d e n t a l m a t e r i a l s 2 7 ( 2 0 1 1 ) 144149

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Repairability of dental siloranes in vitro

Anne-Katrin Lhrs , Barbara Grmann, Silke Jacker-Guhr, Werner Geurtsen
Department of Conservative Dentistry, Periodontology and Preventive Dentistry, Hannover Medical School, Hannover, Germany

a r t i c l e
Article history:

i n f o

a b s t r a c t
Objectives. Aim of the study was the investigation of the repairability of a silorane (Filtek Silorane, 3M Espe, Seefeld, Germany) after different surface pretreatments in vitro. Methods. 54 silorane specimens (5 mm 5 mm 5 mm) were fabricated and stored in saline solution (24 h/37 C). Their surface was polished with abrasive paper (600 grit), etched with phosphoric acid (10 s) and rinsed with water (30 s). Repair was performed with a silorane based on one of the 9 treatment protocols (each n = 6): no additional treatment (NAT), silorane primer (P) and silorane bond (B), B only, sandblasting (SB), SB plus P/B, SB plus B, CoJet

Received 29 December 2009 Received in revised form 20 September 2010 Accepted 20 September 2010

Keywords: Silorane Repair Surface pretreatment CoJet Sandblasting Silane

and silane (CJ), CJ plus P/B, CJ plus B. Whole silorane specimens (5 mm 5 mm 10 mm) with no repair served as control. Specimens were sectioned and microtensile bond strength ( TBS) was measured (30 beams per group, surface area approx. 1.2 mm2 , crosshead-speed 1 mm/min) statistical analysis (ANOVA, Tukey HSD, p < 0.05) was performed. Results. TBS of the specimens was signicantly inuenced by the surface pretreatment (p < 0.001). The highest TBS was determined for CJ/B and SB/B, which were not signicantly different from the control. NAT, SB and CJ beneted from an additional treatment with B (p < 0.01). The additional use of P did not improve TBS, but was detrimental for the SB and CJ groups (p < 0.05). Signicance. Siloranes can be repaired with either SB or CJ in combination with a silorane bond, the additional use of silorane primer is disadvantageous. 2010 Academy of Dental Materials. Published by Elsevier Ltd. All rights reserved.

1.

Introduction

Tooth colored composite materials gained a wide popularity during the last decades. Apart from the development of a minimal invasive preparation technique as well as improved adhesion to tooth structures these materials exhibit predictable long-term-stability with annual failure rates that are comparable for composites and amalgam in stress-bearing class I- and class II-cavities [1]. Due to polymerization shrinkage of composite materials which leads to shrinkage stress at the adhesive interface, possible consequences like cuspdeection and loss of marginal integrity occur resulting in

fractures at the interface, marginal staining, microleakage and gap-formation [2,3]. In order to overcome those shortcomings, dental siloranes that consist of a new organic matrix (i.e. monomers with a ring-opening oxirane) were marketed in 2007 [4]. The goal of developing siloranes was to create a material with reduced polymerization shrinkage and less polymerization stress [4,5]. So far, reduction of polymerization shrinkage could only be achieved if for example high molecular monomers or larger amounts of ller particles were added to the organic matrix. Siloranes reveal shrinkage of approx. 1 vol% [4]. In posterior mod-cavities the application of siloranes causes a signicantly lower cusp deection in comparison to methacrylate-based

Corresponding author at: Department of Conservative Dentistry, Periodontology and Preventive Dentistry, OE 7740, Hannover Medical School, Carl-Neuberg-Strae 1, 30625 Hannover, Germany. Tel.: +49 511 532 4836; fax: +49 511 532 4811. E-mail address: Luehrs.Anne-Katrin@mh-hannover.de (A.-K. Lhrs). 0109-5641/$ see front matter 2010 Academy of Dental Materials. Published by Elsevier Ltd. All rights reserved. doi:10.1016/j.dental.2010.09.009

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materials, which was attributed to the lower shrinkage values of this material [6]. Regarding the effect of a cavitys c-factor, the silorane material revealed equal TBS-values on at surfaces when compared to a conventional methacrylate based composite resin. In contrast, a bulk lling technique leads to signicantly decreased TBS-values for the silorane [7]. Clinically, the use of an inappropriate layering technique could cause a failure of the restoration. Silorane-based materials are not investigated widely in vivo due to their relative short existence on the dental market. One clinical trial that examined a methacrylate-based composite resin material and a silorane in class II-cavities revealed an inferior marginal adoption for the silorane compared to a methacrylate based material both occlusally and approximately [8]. Although to our knowledge only one study with a limited observation time is published so far, questions arise regarding the long-term-stability of silorane-based materials. The long-term-stability of dental restorations improved within the last years, but one of the main reasons for placing new restorations is the replacement of preexisting llings, which is associated with the risk of sacricing sound tooth structure [9]. In order to preserve healthy dental hard tissues the repair of dental restorations has become an important treatment option in modern operative dentistry. The complete removal of a tooth colored restoration, i.e. glass-ceramic or composite, caused a loss of tooth structure that was twice as high compared to amalgam or glass-ionomer [10]. As a result, numerous repair modalities have been evaluated in vitro for conventional methacrylate-based composites: surface pretreatment with sandblasting, silica-coating and silanization, roughening of the surface with diamond burs or silicon carbide paper, use of phosphoric acid, different adhesive techniques and preparation methods [1115]. In class II-cavities with the composite surface pretreated with silicon-carbide-burs, best fracture-resistance was achieved after approximal repair for parallel box-preparations without undercuts [11]. Regarding different repair procedures, the treatment of composite surfaces with silica-coating and a bonding agent yielded the highest shear bond strength among different repair procedures [12]. 50- m aluminium oxide air abrasion followed by 37% phosphoric acid etching and the application of a one-step total-etch adhesive resulted in the highest TBS values for composite repair [15]. Another recently published study also conrmed the superiority of sandblasting with aluminium oxide over surface roughening with a diamond bur which led to a lower TBS [16]. Minimal invasive interventions such as sealing of margins and repair of defective lling areas can improve the long-term-stability of resin-based composite materials after 2 years in vivo [17]. The repair of siloranes was not yet investigated in detail. If a silorane lling has to be repaired, no protocol about the surface pretreatment of these restorations exists so far. The pretreatment of the surface could be performed equivalent to the repair of methacrylate-based composite materials, as done by [18], where the surface was roughened with silicon-carbide paper, cleaned with 37% phosphoric acid and coated with the silorane bonding agent. The repair protocol for silorane classV restorations described by [19] included surface roughening with a diamond bur, etching of the cavity with 36% phosphoric acid and application of the complete silorane adhesive system.

Therefore, the aim of this study was to evaluate different pretreatment protocols for the repair of a dental silorane. The null hypothesis that was set forth was that different repair procedures do not inuence the microtensile bond strength ( TBS) of a repaired silorane-based restoration.

2.

Materials and methods

54 silorane specimens fabricated in Teon moulds (5 mm 5 mm 5 mm) were used for these experiments. For each specimen, 2 layers of silorane were placed and cured separately. The last layer was covered with a transparent matrix in order to obtain a at surface. Each layer (thickness max. 2.5 mm) was cured for 40 s with an LED polymerization light (Elipar Freelight 2, 3 M Espe, Seefeld, Germany) with an output of at least 1000 mW/cm2 . The LED was placed directly at the surface of the mould. The output of the curing device was controlled during each polymerization circle with a digital radiometer (bluephase meter, Ivovlar Vivadent, Schaan, Liechtenstein). Afterwards, the specimens were stored in saline solution for 24 h at 37 C. The surfaces of all specimens were wet-polished with abrasive paper (600 grit, Buehler GmbH, Dsserdorf, Germany) in order to remove the oxygen-inhibited layer, etched with phosphoric acid (30 s) and rinsed with water (30 s). All used materials, their manufacturers and the manufacturers instructions for use are shown in Table 1. After surface pretreatment, the specimens were randomly assigned to one of the 9 test groups (each n = 6): no additional treatment (NAT); silorane primer (P) and silorane bond (B); B only; sandblasting (SB) with aluminium oxide; SB plus P & B; SB with B only; Chairside silica-coating (CoJet) and silane (CJ); CJ plus P & B; CJ with B only.

A dental microblaster was used to apply aluminium oxide (groups SB, SB/B and SB/P/B) or CoJet Sand (groups CJ, CJ/B and CJ/P/B) at the surface (Dento-Prep, Rnvig Dental Mfg. A/S Daugaard, Denmark). After surface treatment, the specimens were transferred to a second Teon mould (10 mm 5 mm 5 mm) and the repair was performed with a silorane placed on top of the pretreated surface using the layering technique described above. For repair, a different shade was selected in order to identify the demarcation between the lower part of the specimen (substrate for repair) and the upper part (repair silorane placed after surface pretreatment). Whole silorane specimens (5 mm 5 mm 10 mm) without repair served as control. The groups NAT, SB and CJ served as internal negative controls within each group of additional surface treatment (application of the silorane adhesive or bonding agent only). All specimens were mounted with sticky wax to an acrylic mount and sectioned vertically with a low speed diamond saw (Isomet, Buehler GmbH, Dsserdorf, Germany) under water cooling as described by [14]. The non-

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Table 1 Materials, manufacturers and manufacturers instructions. Product

DeTrey Conditioner 36 CoJet Sand Monobond S Aluminium Oxide Silorane Primer Silorane Bond Filtek Silorane B2

Manufacturer
Dentsply, Konstanz, Germany 3M Espe, Seefeld, Germany Ivoclar Vivadent, Schaan, Liechtenstein Rnvig Dental Mfg. A/S Daugaard, Denmark 3M Espe, St. Paul, USA 3M Espe, St. Paul, USA 3M Espe, St. Paul, USA

Lot
0805002679 306931 15382 Item no. 1906 7AH 7AG 7AK, 8BB

Application
Etching of the surface for 10 s, rinsing with water for 30 s, air-drying Applying particles with sandblaster for 10 s at a distance of 5 mm Applying, air-drying after 60 sec Applying particles (size 50 m) with sandblaster for 10 s at a distance of 5 mm Applying self-etch primer for 15 s, air-blowing, polymerization for 10 s Applying for 10 s, air-blowing, polymerization for 10 s Placing the material in Teon mould, each increment max. 2.5 mm, polymerization for 40 s Placing the material in Teon mould, each increment max. 2.5 mm, polymerization for 40 s

Filtek Silorane A3

3M Espe, St. Paul, USA

8BR, 8CP

trimming technique was used in order to obtain at least 30 beams per group. All silorane sticks were stored in saline solution for 24 h at 37 C before microtensile bond strength ( TBS) testing. The diameter of the beams was measured with digital calipers (Powerx Electronic Digital Caliper, Padget Services, London, England) with an accuracy of at least 0.01 mm and the area of the repaired surface area was calculated. Each beam was checked for voids or defects within the material with a light microscope (Stemi SV 6, Firma Zeiss, Jena, Germany). The TBS-test was performed with a crosshead-speed of 1 mm/min in a universal testing machine (MTD-500, SD Mechatronik, Feldkirchen-Westerham, Germany). Load was applied until failure and beams were removed from the testing machine for microscopic examination using a light microscope at 8- and 50-fold magnication. As no mixed fracture occurred, the fractured beams were assigned to either adhesive or cohesive fracture type. Statistical analysis (one-way ANOVA, Tukey HSD, p < 0.05) was performed using SPSS 15.0 software (SPSS Inc., Chicago, IL, USA). Specimens that fractured during the mounting procedure were excluded from statistical analysis. No zero-bonds were present after water storage. In order to analyze the inuence of the surface area of the specimens on the data, beams of every group were divided into specimens smaller 1.2 mm2 and specimens not less than 1.2 mm2 . This size of the square cross section was described by [20] as upper limit for the non-trimming technique. Within each group, data were statistically analyzed again by Tukey HSD (p < 0.05).

3.

Results

One-way ANOVA showed signicant differences for the various repair techniques (p < 0.001). The mean values and standard deviations for all tested groups are listed in Table 2. Tukey HSD test showed that the highest TBS was determined for group CJ/B and SB/B, which were not signicantly different from the control. Compared to group NAT, which showed the lowest TBS, all other groups beneted from further surface treatment (p < 0.001). The application of the bonding agent in groups B, SB/B and CJ/B compared to NT, SB and CJ resulted in higher bond strength values (p < 0.001/p = 0.007/p < 0.001). After treatment with SB/B and CJ/B, the TBS values of the repaired specimens did not differ from the control. The TBS of the repaired specimens did not benet from the additional use of the primer, for SB/P/B and CJ/P/B this procedure reduced bond strength signicantly compared to SB/B and CJ/B (p < 0.05/p < 0.001). For group P/B compared to B, no signicant inuence of the primer was detected (p > 0.05). Results are shown in Fig. 1. Within the test groups, the size of the specimens did not inuence the TBS (p > 0.05, Tukey HSD). The surface area of the specimens is shown in Table 2. The fracture analysis revealed mainly adhesive fractures (Table 2). Only for B and CJ/B, the majority of beams fractured cohesively (B: 63.3%, CJ/B: 76.7%). No mixed fractures were detected.

Table 2 Mean values and standard deviations of control and test groups, similar superscripts indicate no signicant difference between groups (p > 0.05, Tukey HSD), SA = surface area of the specimens, Fx = results of fracture analysis (only adhesive fractures displayed, number of specimens, percentage in parenthesis). Control
Mean (MPa) SD SA (mm2 ) Fx N 59.3E 10.5 1.2 0.2 0 (0) 30

NAT
19.3A 5.3 1.2 0.1 27 (100) 27

B
35.0B 15.1 1.2 0.1 11 (36.7) 30

P/B
40.1B,C 12.8 1.2 0.2 19 (63.3) 30

SB
42.4B,C 12.5 1.3 0.1 22 (75.1) 29

SB/B
54.4D,E 8.1 1.2 0.2 21 (72.4) 29

SB/P/B
43.6B,C 14.1 1.2 0.2 26 (86.7) 30

CJ
46.4C,D 15.2 1.3 0.1 25 (83.3) 30

CJ/B
62.1E 13.2 1.2 0.1 7 (23.3) 30

CJ/P/B
36.9B,C 9.3 1.2 0.2 28 (96.6) 29

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Fig. 1 Box plots with median values and standard deviation of control and test groups according to different pretreatment procedures.

4.

Discussion

The repair of methacrylate-based composite restorations can be considered as a standard procedure in todays dentistry due to the fact that sound hard tooth tissues can be preserved. The complete removal of tooth colored restorations is a technically demanding procedure that is associated with extended treatment time [9,10]. Bonding between layers of methacrylate-based composites during repair can be signicantly inuenced by specic pretreatment methods [1115]. As mechanical interlocking seems to be an important approach to establish an adequate repair bond strength, either sandblasting with 50 m aluminium oxide or the use of intraoral silication and silane application in combination with an adhesive system seems to be superior when compared to other methods like the use of phosphoric acid, hydrouoric acid or surface roughening with a diamond bur [1116]. For silorane, only very scarce data have been reported about their repair or different surface pretreatments. Because of the results regarding the appropriate surface pretreatment for methacrylate materials, sandblasting with aluminium oxide and silication/silane application were included in this study. Regarding the repair of class V-silorane and methacrylatebased composite restorations, in a recently published study the microleakage after TC (5000 cycles, 555 C) and cyclic loading was examined [19]. The surface pretreatment was performed with either an Er:YAG Laser or a diamond bur, followed by the application of the silorane adhesive system. The authors found no signicant difference regarding the surface pretreatment and the materials used and concluded that silorane materials can be repaired successfully with both surface pretreatments. In our study, surface roughening and the application of the silorane adhesive yielded TBS-values that were not signicantly different from sandblasting and silication/silane application. If no application of the silorane primer was performed, signicantly higher TBS-values were measured for the last two methods (p < 0.05/p < 0.001). Therefore,

these repair protocols seem to be superior if only the silorane bond is applied. The cited study about the repair of siloranes showed that silorane repair was not yet investigated sufciently. Furthermore, a different method was used (microleakage evaluation vs. TBS), which makes it difcult to compare the results of our study with other data published about silorane repair. Thus, data from our study can be only compared with results of experiments that analyzed the repair of methacrylate-based composite resins and different surface pretreatments. Higher TBS values for silica-coating and silane pretreatment were determined compared to phosphoric acid etching and application of a bonding agent [13]. This is in accordance with our results for siloranes, where group CJ/B resulted in a higher TBS than groups B and P/B (p < 0.001). In contrast to our study, different aging procedures (immersion in citric acid, boiling in water or thermocycling) were performed whereas our specimens were stored in 37 C saline solution for 24 h before and after repair. Aluminium oxide pretreatment of the repaired surfaces resulted in signicantly higher TBS-values compared to surface roughening with a diamond bur, independent of the hydrophilicity of the adhesive used or aging procedures (immediate repair vs. 6 months water storage) [16]. The TBS-values determined after sandblasting and application of a hydrophobic bonding agent were 56.4 MPa (7.4), which is equivalent to our group SB/B (54.4 8.1 MPa). These results support our ndings for silorane repair, where sandblasting with aluminium oxide followed by the application of the silorane bond (group SB/B) revealed TBS-values that were not signicantly different from the control and group CJ/B. The importance of surface roughening and the application of an adhesive system during composite repair were also demonstrated by [21]. But in contrast to our ndings for siloranes, sandblasting followed by the application of a hydrophobic adhesive in combination with its hydrophilic primer resulted in signicantly higher bond strength values compared to adhesive coating only. For silica coating, but without the use of a silane, this effect was not detectable. Our results for silorane repair show a different effect, for both roughening procedures (i.e. sandblasting and silication/silane application) the additional use of the hydrophilic silorane primer was detrimental for the TBS (SB/P/B vs. SB/B and CJ/P/B vs. CJ/B, p < 0.05/p < 0.001). The superiority of surface roughening with aluminium oxide or silication was also shown by [22]. Repair of a microhybrid or a nanoparticle composite resin showed higher TBS-values for these two methods compared to abrasion with a diamond bur or surface etching with 9.5% hydrouoric acid. For both methods, the results were independent of the use of a silane, a one-stepadhesive or their combination. This also supports our ndings for silorane repair, were both air-abrasion methods in combination with the silorane bonding resulted in signicantly higher TBS-values than roughening with silicium-carbide paper. The surface pretreatment with aluminium oxide in combination with a two-step self-etch adhesive resulted in TBS-values (24 h after repair) that were similar to the whole control specimens where no repair was performed [23]. Again, air abrasion with aluminium oxide was superior to surface roughening with diamond burs. For pretreatment with alu-

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minium oxide during silorane repair, only the combination with the silorane bond revealed similar results. Questions arise why the primer caused detrimental effects on the TBS of a repaired silorane that were observed after both air abrasion pretreatments (SB/B vs. SB/P/B and CJ/B vs. CJ/P/B). One possible explanation for this observation could be that the primer of the silorane adhesive is rather hydrophilic and the silorane bond is hydrophobic [24]. During repair, a hydrophilic primer (that is normally used for connecting the hydrophilic tooth tissue with the hydrophobic bonding agent) was applied directly to the hydrophobic silorane surface. This nding is partly supported by the fracture analysis. After surface roughening with abrasive paper, 63.3% of the specimens fractured adhesively in group P/B in contrast to only 36.7% in group B. In the aluminium oxide groups, this effect was not found, maybe due to the increased surface roughening induced by the greater particle size. For the CJ groups the same effect as in groups NAT, B and P/B was detected, which could be due to possible interactions of the silorane primer with the silane. TEM photomicrographs of the silorane adhesives interface also exhibited nanoleakage between primer and bond. This was demonstrated by silver penetration between the two adhesive layers [24]. Nevertheless it has to be taken into account that nanoleakage is not necessarily associated with an impaired TBS or clinical performance, especially for etch and rinse adhesives [25,26]. Focus of further research should be the long-term stability of silorane repair and aged silorane surfaces. This will contribute to the optimization of the protocol for silorane repair.

5.

Conclusion

The repair methods used for methacrylate-based composite resins can be also applied for silorane repair. Surface roughening either with sandblasting or silication/silanization followed by the application of the silorane bonding agent resulted in bond strength values comparable to control. Because the additional use of the silorane primer impaired the bond of repaired silorane, the primer should not be applied in cavities where no tooth substance is exposed (for example chipping fractures).

Acknowledgements
Our thanks are due to Dr. L. Hoy, Department of Biometry, Hannover Medical School, for his help with the statistical analysis of our data. The materials used for this study were provided by 3M Espe, Seefeld, Germany.

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