bond strength and failure characteristics of zirconia ... · clear plastic film, approximately 0.5...

13Bond strength and failure characteristics of zirconia-based dental ceramic to resin cements Premwara Triwatana, Porntida Visuttiwattanakorn, Kallaya Suputtamongkol, Nutthakrij Butrangamdee

Premwara Triwatana, Porntida Visuttiwattanakorn, Kallaya Suputtamongkol, Nutthakrij Butrangamdee Prosthodontic Department, Faculty of Dentistry, Mahidol University

Bond strength and failure characteristics of zirconia-based dental ceramic to resin cements

Corresponding author: Kallaya Suputtamongkol Prosthodontic Department, Faculty of Dentistry, Mahidol University 6 Yothi Street, Rachathewi, Bangkok, Thailand 10400 Tel. 668-13186657 E-mail: [email protected] Received: 20 January 2016 Accepted: 15 February 2016

AbstractPurpose: The objectives of this study were to determine the microtensile bond strength of zirconia-based dental ceramics to three resin cements and to define their failure characteristics.

Materials and Methods: Zirconia specimens (IPS Emax ZirCAD) were cut from pre-sintered blocks and fired to the final dimension of 10mmx10mmx4mm. Bonding between zirconia material was made using three resin cements and their corresponding adhesives, which were Panavia F2.0, Multilink N, and Calibra Esthetics resin cements. All bonded specimens were stored at 37°C for 24 hr and cut into microbars (1mm x 1mm x 8 mm). All microbars were loaded in tension at a crosshead speed of 1 mm/min using a universal testing machine. Microtensile bond strength were calculated and analyzed using one-way ANOVA at α=0.05. The fracture surfaces were investigated using a scanning electron microscope.

Results: The mean microtensile bond strength of zirconia bonded to Multilink N (35.5±7.6 MPa) was significantly higher than those bonded with other resin cements. The mean microtensile bond strength of zirconia bonded to Panavia F2.0 and Calibra Esthetics were comparable (21.6-22.9 MPa) Failure of specimens in all groups originated at the interface between resin cement and core ceramic.

Key words: adhesive bonding, bond strength, dental zirconia, resin cement, microtensile

How to cite: Triwatana P, Visuttiwattanakorn P, Suputtamongkol K, Butrangamdee N. Bond strength and failure charcteristics of zirconia-based dental ceramic to resin cements. M Dent J 2016; 36: 13-23.

Dental Journal Original ArticleMahidol Dental Journal

14 Bond strength and failure characteristics of zirconia-based dental ceramic to resin cements Bond strength and failure characteristics of zirconia-based dental ceramic to resin cements Premwara Triwatana, Porntida Visuttiwattanakorn, Kallaya Suputtamongkol, Nutthakrij Butrangamdee

M Dent J Volume 36 Number 1 January-April 2016


Introduction Adhesive bonding of all- ceramic prosthesis to tooth abutment has become a basic procedure to achieve esthetically durable cementation. Using a combination of adhesive primer and/or resin cement has been an essential protocol for luting of all-ceramic restoration especially when its retention to tooth structure is unfavorable. Not only aiding in retention, an esthetic outcome of resin-based luting cement is exceptional with its translucency and chosen shades. An increase in fracture resistance of cemented crown has also been reported when an effective bonding of this crown to tooth structure was made.1 Concerning the importance of effective bonding to tooth abutment, several research have been conducted to evaluate an appropriate bonding protocols for various dental ceramics.2 Silane coupling agent is a typical primer used for silica-containing dental ceramics. The inorganic part of silane chemically reacts with –SiOH on the ceramic surface, while an organic group chemically bond to resin-based materials.3 An increase in wettability and reduction in contact angle have also been reported after applying silane on the ceramic surface.4 The results from several studies have been shown that application of silanes after hydrofluoric acid etching could improve the adhesion between silica-containing dental ceramics and some resin-based dental cements. As reported by previous studies, the microtensile bond strength of leucite-reinforced glass-ceramics were 22.8-34.6 MPa5-6, and 32.2-56.8 MPa for lithia-disilicate-based ceramics7-9. Currently, zirconia-based dental ceramics are widely used for fabrication of fixed dental prostheses with wide-range applications. This group of materials possesses high fracture toughness, tooth-like color and translucency and excellent biocompatibility which make them a leading choice for fabrication of anterior and posterior fixed prostheses. Because they have

minute amount or no silica in their compositions, silanes would no longer be a suitable primer for zirconia-based dental ceramics for bonding with resin cement. Some specific surface treatments have been developed to improve the inertness of zirconia surface such as selective infiltration etching, tribochemical silica-coating, laser or acid treatment, etc.10-12 However, these techniques require some special equipment and processes which would not be clinically practical for use in daily practice. The surface treatment with some primers has been an alternative way and it becomes a topic of interest for many dental researchers. Various kinds of adhesive primer have been investigated such as zirconia coupler, some silanes and phosphate-based functional monomers.13-14 However, using phosphate-based functional monomers such as 10-methacryloyloxy-decyl dihydrogenphosphate (MDP) after sandblasting of zirconia surface is proposed to be an effective technique.15-16 Various testing methods (such as shear/microshear, tensile/microtensile) and many surface treatment protocols have been used by numerous dental researchers and resulted in wide-range of bond strength values obtained from these studies, extending from 0 to > 50MPa as reported by Papia et al in 2014.17 In that review study, acceptable bond strength was set at 20 MPa, regardless of the testing techniques. For phosphate-based functional monomers, bonding via chemical reaction is proposed and may occur between hydroxyl groups from the functional monomer and Zr-OH on the zirconia surface.13 The results from a previous study showed that phosphate functional monomer could chemically react with inert zirconia surface, but the extent of bonding and bonding mechanism were not identified.18 Not only chemical reaction that is responsible for the effective bonding of zirconia to resin-based materials, the micromechanical retention would also play a part in the bonding mechanism.

Bond strength and failure characteristics of zirconia-based dental ceramic to resin cements 15Bond strength and failure characteristics of zirconia-based dental ceramic to resin cements Premwara Triwatana, Porntida Visuttiwattanakorn, Kallaya Suputtamongkol, Nutthakrij Butrangamdee


Air-borne particle abrasion of the zirconia surfaces before primer or cement application is recommended; otherwise the bonding could not be achieved.15-16 Air-borne particle abrasion not only creates rough surface but also increases the surface area for bonding. The decrease in apparent contact angle when a surface is roughened is also reported and results in improving the wettability.19

Presently, computer-aided design and computer-aided manufacturing (CAD-CAM) systems are widely used in dentistry for fabrication of fixed dental prostheses, i.e., crown and bridges and implant abutment. Because zirconia-based dental prosthesis can only be fabricated using CAD-CAM systems,

many zirconia blocks are available for different CAD-CAM systems. Still, there are some controversies regarding their bonding ability with resin cements. The objective of this study was to determine the microtensile bond strength of a zirconia-based dental ceramic (IPS Emax ZirCAD) to three resin cements (Panavia F2.0, Multilink N and Calibra®Esthetic resin Cements) which have been widely used in clinical dental practice. The failure patterns of all groups were characterized to define the failure origin and fracture paths of these specimens.

Materials and methods Materials used in this study are summarized in Table 1.

Table 1 Details of materials used in this study obtained from their manufacturersBrand Manufacturer Compositions

IPS e.max® ZirCAD Ivoclar Vivadent, Schaan, Liechtenstein

Pre-sintered, yttrium-stabilized zirconium oxide

Panavia F2.0 Kuraray America Inc., NY, USA

Paste A: 10-Methacryloyloxydecyl dihydrogen phosphate (MDP), Hydrophobic aromatic dimethacrylate, Hydrophobic aliphatic dimethacrylate Hydrophilic aliphatic dimethacrylate, Silanated silica filler, Silanated colloidal silica, dl-Camphorquinone, Catalysts, InitiatorsPaste B:Hydrophobic aromatic dimethacrylate, Hydrophobic aliphatic dimethacrylate, Hydrophilic aliphatic dimethacrylate, Silanated barium glass filler, Surface treated sodium fluoride, Catalysts, Accelerators, Pigments

Multilink N Ivoclar Vivadent, Schaan, Liechtenstein

Base & CatalystDimethacrylate and HEMA, Barium glass filler and silicon - dioxide filler, Ytterbiumtrifluoride, Catalysts and stabilizers, Pigments

Calibra® Esthetic Resin Cement

Dentsply, NY USA Base & CatalystDimethacrylate Resins; Camphorquinone (CQ) Photo-initiator; Stabilizers; Glass Fillers; Fumed silica; Titanium Dioxide; Pigments

Prime & Bond® NTTM Dentsply, NY USA Di- and Trimethacrylate resins, PENTA(dipentaerythritolpenta acrylate monophosphate), Photoinitiators, Stabilizers, Nanofillers - Amorphous Silicone Dioxide Cetylaminehydrofluoride, Acetone

Monobond N Ivoclar Vivadent, Schaan, Liechtenstein

Alcohol solution of silane methacrylate, phosphoric acid methacrylate and sulphide methacrylate.




A pre-sintered yttrium-stabilized zirconia oxide block was cut using a precision cutting machine (Accutom-50, Struers A/S, DK-2750 Ballerup, Denmark) into the dimension of 12.5 x 12.5 x 5 mm. Zirconia blocks were sintered to their final density at 1500°c for 5 hours in the furnace (Sirona in Fire HTC, Sirona Dental Systems, Inc., NC, USA). The final dimension was approximately 10x10x4 mm.

Surface treatments and Cementation Procedures The surface of sintered zirconia blocks was sandblasted perpendicularly for 10 s using 50 μm Al2O3 particles at 1 bar according to manufacturer’s instruction. Then they were cleaned with 95% ethanol in an ultrasonic bath for 5 min before bonding. Before cementation, a 40-micron-thick clear plastic film, approximately 0.5 mm in width, was attached on two opposite border of treated surface of one ceramic block to control the cement thickness. Then two zirconia blocks were bonded together with three resin cements. For Panavia F2.0 resin cement, four blocks of zirconia were used for cementation. Paste A and B were dispensed by half turned of each syringe, then hand-mixed for 20 s. Resin cement was applied over the entire surface of zirconia block. A clear acrylic loading mold was used for holding the bonded specimen in place and also controlling the direction of vertical loading force. Then 50 N load was applied using a loading device, light cured on four surfaces for 3 s at each surface. Then excess cement was removed and light curing was continued on four surfaces of bonded specimens for 20 s each time. For Multilink N resin cement, a universal primer (Monobond N) was applied using a disposable brush on entire surface of all zirconia specimens for 60 s and gently air-blown for 5

s. The resin cement was mixed automatically through a mixing tip and applied over the surface and placed in a loading plastic mold with 50 N loading force. Then the bonded specimen was light cured on 4 surfaces for 3 s and excess cement was removed. Light curing was continued for 20 s at 4 surfaces before removal from a loading jig. For Calibra®Esthetic resin Cement, light cured dental adhesive (Prime & Bond® NTTM) were mixed 1:1 and applied using a disposable brush on entire surfaces of all zirconia specimens and gently air-blown for 5 s then light cured for 20 s. Resin cement was mixed according to the manufacturer’s instructions and applied over the bonding surfaces. Then bonded specimen was placed in a loading mold and vertically loaded with 50N force, light cured on 4 surfaces for 3 s then excess cement was removed. Light curing was continued for 20 s at 4 surfaces. All bonded ceramic blocks were stored at 37°C for 24 hr before microbars fabrication and testing. These blocks were sectioned using a precision cutting machine to obtain microbars with dimension of 1x1x8 mm. All microbars were examined for voids, micro-cracks and any defects in the resin cement layer with an optical light microscope (Nikon Eclipse E400, Nikon imaging Japan Inc., Fukuoka, Japan) at 10X magnification. The microbars at the peripheral of the blocks and those with defects were discarded from the study. Width and depth of all specimens were measured with a digital caliper prior to testing. The microbar was attached to a custom-made microtensile fixture using cyanoacrylate glue. Specimen was positioned parallel to the long axis of the jig and cement layer was at the middle of testing device gap in order to minimize bending stresses. The tensile loading was performed at a crosshead speed of 1 mm/min using a universal testing machine (Instron5565, Instron Corp, Canton, MA, USA)



until fracture occurred. The breaking force was used to calculate the microtensile bond strength (MTBS) using the following equation:

σ = F / AWhere σ is the MTBS (MPa), F = load at fracture (N), and A = surface area of bonding surface (mm2) The mean MTBS values and standard deviation were calculated. Shapiro-Wilk test was used to test the normality of the data and Levene’s test was used for testing the equality of variances. One-way ANOVA was used to analyze the effect of resin cement types on the MTBS values at a significance level of .05.

Fractographic analysis All fractured specimens were ultrasonically cleaned in distilled water for 10 min and dried with oil-free air blow. All surfaces were sputter-coated with gold and examined by a scanning electron microscope (JSM-5410LV, JEOL Ltd., Tokyo, Japan) at different magnifications. A combination of SEM photographs taken in backscattered electron topographic (BET) and backscattered electron composition (BEC) mode of a fracture surface of each specimen was utilized to define the origins and patterns of failure. Mode of failure were categorized into 2 types; adhesive failure when fracture started at the interface between resin cement and ceramic or cohesive failure when fracture started within the resin cement layer

Results The mean MTBS values of all groups are summarized in Table 2. The results from one-way ANOVA showed that type of resin

cement had an effect on the MTBS values. Zirconia specimens bonded with Multilink N resin cement had the highest MTBS. The MTBS values obtained from zirconia specimens bonded with Panavia F2.0 and Calibra Esthetic were comparable. The representative SEM photographs of fracture surfaces of specimens in these groups are shown in Fig.1. Interfacial failure was observed in all zirconia specimens in all groups. The fracture origin was at the interface, but the propagation of a critical crack was sometime into the cement layer. The fracture pattern was similar for all resin cement types. In this study, the delamination type of fracture was dominated in zirconia material. The zirconia surface was also not affected much by the sandblasting process. Small facets and shallow grooves were observed on their surfaces (Fig.2). After fracture, the retention of resin cement remnant was regularly observed on the surfaces of IPS e.max ZirCAD (Fig.3-5).

Discussion In this study, zirconia core material was bonded side by side using three resin cements. Because of its higher fracture resistance compared with those of resin cements, the fracture was confined to occur within the resin cement or at the interfaces. Therefore, the actual bond strength of ceramic to the assigned resin cement could be determined. This technique has been used in some studies and the authors suggested the benefit of this technique that the factual bond strength between ceramic and resin cement could be obtained by excluding substrate variables.6, 20

Table 2 The mean MTBS values of zirconia dental core ceramics bonded to three resin cementsMaterials Panavia F2.0 Multilink N Calibra Esthetics

IPS e.max ZirCAD 22.9±5.6 a 35.5±7.6 b 21.6±5.6 a

Different superscripts mean statistically significant differences between those mean values.




Figure 1 The representative SEM photographs of fracture surfaces of zirconia specimens bonded to three resin cements in BEC (a,c,e) and BET modes of a similar surface (b,d,f).



Figure 2 Sandblasted surfaces of zirconia ceramics used in this study, IPS e.max ZirCAD

Figure 3 The representative SEM photographs of zirconia bonded to Calibra Esthetics cement: (a) fracture surface at 90X, (b) fracture surface near zirconia-adhesive interface, (c) fracture surface on zirconia side at 5000X in BEC mode, and (d) at 5000X in the same area as (c) in SEI mode




Figure 4 The representative SEM photographs of zirconia bonded to Panavia F2.0: (a) at higher magnification in BEC mode, (b) in the same area as (a) in SEI mode

Figure 5 The representative SEM photographs of zirconia bonded to Multilink N: (a) at higher magnification in BEC mode, (b) in the same area as (a) in SEI mode

IPS e.max ZirCAD was chosen in this study because it has wide range of applications and frequently used in clinical practice. This zirconia material was cemented together using three phosphate-based functional monomers which were MDP (in Panavia F2.0), phosphoric acid methacrylate (in Monobond N) and PENTA (dipentaerythritol penta acrylate monophosphate in Prime&Bond NT). For zirconia-based materials, bonding mechanism to resin cement was not as well-established as that of silica-based materials. Bonding zirconia with phosphate monomer groups appeared to be more successful based on the results from several studies.13,15-16,21 In this study, the MTBS of zirconia bonded to

Panavia F2.0 and Calibra Esthetic cements were not as high as that bonded with Multilink resin cement. Because of some variations in adhesive composition (phosphate-based functional monomers) and the application techniques (functional monomers incorporated into the cement or mixed in the bonding adhesive separately), these variations could be the factors responsible for the differences in MTBS values obtained from these three resin cements. However, the observation of fracture surfaces of zirconia specimens revealed that the pattern of remnants left on the zirconia surfaces were differed as shown in Fig.3-5.



For Calibra Esthetics (with Prime and Bond NT), the adhesive layer was thick and strongly attached to resin cement, not the zirconia surface. As a result, delamination of adhesive layer from zirconia was observed (Fig 3.). This delamination seemed to be a clear separation between resin material and zirconia surface at the failure origin and zirconia surface was clearly observed (Fig.3a). However when these fracture surfaces were observed using SEM at higher magnification, the remnant adhesive or cement were left on the pits or grooves on zirconia surface (Fig.3b-d). The zirconia grains were scarcely observed on the surface. This observation might positively indicate the effect of micro-mechanical retention between zirconia and adhesive or resin cements. This clear delamination was also observed for zirconia specimens bonded to Panavia F2.0 and Multilink N at low magnification (Fig.1 c, e). Because of the viscous adhesive (such as Prime and Bond NT) or a resin cement (such as Panavia F2.0), it might not be able to make intimate molecular contact with the entire surface area of zirconia. Therefore, these adhesive or resin cements could not gain the benefit of mechanical or chemical retention as much as that with the thinner adhesive primer that could properly wet the surface. The representative SEM photographs of zirconia specimens bonded to Panavia F2.0 are shown in Fig.4. For zirconia bonded to Multilink resin cement as shown in Fig.5, the thin layer of resin cement covered the zirconia surface was still detected. This better adhesion of Multilink resin cement, caused from either mechanical or chemical retention or both, could explain the differences in MTBS values obtained from three different resin cements. According to this observation, it implied that the compositions and mechanical properties of adhesive and resin cement would play a significant role in the adhesion performance between zirconia and resin cement.

It was clear that the MTBS values obtained in this study were dependent on several factors. The fracture resistance of cement and ceramic was definitely the factors that controlled the bond strength of bilayer. The characteristics of ceramic surface after treatment also determined the failure strength and mode of fracture. Use of adhesive primer was crucial for resin cement that did not contain functional monomer groups necessary for chemical reaction with a ceramic surface. The surface treatment and type of adhesive primers used for bonding of zirconia-based dental ceramics have been the topics of interest to many researchers. However, sandblasting of zirconia surfaces was considered to be an important factor to create effective bonding with resin cement. Even much pressure and larger particles would produce more roughness on a zirconia surface, but phase transformation from tetragonal to monoclinic form could be detrimental to short- and long-term strength of this material.22 Microcracks caused from damaging air-abrasion would also lead to catastrophic failure when subjected to loading.23 However, the mean MTBS values of all groups obtained in this study were greater than the value indicated previously as an acceptable bond strength (20 MPa). This result showed that three resin cements used in this study could provide adequate adhesion with this zirconia-based dental ceramic. The most widely used adhesive primer for bonding with zirconia-based dental ceramics is MDP which is phosphate functional monomer. Even several studies have shown the usefulness of using 10-MDP to produce a strong durable bond with zirconia, but the results are not consistent and the mechanism for bonding is unclear, unlike the bonding mechanism of silane coupling agents. The chemical reaction between zirconia and resin cement containing MDP has been proposed that MDP would bond to OH- groups on the zirconia surface. This




bonding process requires the chemisorption of H2O on the zirconia surface. Few computational models have been constructed to characterize the pattern of water adsorption on yttrium-stabilized tetragonal zirconia polycrystal (Y-TZP) surface. The results showed that the adsorption depended on the crystallographic orientation of the exposed surfaces and atomic arrangement of anions and cations.24-26 Some studies have shown that hydroxylation of tetragonal zirconia surface could take place at moderate temperature (>65°C) and adequate pressure which favors the conditions for low temperature degradation of zirconia.27 On the contrary, there is no information regarding the hydroxylation on zirconia surface at room temperature and pressure. Moreover, airborne-particle abrasion with Al2O3 has been recommended as a surface pretreatment of zirconia surface before adhesive and resin cement application, but phase transformation from tetragonal to monoclinic occurred after this mechanical process. The transformation zone depth was 0.9-1.6 μm from the surface.28 Therefore, bonding to monoclinic phase, instead of tetragonal zirconia has to be taken into account because these two phases have different physical and mechanical properties.29 Further studies on these topics would provide more information for appropriate selection of bonding procedures for zirconia-based dental ceramics.

Conclusions Within the limit of this study, the following conclusions could be drawn: 1. For zirconia-based dental ceramic, specimens bonded with Multilink resin cement had the highest microtensile bond strength. The microtensile bond strength of specimens bonded with Panavia F2.0 and Calibra Esthetics resin cements were comparable. 2. The dominant failure mode of specimens in all groups was interfacial failure.

Funding: noneCompeting interests: noneEthical approval: none

Acknowledgement Materials used in this study were partially supported from Ivoclar Vivadent AG and Dentsply Dental companies.

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