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Evaluation of the bond strength of feldspathic porcelain applied on aged and non-aged zirconia substructures

BMC Oral Health volume 25, Article number: 517 (2025) Cite this article

Abstract

Background

In the use of zirconia as a substrate material, the bonding mechanism with veneer ceramic and the effect of aging on the material are not yet fully known. The aim of this study is to evaluate the bond strength of zirconia substructure material with veneer ceramic before and after aging, which has been applied different surface treatments.

Materials and methods

In this study, a total of 60 samples were obtained from the zirconia block in the same dimensions by using a microcut device. The prepared samples were randomly divided into three groups (n = 20) to apply different surface treatments (sandblasting, sandblasting + acid + silane-containing primer, Rocatec system + silane-containing primer). Afterwards, each group that applied different surface treatments was divided into two, and 10 samples from each group were subjected to thermal cycle treatment. The surface treatments applied before the thermal cycle on a total of 30 samples that came out of the thermal cycle were repeated under the same standards. A total of 60 specimens, whose surface preparations were completed, were covered with superstructure ceramic. Then, a shear bond strength test, was applied to each sample and statistical analysis was evaluated with the Post-Hoc LSD test by applying 2- way analysis of variance (Two Way Anova) and Bonferroni correction (α = 0.05).

Results

According to the results of the statistical analysis, the highest bond strength was found in the Rocatec system + silane-containing primer group between both the aged and non-aged groups (p < 0.05). No statistically significant difference was found between the sandblasting group and the sandblasting + acid + silane-containing primer group. Shear bond strength was found to be statistically significantly lower in all groups that applied different surface treatments after the aging process (p < 0.05).

Conclusions

According to the results of this study, the application of Rocatec system + silane- containing primer to zirconia as a surface treatment significantly increases the bond with veneer ceramic.

Peer Review reports

Introduction

High-strength zirconia is used because of their chemical stability, physical and mechanical characteristics, and the use of new technologies (CAD/CAM) for fabricating a substructure for all-ceramic restorations [1,2,3].

Zirconia ceramics have a high crystal content, resulting in lower translucency compared to natural teeth [4]. For esthetic reasons, appropriate veneering ceramic can be veneered into zirconia core by either a hand-layered powder build-up or a pressed technique [5]. However, to date hand-layering technique is more common [6].

According to studies, the most common failures observed in these restorations are the complete or layered separations of the superstructure porcelain from the core material [7]. The inability to achieve adequate bond strength between the two materials has raised concerns regarding the long-term clinical success of zirconia restorations [8].

There are many factors affecting the bond strength between the core material and veneer ceramic in zirconia-based fixed prosthetic restorations. These factors include patient-related factors, inability to achieve ideal occlusion, surface treatments applied to the zirconia core material, residual stresses resulting from differences in thermal expansion coefficients between the core structure and veneer ceramic, structural defects in materials (cracks, fractures, etc.), phase transformations of zirconia, surface wettability, inappropriate geometry of the restoration, veneer ceramic application technique, number of firings, volumetric shrinkage of veneer ceramics, and inadequate cooling systems [9].

Many studies have investigated different surface treatment applications to increase surface area and bonding quality for a stronger micromechanical connection. Researchers have evaluated the effects of mechanical abrasion methods such as grinding with diamond (or other) rotary instruments to increase surface roughness on zirconia [10], sandblasting with Al2O3 particles [11], acid etching (mostly HF) [10], plasma spraying [12], roughening with heat [13], silica coating [14], laser application [11], and combinations of any of these techniques [15].

Since the most significant reason for failure in zirconia is the bond failure between the core and veneer ceramic, many studies have evaluated this issue. However, this failure persists [9, 14, 16,17,18].

It has not been fully explained how the bond strength of veneer porcelain applied on a zirconia substructure changes due to aging effects and different surface treatments. In a zirconia substructure used in the oral cavity, when fracture or chipping of the superstructure porcelain occurs, it is a matter of curiosity whether it is more effective to replace the aged substructure or to repair it by adding new porcelain. Therefore, the aim of this study is to investigate the effect of different surface treatments on the bond strength of aged and non-aged zirconia substructures and to compare the effectiveness of substructure replacement and repair methods in aged restorations. The null hypothesis of this study is that different surface treatments and thermal cycling applications would not affect the bond between the zirconia substructure and veneer ceramic.

Materials and methods

In this study, the bond strength created by zirconia frameworks subjected to different surface treatments was compared before and after thermal cycling with the superstructure porcelain.

Preparation of zirconia framework samples

The material used in this study was partially sintered yttria-stabilized zirconia, specifically Nacera® Shell (Doceram Medical Ceramics, Dortmund, Germany). Zirconia blocks were sectioned into dimensions of 12 × 12 × 1.2 ± 0.5 mm using a microcut device (Microcut 201, Mekton Instruments Inc., Bursa, Turkey). A total of 60 zirconia framework samples were prepared, with 10 framework samples in each subgroup (n = 10) (Fig. 1).

Fig. 1
figure 1

Appearance of the prepared zirconia framework samples before sintering and the measurement of their dimensions with a digital micrometer

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The framework samples were sintered in a sintering furnace (InFire HTC Speed, Sirona Dental Systems GmbH, Bensheim, Germany) at a sintering temperature of 1500 °C, following the manufacturer’s recommendations. The framework samples were left to cool according to the manufacturer’s guidelines after being removed from the furnace. To eliminate the effects of dimensional changes, the framework samples were re-measured using a digital micrometer (Mahr, GmbH, Esslingen, Germany). Framework samples that did not meet the specified dimensions were discarded and re-prepared to achieve the final dimensions of 10 × 10x1 mm.

A total of 60 zirconia framework samples were randomly divided into three groups for different surface treatments after the sintering process:

  1. 1.

    Group 1: Sandblasting group.

  2. 2.

    Group 2: Sandblasting + acid + silane-containing primer group.

  3. 3.

    Group 3: Rocatec sandblasting system + silane-containing primer group.

Surface treatments

In Group 1, the zirconia framework samples were roughened using aluminum oxide (Al2O3) sand with a particle size of 50 μm (Arge Dental, Germany) in a sandblasting device (Combilabor CL-FSG3 Heraeus Kulzer, Hanau, Germany) at approximately 10 mm distance for 10 s under 2 atmospheres of air pressure. A metal apparatus was used to standardize the 10 mm distance (Fig. 2). After the process, the framework samples were cleaned in an ultrasonic cleaning device (Elmasonic S 300 H, Elma Company, Germany) first in acetone and then in distilled water for 10 min each. This group was evaluated as the control group with surface treatment applied according to the manufacturer’s instructions.

Fig. 2
figure 2

Sandblasted zirconia framework sample

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In Group 2, the zirconia framework samples were sandblasted under the same conditions as Group 1, followed by cleaning in an ultrasonic cleaning device (Elmasonic S 300 H, Elma Company, Germany) with acetone and distilled water for 10 min each. A solution of hydrofluoric acid (Ivoclar Vivadent, Schaan, Liechtenstein) at a concentration of 9.5% was applied to the sandblasted surfaces for 2 min. The samples were rinsed and dried using an air–water spray, and a silane-containing primer (G-Multi Primer) was applied for 60 s, followed by air drying.

In Group 3, the zirconia framework samples were processed according to the Rocatec system instructions; initially, Rocatec Pre abrasive material composed of 110 μm Al2O3 particles was used to roughen the framework samples from a distance of 10 mm under 2.8 bar pressure for 10 s. Following this, Rocatec Plus abrasive coating material (3 M ESPE AG Dental Products, Seefeld, Germany), composed of 110 μm Al2O3 particles coated with silicon oxide, was applied to the framework sample surfaces from a distance of 10 mm under 2.8 bar pressure for 13 s. After roughening and silica coating, a silane-containing primer (G-Multi Primer, GC Europe) was applied for 60 s and dried.

Thermal cycling procedure

Following the surface treatments applied to the total of 60 zirconia framework samples, each group (n = 20) was divided into two subgroups: thermally cycled (TC(+)) and non-cycled (TC(-)) groups (n = 10). Thirty framework samples from the differently treated surfaces were subjected to thermal cycling in a thermal cycle device (SD Mechatronik Thermocycler, Westerham, Germany) with a bath temperature of 5–55 °C, a transfer time of 10 s between baths, and a dwell time of 30 s in the bath. The ISO value for thermal cycles was obtained from a study by Morresi et al. [19]. This cycle simulates one year of use in the oral cavity, totaling 10,000 cycles [20].

The surface treatments performed before thermal cycling were reapplied under the same conditions to the 30 framework samples emerging from the thermal cycling device.

Layering technique

The layering technique was used for the Vita VM9 Base Dentine (Vita Zahnfabrik Bad Säckingen, Germany) veneer porcelain applied to the framework samples. To ensure standardization, a mold was prepared from teflon material (Fig. 3). ISO’s TR 11405 specification for the bonding of materials to dental tissues (ISO/TR 11405:2003) was used in this study. In this specification, the final dimensions of the superstructure material to be applied were determined to be 5 mm in diameter and 3 mm in height. In the layering technique, to compensate for the shrinkage that would occur after firing and to avoid the need for additional firing, the mold was prepared to be wider and taller than the desired final dimensions. The mold was split in half using a separator and joined with dental wax. This way, after the porcelain stacking process was completed, it could be easily separated into two pieces, allowing the porcelain to be obtained as a single piece (Figs. 4 and 5).

Fig. 3
figure 3

Teflon mold to ensure standardization

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Fig. 4
figure 4

Condensation of porcelain in a teflon mold

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Fig. 5
figure 5

a Samples before firing. b Samples after firing

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The zirconia framework sample was placed under the prepared teflon mold, and the veneer porcelain was applied into the mold using the condensation method. During the process, excess liquid accumulating on the porcelain was removed with a paper towel. To prevent the porcelain from sticking to the teflon mold, a low-viscosity silicone-based separator material (Picosep- 1552–0030, Germany) was used. After the procedure was completed, the teflon mold was carefully separated into two halves. Thus, porcelain was obtained as a single piece with the width of the mold used. The firing process (Ivoclar Programat P90, Ivoclar Vivadent AG, Schaan, Liechtenstein) was carried out according to the manufacturer’s recommendations.

Shear bond strength (SBS) test

The measurement of bonding strength was performed using a universal testing machine (Lloyd-LRX; Lloyd Instruments, Fareham, UK). A total of 60 samples prepared with veneer porcelain applied over a zirconia base were fixed in a special mold using self-polymerizing acrylic resin to be placed in the testing machine. The tip of the cutting device was positioned at a 90-degree angle to the surface where the zirconia base and veneer porcelain met. The test was conducted by applying a load at a speed of 1 mm/min.

The force value at the point of separation between the two surfaces was measured in Newtons (N). To calculate the load per unit area, the following formula was used to convert the Newton (N) values to Megapascals (MPa).

$$\mathrm{Shear}\;\mathrm{bonding}\;\mathrm{strength}\;\left(\mathrm{MPa}\right)=\mathrm{Load}\;(\mathrm N)/\;\mathrm{Area}\;(\mathrm{mm}^2)$$
$$\mathrm{Area}=(\pi\times\mathrm r^2)/4(\mathrm{mm}^2)$$

r = radius of the bonding surface

Statistical analysis

The statistical analysis of the obtained data was performed using the SPSS Analysis Program. The normality of the data was assessed using the Shapiro–Wilk test, and it was determined that the data exhibited a normal distribution. The shear bonding strength data obtained from different groups were evaluated using two-way ANOVA and Bonferroni correction (α = 0.05), followed by Post-Hoc LSD testing. Statistical significance was accepted at the level of p < 0.05.

Results

In this study, in accordance with the data obtained, the effect of different surface treatments on shear bonding strength was compared, using 10 samples (n = 10) in each group. The post hoc power analysis of this study was found to be 98.6%, with a 95% confidence interval and a 5% type I error rate.

Statistical analysis indicated that both the aging procedure and surface treatment had a significant effect on the shear bond strength of the samples, and the interaction of these two factors was not statistically significant (p > 0.05).

Table 1 presents the mean, standard deviation (SD), minimum (Min), and maximum (Max) values of shear bond strength (MPa) in non-aged TC (-) groups. Among the non-aging TC(-) groups, the highest shear bond strength was observed in the group using the “Rocatec system + silane-containing primer” as a surface treatment. The shear bond strength values of the other 2 groups that were not aged were significantly lower than the “Rocatec system + silane-containing primer” group. There was no statistically significant difference between these two groups.

Table 1 Mean, standard deviation (SD), minimum (Min) and maximum (Max) values of shear bond strength (MPa) in non-aged TC (-) groups
Full size table

Table 2 presents the mean, standard deviation (SD), minimum (Min), and maximum (Max) values of shear bond strength (MPa) in aged TC (+) groups. Among the aged TC (+) groups, the highest shear bond strength was observed in the group using the “Rocatec system + silane-containing primer” as a surface treatment. The shear bond strength values of the other 2 groups that were aged were significantly lower than the “Rocatec system + silane-containing primer” group. There was no statistically significant difference between these two groups.

Table 2 Mean, standard deviation (SD), minimum (Min), and maximum (Max) values of shear bond strength (MPa) in aged TC (+) groups
Full size table

It was observed that the shear bond strength values decreased significantly in the aging TC (+) samples compared to the non-aging TC (-) groups (Tables 3, 4 and Fig. 6).

Table 3 Mean shear bond strength values of samples in all groups (p < 0,05)
Full size table
Table 4 Statistical comparison of mean shear bond strength values of all groups
Full size table
Fig. 6
figure 6

Graphical representation of shear bond strength values of all groups (p<0.05)

Full size image

Discussion

Although fractures are rarely encountered in zirconia substrates, chipping between the substrate and veneer ceramic is the most common cause of clinical failures [21]. Restorations are exposed to different temperatures, forces and humidity in the oral environment. This causes mechanical and thermal fatigue, triggering transient deformations and internal stresses in materials and interfaces [22, 23].The bond strength of veneer porcelain applied to a zirconia substructure and its changes due to aging effects and different surface treatments have not been fully elucidated. In clinical practice, when chipping or fracture occurs in the veneer porcelain, it remains unclear whether replacing the aged zirconia substructure or repairing it by adding new porcelain is the more effective approach. This study aims to compare the effectiveness of substructure replacement and repair methods in aged restorations and to evaluate the impact of different surface treatments on bond strength.

The null hypothesis, which states that different surface treatments and thermal cycling applications would not affect the bond between the zirconia framework and veneer ceramics, was compared with the results of our study. The null hypothesis, which stated that surface treatments and thermal cycling applications would not affect the bond between the zirconia framework and veneer ceramics, was rejected. The results of the study indicate that surface treatments and aging do have a significant impact on bond strength.

Mosharraf et al. investigated the effects of different surface treatments on the shear bond strength between various zirconia frameworks and veneer ceramics. They reported that these treatments significantly affected the bond strength between the two materials [24].

Rosellini et al. examined the effects of different surface treatments and thermal cycling on the bond between zirconia and veneer ceramics. They stated that while different surface treatments did not have a significant effect on shear bond strength, thermal cycling significantly reduced this value [25].

HF is insufficient for roughening high crystalline ceramics, such as zirconia, which has a weak glassy content. Additional methods are needed to achieve adequate mechanical interlocking in these ceramics [26]. In this study, a combination of sandblasting, acid, and silane-containing primer was used to roughen the zirconia framework. The reason that the primer group with sandblasting, acid, and silane did not show a significantly higher bond strength compared to the group that only underwent sandblasting may be due to the 2-min application time. The potential increase in bond strength between the veneer ceramic and the substrate due to increased surface roughness with a 15-min application should be investigated in upcoming studies.

In a study by Ghaffari et al., the effects of thermal and mechanical cycles on the bonding of zirconia frameworks with veneer ceramics subjected to different surface treatments were investigated [27]. The control group consisted of polished surfaces, while tribochemical abrasion prepared with the Rocatec system and sandblasting with Al2O3 were applied as surface treatments. It was observed that the shear bond values were lower in all samples subjected to aging, but this was not statistically significant. In this study, however, all values were statistically significantly lower after aging. Thus, the study by Ghaffari et al. partially supports this study. The difference observed between the two studies may be attributed to Ghaffari et al.’s use of a thermal cycle consisting of 6,000 cycles, with a 15-s dwell time and a 5-s transfer time. In our study, 10,000 cycles, a 30-s dwell time, and a 10-s transfer time were used. The highest values were observed in the group treated with Al2O3 sandblasting + primer among both aged and non-aged samples. In this study, however, the highest values among both aged and non-aged groups were found in the Rocatec system + primer group. This difference can be interpreted as a result of the different formulations of the primers used in the Rocatec system in the two studies. In both studies, the same silane-containing primer (GC Corporation, Yahishama Co., Tokyo, Japan) was used in the groups with Al2O3 sandblasting + primer without aging, and similar values were found.

In the study conducted by Cengiz and Çevik, the effects of different surface treatments applied to zirconia surfaces on the shear bond strength between composite resin and zirconia after aging were examined [28]. According to the results of the shear bond strength tests, the highest value was observed in the group using the Cojet system. The Cojet system can be described as the chairside application form of the Rocatec system used in this study. This result parallels the findings of this study. Specifically, we can say that the tribochemical surface treatment after aging reduced the bond strength between the two materials less than other surface treatments.

Guess et al. investigated the effect of thermal cycles on the shear bond strength between various zirconia frameworks and veneer ceramics [18]. At the end of the study, no statistically significant difference was found between aged and non-aged samples. However, in this study, the shear bond values significantly decreased after aging. The differences may be attributed to the variations in the mechanical and physical properties of the materials used and the fact that the veneer ceramic application was performed by different individuals, leading to inconsistencies in application standards. Korkmaz et al. studied the effect of different surface treatments on the bond between veneer ceramics and zirconia frameworks, applying five different surface treatments to the samples [29]. The samples were then subjected to shear bond strength testing. The highest shear bond strength value was found in the group with metal primer, and no statistically significant difference was found among the other groups. In light of this information, it is thought that chemical surface treatment may provide more benefits compared to mechanical surface treatments to strengthen the bond between the two materials. In this study, metal primer was not used; however, the lack of significant difference between the sandblasting group and the sandblasting + acid + silane-containing primer group is similar to the lack of significant differences among the other four groups in this study.

The limitations of this study include the limited number of surface treatments applied, the use of a single type of zirconia and veneer ceramic material, the aging process being conducted under in vitro conditions, the inability to fully replicate intraoral usage, and the aging process representing only one year of use. Other limitations include the layering method applied to the veneer ceramic on the zirconia and the inability to maintain the same conditions for each sample.

Conclusion

  1. 1.

    To enhance the bond strength between the zirconia framework and veneer ceramics, it is recommended to perform surface treatment using the Rocatec system + silane-containing primer before applying veneer ceramics and during fracture repair.

  2. 2.

    Considering the differences in bond strength between aging zirconia and non-aging zirconia, it is advised to replace the substructure rather than reapplying porcelain onto the aging zirconia substructure. The bond strength of aging zirconia may fall below the accepted clinical threshold, making substructure replacement a more reliable option compared to simply reapplying veneer ceramics.

Further research

Further studies are needed to deepen the understanding and development of the bond between the zirconia framework material and the superstructure.

Data availability

The datasets used and/or analyzed during the current study are available from the corresponding author upon reasonable request.

Abbreviations

Al2O3 :

Aluminum Oxide

ANOVA:

Repeated Measures Analysis of Variance

CAD-CAM:

Computer Aided Design And Computer Aided Manufacturing

HF:

Hydrofluoric Acid

TC(+):

Thermally Cycled

TC(-):

Non-thermal Cycled

Y-TZP:

Yttria Stabilized Tetragonal Zirconia Polycrystal

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Acknowledgements

I would like to thank the staff of the Central Research Laboratory of Ankara University for their contributions while conducting this study.

Funding

The authors received no specific funding for this work.

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Authors and Affiliations

  1. Department of Prosthodontics, Faculty of Dentistry, Ankara University, Beşevler, Ankara, 06560, Turkey

    Berna Ozdemir, Derya Oztas, Fehmi Gonuldas & Zeynep Bilen

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  1. Berna Ozdemir
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Contributions

Berna Ozdemir: Investigation and data collection, methodology. Derya Oztas: Data interpretation. Fehmi Gonuldas: Concept/design, methodology, corresponding, critical revision of the article. Zeynep Bilen: Data analysis and statistical analysis, critical revision of the article.

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Correspondence to Fehmi Gonuldas.

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Ozdemir, B., Oztas, D., Gonuldas, F. et al. Evaluation of the bond strength of feldspathic porcelain applied on aged and non-aged zirconia substructures. BMC Oral Health 25, 517 (2025). https://doiorg.publicaciones.saludcastillayleon.es/10.1186/s12903-025-05884-9

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  • DOI: https://doiorg.publicaciones.saludcastillayleon.es/10.1186/s12903-025-05884-9

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BMC Oral Health

ISSN: 1472-6831

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