Clinical Research

Preheated composite resin used as

a luting agent for indirect restorations:
effects on bond strength and resin–
dentin interfaces
Marcelo Goulart, DDS, MSc
Department of Conservative Dentistry, Federal University of Rio Grande do Sul, Brazil

Barbara Borges Veleda, DDS, MSc

Department of Conservative Dentistry, Federal University of Rio Grande do Sul, Brazil

Deisi Damin, DDS, MSc

Department of Surgery and Orthopedics, Federal University of Rio Grande do Sul, Brazil

Glaucia Maria Bovi Ambrosano, Agr.Eng, MSc, PhD

Department of Social Dentistry, Piracicaba Dental School, State University of Campinas,
Piracicaba, SP, Brazil

Fabio Herrmann Coelho de Souza, DDS, MSc, PhD

Department of Conservative Dentistry, Federal University of Rio Grande do Sul, Brazil

Maria Carolina Guilherme Erhardt, DDS, MSc, PhD

Department of Conservative Dentistry, Federal University of Rio Grande do Sul, Brazil

Correspondence to: Dr Maria Carolina Guilherme Erhardt

Av. Ramiro Barcellos, 2492, Porto Alegre, RS, 90035-003, Brazil; Tel: +55 51 33085202, Email: carolinabee@hotmail.com

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Abstract
Purpose: The aim of this study was to
evaluate the effect of preheating com-
posite resins used as luting agents for
indirect restorations on microtensile
bond strength (µTBS) and adhesive in-
terfaces.
Material and methods: Fifty sound ex-
tracted third molars were used. Ten
experimental groups were formed with
three different luting agents: one resin
cement (RelyX ARC) and two composite
resins (Venus and Z250  XT). The com-
posite resins were tested both at room
temperature and when preheated to
64°C. Restoration depth was tested us-
ing 2 or 4 mm-height indirect composite
resin restorations, previously made on
cylindrical molds. Adhesive and luting
procedures were done under simulated
pulpal pressure. After luting, the teeth
were sectioned into beams with a cross-
sectional area of 1 mm2 at the bonded
Goulart et al
interface, and tested in tension at 0.5 mm/
min. The characteristics of the adhesive
interfaces were observed under scan-
ning electron microscopy (SEM). The
µTBS data were analyzed using ANOVA
and the Tukey test (α = 0.05).
Results: When luting 2 mm restorations,
the composite resin Z250 XT, preheated
or at room temperature, achieved signifi-
cantly higher µTBS than did RelyX ARC.
At this depth, Venus did not differ from
the resin cement, and with the 4 mm
restorations, only preheated Venus pre-
sented significantly higher µTBS than
RelyX  ARC. Preheating the composite
resin resulted in thinner luting interfaces,
with a more intimate interaction between
luting agent and adhesive layer.
Conclusion: Preheating composite resin
for luting procedures may not improve
µTBS, although it could be used to re-
duce material viscosity and improve res-
toration setting.
(Int J Esthet Dent 2018;13:2–13)
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 Clinical Research
Introduction
Indirect restorations such as inlays and
onlays have been widely used in the
past. Although they have shown good
results in follow-up studies,1,2 most re-
ported failures are related to restoration
margins. After 11 years of placement,
50% of indirect inlays presented mar-
ginal discoloration, against 26% for di-
rect inlays.3 Also, 69% of indirect inlays
presented cement wear in this period.
Adhesive luted restorations differ from
direct fillings due to the presence of a
luting agent on the margin. Therefore,
marginal defects on indirect restorations
are mainly associated with the luting
agent.
Among all luting materials, resin ce-
ment is the standard adhesive luting
agent for indirect restorations. Yet, the
presence of light passing through the
restoration to activate the luting agent
is a major concern.4 Thus, dual-cure
resin cements are most commonly pre-
ferred over self-curing or light-activated
cements.5 Composite resin has been
suggested as an alternative material
to improve restoration performance.6
In a recent study, similar results were
reported after 10 years of follow up for
composite resin indirect restorations lut-
ed with dual-cure resin cement or con-
ventional composite resin at room tem-
perature.7 Composite resin may perform
better than resin cement on restoration
margins in the long term due to more
inorganic load filling. This higher filler
content on the composite resin gives
the material better mechanical proper-
ties.8 Moreover, composite resin does
not contain chemical activators, which
are related to long-term color instability.9
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Heating composite resin was report-
ed to be a way of achieving a higher
degree of conversion for light-curing
composite resins.10 Acquaviva and
Cerutti11 observed that preheated com-
posite resins showed a similar degree of
conversion to dual-cure resin cements
under ceramic blocks of 2, 3, and 4 mm.
It has also been reported in the literature
that this heating strategy reduces com-
posite resin viscosity,12,13 which could
benefit the luting procedure. With regard
to temperature aggression, preheated
composite resin presented a low tem-
perature rise in the pulpal chamber and
was shown to be a safe clinical proced-
ure even on vital teeth.14
Despite all the evidence, luting indi-
rect restorations with preheated com-
posite resin has not yet been tested and
compared to resin cement. Thus, the
aim of this in vitro study was to evaluate
the effect of preheating composite resin
used as a luting agent for indirect res-
torations on microtensile bond strength
(µTBS) and adhesive interfaces.
Materials and methods
Fifty recently extracted caries-free hu-
man third molars were used in this study
(n = 5). The teeth were stored in distilled
water containing 0.5% chloramine-T at
4ºC and used within 6 months after ex-
traction. The teeth were obtained under
informed consent, with protocols that
were approved by the local ethics com-
mittee review board (n. 92.939).
All the teeth had a flat occlusal dentin
surface that was exposed by removing
the occlusal enamel with a diamond saw
(Microdont). To standardize the smear

layer, all dentin surfaces were wet grind-
ed with 600 grit SiC papers for 30 s (Lab-
pol, Extec). All the teeth also had their
roots removed using a diamond saw to
perform a cut 2 mm below the cemento-
enamel junction (CEJ).
To simulate pulpal pressure, the teeth
were connected with a 18 gauge stain-
less-steel tube inside the root to a device
with a container of distilled water deliver-
ing 15 cm of water pressure.15 The teeth
were bonded to the device with cyano-
acrylate adhesive (Super Bonder, Hen-
kel) for 5 min to stabilize the pulpal pres-
sure before the adhesive procedures.
Ten experimental groups were defined
to test three different materials (one resin
cement and two composite resins), two
restoration heights (2 and 4 mm), and
two temperatures (room temperature
and preheating to 64ºC).
Fifty composite resin discs were
made by layering increments of a nano-
hybrid composite resin (Tetric N-Ceram,
Ivoclar Vivadent) inside two PVC cylin-
drical molds of 2- and 4-mm depth and
10-mm diameter. Each increment was
light activated for 20 s with a LED curing
unit (Optilight Max, Gnatus). The molds
were placed above a polyester sheet,
and a glass slab was pressed on top of
the molds to standardize and activate
the last increment. One side of the res-
toration was airborne-particle abraded
with 50 µm aluminum oxide particles
for 10 s (Microjato, Bio-Art). Silane was
then applied for 60 s and air dried (Pros-
il, FGM). Then, a thin layer of adhesive
(Scotchbond Multi-Purpose, 3M  ESPE)
was applied and light activated for 20 s.
The materials and methods used for
the adhesive and luting procedures were
applied according to the manufacturers’
Goulart et al
instructions (Table 1). The dentin sur-
faces were etched for 15 s and washed
with air-water spray. A three-step etch-
and-rinse adhesive system was ap-
plied according to instructions. All ad-
hesive procedures took place in a room
with a controlled temperature of 22ºC.
The light-curing unit was periodically
checked with a radiometer (Coltolux 4,
Coltene Whaledent) during all proced-
ures in this study. Light irradiance was
stable at 900 mW/cm2.
Luting procedures were randomly
processed according to a table of ran-
dom numbers. After the dentin and res-
toration surfaces were ready, a stand-
ard portion of luting agent (0.05 ml) was
placed on the restoration. Then, the res-
toration was pressed over dentin using
finger pressure, and stabilized under a
500 g static load for 10  min.16 Excess
cement was removed with a brush, and
light activation was undertaken for 40 s
on top of the restoration, on the buccal
and lingual surfaces. For the preheated
groups, the composite resin and restor-
ation were preheated to 64ºC for 5 min
prior to luting in a digital wax pot (SJK).
The time of the restoration setting with
the static load was reduced to 30 s to
avoid temperature loss at the time of ac-
tivation.
After storage in distilled water, the
teeth were sectioned perpendicular
to the luting interface into slabs and
then into beams with a cross-sectional
bonded area of approximately 1 mm2
using a diamond saw (Labcut 150, Ex-
tec). Twenty central beams presenting
only dentin were selected for each ex-
perimental group. The beams were in-
dividually bonded to a µTBS jig with a
cyanoacrylate adhesive and stressed to
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 Clinical Research

Table 1  Adhesive materials, composition, and application techniques used

Material and Composition Mode of application

manufacturer (Batch No.)

Adper Scotch- HEMA, polyalkenoic 1.  Apply etchant for 15 s

bond Multiuse acid polymer, water 2.  Rinse thoroughly for 15 s
Primer – (#N295761) 3.  Dry for 5 s
3M ESPE 4.  Apply primer for 10 s
5.  Dry gently for 5 s

Adper Scotch- Bis-GMA, HEMA, tertiary 1.  Apply adhesive

bond Multiuse amines, and photoinitia- 2.  Light cure for 10 s
Adhesive – 3M tor (#N329945)
ESPE

Silane Prosil – Ethanol, water and 1.  Apply for 60 s

FGM methacryloxypropyl-tri- 2.  Air dry
methoxysilane (#160911)

Resin cement Bis-GMA, TEGDMA, 1.  Dispense automatic standard portion (clicker)

RelyX ARC – camphorquinone, 2.  Hand mix for 10 s
3M ESPE benzoyl peroxide and 3.  Apply at luting surface
zirconia/silica filler 4.  Set restoration and remove excess
(#N399165) 5.  Light cure for 40 s

Nanohybrid resin Bis-GMA, UDMA, 1.  Light cure for 40 s (used in this study for luting)
composite Z250 Bis-GMA, PEGDMA,
XT – 3M ESPE/A2 TEGDMA, zirconia and
shade silica, 82% filler weight
(#N412437BR)

Microhybrid resin Bis-GMA, TEGDMA, 1.  Light cure for 40 s (used in this study for luting)
composite Venus barium glass and
– Heraeus Kulzer/ silica, 78% filler weight
A2 shade (#010401)

Nanohybrid Bis-GMA, Bis-GMA, 1.  2-mm height layering

resin composite barium glass, ytterbium 2.  Light cure for 20 s (used for resin build-up)
Tetric N-Ceram – trifluoride and copoly-
­Ivoclar Vivadent/ mer, 80% filler weight
A3.5 shade (#P58315)

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Table 2  Mean microtensile bond strength (MPa) (standard deviation) obtained for each tested group

Temperature
Depth Resin
Room 64°C

Venus 29.11 (12.22) Ab #27.78 (6.76) Aa

2 mm Z250 XT *36.90 (6.38) Aa *32.43 (5.54) Aa

RelyX ARC 25.48 (7.92) -

Venus 28.25 (6.76) Bb *37.36 (3.99) Aa

4 mm Z250 XT 35.92 (8.12) Aa 33.08 (6.50) Aa

RelyX ARC 31.22 (8.94) -

*Differs from RelyX ARC at same depth.

#Differs from same material and temperature at 4 mm depth.
Means followed by different letters (upper case for lines; lower case for columns at same depth) are significantly different (P ≤ 0.05).

failure in tension at a crosshead speed specimens were gold-sputtered and

of 0.5 mm/min (EMIC DL1000, EMIC).
The cross-sectional area at the site of
failure was measured with a precision
of 0.01 mm with a digital caliper (Star-
rett 727, Starrett). Bond strength means
were calculated (MPa) and analyzed us-
ing the three-way ANOVA and Dunnett’s
test (P < 0.05).
Failure modes were evaluated after
testing under a stereomicroscope (EMZ,
Meiji Techno) at 40x magnification and
classified as adhesive, mixed, or cohe-
sive. Fracture patterns were analyzed
with the chi-square test (P < 0.05). Ad-
ditional resin–dentin bonded slabs from
each experimental group were used for
scanning electron microscopy (SEM)
evaluation. The slabs were polished with
waterproof papers of decreasing abra-
siveness up to 1200 grit. After polish-
ing, the surfaces were treated with 37%
phosphoric acid for 30 s and 10% so-
dium hypochlorite for 2  min. Prepared
examined in a scanning electron mi-
croscope (JSM-6060, JEOL) at an ac-
celerating voltage of 20 kV in order to
observe the morphology of the bonded
interfaces.
Results
Mean µTBS values obtained in all exper-
imental groups are displayed in Table 2.
One-way ANOVA detected significant
differences between groups. When lut-
ing 2 mm restorations, Z250 XT, preheat-
ed or at room temperature, achieved sig-
nificantly higher µTBS than RelyX  ARC
(P < 0.05). At this depth, Venus was
not different from the resin cement, al-
though with the 4 mm restorations, only
preheated Venus presented significantly
higher µTBS than RelyX ARC (P < 0.05).
RelyX ARC, Venus at room temperature,
and Z250 XT at both temperatures were

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Table 3  Three-way ANOVA not different for 4 mm restorations. At

room temperature, Z250  XT presented
Source Pr > F
higher µTBS compared to Venus. When
Resin 0.0008 comparing preheated composites, there
was no difference between both res-
Temp 0.9106 ins with both 2 and 4 mm restorations
(P > 0.05).
Depth 0.0594
Results from the factorial (three-way)
Resin*temp 0.0013 ANOVA are displayed in Table 3. Bond
strength was influenced by the compos-
Resin*depth 0.0435
ite resin factor (P < 0.001). Tempera-

Temp*depth 0.0085
ture and depth did not influence bond
strength values (P > 0.05). Interaction
Resin*temp*depth 0.0487 between all factors was found. Table 4
shows the failure modes of all the experi-
mental groups. No statistical difference
was found for fracture patterns.

Table 4  Distribution of failure modes after microtensile bond strength test

Fracture pattern
Temperature Depth Resin
Adhesive Mixed Cohesive

Venus 10 (50%) 1 (5%) 9 (45%)

2 mm Z250 XT 11 (55%) 2 (10%) 7 (35%)

RelyX ARC 14 (70%) 1 (5%) 5 (25%)

Room
Venus 7 (35%) 3 (15%) 10 (50%)

4 mm Z250 XT 6 (30%) 1 (5%) 13 (65%)

RelyX ARC 11 (55%) 4 (20%) 5 (25%)

Venus 9 (45%) 4 (20%) 7 (35%)

2 mm
Z250 XT 9 (45%) 5 (25%) 6 (30%)
64°C
Venus 8 (40%) 1 (5%) 11 (55%)
4 mm
Z250 XT 7 (35%) 2 (10%) 11 (55%)

P = 0.2110

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G6 – RelyX (4 mm) G7 – Venus (4 mm) G8 – Z250 XT (4 mm)

Fig 1    Adhesive interfaces of groups at room temperature.

G2 – Venus (2 mm) G4 – Venus 64° (2 mm)

Fig 2    Adhesive interfaces of Venus composite resin, at room temperature and preheated.

G8 – Z250 XT (2 mm) G5– Z250 XT 64° (4 mm)

Fig 3    Adhesive interfaces of Z250 XT composite resin, at room temperature and preheated.

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 Clinical Research
Regarding resin–dentin bonded inter-
faces, different characteristics for each
experimental group could be observed
under SEM examination. Resin cement
presented thin films of luting material
that could easily be identified between
dentin and restoration adhesive layers
(Fig 1). Luting film thickness of this ma-
terial ranged around 30 µm.
The effects of preheating compos-
ite resin were clearly noticed on resin–
dentin bonded interfaces. A reduction
of the entire interface thickness (ad-
hesive–resin–adhesive) was observed
due to the composite resin viscosity de-
crease. While the thickness of unheated
groups ranged around 60 to 80 µm (Ve-
nus), and 90 to 110 µm (Z250 XT), pre-
heated materials showed thicknesses of
50 to 80 µm (Venus), and 35 to 45 µm
(Z250 XT) along the entire adhesive in-
terface (Figs 2 and 3).
Although it resulted in a clear viscos-
ity reduction, preheating did not allow
for an accurate observation of the ma-
terial thickness inside the luting film. A
more intimate interaction caused by the
homogenization of the adhesive with
the composite resin layer was observed
when heating was employed. Due to
this behavior, a clear identification of the
adhesive layer and the luting material
on the interface was not possible. Fig-
ures 2 and 3 show this different heating
behavior.
Discussion
The aim of this study was to evaluate
the effect of preheating composite resin
used as a luting agent for indirect res-
torations on the µTBS and adhesive
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VOLUME 13 • NUMBER 1 • Spring 2018
interfaces. Regarding µTBS, compos-
ite resin showed similar or higher re-
sults compared to resin cement at both
temperatures and depths. Temperature
and depth did not influence µTBS in the
factorial analysis. The SEM evaluation
showed different adhesive interface
characteristics. Preheated composite
resin showed a different interaction with
the adhesive compared to the other ma-
terials.
Other studies have shown negative
effects of light attenuation with different
materials such as composite resin and
ceramics.17,18 It was reported that com-
posite resin presented less light attenua-
tion compared to ceramic.5 Regardless
of the restorative material, light attenua-
tion causes a reduction in the degree of
conversion of the luting agent. This re-
duction is associated with poor mechan-
ical properties of the material. Therefore,
luting agent selection for indirect restor-
ations is generally affected by the mater-
ial activation mode. However, a clinical
study that followed resin indirect restor-
ations luted with a dual-cure resin ce-
ment and a light-curing composite resin
for 10 years did not find any difference
between the two luting agents.7
Despite many in vitro reports of light
attenuation and its influence on me-
chanical properties, the present study
did not show this behavior, since res-
toration height could not be related to
a decrease in bond strength. Although
it was expected that groups luted with
composite resin at room temperature
would show that light attenuation affect-
ed final bond strength, this trend was not
observed. Our results therefore corrobo-
rate with those found in the previously
mentioned clinical study. This could be

explained by a proper degree of con-
version achieved with the light activation
protocol followed for all experimental
groups. The protocol used in this study
does not seem to overestimate light
activation, since one activation of 40 s
(900 mW/cm2) on occlusal, buccal, and
lingual surfaces is easily carried out in
clinical situations. Also, composite resin
presents less light transmittance (450 to
500 nm) compared to enamel.19 Com-
posite resins are comparable to dentin
regarding light transmittance,20 thus the
restoration design used in this study did
not seem to increase clinically possible
luting irradiation.
Clinically, the use of preheated com-
posite resins may be a challenge be-
cause of the shorter working time. To
benefit from heating features,21,22 the
composite resin must still be heated at
the moment of light activation. Accord-
ing to Daronch et al,23 a temperature
loss of 50% is observed 2 min after leav-
ing the heating device. Therefore, luting
or restorative procedures using preheat-
ed composite resin must be performed
carefully so that the material is quickly
light activated after leaving the heating
device. In this study, this temperature
loss was avoided by reducing the restor-
ation setting time to 30 s. Also, heating
effects were clearly noticed in the SEM
images.
Film thickness is a feature that was
considered in the luting agent selec-
tion.4 Nevertheless, there is no clear
evidence in the literature of a specific
correct thickness for luting inlays and on-
lays. The American Dental Association
Specification No. 8, which established
standards for zinc phosphate cements,
is commonly used as a reference.24
Goulart et al
According to this specification, type  II
cements must not exceed a film thick-
ness of 40 µm. However, there is no evi-
dence of the clinical implications of this
value for an indirect restoration, since
most studies are conducted for crowns.
Composite resins present higher film
thicknesses compared to resin cements,
but preheating was shown to reduce
the viscosity of some composite resins
to comparable values that are attained
with resin cements. In a previous study,
a preheated microhybrid composite res-
in presented a film thickness of 45 µm,
showing a reduction of 24% of the thick-
ness compared to that under room tem-
perature.25 Therefore, preheating may
be important to avoid a poor restoration
setting.
Composite resin composition plays a
major role in the viscosity of the mater-
ial. Among other factors, filler and mon-
omer composition are directly related
to mechanical properties and viscos-
ity of composite resin.26,27 Regarding
filler load, higher filled composite res-
ins present higher viscosity. Moreover,
filler size and shape are also related to
viscosity. Composite resins with bigger
filler particle size present less viscosity,
and nanohybrid composite resins tend
to present higher viscosity than micro-
hybrid ones. This behavior was con-
firmed for both composite resins under
SEM evaluation. Despite other factors
that may influence viscosity, microhy-
brid composite resin presented shal-
lower luting films.
Apart from all the evidence for the
possibility of using composite resin as a
luting agent for indirect restorations, fur-
ther studies could confirm the long-term
benefits of this material. Longitudinal
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THE INTERNATIONAL JOURNAL OF ESTHETIC DENTISTRY
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 Clinical Research
clinical studies might show whether
composite resins can perform better
than resin cements, mainly in terms of
marginal defects.
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VOLUME 13 • NUMBER 1 • Spring 2018