Ó

Operative Dentistry, 2012, 37-1, 28-36

Reparability of Aged
Silorane With
Methacrylate-Based Resin
Composite: Micro-Shear
Bond Strength and
Scanning Electron
Microscopy Evaluation
L Giachetti  D Scaminaci Russo  M Baldini
C Goracci  M Ferrari

Clinical Relevance
Aged silorane composite restorations can be repaired with a methacrylate-based resin
composite by using a phosphate-methacrylate–based adhesive as the intermediate layer.

*Luca Giachetti, MD, DMD, MSc, Tuscany School of Dental

Medicine, University of Florence and Siena, Italy, Depart- SUMMARY
ment of Public Health, Dentistry, University of Florence
Daniele Scaminaci Russo, DDS, Tuscany School of Dental
Objectives: To evaluate the compatibility be-
Medicine, University of Florence and Siena, Italy, Depart- tween aged siloranes and methacrylate-based
ment of Public Health, Dentistry, University of Florence composites by simulating a common repair-
Matteo Baldini, DDS, Tuscany School of Dental Medicine, technique.
University of Florence and Siena, Italy, Department of Public Methods: Twenty substrates were constructed
Health, Dentistry, University of Florence using silorane (Filtek Silorane, 3M ESPE) and
Cecilia Goracci, DDS, MSc, PhD, Tuscany School of Dental methacrylate composites (Filtek Supreme XT,
Medicine, University of Florence and Siena, Italy, Depart- 3M ESPE). Substrates were aged in 0.9% NaCl
ment of Dental Materials and Fixed Prosthodontics, Univer-
solution at 378C for 72 hours. Silorane build-
sity of Siena
ups were constructed on silorane substrates
Marco Ferrari, MD, DMD, PhD, Tuscany School of Dental without any intermediate layer (IL). Methac-
Medicine, University of Florence and Siena, Italy, Depart-
rylate build-ups were constructed on silorane
ment of Dental Materials and Fixed Prosthodontics, Univer-
sity of Siena substrates without any IL, with a methacrylate
IL (Heliobond, Ivoclar Vivadent), or with a
* Corresponding author: Viale Morgagni 85, Firenze, 50134
Italy; e-mail: luca.giachetti@unifi.it phosphate-methacrylate IL (Silorane System
Adhesive Bond, 3M ESPE). Methacrylate build-
DOI: 10.2341/10-397-L
ups were also constructed on methacrylate
Giachetti & Others: Repairing of Aged Silorane-Based Composites 29

substrates without any IL. The micro-shear ly lower polymerization stress. In addition, more
bond strength test was carried out after ther- esthetically satisfactory results could be achieved by
mocycling. Bond strength data were statisti- using methacrylate composite resin as an enamel
cally analyzed using analysis of variance and restorative. According to the literature,11,12 in order
Tukey post hoc tests. Failure modes were to stratify a methacrylate composite on a silorane
assessed by means of scanning electron mi- composite, the use of a phosphate-methacrylate–
croscopy observations. based intermediate resin such as the second compo-
Results: The silorane-methacrylate group nent (Bond) of the Silorane Adhesive System (3M
without any IL showed the lowest bond ESPE) is required. The application of this hydropho-
strength values (0.4 6 0.1 MPa). The use of a bic resin coating promotes bonding not only to
methacrylate-based IL (1.6 6 1.7 MPa) led to a silorane-based composites but also to methacrylate-
slight increase in bond strength, whereas the based materials.13 The phosphate group reacts with
use of phosphate-methacrylate IL (9.1 6 5.4 oxirane, whereas the acrylate group reacts with
MPa) significantly increased bond strength. dimethacrylate, thus resulting in the adhesion be-
There was no statistically significant differ- tween the two composites.11 Tezvergil-Mutluay11 also
ence in bond strength between silorane-silor- demonstrated that the bond strength between con-
ane (7.9 6 3.6 MPa) and methacrylate- secutive layers of silorane composite decreased when
methacrylate (9.5 6 4.1 MPa) groups without the time of placement between consecutive layers
any IL. increased. This suggests that as the chemical reac-
tivity decays over time,14 the bond strength could be
INTRODUCTION affected. Consequently, another clinically interesting
point to consider is the possibility of repairing an aged
The use of composite resin restorative materials has silorane restoration with a conventional methacrylate
been widely accepted in dental practice.1 However, composite system. According to the manufacturer,
although methacrylate-based composites exhibit silorane restorations can be repaired with a conven-
acceptable clinical performance, polymerization tional methacrylate composite system using a dime-
shrinkage is still a drawback.2 Polymerization
thacrylate-based intermediate layer. On the other
shrinkage results in volumetric contraction, causing
hand, according to the literature,11,12 the use of a
stress in bonded restorations that can lead to clinical
phosphate-methacrylate–based adhesive as an inter-
failure.3-7 Recently, a new category of polymers for
mediate layer could be more appropriate. However,
dental-restorative use was introduced: silorane-
the studies by Tezvergil-Mutluay and others11 and
based composites. Polymerization of silorane-based
Lührs and others12 were conducted on fresh sub-
composites occurs through a photocationic ring-
strates, while it has not yet been determined whether
opening reaction, which results in a lower polymer-
a phosphate-methacrylate–based adhesive should
ization contraction compared with the free radical
also be applied as an intermediate layer on aged
polymerization of dimethacrylate monomers.8,9 The
silorane composite restorations.
volumetric shrinkage of the silorane composite was
determined to be 0.9%, which is clearly the lowest Using the micro-shear bond strength test (lSBS)
value observed for the investigated materials.9 This and scanning electron microscopy (SEM), the aim of
is in good agreement with stress measurements by this study was to evaluate the ability of silorane- and
Ernst and others,10 showing the lowest stress methacrylate-based aged composites to be repaired
development for siloranes among all tested compos- and to examine the compatibility between siloranes
ite materials. and methacrylate-based composites by simulating a
common repair technique. The tested null hypothe-
According to the manufacturer of Filtek Silorane
ses were 1) there is no difference in bond strength
(3M ESPE, St Paul, MN, USA), which is the only
between silorane-silorane, methacrylate-methacry-
silorane-based marketed composite, silorane compos-
late, and silorane-methacrylate combinations, and 2)
ite resin can be used for direct class I and class II
similar bond strength develops between silorane-
restorations and as a base under a methacrylate-
based and methacrylate-based composites regardless
based composite. In fact, siloranes can have an
of the application of an intermediate bonding layer.
important role as a base under methacrylate compos-
ite resin in what is commonly referred to as a
MATERIALS AND METHODS
sandwich restoration. By replacing part of the
methacrylate composite with silorane composite, it The materials used in this study are listed in Table
is possible to obtain lower shrinkage and consequent- 1. A silorane composite (Filtek Silorane, A3 shade,
30 Operative Dentistry

Table 1: Chemical Composition and Batch Numbers of the Tested Materials

Materials Manufacturer Batch No. Material Composition

Filtek Silorane 3M, ESPE 7AU 1,3,5,7-Tetrakis (ethyl cyclohexane epoxy)

1,3,5,7-tetramethyl cyclotetrasiloxanemethyl-bis[2-(7-
oxabicyclo[4.1.0]hept-3-yl)ethyl]phenyl

Filtek Supreme 3M, ESPE 6FK bis-GMA, Bis-EMA, TEGDMA, UDMA

Silorane System 3M, ESPE 7AJ TEGDMA, Phosphoric acid methacryloxyhexylesters, 1,6-hexanediol
Adhesive Bond dimethacrylate

Heliobond Vivadent-Ivoclar 405316 bis-GMA, TEGDMA

Abbreviations: bis-EMA, bisphenol A polyethylene glycol diether dimethacrylate; bisGMA, bisphenol A-glycidyl dimethacrylate; TEGDMA, triethylene glycol
dimethacrylate; UDMA, urethane dimethacrylate.

3M ESPE, St Paul, MN, USA) and a methacrylate Hanau, Germany) in order to allow for repeatable
composite (Filtek Supreme XT, A3B shade, 3M placement of the disk during the mechanical test.
ESPE) were used as substrate and adherent mate- Substrates were aged in 0.9% NaCl solution in a
rials. As a substrate material, silorane was used in light-proof container at 378C for 72 hours and then
groups 1 to 4, whereas a methacrylate-based com- randomly divided into five groups (n=4) according to
posite was used as a substrate in group 5 (Table 2). the used method of substrate preparation (Table 2).
The substrates were fabricated by placing unpoly- One of the two surfaces of each disk was roughened
merized composite between two glass microscope for five seconds with P600-grit abrasive paper (WS
slides. The material was then light polymerized for Flex 18 C, Hermes Abrasives Ltd, Virginia Beach,
30 seconds with a light-curing device (Astralis 10, VA, USA) under running water using a lapping
High Power Program 1200 mW/cm2, Vivadent- machine (LS2, Remet, Bologna, Italy). Silorane
Ivoclar, Schaan, Liechtenstein). Thus, disks of about build-ups were constructed on silorane substrates
15 mm in diameter and 1 mm in thickness were without any intermediate layer (IL; group 1).
obtained. A 2-mm-diameter hole was produced near Methacrylate build-ups were constructed on silorane
the margin of the disk using a hand piece and a substrates without any IL (group 2), with a methac-
parallelometer (CL-MF2002S, Heraeus-Kulzer Inc, rylate IL (Heliobond, Ivoclar Vivadent; group 3) or

Table 2: Descriptive Statistics of Micro-Shear Bond Strength and Distribution of Failure Modesa

Number Bond Strength Fracture Mode

Intermediate of Tested (MPa)
Group Substrate Layer Build-up Specimens Mean 6 SD Adhesive Cohesive Mixed

1 F.Silorane / F.Silorane 27 7.9 6 3.6a 12 (44%) 15 (56%) —

2 F.Silorane / F.Supreme 4 0.4 6 0.1b 4 (100%) — —

3 F.Silorane Heliobond F.Supreme 25 1.6 6 1.7b 25 (100%) — —

4 F.Silorane Silorane System F.Supreme 30 9.1 6 5.4a 19 (63%) 6 (20%) 5 (17%)

Adhesive Bond

5 F.Supreme / F.Supreme 27 9.5 6 4.1a 5 (18%) 22 (82%) —

a
In the Bond Strength column, different superscript letters label statistically significant between-group differences (p,0.05).
Giachetti & Others: Repairing of Aged Silorane-Based Composites 31

The methacrylate IL and the silorane IL were

applied to one surface of each disk by means of a
micro brush, thinned with a light air stream, and
light polymerized for 20 seconds.
The build-ups were constructed using a custom-
made device (Figure 1), consisting of two parallel
metal plates that could be joined by means of four
screws. The upper plate had nine holes. Each hole
was made of two sections: a lower section (1.7 mm in
diameter) and an upper section (1.45 mm in
diameter). Nine silicone tubules having an internal
diameter of 0.7 mm, an external diameter of 1.7 mm,
and a height of 0.5 mm were custom made from a
silicone tube (art.30/07; Stonfo, Florence, Italy). The
tubules were embedded into the holes of the lower
section. Each resin substrate was placed between the
two plates, which were then joined together with the
four screws. The silicone tubules were then filled
with the resin composite, which was subsequently
light cured for 20 seconds. After opening the device,
the silicone tubules were easily removed from the
build-up (Figure 2). The built-up specimens were
stored in 0.9% NaCl solution in a light-proof
container at 378C for 24 hours and then thermo-
cycled (1500 cycles between 58C and 558C; 10-second
dwell time in each 0.9% NaCl bath; LTC, LAM
Technologies, Firenze, Italy). The specimens were
observed under a stereomicroscope (403 magnifica-
tion; SMZ-10, Nikon Corporation) to verify integrity
at the build-up/substrate interface. Build-ups that
showed apparent interfacial gap formation, bubble
inclusion, or any other relevant defect were excluded
from the study.
Specimens were subjected to a lSBS test using a
universal testing machine (LMT-100, LAM Technol-
ogies). The specimen was placed on the testing
machine by positioning the hole in the specimen
around a pin on the moving part of the machine. The
hole could freely rotate around the pin. A thin
stainless-steel wire (diameter = 0.20 mm) was looped
around a pin on the stationary part of the machine as
well as around the resin build-up. The wire contact-
ed half the circumference of the build-up and was
gently held flush against the disk at the build-up–
Figure 1. Metal device for specimen construction. Silicone tubules substrate interface. Thus, the wire loop exerted
(blank arrow) were embedded into the lower sections of the holes. A
resin composite disc (asterisk) was placed between the two plates, shear forces parallel to the bonded interface, at a
which were then joined together with four screws (black arrow). crosshead speed of 1 mm/min until failure occurred.
The lSBS was expressed in MPa by dividing the load
with a phosphate-methacrylate IL (Silorane System at failure (N) by the surface area (mm2).
Adhesive Bond; group 4). Methacrylate build-ups
were also constructed on methacrylate substrates Statistical Analysis of lSBS Data
without any IL (group 5). The latter group was As the data distribution was normal in each group
tested as a control. (Kolmogorov–Smirnov test) and group variances
32 Operative Dentistry

Figure 2. A schematic representation of a specimen showing the

hole near the margin of the resin composite disc (asterisk) and resin
Figure 3. The means and standard deviations of micro-shear bond
composite build-ups (blank arrow).
strengths in different groups. Group 1: Silorane þ Silorane. Group 2:
Silorane þ Supreme. Group 3: Silorane þ Heliobond þ Supreme.
were homogeneous (Levene test), the one-way anal- Group 4: Silorane þ Silorane System Adhesive Bond þ Supreme.
Group 5: Supreme þ Supreme.
ysis of variance (ANOVA) was applied, followed by
the Tukey test for post hoc comparison. Between-
group differences in the distribution of failure modes defects at the adhesive interface and were discarded.
were statistically assessed using chi-square tests. In Nineteen build-ups from group 2 and eight build-ups
all the analyses, the level of significance was set at from group 3 failed during thermocycling. Conse-
p,0.05 (SigmaStat 3.5 Statistical Software package, quently, 127 build-ups (27 build-ups from group 1,
Systat Software Inc, San Jose, CA, USA). four build-ups from group 2, 25 build-ups from group
3, 30 build-ups from group 4, and 27 build-ups from
Specimen Preparation for SEM Observation group 5) were subjected to lSBS testing.
Following the lSBS test, the substrates and the
debonded build-ups were prepared for SEM analysis. lSBS Test
The specimens were mounted on aluminum stubs Descriptive statistics of lSBS are reported in Table 2
with colloidal silver paint and sputter coated (SCD and Figure 3 along with statistically significant
005, BAL-TEC AG, Balzers, Liechtenstein) with 200- between-group differences. Measured bond
Å gold-palladium alloy (Foil Target AU, BAL-TEC
strengths were (mean 6 standard deviation) 7.9 6
AG). To determine the mode of failure, each
3.6 MPa for group 1, 0.4 6 0.1 MPa for group 2, 1.6
specimen was observed under the SEM (Philips
6 1.7 MPa for group 3, 9.1 6 5.4 MPa for group 4,
515, Philips Co, Amsterdam, The Netherlands; 15-
and 9.5 6 4.1 MPa for group 5. The one-way ANOVA
KV accelerating voltage) at 1003 magnification.
showed that groups differed significantly (p,0.001).
Images were acquired by means of a computerized
In particular, the post hoc test revealed that the
program (Analysis 2.1, Soft Imaging System GmbH,
bond strengths measured in groups 1, 4, and 5 were
Munster, Germany).
significantly higher than those recorded in groups 2
and 3.
RESULTS
This study involved the preparation of nine build- SEM Observation
ups on each substrate. Of 180 build-ups, 4 from
SEM observation showed different fracture patterns
group 1, seven from group 2, three from group 4, and
among the groups (Figure 4).
three from group 5 either prematurely failed or
accidentally detached from their base after opening All specimens of groups 2 and 3 failed adhesively.
the device. Under stereomicroscope observation, five Both adhesive (44%) and cohesive (56%) failures
build-ups from group 1, six build-ups from group 2, were noticed in group 1, while failures were mostly
three build-ups from group 3, three build-ups from adhesive (63%) in group 4 and mainly cohesive in
group 4, and six build-ups from group 5 showed group 5 (82%).
Giachetti & Others: Repairing of Aged Silorane-Based Composites 33

methacrylate-based composite by simulating a com-

mon repair technique. Based on the study’s findings,
the first null hypothesis has to be rejected. As a
matter of fact, the silorane-methacrylate group
without any intermediate layer (group 2) exhibited
significantly lower bond strengths than those re-
corded by the silorane-silorane and the methacry-
late-methacrylate groups without adhesive layer
(groups 1 and 5, respectively). Also, in group 2, the
highest number of failures during thermocycling was
recorded, and all the tested specimens failed adhe-
sively at the silorane-methacrylate interface. No
statistically significant difference in bond strength
emerged between silorane-silorane (group 1) and
methacrylate-methacrylate (group 5) groups. How-
ever, the two groups exhibited significantly different
failure patterns. Specifically, group 5 had a predom-
inance of cohesive failures. Also, the second formu-
lated null hypothesis has to be rejected because the
use of the phosphate-methacrylate–based adhesive
as IL (group 4) significantly increased the bond
strength. Statistically similar adhesion levels were
instead obtained either with or without the applica-
tion of a methacrylate-based IL (groups 3 and 2,
respectively). The application of the phosphate-
methacrylate–based IL also had an influence on
specimen failure mode. It was indeed only with the
interposition of this bonding material that mixed
and cohesive failures occurred in silorane-methacry-
late combinations. Therefore, according to the re-
sults of this study, the application of the phosphate-
methacrylate–based adhesive as IL is beneficial
when repairing an aged silorane-based composite
with a conventional methacrylate-based composite.
The ring-opening reaction of the silorane is a
cationic polymerization reaction, and no oxygen
inhibition occurs on the polymerized surface.11
Therefore, the bond between consecutive layers
Figure 4. Scanning electron microscopy microphotographs of the depends on the reactivity of the material.11 Chemical
debonded surface of tested substrates (1003). (A): Adhesive failure in reactivity is known to decrease over time.14 As a
a silorane-silorane specimen (group 1). (B): Cohesive fracture of a
methacrylate build–up, which was constructed on a methacrylate result, the time interval between placement of
substrate (group 5). (C): Mixed fracture of a silorane build-up created consecutive silorane layers must not be overly long.
on a methacrylate substrate with the interposition of a phosphate- A five-minute delay between layers results in
methacrylate intermediate layer (group 4).
significantly decreased bond strengths and increased
percentage of adhesive failures.11 However, the
The differences in failure mode distribution were
results of this study showed that the bond strength
statistically significant, with the exception of the
of an additional layer of silorane composite added to
comparison between groups 2 and 3, both of which
an aged silorane substrate is comparable to the bond
exhibited exclusively adhesive failures.
strength of a layer of methacrylate composite added
to an aged methacrylate resin substrate. On the
DISCUSSION
other hand, the fact that the specimens in group 2
This study was designed to evaluate the ability of an showed the lowest bond strength and the highest
aged silorane-based composite to be repaired with number of premature failures, when compared with
34 Operative Dentistry

the other groups, suggests that there is no chemical base of the cylinder. Consequently, to avoid such
compatibility between the aged silorane substrate inconvenience, samples were prepared by means of
and the added methacrylate resin composite. How- an especially designed, custom-made device. The
ever, the use of Silorane System Adhesive Bond as lower bond strength measured in this study can be
an intermediate layer between the aged silorane attributed to this newly devised method of sample
composite and a methacrylate composite led to a preparation. In this study, the lSBS test was
significant increase in bond strength. Silorane IL is preferred to the microtensile test as it allowed easier
based on methacrylate chemistry with the addition quantification of the number of specimens that
of phosphate groups. The reaction of the phosphate prematurely failed or accidentally detached during
group with oxirane and of the acrylate group with preparation. The number of prematurely failed,
dimethacrylate might account for the recorded discarded specimens in each test is probably related
increase in bond strength.11 to the aggressiveness of the preparation proce-
dure.35 The cutting procedure that is carried out
Numerous repair modalities have been evaluated
during the microtensile test transmits vibrations to
in vitro for conventional methacrylate-based com-
the specimens. Consequently, a common occurrence,
posites.15-19 The treatment of methacrylate compos-
especially if the bond strengths are relatively low
ite surfaces with a methacrylate bonding agent can
(5–7 MPa),36 is a premature failure of the specimen,
be regarded as a standard procedure in today’s
which makes microtensile useless. 37-39 In this
dentistry. On the other hand, this study demon-
regard, because of the weak bond strength between
strated that the application of a methacrylate-based
silorane-based and methacrylate-based resin com-
IL is not beneficial when repairing an aged silorane-
posites, the micro-shear test was preferred to
based composite with a conventional methacrylate-
microtensile as it did not require cutting after
based composite. Therefore, it can be hypothesized
bonding, which avoided any additional stress on
that the repair modality for a silorane-based com-
specimens.
posite is different from that of a methacrylate-based
resin composite. However, in clinical practice, the
CONCLUSION
operator is blind to the type of composite resin that
was originally used to restore the tooth. According to A reliable bond between aged silorane composite and
the literature,20 Silorane System Adhesive can also methacrylate composite was obtained by using a
be used to bond conventional methacrylate-based phosphate-methacrylate–based adhesive as an in-
composites to dentin. However, the application of the termediate layer. The interfacial bond strength
Silorane System Adhesive Bond as an intermediate achieved when repairing aged silorane with silorane
layer when repairing an aged methacrylate-based was similar to that obtained by repairing aged
composite with a fresh methacrylate-based compos- methacrylate-based composite with methacrylate-
ite has not yet been tested. Further research should based composite.
be carried out to allow clinicians to use Silorane
System Adhesive Bond as an IL in reparations (Accepted 26 July 2011)
regardless of the type of composite used in the
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