelyX Unicem
[3M ESPE]).
Results of the SEM analysis in-
dicates improved micromechanical re-
tention of dentin substrates with resin
in the groups that received surface
The Journal of Prosthetic Dentistry
treatment (dentin-phosphoric acid-
U100, dentin-phosphoric acid-U200,
and the dentin-phosphoric acid-ARC);
however, similar SBS values were ob-
served among all dentin groups. Most
of the observed fractures were of the
adhesive type, similar to what was re-
ported 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
superficial and highly irregular, without
demineralization of the smear layer and
formation of a real hybrid layer, and
possibly without resin tags.21,24 There-
fore, this formation is likely an irregular
layer of interaction between the cement
and the substrate. However, the in-
dications from the photoelectron
spectroscopy radiograph analysis of the
relevant chemical interaction with cal-
cium hydroxyapatite indicate that this
approach provides micromechanical re-
tention, even without infiltration of
more than 1 mm in the surface of the
dentin.20
The adhesion mechanisms are de-
pendent on the micromechanical reten-
tion 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 mecha-
nism 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,
Rodrigues et al
- 2014 7

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.

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.

which demineralizes and infiltrates the adhesive cements provide satisfactory However, long-term clinical studies are
tooth surface and provides micro- results regarding the bond strength in needed to confirm self-adhesives
mechanical retention.23,30 Usually, self- enamel and dentin in in vitro studies. cement effectiveness.
Rodrigues et al
8 Volume
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 adhesive 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
E-mail: afborges@fob.usp.br
Copyright ª 2014 by the Editorial Council for
The Journal of Prosthetic Dentistry.
Rodrigues et al