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ORIGINAL ARTICLE
Year : 2019  |  Volume : 22  |  Issue : 11  |  Page : 1475-1482

Evaluation of shear bond strength of zirconia-based monolithic CAD-CAM materials to resin cement after different surface treatments


1 Department of Prosthodontics, Faculty of Dentistry, Istanbul University, Istanbul, Turkey
2 Department of Prosthodontics, Faculty of Dentistry, University of Health Sciences, Istanbul, Turkey

Date of Submission20-Mar-2019
Date of Acceptance29-May-2019
Date of Web Publication13-Nov-2019

Correspondence Address:
Dr. B Altan
Department of Prosthodontics, Faculty of Dentistry, Istanbul University, Istanbul
Turkey
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Source of Support: None, Conflict of Interest: None


DOI: 10.4103/njcp.njcp_157_19

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   Abstract 


Objective: To compare the shear bond strength of resin cement to zirconia-based monolithic CAD-CAM materials subjected to different surface treatments. Methods: 2 brands of monolithic zirconia blocks (Vita YZ HT, Sirona inCoris TZI), yttrium-stabilized tetragonal zirconia (IPS e.max ZirCAD) and zirconia-reinforced lithium silicate ceramic (Vita Suprinity) were divided into six groups according to the surface treatment received: no treatment (control), HF acid etching, sandblasting, sandblasting + Er:YAG laser irradiation, Er:YAG laser irradiation and CoJet. Composite resin cylinders were bonded to blocks with self-adhesive resin cement (Theracem). Shear bond strength was evaluated after thermocyling. Failure modes were examined using SEM. Data was analyzed statistically by using 2-way ANOVA and post-hoc Tukey's test (P < 0,05). Results: The bond strength was significantly affected by the surface treatment and the type of CAD-CAM blocks (P < 0,001). Surface treatment with CoJet revealed significantly higher bond strength compared to sandblasting in Y-TZP and monolithic zirconia specimens. Conclusions: Monolithic zirconia blocks showed higher bond strength values compared to Y-TZP zirconia block in sandblasting and CoJet groups. HF acid etching is more effective than sandblasting and CoJet for Vita Suprinity.

Keywords: Bond strength, CAD-CAM, monolithic zirconia, self-adhesive resin cement, surface treatment


How to cite this article:
Altan B, Cinar S, Tuncelli B. Evaluation of shear bond strength of zirconia-based monolithic CAD-CAM materials to resin cement after different surface treatments. Niger J Clin Pract 2019;22:1475-82

How to cite this URL:
Altan B, Cinar S, Tuncelli B. Evaluation of shear bond strength of zirconia-based monolithic CAD-CAM materials to resin cement after different surface treatments. Niger J Clin Pract [serial online] 2019 [cited 2019 Dec 12];22:1475-82. Available from: http://www.njcponline.com/text.asp?2019/22/11/1475/270851




   Introduction Top


Over recent years, the use of zirconia-based materials has increased due to their biocompatibility, high flexural strength (more than 1000 MPa) and esthetic capability.[1] With CAD-CAM technology, the design and fabrication process is less time-consuming, less technique sensitive, and does not require multiple steps when compared with the conventional method.[2] Furthermore, CAD-CAM ceramics are homogeneous in structure and could be milled. Zirconia framework is also milled using CAD-CAM technology. After milling, Y-TZP framework has to be veneered with glass ceramics because of its opacity.[3] However, chipping has been reported to be a major complication of zirconia-based restorations.[4] To overcome this problem, the monolithic zirconia has been developed. Although optimum porcelain thickness is recommended to be between 0.75 and 1.25 mm, monolithic zirconia can be used in cases with limited interocclusal space because of its ability to resist high loads with only 0.5 mm occlusal thickness.[5],[6] In addition to this, the improved translucency of monolithic zirconia is achieved with decrease in alumina content.

To create a strong bond between a resin and ceramic, mechanical and chemical retention are needed. Various surface treatments have been suggested for resin bonding to zirconia including sandblasting, tribochemical silica coating, hydrofluoric acid and laser irradiation.[7] However, hydrofluoric acid etching does not result in satisfactory resin bond to zirconia because of high crystalline content and the lack of glassy phase.

Sandblasting creates a rough surface for mechanical retention by luting cement. At the same time, sandblasting increases the strength of the Y-TZP and can compromise the compressive stress layer and enhance crack propagation.[8] Tribochemical silica coating process not only roughen but also chemically activate the surfaces of ceramics. As a result of blasting pressure, the embedded silica and alumina particles chemically react with the silane coupling agent.

Another recently developed surface treatment method is laser irradiation. Lasers have been suggested for modifying the surface of zirconia ceramics.[7] Er:YAG lasers are used in dentistry, owing to wavelength and amount of absorption. Er:YAG with appropriate parameters can roughen zirconia surface that enhances the micromechanical retention.[9]

The successful cementing of zirconium oxide-based prosthesis is an important factor in its clinical success. They can be cemented using conventional cements. However, adhesive luting of these restorations has been recommended to improve their retention, marginal adaptation and fracture resistance.[10] MDP-based and self-adhesive resin cements are recommended for zirconia-based restorations. 10-MDP improves surface wettability and forms cross-linkages with methacrylate groups of the resin cement, as well as siloxane bonds, with the hydroxyl groups of the ceramic surface.[11]

The purpose of this study is to evaluate the effects of surface treatments on the bond strength of zirconia-based materials to novel self-adhesive resin cement. The null hypothesis of this study is that surface conditioning methods would not improve adhesion compared to the control group.


   Methods Top


Two monolithic zirconia (Vita YZ HT, Sirona inCoris TZI), Y-TZP zirconia ceramic (IPS e.max ZirCAD) and zirconia-reinforced lithium silicate ceramic (Vita Suprinity) were tested. The type, composition, manufacturer and batch number of the materials used in this study are summarized in [Table 1].
Table 1: Materials used in this study

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Specimen preparation

CAD-CAM blocks were sectioned by using a water-cooled low speed diamond saw (Isomet 1000, Buehler; Germany). Monolithic and Y-TZP zirconia blocks were cut 20% larger than the required dimension to take its shrinkage into account. Subsequently, the specimens were sintered to final dimension according to the manufacturers' instructions. Specimens with 2.5 mm thickness were then embedded in autopolymerizing acrylic resin with their polished surfaces exposed. The surfaces were polished with 600, 800 and 1200 grit silicon carbide paper with water cooling and then ultrasonically cleaned for 5 min.

Specimens were divided into 6 groups (n = 10) according to the surface treatment conducted, as follows:

  1. Control: No surface treatment applied to specimens.
  2. HF acid etching: Surfaces of specimens were etched with 9.5% hydrofluoric acid (Bisco, USA) for 60 s for monolithic and Y-TZP zirconia blocks and 20 s for Vita Suprinity. After that, the specimens were rinsed with water for 30 s and then air dried.
  3. Sandblasting: Specimens were sandblasted with 50 μm Al2O3 particles (Korox, Bego) under a pressure of 2 bar at a distance of 10 mm for 15 s. After that, the specimens were washed under running water for 30 s and then air dried.
  4. Sandblasting + Laser irradiation: Specimens were sandblasted with 50 μm Al2O3 particles under a pressure of 2 bar at a distance of 10 mm and then irradiated by Er:YAG laser with a 2,94 μm. The laser parameters were as follows: power output of 4W, pulse penetration rate of 10 Hz, energy of 400 mJ, pulse duration of 100 μs. A no-contact probe was used perpendicular to the surface with a distance of 10 mm and the surfaces were irradiated with water irrigation for 15 s.
  5. Laser irradiation: Surfaces of specimens were irradiated by an Er:YAG laser. Procedures were developed as previously described.
  6. CoJet: Tribochemical silica coating (CoJet Sand, 3M ESPE, Seefeld, Germany) was applied for 15 s at 2.8 bar air pressure and a distance of 10 mm from the surface of ceramic. Then, silane (ESPE Sil, 3M ESPE) was applied and allowed to dry for 5 min.


Composite resin (Filtek Z250, 3M ESPE, Seefeld, Germany) was incrementally packed into plastic mold with diameter of 5 mm and height of 3 mm and light cured for 40 s using light-curing unit (1200 mW/cm 2) (Woodpecker, LED B). Polyethylene adhesive tape with a circular hole of 4 mm diameter was positioned on the surfaces of the blocks to define the bonding area. The composite resin cylinders were bonded to the surface of specimens with self-adhesive resin cement (Theracem, Bisco, USA) under a force of 50 N. The excessive resin cement was then removed and light polymerized for 40 s from two lateral directions. Then, the specimens were stored at 37°C in a distilled water. After 24 h, the specimens were subjected to thermocycling between 5° to 55°C for 5000 cycles with 30 s dwell time (DTS B1 Dentester, Salubris Technica, Massachusetts, USA).

Shear bond test

Shear bond strength test was conducted with universal testing machine (Instron, Instron Corp. Norwood, MA, USA) at a crosshead speed of 0.5 mm/min [Figure 1]. The SBS values were recorded in MPa by dividing failure load (N) with the bonding area (mm 2).
Figure 1: Shear bond testing (a) Metal jig (b) Acrylic mould (c) Ceramic (d) Composite resin cylinder (e) Shearing rod

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Failure mode analysis

The failure mode analysis was performed by examining specimens under SEM at 30 × magnification and classified according to one of the following three types: adhesive failure at the ceramic/cement interface, cohesive failure within the resin cement, and mixed failure.

SEM evaluation

Specimens were sputter-coated with gold (Quorum SC 7620 Sputter Coater, East Sussex, England) and evaluated under SEM (Zeiss Evo LS 10, Germany) at 1000 × magnification to observe topographic changes after different treatments.

Statistical analysis

Statistical analysis was performed using SPSS 23.0 (SPSS Inc., Chicago, IL, USA). The data were normally distributed according to the Kolmogorov-Smirnov test. 2-way ANOVA with one between-group factor (6 surface treatments) and one within-group factor (4 CAD-CAM blocks) were used to analyze the data. Tukey's post-hoc test was used for multiple comparisons. P values less than 0.05 were considered to be statistically significant in all tests.


   Results Top


The results of 2-way ANOVA showed that both surface treatment and CAD-CAM material type had a significant effect on the bond strength values (P < 0,05). The mean values and standard deviations of the shear bond strength values for all groups are summarized in [Table 2].
Table 2: Shear bond strength values (MPa)

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All surface treatments enhanced the bond strength between CAD-CAM materials and resin cement. The statistical analysis revealed that bond strength of monolithic zirconia blocks was significantly higher than Y-TZP zirconia blocks in sandblasting and CoJet groups. However, there was no significant difference between bond strengths of two brands of monolithic zirconia blocks. The bond strength values achieved in CoJet groups were significantly higher compared to sandblasting for Y-TZP zirconia and monolithic zirconia blocks. For Vita Suprinity, HF acid etching yielded the highest bond strength. Laser irradiation group showed higher bond strength values compared to control group. Specimens that are lased after sandblasting exhibited lower bond strength than sandblasted specimens.

Y-TZP and monolithic zirconia blocks showed predominantly mixed failure in sandblasting, CoJet and sandblasting + laser groups. Adhesive failure mode was observed for control, HF acid etching and laser groups. For Vita Suprinity, mixed failure was observed in HF acid etching, sandblasting and CoJet groups while adhesive failure was observed in control, sandblasting + laser and laser groups [Figure 2].
Figure 2: SEM images of failure types at magnification of 30×. (a) Adhesive failure; (b) Cohesive failure; (c) Mixed failure

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Representative SEM images of the monolithic zirconia and Y-TZP zirconia groups are reported in [Figure 3], [Figure 4], [Figure 5]. The control groups revealed homogenous structures. The SEM micrographs of HF acid etching and laser irradiation did not show remarkable surface irregularities that differ from the control. Microporosities and microstratches were visible after HF acid etching and laser irradiation. The surface of sandblasted and CoJet applied specimens showed microretentive grooves. Although SEM graphs of CoJet and sandblasting had similar surface topography, Cojet-treated surfaces were characterized by a finer texture. Sandblasting + laser group showed smooth surface according to sandblasting group. [Figure 6] shows the SEM image of Vita Suprinity blocks. The control groups displayed smooth surface topography. SEM analysis has showed HF acid etching created uniform microporosities. After sandblasting, sandblasting + laser and CoJet treatments, surface of Vita Suprinity blocks exhibited sharp edges and shallow pits. Specimens demonstrated microporosities and microstratches after laser irradiation.
Figure 3: SEM images of Vita YZ HT block surfaces at a magnification of 1000×. (a) Control; (b) HF acid etching; (c) Sandblasting; (d) Sandblasting + Laser irradiation; (e) Laser irradiation; (f) CoJet

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Figure 4: SEM images of Sirona inCoris TZI block surfaces at a magnification of 1000×. (a) Control; (b) HF acid etching; (c) Sandblasting; (d) Sandblasting + Laser irradiation; (e) Laser irradiation; (f) CoJet

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Figure 5: SEM images of IPS e.max ZirCAD block surfaces at a magnification of 1000×. (a) Control; (b) HF acid etching; (c) Sandblasting; (d) Sandblasting + Laser irradiation; (e) Laser irradiation; (f) CoJet

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Figure 6: SEM images of Vita Suprinity block surfaces at a magnification of 1000×. (a) Control; (b) HF acid etching; (c) Sandblasting (d) Sandblasting + Laser irradiation; (e) Laser irradiation; (f) CoJet

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   Discussion Top


The null hypothesis of the present study was rejected since the results indicated that shear bond strength is affected by different surface treatment methods. All of the surface treatment methods enhanced the shear bond strength values of the zirconia-based materials to resin cement.

The long-term success of zirconia-based restorations depends on the adhesion between zirconia and resin cement. As a result of a weak adhesion, the crack formed in the restorative material move along the cement interface, causing the restoration to break.[12] It has been reported that the roughening of the inner surfaces of full ceramic restorations increases the surface area, which facilitates wetting of the ceramic surface with resin-based materials. As seen in prior studies,[10] hydrofluoric acid etching is not effective to create a bond between resin cement to zirconia surfaces since Y-TZP ceramics do not contain glassy phase.

In order to enhance the bond strength of zirconia to resin cement, several surface conditioning methods have been used including sandblasting with Al2O3, tribochemical silica coating, laser irradiation etc. Nevertheless, there is no consensus regarding the best surface treatment for zirconia. For this purpose, HF acid etching, sandblasting, sandblasting + laser irradiation, laser irradiation and tribochemical silica coating were applied to Vita YZ HT, Sirona inCoris TZI, IPS e.max ZirCAD and Vita Suprinity blocks. HF acid etching treatment has been included in surface treatment groups because it is the recommended method for Vita Suprinity blocks. Thus, the bond strengths of zirconia-reinforced lithium silicate ceramics, Y-TZP zirconia and monolithic zirconia specimens with HF acid treated were also compared.

In the present study, HF acid etching group showed higher bond strength compared to control groups regarding Vita YZ HT, Sirona inCoris TZI and IPS e.max ZirCAD. It can be associated that even HF acid etching does not change surface morphology of zirconia, it increases wettability and surface energy.[13] HF acid etching treatment resulted in the highest bond strength values for Vita Suprinity blocks. These results are in agreement with the findings of Ataol et al. and Sato et al., who stated that HF acid etching group showed the highest bond strength for Vita Suprinity.[14],[15] These results may be explained by the fact that HF acid etching enhanced micromechanical retention by dissolving the glassy matris of Vita Suprinity.[12]

Sandblasting enhances bond strength by increasing surface area and roughness. Zhang et al. claimed that sandblasting causes formation of microcracks which decrease strength of zirconia.[8] However, it was proven that resin cement flowed into microcracks and therefore significantly strengthened the ceramic. Moreover, in CoJet system, silica particles not only roughen the surface, they also support chemical retention by bonding silane and silica-coated zirconia surface.[16] The present studies [17],[18] reported that CoJet application increased bond strength values more than did sandblasting.

The results showed that shear bond strength of group CoJet were significantly higher than those of group sandblasting for Y-TZP and monolithic zirconia. SEM images of CoJet groups have microretentive grooves with finer texture than sandblasting groups. SEM analysis supports the bond strength values. Similar to our study, Elsaka stated that specimens treated with CoJet exhibited significantly higher bond strength than sandblasted specimens. These results may be explained by the fact that CoJet enhanced mechanical and chemical bonding.[19] Additionally, our findings are in line with those of Bavbek et al. who reported bond strength values of CoJet group have higher those of sandblasting group.[20] They stated that type of monolithic zirconia did not significantly influence the bond strength values, which is in agreement with our study. Sandblasting and CoJet treatment are not effective on Vita Suprinity blocks as well as on zirconia-based ceramics. This result was probably achieved due to lower surface hardness of Vita Suprinity blocks compared to zirconia.[14]

Laser irradiation is an alternative method to conventional surface treatment methods. The principle effect of laser energy is the conversion of light energy into heat, and the most important interaction between laser and substrate is the absorption of the laser energy by the substrate.[9] Er:YAG, Nd:YAG and CO2 laser are used to roughen the ceramic surface and improve micromechanical retention. However, Arami et al. reported that Nd:YAG and CO2 lasers were destructive on the zirconia surfaces since they created extensive cracks and high temperatures.[21] On the other hand, Akin et al. stated that Er:YAG laser application significantly increased the bond strength.[22] In addition, Kirmali et al. reported that Er:YAG laser irradiation was resulted in more surface roughness compared to Nd:YAG laser irradiation.[23] These results were in accordance with those of Ozdemir et al. who reported that specimens which Er:YAG laser was applied showed higher bond strength than specimens treated with Nd:YAG laser.[24] Based on these findings, Er:YAG laser application is likely to enhance the bond strength.

Laser irradiation group showed higher bond strength compared to control groups. Lower bond strength of laser groups demonstrated that laser irradiation could not create enough microdepth and this resulted in limited penetration of the cement. Similarly, in another study conducted by Erdem et al., laser irradiation resulted in lower bond strength. It is thought that the heat-damaged zirconia surface, where bubbled blister-like appearance and microcracks were present, adversely affected bonding.[25] Higher bond strength values in our study may be attributed to low output energy (2W) of Er:YAG laser in Erdem et al's study. Ataol et al. evaluated the effect of the laser irradiation on the bond strength of Y-TZP zirconia. In the present study, higher bond strength values were obtained compared to bond strength values found in their study.[14] These findings can be directly related to the different laser devices used and the parameters applied. While Ataol et al. used Er, Cr:YSGG laser with output energy 3W; in our study, Er:YAG laser was applied with 4W. In present study, sandblasting plus laser irradiation group showed lower bond strength values compared to sandblasting group. This result may be associated with decrease in surface roughness when laser irradiation was applied after sandblasting. Considerably close to our study, Akyıl et al. found lower bond strength values in sandblasting plus laser group compared to sandblasting group.[26]

Monolithic zirconia blocks had higher bond strength values compared to Y-TZP zirconia in sandblasting and CoJet groups. It can be speculated that it is related that monolithic zirconia has a homogenous structure and smaller particle size than conventional zirconia.

Selection of the luting cement is more relevant factor while bonding to zirconia ceramics. MDP-based resin cements provide a stronger bond strength than other cement types. MDP-containing systems are proposed for long-term durability of the adhesion between zirconia ceramics and resin cement.[27] It is thought that the MDP monomer reacts with the hydroxyl group on the ceramic surface and chemically bonds with zirconia and is not hydrolyzed since it contains a long carbonyl chain.[7] Zirconia specimens bonded with self-adhesive cement containing MDP showed higher bond strength values than the other cement types.[28],[29]

A number of factors (temperature, pH, saliva chemistry, food or drink interaction, presence of microorganism) may interfere bond strength. The effect of remineralizing agent on bond strength is investigated in Rizvi et al.'s study.[30] In our study, the bond strengths of the specimens which are subjected to thermocycling is evaluated.

Bond strength tests have been performed with regards to shear bond strength, tensile bond strength, microshear bond strength and microtensile bond strength. Although microtensile tests are more uniform at the interface, it requires fine sectioning of a material which may lead to initial cracks in the sample. In the present study, shear bond test has been used. This commonly used test is fast and easy to perform and also reflects the clinical situation.[31],[32],[33]

When it comes to analysis of the failure type that occurs in the shear test, while mixed failure was mostly observed in sandblasting, sandblasting + laser and CoJet groups; control, HF acid etching and laser groups showed predominantly adhesive failure for Y-TZP and monolithic zirconia. Moreover, for Vita Suprinity, HF acid etching, sandblasting and CoJet groups mainly showed mixed failure and control, sandblasting + laser and laser groups predominantly demonstrated adhesive failure. The failure modes also supported the bond strength values. In the groups with the lower bond strength values, mainly adhesive failures were observed, whereas in the groups with higher bond strength values mostly mixed failures were found.

In this study, the initial bond strength was not evaluated, this might be considered as a limitation. Further investigation should consider this issue and compare differences between initial and post-thermocycling bond strength values. Another limitation was that only 1 resin cement was used, different results might have been obtained with different types of cements. In addition, long-term clinical studies are recommended to confirm the success of treatment procedures.


   Conclusions Top


Within the limitations of this in vitro study, the following conclusions can be drawn:

  1. Tribochemical silica coating provided satisfactory bond strength for monolithic zirconia and Y-TZP zirconia. Tribochemical silica coating can be preferred to sandblasting in clinical practise.
  2. HF acid etching was more effective than sandblasting and CoJet for Vita Suprinity.
  3. Laser irradiation improved the adhesion compared to control groups but did not present clinically acceptable bond strength value.
  4. Monolithic zirconia blocks showed higher bond strength values compared to Y-TZP zirconia block in sandblasting and CoJet groups. This result is promising for clinical success of monolithic zirconia restorations.
  5. There was no significant difference between two different brands of monolithic zirconia blocks.


Financial support and sponsorship

Scientific Research Projects Coordination Unit of Istanbul University. Project number: 30164.

Conflicts of interest

There are no conflicts of interest.



 
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Homae E, Jin XZ, Pow EHN, Matinlinna JP, Tsoi JK, Farhangdoost K. Numerical fatigue analysis of premolars restored by CAD/CAM ceramic crowns. Dent Mater 2018;34:e149-57.  Back to cited text no. 33
    


    Figures

  [Figure 1], [Figure 2], [Figure 3], [Figure 4], [Figure 5], [Figure 6]
 
 
    Tables

  [Table 1], [Table 2]



 

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