+

Journal of Dental Sciences (2013) xx, 1e10

MODEL

Available online at www.sciencedirect.com

journal homepage: www.e-jds.com

ORIGINAL ARTICLE

Push-out bond strength and SEM analysis of two self-adhesive resin cements: An in vitro study
Bogdan Baldea a, Gabriel Furtos b, Mark Antal c, Katalin Nagy d, Dragos Popescu e, Luminita Nica f*
a

Department of Prosthodontics, Faculty of Dental Medicine, Victor Babes University of Medicine and Pharmacy, 9 Revolutiei 1989 Avenue, 300070 Timisoara, Romania b Department of Dental Materials, Raluca Ripan Institute of Research in Chemistry, 30 Fantanele Street, 400294 Cluj-Napoca, Romania c Department of Operative and Esthetic Dentistry, Faculty of Dentistry, University of Szeged, Tisza Lajos Korut 64, H-6720 Szeged, Hungary d r 13, H-6720 Szeged, Hungary Department of Oral Surgery, Faculty of Dentistry, University of Szeged, Dugonics te e Private Dental Clinic, 72 Martir Petru Domasneanu Street, 300351 Timisoara, Romania f Department of Endodontics, Faculty of Dental Medicine, Victor Babes University of Medicine and Pharmacy, 9 Revolutiei 1989 Avenue, 300070 Timisoara, Romania Received 6 November 2012; Final revision received 28 December 2012 Available online - - -

KEYWORDS
ber posts; push-out bond strength; root canal dentine; self-adhesive resin cements

Abstract Purpose: The retentive strength of two self-adhesive resin cements used for the cementation of ber posts into root canals lled with methacrylate-based sealer and core material (Resilon) was evaluated using the thin-slices push-out test on human molars. Materials and methods: RelyX Fiber Posts #3 (3M ESPE, Seefeld, Germany) were luted with RelyX U200 (3M ESPE) (n Z 10) and Maxcem Elite (Kerr Corporation, Orange, CA, USA) (n Z 10). Mean values of push-out bond strength for each group and root region (cervical, middle and apical) were calculated. Data were statistically analyzed with one-way ANOVA and Tukeys test (P < 0.05). Failure modes were evaluated using optical microscopy and scanning electron micrography (SEM). Results: Without being statistically signicant, the bond strength of RelyX was higher (8.23 4.46 MPa) when compared to that of Maxcem Elite (6.52 3.68 MPa). Conclusions: Signicant differences (P < 0.05) were observed between the apical and cervical regions. More frequent (>60%) adhesive failures at the resin cement-dentine interface were observed. Copyright 2013, Association for Dental Sciences of the Republic of China. Published by Elsevier Taiwan LLC. All rights reserved.

* Corresponding author. Department of Endodontics, Faculty of Dental Medicine, Victor Babes University of Medicine and Pharmacy, 9 Revolutiei 1989 Avenue, 300070 Timisoara, Romania. E-mail address: [email protected] (L. Nica). 1991-7902/$36 Copyright 2013, Association for Dental Sciences of the Republic of China. Published by Elsevier Taiwan LLC. All rights reserved. http://dx.doi.org/10.1016/j.jds.2013.01.007

Please cite this article in press as: Baldea B, et al., Push-out bond strength and SEM analysis of two self-adhesive resin cements: An in vitro study, Journal of Dental Sciences (2013), http://dx.doi.org/10.1016/j.jds.2013.01.007

+
2

MODEL

B. Baldea et al University of Medicine of Timisoara. After extraction, the teeth were cleaned of soft tissue and calculus and stored in 0.1% thymol solution steam at 9 C. Before use, teeth were washed under running water for 24 hours, blot dried and stored in normal saline at 37 C and 95% humidity until testing.3 The crowns were sectioned 2 mm occlusally, above the cemento-enamel junction (CEJ), with a low-speed diamond saw (IsoMet 1000, Buehler Ltd., Lake Bluff, IL, USA) with water cooling (Fig. 1A), which exposed the pulp chamber. The pulp chambers were opened completely, the dental pulp was removed and the root canal preparation was completed (Fig. 1B) with a size-40 master apical le, 10% taper, using a crown-down motion and nickel-titanium (NiTi) rotary GT instruments (Dentsply Tulsa Dental, OK, USA). The tooth samples in which the size and shape of the root canal were different from that of the post were excluded from the beginning of the study and were not endodontically treated. All procedures were performed using the OPMI Pico (Carl Zeiss AG, Oberkochen, Germany) dental operating microscope. Irrigation was performed during instrumentation with sodium hypochlorite (NaOCl) 5.25%, which was delivered through the master delivery tip (MDT) of the EndoVac system (Discus Dental, Culver City, CA, USA) until the endodontic preparation was completed. The macrocannula of the EndoVac system was then used for a 30 second period of irrigation with 5.25% NaOCl. The canal was then left full of irrigant for 30 seconds. Three cycles of micro irrigation using the microcannula placed at full working length followed. These involved the use, alternatively, of 5.25% NaOCl and 17% ethylenediaminetetraacetic acid (EDTA) solution.7 Finally, another cycle of micro irrigation using EDTA as the nal irrigant was performed, because the teeth were adhesively obturated using Resilon core material (Epihany, Pentron Clinical Technologies LLC) and Epiphany SE (Pentron Clinical Technologies LLC) as sealer. The canals were then rinsed with distilled water and dried with paper points. Epiphany SE sealer (Pentron) was applied to the root canals using ne-medium paper points (Dentsply Maillefer, Ballaigues, Switzerland). Epiphany core material was injected to the full working length from a 27-gauge needle from the Obtura III System (Obtura Spartan, Fenton, MO, USA) set at 140 C and compacted using special handpluggers (Obtura S-Kondensors, Obtura Spartan) in three waves of injection-compaction, until the root canals were lled to the coronal orice on the pulp chamber oor (Fig. 1B). The llings were light-cured for 40 seconds according to the manufacturers instructions. The access cavities were sealed with a temporary cement (Coltosol, Coltene Whaledent, Mahwah, NJ, USA), and the specimens were stored in humidity at 37 C for 48 hours, to allow for complete setting of the sealer as in previous studies. Post space preparation A 9-mm deep post space was prepared in the palatal root of the maxillary molars (Fig. 1C) and in the distal root of the mandibular molars, with a precalibrated size-3 drill (3M ESPE, Seefeld, Germany) to match the size of the corresponding RelyX Fiber Post (3M ESPE) # 3 (1.9 mm in diameter). The canals were rinsed with 17% EDTA solution for 1 minute, using the EndoVac system, then with de-ionized water until they appeared completely free of debris or

Introduction
Prefabricated composite resin ber posts have been used for the restoration of endodontically treated teeth since the 1990s, when carbon ber posts, with an elastic modulus similar to dentine, were introduced.1 Adhesively luted ber-reinforced composite (FRC) posts were introduced in 1997 and have increasingly been used since then for the restoration of endodontically treated teeth.2 The retention of ber posts in root canals is dependent upon adhesion between the resin cement and the dentine, as well as on adhesion between the resin cement and the posts. However, the adhesion between the resin cement and the dentine is considered to be the weak point in luting a ber post.3 Although bonding between the post and the root canal dentine plays a pivotal role in the long-term success of a restoration, ensuring reliable bonding between the post and the composite core is also necessary. If the bonding of that interface is poor, de-bonding and/or fracture of the core and post can occur.4 Successful bonding minimizes the wedging effect of the post within the root canal and requires less dentine removal to accommodate a shorter and thinner post; in addition, it leads to lower susceptibility to tooth fracture.1 Bonding to root canals might be difcult, because of the handling characteristics of the adhesive system, root anatomy, tooth position, the presence of coronal residual tissue, the use of a light-curing technique, the experience and skill of the operators, etc.5 Self-adhesive cements were introduced in 2002 as a new subgroup of resin cements.6 They were designed with the intent of integrating the favorable characteristics of different cement classes into a single product.6 Their main advantage is the simplicity of clinical use. These cements are expected to offer properties analogous to those of resin cements. The aim of the present study was to evaluate the pushout bond strength of two new self-adhesive resin cements (SARCs) used for luting glass ber posts into endodontically treated root canals lled with methacrylate resin-based sealer (Epiphany SE, Pentron Clinical Technologies LLC) and core material (Resilon Epiphany, Pentron Clinical Technologies LLC). The failure modes were examined by optical microscopy, and different interfaces of randomly selected samples were evaluated with scanning electron micrography (SEM) after the push-out test. The null hypotheses tested were as follows: (1) the type of resin cement does not affect bond strength and (2) the region of the post/root canal does not inuence bond strength.

Materials and methods

Specimen preparation
Sample preparation and root canal lling Twenty recently extracted, non-carious human maxillary and mandibular molars, with one straight palatal or distal root canal and fully developed apices, extracted for periodontal reasons, were selected for this study. All patients provided their informed consent. The study was approved by the Commission on Bioethics of the Victor Babes

Please cite this article in press as: Baldea B, et al., Push-out bond strength and SEM analysis of two self-adhesive resin cements: An in vitro study, Journal of Dental Sciences (2013), http://dx.doi.org/10.1016/j.jds.2013.01.007

+
Push-out bond strength of two resin cements

MODEL

Figure 1 Schematic drawing of the specimen preparation procedure for the push-out bond strength test on 1 mm thick slices. (A) The crowns were removed 2 mm above the cemento-enamel junction (CEJ). (B) After the cleaning-shaping procedure, an adhesive root canal lling was performed. (C) Preparation of the post-space with pre-calibrated burs. (D) Cementation of the ber post into the root canal. (E) Six slices were obtained from each root canal. (F) Cervical, middle and apical regions of the root canal, each containing two slices, were evaluated for push-out.

residual lling material under the dental operating microscope (OPMI Pico) and dried with paper points (Dentsply Maillefer). Fiber post luting procedure The teeth (n Z 20) were divided to two groups according to the SARC used for cementation of the posts in the root canals: Group I - RelyX U200 (RXU2) (3M ESPE, Seefeld, Germany) and Group II - Maxcem Elite (MAX) (Kerr Corporation, Orange, CA, USA). Each of the SARCs was used in the dual-cured mode. A small amount of cement was applied to the root canal with a lentulo spiral ISO #40 (Dentsply Maillefer). An additional amount of cement was applied on the ber post, to ensure sufcient cement lling, and then the post was xed (Fig. 1D) into the root canal. While the post was loaded under nger pressure, the excess cement was carefully removed with a spatula and 40 seconds of light polymerization through the translucent ber post with a Valo LED curing light device (Ultradent Products Inc., South Jordan, UT, USA) at 1000 mW/cm2. Five minutes of the auto-curing mode followed. The free portion of the post and coronal dentine was treated with a self-etch adhesive (Adper One Bond Self-Etch Adhesive, 3M ESPE), and the core build-up was performed with a light-curing resin composite material (Filtek Supreme XT, 3M ESPE). A free portion of the ber post, extruding 3 mm from the build-up material, was left to conrm the direction of the post in the root canal. Digital periapical radiographs were taken to assess the quality of the root canal lling and the post and core build-up procedure, in the buccolingual and mesiodistal directions, to detect cracks extending into the roots. The specimens were stored at room temperature, in a ower sponge slightly moistened with deionized water, for 1 week, to prevent dehydration until the push-out test was performed. Push-out test specimen preparation Perpendicular to the post and to the long axis of the root canal, six sections of 1 mm height were cut from each specimen, using a saw microtome (IsoMet 1000), starting at 1 mm from the tip of the post (Fig. 1E). The tested samples did not include the slices with the post into the pulp

chamber, because in this region, the post might have an angulation with the dentinal walls. For each specimen, a total of six sections with the form of an inverted cone were obtained: two were classied as coronal, two as middle and two as apical, according to the position of the post in the root canal (Fig. 1F). The diameter of the post was determined in triplicate on both surfaces (apical and coronal) of each slice using a stereomicroscope (Stemi 2000-C, Carl Zeiss AG), and the readings were averaged for each surface. The height of each section (H) was determined using a micrometer screw (Mitutoyo Messgerate GmbH, Neuss, Germany). The adhesive surface (A) of the post was calculated using Equation 1 8,9: AZ3:14 L R1 R2 Equation 1

where A is the adhesive surface (mm2), L is the slant height of the inverted cone (mm), R1 is the smaller base radius of the post (mm) and R2 is the larger base radius (mm) (Fig. 2). The slant height was calculated using Equation 2 8,9: i1=2 h LZ H2 R2 R1 2 Equation 2

where H is the height of the inverted cone (Fig. 2).

Figure 2 Schematic representation of the 1 mm thick post section used for calculation of the adhesive surface.

Please cite this article in press as: Baldea B, et al., Push-out bond strength and SEM analysis of two self-adhesive resin cements: An in vitro study, Journal of Dental Sciences (2013), http://dx.doi.org/10.1016/j.jds.2013.01.007

+
4

MODEL

B. Baldea et al

Push-out bond strength test Push-out bond strength was tested on each slice with the help of a 0.70 mm thick cylindrical at end stylus attached to a testing machine (Lloyd Instruments Ltd, West Sussex, UK). A stainless steel support (Fig. 3) was used to hold the specimens in the testing machine, in such a way that the side with the smaller diameter faced upward. The force of the cylindrical plunger of the testing machine was used to dislodge each inverted, truncated ber post section from the root dentine in an apical-coronal direction. A constant load (0.5 mm/minute) was then applied only to the post surface (Fig. 3), until a bond failure occurred at one of the interfaces.10 The retentive strength (S) (MPa) of the post fragment was calculated by dividing the load at failure (F) (N) to the interfacial area (A) of the post segment (mm2) using Equation 3 8,9: SZF=A Equation 3

Statistical analysis
The data were statistically analyzed by using the SPSS software package (Version 11.5, SPSS Inc., Chicago, IL, USA). Subsequent comparisons between groups were performed with Tukeys post-hoc analysis, with the level of signicance set at 0.05, to determine the statistically signicant differences between the mean values of the materials tested. The results achieved, using the push-out test, were compared among three parts of the root canal corresponding to the section regions (cervical, middle and apical parts).

Results
When the push-out bond strength values of all three regions (apical, middle, and cervical) were pooled, the mean values for each group of material were obtained (Table 1). The mean push-out bond strength of RelyX U200 varied between 8.23 4.46 MPa and was higher than that of Maxcem Elite, for which the values were 6.52 3.68 MPa, but no statistically signicant differences between the groups were recorded (P > 0.05). Instead, statistically different mean values were observed between different regions of the analyzed specimens belonging to Group I (RXU2): the apical region, where the highest mean value recorded was 9.55 MPa, and the cervical region, with a mean value of 4.68 MPa (P < 0.05). In this group, a constant decreasing trend was observed for the mean values of push-out bond strength, when traveling from apical to cervical regions. In Group II (MAX), no statistically signicant differences (P > 0.05) among the three regions of the analyzed samples were recorded, with the highest push-out bond strength values obtained in the middle third, at 7.38 MPa. The failure modes were analyzed for both groups using stereomicroscopy (40) (Fig. 4) and expressed as a percentage of the total number of evaluated samples for each group. The predominant failure mode, observed in >70% of the samples in Group I and in 63% of the samples in Group II, was represented by adhesive failures at the resin cement/ dentine interface followed by adhesive failures between resin cement/dentine and resin cement/post (mixed failures). Clear adhesive failures between the ber post and the resin cement were observed just in a small percentage: 11.36% for RXU2 and 14.63% for MAX. The percentages of failures in each root region for both materials are represented in Fig. 6. Almost the same percentage of adhesive failures at the resin cement/dentine interface was observed in each of the examined thirds for both groups, recording the highest values. The mixed type of failures (Fig. 5) occurred more frequently in the apical third for the RXU2 group, while for the MAX group, adhesive failures between post/cement were more frequently observed also in this third. Cohesive failures inside the post (4.54%) were observed just in the middle root region of the RXU2 group (Fig. 4F). SEM evaluation revealed numerous resin tags formed by the Epiphany SE sealer, with the intratubular dentine in some of the areas analyzed (Fig. 7A). Cohesive failures inside the post with detached glass bers could be observed

After the push-out test, the failure modes of each specimen on both surfaces, were evaluated by a single operator under a stereomicroscope (Stemi 2000-C, Carl Zeiss AG) at 40 magnication and classied as follows: A Z adhesive failures between the dentine and the resin cement; B Z adhesive failures between the post and the resin cement; C Z cohesive failures within the post; M Z mixed failures (between the dentine-resin cement and between the post cement). No cohesive failures were recorded in either dentine or cement, so these failure modes were not included in the classication. SEM evaluation Ten randomly selected specimens from each group, with their corresponding posts, were prepared for SEM observation, under a scanning electron microscope (SEM Quanta 3D FEG D9399, FEI Company, Eindhoven, the Netherlands). After cleaning with ultrasonic running deionized water for 10 minutes, the specimens were demineralized with a phosphoric acid 37% solution for 20 seconds, mounted on stubs and gold sputter-coated (Bio-Rad Polaron Division SEM Coating System, Polaron Instruments Inc, Agawan, MN, US). The fractured specimens were inspected for different interfaces. The sites of failure and voids, cracks and failure patterns were observed, and the formation of resin tags was analyzed.

Figure 3 Schematic diagram of the push-out test procedure on 1 mm thick tooth slices.

Please cite this article in press as: Baldea B, et al., Push-out bond strength and SEM analysis of two self-adhesive resin cements: An in vitro study, Journal of Dental Sciences (2013), http://dx.doi.org/10.1016/j.jds.2013.01.007

+
Push-out bond strength of two resin cements
Table 1

MODEL

Mean values of the push-out bond strength (MPa) and the standard deviation (SD). Push-out bond strength MPa (SD) Mean value Apical 8.23 (4.46)b 6.52 (3.68)b 9.55 (4.74)a 5.93 (3.04) Region Middle 8.25 (3.50) 7.38 (3.38) Cervical 4.68 (3.42)a 6.41 (5.30)

Experimental groups

RelyX U200, 3M ESPE Maxcem, KERR

a b

Mean values with a statistically signicant difference from each other, when compared using Tukeys test, (P < 0.05). No signicant differences, when compared using Tukeys test (P > 0.05).

(Fig. 7B), but only in a small percentage of the samples. Adhesive failures between the post and the cement and between the cement and the dentine were observed in both groups (Fig. 7CeF). Fractured resin tags in contact with the dentine could be observed in the RXU2 group (Fig. 7F).

Discussion
The present study showed that the type of resin cement used did not signicantly inuence the strength of the bond to the root canal dentine, although higher mean values were recorded for RelyX U200 (P > 0.05). The push-out bond strength was higher at the apical post/root canal region than at the middle and cervical thirds only in the RXU 2 group (P < 0.05). A variety of experimental tests has been described for evaluating the strength of the bond between the root canal dentine and the ber posts, such as the pull-out test,11 the microtensile test,12,13 and the push-out test.10,14 In the present study, the push-out test was performed using 1 mm thick tooth slices, because this approach offers the advantage of smaller adhesive areas, which help to avoid the difculties of microtensile specimen preparation.8,10,15 The technique has been reported as an important experimental tool with which to evaluate the mechanical properties of the interfaces9,10 due to its precision. Cylindrical or conical ber posts may be used in the push-out test procedure. In both cases, the result is a complex stress distributed at the interface between the dentine and the resin cement and between the post and the cement, with a shear stress component.10,14 Cylindrical posts used in the push-out test have been reported in some studies to increase the risk of friction.16 Conical ber posts with a shape more appropriate for root canal preparation will eliminate some of the friction between the resin cement and the post from the push-out test. This is why conical ber posts (RelyX Fiber Post) were used in the present study for evaluation of the push-out. Furthermore, it has been demonstrated that the conical design of the post will result in improved adaptation of the post to the root canal anatomy, thus minimizing the amount of residual root structure that has to be sacriced to get the post to t.17,18 Consequently, shaping of the root canal with a taper close to that of the ber post may be useful, as no additional sound dentine will be removed, and the reconstruction will not impinge further upon the fracture resistance of non-vital teeth.19 In the present study, the taper of the

conical posts used was the same as that of the root canal preparation after the cleaning-shaping procedures (10%). The posts t the root canal walls extremely well, especially in the apical and middle portions. The results of the present study indicate (Table 1) that the highest push-out bond strength values were recorded in the apical third for RXU2 and in the middle third for MAX. In the RXU2 group, push-out bond strength tended to decrease from the apical to the cervical region, and statistically signicant differences were observed between these two thirds. Similar results were obtained in a study by Bitter et al.14 These ndings might be explained by superior adaptation of the post to the root canal walls in this region and the typical behavior of the SARC, which is higher in the apical third.20 As was reported by Goracci et al,8 the pushout bond strength on root slices also has a friction component that largely depends on the anatomy of the root canal in the region tested. Regarding the frictional component, better results were obtained on the push-out test in the present study in the regions where the morphology of the root canal was closer to the shape, the diameter, and the taper of the posts. Due to the anatomy of the root canal, cement thickness increased in the cervical area in both tested groups. As previous in vitro studies showed, increasing the cement thickness may negatively affect the retentive bond strength of adhesively cemented ber posts.21 These ndings may also explain the lower values of push-out bond strength recorded in the cervical region for both groups. Other studies found that the cement thickness around the post did not signicantly affect the bond strength of ber posts to root dentine.9,22 Self-adhesive resin cements are still relatively new, and detailed information on their composition and adhesive properties is scarce. The basic adhesion mechanism appears to be based on the micromechanical retention and chemical interaction between the monomer acidic groups and hydroxyapatite.6,23 Multifunctional monomers with phosphoric acid groups simultaneously demineralize and inltrate enamel and dentine.6,24 The mechanism of adhesion to the dentine of SARCs was reported as incapable of dissolving the smear layer. Consequently, no mechanical interlocking between the substrates will occur.6 SARCs cannot form a hybrid layer into the root canal, as they are unable to etch through the smear layer formed during the mechanical instrumentation, or after the post space preparation.8 Because aggressive acid etching is detrimental to the dentine adhesion of SARCs, due to their inability to inltrate the collagen

Please cite this article in press as: Baldea B, et al., Push-out bond strength and SEM analysis of two self-adhesive resin cements: An in vitro study, Journal of Dental Sciences (2013), http://dx.doi.org/10.1016/j.jds.2013.01.007

+
6

MODEL

B. Baldea et al

Figure 4 Representative optical microscopy images (40) of the failure types: (A) sample with RXU2 before testing (red arrowsd Resilon lling material) and (B) adhesive failure on the dentine interface after testingdResilon remained on the cement surface (red arrows); (C) sample with MAX before testing and (D) mixed failure after testing (white arrowdadhesive failure between cement and the post; red arrowd adhesive failure at the dentine interface); (E) sample with RXU2 before testing; and (F) cohesive failure within the post after testing (red arrow). D Z dentine; P Z post.

depleted by the etching step,25 the post space was cleaned with 17% EDTA solution to remove the smear layer that developed. By rinsing the canals with 17% EDTA solution for 1 minute, using the EndoVac system, followed by a rinse with de-ionized water, the dentinal tubules of the root canal were opened to allow for better adhesion of the SARC to the dentine.26

The removal of the smear layer is also indicated during the biomechanical preparation of the root canal, because it allows better penetration of the sealer into the dentinal tubules, increasing the contact surface of the lling material with the dentine.27 In our study, the penetration of the sealer Epiphany SE (Fig. 7A) into the cleaned and opened dentinal tubules of the root canal was revealed by

Please cite this article in press as: Baldea B, et al., Push-out bond strength and SEM analysis of two self-adhesive resin cements: An in vitro study, Journal of Dental Sciences (2013), http://dx.doi.org/10.1016/j.jds.2013.01.007

+
Push-out bond strength of two resin cements

MODEL

Figure 5 Representative optical microscopy images (40) of the same tooth sample (RXU2) analyzed on both surfaces (apical and cervical view), representing the mixed type of failure: (A) cervical view before testing; (B) adhesive failure between the post and resin cement after testing (red arrow); (C) apical view before testing; and (D) adhesive failure at the dentine/resin cement interface, after testing (red arrow). C Z resin cement; D Z dentine; P Z post.

Figure 6 Failure mode distribution (%) in each third (apical, middle, cervical) of the experimental groups. Blue bars, RXU2 group and red bars, MAX group. A Z adhesive failures between the dentine and the luting agent; B Z adhesive failures between the post and the cement; C Z cohesive failures within the post; M Z mixed failures.
Please cite this article in press as: Baldea B, et al., Push-out bond strength and SEM analysis of two self-adhesive resin cements: An in vitro study, Journal of Dental Sciences (2013), http://dx.doi.org/10.1016/j.jds.2013.01.007

+
8

MODEL

B. Baldea et al

Figure 7 Representative scanning electron micrography (SEM) micrographs of the samples examined: (A) image of a Group I sample showing fractured Epiphany SE resin tags (red arrow) penetrating the dentinal tubules at the interface with the Resilon core material; (B) cohesive failure within the postddetached glass bers (red arrow) can be observed; (C) adhesive failure between the post and cement (RXU2)dsmall amounts of cement remained on the retentive surface of the post (red arrow); (D) adhesive failure between the cement (RXU2) and the dentinedfractured resin tags can be observed in contact with the dentine (red arrow); (E) adhesive failure between the post and MAX in a Group II sample; and (F) fractured interface between the post and the cement in the same sample (red arrowdcement remains on the dentine surface). D Z dentine; P Z post.

SEM evaluation of the selected samples. The endodontic irrigation protocol of the present study, which entirely removed the pulpal tissue and the smear layer through use of the EndoVac system, may have contributed to the bond strength of the SARCs and the adhesion of the Epiphany SE sealer by creating resin tags from the root canal dentine. Although other studies evaluated the push-out bond strength of the ber posts used in association with guttapercha and an endodontic sealer,2e4,28 a resin-based sealer (Epihany SE) and a resin-based endodontic core material (Resilon) were used in accordance with the monoblock concept.5 The monoblock formed in the root canal by creating resin tags in the dentinal tubules from the resin contained in the self-etch sealer and by the adhesion between the sealer and the Resilon core material.29,30 This monoblock has the potential to strengthen the tooth structure31 and, at the same time, ensures complete sealing of the root canal, such that it is resistant to bacterial leakage.32 As demonstrated by optical microscopy (Fig. 4B and D) and SEM evaluation (Fig. 5A), the strong capability of the SARCs to bond to the Resilon material was observed. The failure modes in the present study showed that the interfaces between the SARCs and Resilon were more stable (Fig. 6). A recent study by Cecchin et al33 comparing guttapercha and Resilon found no differences in the push-out bond strength of the tested teeth, which were obturated with these two materials. Further studies are needed to evaluate Epiphany SE sealer and resin-based core

materials, as gutta-percha is still considered to be the golden standard with respect to root canal-lling materials. Different studies conrmed that the push-out bond strength of SARCs might be affected by the thermocycling of the samples before testing,14,34,35 or by the time for which the samples were stored between luting of the ber posts into the root canal and the mechanical testing.12 In the present study, all samples were tested for push-out bond strength 7 days after curing, similarly to previous studies.12,28 In the studies mentioned, the bond strength values noted after 7 days of storage were higher than after 24 or 48 hours. An explanation of these higher values, recorded at 7 days, may be related to a higher degree of monomer to polymer conversion, which increases the degree of conversion.36 According to the manufacturers instructions (3M ESPE), the procedure used for post luting requires no pretreatment because the machine-shaped outer surface of the post will provide a sufcient retentive surface for the resin cement, despite its inert chemical behavior.37 Analysis of the cohesive failures within the post (Fig. 4F) revealed that the fracture lines might propagate throughout the resin matrix of the post (Fig. 7B), and this could be inuenced by a nonuniform distribution of the glass-bers inside the post, by the highly adhesive properties of the luting cement or by the high frictional effect with the dentinal walls. Also, other studies regarding the bond strength of SARCs reported

Please cite this article in press as: Baldea B, et al., Push-out bond strength and SEM analysis of two self-adhesive resin cements: An in vitro study, Journal of Dental Sciences (2013), http://dx.doi.org/10.1016/j.jds.2013.01.007

+
Push-out bond strength of two resin cements

MODEL

9
7. Nielsen BA, Craig Baumgartner J. Comparison of the EndoVac system to needle irrigation of root canals. J Endod 2007;33: 611e5. 8. Goracci C, Sadek FT, Fabianelli A, Tay FR, Ferrari M. Evaluation of the adhesion of ber posts to intraradicular dentin. Oper Dent 2005;30:627e35. 9. Coniglio I, Magni E, Cantoro A, Goracci C, Ferrari M. Push-out bond strength of circular and oval-shaped ber posts. Clin Oral Investig 2011;15:667e72. 10. Goracci C, Tavares AU, Fabianelli A, et al. The adhesion between ber posts and root canal walls: comparison between microtensile and push-out bond strength measurements. Eur J Oral Sci 2004;112:353e61. 11. De Santis R, Prisco D, Apicella A, Ambrosio L, Rengo S, Nicolais L. Carbon ber post adhesion to resin luting cement in the restoration of endodontically treated teeth. J Mater Sci Mater Med 2000;1:201e6. 12. Vano M, Cury AH, Goracci C, et al. Retention of ber posts cemented at different time intervals in canals obturated using an epoxy resin sealer. J Dent 2008;36:801e7. 13. Magni E, Mazzitelli C, Papacchini F, et al. Adhesion between ber posts and resin luting agents: a microtensile bond strength test and an SEM investigation following different treatments of the post surface. J Adhes Dent 2007;9:195e202. 14. Bitter K, Meyer-Lueckel H, Priehn K, Kanjuparambil JP, Neumann K, Kielbassa AM. Effects of luting agent and thermocycling on bond strengths to root canal dentine. Int Endod J 2006;39:809e18. 15. Bouillaguet S, Scu tt A, Alander P, et al. Hypothermal and mechanical stresses degrade ber-matrix interfacial bondstrength in dental ber-reinforced composites. J Biomed Mater Res B Appl Biomater 2006;76:98e105. 16. Toman M, Toksavul S, Sarkanat M, Firidino glu K, Akin A. The evaluation of displacement resistance of glass FRC posts to root dentine using a thin slice push-out test. Int Endod J 2009; 42:802e10. 17. Grandini S, Goracci C, Tay FR, Grandini R, Ferrari M. Clinical evaluation of the use of ber posts and direct resin restorations for endodontically treated teeth. Int J Prosthodont 2005;18: 399e404. 18. Schwartz RS, Robbins JW. Post placement and restoration of endodontically treated teeth: a literature review. J Endod 2004;30:289e301. 19. Cheung W. A review of the management of endodontically treated teeth: post, core and the nal restoration. J Am Dent Assoc 2005;136:611e9. 20. Zicari F, Couthino E, De Munck J, et al. Bonding effectiveness and sealing ability of ber-post bonding. Dent Mater 2008;24: 967e77. 21. DArcangelo C, Cinelli M, De Angelis F, DAmario M. The effect of resin cement lm thickness on the pullout strength of a ber-reinforced post system. J Prosthet Dent 2007;98:193e8. 22. Perez BE, Barbosa SH, Melo RM, et al. Does the thickness of the resin cement affect the bond strength of a ber post to the root dentin? Int J Prosthodont 2006;19:606e9. 23. Van Landuyt KL, Yoshida Y, Hirata I, et al. Inuence of the chemical structure of functional monomers on their adhesive performance. J Dent Res 2008;87:757e61. 24. Ferracane JL, Stansbury JW, Burke JT. Self-adhesive resin cements e chemistry, properties and clinical considerations. J Oral Rehabil 2011;38:295e314. 25. De Munck J, Vargas M, Van Landuyt K, Hikita K, Lambrechts P, Van Meerbeek B. Bonding of an auto-adhesive luting material to enamel and dentin. Dent Mater 2004;20:963e71. 26. Barbosa De Souza F, Sincle r Delno C, Lacalle Turbino M, Braz R. Deproteinized dentin: a favorable substrate to selfbonding resin cements? J Biomed Mater Res B Appl Biomater 2011;98:387e94.

cohesive failures inside the post,38,39 but they did not explain them. The push out bond strength test has an important frictional component between the post and the dentine.8 As the cohesive failures inside the post were observed in the present study only in the RXU group (Fig. 6), it can also be supposed that in these samples the frictional component was higher, enhanced by the good retentive strength between the post and the cement (Figs. 4F and 7B). Regarding their clinical characteristics, both cements proved to be easy to use, making the technique more predictable compared to the use of other types of luting cements. RXU2 had a better ow capability, and fewer voids were observed in this group when compared to MAX. Good adhesion between the RelyX Fiber Posts and SARCs, RXU2, and MAX, was observed. Instead, adhesive failures between the dentine and the resin cement were commonly observed, which may be attributed to stress under clinical conditions.14,40 These ndings are in agreement with previous studies,3,8,20,39 which showed that most of the failures occurred at the cement-dentine interface. Within the limitations of this in vitro study, the following conclusions may be drawn: 1. The mean push-out bond strength of teeth samples containing RelyX U200 was higher than that observed for Maxcem Elite. 2. The most fragile region appeared to be the adhesive interface between the SARC and the dentine. Therefore, it can be presumed that the interface between the SARC and ber post was more stable in this study.

Acknowledgments
This study received nancial support from project POSDRU/ 88/1.5/S/63117, co-nanced by the European Social Fund, Sectorial Operational Programme for Human Resources Development 2007e2013. The authors also thank the project COST Action TD0906 Biological Adhesives from Biology to Biomimetics for meeting support.

References
1. Sidoli GE, King PA, Setchell DJ. In vitro evaluation of a carbon ber-based post and core system. J Prosthet Dent 1997;78: 5e9. 2. Bitter K, Kielbassa AM. Post-endodontic restorations with adhesively luted ber-reinforced composite post system: a review. American J Dent 2007;20:350e60. 3. Manicardi CA, Versiani MA, Saquy PC, Pe cora JD, de SousaNeto MD. Inuence of lling materials on the bonding interface of thin-walled roots reinforced with resin and quartz ber posts. J Endod 2011;37:531e7. 4. Perdiga o J, Gomes G, Augusto V. The effect of dowel space on the bond strengths of ber posts. J Prosthodont 2007;16: 154e64. 5. Tay FR, Pashley DH. Monoblocks in root canals: a hypothetical or a tangible goal. J Endod 2007;33:391e8. 6. Radovic I, Monticelli F, Goracci C, Vulicevic ZR, Ferrari M. Selfadhesive resin cements: a literature review. J Adhes Dent 2008;10:251e8.

Please cite this article in press as: Baldea B, et al., Push-out bond strength and SEM analysis of two self-adhesive resin cements: An in vitro study, Journal of Dental Sciences (2013), http://dx.doi.org/10.1016/j.jds.2013.01.007

+
10

MODEL

B. Baldea et al
cemented with self-adhesive resin cements. Int Endod J 2011; 44:314e20. Sadek FT, Goracci C, Monticelli F, et al. Immediate and 24-hour evaluation of the interfacial strengths of ber posts. J Endod 2006;32:1174e7. Mazzoni A, Marchesi G, Cadenaro M, et al. Push-out stress for bre posts luted using different adhesive strategies. Eur J Oral Sci 2009;117:447e53. Bande ca MC, El-Mowafy O, Saade EG, Rastelli ANS, Bagnato VS, Porto-Neto ST. Changes on degree of conversion of dual-cure luting light-cured with blue LED. Laser Physics 2009;19:1050e5. Zhang L, Wang Y, Radovic I, Chief N, Chen J, Ferrari M. Adhesion of two dual-cure core resins to silica ber posts treated with different bonding agents. Int Dent SA Australas Ed 2006;5:70e80. Dimitrouli M, Gu nay H, Geurtsen W, Lu hrs A-K. Push-out strength of ber posts depending on the type of root canal lling and resin cement. Clin Oral Invest 2010;15:273e81. Dimitrouli M, Geurtsen W, Lu hrs A-K. Comparison of the pushout strength of two ber post systems dependent on different types of resin cements. Clin Oral Invest 2011;16:899e908. Van Meerbeek B, De Munck J, Yoshida Y, et al. Buonocore memorial lecture. Adhesion to enamel and dentin: current status and future challenges. Oper Dent 2003;28:215e35.

27. Nunes VH, Silva RG, Alfredo E, Sousa-Neto MD, Silva-Sousa YT. Adhesion of Epiphany and AH Plus Sealers to human root dentin treated with different solutions. Braz Dent J 2008;19: 46e50. 28. Bande ca MC, Kassem AS, El-Mowafy O, et al. Inuence of storage times on bond strength of resin cements to root canal. Mater Res 2010;13:25e8. 29. Resende LM, Rached-Junior FJ, Versiani MA, et al. A comparative study of physicochemical properties of AH Plus, Epiphany, and Epiphany SE root canal sealers. Int Endod J 2009;42: 785e93. 30. Costa JA, Rached-Junior FA, Souza-Gabriel AE, SilvaSouza YT, Souza-Neto MD. Push-out strength of methacrylate resin-based sealers to root canal walls. Int Endod J 2010;43: 698e706. 31. Teixeira FB, Teixeira EC, Thompson JY, Trope M. Fracture resistance of roots endodontically treated with a new resin lling material. J Am Dent Assoc 2004;135:646e52. 32. Shipper G, rstavik D, Teixeira FB, Trope M. An evaluation of microbial leakage in roots lled with a thermoplastic synthetic polymer-based root canal lling material (Resilon). J Endod 2004;30:342e7. 33. Cecchin D, Farina AP, Souza MA, Carlini-Junior B, Ferraz CC. Effect of root canal sealers on bond strength of breglass posts

34.

35.

36.

37.

38.

39.

40.

Please cite this article in press as: Baldea B, et al., Push-out bond strength and SEM analysis of two self-adhesive resin cements: An in vitro study, Journal of Dental Sciences (2013), http://dx.doi.org/10.1016/j.jds.2013.01.007