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Article

Improving Zirconia–Resin Cement Bonding Through Laser Surface Texturing: A Comparative Study

by
Ji-Young Yoon
Department of Conservative Dentistry, Section of Dentistry, Seoul National University Bundang Hospital, Seongnam 13620, Republic of Korea
Prosthesis 2025, 7(1), 19; https://doi.org/10.3390/prosthesis7010019
Submission received: 10 January 2025 / Revised: 11 February 2025 / Accepted: 13 February 2025 / Published: 17 February 2025
(This article belongs to the Special Issue Advancements in Adhesion Techniques and Materials in Prosthodontics)

Abstract

:
Objectives: This study evaluates the effectiveness of laser surface texturing (LST) using a Surface Transition Machine (STM) on pre-sintered zirconia, comparing its impact on surface characteristics and shear bond strength (SBS) with resin cement to conventional sandblasting techniques. Methods: Zirconia specimens were treated with either STM or sandblasting, followed by surface analysis through scanning electron microscopy (SEM) and White Light Interferometry (WLI), wettability assessment via contact angle measurements, and SBS testing with resin cement and a 10-MDP-containing primer. Results: SEM and WLI revealed significant surface alterations in STM-treated zirconia, producing microscale textures. STM-treated surfaces exhibited significantly lower contact angles (28.4 ± 10.0°) compared to untreated (78.2 ± 8.0°) and sandblasted (79.2 ± 5.7°) surfaces, indicating enhanced wettability (p < 0.05). SBS was highest in the STM with primer group (46.3 ± 8.3 MPa) and STM without primer (43.4 ± 4.3 MPa), both of which significantly outperformed sandblasting with primer (30.06 ± 3.09 MPa) and sandblasting alone (9.8 ± 3.7 MPa) (p < 0.05). Conclusions: These findings suggest that STM-based LST is a more effective method for improving zirconia surface characteristics and adhesion in dental restorations, simplifying bonding procedures, and potentially offering better clinical outcomes than conventional sandblasting.

1. Introduction

Zirconia has emerged as a prominent material in modern dentistry, particularly for posterior restorations and implant-supported crowns, due to its exceptional mechanical properties [1]. With flexural strength exceeding 1000 MPa and high fracture toughness, zirconia exhibits remarkable resistance to masticatory forces, making it highly suitable for use in load-bearing areas of the oral cavity [2,3,4]. However, zirconia’s non-silica-based crystalline structure poses challenges in achieving reliable adhesion, especially in cases like short crowns, overlay restorations, and Maryland bridges, where mechanical retention is inherently limited [5,6,7]. This highlights the need for optimized bonding protocols to ensure clinical success in these challenging scenarios.
Surface treatment methods to enhance zirconia’s bond strength can be broadly categorized into mechanical and chemical approaches. Mechanical treatments, such as alumina sandblasting, increase surface roughness to improve micromechanical retention [8,9]. On the other hand, chemical treatments leverage 10-Methacryloyloxydecyl dihydrogen phosphate (10-MDP)-containing primers and cements, which have demonstrated efficacy in bonding to zirconia [10,11,12]. Notably, combining sandblasting with MDP application has shown synergistic improvements in shear bond strength (SBS) compared to either method alone [13,14].
Despite its efficacy, sandblasting has limitations, including the potential formation of microcracks that may compromise zirconia’s mechanical integrity and induce phase transformation from tetragonal to monoclinic, thereby altering its properties [15,16,17]. To mitigate these drawbacks, researchers have investigated alternative surface modification techniques, including laser surface texturing (LST) [18]. High-intensity lasers, such as neodymium-doped yttrium aluminum garnet (Nd:YAG) and neodymium-doped yttrium orthovanadate (Nd:YVO4), have been employed to create precise microstructures on zirconia, enhancing adhesion and surface wettability [19,20]. However, most studies focus on the SBS between zirconia and veneering porcelain, with limited exploration of adhesion to resin cement. Furthermore, the potential of laser irradiation applied before sintering remains largely unexplored.
The purpose of this study is to observe the surface changes in and characteristics of zirconia’s inner surface after applying LST before sintering and to measure the SBS with resin cement, comparing the results with other methods.

2. Materials and Methods

In this study, LST was performed using the Surface Transition Machine (STM) (STM-Z; Ceramic Technology Co., Ltd., Seoul, Republic of Korea), a fiber laser device. The zirconia blocks used in the experiments were TT One (Upcera, Zhenjiang, China). The chemical composition of these blocks primarily includes zirconium dioxide (ZrO2), hafnium dioxide (HfO2), and yttrium oxide (Y2O3), with these components collectively accounting for more than 96.5% of the total composition. The zirconia surface was irradiated using the STM-Z for one hour before sintering (Figure 1). Following laser treatment, the specimens were prepared for their respective experimental procedures.

2.1. Scanning Electron Microscopy (SEM) and White Light Interferometry (WLI)

The surfaces of untreated and STM-treated zirconia were analyzed using both SEM and WLI. SEM analysis was performed using a Verios 5 UC (Thermo Fisher Scientific, Waltham, MA, USA). Images were captured at three random areas at magnifications of 250×, 500×, 2000×, and 30,000× in the frontal view, and at 500× and 2000× in the lateral view. The VK-X3000 white light interferometer (KEYENCE, Osaka, Japan) was used to obtain three-dimensional images and precise height measurements of the zirconia surfaces, enabling the evaluation of surface roughness and texture.

2.2. Surface Contact Angle Measurement Experiment

The experimental groups are as follows:
Group 1: Untreated zirconia (G-UT).
Group 2: Zirconia treated with STM (G-STM).
Group 3: Zirconia treated with sandblasting (G-SB).
The sandblasting samples were prepared using a sandblasting machine (Basic Eco; Renfert, Hilzingen, Germany) by spraying alumina beads (110 µm particle size) at a pressure of 3 bar and an angle of 70 degrees, maintaining a distance of approximately 50 mm for 10 s. Contact angles were measured on the surfaces of 10 specimens in each group. The contact angle measurements were performed using a goniometer (Phoenix 300; SEO, Suwon, Republic of Korea) with deionized (DI) water as the test liquid. A droplet of DI water is deposited onto the surface using an automated dispenser integrated into the goniometer. The shape of the droplet is captured using a high-resolution camera, and the contact angle is calculated by analyzing the angle between the droplet’s tangent and the surface. The average contact angles for each group were analyzed using one-way ANOVA with a significance level set at p < 0.05 (SPSS 18; IBM, Armonk, NY, USA). Following the ANOVA, Tukey’s honestly significant difference (HSD) test was performed as a post hoc analysis to identify specific differences between group means.

2.3. SBS Test

As shown in Figure 2, zirconia specimens were fabricated in two shapes: square (15 mm × 15 mm × 10 mm, W × D × H) and cylindrical (4 mm diameter × 10 mm height). A total of 20 specimens per group were prepared, consisting of 10 square and 10 cylindrical specimens. The groups were differentiated based on the zirconia surface treatment methods and bonding conditions as follows:
Group 1: Sandblasting + resin cement (without primer application) (G-SB).
Group 2: Sandblasting + resin cement (with primer application) (G-SB+P).
Group 3: STM + resin cement (without primer application) (G-STM).
Group 4: STM + resin cement (with primer application) (G-STM+P).
The cylindrical specimens were adhered to the center of the square specimens using resin cement, following the respective conditions. For resin cement, Ivoclar Variolink Esthetic (Ivoclar Vivadent, Schaan, Liechtenstein) was used, and for the primer, Monobond Plus (Ivoclar Vivadent, Schaan, Liechtenstein), which contains 10-MDP, was applied. The resin cement was cured for 20 s on each of the four sides using a curing light (Noblesse.A; Max Dental Co., Ltd., Bucheon, Republic of Korea).
The universal testing machine (Quorum Technologies, Laughton, UK) was used, with a lower jig to secure the zirconia specimens (square and cylindrical disc specimens) and an upper jig to apply a load to the cylindrical specimens for SBS testing. The crosshead speed was set to 1 mm/min, and the applied load was measured in Newtons. The SBS (MPa) was calculated by dividing the measured load by the bonding area (mm2). The average SBS and standard deviation for each group were calculated, and the data were analyzed using one-way ANOVA with a significant level of p < 0.05. Tukey’s HSD test was performed as a post hoc analysis to identify specific differences between group means.

3. Results

3.1. SEM and WLI Analyses

As shown in Figure 3, SEM images reveal the surface characteristics of untreated zirconia and STM-treated zirconia. The heat generated by the laser beam induces localized melting and re-solidification of the zirconia, creating a textured surface with enhanced microtopography. As seen in the lateral view of ×500 magnification, the STM-treated zirconia surface demonstrates repetitive etching to a depth of approximately 50 μm, resulting in macroscale texturing. At ×30,000 magnification, the frontal view reveals holes approximately 2 μm in diameter, indicating the formation of micro-patterns. Importantly, the zirconia crystal structure remains unaltered, with surface etching as the sole modification observed. This surface texturing is also distinctly visible in the WLI images shown in Figure 4. The three-dimensional topographic map of the STM-treated surface shows enhanced roughness with increased step heights and surface irregularities.
Microscopic examination through SEM analysis demonstrates distinct morphological differences between the control and STM-processed zirconia specimens. Unlike the relatively smooth control, the STM treatment process induced distinct surface modifications on the zirconia substrate, producing characteristic macro- and microscale patterns along with textural features.
The WLI analysis reveals that zirconia surfaces subjected to STM treatment exhibit enhanced surface texture, characterized by distinct microstructural features and increased topographical complexity compared to untreated zirconia.

3.2. Surface Contact Angle Analyses

Figure 5 shows the contact angle measurement results for each group. The contact angle values were 78.2 ± 8.0°, 28.4 ± 10.0°, and 79.2 ± 5.7° for G-UT, G-STM, and G-SB, respectively. The G-STM exhibited a significantly lower contact angle compared to both the G-NT and the G-SB (p < 0.05), indicating that STM treatment significantly enhances the wettability of the zirconia surface. In contrast, the G-NT and the G-SB showed similar contact angles.
(a) Images of water droplet on untreated zirconia surface (Mean contact angle: 78.2 ± 8.0°); (b) Images of water droplet on STM-treated surface (Mean contact angle 28.4 ± 10.0°; (c) Images of water droplet on zirconia surface treated with sandblasting (Mean contact angle 79.2 ± 5.7°. Images of water droplet on STM-treated surface (Mean contact angle 28.4 ± 10.0°). Contact angles of the water droplet on the zirconia surface treated with STM were significantly lower, confirming its superior hydrophilicity.

3.3. SBS Test

Table 1 shows the mean SBS and standard deviation for each experimental group. The G-STM+P demonstrated the highest bond strength at 46.3 ± 8.3 MPa, while the G-SB exhibited the lowest at 9.8 ± 3.7 MPa (p < 0.05). The G-STM showed a high bond strength of 43.4 ± 4.3 MPa. Although the G-STM+P group had a higher mean (46.3 MPa) compared to the G-STM group (43.4 MPa), this difference was not statistically significant (p > 0.05). The large standard deviation (8.3 MPa) in the G-STM+P likely contributed to this lack of statistical significance. The G-SB+P, with a mean bond strength of 30.06 ± 3.09 MPa, showed a significant increase of approximately 20 MPa compared to the G-SB (p < 0.05). However, its bond strength remained significantly lower than that of both G-STM and G-STM+P (p < 0.05).

4. Discussion

The results of this study demonstrate the potential of LST using the STM as an effective method for enhancing the bond strength between zirconia and resin cement. The findings provide valuable insights into the surface characteristics, wettability, and bonding performance of STM-treated zirconia compared to conventional sandblasting techniques.
SEM and WLI analyses revealed notable changes in the surface topography of STM-treated zirconia. Laser-induced etching generated macro- and microscale textures, resulting in a more intricate surface microtopography compared to untreated zirconia. SEM lateral views showed etching depths of approximately 50 μm, significantly deeper than the 11 μm depth typically achieved by sandblasting with 105 μm particles [21]. Additionally, holes with a diameter of approximately 2 μm were observed between zirconia crystals, indicative of micro-patterning. This pronounced surface etching facilitates the formation of deeper resin tags and enhances macro- and micromechanical retention, potentially improving the bond strength of resin cements [21,22]. Contact angle measurements further confirmed the efficacy of STM treatment in modifying surface properties. The significantly lower contact angle observed in STM-treated zirconia compared to untreated and sandblasted samples indicates improved surface wettability. Enhanced wettability promotes better adhesive penetration into surface irregularities, leading to stronger micromechanical interlocking and superior bonding performance [23].
The SBS test is one of the most commonly used methods for evaluating the bonding performance of adhesive materials [24]. STM-treated groups, with and without 10-MDP primer, exhibited higher bond strengths than sandblasted groups. Notably, STM treatment alone outperformed sandblasting and 10-MDP application after sandblasting. Combining STM with 10-MDP primer resulted in the highest bond strength, but the incremental improvement was not statistically significant. This suggests that STM treatment alone may provide a surface highly conducive to bonding, potentially reducing the additional benefit of chemical primers.
Generally, the posterior region (molars) experiences high masticatory forces and repetitive loading, making an SBS of over 30 MPa essential for ensuring durability and functionality [25,26]. This value may be even more critical for short-length crown restorations, which require enhanced bond strength for stability. It is well-known that MDP forms a strong chemical bond with the hydroxyl groups on the zirconia surface, enhancing adhesion [25,26,27]. In our experiment, the G-SB+P showed an SBS of approximately 30.1 MPa. However, considering the standard deviation, there remains some uncertainty regarding its retention in the posterior region. In contrast, the STM-treated groups, regardless of primer application, demonstrated consistent SBS that exceeded 30 MPa. Therefore, STM treatment appears to be more suitable for applications requiring higher SBS.
Although STM treatment takes significantly longer—about 1 h compared to the mere 10 s required for conventional sandblasting—STM offers several advantages over traditional sandblasting. Unlike sandblasting, which requires materials such as aluminum oxide, STM utilizes a laser and does not require additional consumables, potentially reducing long-term operational costs. In terms of material properties, STM treatment not only provides higher bond strengths and improved wettability but also reduces the potential for damage to zirconia. Unlike sandblasting, which can induce microcracks and phase transformation, LST provides a more controlled and less invasive method for surface modification, preserving the mechanical integrity of zirconia [28,29]. In our study, we also confirmed that no changes occurred in the zirconia crystal structure before and after STM treatment, and no microcracks were observed. However, when STM is applied after zirconia sintering, it can lead to discoloration, with the material turning black. Research indicates that laser irradiation on sintered zirconia may cause microcracks and reduce oxygen content on the surface, which in turn alters the chemical structure of the material [30]. This chemical modification is a primary factor behind the observed discoloration. In contrast, laser treatment applied prior to sintering does not affect the mechanical or optical properties of zirconia. Therefore, the timing of STM application is crucial to preserving both the aesthetic and functional properties of zirconia.
These findings highlight the potential clinical benefits of STM treatment compared to conventional zirconia. The enhanced bond strength could contribute to more durable zirconia restorations, reducing the risk of debonding and improving long-term outcomes. Typically, zirconia restorations have not been preferred in clinical applications requiring strong adhesion, such as short clinical crowns, overlays, laminate veneers, and Maryland bridges, due to their lower bond strength. However, STM-treated zirconia demonstrates improved bonding capabilities while maintaining its inherent strength, suggesting its potential for use in previously underutilized clinical areas [31]. The high bonding performance of STM treatment, without the need for 10-MDP primers, suggests the potential to simplify bonding procedures, reducing the likelihood of errors and saving both time and resources in clinical practice. Furthermore, the reduced risk of structural damage during STM treatment could enhance the longevity and mechanical reliability of zirconia restorations.
While the results of this study are promising, several limitations must be addressed. First, the SBS in this study was measured by bonding resin cement to zirconia specimens, focusing on zirconia–zirconia interfaces rather than tooth–zirconia interfaces. For greater clinical relevance, future research should focus on bonding to tooth substrates and evaluating SBS under these conditions. Additionally, the comparison was limited to a narrow selection of surface treatments and primers. Expanding future studies to include STM treatment alongside a broader range of surface treatments would allow for a more comprehensive assessment of its relative effectiveness. Investigating bond strength stability after artificial aging, fatigue testing, or thermocycling would also provide valuable insights into the long-term performance of STM-treated zirconia. Moreover, optimizing STM parameters—such as laser power, duration, and pattern—remains crucial for achieving an optimal balance between effective surface modification and the preservation of zirconia’s mechanical properties.

5. Conclusions

LSM using the STM shows great promise as an alternative to conventional sandblasting for improving the bond strength between zirconia and resin cement. The technique’s ability to create favorable microtopography and enhance surface, without the potential drawbacks of sandblasting, makes it an attractive option for clinical application. However, further research is needed to fully understand its long-term performance and optimize its implementation in dental practice. Ex vivo studies on the bond strength of STM-treated zirconia restorations to extracted human teeth using resin cement are needed. Additionally, long-term retrospective studies on clinical cases applying this technique would provide insights into its efficacy and durability.

6. Patents

The STM-Z used in this study is a patented machine.
Patent Number: 10-2024-0198682
Patent Office: Korean Intellectual Property Office (KIPO)

Funding

This research was supported by Ceramic Technology Co., Ltd. (no formal grant number is applicable). The funding covered the provision of the STM device and experimental preparation expenses (including zirconia specimen preparation and experimental condition setup). The funder had no role in the data analysis, interpretation, or writing of the manuscript.

Institutional Review Board Statement

Not applicable.

Informed Consent Statement

Not applicable.

Data Availability Statement

The data supporting the reported results can be provided upon request to the corresponding author.

Acknowledgments

I would like to thank Ceramic Technology Co., Ltd. for their support in providing the STM device and funding the experimental preparation.

Conflicts of Interest

The author declares no conflicts of interest. The funders had no role in the design of the study; in the collection, analyses, or interpretation of data; in the writing of the manuscript; or in the decision to publish the results.

Abbreviations

The following abbreviations are used in this manuscript:
MDP10-Methacryloyloxydecyl dihydrogen phosphate
LSTLaser Surface Texturing
STMSurface Transition Machine
SBSShear bond strength

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Figure 1. The process of LSM using the STM-Z.
Figure 1. The process of LSM using the STM-Z.
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Figure 2. A schematic diagram of the bond-strength-testing method.
Figure 2. A schematic diagram of the bond-strength-testing method.
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Figure 3. SEM images of untreated zirconia and STM-treated zirconia.
Figure 3. SEM images of untreated zirconia and STM-treated zirconia.
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Figure 4. WLI images of zirconia surfaces of control and STM-treated.
Figure 4. WLI images of zirconia surfaces of control and STM-treated.
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Figure 5. Surface Contact Angle Measurements.
Figure 5. Surface Contact Angle Measurements.
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Table 1. Results of SBS test.
Table 1. Results of SBS test.
Treatment GroupNMean + Standard Deviation (MPa)
G-SB109.8 ± 3.7 a
G-SB+P1030.1 ± 3.1 b
G-STM1043.4 ± 4.3 c
G-STM+P1046.3 ± 8.3 c
Note. Both STM groups significantly outperformed sandblasting with primer (30.06 ± 3.09 MPa) and sandblasting alone (9.8 ± 3.7 MPa). Means followed by different superscript letters are significantly different (p < 0.05) based on Tukey’s HSD test.
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Yoon, J.-Y. Improving Zirconia–Resin Cement Bonding Through Laser Surface Texturing: A Comparative Study. Prosthesis 2025, 7, 19. https://doi.org/10.3390/prosthesis7010019

AMA Style

Yoon J-Y. Improving Zirconia–Resin Cement Bonding Through Laser Surface Texturing: A Comparative Study. Prosthesis. 2025; 7(1):19. https://doi.org/10.3390/prosthesis7010019

Chicago/Turabian Style

Yoon, Ji-Young. 2025. "Improving Zirconia–Resin Cement Bonding Through Laser Surface Texturing: A Comparative Study" Prosthesis 7, no. 1: 19. https://doi.org/10.3390/prosthesis7010019

APA Style

Yoon, J.-Y. (2025). Improving Zirconia–Resin Cement Bonding Through Laser Surface Texturing: A Comparative Study. Prosthesis, 7(1), 19. https://doi.org/10.3390/prosthesis7010019

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