journal of dentistry 37 (2009) 454–461

available at www.sciencedirect.com

journal homepage: www.intl.elsevierhealth.com/journals/jden

Bonding potential of self-adhesive luting agents used at

different temperatures to lute composite onlays

Amerigo Cantoro, Cecilia Goracci *, Carlos Augusto Carvalho,

Ivanovic Coniglio, Marco Ferrari
Department of Dental Materials and Fixed Prosthodontics, University of Siena, Policlinico ‘Le Scotte’, viale Bracci, Siena 53100, Italy

article info abstract

Article history: Objectives: To assess whether the bonding potential to dentin of self-adhesive resin cements
Received 25 September 2008 was affected by their pre-cure temperature.
Received in revised form Methods: Composite overlays (Paradigm MZ100, 3M ESPE) were luted on 100 extracted
10 February 2009 molars with G-Cem (GC Corp.), BisCem (Bisco), Multilink Sprint (Ivoclar Vivadent), SAC-A
Accepted 24 February 2009 (Kuraray Co.), XP Bond/Calibra (Detrey Dentsply). The cements were used at pre-cure
temperatures that recur in their handling (4 8C refrigerator, 24 8C room and 37 8C intraoral),
as well as following pre-heating up to 60 8C. Microtensile bond strengths to dentin were
Keywords: measured and compared with statistical tests. Scanning electron microscope observations
Bonding of cement–dentin interfaces were performed.
Self-adhesive resin cements Results: The bond strength of G-Cem and Calibra was not significantly affected by tem-
Dentin perature changes from refrigerator storage to intraoral application. At any assessed pre-cure
Pre-cure temperature temperature the total-etch luting agent Calibra achieved a significantly stronger adhesion
Pre-heating than the auto-adhesive cements. Limited to null adhesion was yielded by BisCem and SAC-
A. The procedure of 60 8C pre-heating, proposed in previous studies for restorative resin
composites, was of no use for the tested luting agents. Only the total-etch luting agent
Calibra developed a distinct hybrid layer. The self-adhesive cements exhibited a more
superficial interaction with dentin.
Conclusions: Regardless of the pre-cure temperature, the bonding potential of the self-
adhesive resin cements was inferior to that of the total-etch luting agent tested as control.
The adhesive properties of the BisCem and SAC-A were extremely scarce.
# 2009 Elsevier Ltd. All rights reserved.

1. Introduction pulp reaction, the ability to bond to different substrates, and

Self-adhesive resin cements have gained popularity for luting
ceramic, metal, and composite indirect restorations, as well as
fiber posts.1
The simplified handling of these materials is expected to
render the luting procedure less technique-sensitive and time-
consuming as compared with multi-step resin cements.2–6
Lower risk for post-operative sensitivity along with moderate
the potential for fluoride release have also been credited to
these new luting materials.7–12
However, a limited demineralizing action, yielding a super-
ficial and irregular interaction with hard dental tissues, has been
reported for RelyX Unicem (3M ESPE, Seefeld, Germany).2–6,13
The relatively high viscosity and the moderate etching potential
do not favor a deep infiltration of the resin into the collagen
network, to generate an evident hybrid layer.4

* Corresponding author. Tel.: +39 0577 233131; fax: +39 0577 233117.
E-mail address: cecilia.goracci@gmail.com (C. Goracci).
0300-5712/$ – see front matter # 2009 Elsevier Ltd. All rights reserved.
doi:10.1016/j.jdent.2009.02.006
 journal of dentistry 37 (2009) 454–461
Additionally, the presence of voids in the cement layer
possibly affecting the resistance of restorations under
dynamic loading has been described for RelyX Unicem.12
The application of a static seating force heavier than finger
pressure in onlays luting was found to enhance homogeneity
and adaptation on the dentin substrate of RelyX Unicem and
Panavia F2.0.5
Also, in a recent study, the influence on bonding effec-
tiveness of the temperature changes from refrigerator to room
and oral cavity was assessed. The recommendation to let the
cements reach the room temperature prior to the clinical use
for improved adhesion emerged from this investigation.14
Furthermore, the applicability to luting agents of a pre-
heating procedure previously proposed for restorative resin
composites was investigated.14 It was reported that pre-heating
to 558–60 8C had the effects of reducing viscosity, improving
flowability, and decreasing film thickness of restorative resin
composites.15,16 Moreover, as a result of enhanced monomer
conversion, pre-heating was claimed to positively affect
properties such as surface hardness, flexural modulus, fracture
toughness, tensile strength,15,16 and wear resistance,17 that may
be clinically relevant also for luting agents. With regard to the
latter materials, pre-heating to 60 8C promoted the adhesion of
Panavia F 2.0, while uselessly accelerating the RelyX Unicem
setting.14
A variety of new self-adhesive resin cements have lately
been introduced in the market. The information currently
available in the literature on these materials is scarce to
absent.1
Therefore, the present study was directed at assessing in
vitro the bonding potential to dentin of four newly developed
self-adhesive resin cements that were tested in comparison
with a total-etch resin cement considered as control. The
luting agents were used at temperature levels that recur in
their handling: refrigerator storage (4 8C), room (24 8C), and
intraoral (37 8C) temperature. It was additionally verified
whether the 60 8C pre-heating procedure proposed for
restorative resin composites15 was practical and beneficial
also for bond strength and adaptation of the new simplified
cements. Such parameters were assessed with microtensile
bond strength testing and scanning electron microscopic
observations of the cement–dentin interfaces.
The tested null hypothesis was that neither the cement
nor its pre-cure temperature had a significant influence on
interfacial morphology and microtensile bond strength
achieved on dentin when luting composite onlays.
2. Materials and methods
The research protocol was reviewed and approved by the
Institutional Review Board from the University of Siena, Italy.
A hundred non-carious extracted human third molars were
selected and stored in a 1% chloramine T solution at 4 8C for
one month. Teeth were retrieved from the disinfectant
solution, abundantly rinsed with distilled water, and finally
stored in the same medium at 37 8C during the last 24 h before
use.
Four self-adhesive resin cements recently introduced on
the market were investigated: G-Cem (GC corp., Tokyo, Japan),
455
BisCem (Bisco, Schaumburg, IL, USA), Multilink Sprint (Ivoclar
Vivadent, Schaan, Liechtenstein), SAC-A (Kuraray Co., Tokyo,
Japan) were tested in comparison with the total-etch luting
system XP Bond/Calibra (Detrey Dentsply, Konstanz, Ger-
many), that was considered as control. Also bond strength
data collected for RelyX Unicem (3M ESPE, Seefeld, Germany)
in a previous study with the same design as the present
investigations were included for comparison.14 All the
materials were used in dual-cure mode for luting composite
overlays (Paradigm MZ100, 3M ESPE, St. Paul, MN) on the
exposed dentin substrate. Chemical composition and batch
numbers of the investigated cements are reported in Table 1.
Paradigm MZ100 blocks were cut using a slow-speed
diamond saw (Isomet, Buehler Ltd., Lake Bluff, IL, USA) into
2 mm thick blocks, whose surface area was sufficient to cover
the prepared substrate. The intaglio surface of each composite
block was polished with 180-grit SiC paper, cleaned with
ethanol, and air-dried.
Teeth were randomly divided into 20 groups according to
the material to be applied on the dentinal substrate and to the
cement at pre-cure temperature:
Groups (1–4) G-Cem at pre-cure temperatures of 4 8C, 24 8C,
37 8C, and 60 8C, respectively.
Groups (5–8) BisCem at pre-cure temperatures of 4 8C, 24 8C,
37 8C, and 60 8C, respectively.
Groups (9–12) Multilink Sprint at pre-cure temperatures of
4 8C, 24 8C, 37 8C, and 60 8C, respectively.
Groups (13–16) SAC-A at pre-cure temperatures of 4 8C,
24 8C, 37 8C, and 60 8C, respectively.
Groups (17–20) Calibra at pre-cure temperatures of 4 8C,
24 8C, 37 8C, and 60 8C, respectively.
Data collected in the previous study14 for RelyX Unicem at
4 8C, 24 8C, and 37 8C were labelled as Groups 21, 22, and 23,
respectively.
For testing at pre-cure temperature of 4 8C, the cements
were used right after removing them from the refrigerator,
where they had been stored for at least 1 day.
For testing at pre-cure temperature of 24 8C, the luting
materials were taken out of the refrigerator and left at the
room temperature of 24 8C for at least 1 day.
For testing at pre-cure temperature of 37 8C and 60 8C, a
thermostatically controlled laboratory oven (Precision Thelco,
Thermo Fisher Scientific, Walthan, MA) was used to pre-heat
the luting agents. Prior to testing, all the materials were
allowed to stabilize at the established temperatures for at least
24 h.18
Following warming up to 60 8C, however, curing of G-Cem
was so accelerated that at the time of dispensing the material
was already set and could not extrude from the capsule tip.
Multilink Sprint and the catalyst syringe of Calibra, pre-heated
at the same temperature, set before the time of mixing.
Consequently, groups 4, 12, and 20 were excluded from the
study.
2.1. Bonding procedure
Three teeth per group were destined to microtensile bond
strength testing.
456 journal of dentistry 37 (2009) 454–461

Table 1 – Chemical composition and batch numbers of the tested materials.

Calibra XP BOND
Tert-butanol: TEGMA; UDMA; PENTA; TCB resin;
nanofiller; Camphorquinone; DMABE; Butylated
benzenediol; HEMA (Batch # 0703001576)
Self-cure activator: UDMA, HEMA, catalyst,
photoinitiators, acetone, water (Batch # 070119)
Calibra
Base paste: Barium boron fluoroaluminosilicate
glass; bis-phenol A diglycidylmethacrylate;
polymerizable dimethacrylate resin; hydrophobic
amorphous fumed silica; titanium dioxide;
di-camphoroquinone (Batch # 060112)
Catalyst paste: Barium boron
fluoroaluminosilicate glass; bis-phenol A
diglydidylmethacrylate; polymerizable
dimethacrylate resin; hydrophobic amorphous
fumed silica; titanium dioxide; benzoyl peroxide.
(Batch # 0705291)

RelyX Unicem (Batch # 233110) Powder Liquid

Glass fillers, silica, calcium hydroxide, self-cure Methacrylated phosphoric esters,
initiators, pigments, light-cure initiators dimethacrylates, acetate, stabilizers, self-cure
initiators, light-cure initiators

G-Cem (Batch # 0611091) Powder Liquid

Fluoro–alumino–silicate glass, initiator, pigment UDMA, dimethacrylate, 4-META, distilled water,
phosphoric acid ester monomer, silicon dioxide,
initiator, inhibitor

Multilink Sprint (Batch # J22739) Dimethacrylate, acidic monomers, barium glass,

ytterbium trifluoride, silicon dioxide, initiators,
stabilizers

SAC-A (Batch # SACA-A-061211) Paste A Paste B

Bis-GMA: TEGMA; other methacrylate monomers; Bis-GMA: other methacrylate monomers;
MDP; silanated barium glass filler; silanated silanated barium glass filler; silanated colloidal
colloidal silica; camphorquinone; benzoyl silica; surface treated sodium fluoride;
peroxide; others accelerators; pigments; others

BisCem (Batch # 0600011983) Bis (hydroxyethylmethacrylate) phosphate (base),

tetraethylene glicol dimethacrylate, dental glass

Paradigm MZ100 (Batch # 20060213) Bis-GMA, TEGDMA, zirconia silica filler

HEMA: 2-hydroxyethyl methacrylate, Bis-GMA: bis-phenol A glycidyldimethacrylate, TEGDMA: triethylenglycol dimethacrylate; UDMA:
urethane dimethacrylate; MDP: 10-methacryloxydecyl dihydrogen phosphate; 4-META: 4 methacryloyloxyethyl trimellitate anhydride.

On each tooth a flat deep coronal dentin surface was copiously with water, and blot-dried with a cotton gauze for 5 s
created by removing the coronal enamel and superficial dentin prior to the luting procedure.
with the Isomet water-cooled saw. The dentine surfaces were The luting materials were handled strictly according to
finished by wet grinding with 180-grit SiC paper,19 rinsed manufacturers’ instructions reported in Table 2.

Table 2 – Handling of the luting agents.

Calibra -Silanize resin composite overlay.
-Etch with 37% phosphoric acid for 15 s. Water rinse and
air.dry. Apply adhesive in a single coat. Dry with a
gentle airflow after 5 s. Light cure for 20 s.
-Mix equal amounts of base and catalyst.

RelyX Unicem -Activate the capsule for 2 s and mix it for 10 s with
Rotomix (3M ESPE).
-Apply the cement onto the substrate.
-Let the cement autocure for 5 min at 37 8C and 100%
G-Cem -Activate the capsule and mix it for 10 s. humidity under pressure. -Light-cure through the
-Apply the cement onto the substrate. composite overlay for 20 s

Multilink Sprint -Extrude the cement from the automix syringe.

-Apply the cement onto the substrate.

SAC-A -Extrude the cement from the automix syringe.

-Apply the cement onto the substrate.

BisCem -Extrude the cement from the automix syringe.

-Apply the cement onto the substrate.
 journal of dentistry 37 (2009) 454–461
When Calibra was used for luting, a silane solution (Calibra
Silane Coupling Agent, DeTrey Dentsply) was applied to the
composite block surface and spread by air blowing.
The composite block was luted on the dentin substrate
under a pressure of 40 g/mm2. The seating force was applied
by means of a plunger loaded with a box of lead pellets, whose
weight was adjusted based on the substrate area. The
specimens were kept under pressure inside a laboratory oven
at 37 8C and 100% of relative humidity for the first 5 min of
cement auto-cure reaction. After 5 min of self-curing, the
luting cement was light cured from the top of the 2 mm thick
composite block for 20 s with a halogen light curing unit
(XL3000, 3M ESPE, St. Paul, MN). The curing device was
operated at 550 mW/cm2 and the cement layer below the
composite block was irradiated by 100 mW/cm2. Another
2 mm-thick resin composite block was then luted onto the first
one, using RelyX Unicem (3M ESPE, Seefeld, Germany) in a self-
cure mode, in order to allow an adequate handling of the
specimens in the microtensile test.
After a 24-h storage period at 37 8C under 100% relative
humidity, teeth were sectioned occluso-gingivally into serial
slabs, using the Isomet saw under water cooling at low speed and
without any additional pressure. Each slab was fixed on a glass
slide with sticky wax, and further sectioned into 0.9 mm 
0.9 mm composite-dentin sticks, according to the ‘‘non-trim-
ming’’ method of the microtensile test. The specimens were
stressed to failure under tension using a universal testing
machine (Controls, Milano, Italy; crosshead speed: 1 mm/min).
2.2. Statistical analysis of microtensile bond strength
data
Some groups (all the cements at 60 8C, BisCem at 24 8C and
37 8C, Multilink Sprint at 37 8C, SAC-A at 4 8C and 37 8C) had to
be excluded from the statistical analysis as all the specimens
failed prior to testing.
In groups that had some premature failures, the latter were
included into statistical calculations as ‘zero’ values.
Separate analyses were conducted in order to assess the
influence of pre-cure temperature on the adhesive potential of
each cement, and to compare different cements for the bond
strength obtained at each tested temperature.
For Calibra differences in bond strength among 4 8C, 24 8C,
and 37 8C were assessed with the one-way analysis of variance
and the Tukey test for post hoc comparisons, as the data
passed the tests of normality and homogeneity of group
variances (Kolmogorov–Smirnov test and Levene test, respec-
tively). Since such requirements were not met by G-Cem and
RelyX Unicem data, the Kruskal–Wallis non-parametric
ANOVA was used, followed by the Dunn’s multiple range test.
For Multilink Sprint the difference in bond strength between
4 8C and 24 8C was assessed with the Mann–Whitney U test.
Differences in bond strengths among BisCem, G-Cem,
Multilink Sprint, and Calibra at 4 8C were statistically analyzed
with the Kruskal–Wallis non-parametric ANOVA, followed by
the Dunn’s multiple range test.
Also, the bond strengths of SAC-A, G-Cem, Multilink Sprint,
RelyX Unicem, and Calibra at 24 8C were compared with the
Kruskal–Wallis non-parametric ANOVA and the Dunn’s
multiple range test. The same tests were applied to compare
457
G-Cem, RelyX Unicem, and Calibra with regard to the adhesion
achieved at 37 8C.
In all the analyses the level of significance was set at
a = 0.05.
2.3. Scanning electron microscopy examination
The dentin–cement interface of two teeth from each experi-
mental group was observed under a scanning electron
microscope (JSM 6060 LV, JEOL, Tokyo, Japan). Each tooth
was cut with the Isomet saw in order to obtain a 2 mm thick
slab containing the investigated surface. After polishing under
wet condition with increasingly finer grits of SiC papers
(Buelher, #600, #1000, #1200), the coupled interface was
brought into relief by etching with 32% silica-free phosphoric
acid gel (Uni-Etch, Bisco, Schaumburg, IL), and briefly
deproteinized with a 2% sodium hypochlorite solution for
60 s. Then, the interface was rinsed with water, air-dried for
10 s, and an impression was taken using a PVS impression
material (Affinis, Coltène-Whaledent AG, Alstätten, Switzer-
land). After separation of the impression material from the
bonded interface, positive replicas were obtained using a
polyether impression material (Permadyne, 3M ESPE AG,
Seefeld, Germany). Finally, all replicas were mounted on
aluminum stubs, sputter coated with gold (Polaron Range,
Quorum Technologies, England) and inspected with the
scanning electron microscope at different magnifications.
3. Results
3.1. Microtensile bond strength data
Descriptive statistics and percentage of pre-test failures for
each experimental group are reported in Table 3, along with
statistical significance of the differences.
No statistically significant difference emerged for Calibra
and G-Cem when the cement was used at 4 8C, 24 8C, or 37 8C
( p > 0.05).
Multilink Sprint achieved a significantly higher bond
strength at 24 8C than at 4 8C ( p < 0.001).
At each assessed temperature level significant differences
emerged among the cements (Table 3).
For all the self-adhesive cements the bond strengths
measured at any temperature were lower than those achieved
by the total-etch luting agent Calibra. Differences were
statistically significant except for Multilink Sprint at room
temperature (Table 3).
3.2. Scanning electron microscopy examination
Calibra appeared homogeneous and uniformly adapted on the
substrate. Moreover, a thick hybrid layer with diffuse resin
tags could be seen (Fig. 1).
When RelyX Unicem was used at 4 8C, the cement layer
appeared porous, densely filled with glass particles and gaps
could be identified along the interface. The presence of resin
tags was extremely reduced and alternated to areas of
discontinuities. The hybrid layer was extremely thin to non-
existent (Fig. 2).
458 journal of dentistry 37 (2009) 454–461

Table 3 – Descriptive statistics of the microtensile bond strength data in MPa for all the experimental groups. For each
temperature level significant differences among the cements are labelled with different capital letters in the ‘Significance’
column. For each cement significant differences in bond strength among the assessed pre-cure temperatures are
highlighted by different italic and greek small letters in the ‘Cement’ column.
Cement % of pre-test # of tested Mean Median Standard Significance
failures specimens deviation ( p < 0.05)

SAC-A 4 8C 100% 0 0 0 0 –
BisCem 4 8C 64.7% 31 3.4 0 6.1 A
RelyX Unicem 4 8Ca 29.2% 34 5.4 5.1 1.7 A
G-Cem 4 8C 0 51 11.3 8.6 8.4 B
Multilink Sprint 4 8Ca 13.1% 38 9.4 9 5.8 B
Calibra 4 8C 0 50 27.5 29.1 13.5 C

BisCem 24 8C 100% 0 0 0 0 –
SAC-A 24 8C 26.5% 13 1.6 0 3 A
RelyX Unicem 24 8Cb 44.9% 27 11.4 10 6.1 B
G-Cem 24 8C 9.6% 52 13.5 11.6 10.2 B
Multilink Sprint 24 8Cb 0 46 19.5 19.5 9.9 BC
Calibra 24 8C 0 50 28.3 21.9 20.8 C

BisCem 37 8C 100% 0 0 0 0 –
SAC-A 37 8C 100% 0 0 0 0 –
Multilink Sprint 37 8C 100% 0 0 0 0 –
RelyX Unicem 37 8Cb 13% 67 10.6 9.7 4.3 A
G-Cem 37 8C 12.1% 66 12.4 7.3 8.4 A
Calibra 37 8C 5.3% 56 32.9 20.1 18.1 B

SAC-A 60 8C 100% 0 0 0 0 –
BisCem 60 8C 100% 0 0 0 0 –

G-Cem 60 8C, Multilink Sprint 60 8C, RelyX Unicem 60 8C, Calibra 60 8C set before the use. Bold entries indicate the statistically significant
differences among the cements tested at 37 8C temperature.

4. Discussion

The collected data require rejection of the null hypothesis that

neither the cement nor its pre-cure temperature had a
significant influence on interfacial morphology and micro-
tensile bond strength achieved on dentin when luting
composite onlays.

Fig. 1 – SEM micrograph of specimens luted with XP Bond/

Calibra system at 4 8C (X250, bar = 100 mm, CO = composite
overlay, RC = resin cement, and D = dentin). A thick hybrid
layer with resin tags uniformly distributed along the
interface with dentin was seen.

Similarly thin was the hybrid layer created at the same

temperature by G-Cem that, however, exhibited a better
marginal continuity and less porosities within the cement
layer (Fig. 3).
A large gap was evident at the interface between dentin and
BisCem used at a 24 8C temperature. The cement layer
appeared quite homogeneous (Fig. 4).
Fig. 2 – SEM micrographs of specimens luted with RelyX
Unicem at 4 8C (X250, bar = 100 mm, CO = composite
overlay, RC = resin cement, and D = dentin).
Discontinuities were present along the interface with
dentin and porosities could be noted within the cement
layer. The hybrid layer was thin to undetectable.
 journal of dentistry 37 (2009) 454–461
Fig. 3 – SEM micrographs of specimens luted with G-Cem at
4 8C (X250, bar = 100 mm, CO = composite overlay,
RC = resin cement, and D = dentin). Good continuity could
be seen between the luting agent and the dental substrate.
The cement layer appeared porous.
With the exception of Multilink Sprint, that at room
temperature measured bond strengths statistically similar
to those of Calibra, all the other self-adhesive cements
developed at any temperature a weaker adhesion than that
achieved by the total-etch luting agent tested as control.
In the present study Calibra was used in combination with
the total-etch adhesive system XP Bond. The phosphoric acid
used in etch-and-rinse systems is able to completely remove
smear layer and smear plugs and to promote demineralization
of the underlying intact dentin, thus exposing the network of
collagen fibrils. As the latter is subsequently infiltrated by the
adhesive resin, a hybrid layer develops in intertubular dentin,
and resin tags form within the dentin tubules.20
The ability of the total-etch cement Calibra to produce a
deeper demineralization and a thicker hybrid layer in
Fig. 4 – SEM micrographs of specimens luted with BisCem
at 24 8C (X250, bar = 100 mm, CO = composite overlay,
RC = resin cement, and D = dentin). The cement layer
appeared homogeneous. However, no signs of hybrid
layer formation were detectable.
459
comparison with self-adhesive materials was confirmed in
the SEM images of the present study (Fig. 1). A thick layer
of resin-infiltrated dentin represents a valid substrate for
copolymerization of the overlaid cement. This may account
for the superior bond strength expressed by Calibra regardless
of the pre-cure temperature. As a matter of fact, pre-heating
did not influence either the bond strength or the interfacial
adaptation of Calibra to dentin.
Also the bond strength of G-Cem was not significantly
affected by pre-heating. At refrigerator temperature its bond
strength was significantly higher than that of RelyX Unicem
and BisCem. Moreover, in microscopic observations G-Cem
appeared capable of penetrating the dentin substrate to a
greater depth than RelyX Unicem (Fig. 3). The relatively lower
pH of G-Cem may provide an explanation for this finding. The
pH of RelyX Unicem is reported to be higher than that of G-
Cem at 20 s after light curing and neutralized after 48 h.
Conversely, G-Cem has a pH of 3.6 at this stage.21 The acidity of
G-Cem, although beneficial for the initial interaction with the
dental substrate,22 may however expose the bond to hydro-
lytic degradation phenomena if retained over time.21
In addition to phosphoric acid esters as etching monomers,
G-Cem contains 4-META, that in the presence of the water
contained in the cement or coming from the underlying
dentin, is hydrolyzed to form 4-MET. The latter is capable of
chelating calcium ions of hydroxyapatite crystals still avail-
able at the demineralization front.23 Such chemical reactions
would add to micromechanical retention in the overall
bonding mechanism of G-Cem. However, porosities were
noted within the cement layer, possibly affecting the
mechanical properties of the cement and accounting for the
lower retentive potential in comparison with Calibra.
Poor bonding ability to dentin was exhibited in this
investigation by BisCem and SAC-A. According to the
manufacturer’s claim, BisCem would react with hydroxyapa-
tite, creating a diffusion layer rather than the hybrid layer that
normally occurs in the adhesive process. The diffusion layer
would consist of ion bonds or a complex of BisCem with
calcium and phosphate from the tooth.
However, BisCem includes in its composition the acidic
monomer HEMA phosphate. HEMA phosphate in an aqueous
solution is hydrolyzed into HEMA and the strongly acidic
phosphoric acid.24 The latter may be responsible for deminer-
alization of the dentin surface and reduction of the calcium
ions needed for creation of the diffusion layer. Moreover,
despite the content of HEMA, a discrepancy between front of
dentin demineralization and depth of resin infiltration may be
responsible for the null bond strength yielded by BisCem in
this study. Particularly, filler particles may have hampered
good infiltration of the resin into the collagen network. Also, at
24 8C and 37 8C, the higher temperatures may have sped up the
setting of the material, thus limiting the penetration time.
It is known that incomplete infiltration of resin into
demineralized dentin places the bond at risk of degradation.25
Longevity of adhesion may also be undermined in HEMA-rich
formulations. As a monofunctional monomer, HEMA forms
weaker and linear polymers upon polymerization.22 Moreover,
HEMA can retain water within the cement, thus weakening
the mechanical strength of the cement and making it
susceptible to hydrolytic degradation over time.26
460 journal of dentistry 37 (2009) 454–461
SAC-A produced a detectable adhesion only at 24 8C. SAC-A
contains the acidic monomer 10-MDP, that is used as an
etching monomer in adhesive systems due to its dihydrogen-
phosphate group, which can dissociate in water to form two
protons. Although the bonding potential of 10-MDP to
hydroxyapatite is reported to be greater than that of 4-
MET,27 SAC-A recorded lower bond strengths than G-Cem at
the same temperature. The incorporation of Bis-GMA and
TEGDMA without hydrophilic monomers favoring spreading
on the substrate may have generated high contact angle
values that hindered dentin wetting, resin infiltration into the
demineralized dentin, and hybrid layer formation.28
With regard to Multilink Sprint, this cement particularly
benefited from the temperature increase from 4 8C to 24 8C,
achieving at the latter temperature bond strengths compar-
able to those of the total-etch system Calibra. Conversely, in a
previous study in which Multilink Sprint was used at room
temperature to cement composite onlays to dentin, high
frequency of premature failures and low bond strengths were
reported, particularly for specimens luted under simulated
pulpal pressure.29
At 37 8C null bond strength was observed in our study for
Multilink Sprint. Further investigation is needed to under-
stand the reason for such behavior of the material at oral
temperature. Unfortunately, no detailed information is avail-
able regarding the chemical composition of this cement.
In summary, warming the cements to body temperature
did not bring any significant advantage over using them at
room temperature. In this regard it should be noticed that
although teeth were stored at 37 8C during the last 24 h before
use, however, cutting and grinding to create the bonding
substrate were performed under water-cooling, as water-
cooling would be used clinically while cutting the onlay
preparation with burs. Also, the composite blocks were stored
at room temperature. Therefore, heat transfer expectedly
occurred from the pre-heated luting agent to the substrates,
leading to cooling of the cement. This may explain in
particular why no significant differences emerged in the bond
strengths developed by Calibra, RelyX Unicem and G-Cem
when applied at room or at oral temperature. For the other
cements pre-heating was actually detrimental.
Warming up to 60 8C was useless for all the materials. RelyX
Unicem and G-Cem set already during mixing. Plausibly, the
heat catalyzed the acid–base reaction between acidic mono-
mers and basic fillers. Calibra and Multilink Sprint were set
even before the time of mixing. Both the materials contain
benzoylperoxide. The increase in temperature may have
favored the formation of radicals, responsible for the
premature curing of the cements.
BisCem and SAC-A at 60 8C could be applied onto the
substrate. However, the pre-heating procedure did not bring
any improvement to the scarce bonding potential of these
cements.
In the present study, the luting procedure involved the
application of a resin composite overlay on a flat coronal
dentin substrate, therefore in a geometric configuration
favoring stress relief. Repeating the study under less favorable
conditions of C-factor, such as inlays luting, would allow an
appreciation of the influence of contraction stress on the
adhesion of these new cements.30
Moreover, the seating pressure applied for luting in the
present investigation was chosen in consideration of the
outcome of a previous study in which a seating force heavier
than finger pressure during the initial self-curing period had a
beneficial effect on the interfacial bond strength and adapta-
tion of Panavia F 2.0 and RelyX Unicem.5
5. Conclusions
The temperature changes from refrigerator storage to
intraoral application did not significantly influence the bond
strength to dentin of G-Cem and Calibra.
At any assessed temperature the total-etch luting agent
achieved a significantly stronger adhesion than the self-
adhesive cements.
Scarce to null bonding potential was exhibited by BisCem
and SAC-A.
The procedure of 60 8C pre-heating, proposed in previous
studies for restorative resin composites, was of no use for the
tested luting agents.
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