SCANNING VOL. 9999, 1–7 (2015) © Wiley Periodicals, Inc.
Repair Bond Strength of Composite Resin to Sandblasted and Laser Irradiated Y-TZP Ceramic Surfaces OMER KIRMALI,1 C S AGATAY BARUTCIGIL,2 MEHMET MUSTAFA OZARSLAN,1 KUBILAY BARUTCIGIL,1 2 AND OSMAN TOLGA HARORLI 1 2
Department of Prosthetic Dentistry, Faculty of Dentistry, Akdeniz University, Antalya, Turkey Department of Restorative Dentistry, Faculty of Dentistry, Akdeniz University, Antalya, Turkey
Summary: This study investigated the effects of different surface treatments on the repair bond strength of yttrium-stabilized tetragonal zirconia polycrystalline ceramic (Y-TZP) zirconia to a composite resin. Sixty Y-TZP zirconia specimens were prepared and randomly divided into six groups (n ¼ 10) as follows: Group 1, surface grinding with Cimara grinding bur (control); Group 2, sandblasted with 30 mm silica-coated alumina particles; Group 3, Nd:YAG laser irradiation; Group 4, Er,Cr:YSGG laser irradiation; Group 5, sandblasted þ Nd:YAG laser irradiation; and Group 6, sandblasted þ Er,Cr:YSGG laser irradiation. After surface treatments, 1 the Cimara System was selected for the repair method and applied to all specimens. A composite resin was built-up on each zirconia surface using a cylindrical mold (5 3 mm) and incrementally filled. The repair bond strength was measured with a universal test machine. Data were analyzed using a one-way ANOVA and a Tukey HSD test (p ¼ 0.05). Surface topography after treatments were evaluated by a scanning electron microscope (SEM). Shear bond strength mean values ranged from 15.896 to 18.875 MPa. There was a statistically significant difference between group 3 and the control group (p < 0.05). Also, a significant increase in bond strength values was noted in group 6 (p < 0.05). All surface treatment methods enhanced the repair bond strength of the composite to zirconia; however, there were no significant differences between treatment methods. The results revealed that Nd:YAG
Contract grant sponsor: Akdeniz University; Contract grant number: 2014.01.0151.001. Conflicts of interest: None Address for reprints: Ca gatay Barutcigil, DDS, PhD., Department of Restorative Dentistry, Faculty of Dentistry, Akdeniz University, 07058 Antalya, Turkey. E-mail: [email protected]
Received 26 November 2014; Accepted with revision 22 January 2015 DOI: 10.1002/sca.21197 Published online XX Month Year in Wiley Online Library (wileyonlinelibrary.com).
laser irradiation along with the combination of sandblasting and Er,Cr:YSGG laser irradiation provided a significant increase in bond strength between the zirconia and composite resin. SCANNING 9999:1–7, 2015. © 2015 Wiley Periodicals, Inc. Key words: CoJet sandblasting, laser irradiations, repair bond strength, SEM, Y-TZP zirconia
Introduction To increase the mechanical properties of all-ceramic restorations, various core materials, such as glassinfiltrated alumina ceramic and lithium-disilicate-based glass ceramic, have been used in dentistry. Ceramics strengthened with zirconia have also been developed as a core material for improving the highest fracture toughness of the materials. Zirconia ceramics, especially yttrium-stabilized tetragonal zirconia polycrystalline ceramic (Y-TZP), are some of the most popular dental materials for dentists because of their superior mechanical properties, such as high fracture toughness (7–10 MPa m1/2), high flexural strength (700– 1,200 MPa), and natural appearance (Brodbeck, 2003; Hisbergues et al., 2009; Pittayachawan et al., 2009; Vagkopoulou et al., 2009). Thus, Y-TZP zirconia has the potential for being accepted as a suitable material for framework in fixed restorations (Raigrodski et al., 2006). Zirconia has three different crystal structures: monoclinic (m) at low temperatures, tetragonal (t) above 1,170˚C, and cubic (c) above 2,370˚C. After firing, and the t–m phase transformation, there is a change in the crystal structure from tetragonal to monoclinic during cooling, resulting in a volume increase (3–5%). If the phase transformation cannot be controlled, cracks and fractures can form because of the compressive stresses (Pittayachawan et al., 2009; Akin et al., 2011; Kirmali et al., 2013). The adhesiveness between the zirconia core and veneering ceramic is very important for the long-term
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performance of all restorations. Previous studies have shown that the failure of zirconia occurs mostly between the zirconia and veneering ceramic (Raigrodski et al., 2006; Sailer et al., 2006). Sailer et al. (2006) reported fracture rates of 13% for veneer ceramics at the end of 3 years, and Raigrodski et al. (2006) reported fracture rates of 25% of zirconia for veneer ceramics at the end of 31 months. Numerous reasons for these fractures have been suggested, such as surface defects, improper support by the framework (Marchack et al., 2008), overloading and fatigue (Coelho et al., 2009) and low fracture toughness of the veneering porcelain (Beuer et al., 2009). When a fracture occurs in veneer ceramics, the repair of the restoration is a suitable option compared to a complete replacement. Increasing attention has been given to repairing restorations, especially in dental schools (Blum et al., 2012). Alternatively, intraoral repair methods may be a more acceptable, easier, and less traumatic for the patient, especially with zirconia, which is an expensive and delicate restoration. To date, some manufacturers have introduced intraoral repair systems for ceramic and zirconia restorations and some researchers have used these systems in their studies with successful results (Blum et al., 2012). Various surface treatments have been used on zirconia surfaces to improve their bond strength with resin cement or veneering ceramic (Della et al., 2007) and to enhance the surface activation for chemical adhesion (Xible et al., 2006). To date, several studies have used varying pretreatments such as air abrasion with Al2O3, acid etching, grinding with diamond-disc with the aim of improving the bonding properties of zirconia ceramics. Another recently developed method for increasing the surface treatment methods utilizes lasers, a method that has the advantage of a chair-side practice. The erbium: yttrium aluminum garnet (Er:YAG), carbon dioxide (CO2), and neodymium-doped yttrium aluminum garnet (Nd:YAG) lasers have frequently been used by investigators to determine their effects on the surface of different materials (Cavalcanti et al., 2009; Akyil et al., 2010; Paranhos et al., 2011; Liu et al., 2013; Usumez et al., 2013). The erbium chromium: yttrium scandium gallium garnet (Er,Cr:YSGG) laser is another effective hard tissue laser that was recently used in a study to investigate its surface effects on zirconia (Ghasemi et al., 2014). However, there are limited data regarding laser systems and combinations of lasers with other techniques on the surface treatment of Y-TZP materials. Thus, this study was designed to evaluate the repair bond strength between composite resins and zirconia surfaces treated with various surface treatment methods. The objectives of this study were to determine the most effective surface conditioning protocol that may include a combination of traditional and popular techniques for the repair strength of a resin composite to the Y-TZP zirconia. The null hypothesis tested was that different
surface conditioning methods would not affect the repair bond strength.
Materials and Methods Sample Preparation
Sixty Y-TZP specimens (Noritake Alliance, Noritake Co., Nagoya, Japan), 7 mm in diameter, and 3 mm in height, were prepared. The surfaces of all specimens were smoothed with 600-, 800-, and 1,200-grit silicon carbide papers (English Abrasives, London, England) using a polisher (Phoenix Beta Grinder/Polisher, Buehler, Germany) to obtain a standardized surface polish. The specimens were then ultrasonically cleaned for 3 min in 96% isopropyl alcohol and steam-cleaned for 10 s. Specimens were then randomly distributed into six groups of 10 zirconia discs each, as follows:
Group 1—Control: Surface grinding with a Cimara grinding bur (10 strokes).
Group 2—CoJet Sandblasting: Bonding surfaces of zirconia specimens were treated with 30-mm Al2O3 particles modified by silica (CoJet System, 3 M ESPE) using an airborne-particle–abrasion device (CoJet System; 3 M ESPE) filled with 30-mm silicondioxide particles (CoJet Sand, 3 M ESPE) for 20 s at a distance of 10 mm. Group 3—Nd:YAG: Bonding surfaces of zirconia specimens were irradiated by a Nd:YAG laser (Smarty A10, Deka Laser, Florence, Italy) with a wavelength of 1.064 lm. Laser energy was delivered in a pulse mode by a 300 mm diameter laser optical fiber with a repetition rate of 20 Hz, an energy of 200 mJ, an output power of 1 W, an energy density of 113.23 J/cm2, and a pulse duration of 300 ms for 20 s. The distance of the application was 1 mm. Group 4—Er,Cr:YSGG: Bonding surfaces of zirconia specimens were irradiated by an Er,Cr:YSGG laser (Waterlase iPlus, Biolase Technology Inc., CA, USA) with a 2.78 mm wavelength, a pulse duration of 140– 200 ms with a repetition rate of 20 Hz. The output power of this equipment ranges from 0.25 to 6.0 W. A 600-mm diameter laser optical fiber was aligned perpendicular to the zirconia surface at a 10 mm distance and scanned over the whole ceramic area for 20 s. The energy parameters, 1.5 W with water/air flow of 55% and 65%, respectively, were used continuously during the irradiations. Group 5—Sandblasting þ Nd:YAG: The surfaces of zirconia specimens were sandblasted by silicatecoated alumina particles (CoJet system; 3 M ESPE, St. Paul, MN) with a diameter of 30 mm at a pressure of 2.3 bar (2.3 105 Pa) from a distance of 10 mm for 20 s. The specimens were then washed under running water and air dried. Each sandblasted specimen was
O. Kirmali et al.: Repair bond strength of composite resin to zirconia
irradiated by a 200 mJ, 1 W, 20 Hz power Nd:YAG laser from 1 mm for 20 s. Group 6—Sandblasting þ Er,Cr:YSGG: Zirconia specimens were treated with CoJet sandblasting followed by washing with water and air drying. Each sandblasted specimen was then irradiated by a 300 mJ, 1.5 W, 20 Hz power Er,Cr:YSGG laser from 10 mm for 20 s.
After the surface treatments, all specimens were ultrasonically cleaned in 96% isopropyl alcohol (Sigma–Aldrich, St. Louis, MO) for 3 min. Before the 1 composite resin repair, a repair system, Cimara System (Voco, Cuxhaven, Germany), was used and applied to all specimen surfaces according to the manufacturer’s instructions. Briefly, Haftsilan was applied to the zirconia surface for 2 min with no air drying. Opaquer liquid was then applied in a thin layer and photopolymerization occurred for 20 s. A composite resin, Grandio (Voco, Cuxhaven, Germany), was applied to the zirconia using a cylindrical mold (5 mm diameter and 3 mm length) and incrementally filled according to the manufacturer’s instructions. Each layer was lightpolymerized for 40 s at a distance of 1 mm using a lightpolymerizing unit (Astralis 3, Ivoclar Vivadent, Liechtenstein) with an output power of 600 mW/cm2.
Bond Strength Test
Zirconia-composite specimens mounted in a block of acrylic resin were stored in distilled water at 37˚C for 24 h. The specimens were then placed in a universal testing machine (LF Plus, LLOYD Instruments, Ametek Inc., England) at a crosshead speed of 1 mm/min for measuring the repair bond strength values. The maximum load at failure was recorded in Newtons (N) unit and was divided the bonded area to convert to MPa unit. The shear bond strength test method was preferred for determining repair bond strength. The samples had 5 mm in diameter that prepared by a cylindrical mold. The surfaces of the fractured specimens were examined through a stereomicroscope (Stemi DV4, G€ottingen, Germany) at 32 magnification. Failure modes were observed as adhesive failure, in which composite completely separated from the zirconia surface; cohesive failure, in which the fracture completely occurred in the composite; and mixed failure, in which both failure types (adhesive and cohesive) were observed.
Scanning Electron Microscopy (SEM) Analysis
Scanning electron microscopy (SEM) evaluations were performed for an additional zirconia sample from
each group. The samples were first dried and sputtercoated with gold and palladium using a sputter-coated device (Polaron SC7620 Sputter Coater, VG Microtech, West Sussex, England). The SEM images were then obtained using an electron microscope (Zeiss-Leo 1430 SEM, Angstrom Scientific Inc., NJ) with a magnification of 5,000.
The data were normally distributed according to the Kolmogorov–Smirnov test (a ¼ 0.05). The results were statistically analyzed by a one-way ANOVA and a Tukey honestly significantly difference (HSD) was used for pairwise comparisons of repair bond strength data (MPa) with SPSS 15.0 (SPSS Inc., Chicago, IL). A 95% confidence level was used.
Results The means and standard deviations of the repair bond strength values for all groups are summarized in Table I. The highest mean bond strength value was observed in group 3 followed by group 6. The lowest value for bond strength was in the controls. All zirconia surface treatments enhanced the bonding of repair composite resins. However, there were no statistically significant differences between group 1 and groups 2, 4, and 5, as shown in Table I (p > 0.05). Table I also shows that groups 3 and 6 were statistically significantly different according to the Tukey HSD multiple comparison test (p < 0.05). Modes of failure were also evaluated and represented in the Figure 1. The failure analysis revealed that fractures occurred predominantly in the adhesive at the composite/zirconia interface (60% of failures), followed by mixed failures in both failure types (adhesive and cohesive; 28.33% of failures), and finally by cohesive failures in the composite resin (11.66% of failures) (Fig. 2).
TABLE I Mean and standard deviations of shear bond strength values Standard Mean deviations Control CoJet Sandblasting Nd:YAG laser irradiation Er,Cr:YSGG laser irradiation Sandblasted þ Nd:YAG laser irradiation Sandblasted þ Er,Cr:YSGG laser irradiation
15.896 16.731 18.875 16.553 17.436 18.831
0.96a 1.99ab 1.84b 2.38ab 1.95ab 2.24b
Different lowerscript letters indicate statistical differences (p < 0.05).
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Stereomicroscope images of failure types at magnification of 32 (A: adhesive failure, B: cohesive failure, C: mixed failure).
The surface topography was evaluated with SEM analyzes after surface treatments under at a magnification of 5,000 (Fig. 3). The surface treatment with diamond discs (Cimara grinding bur) showed a distinct micro-morphological pattern, such as scratches parallel to the direction of the grinding tool propagation, compared to the typical untreated zirconia surface (Fig. 3(A)). The zirconia specimen from all treated groups also exhibited an increased surface irregularity, as well as an over destruction of the surface. However, more surface irregularities and deeper crevices within the melting area were observed in groups 3 and 6 compared with group 1 on the zirconia surface; this occurred despite the absence of a significant difference in repair bond strength values. The SEM images taken after sandblasting with 30 mm silica-coated alumina particles showed only a slight micromechanical roughening and an irregular modification of the zirconia surface, such as small pits and the formation of microretentive grooves (Fig. 3(B)). The SEM micrographs of Nd:YAG demonstrated that laser-treatment produced a surface with typical blister-like globules with microcracks surrounded by a porous layer. Irregular surfaces were observed on the zirconia surface in both laser
Failure pattern distribution among the groups tested.
irradiation treatments; but, the Nd:YAG treatment caused a more irregular surface with melting and rare crevice formation by the laser optical fiber tip than with the Er,Cr:YSGG treatment (Fig. 3(C) and (D), respectively). Figure 3 (E) and (F) represents the combination effect of lasers and sandblasting on the zirconia surface. These images show remarkable surface irregularities and microcracks that differ from the control.
Discussion The null hypotheses of present study was rejected, since the Nd:YAG laser etching and the combination of sandblasting and Er,Cr:YSGG laser treatments of the Y-TZP zirconia surface presented significantly higher repair bond strength values that those of the control group. In fact, all of the surface treatment methods enhanced the repair bond strength values of the composite resin to zirconia. Ceramic restorations with Y-TZP frameworks have shown a high incidence of veneer chipping and delamination that expose the underlying zirconia (Sailer et al., 2007a,b). The immediate repair of this kind of failure is important (Cristoforides et al., 2012) and for repairing many systems, a resin composite has been developed (Attia, 2010). When the framework is exposed, bonding performance between the composite resin and zirconia should be effective (Goia et al., 2006). To improve bond strength of the resin composite to the ceramic materials, mechanical or chemical surface conditioning methods have been used. The use of acid etching (Brentel et al., 2007; Goia et al., 2006), sandblasting (Barragan et al., 2014; Cristoforides et al., 2012), selective infiltration etching, experimental hot etching solution (Casucci et al., 2011; Casucci et al., 2009), resin cement containing phosphate-based monomers (Quaas et al., 2007), the combination of sandblasting and silane (Ozcan et al., 2013), or tribochemical silica coating (CoJet sandblasting) (May et al., 2010; Passos et al., 2010) have been investigated for their
O. Kirmali et al.: Repair bond strength of composite resin to zirconia
Fig. 3. SEM images of Y-TZP surfaces at a magnification of 5,000 (A: control, B: CoJet sandblasting, C: Nd:YAG laser irradiation, D: Er,Cr:YSGG laser irradiation, E: sandblasted þ Nd:YAG laser irradiation, F: sandblasted þ Er,Cr:YSGG laser irradiation).
ability at enhancing the bonding between the composite resin and the Y-TZP. The tribochemical silica coating (CoJet system) of zirconia ceramics is an effective method of increasing the bond strength of adhesive cements to zirconia ceramics (Atsu et al., 2006). Bottino et al. (2005) used the CoJet system to increase the bond strength between a resin composite and zirconia samples and found that tribochemical silica coating systems could be used for that purpose. Additionally, Han et al. (2013) advocated that the shear bond strength between zirconia and a composite resin was improved when they used the CoJet system and additional chemical bonding with a phosphate-based monomer-containing repair kit. The CoJet system resulted in higher shear bond strength values than control in the present study; however, this difference was not statistically significant in accordance with the Shin et al.(2014) reports. The tribochemical reaction produces a high temperature contact area that can hold the blasted particles and/or the silica layer on the ceramic surface (Haselton et al., 2001). SEM analysis of the blasted surface revealed a thin and microretentive layer that may increase the bond strength to the resin. This adhesive surface supports the bond strength values, and it can be a suitable alternative surface treatment method for zirconia repair. However, there has been little consensus concerning whether the silica is chemically bonded to zirconia or just superficially attached (Yi et al., 2014). Yi et al. (2014) reported that, using the CoJet system, the surface is roughened with silicamodified alumina particles; thus, chemical bonds between resin-based materials and the silica-modified
zirconia surface may be formed. However, the tribochemical treatment mechanism on zirconia where attached the silica is still not well known. The use of laser etching for surface roughening is an alternative and innovative method (Paranhos et al., 2011). The effect of the Nd:YAG laser for surface roughening on dental ceramic has been investigated in several studies (Li et al., 2000; da Silveira et al., 2005; Paranhos et al., 2011; Liu et al., 2013; Usumez et al., 2013). da Silveira et al. (2005) reported that Nd:YAG laser treatments showed a rough surface pattern on alumina-based ceramics. Additionally, Li et al. (2000) stated that using Nd:YAG laser on feldspathic porcelain could improve the bond strength values as well as hydrofluoric acid etching does. Alternatively, Liu et al. (2013) used the Nd:YAG laser with different power settings and durations on zirconia ceramic and found that laser irradiation could change morphological characteristics of dental zirconia ceramics and roughen the ceramic surface. However, this same group also reported that this treatment could not increase the shear bond strength of the ceramics to the resin cement. In the present study, Nd:YAG laser treatments on Y-TZP samples enhanced the shear bond strength to the resin composite. The difference between these results was probably due to the structural properties of ceramics and their reflectance (Liu et al., 2013). However, these results are in agreement with Usumez et al.(2013) who suggested that Nd:YAG laser irradiation increases bond strength of Y-TZP zirconia. Additionally, Paranhos et al. (2011) showed that Nd:YAG lasers created more roughness on zirconia compared to abrasion treatments, similar to the present results.
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The Er,Cr:YSGG lasers have previously been used to improve adhesion on several occasions. However, few studies have used Er,Cr:YSGG lasers to modify zirconia ceramic surfaces with the purpose of increasing its bond strength to the resin composite; thus, there is little information regarding the effects of Er,Cr:YSGG laser treatments on Y-TZP ceramics. Eduardo Cde et al. (2012) reported that Er,Cr:YSGG laser treatments with various power outputs from 0.5 to 5.0 W had an acceptable effect when used on glass-infiltrate alumina blocks. Furthermore, Ghasemi et al.(2014) evaluated the effect of air abrasion with 50-mm alumina powder and Er,Cr:YSGG laser (2 and 3 W) treatment on the microshear bond strength of zirconia to resin cements before and after sintering. This group found that roughening the zirconia surface with air abrasion and Er,Cr:YSGG laser irradiation with 3 W after sintering increased the bond strength values compared to untreated surfaces. In the present study, air abrasion and Er,Cr:YSGG laser irradiation increased the repair bond strength values, but the difference was not significant (p > 0.05). This discrepancy may be due to the differences between the alumina particle sizes used in the sandblasting procedure and differences in the laser irradiation power settings, since only a 1.5 W power setting was used in the present study. When compared to the Nd:YAG laser treatments, the Er,Cr:YSGG laser showed lower bond strength results. The pattern of surface topographies created by the Nd:YAG and Er,Cr: YSGG lasers observable in the SEM images can explain this difference. The SEM images of the Er,Cr:YSGG laser-treated surface showed a smooth, non-retentive surface compared to the treated surface with the Nd: YAG laser. No studies have simultaneously evaluated the effect of Nd:YAG and Er,Cr:YSGG laser treatments on a zirconia surface. Additionally, the shear bond strength values were slightly higher in the Er,Cr:YSGG laser and the CoJet sandblasting group compared with the nonlased and nonsandblasted groups. The silicacoating surface enhanced the performance of the Er,Cr: YSGG lasers, probably because of the chemical bond that was created with the silane (Bottino et al., 2005; Della et al., 2007). Previous studies using a combination of lasers and sandblasting are not available. Therefore, the results of the present study will need to be supported by further studies. The failure mode analysis found that the fracture pattern was of the adhesive variety in most of the samples; but, for the Nd:YAG laser groups, a high percentage of mixed failures was also observed, supporting a previous report (Paranhos et al., 2011).
Conclusion Within the limitations of this study, we conclude that various treatment methods of zirconia surfaces,
including combinations of laser-enhanced effects with sandblasting, especially with Er,Cr:YSGG, improves the ceramic-resin composite bonding strength. Additionally, Nd:YAG laser treatments seem to be an appropriate method for surface roughening when repairing zirconia. These results, which provide interesting options for zirconia repair, differ from previous techniques and features the possibility of treatments being performed chairside.
Acknowledgments The authors would like to thank Hakan Er from Technology Research and Developing Center of Akdeniz University for SEM analysis.
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