journal of dentistry 40 (2012) 347351

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Short communication

Improved bonding of zirconia substructures to resin using a glaze-on technique

Peter Everson a, Owen Addison b, William M. Palin c, F.J. Trevor Burke d,*
General Dental Practitioner, Leeds, UK Restorative Dentistry, University of Birmingham, School of Dentistry, College of Medical and Dental Sciences, St. Chads Queensway, Birmingham B4 6NN, UK c Biomaterials Unit, University of Birmingham, School of Dentistry, College of Medical and Dental Sciences, Birmingham B4 6NN, UK d Primary Dental Care Research Group, University of Birmingham, School of Dentistry, College of Medical and Dental Sciences, St. Chads Queensway, Birmingham B4 6NN, UK
b a

article info
Article history: Received 11 May 2011 Received in revised form 13 December 2011 Accepted 13 December 2011

abstract
Objective: To investigate the inuence of applying thin intermediary coatings of acid-etchable glasses on the shear bond strength between a methacrylate resin based cement and an yttria-stabilized zirconia dental ceramic substrate. Methods: The upper and lower surfaces of 110 sintered yttria-stabilised tetragonal zirconia polycrystalline disc-shaped specimens were polished using sequential grades of Silicon Carbide, then air-abraded with 25 mm diameter alumina particles. Specimens were randomly allocated to 11 groups (AK) (n = 10), group A acting as control. The upper surface of

Keywords: Zirconia Bonding Ceramic Resin luting cement

Group A specimens was subjected to a tribochemical coating regime (CoJet, 3M ESPE). Five glazing ceramics were applied and red according to the manufacturers recommended ring regime. The glaze was etched with 10% HF acid and all specimens coated with a silane primer. Two differing storage regimes were employed (wet storage vs thermocycling). Shear bond strength testing specimens were created by cementing resin-based composite cylinders to the centre of the prepared ceramic surface using Rely-X Unicem (3M ESPE) resin based cement. Shear bond strength testing was performed and load at failure recorded. Results: A factorial analysis of variance at a 95% signicance level demonstrated that all glazing techniques resulted in a signicant increase in the shear bond strength compared with using the resin based cement alone (P < 0.01), with the different glazing ceramics resulting in signicant differences in mean shear bond strength (P = 0.008). The differences were a function of the storage state (wet storage vs thermocycling (P = 0.013)). Conclusion: The glazing techniques used in the current investigation resulted in a signicantly enhanced shear bond stress to the resin based cement when compared with the current gold standard tribochemical coating. # 2012 Published by Elsevier Ltd.

* Corresponding author. Tel.: +44 121 237 2767; fax: +44 121 237 2768. E-mail address: f.j.t.burke@bham.ac.uk (F.J. Trevor Burke). 0300-5712/$ see front matter # 2012 Published by Elsevier Ltd. doi:10.1016/j.jdent.2011.12.011

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1.

Introduction

Since the properties of zirconium dioxide (hitherto termed Zirconia in this paper) were rst considered by Garvie et al. in 1975, there has been considerable focus on the use of zirconia in biomedical applications.1 In this respect, zirconia possesses attractive properties for consideration as a dental restorative material. It exists as a chemically stable, dense, opaque material possessing a high exural strength and a fracture toughness exceeding all previous classes of commercially available dental ceramic. Within dentistry, the advancement of Computer Aided Design/Computer Aided Machining (CAD/ CAM) technologies have facilitated the manufacture of zirconia prostheses and have allowed the manufacture of restorations of ever increasing complexity and accuracy.2 Following the introduction of the Lava all-ceramic system in 2001 by 3M ESPE (Seefeld, Germany), in vivo clinical studies have demonstrated promising clinical performance,3,4 and, in the ensuing ten years, a wide variety of zirconia core materials have been developed and are now commercially available. By providing a genuine alternative to the metal in metalceramic restorations, the recent improvements in technologies for machining, veneering and bonding zirconia offer the opportunity to expand the perceived roles of the zirconia restorations. A key problem facing dental operators using highly crystalline ceramic restorations such as high purity alumina or zirconia is the inability to etch and silanise the surface to create a topography conducive to micromechanical and chemical bonding to dental resin cements. Operators currently may roughen the surfaces with particle air abrasion or rotary instrumentation, employ phosphate monomer conditioners, which bond weakly to ceramic oxides, or use tribochemical techniques to enhance the resin bond to the ceramic substrate.5 The tribochemical techniques have been considered the gold standard by some manufacturers and involve impregnating the ceramic surface with silica. This creates a chemically modied surface onto which conventional silane-based primers will condense and bond.5 However, the bond strengths achieved are considerably lower than those achievable to conventional dental glass ceramics, where the gold standard may be considered to be the bond between the HF-etched surface of a feldspathic ceramic veneer and phosphoric acidetched enamel via a resin-based luting material.6 The search for innovative processes to allow bonding between resin based cements and highly crystalline (nonetchable) ceramics is therefore one of the most studied topics

in the eld of Dental Materials research. Processes that have been suggested include tribochemical techniques, use of phosphate monomers, modication of zirconia surfaces to include microporosity, precipitation of nano-sized alumina crystals on the zirconia surfaces and selective inltration etching.5,710 The latter essentially is the application of a glaze which is applied to the zirconia. During the fusion of the veneering layer with the zirconia, the veneering layer inltrates the supercial layer of zirconia, leading to separation of the crystals. Subsequent dissolution of the glass ceramic using 5% hydrouoric acid solution in an ultrasonic bath leads to a micromechanically retentive zirconia surface,7,8 which has been considered to establish a strong and durable bond of resin to zirconia-based materials.8 The current status of adhesive cementation of zirconia has recently been the subject of a comprehensive review 11, so it is not the intention of this work to add to this, but only to repeat its conclusion, namely, that although the science applied to adhesive bonding with zirconia has improved, there is still much to be learned to make this a predictable behaviour for clinical use.11 The present work therefore suggests an hypothesis that a simple, inexpensive and accessible laboratory process which is to glaze-on a thin coating of a thermal expansion-matched etchable ceramic onto the inner/t surface of the zirconia restoration and subsequently etch this layer with HF-acid in order to facilitate bonding to this layer. Should this technique be successful, the role of zirconia may be expanded to be used in minimally retentive situations, including adhesive bridgework.11

2.

Objectives

To investigate the impact of applying thin intermediary coatings of acid-etchable glasses on the shear bond strength between a methacrylate resin based cement and an Yttriastabilized zirconia dental ceramic substrate.

3.

Materials and methods

One hundred and ten sintered yttria (-stabilised) tetragonal zirconia polycrystalline (Y-TZP; LAVA) disc-shaped specimens (12 mm diameter and 2 mm thickness) were supplied by 3M ESPE (Seefeld, Germany). The upper and lower surfaces were polished using sequential grades of Silicon Carbide abrasives from P80 through P220, P320, P500, P800, P1200 to a P2000 grit

Table 1 Glazing ceramics utilized in the study. Ceramic material Manufacturer Thermal expansion coefcient a (mm/mK), mean (SD)
7.3 9.5 9.9 9.3 9.9 10.8 (0.1) (0.2) (0.3) (0.1) (0.1) (0.1)

Glaze thickness (mm), mean (SD)

120 150 130 140 140 (20) (30) (20) (10) (20)

Vitadur Alpha Ivoclar Emax Ceram Noritake Cerabien Vita VM9 Lava Ceram Lava (Y-TZP)

Vita Zahnfabrik Ivoclar Vivadent Noritake Ceramics Vita Zahnfabrik 3M ESPE 3M ESPE

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for controlled time intervals. The specimen surfaces were then air-abraded with 25 mm diameter alumina particles (Plas Dent, West Midlands, UK) delivered perpendicular to the specimen surface at a pressure of 5000 hPa from a distance of 20 mm for 5 s prior to thorough washing in distilled water. Specimens were randomly allocated to 11 groups (AK) (n = 10) with group A acting as the control. The upper surface of Group A specimens was subjected to a tribochemical coating regime (CoJet, 3M ESPE), delivered according to the manufacturers recommendations, whereas all remaining groups received a surface glaze. Five glazing ceramics (Table 1), which possessed thermal expansion coefcients matched for application to zirconia substrates, were used in the current investigation. The thickness of the LAVA specimens was determined prior to coating using a screw gauge accurate to 10 mm (Moore and Wright, Shefeld, UK). A thin slurry of each glazing ceramic was formed by manipulating 0.035 g of ceramic frit with 0.2 ml of distilled deionised water. The slurry was carefully transferred to the LAVA surface with a clean brush, distributed evenly using a vibrating technique, and allowed to air dry. Each glaze coating was red according to the manufacturers recommended ring regime in a Vita Vacuumat 40 furnace (Vita Zahnfabrik, Bad Sackingen, Germany) followed by slow cooling in air. The thickness of the coated specimens was re-determined prior to etching of the glaze with 10% hydrouoric (HF) acid (Fisher Scientic, Loughborough, UK) for 90 s. Following etching, the specimens were repeatedly washed (10) in distilled water. All specimens were coated with a silane primer (Rely-X Ceramic Primer, 3M ESPE), air dried and stored in a desiccator until required for further testing. The bond of the resin composite luting cement to the modied zirconia surface was characterised using a shear bond strength methodology. All specimens were coated with a silane primer (Rely-X Ceramic Primer, 3M ESPE, St Paul, USA) and allowed to air dry. Shear bond strength testing specimens were created by cementing Z100 resin-based composite (3M ESPE, St Paul, USA) cylinders (2.4 mm diameter and 4 mm length) to the centre of the prepared ceramic surface with a

controlled volume of mechanically mixed Rely-X Unicem (3M ESPE) resin based cement, under a standard seating force, in a silicone guide mould to minimise the cement ash. The cement was light cured in accordance with the manufacturers instructions. Shear bond strength testing was performed on specimens from Groups AF following 24 h of water storage at 37 8C. Specimens from Groups GK were subjected to 1800 cycles of thermal cycling between temperature extremes of 5 and 55 8C with a 6 s dwell time at each temperature. Shear bond strength was determined by loading the cylinder parallel to the ceramic surface with a at blade in a Bencor Multi-T alignment apparatus (Danville Engineering Inc., San Ramon, USA) using a universal tensile-testing instrument (Instron Model 5544, Instron Ltd., Buckinghamshire, England) at a crosshead speed of 1 mm per minute. The load at failure was recorded and the shear stress calculated as a function of the loaded area. In addition, the fracture surface of each debonded RBC specimen was examined under a stereo-microscope (Wild M3C, Heerburg, Switzerland) at 20 magnication to determine whether failure was cohesive or adhesive. Scanning electron microscopy (SEM) with a JEOL JSM 5300 LV (JEOL Ltd., Akishima Tokyo, Japan) was used for the examination of representative prepared ceramic surfaces and cross-sections of the resin-coated ceramic specimens, following deposition of a 2 mm gold layer. Statistical analysis of the shear bond strength data was performed using a factorial analysis of variance and post hoc Tukey tests at a 95% signicance level.

4.

Results

A factorial analysis of variance at a 95% signicance level demonstrated that all glazing techniques resulted in a signicant increase in the shear bond strength compared with using the resin based cement alone (P < 0.01). The use of different glazing ceramics resulted in signicant differences in mean shear bond strength (P = 0.008) and the

Wet storage
50 45

Thermocycled

Shear Bond Strength (MPa)

40 35 30 25 20 15 10

5 0 CoJet (A) Alpha (B/G) Noritake (C/H) Emax (D/I) VM9 (E/J) Lava Cer (F/K)

Glaze Material
Fig. 1 Shear bond strength values for the materials under test in wet storage conditions and after thermocycling.

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journal of dentistry 40 (2012) 347351

Fig. 2 (a)(d). Scanning electron micrographs of the Emax glazed fracture surface after bond strength testing (a) the etched glazed surface demonstrating the microporosity induced by selective phase dissolution (b), the fracture surface demonstrating residual glass on the zirconia surface (c) demonstrating cohesive failure within the glazing ceramic and (d) the oblique fracture of the veneering ceramic.

differences were a function of the storage state (wet storage vs thermocycling) (P = 0.013) (Fig. 1). Post hoc Tukey tests demonstrated a signicantly increased shear bond strength when Noritake ceramic was used when compared with the manufacturers recommended ceramic, Lava Ceram (P = 0.049) and Vita VM9 (P = 0.014). Scanning electron microscopy demonstrated that the predominant failure modes were mixed, namely, cohesive within the veneering ceramic and adhesive between the veneering ceramic and the zirconia substrate. All glazed surfaces demonstrated modication following HF-acid etching. Vitadur-alpha, despite being microstructurally largely amorphous, demonstrated etching patterns consistent with the selective dissolution of pits and aws. The remaining veneering ceramics possessed microstructurally mixed phases and demonstrated etching patterns consistent with selective phase etching8 (Fig. 2ad).

5.

Discussion

There appears to be an increased demand from patients for restorations of optimum aesthetics, so a reliable method for the construction of all-ceramic crowns and bridges could therefore be considered advantageous. In this respect, a

number of zirconia-based materials are now capable of being stained with a variety of shades 12 prior to sintering, thereby optimising the aesthetic quality of the completed restoration in comparison with those formed in metalceramic types. However, a reliable means of facilitating the bonding of zirconia to tooth substance using resin-based luting materials, in particular, the increasing popularity of self-adhesive resin luting materials13, has proved elusive. Therefore, the use of zirconia has been limited to its use in cavities/preparations, which achieve resistance and retention form. Achieving a reliable bond would allow zirconia-based restorations to be used in, for example, resin-retained bridgework. Hence the clinical application of the present work. The statistically signicant interaction between storage state and mean shear bond strength is consistent with observations of previous investigators. Although a detrimental effect of thermal fatigue on bond strength would be expected from basic theory, the observations are thought to reect the modied compliance of the test specimen following fatigue and are an acknowledged limitation of the testing methodology. Although different glazing materials resulted in differences in shear bond strength, there was no simple relationship with thermal expansion coefcients. This is not unexpected as the layering and sintering of thin coatings will be inuenced by numerous variables introduced by the

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operator and other materials variables, which have not been explored within the constraints of this short investigation. Furthermore, it would appear appropriate to use the same methodology with a variety of zirconia core materials, since, whilst this study used ve veneering ceramics, only one core material (Lava:3M ESPE) was employed. The advantages of this technique are clear. The laboratory technique is relatively simple in comparison to selective inltration, differing from it by not completely dissolving away the veneering ceramic. It therefore requires no additional materials or equipment and therefore is cheap and simple to perform. Additionally, as veneering ceramics are silicacious, the etched surface is also conducive to silane bonding (which enhances the bond strength to resin based cements) using conventional material formulations. The glazing techniques used in the current investigation resulted in a signicantly enhanced shear bond stress to the resin based cement when compared with the current gold standard tribochemical coating. However, the most important detracting issue in the technique utilized in this work is the requirement to accommodate space for the glaze itself. Although renement in ceramic frit size will inevitably allow for materials that can be used to produce a glaze nish well below the 120 mm thickness achieved in the current investigation, concerns regarding accuracy of restoration t may arise. CAD-CAM restoration construction technology already has the capacity to account for the glaze thickness but for the immediate future this technique should be limited for adhesive bridges where the geometry of retaining wings is simple and t is unlikely to be compromised. Future work is required to examine the impact of glaze thickness on shear bond strength and longer term fatigue simulation would appear to be sensible to provide an indication of likely clinical performance in the medium and long term.

resin based cement when compared with tribochemical coating.

references

6.

Conclusion

The glazing techniques used in the current investigation resulted in a signicantly enhanced shear bond stress to the

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