Professional Documents
Culture Documents
Estresse de Contração
Estresse de Contração
available at www.sciencedirect.com
Annelies Van Ende, Jan De Munck ∗, Atsushi Mine, Paul Lambrechts, Bart Van Meerbeek
Leuven BIOMAT Research Cluster, Department of Conservative Dentistry, School of Dentistry, Oral Pathology and Maxillo-facial Surgery,
Catholic University of Leuven, Kapucijnenvoer 7, 3000 Leuven, Belgium
a r t i c l e i n f o a b s t r a c t
∗
Corresponding author. Tel.: +32 16 33 26 16; fax: +32 16 33 27 52.
E-mail address: jan.demunck@med.kuleuven.be (J. De Munck).
0109-5641/$ – see front matter © 2009 Academy of Dental Materials. Published by Elsevier Ltd. All rights reserved.
doi:10.1016/j.dental.2009.10.003
216 d e n t a l m a t e r i a l s 2 6 ( 2 0 1 0 ) 215–222
Fig. 1 – Schematic explaining the study set-up. (a) A flat surface or a standardized occlusal class-I cavity was prepared. (b)
The cavities were filled using either the low-shrinking composite (Filtek Silorane) or a conventional methacrylate-based
composite (Filtek Z100). (c) Resin–dentin micro-specimens (1 mm × 1 mm) were cut using an automated diamond saw and
(d) stressed in tension until failure.
none of these techniques can eliminate the stress completely. by 3M-ESPE, SSA-Bond contains a hydrophobic bifunctional
Naturally, the surest way to avoid shrinkage stress is to use monomer in order to match the hydrophobic silorane resin
non-shrinking resins. [10,11]. In addition, TEM adhesive–composite interfacial char-
Recently, a low-shrinking composite, commercialized as acterization [12] did not disclose any separations between
Filtek Silorane (3M-ESPE, Seefeld, Germany), was introduced. SSA-Bond and the silorane composite, while a clear incompat-
So-called siloranes replace the methacrylates in the resin ibility existed with the experimental precursor of SSA (before
matrix of dental composites [6–8]. The ring-opening chemistry being referred to as ‘Hermes Bond’, 3M-ESPE) [13].
of the resin reduces shrinkage of the composite below 1 vol% Because of the low-shrinking nature of this silorane
[9]. Filtek Silorane comes with a two-step self-etch adhe- composite, the cavity configuration and the need for an incre-
sive, commercialized as ‘Silorane System Adhesive’ (SSA). mental application technique is expected to be less critical.
First, a hydrophilic self-etch primer (Silorane System Adhe- The hypotheses tested were therefore that (1) the cavity con-
sive Self-Etch Primer, SSA-Primer) is applied and light-cured figuration and (2) the composite application technique do not
separately prior to the application of a hydrophobic adhesive affect the bonding effectiveness of a low-shrinking silorane-
resin (Silorane System Adhesive Bond, SSA-Bond). SSA-Bond based composite to dentin. We determined the micro-tensile
is methacrylate-based and is therefore compatible with con- bond strength (TBS) of Filtek Silorane in two different cavity
ventional methacrylate composites as well. Further details on configurations and using five different application techniques
how SSA-Bond links to the silorane composite is currently not in comparison to that of a conventional resin composite (con-
known, but according to the technical information provided trol).
Table 1 – Overview of the different application protocols used in the eight experimental groups.
Group Description Total curing time (s)
‘flat’(1) The composite was applied to a flat surface and cured in 2 × 20 + 40
Filtek Z100
three horizontal layers.
‘cavity’(2) The composite was applied in a cavity and cured in bulk. 40
Fig. 2 – Box whisker plots of the TBS (MPa). The box represents the spreading of the data between the first and third
quartile. The central vertical line represents the median. The whiskers denote minimum and maximum values. Groups that
are statistically not different are connected with a vertical line (Tukey–Kramer multiple comparisons, p > 0.05).
d e n t a l m a t e r i a l s 2 6 ( 2 0 1 0 ) 215–222 219
Filtek Silorane
‘flat’(3) 33.4 (11.2)a 20 2% 8% 25% 56% 10%
‘flat/bulk-filled’(4) 19.7 (10.2)c,d,e 22 2 0% 7% 12% 67% 15%
‘cavity/bulk-filled’(5) 13.2 (9.2)d,e 18 2 2% 0% 38% 49% 11%
‘cavity/layered-filled’(6) 21.5 (10.1)b,c,d 18 9% 2% 27% 37% 25%
‘cavity/flowable cured’(7) 23.7 (7.9)b,c 20 3% 19% 18% 23% 37%
‘cavity/flowable uncured’(8) 11.6 (4.5)e 17 0% 4% 11% 61% 23%
SD = standard deviation; n = total number of specimens; ptf = pre-testing failures. Means with the same superscript are not significantly different
(ANOVA and Tukey–Kramer multiple comparisons, p > 0.05). A/C = failure at the adhesive/composite interface.
Fig. 3 – (a) Overview Feg-SEM photomicrograph of a fracture surface of the FS ‘cavity/flowable cured’(7) group, showing a
‘mixed’ failure pattern. Note the smooth glossy appearance of the bonding resin due to the absence of large filler particles.
Circular scratches typical of the cavity-bottom when prepared with the tip of the diamond-bur of a cylindrical, regular-grit
diamond-bur, can be observed. (b) Fracture surface of a Z100 ‘flat’(1) micro-specimen, showing a ‘mixed’ failure pattern.
Insert: higher magnification of the interfacially failed area; failure occured at the level of the hybrid layer. (c) Fracture surface
of a FS ‘flat’(3) micro-specimen, showing a mixed failure pattern. Straight scratches from diamond-bur preparation are
clearly visible (hand pointer). The adhesive resin was preferentially retained in these grooves. (d) Fracture surface of a Z100
‘cavity’(2) micro-specimen, showing a ‘mixed’ failure pattern, similar to that typically observed for the flat control.
220 d e n t a l m a t e r i a l s 2 6 ( 2 0 1 0 ) 215–222
Both composites Filtek Z100 and Filtek Silorane bonded composite to polymerize properly at the interface when filling
equally well to a flat dentin surface using the two-step self- occurred in bulk. Low conversion rates have been associated
etch adhesive, Silorane System Adhesive. Silorane System with decreased mechanical strength of adhesives [27]. It is
Adhesive is based on methacrylate chemistry (technical infor- possible that the silorane composite is more susceptible to
mation from 3M-ESPE [10,11]), by which it can be used to reduced curing with depth than Filtek Z100, and this may
bond conventional methacrylate-based composites to dentin explain why only the silorane composite was “significantly”
as well. Compared to previous research conducted following affected by the reduced curing energy (though both compos-
the same methodology [19,20], the Silorane System Adhesive ites showed a decline in TBS when cured in bulk for only
performed in combination with Filtek Z100 equally well as 40 s). Previous studies have demonstrated that Filtek Silo-
other two-step self-etch adhesives like for instance AdheSE rane exhibits a polymerization reaction with a slower onset
or Protect Bond in terms of TBS. because more time is needed to form sufficient cations to ini-
Bonding to cavity-bottom dentin lowered the TBS, but this tiate polymerization [14,28]. On the other hand, Filtek Z100 is
was somewhat unexpectedly not statistically significant for a rather transparent composite with a higher filler load than
Filtek Z100 (p = 0.9259). This suggests that the bond to dentin Filtek Silorane (85% vs. 76% weight volume) and may therefore
was sufficiently strong to resist the polymerization shrink- also transmit light better than Filtek Silorane. Because Filtek
age stress induced by Filtek Z100. This could be due to the Z100 cures more rapidly than Filtek Silorane, polymerization
higher viscosity of the filled, two-layered adhesive Silorane efficiency of Filtek Z100 may be less affected by the reduced
System Adhesive [21], enabling a thick layer of adhesive to curing energy provided to the Z100 ‘cavity’(2) group.
be placed on the tooth surface. This thick layer may have The final application protocol used with the intention to
increased the strain capacity of the restoration by acting as an improve material adaptation in the narrow class-I cavity was
elastic buffer [5,22,23]. Previous research has shown that Fil- the use of an intermediary layer of an experimental silorane
tek Z100 bonded to cavity-bottom dentin using the two-step flowable composite (FS ‘cavity/flowable cured’(7) and FS ‘cav-
etch-and-rinse Scotchbond 1 lowered the TBS significantly, ity/flowable uncured’(8)). Whether or not the intermediate
while adhesives with a separate hydrophobic adhesive resin, layer was cured separately, caused a statistically significant
like Clearfil SE and OptiBond FL, were less affected [18]. difference (p = 0.0041). When the flowable silorane compos-
The decrease in TBS, when bonding to cavity-bottom ite was not cured, there was no difference compared to
dentin, was statistically highly significant for Filtek Silo- bulk-filling the cavity (p = 0.9997). This indicates that polymer-
rane (p = 0.0001). Previous studies have shown that the TBS ization at the interface level is probably more critical than
may decrease with increasing C-factor [1,3,18,24]. This find- adaptation of the composite to the bond.
ing is most commonly attributed to the shrinkage stress that The self-etching primer of Silorane System Adhesive has
accompanies the polymerization process. However, since Fil- a pH of 2.7 and thus can be classified as ‘ultra-mild’ [29].
tek Silorane is a low-shrinking composite and there was TEM revealed a thin interaction zone, most likely represent-
no significant decrease recorded in the control group, it is ing a combination of resin-impregnation of the smear layer
very unlikely that shrinkage stress is the cause in this par- and actual dentin hybridization [30,12]. The SSA-Primer and
ticular case. Because the uncured composite is rather stiff, SSA-Bond are distinguishable as two distinct layers [12], since
close adaptation to the dentin surface in the narrow cavity they are cured separately. Despite its two-step application
may have been problematic. In some specimens of the FS technique, its mechanism of adhesion resembles more that
‘cavity/bulk-filled’(5) group, air bubbles were indeed observed of a one-step adhesive because the actual bond to the tooth
at the composite–dentin interface, which must have led to surface is realized by the SSA-Primer only [10]. As such ‘ultra-
fracture at a lower TBS. This probably also caused the low mild’ one-step self-etch adhesives only interact superficially
amount of ptf’s observed in the FS ‘flat/bulk-filled’(4) and FS with the smear layer-covered dentin, they are much more
‘cavity/bulk-filled’(5) groups. dependent on the properties of this smear layer [31]. In this
Filling the cavity using an incremental technique (FS study, flat surfaces were prepared using the long side of the
‘cavity/layered-filled’(6)) increased the TBS when compared cylindrical bur (producing parallel scratches), while the cavity-
to a bulk-filling application technique. Previous studies using bottoms were prepared using the tip of the same diamond-bur
conventional composites have already demonstrated that (resulting in circularly oriented scratches) (Fig. 3c vs. d). The
an incremental technique has a beneficial effect on the latter smear layer is expected to have different properties due
bond strength [25,26]. Mostly, this positive effect should be to different pressure, cutting and cooling efficiency. This dif-
attributed to reduced shrinkage stress by decreasing the C- ferent kind of smear layer, along with the use of an ‘ultra-mild’
factor of each layer. For the same reasons mentioned above, self-etch adhesive, may explain, at least to a certain extent, the
other factors are more likely to have improved the bond differences observed in TBS at the cavity-bottom vs. at the
strength. Firstly, adaptation of the rather stiff silorane com- flat surface [31].
posite might have been better. Secondly, curing at the interface Because of the reduced polymerization shrinkage of the
level might have been more efficient by an increase in power silorane composite compared to that of a conventional
(light is only dimmed by a thin layer of composite) and cur- methacrylate composite, the interface is exposed to signifi-
ing time (the total curing time was increased as well, Table 1). cantly less stress [28,4], so the need for a very strong adhesive
This is substantiated by a significant correlation that exists is reduced. The values found in this study are probably still
between TBS and the total curing time for all Filtek Silo- sufficient to withstand the lower shrinkage stress. This is sus-
rane groups (correlation coefficient of 0.8357 with p = 0.019). tained by the little number of pre-testing failures recorded
The reduced light intensity may have impaired the silorane in this study. Light-microscopic evaluation showed that most
d e n t a l m a t e r i a l s 2 6 ( 2 0 1 0 ) 215–222 221
failures occurred cohesively in the adhesive layer or adhe- comparison study using a double-staining/confocal
sively between the adhesive and the silorane composite, microscopy technique. Eur J Oral Sci 2008;116:184–93.
which will lead to fewer clinical consequences as the dentin [12] Mine A, De Munck J, Van Landuyt KL, Lambrechts P, Van
remains sealed [10]. Meerbeek. TEM interface characterization of a low-shrinking
composite bonded to enamel/dentin. J Dent Res 2008;87
[Special issue C, abstract 0252].
5. Conclusion [13] Ernst CP, Galler P, Willershausen B, Haller B. Marginal
integrity of class V restorations: SEM versus dye penetration.
Dent Mater 2008;24:319–27.
The low-shrinking silorane composite and the methacrylate-
[14] Bouillaguet S, Gamba J, Forchelet J, Krejci I, Wataha JC.
based composite bonded equally well to flat dentin using Dynamics of composite polymerization mediates the
the Silorane System Adhesive. From the different application development of cuspal strain. Dent Mater 2006;22:896–902.
techniques evaluated in this study can be concluded that ade- [15] Poitevin A, De Munck J, Van Landuyt K, Coutinho E, Peumans
quate polymerization, especially at the bottom of the cavity, M, Lambrechts P, Van Meerbeek B. Critical analysis of the
is more important than the cavity configuration. Therefore, influence of different parameters on the microtensile bond
strength of adhesives to dentin. J Adhes Dent 2008;10:7–16.
a layering technique remains recommended, even for these
[16] Perdigão J, Lambrechts P, Van Meerbeek B, Vanherle G, Lopes
low-shrinking composites.
ALB. Field emission SEM comparison of four postfixation
drying techniques for human dentin. J Biomed Mater Res
1995;29:1111–20.
Acknowledgements
[17] Kleverlaan CJ, Feilzer AJ. Polymerization shrinkage and
contraction stress of dental resin composites. Dent Mater
This paper is part of a thesis submitted by A. Van Ende 2005;21:1150–7.
to the School of Dentistry, Oral Pathology and Maxillo-facial [18] Shirai K, De Munck J, Yoshida Y, Inoue S, Lambrechts P,
Surgery, Catholic University of Leuven, in partial fulfillment Suzuki K, Shintani H, Van Meerbeek B. Effect of cavity
of the requirements to obtain the Flemish degree of Master configuration and aging on the bonding effectiveness of six
adhesives to dentin. Dent Mater 2005;21:110–24.
in Dentistry. This study was supported in part by the FWO
[19] De Munck J, Van Landuyt KL, Coutinho E, Poitevin A,
No. G.0206.07 and the KULeuven OT/06/55 research grants. 3M
Peumans M, Lambrechts P, Van Meerbeek B. Micro-tensile
ESPE (Seefeld, Germany) is gratefully acknowledged for the bond strength of adhesives bonded to class-I cavity-bottom
generous donation of materials used in this study. dentin after thermo-cycling. Dent Mater 2005;21:999–1007.
[20] De Munck J, Vargas M, Iracki J, Van Landuyt K, Poitevin A,
references Lambrechts P, Van Meerbeek B. One-day bonding
effectiveness of new self-etch adhesives to bur-cut enamel
and dentin. Oper Dent 2005;30:39–49.
[21] Tezvergil-Mutluay A, Lassila LVJ, Vallittu PK. Incremental
[1] Choi KK, Ryu GJ, Choi SM, Lee MJ, Park SJ, Ferracane JL. layers bonding of silorane composite: the initial bonding
Effects of cavity configuration on composite restoration. properties. J Dent 2008;36:560–3.
Oper Dent 2004;29:462–9. [22] Kemp-Scholte CM, Davidson CL. Complete marginal seal of
[2] Feilzer AJ, de Gee AJ, Davidson CL. Setting stress in class V resin composite restorations effected by increased
composite resin in relation to configuration of the flexibility. J Dent Res 1990;69:1240–3.
restoration. J Dent Res 1987;66:1636–9. [23] Van Meerbeek B, Willems G, Celis JP, Roos JR, Braem M,
[3] Yoshikawa T, Sano H, Burrow MF, Tagami J, Pashley DH. Lambrechts P, Vanherle G. Assessment by nano-indentation
Effects of dentin depth and cavity configuration on bond of the hardness and elasticity of the resin–dentin bonding
strength. J Dent Res 1999;78:898–905. area. J Dent Res 1993;72:1434–42.
[4] Ferracane JL. Developing a more complete understanding of [24] Armstrong SR, Keller JC, Boyer DB. The influence of water
stresses produced in dental composites during storage and C-factor on the dentin-resin composite
polymerization. Dent Mater 2005;21:36–42. microtensile bond strength and debond pathway utilizing a
[5] Labella R, Lambrechts P, Van Meerbeek B, Vanherle G. filled and unfilled adhesive resin. Dent Mater 2001;17:268–76.
Polymerization shrinkage and elasticity of flowable [25] Nayif MM, Nakajima M, Foxton RM, Tagami J. Bond strength
composites and filled adhesives. Dent Mater 1999;15:128–37. and ultimate tensile strength of resin composite filled into
[6] Eick JD, Kotha SP, Chappelow CC, Kilway KV, Giese GJ, Glaros dentine cavity; effect of bulk and incremental filling
AG, Pinzino CS. Properties of silorane-based dental resins technique. J Dent 2008;36:228–34.
and composites containing a stress-reducing monomer. [26] He Z, Shimada Y, Tagami J. The effects of cavity size and
Dent Mater 2007;23:1011–7. incremental technique on micro-tensile bond strength of
[7] Eick JD, Smith RE, Pinzino CS, Kostoryz EL. Stability of resin composite in class I cavities. Dent Mater 2007;23:
silorane dental monomers in aqueous systems. J Dent 533–8.
2006;34:405–10. [27] Yamamoto A, Tsubota K, Takamizawa T, Kurokawa H, Rikuta
[8] Guggenberger R, Weinmann W. Exploring beyond A, Ando S, Takigawa T, Kuroda T, Miyazaki M. Influence of
methacrylates. Am J Dent 2000;13:82D–4D. light intensity on dentin bond strength of self-etch systems.
[9] Weinmann W, Thalacker C, Guggenberger R. Siloranes in J Oral Sci 2006;48:21–6.
dental composites. Dent Mater 2005;21:68–74. [28] Palin WM, Flaming GJ, Nathwani H, Burke FJ, Randall RC. In
[10] Santini A, Miletic V. Comparison of the hybrid layer formed vitro cuspal deflection and microleakage of maxillary
by silorane adhesive, one-step self-etch and etch and rinse premolars restored with novel low-shrink dental
systems using confocal micro-Raman spectroscopy and composites. Dent Mater 2005;21:324–35.
SEM. J Dent 2008;36:683–91. [29] Sarr M, De Munck J, Kane AW, Faye B, Vreven J, Peumans M,
[11] Sauro S, Pashley DH, Mannocci F, Tay FR, Pilecki P, Sherriff M, et al. Micro-tensile bond strength and interfacial
Watson TF. Micropermeability of current self-etching and characterization of 11 contemporary adhesives bonded to
etch-and-rinse adhesives bonded to deep dentine: a bur-cut dentin. Oper Dent; accepted for publication.
222 d e n t a l m a t e r i a l s 2 6 ( 2 0 1 0 ) 215–222
[30] Koshiro K, Sidhu SK, Inoue S, Ikeda T, Sano H. New concept [31] Ermis RB, De Munck J, Cardoso MV, Coutinho E, Van Landuyt
of resin–dentin interfacial adhesion: the nanointeraction KL, Poitevin A, Lambrechts P, Van Meerbeek B. Bond strength
zone. J Biomed Mater Res B: Appl Biomater 2006;77: of self-etch adhesives to dentin prepared with three
401–8. different diamond burs. Dent Mater 2008;24:978–85.