Influence of the LED curing source andselective enamel etching on dentin bondstrength of self-etch adhesives in class Icom...
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Authors personal copyLasers Med SciDOI 10.1007/s10103-011-1030-y ORIGINAL ARTICLEInfluence of the LED curing source and se...
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Authors personal copyLasers Med SciTable 1 Characteristics of the LCUs used in this studyLCU                   Manufacture...
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Authors personal copyLasers Med SciTable 5 Percentage of specimens (%) from Clearfil SE bond adhesive distributed accordin...
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  1. 1. Influence of the LED curing source andselective enamel etching on dentin bondstrength of self-etch adhesives in class Icomposite restorationsEduardo José Souza-Junior, CíntiaTereza Pimenta Araújo, Lúcia TrazziPrieto & Luís Alexandre Maffei SartiniPaulilloLasers in Medical ScienceISSN 0268-8921Lasers Med SciDOI 10.1007/s10103-011-1030-y 1 23
  2. 2. Your article is protected by copyright and allrights are held exclusively by Springer-VerlagLondon Ltd. This e-offprint is for personaluse only and shall not be self-archived inelectronic repositories. If you wish to self-archive your work, please use the acceptedauthor’s version for posting to your ownwebsite or your institution’s repository. Youmay further deposit the accepted author’sversion on a funder’s repository at a funder’srequest, provided it is not made publiclyavailable until 12 months after publication.1 23
  3. 3. Authors personal copyLasers Med SciDOI 10.1007/s10103-011-1030-y ORIGINAL ARTICLEInfluence of the LED curing source and selective enameletching on dentin bond strength of self-etch adhesivesin class I composite restorationsEduardo José Souza-Junior &Cíntia Tereza Pimenta Araújo & Lúcia Trazzi Prieto &Luís Alexandre Maffei Sartini PaulilloReceived: 18 July 2011 / Accepted: 7 November 2011# Springer-Verlag London Ltd 2011Abstract The aim of this study was to evaluate the compared to the non-etched specimens (26.7±2.2). ULinfluence of the LED curing unit and selective enamel yielded higher μTBS values (24.1±3.2) in comparison toetching on dentin microtensile bond strength (μTBS) for the photoactivation approach with FL (18.8 ±3.9) and RDself-etch adhesives in class I composite restorations. On 96 (19.9 ±1.8) for CSE. The two-step CSE was not influencedhuman molars, box-shaped class I cavities were made by the enamel etching (p≥0.05). Enamel acid etching inmaintaining enamel margins. Self-etch adhesives (Clearfil class I composite restorations affects the dentin μTBS ofSE – CSE and Clearfil S3 – S3) were used to bond a the one-step self-etch adhesive Clearfil S3, with nomicrohybrid composite. Before adhesive application, half alterations for Clearfil SE bond strength. The polywaveof the teeth were enamel acid-etched and the other half was LED promoted better bond strength for the two-stepnot. Adhesives and composites were cured with the adhesive compared to the single-peak ones.following light curing units (LCUs): one polywave (Ultra-Lume 5 - UL) and two single-peak (FlashLite 1401 - FL Keywords Acid etching . Enamel . Self-etch adhesives .and Radii Cal - RD) LEDs. The specimens were then Light curing units . Bond strengthsubmitted to thermomechanical aging and longitudinallysectioned to obtain bonded sticks (0.9 mm2) to be tested intension at 0.5 mm/min. The failure mode was then Introductionrecorded. The μTBS data were submitted to a three-wayANOVA and Tukey’s (α=0.05). For S3, the selective Resin composites have been widely used in direct aestheticenamel-etching provided lower μTBS values (20.7±2.7) restorative procedures. Self-etching bond systems were introduced in order to reduce the sensitivity of techniques that affect the bonding ability of adhesive systems; theyE. J. Souza-Junior also decrease the number of steps in the bonding approachDepartment of Restorative Dentistry, Dental Materials Area, because they include acidic monomers that simultaneouslyPiracicaba Dental School, University of Campinas (UNICAMP), etch and prime both enamel and dentin [1, 2]. The absenceAreião, SP, Brazil of the rinsing approach and partial removal of the smearC. T. P. Araújo : L. T. Prieto layer and smear plugs with these adhesives lead to lessDepartment of Restorative Dentistry, Operative Dentistry Area, technique-sensitive, time-consuming procedures, and con-Piracicaba Dental School, University of Campinas (UNICAMP), sequently, a possible reduction of postoperative sensitivityAreião, SP, Brazil results [2–5].E. J. Souza-Junior (*) : L. A. M. S. Paulillo Moreover, a recent study has shown that enamel smearDepartment of Restorative Dentistry, Piracicaba Dental School, layer compromises bonding by mild self-etch adhesives [6].University of Campinas (UNICAMP), Separate preliminary etching is known to remove the smearAvenida Limeira, 901,Areião 13414-903 52 SP, Brazil layer created by instrumentation and to demineralize thee-mail: edujcsj@gmail.com dental substrate. The prior enamel phosphoric acid etching
  4. 4. Authors personal copy Lasers Med Scias an additional step for self-etch adhesives has been units on dentin microtensile bond strength (μTBS) of self-proposed to improve the durability of the enamel bond [7– etching bond systems in class I composite restorations. The10]. Hence, the selective enamel etching increases marginal first hypothesis tested was that the previous enamel etchingadaptation of self-etch adhesives as evidenced by numerous would not affect microtensile bond strength values of thestudies [4, 5, 11–14]. tested adhesive systems. The second hypothesis was that While it is clear that selective enamel etching may have the third-generation polywave LED would present highersome beneficial effects on marginal integrity in class V dentin bond strength values for the tested bond systems.cervical lesions [5, 11, 13], the literature provides noevidence for the bonding performance of self-etchingadhesives in class I cavities for direct composite restora- Materials and methodstions in vitro. Since class V cervical lesions restorationspresent smaller amounts of dental enamel, it may not be the LED curing unitsbest model for understanding the real effects of enameletching on dentin substrate and the stress development on Three light-emitting diodes (LEDs) were tested: FlashLitethe tooth/adhesive interface, like class I restorations [13, 1401 (FL) (Discus Dental, Culver City, CA, USA), Radii-15]. In this sense, the literature gives no evidence about the Cal (RD) (SDI Limited, Victoria, Australia) and UltraLumerole of prior enamel acid etching on the bond strength of LED 5 (UL) (Ultradent, South Jordan, Utah, USA).self-etch adhesives to dentin in class I cavities in vitro. Characteristics of the LCUs used in this work are presented It is important to consider when restoring class I cavities in Table 1. Irradiance (mW/cm2) was measured dividing thewith self-etch bond systems is the selection of an efficient output power (measured by a calibrated power meter -light curing unit (LCU). The LCU should guarantee a Ophir Optronics, Har – Hotzvim, Jerusalem, Israel) by thesatisfactory monomer conversion of the adhesive and resin tip end area of the LCUs. The spectra of the LED units wascomposite. Consequently, it may improve the material’s measured with a calibrated spectrometer (USB2000, Oceanphysical and mechanical properties, such as ultimate tensile Optics, Dunedin, FL, USA), as shown in Fig. 1. The energystrength and bond strength to dental substrate [16–20]. dose was standardized to approximately 11 J/cm2 for theLight emitting diodes (LEDs) have been shown to bonding systems curing approach and 22 J/cm2 for the cureeffectively cure composites and dental adhesives, emitting of each composite increment. Because the RD light sourceunfiltered blues light [17, 21]. These LCUs generate a mandatorily operates in ramp mode for 5s, these initialnarrow spectral range that targets the absorption wave- seconds were discarded and further application was realizedlength of camphorquinone, yielding low amounts of wasted in order to maintain the standardized irradiance, conse-energy and minimum heat generation [22, 23]. quently equaling the energy density obtained for each of the Previous studies have shown that current LED curing LCUs.units can replace, in most situations, the conventional QTHlight units [24–26]. Some adhesive systems are not well Specimen preparationcured with single-peak LEDs [21] due to alterative photo-initiators content; to overcome this problem, polywave Ninety-six freshly extracted, sound human molars werethird-generation LEDs were introduced to the market [24– selected. This study had the approval of the Ethical26]. These LEDs emit light wavelengths targeting the Committee of the State University of Campinas, Piracicabaabsorption peak of camphorquinone. However, they deliver Dental School. The teeth were cleaned, their roots insertedadditional light output at the UV-Vis region of the in polystyrene resin and the occlusal surfaces wet polishedelectromagnetic spectrum (400–415 nm). The second peak with 320-grit SiC paper under running water (Politriz,in the UV-VIS region may promote a satisfactory cure of AROTEC – São Paulo, SP) in order to expose a flat enamelthese adhesives, containing alternative photoinitiators sys- surface without exposing dentin. Box-shaped class Items, such as phenyl propanedione (PPD), bis-alquyl cavities were prepared using #56L diamond burs (KGphosphinic oxide (BAPO) and trimethylbenzoyl-diphenyl- Sorensen, Barueri, SP, Brazil) at high-speed, under air–phosphine oxide (TPO) [26]. This point is crucial because water cooling. A custom-made preparation device allowedsome manufacturers do not state all of the photoinitiator the standardization of the cavity dimensions to 5-mmsystems used in their proprietary products, [25, 27] and the mesio-distal length, 5-mm bucco-lingual width, and 3-mmselection of an adequate LCU is primordial to yielding an depth, all cavity margins on enamel substrate. The used buradequate adhesive polymerization and resin/dentin bond was replaced after four-cavity preparation.strength. After cavity preparation, the teeth were assigned to 12 Thus, this study aimed to investigate the influence of groups (n=8) according to the three studied factors:selective enamel acid etching and different LED curing selective enamel etching, bond system and curing light (2
  5. 5. Authors personal copyLasers Med SciTable 1 Characteristics of the LCUs used in this studyLCU Manufacturer Type Tip diameter Irradiance Radiant exposure (mm) (mW/cm2) (J/cm2)FlashLite 1401 Discus Dental, Culver City, CA, USA Single-peak 7 1077 22Radii Cal SDI Limited, Victoria, Australia Single-peak 7 731 22UltraLume LED 5 Ultradent products Inc, South Jourdan, Utah, USA Polywave 11 x 7 800 22conditioning protocols x 2 adhesives x 3 LEDs). Two self- interface. This sectioning was done with a diamond sawetch adhesive systems (two-step and one-step) were used (Isomet 1000, Buehler Ltd, Lake Bluff, IL, USA) at 300for the bonding procedure: Clearfil Tri-S Bond (pH=2.7; rpm to obtain sticks with a cross-sectional area ofKuraray Medical Inc., Tokyo Japan) or Clearfil SE Bond approximately 0.9 mm2. The cross-sectional area of each(pH = 2.0; Kuraray Medical Inc., Tokyo Japan). The stick thus was measured with the digital caliper to thecomposition, application mode, and batch number of the nearest 0.01 mm and recorded for the bond strengthadhesive systems are presented in Table 2. All groups were calculation. The bonded sticks originated from the samerestored with B1-shade Charisma microhybrid composite teeth were assigned to the tested groups. Sticks were(Heraeus Kulzer, Hanau, Germany) using an incremental individually attached to a jig for microtensile testing withoblique technique with increments approximately 2 mm cyanoacrylate resin (Super Bond gel, Loctite, Henkel,thick. Then, the finishing and polishing procedures were Brazil) and subjected to a tensile force in a universalperformed with medium-, fine-, and extra fine-grit alumi- testing machine (EMIC DL500, São José dos Pinhais,num oxide disks (Sof-Lex – 3M/ESPE), respectively. After Brazil) at a crosshead speed of 0.5 mm/min until failure.polishing, the specimens were submitted to 200,000 Bond failure modes were evaluated with a scanningmechanical loading (2 Hz) and 500 thermal cycles (ranging electron microscope (JEOL, JSM-5600LV, scanning elec-from 5 to 55°C with a dwell time of 60 s in each bath with tron microscope, Japan) and classified as: (1) cohesivean interval of 5 s) at a thermo-mechanical device ER-11000 (failure exclusive within dentin or resin composite, (2)(ERIOS, São Paulo, Brazil) in order to simulate similar adhesive (failure at resin/dentin interface or cohesive inageing of the composite restorations in oral environment adhesive resin) or (3) mixed (mixed with cohesive failure ofconditions. the neighboring substrates). The obtained data were subjected to a three-way ANOVA and Tukey’s test at aMicrotensile bond strength pre-set alpha of 0.05.After storage in distilled water at 37ºC for 24 h, specimensassigned to the MTBS test were longitudinally sectioned in Resultsboth “x” and “y” directions across the pulpal wall bonded Microtensile bond strength Approximately 16 sticks could be obtained per tooth, including those with premature debonding. Pre-test failures were included in the statistical analysis as half of the minimum bond strength measured for each tooth [27]. The results of μTBS are shown in Tables 3 and 4. The double interactions between the factors adhesive x selective etching (p≤0.05) and adhesive x LED light (p≤0.05) were statistically significant. Phosphoric acid-etching pre-treatment of enamel prior to application of S3 led to lower dentin μTBS values (p≤ 0.05). However, for CSE, the pre-etched enamel yielded a similar dentin μTBS mean compared to the non-etched specimens. Dentin bond strength of CSE did not statisti- cally differ from S3 when prior etching was used before the adhesive application. Moreover, when these adhesives wereFig. 1 The spectrum range distribution of each LCU used in this study applied following the conventional approach, S3 presented
  6. 6. Authors personal copy Lasers Med SciTable 2 Composition, application mode, and manufacturer’s information for the adhesive systems testedAdhesive systems Composition Application modeClearfil SE Bond Primer (Batch #00896A): water, MDP, HEMA, Selective H3PO4 conditioning for 15 s. Rinse with water (Kuraray Medical camphorquinone, hydrophilic dimethacrylate. spray for 10 s, leaving the tooth dry. Apply primer for Inc., Tokyo, Japan) Adhesive (Batch #01320A): MDP, bis-GMA, HEMA, 20 s. Mild air stream. Apply bond. Gentle air stream. camphorquinone, hydrophobic dimethacrylate, N,N- Light cure at an energy density of 11 J diethanol p-toluidine bond, colloidal silicaClearfil S3 Bond Adhesive (Batch #00116A): MDP, Bis-GMA, HEMA Selective H3PO4 conditioning for 15 s. Rinse with water (Kuraray Medical hydrophobic dimethacrylate, dl-camphorquinone, spray for 10 s, leaving the tooth dry. Apply the bond Inc., Tokyo, Japan) silanated colloidal silica, ethyl alcohol, and water system for 20 s. Gentle air stream for 10 s. Light cure at a energy density of 11 J.higher bond strength mean in comparison to the two-step step on the bond strength approach to pulpal dentin inself-etch adhesive. class I composite restoration has not been clarified. In All LED curing units promoted similar dentin μTBS for this sense, the selective etching increases the free surfacethe one-step self-etch bond system S3 (p≥0.05). In contrast, energy of the enamel substrate and favors mechanicalthe two-step CSE showed higher dentin μTBS (24.1±3.2) interlocking with the bonding resin [28]. In this study, thewhen UL was used in comparison to the single-peak LEDs bonding ability of self-etch adhesives to pulpal dentin withFL (18.8±3.9) and RD (19.9±1.8). different application approaches was evaluated in class I The descriptive analysis of the failure mode for each restorations. These class I preparations frequently present aadhesive is shown in Table 5 and 6. SEM evaluation of the thick enamel layer on the cavosurface angle surrounding allfractured surfaces showed predominant adhesive failures the restoration margins, compared to a class V or a class IIIfor CSE when the enamel prior acid etching was used for cavity. In contrast, there are many studies evaluating thethe bonding approach (Fig. 2). A similar failure mode was bonding performance of self-etch adhesives and prior acidfound for S3 in the same condition. However, when the etching on flat enamel surfaces [29–31]. These circum-self-etch adhesives were conventionally used, mixed fail- stances do not simulate clinical situations for direct compos-ures were present (Fig. 3), and one cohesive failure was ite application because the bond performance of dentalshown on composite for CSE when photocured with FL. adhesives occurs with the shrinkage stress influenced by theFigure 4 shows osmosis-induced droplets due to the cavity configuration and the restoration is surrounded byadhesive hydrophilicity for Clearfil S3. different dental substrates [32, 33]. Based on the results, the first hypothesis tested was partially validated, since for CSE, the previous acid etchingDiscussion did not influence the μTBS results. In contrast, S3 adhesive showed lower dentin μTBS when this additional etchingThe selective enamel etching is related to increased step was performed. The conventional application of thebond performance of self-etch adhesives to ground self-etch adhesive generally ensure good retention perfor-enamel [8, 9]. However, the influence of this additional mance for dentin and a poor bonding approach for enamelTable 3 Means and standard deviation of the microtensile bond Table 4 Means and standard deviation of the microtensile bondstrength for the interaction between adhesive system and selective strength for the interaction between adhesive system and light curingetching unitAdhesive system Selective acid etching Adhesive system Light curing unit Etching No etching FlashLite 1401 Radii Cal UltraLume 5Clearfil SE bond 20.3 (3.3) Bb 21.6 (3.2) Bb Clearfil SE bond 18.8 (3.9) Bb 19.9 (1.8) Bb 24.1 (3.2) AaClearfil S3 20.7 (2.7) Bb 26.7 (2.2) Aa Clearfil S3 24.1 (2.8) Aa 23.2 (3.4) Aa 23.5 (3.8) AaMean values followed by different small letters in the column and Mean values followed by different small letters in the column andcapital letters in the row differ statistically among themselves for the capital letters in the row differ statistically among themselves for theTukey test at the level of 5% Tukey test at the level of 5%
  7. 7. Authors personal copyLasers Med SciTable 5 Percentage of specimens (%) from Clearfil SE bond adhesive distributed according to the failure modeLCU Prior phosphoric acid etching Without prior phosphoric acid etching A M C A M CFlashLite 1401 75 25 0 64 24 1Radii Cal 100 0 0 100 0 0UltraLume LED 5 60 40 0 70 30 0A adhesive failure and cohesive failure within the adhesive; M mixed failure; C cohesive failure within dentin or composite resin[5, 28, 31]. Thus, the slightly inferior enamel bonding therefore an important bonding behavior since gap forma-performance may yield minor stress at the margins, tion represents the first sign of restoration failure, whichresulting in fewer gaps and paramarginal enamel fractures can be clinically evidenced by marginal staining [5, 8, 11,[15]. However, when enamel is pre-etched before the self- 34, 35]. However, the S3 can promote a small decrease inetch adhesive application, higher bond strength between the bonding ability of this single-step adhesive to theenamel/adhesive and resulting stress may occur and retention on the pulpal dentin. Therefore, for a gold-consequently affect dentin bond performance. The enamel standard CSE, it is assumed that prior acid etching canselective etching for the S3 application may have caused promote better marginal sealing without compromising thehigher stress and bond strength for the enamel substrate, dentin μTBS.especially due to its ultra-mild pH characteristic, while the The impact of the adhesive bonds to the dental substrateadhesive layer bonded to dentin might have disrupted and of composite restorations is strongly related to LCUdecreased the dentin μTBS. efficacy, which will promote satisfactory materials poly- In addition, the stress might have been enhanced due to merization [21]. LED technology has been used forthe thermal and mechanical ageing promoted to the class I resinous materials polymerization as a substitute forrestorations, favoring the decrease in the retention values. conventional QTH curing lights [36, 37]. However, theThe failure mode was mainly adhesive when the previous conventional single-peak second-generation LEDs stillacid etching was performed for S3; therefore, mixed harm the cure of dental resins due to the narrower spectrafailures were more present when this adhesive was used emitted to the camphorquinone initiator [38–40]. They doin the conventional way. For the CSE, the application of the not allow an optimal cure for other photosensitizes, likehydrophobic resin layer may have supported the stress phenyl propanedione and TPO, present in some dentalpromoted by enamel selective etching, but did not affect the materials [26]. Polywave LEDs were introduced in order todentin μTBS when compared to the unique layer applied overcome these concerns, promoting the conversion of thisfor the S3. It is suggested that previous enamel etching UV–Vis photoinitiator content [24–26].needs to be considered for S3 in restorations whose In the present work, the second hypothesis was partiallyretention primarily depends on a strong bond to the enamel validated, since for CSE, the polywave third-generationsurface, such as large class III and IV or veneer restorations. LED UL promoted higher dentin μTBS values compared to In recent studies [5, 11, 14, 31], selective enamel etching the single-peak second-generation ones. However, S3was shown to improve marginal integrity of composite presented similar dentin bond strength regardless of therestorations using either a two-step or a one-step self- LCU used. For CSE, the results are in accordance withetching adhesive. The decrease in marginal gaps is some authors [21, 41] who observed that single-peak LEDsTable 6 Percentage of specimens (%) from Clearfil S3 adhesive distributed according to the failure modeLCU Prior phosphoric acid etching Without prior phosphoric acid etching A M C A M CFlashLite 1401 80 20 0 50 50 0Radii Cal 70 30 0 66 34 0UltraLume LED 5 85 15 0 60 40 0A adhesive failure and cohesive failure within the adhesive; M mixed failure; C cohesive failure within dentin or composite resin
  8. 8. Authors personal copy Lasers Med Sci Fig. 4 SEM observation of Clearfil S3 - osmosis induced droplets due to the adhesive hydrophilicity, especially because of the presence ofFig. 2 SEM of the fractured specimen showing a pure adhesive HEMA. It is not a phase separation droplets, because this adhesive dofailure within the bonding interface not present phase separation – Clearfil S3promoted a lower degree of cure for CSE compared to aLCU with a large spectrum range distribution, comprising curing light may have excited the material’s photoinitiatorthe UV–Vis wavelength. This finding may be attributed to content. Nevertheless, the energy dose for all LEDs wasthe photoinitiator content of CSE; the manufacturer may standardized at approximately 11 J/cm2 for the bondingomit the presence of other photosensitizers that may have system, which may have delivered the same quantity oflarger spectrum ranges that comprise the UV–Vis region. photons to allow the satisfactory cure of S3. Consequently,Another possible explanation is that the absorption peak of similar dentin bond strength values were achieved, regard-camphorquinone can be moved to lower wavelengths. The less of the spectrum range and irradiance of the LCUs.LED unit continues to deliver shining light because the Although the etching approach for self-etch adhesives isstructural part of this initiator, responsible for the short- recommended by many authors [4, 5, 11–14], the inclusionwavelength absorption, remains unchanged while the of an additional step for these bond systems may bephotoreaction at the initial maximum absorption peak controversial, since these adhesives intend to represent a(468 nm) ends [42]. It may contribute to better bond clear simplification of the clinical application of bondstrength values with the polywave LED UL, which have systems. In this sense, the adverse points of this selectivebroader emission spectra, and it may have promoted a approach include the increase of the bonding steps and thebetter monomer conversion compared to the single-peak technique sensitivity [13].ones. However, it is questionable whether 10–20 s of light Although some in vitro studies exist, final conclusionsactivation is sufficient to enable this effect. regarding the role of the enamel selective acid etching for The dentin bond strength of S3 was not affected by the self-etch adhesives in class I composite restorations willLCU used. A thin adhesive layer was applied onto the depend on the outcomes of clinical trials. Clinical long-termenamel and dentin surface of the class I preparation, and the studies and investigations of this approach’s retention ability for bond systems in the oral environment can best evaluate the quality and durability of these restorations. Conclusions The additional selective enamel acid etching in class I composite restorations does affect the dentin bond strength of the ultra-mild one-step self-etch adhesive Clearfil S3. However, this selective step does not affect the bond performance of the two-step self-etch bond systems Clearfil SE. The polywave LED promoted better bond strength for the two-step adhesive when compared to the single-peakFig. 3 SEM of the fractured specimen showing mixed failure within ones. Moreover, all LCUs presented similar cure potentialcohesive in adhesive layer and hybrid layer adhesive failure for the one-step self-etch adhesive.
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