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Year : 2019  |  Volume : 22  |  Issue : 3  |  Page : 335-341

Effect of different surface treatments and ceramic primers on shear bond strength of self-adhesive resin cement to zirconia ceramic

1 Private Practice, Istanbul, Turkey
2 Department of Prosthodontics, Faculty of Dentistry, İstanbul Yeni Yüzyıl University, İstanbul, Turkey

Date of Acceptance28-Nov-2018
Date of Web Publication6-Mar-2019

Correspondence Address:
Dr. G Yildirim
Department of Prosthodontics, Faculty of Dentistry, İstanbul Yeni Yüzyıl University, Sütlüce Mahallesi, Binektaşı Sok. No: 10, Beyoğlu - 34445, Istanbul
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Source of Support: None, Conflict of Interest: None

DOI: 10.4103/njcp.njcp_394_18

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Aims: To evaluate the effect of different surface treatments and ceramic primers on the shear bond strength (SBS) of self-adhesive resin cement to zirconia ceramic. Materials and Methods: A total of 40 zirconia discs (10 mm in diameter and 3 mm in height; StarCeram Z-Med, H.C. Starck, Selb, Germany) were prepared from pre-sintered zirconia blocks. Discs were divided into two groups according to surface treatment: (a) airborne particle abrasion (sandblasting) with 50-μm Al2O3 particles and (b) 9.5% hydrofluoric acid etching. Each of these groups was subdivided into two groups according to the type of primer applied: (a) Z-Prime Plus primer and (b) Clearfil Ceramic Primer. A self-adhesive resin cement (Multilink Speed, Ivoclar Vivadent, Schaan, Liechtenstein) was used to bond with polyethylene molds. All specimens were tested at thermocycled (5000 cycles at 5–55°C for 30 s) conditions. The SBS of the luting cement to the ceramic was measured in a universal testing machine (1 mm/min). Results: The sandblasted groups showed significantly higher SBS values than the acid-etched groups for both primers (P = 0.0001). Independent of the surface treatment, the Z-Prime Plus primer groups showed higher SBS values than the Clearfil Ceramic Primer groups (P = 0.0001). Conclusions: Sandblasting is a more effective method to increase bond strength on zirconia ceramics than hydrofluoric acid etching, and the application of Z-Prime Plus primer increases SBS better than Clearfil Ceramic Primer.

Keywords: Acid etching, ceramic primer, surface conditioning, zirconia ceramics

How to cite this article:
Saleh N E, Guven M C, Yildirim G, Erol F. Effect of different surface treatments and ceramic primers on shear bond strength of self-adhesive resin cement to zirconia ceramic. Niger J Clin Pract 2019;22:335-41

How to cite this URL:
Saleh N E, Guven M C, Yildirim G, Erol F. Effect of different surface treatments and ceramic primers on shear bond strength of self-adhesive resin cement to zirconia ceramic. Niger J Clin Pract [serial online] 2019 [cited 2022 Dec 8];22:335-41. Available from:

   Introduction Top

In the past, fixed partial dentures were primarily made of metal or metal covered by ceramic. With improvements in technology, all-ceramic dental restorations have recently been developed.[1] The popularity of all-ceramic dental restorations has continued to increase because of their superior esthetic appearance, wear resistance, and metal-free structure.[2] Additionally, all-ceramic restorations use biocompatible materials and have demonstrated adequate resistance to occlusal forces. However, their use has been limited to single crown and short-span fixed partial dentures.[3] All-ceramic restorations are considered to be brittle, particularly when they are placed on posterior teeth,[4],[5] because these materials are subject to high tensile stresses.[6] In order to prevent high clinical failure rate, tooth preparation, restoration design, margin thickness, and preparation height should be taken into consideration.[7] Owing to such problems, the biocompatibility, chemical stability, and high mechanical properties of zirconia make it an attractive core material for all-ceramic restorations.[8] Zirconia exhibit better mechanical performance, strength, and fracture resistance than other ceramic materials because they have a flexural strength of more than 900 MPa, fracture toughness of up to 10 MPa, and an elastic modulus of 210 GPa.[9],[10] Along with the mechanical properties of the material used in a restoration, the cementation technique is also important to clinical success. For example, the use of adhesive techniques is recommended to improve the retention, marginal suitability, and fracture resistance of restorations.[11],[12] The adhesion techniques used in all-ceramic restorations depend on the chemical composition of the ceramic system,[13] and surface treatments are necessary to ensure adhesion between the luting agent and the ceramic surface.[14],[15] In addition, the composition of the ceramic determines which surface treatment is appropriate.[2],[16] For example, hydrofluoric acid etching and silanization are obligatory steps for silica ceramics.[13] However, ceramics with high alumina [13],[14] or zirconia [17],[18] cannot be roughened by hydrofluoric acid etching because they do not contain a silicon dioxide (silica) phase. Nevertheless, most previous studies have examined hydrofluoric acid-etched zirconia in terms of its mechanical properties and its surface bond strength with the resin cement.[17],[19],[20] Specifically, these studies have investigated various surface treatments applied to improve bonding to the zirconia ceramic,[21],[22],[23] including selective infiltration etching (SIE),[24] laser etching,[25] alumina coating,[26] silica ceramic coating,[27] tribochemical silica coating,[13],[17],[21],[22] and airborne-particle abrasion (also called sandblasting).[17],[21],[22]

Mechanical surface treatments are used to produce roughness on the ceramic's surface,[16] which increases its surface energy and wettability and exposes more of its surface area to the resin cement, thereby increasing mechanical interlocking and bond strength.[2],[16],[28],[29],[30],[31] For example, sandblasting uses air that contains aluminum oxide (Al2O3) particles with different sizes at a specific pressure to treat the ceramic's surface.[2],[28],[29],[32] It is more effective at treating alumina than zirconia because alumina is less ductile and has a higher surface hardness and larger grain.[32]

Recently, several new ceramic primers have been introduced to the dental market to increase chemical bonding to zirconia ceramics.[13],[33],[34] These include primers that contain a phosphoric acid monomer, 6-methacryloxyhexylphosphonoacetate (6-MHPA), (AZ, primer) or 3-trimethoxysilylpropyl methacrylate, 10-methacryloyloxydecyl dihydrogen phosphate (MDP), ethanol (Clearfil Ceramic Primer) and organophosphate monomer, carboxylic acid monomer and others (Z-Prime Plus).[13],[33],[34] The application of MDP containing bonding agents can increase bond strength to zirconia [35],[36] because of an interaction between the hydroxyl groups of MDP and the cationic surface of zirconia.[37]

Glass ionomer cements from conventional luting agents are often used in the cementation of zirconia ceramic restorations;[23],[34],[38] however, adhesive cementation is preferred due to inadequate retention and resin-bonded fixed dental prosthesis.[21],[23],[34],[39] Self-adhesive resin cements have been developed to simplify bonding procedures.[40] Nevertheless, the results from the literature on bond strength to zirconia ceramics remain very controversial.[38],[40],[41],[42],[43]

The aim of our study was to evaluate the effect of different surface treatments and ceramic primers on the shear bond strength (SBS) of self-adhesive resin cement to zirconia ceramic.

   Materials and Methods Top

In this study, 40 zirconia discs (measuring 10 mm in diameter and 3 mm in thickness; StarCeram Z-Med, Germany) were prepared from pre-sintered zirconia blocks using a CAD/CAM system (Coritec T 350I loader imes-icore, Germany). Following this zirconia discs were polished manually using 600-, 800-, and 1200-grit silicon carbide abrasive paper under cooling water for 1 min and then were sintered in a high-temperature sintering furnace. Subsequently, the discs were cleaned with distilled water in an ultrasonic cleaning machine.

The zirconia discs were divided into two groups according to the type of surface treatment used. The first group was sandblasted with alumina according to the manufacturer's instructions: 50-μm aluminum oxide (Al2O3) particles were applied at a pressure of 0.2 MPa for 20 s and at a distance 20 mm. In the second group, etching was applied with 9.5% hydrofluoric acid (Porcelain Etchant, Bisco, Schaumburg, IL, USA) for 90 s. Each group was subdivided according to the primer applied. The primers were applied to a layer of dry zirconia surface and allowed to react for 1 min, then dried with light air for 10 s [Figure 1]. The test groups are listed in [Table 1].
Figure 1: Light cure the self-adhesive resin cement

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Table 1: Test groups

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For all groups, the self-adhesive resin cement (Multilink Speed, Ivoclar Vivadent, Schaan, Liechtenstein) was used according to the manufacturer's instructions. To standardize the cementation procedure, a special plexiglass mold measuring 4 mm in diameter and 3 mm in depth was designed. The plexiglass mold was placed at the center of the zirconia discs and the cement was applied directly from a mixing syringe; then light polymerized (Elipar 3M ESPE, Seefeld, Germany) for 20 s from each side. The light intensity was 800 mW/cm2. An oxygen-blocking gel (Oxyguard II, Kuraray Medical Inc., Osaka, Japan) was applied for 10 min. The zirconia discs were then removed from the plexiglass mold. The materials used in this study are listed in [Table 2].
Table 2: Materials used in this study

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The cemented samples were applied to the thermocycling at a water temperature of 5–55°C for 5000 cycles and a dwell time of 30 s; the transfer time from one bath to the next was 4 s.

All samples were embedded in blocks of self-cure acrylic resin (Imicryl, Konya, Turkey) using a specially designed steel mold (measuring 20 mm in diameter and 12 mm in depth) and then seated in a shear testing jig. SBSs were determined with a mechanical testing device (Model 3345, Instron, Norwood, MA, USA) at a 1 mm/min crosshead speed [Figure 2]. Data were calculated in Newtons and then converted to megapascals.
Figure 2: Universal testing machine

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Statistical calculations were performed with the Number Cruncher Statistical System 2007 statistical software (NCSS, Kaysville, UT, USA) program for Windows. In addition to the standard descriptive statistical calculations (i.e., mean and standard deviation), the four groups were compared using one-way analysis of variance and Tukey's post-hoc test. An unpaired t-test was used for comparisons between groups. Statistical significance was set at P < 0.05.

   Results Top

The mean SBS values for the SC, SZ, EC, and EZ groups were 2.16 ± 0.45, 2.94 ± 0.42, 0.96 ± 0.42, and 1.78 ± 0.26 MPa, respectively. Significant differences in SBS were observed between the different surface treatments and ceramic primers (P = 0.0001). The SBS values are shown in [Table 3].
Table 3: Shear bond strength (MPa) means for ceramic primers

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The sandblasted groups (SZ and SC) showed significantly higher SBS values than the acid-etched groups (EZ and EC) for both primers (P = 0.0001). Independent of the surface treatment, the Z-Prime Plus primer groups (SZ and EZ) showed higher values than Clearfil Ceramic Primer groups (SC and EC; P = 0.0001) [Table 4]. The highest SBS values were in the SZ group (2.94 ± 0.42 MPa), whereas the lowest SBS values were in the EC group (0.96 ± 0.42 MPa; [Figure 3]).
Table 4: SBS means for all zirconia groups

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Figure 3: The SBS of the four groups

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   Discussion Top

Zirconia ceramics have been widely used as a framework material for tooth-supported or implant-supported restorations owing to their excellent biocompatibility, enhanced strength, and inherent esthetic properties.[44]

Previous studies have found zirconia ceramic restorations to be resistant to fracture loads and to have an optimum in vitro strength;[45],[46],[47] however, along with mechanical properties, the cementation technique used and the reliability of the bond with the luting agent are important to clinical success. The null hypothesis of this study was that the SBS values of the self-adhesive resin cement to the zirconia ceramic interfaces would not be affected by the surface treatment or ceramic primer used. However, our study found that the groups treated with sandblasting demonstrated higher SBS values than those treated by hydrofluoric acid etching, regardless of the ceramic primer used. Also, the groups to which Clearfil Ceramic Primer was applied had lower values than those to which Z-Prime Plus primer was applied. The null hypothesis was therefore rejected.

Various surface treatments have been explored to improve bonding to zirconia ceramic,[21],[22],[23] including SIE,[24] laser etching,[25] alumina coating,[26] silica ceramic coating,[27] tribochemical silica coating,[13],[17],[21],[22] and sandblasting.[17],[21],[22] Previous studies have found hydrofluoric acid etching to be incapable of roughening high-alumina [48],[49] and zirconia ceramics [17],[18] due to their lack of a silica phase. Despite this, several studies have investigated the effects of hydrofluoric acid etching on the mechanical properties of zirconia and on the bond strength between the zirconia's surface and resin cements.[17],[19],[20] For example, Sriamporn et al. evaluated dental zirconia's surface morphology following hydrofluoric acid etching and examined changes to its crystal structure. Their results showed that hydrofluoric acid is able to etch dental zirconia ceramics by creating micro-morphological changes on its surface.[50] Hydrofluoric acid is the most commonly used acid in dental clinical practice, and 4–10% concentrations of hydrofluoric acid have been found to be safe and are preferred in dental applications.[51]

Sandblasting is another surface treatment commonly used for micromechanical retention,[34] which has been found to increase the flexural resistance of zirconia ceramics by inducing tetragonal-to-monoclinic (T-M) phase transformations composed of compressive layers on the zirconia surface.[52],[53] Our study examined two surface treatments, sandblasting and hydrofluoric acid etching, and found the SBS values to be higher in the sandblasted groups.

Ceramic primers are materials used to increase the SBS between resin cements and ceramics. Primers that contain phosphoric acid monomers, which bond chemically to metal oxides such as zirconium dioxide and other end of double bond, react to resin cement.[13],[35],[36] Al-Harbi et al. reported that the use of Clearfil Ceramic Primer enhanced the SBS of Yttria-stabilized zirconia Y-TZP ceramics.[54] Similarly, Tanış et al. reported that the use of a primer containing adhesive phosphate monomer MDP (Z-Prime Plus primer) on a sandblasted zirconium surface increased the bond strength between the zirconia ceramic and resin cement.[55] In our study, we used two ceramic primers that contained MDP (Clearfil Ceramic Primer and Z-Prime Plus primer); we found that the Z-Prime Plus primer groups (SZ and EZ) had higher SBS values than the Clearfil Ceramic Primer groups (SC and EC) regardless of the surface treatment used (P = 0.0001).

The success of a zirconia restoration depends on the quality, strength, and durability of the bond between the resin cement and the restoration.[33],[56] Owing to zirconia's opacity, the polymerization of light-cure resin cement may be impaired; therefore, dual- and chemical-cure resin cement are recommended for luting zirconia ceramics.[33] Da Silva et al. compared the SBS of conventional and self-adhesive resin cements used to lute Yttria-stabilized zirconia; although they reported that the micro-SBS of the self-adhesive resin cement was higher, they found that its micro-SBS decreased after 6 months in water storage aging.[57]

Thermocycling is used to simulate clinical conditions. Mair et al. reported that oral temperatures ranged between −4 and 0°C when eating ice cream to 60–65°C when eating a hot cheese sandwich.[58] In our study, we used thermocycling as an aging method. Although the ISO TR 11450 standard (2003) recommended a short regimen of 500 cycles, previous studies have calculated that 6000 cycles are equivalent to 5 years of clinical use.[59],[60] Therefore, our study used 5000 cycles, which is equivalent to approximately 4 years of clinical function.

In our study, the sandblasted groups showed significantly higher SBS values than the hydrofluoric acid-etched groups regardless of whether Clearfil Ceramic Primer or Z-Prime Plus primer was used (P = 0.0001). This agrees with several previous studies.[14],[35],[55],[61],[62],[63] In both surface treatment groups, the Clearfil Ceramic Primer subgroups (SC and EC) showed lower SBS values than the Z-Prime Plus primer subgroups (SZ and EZ; P = 0.0001). The highest SBS was noted in the SZ group (2.94 ± 0.42 MPa), while the EC group (0.96 ± 0.42 MPa) was determined to have the lowest SBS values.

Al Harbi et al. demonstrated that primers that contained MDP, such as Z-Prime Plus primer and Clearfil Ceramic Primer, had higher SBS values than those that did not; they therefore concluded that Z-Prime Plus primer and Clearfil Ceramic Primer obtain better bond strength to zirconia ceramics.[54]

Application of priming agents containing MDP yielded the durable bond strength of resin-based luting agent to zirconia ceramics.[41],[46],[64]

Tanış et al. also investigated the effect of sandblasting and Z-Prime Plus primer on zirconia ceramic and observed a SBS of 15.25 MPa, which is substantially higher than our results for this group (2.94 ± 0.42 MPa).[55] This difference may stem from the lack of thermocycling in Tanış et al.'s study, which the author recommended for future studies.

   Conclusions Top

This study had two significant findings:

  1. Regardless of the type of ceramic primer used, sandblasting is a more effective method to increase SBS than hydrofluoric acid etching
  2. The Z-Prime Plus primer increased SBS better than Clearfil Ceramic Primer.

Financial support and sponsorship


Conflict of interest

There are no conflicts of interest.

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  [Figure 1], [Figure 2], [Figure 3]

  [Table 1], [Table 2], [Table 3], [Table 4]


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