d e n t a l m a t e r i a l s 2 8 ( 2 0 1 2 ) e19–e25

Available online at www.sciencedirect.com

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

Repair of silorane composite—Using the same substrate or a

methacrylate-based composite?

Annette Wiegand a,∗ , Bogna Stawarczyk b , Wolfgang Buchalla a , Tobias T. Tauböck a ,

Mutlu Özcan b , Thomas Attin a
aClinic for Preventive Dentistry, Periodontology and Cariology, University of Zurich, Plattenstrasse 11, CH-8032 Zurich, Switzerland
bClinic for Fixed and Removable Prosthodontics and Dental Materials Science, University of Zurich, Plattenstrasse 11, CH-8032 Zurich,
Switzerland

a r t i c l e i n f o a b s t r a c t

Article history: Objective. The study aimed to analyze the shear bond strength of aged silorane composite
Received 21 March 2011 repaired with the same substrate or a conventional methacrylate-based composite after
Received in revised form different mechanical and adhesive surface treatments.
23 June 2011 Methods. Silorane composite specimens were aged by thermal cycling (5000 cycles, 5–55 ◦ C)
Accepted 4 October 2011 and randomly assigned to different surface treatments (each group n = 16): diamond bur
abrasion, aluminum oxide sandblasting, silica coating, or hydrofluoric acid etching. Then,
an adhesive system corresponding to the repair composite or a combination of silane agent
Keywords: and the respective adhesive was applied. Silorane composite or a nanofiller composite were
Silorane adhered onto the conditioned surfaces. In the control group (n = 16), silorane composite was
Repair adhered to fresh substrate (incremental build up). After further thermal cycling, shear bond
Silane strength was tested and failure modes were assessed. Data were analyzed by ANOVA/post
Adhesive hoc tests, Weibull statistics and Chi2 -test (p ≤ 0.05).
Composite Results. Incremental shear bond strength (control group: 21.0 ± 10.5 MPa) was achieved by
Shear bond strength all groups except those etched with hydrofluoric acid or samples abraded with diamond
Failure bur and repaired with the nanofiller composite without silane application. Generally, the
application of the silane agent improved repair bond strength of the nanofiller but not of
the silorane composite. Cohesive failure was observed more frequently than adhesive failure
when the silane agent was applied or when silorane composite was used for repair.
Significance. Silorane composite can be repaired with either the same substrate or a
methacrylate-based nanofiller composite but requires mechanical surface treatment and
– in case of the methacrylate-based composite – silanization prior to adhesive application.
© 2011 Academy of Dental Materials. Published by Elsevier Ltd. All rights reserved.

composites. Silorane composites were shown to overcome

1. Introduction this problem to a certain extent as they are undergoing a
photocationic ring-opening polymerization instead of a rad-
Polymerization shrinkage is considered as one of the ical polymerization reaction, which results in polymerization
main shortcomings of conventional methacrylate-based shrinkage below 1% and a decrease of shrinkage stress by

∗
Corresponding author. Tel.: +41 44 6343412; fax: +41 44 6344308.
E-mail address: annette.wiegand@zzm.uzh.ch (A. Wiegand).
0109-5641/$ – see front matter © 2011 Academy of Dental Materials. Published by Elsevier Ltd. All rights reserved.
doi:10.1016/j.dental.2011.10.008
e20 d e n t a l m a t e r i a l s 2 8 ( 2 0 1 2 ) e19–e25
27% compared to methacrylate-based composites [1,2]. Fur-
thermore, silorane composites were shown to present an
increased hydrophobicity, which reduces water uptake and
enhances hydrolytic stability [3,4]. As silorane composites
were marketed quite recently, information about their clinical
performance is scarce and limited to one study with an obser-
vation period of 12 months. In this study, it was hypothesized
that reduced polymerization stress would improve marginal
performance, but marginal adaptation of silorane class II
restorations was inferior compared to a methacrylate-based
material [5].
In vitro studies showed that physical properties, such as
flexural strength, dynamic and static moduli of elasticity,
hardness [6,7] and wear resistance [8,9] of silorane composites
are in the range of conventional methacrylate-based compos-
ites. Thus, longevity of silorane composite restorations might
also be affected by mechanical or chemical degradation pro-
cesses leading to clinical failures in the form of chipping, wear,
discoloration or secondary caries, and requiring further oper-
ative treatment.
For the last years, it was shown that new techniques and
materials in adhesive dentistry allow the repair of pre-existing
restorations instead of their complete replacement [10,11].
This approach is considered as conservative and cost-reducing
method as the intact part of the restoration can be main-
tained and unnecessary removal of dental hard tissues and
repeated irritations or injuries to the pulp can be avoided [12].
The repairability of silorane composites was analyzed recently
in several in vitro studies [13–18], but only few studies tested
the ability of methacrylate-based composites to repair silo-
rane restorations [14–16]. These studies investigated either the
effect of the adhesive intermediate agent [14,15] or the impact
of surface preparation [16] on silorane repair. A systematic
investigation combining both different surface pretreatments
(mechanical and chemical) and different adhesive condition-
ing methods (adhesive, silane agent) was not done so far.
Thus, the objective of the present in vitro study was to
evaluate the effect of various combinations of surface pre-
treatments and adhesive conditioning methods on shear bond
strength of aged silorane repairs in order to determine the
optimum repair method when either the same substrate or
a conventional methacrylate-based composite is used. The
null hypotheses tested were (1) the type of surface pretreat-
ment does not affect shear bond strength, (2) the use of silane
does not affect shear bond strength and (3) the kind of adhe-
sive/repair composite does not influence shear bond strength.
2. Materials and methods
2.1. Specimens preparation
Silorane specimens (n = 272, Ø 6 mm × 3 mm) were fabricated
by placing one increment of silorane composite (FiltekTM
Silorane, 3M ESPE, Rüschlikon, Switzerland, shade A2, lot:
N136324) into cylindrical cavities (diameter: 6 mm, height:
3 mm) of stainless steel hollow cylinders. The surface
was leveled using a PTFE roller (CompoRollerTM 5300, Ker-
rHawe, Bioggio, Switzerland) to achieve a flat surface [19].
Photo-polymerization (bluephase, Ivoclar Vivadent, Schaan,
Liechtenstein) was performed for 40 s at a distance of 2 mm to
the surface. Light intensity was higher than 800 mW/cm2 , as
verified by a radiometer (Optilux Model 100, SDS Kerr Danbury,
USA) after every 32 specimens.
Specimens from the control group were immediately pro-
cessed further within 5 min after polymerization [18,19] while
all other groups were aged by thermal cycling prior to treat-
ment (5000 cycles, 5–55 ◦ C, dwell time: 20 s, transfer time: 10 s).
Thermocycled specimens were randomly assigned to one of
the surface conditioning methods.
2.2. Surface conditioning
After thermal cycling, each four silorane composite groups
were conditioned as follows:
• Hydrofluoric acid etching: The aged silorane composite
surface was etched with 5% hydrocfluoric acid gel (Vita
Ceramics Etch, Vita Zahnfabrik, Bad Säckingen, Germany,
lot: 22810) for 2 min, washed for 30 s and air dried.
• Abrasion with diamond bur: The aged silorane compos-
ite surface was roughened with a cylindrical diamond bur
(40 ␮m grit, 4325L, Intensiv, Grancia, Switzerland). Stan-
dardized roughening was ensured by attaching the hand
piece to an apparatus maintaining load and height during
preparation. The hand piece was applied with 100 g load
[20] under water cooling, and the rotation rate amounted
to 40,000 rpm. Diamond bur abrasion resulted in ∼0.1 mm
removal of the silorane composite surface. The bur was
replaced after each 16 specimens.
• Sandblasting with aluminum oxide: The aged silorane com-
posite surface was sandblasted perpendicular to the surface
for 4 s with 50 ␮m aluminum oxide particles (Renfert, Hilzin-
gen, Germany, lot: 1178646) at a distance of 10 mm and
2.8 bar air pressure. Remnants of sandblasting were air
blown.
• Silica coating: The aged silorane composite surface was
sandblasted perpendicular to the surface for 4 s with 30 ␮m
silica-coated aluminum oxide (CoJet, 3M ESPE, Seefeld,
Germany, lot: 412272) at a distance of 10 mm. Loose particles
were air blown.
After surface pretreatment, the specimens were condi-
tioned with the adhesive specific for the matrix of the
repair composite. Prior to the application of the adhesive,
a silane coupling agent (Monobond Plus, Ivoclar Vivadent,
lot: N45336) was applied in half of the groups and allowed
to evaporate for 60 s as recommended by the manufacturer.
The specimens to be repaired with the Silorane compos-
ite were conditioned with a filled (silane treated silica,
5–10 wt%), phosphate-dimethacrylate-based adhesive (Filtek
Silorane Adhesive Bond, 3M ESPE, lot: N141785), while the
specimens to be repaired with the nanofiller composite were
conditioned with an unfilled, conventional methacrylate-
based bonding material (Heliobond, Ivoclar-Vivadent, L49864).
The adhesives were applied with a microbrush for 20 s, gently
air-thinned and light-polymerized for 20 s. The whole sur-
face of the principle substrate was conditioned for repair
(28.6 mm2 ).
 d e n t a l m a t e r i a l s 2 8 ( 2 0 1 2 ) e19–e25 e21

MPa
35
Heliobond + Filtek supreme XTE

30 Filtek Silorane Bond + Filtek Silorane

S

25
°
20
S

15
*
10 * ,S
*
*,°
*
5

0
- + Silane - + Silane - + Silane - + Silane

Hydrofluoric acid Bur Al2O3 sandblasting Silica coating

Fig. 1 – Shear bond strength in the different groups. Mean shear bond strength (MPa, standard deviation) of the repair
composites to aged silorane composite after different surface treatments. Groups being significantly different from the
control group (incremental bond strength 21.0 (10.5) MPa) were marked by *. Values were marked with S when the
application of the silane agent increased shear bond strength significantly compared to the respective groups without silane
application. Filtek Silorane Adhesive Bond/Filtek Silorane revealed significantly higher shear bond strength values (marked
by ◦ ) than Heliobond/Filtek Supreme XT when surface treatment was performed with bur or hydrofluoric acid without
additional application of the silane agent.

2.3. Repair composite application
Silorane composite (shade C2, lot: N136714) and a nanofiller
composite (Filtek Supreme XTE, 3M ESPE, shade C2, lot:
N137774) were used as repair composites. The repair compos-
ites were adhered onto the silorane substrate using stainless
steel hollow cylinders (inner diameter: 3 mm, height: 4 mm).
The composite was packed against the surface in a 2.5 mm
thick increment and light cured for 40 s from a distance of
2 mm. In the control group, the silorane composite increment
was adhered onto fresh substrate in the same way. Bonding
procedures were carried out by the same operator throughout
the experiments.
All test groups (each n = 16) and the control group (n = 16)
were then submitted to an additional thermal cycling proce-
dure (5000 cycles, between 5–55 ◦ C, dwell time: 20 s, transfer
time: 10 s).
2.4. Shear bond strengths and failure analysis
Bond strength was tested with a universal testing machine
(Z010, Zwick, Ulm, Germany). A shear force was applied to the
adhesive interface through a chisel-shaped loading device at
a crosshead speed of 1 mm/min parallel to the surface of the
principle silorane composite. Load at debonding was recorded
and shear bond strength  was calculated using the load at
failure F (N) and the adhesive area A (mm2 ):  = F/A.
The debonded area was examined for failure mode analy-
sis with a stereomicroscope at 25× magnification (M3B, Wild,
Heerbrugg, Switzerland). Failure mode was considered as
adhesive if it occurred at the interface and as cohesive if the
failure affected at least parts of the substrate or the repair
composite.
2.5. Statistical analysis
Shear bond strength (MPa) data were analyzed by three-way
ANOVA, factors being the kind of surface pretreatment, the use
of silane and the kind of adhesive/repair composite, respec-
tively (SPSS Version 19, SPSS Inc., Chicago, IL, USA). Significant
differences between the surface treatments were analyzed
by one-way ANOVA and Scheffe’s post hoc tests, while two
sample t-tests were used to determine significant differences
between samples treated or not with the silane agent and
between both adhesives/repair composites. One-way ANOVA
followed by Dunnett’s post hoc tests was used to detect signif-
icant differences between the repaired groups and the control
group (incremental shear bond strength).
The Weibull distribution parameters (Weibull modulus m,
characteristic bond strength  o ) were calculated using the
maximum likelihood estimation method at 95% confidence
level (MINITAB, State College, PA, USA).
Effects of the kind of surface treatment, the use of silane
and the kind of adhesive/repair composite on failure mode
e22 d e n t a l m a t e r i a l s 2 8 ( 2 0 1 2 ) e19–e25

were analyzed with Chi2 test (binary variable: cohesive fail-

Table 1 – Weibull parameters. Characteristic strength  o (MPa) and Weibull modulus m the different test groups. Values in the control group amounted to  o = 23.8 and
ure). Overall level of significance was set at p ≤ 0.05.

3. Results

21.6 (16.2; 28.7) 20.6 (15.0; 28.2)

Silica coating

27.8 (22.4; 34.5) 13.2 (9.7; 17.8)

1.7 (1.2; 2.5)

1.7 (1.1; 2.5)

Surface pretreatment, the use of silane and the kind of adhe-
sive/repair composite showed a significant effect on shear
bond strength (three-way ANOVA). Significant interactions

+ silane agent
were detected between the surface pretreatment and the

2.4 (1.5; 3.7)

1.8 (1.2; 2.7)

adhesive/repair composite (p = 0.013) and between the use of
silane and the adhesive/repair composite (p = 0.005). No signif-
icant interactions were found between surface pretreatment
and the use of silane (p = 0.192) and when all factors were taken
into consideration (p = 0.246).
Shear bond strength values (MPa, mean ± standard devia-
tion) of the differently repaired groups are presented in Fig. 1.

Al2 O3 sandblasting

17.3 (10.8; 27.6)

17.4 (13.0; 23.2) 18.6 (12.9; 27.0)

−
Incremental shear bond of silorane (control) amounted to

1.1 (0.6; 1.7)

1.4 (0.9; 2.1)

21.0 ± 10.5 MPa. Compared to the control group, all groups
etched with hydrofluoric acid and samples treated with bur
abrasion and repaired with the nanofiller composite with-

+ silane agent
out additional silane application revealed significantly lower

Surface treatment

15.8 (7.2; 34.4)

shear bond strength values.

0.6 (0.4; 1.1)

1.8 (1.2; 2.7)

Generally, groups etched with hydrofluoric acid showed
the lowest shear bond strength. The application of the silane
agent improved bond strength in samples repaired with the
nanofiller composite (except after Al2 O3 sandblasting), but not
in specimens repaired with silorane composite. Regarding the
effect of the adhesive/repair composite, significantly higher

Hydrofluoric acid

3.6 (2.2; 5.8)

1.1 (0.6; 1.7)

7.0 (5.1; 9.7)

1.7 (1.1; 2.5)
shear bond values of Filtek Silorane Adhesive Bond/Filtek Silo-
rane compared to Heliobond/Filtek Supreme XTE could be
found only in groups that were etched with hydrofluoric acid
or pretreated with a bur without application of silane.
+ silane agent

The parameters of the Weibull distributions and their 95%

9.4 (6.9; 12.7)

7.6 (6.2; 9.3)
2.6 (1.7; 4.0)

1.7 (1.1; 2.6)

confidence intervals are presented in Table 1. Characteristic
strength  o amounted from 3.6 to 27.8 MPa and was lowest
in the groups etched with hydrofluoric acid and in samples
treated with bur abrasion and repaired with the nanofiller
composite without silane application. Weibull modulus m
ranged from 0.5 to 2.9 and was similar for all groups except
20.9 (16.7; 26.3) 22.2 19.0; 26.9)
16.5 (12.1; 22.6) 4.3 (1.4; 12.3)

samples repaired with the nanofiller composite after pretreat-

−

0.5 (0.3; 0.8)

2.9 (1.9; 4.5)

ment with the bur (m = 0.5) or after sandblasting with silane

application (m = 0.6).
Bur

In Table 2, failure types in the different groups are pre-

+ silane agent

sented. Cohesive failures were observed more frequently

when the silane agent was used prior to adhesive application
1.7 (1.1; 2.5)

2.3 (1.5; 3.5)

Filtek Silorane Adhesive Bond + Filtek Silorane

or when the samples were repaired with silorane composite

and its corresponding bonding agent, while no significant dif-
ferences in failure type were detected between the different
Adhesive and repair composite

surface treatments.
Heliobond + Filtek supreme XTE

4. Discussion

This study aimed to compare different methods to repair

silorane composite using either the same substrate or a con-
ventional methacrylate-based composite. The latter is of high
clinical relevance as dentists often do not know if the compos-
m = 2.2.

ite to be repaired is a silorane- or methacrylate-based material

o

o
m

and may use a methacrylate-based composite as standard

material in the everyday situation.
 d e n t a l m a t e r i a l s 2 8 ( 2 0 1 2 ) e19–e25 e23

Table 2 – Failure types in the different groups. Failure types of the differently repaired silorane composite and the control
group.
Surface treatment Silane agent Adhesive + composite Failure mode

Cohesive Adhesive Mixed Total

+ Filtek Silorane Adhesive Bond + Filtek Silorane 15 1 0 16
− 10 3 3 16
Bur
+ Heliobond + Filtek supreme XTE 3 10 3 16
− 1 14 1 16

+ Filtek Silorane Adhesive Bond + Filtek Silorane 8 7 1 16

− 5 11 0 16
Hydrochloric acid
+ Heliobond + Filtek supreme XTE 14 2 0 16
− 0 16 0 16

+ Filtek Silorane Adhesive Bond + Filtek Silorane 8 3 5 16

− 6 7 3 16
Al2 CO3 sandblasting
+ Heliobond + Filtek supreme XTE 12 4 0 16
− 4 10 2 16

+ Filtek Silorane Adhesive Bond + Filtek Silorane 15 1 0 16

− 6 7 3 16
SiO2 coating
+ Heliobond + Filtek supreme XTE 12 2 2 16
− 1 15 0 16

Control group 11 3 2 16

The repair bond strength was compared with the incre-
mental bond strength of two silorane composite layers, which
corresponds to the clinical situation of an incremental fill-
ing technique. Immediate curing of silorane resulted in a
sufficient incremental bond strengths probably due to an
interactive effect of free radicals and the presence of an (albeit
small) oxygen-inhibited layer. In contrast, incremental bond
strengths to pre-aged restoratives was significantly lower in
silorane compared to dimethacrylate composites, attributed
to the reduced radical concentration of siloranes as a result of
their cationic polymerization [19]. Silorane substrate was aged
by thermal cycling prior to repair as repairs usually become
necessary month or years after placing the restoration in the
oral cavity. In contrast to previous studies analysing bond
strength immediately after repair [13,18], specimens of the
present experiment were subjected to an additional thermal
cycling prior to shear bond testing to assess the long-term sta-
bility of the repair. Previous studies showed that the repair
bond strength of methacrylate-based materials is significantly
affected by aging and the kind of aging condition [21,22]. So
far, only one study investigated the effect of thermal cycling
on silorane–silorane repairs, but did not find significant dif-
ferences between thermocycled specimens and specimens
immediately processed for the shear strength test [17]. The
effect of aging on mixed repairs (silorane composite repaired
with methacrylate-based material) was not studied yet. How-
ever, as the hydrolytic stability of silorane composite is higher
compared to composites with a bis-GMA-based matrix [4],
it might be possible that thermal cycling affects the bond
strength of the different repair composites to the silorane sub-
strate to a different extent.
On the other hand, the flexural strength and modulus of
elasticity of Filtek Silorane and Filtek Supreme XTE is different
which might also affect the results of shear bond strength tests
and the failure mode of the repair restorations [6,23].
In accordance with studies investigating the repair
of methacrylate-based composites [24], different surface
treatments were tested in this study. Hydrofluoric acid etching
yielded lowest repair bond strength independent of the kind
of adhesive conditioning and the repair composite. Equivalent
to methacrylate-based composites, hydrofluoric acid etching
might lead to filler dissolution and, thus, an increased surface
area exposure, which in turn favors hydrolytic degradation
[25]. Moreover, hydrofluoric acid contamination of dental hard
tissues led to a significant decrease of dentin shear bond
strength [26].
The influence of different mechanical surface treatments
on silorane repair bond strength was not tested so far, but
from the results of the present study it can be assumed
that the kind of mechanical treatment (roughening with bur,
aluminum oxide sandblasting or silica coating) is of minor
relevance for siloranes. However, previous studies showed
that the micromechanical retention by bur abrasion is less
effective than sandblasting or silica coating [24], which was
confirmed by the lower shear bond in samples repaired with
the nanofiller composite, especially when no silane agent was
applied.
A recent study considered silane application as a decisive
factor for adhesion of methacrylate-based adhesives, such
as Heliobond, on silorane surfaces [14]. The results of the
present study confirm the important role of the silane agent
for the repair with methacrylate-based adhesives/composites,
as both the shear bond strength and the amount of cohe-
sive failures increased when the silane agent was applied.
However, the results also indicate that silane application is
not mandatory when silorane composite along with silorane
system adhesive bond is used for repair. Silane is supposed
to increase the wettability of the substrate and either effect
chemical (siloxane) bonding to inorganic filler particles of the
silorane composite [15] or bind chemically to the silorane
matrix [14]. This might enhance the adhesion of methacrylate-
based systems [14], but also of silorane composite itself.
Maneenut et al. [15] showed that a silane-containing adhe-
sive increased the bond strength of silorane repair composite
e24 d e n t a l m a t e r i a l s 2 8 ( 2 0 1 2 ) e19–e25
to the silorane substrate to a higher extent than the use of
the Silorane Adhesive System (Primer and Bond). The influ-
ence of the combined use of a silane agent and the Silorane
Adhesive System Bond on silorane repair bond strength has
not been studied, but the repair bond strength values of
the present study indicate that the bonding ability of Silo-
rane Adhesive System Bond, which is not silorane-based but
phosphate–dimethacrylate-based, to the silane agent is lim-
ited. On the other hand, analysis of failure modes indicate that
both methacrylate-based and silorane composites profit from
silane pretreatment, which approves a previous assumption
[18] that the acrylate group of the phosphate–methacrylate
based bonding can react with methacrylate-based systems
and the phosphate group with the silorane repair compos-
ite. However, as the silane agent did not affect bond strength
of Silorane Adhesive System Bond adversely, but enhanced
repair bond strength of methacrylate-based composites, the
routine application of silane for repair of composite fillings
with unknown composite matrix can be recommended.
The repair composites were used with a bonding agent cor-
responding to their matrix, but without hydrophilic primers,
which are necessary for conditioning only when dental hard
tissue is involved in the repair site. Moreover, repair of silo-
rane composite was shown to be adversely affected by the
hydrophilic primer of the Filtek Silorane Adhesive System. It
was discussed that a nanoleakage between the hydrophilic
primer and the hydrophobic bond or an incompatibility
between primer and silane agent is responsible for the detri-
mental effect of the silorane primer [13].
Shear bond strength test was accompanied by analysis of
failure mode, as groups with equal bond strength values do
not necessarily fail in the same way. Overall, failure analysis
confirmed the results of the shear bond strength test in a way
that specimens pretreated with silane showed more cohesive
failures than samples without silane application. Repair with
silorane composite increased the amount of cohesive failures,
especially when compared to the repair with the nanofiller
composite without silane application.
Statistical analysis was completed by Weibull statistics
as this analysis provides information about the variability
of the results. Once more, techniques involving hydrofluo-
ric acid etching or bur abrasion without additional silane
application produced lowest  o values, indicating that these
measures are not suitable for repair of silorane composite.
On the other hand, Weibull moduli m were similar between
most groups, but overall trend to be low. This observation
might be explained by the number of specimens per group
(n = 16), which is potentially not enough to obtain reliable
results, so that these values should be interpreted with
caution [24].
5. Conclusion
Within the limitations of this in vitro study it is concluded that
silorane composite can be repaired with the same material or
a methacrylate-based composite provided that an appropriate
repair technique is used. Repair requires adequate mechani-
cal surface treatment and the application of the corresponding
bonding component. Silane application is required for repair
with methacrylate-based materials. However, the use of silane
agents might be reasonable in any case the matrix of the com-
posite to be repaired cannot be identified, as it was shown to
increase the repair of methacrylate-based materials without
affecting the shear bond strength of silorane–silorane repairs
negatively. However, further research is necessary to confirm
these results in clinical studies.
As repair bond strength was affected by the type of surface
treatment, the use of silane and the kind of adhesive/repair
composite, the null hypotheses were rejected.
Acknowledgement
The authors thank 3M ESPE for providing the composite mate-
rials and Silorane Adhesive System Bond.
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