Background: Zirconia is a new restorative material that has gained great popularity in the field of prosthodontics because it is superior in terms of mechanical properties, though its inert surface does not allow a reliable adhesion with resin cements. Objective: To determine the impact of various surface modification methods on the bond strength of zirconia crowns with self-adhesive resin cements. Methodology: This experimental study was done at Department of Dental Materials. A total of 60 standardized zirconia (Y-TZP) specimens were produced using the CAD/CAM system and divided into four groups (n = 15 each): laser treatment, airborne-particle abrasion, tribochemical silica coating, and control (no treatment). Under uniform conditions, self-adhesive resin cement was used to adhere all of the specimens to composite resin substrates. The data were examined using SPSS version 26. After testing for normalcy using the Shapiro-Wilk test, one-way ANOVA and post hoc Tukey were performed. Results: The tribochemical silica coating group registered the highest bond strength, followed by airborne-particle abrasion and laser treatment, and the control group registered the lowest values. Surface treatment and failure mode (p = 0.010) were also found to be significantly associated, with treated groups having more mixed and cohesive failures. Conclusion: The bond strength of zirconia crowns with self-adhesive resin cements was significantly improved by surface modification, and the best technique to boost adhesion and failure resistance was tribochemical silica coating.
Aesthetic and durable dental restorations have become a major demand in modern prosthodontics due to the developments in the field of material science and patient expectations.[1] Zirconia-based ceramics have been widely accepted among the restorative materials available because of the improvement in mechanical strength, fracture resistance, and biocompatibility.[2] Zirconia, also known as yttria-stabilized tetragonal zirconia polycrystal, or Y-TZP, is a denture material that exhibits transformation toughening action with a high flexural strength (900–1200 MPa).[3] It is one of the surest materials to use in the fabrication of fixed dental prostheses, especially in the posterior regions.[4] Nevertheless, in spite of all these desirable mechanical properties, the difficulty in ensuring a lasting bond between zirconia and resin-based luting agents is an important clinical problem.
In contrast to silica-based ceramics, zirconia has a polycrystalline structure with low proportions of glass that restricts its capability to be etched by conventional methods of hydrofluoric acid.[4] This chemical inertness leads to lower surface energy and poor micromechanical retention, which eventually leads to a decrease in bond strength with resin cements. It has been demonstrated that the bond strength values of resin cements to untreated zirconia surfaces may be comparatively low, typically between 3 and 8 MPa, based on the cement type and test conditions.[5] Therefore, poor bonding can result in clinical failures like debonding, marginal leakage, and decreased restoration longevity.
To address these shortcomings, several surface modification methods have been proposed, including airborne-particle abrasion (sandblasting), tribochemical silica coating, laser treatment, and the deposition of chemical primers with functional monomers in them, such as 10-MDP. Surface roughening by sandblasting has been demonstrated to provide a significant increase in micromechanical interlocking and improvement in bond strength by increasing the surface area and wettability.[6] There is also an increasing popularity of the self-adhesive resin cements, which have simplified clinical use by removing the need to use two separate clinical steps: etching and bonding, yet offer acceptable bond strength and clinical performance.
Recent research on self-adhesive resin cements has demonstrated good clinical results and retention rates as high as 95% after 24 months when applied to zirconia crowns.[7] Nonetheless, the literature is not consistent on the best surface treatment protocol that is necessary to achieve the maximum bond strength. Although certain reports indicate that varying resin cements display similar values of bond strength (around 11-12 MPa), the effect of surface alteration is a crucial factor that defines the adhesion stability.[8] Moreover, the adhesive interface may also be compromised by other factors like aging, thermocycling, and surface contamination, which may indicate the necessity of standardized and evidence-based procedures.[9]
Despite extensive investigation, the best surface treatment method for strengthening the binding between zirconia restorations and self-adhesive resin cements is still unknown. Most of the available literature either addresses traditional resin cements or considers small-scale surface treatments, which leaves a knowledge gap on the interaction between the new method of surface modification and a simplified luting system. In order to fill this important gap, a comprehensive analysis of the impact of several surface modification techniques on the bond strength of zirconia crowns in conjunction with self-adhesive resin cements was conducted. In addition to improving clinical results, a situation-appropriate methodology is essential for expediting the procedure without compromising the durability of restorations. Finding out how various surface modification techniques affected the bond strength of zirconia crowns bonded with self-adhesive resin cements was the aim of this experimental study.
This in vitro experimental study was conducted to evaluate the influence of surface modification techniques on the bond strength of zirconia crowns when used with self-adhesive resin cements. The study was carried out in the Department of Dental Materials at equipped with CAD/CAM and material testing facilities. The duration of the study was one year. OpenEpi version 3 was used to calculate the sample size by using the standard formula of proportion estimation. An earlier research provided a prevalence of 85% of better bond strength following surface treatment, which was used with a confidence level of 95 (Z = 1.96) and a margin of error of 8, yielding 49 specimens.[10] In order to provide sufficient group distribution and address potential specimen loss during preparation and testing, the number of final samples was set at 60, with each group having 15 samples. A non-probability consecutive sampling method was employed. Zirconia samples meeting the inclusion criteria were then prepared and incorporated in the order they were available to the point of attaining the desired sample size. The inclusion criteria included zirconia specimens that were produced using CAD/CAM technology, zirconia polycrystal with yttria as a stabilizer, and standardized dimensions with uniform surfaces. Specimens that had visible cracks, porosities, contamination or dimensional errors were eliminated. Moreover, specimens broken in the process of either preparation, surface treatment or mechanical testing were not considered in the final analysis. A total of 60 zirconia specimens that had been sintered in accordance with the manufacturer's instructions were subjected to CAD/CAM milling. Based on the type of surface change, the specimens were split into four groups at random. Group I received no surface treatment; Group II received airborne particle abrasion using 50 µm aluminum oxide particles; Group III received tribochemical silica coating; and Group IV received laser surface treatment. Following surface modification, each specimen underwent a 10-minute ultrasonic cleaning in distilled water before being allowed to air dry. The self-adhesive resin cement was then placed on as per the manufacturer's instructions, and the zirconia specimens were bonded to blocks of composite resin at a constant load to achieve standardized cement thickness. After cementation, each specimen was placed in distilled water at 37°C and allowed to stand for a whole day to simulate oral conditions. To simulate heat stressors in the oral cavity, 500 cycles of thermocycling between 5 and 55 degrees Celsius were performed. A universal testing machine was used to test the bonds' strength. Shear force was applied at a crosshead speed of 0.5 mm/min until the bond failed. Megapascals (MPa) were used to convert the peak failure load, which was measured in Newtons. The manner of failure, which was categorized as adhesive, cohesive, or mixed failure, was also identified using a stereomicroscope (40x). For analysis, the collected data was entered into SPSS 26. The failure mode was the qualitative variable and was displayed as a frequency and a percentage, while bond strength was the quantitative variable and its values were shown as mean and standard deviation. The normality of the data distribution was assessed using the Shapiro-Wilk test. The four groups' mean bond strengths were compared using one-way analysis of variance (ANOVA), and multiple group comparisons were performed using a post hoc Tukey test. Fisher's exact test was used to assess categorical variables, and a p-value of 0.05 or less was considered statistically significant.
|
Group |
Surface Treatment |
n |
Mean ± SD (MPa) |
Min–Max |
|
I |
Control (No treatment) |
15 |
5.82 ± 1.12 |
4.10–7.60 |
|
II |
Airborne abrasion |
15 |
11.45 ± 1.35 |
9.20–13.80 |
|
III |
Silica coating |
15 |
13.02 ± 1.18 |
11.00–15.10 |
|
IV |
Laser treatment |
15 |
9.76 ± 1.27 |
7.80–11.90 |
|
Analysis Type |
Comparison |
Sum of Squares |
df |
Mean Square |
F-value |
Mean Difference (MPa) |
95% Confidence Interval |
p-value |
|
ANOVA |
||||||||
|
Between Groups |
412.36 |
3 |
137.45 |
78.92 |
— |
— |
<0.001 |
|
|
Within Groups |
97.56 |
56 |
1.74 |
— |
— |
— |
— |
|
|
Post Hoc (Tukey) |
||||||||
|
I vs II |
— |
— |
— |
— |
-5.63 |
-6.85 to -4.41 |
<0.001 |
|
|
I vs III |
— |
— |
— |
— |
-7.20 |
-8.35 to -6.05 |
<0.001 |
|
|
I vs IV |
— |
— |
— |
— |
-3.94 |
-5.15 to -2.73 |
<0.001 |
|
|
II vs III |
— |
— |
— |
— |
-1.57 |
-2.75 to -0.39 |
0.018 |
|
|
II vs IV |
— |
— |
— |
— |
1.69 |
0.48 to 2.90 |
0.012 |
|
|
III vs IV |
— |
— |
— |
— |
3.26 |
2.13 to 4.39 |
<0.001 |
|
|
Group |
Adhesive n (%) |
Cohesive n (%) |
Mixed n (%) |
p-value |
|
I |
11 (73.3%) |
1 (6.7%) |
3 (20.0%) |
0.010 |
|
II |
6 (40.0%) |
3 (20.0%) |
6 (40.0%) |
|
|
III |
3 (20.0%) |
5 (33.3%) |
7 (46.7%) |
|
|
IV |
8 (53.3%) |
2 (13.3%) |
5 (33.3%) |
The results of this experiment demonstrate that surface modification of zirconia crowns with self-adhesive resin cements greatly increased the bond strength. The tribochemical silica coating group had the strongest bond, followed by airborne particle abrasion, and the control group had the weakest bond. These findings are in excellent agreement with recent research highlighting the importance of surface preparation in enhancing zirconia adhesion. All of the surface-treated groups demonstrated much stronger bonds than untreated zirconia, according to a study published in BMC Oral Health (2023). This result supports the existing conclusion that untreated zirconia has poorer bonding capacity.[11]
Likewise, a recent systematic review and meta-analysis (2023) emphasized that mechanical and chemical surface treatment of zirconia restorations can substantially enhance the bond strength and durability of zirconia restorations in comparison with control groups, which supports the result of the present study.[12] Another meta-analysis further established that the bond strength does not just rely on the surface treatment, but also depends on the aging conditions, whereby treated surfaces have a better duration of existence.[13]
The excellent performance of silica coating in the current study is in line with other recent studies. It has been demonstrated that tribochemical silica coating improves micromechanical retention as well as chemical bonding via silane coupling and thus achieves greater bond strength than alternative methods. Conversely, airborne-particle abrasion has been cited as the most favorable approach in some studies. Although other techniques also shown a considerable increase in bond strength above control groups, a 2024 study published in BMC Oral Health found that airborne-particle abrasion had the best binding strength between various types of zirconia.[14] This minor discrepancy could be explained by the variations in zirconia composition, particle size, and experimental procedures.
The results of the current study are also consistent with the study by Swarnakar et al. (2022), which revealed much greater bond strength values of sandblasted zirconia than unblasted ones, which proves the significance of surface roughening in strengthening adhesion.[15] Moreover, researchers in 2023 have stressed that mechanical and chemical surface treatments show better bonding results in comparison to single-modality strategies, which also aligns with the high performance in the silica-coated group in the current study.[16]
Moreover, recent studies on the topography and wettability of surfaces have shown that a high degree of surface roughness and wettability is also a crucial factor in the strengthening of zirconia bonds.[17] This is in line with the current results, in which the bond strength was significantly greater in treated groups with modified surface properties than in the smooth and untreated control group.
The fact that the majority of adhesive failures occurred in the control group and mixed/cohesive failures in the treated groups in this study further confirms the enhancement in bonding that was attained due to surface modification. The same trends have been observed in the current literature, with stronger adhesion being linked to cohesive or mixed failures, which provides a more stable and lasting bond interface. Recent 2023 studies have continued to show this reduction in failure mode with enhanced surface treatments.[11, 18]
Although the overall consensus is there, there are slight differences in the studies on the best surface treatment method. Although the current research has found silica coating to be the best method, there are studies that have preferred airborne-particle abrasion or a combination of both protocols. Such variations can be attributed to differences in experimental design, type of resin cement, thermocycling conditions, and zirconia composition, especially differences in yttria content, which is observed to affect bonding behavior.[14, 19]
In general, the results of this research are in line with the existing literature, as they prove that the surface modification is a key to optimal bond strength in zirconia restorations.[20, 21] The findings also indicate that the more complex surface treatments, especially those involving both mechanical and chemical processes, can offer better bonding efficacy and could increase the clinical efficacy of zirconia-based restorations in the long term.
This study had many limitations that should be taken into account when evaluating the findings. Since it is an in vitro study, the full simulation of the oral environment was not possible, especially salivary enzymes, masticatory forces, pH changes, and long-term thermal aging, which was not subjected to the thermal thermocycling program. The sample size was relatively small, statistically sufficient, but it included only standardized zirconia discs and not full-contour crowns, which might not be a complete replication of clinical conditions. Moreover, only one type of self-adhesive resin cement was tested, which limits the ability to generalize the results to other cement systems. The fact that operator-dependent procedures and surface treatment parameters, including pressure and time spent in airborne abrasion or laser settings, varied might also have affected the results, even though an effort was made to standardize them.
The binding strength of zirconia crowns treated with self-adhesive resin cements was found to be significantly impacted by surface modification techniques within the limitations of this experimental study. The highest bond strength was demonstrated by the tribochemical silica coating, which was followed by laser treatment and airborne particle abrasion, while untreated zirconia had the lowest bond strength. Surface treatment also positively contributed to the pattern of failure as it enhanced mixed and cohesive failures, which are indicative of enhanced interfacial bonding. These findings clearly show that in order to optimize the adhesive properties of zirconia restorations, appropriate surface modification is essential. This has the potential to improve zirconia restorations' lifespan and clinical performance in the context of restorative dentistry.
21. Lupu, I.-C., et al., Bonding Strategies for Zirconia Fixed Restorations: A Scoping Review of Surface Treatments, Cementation Protocols, and Long-Term Durability. Biomimetics, 2025. 10(9): p. 632.