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Article

Impact of Hydrofluoric Acid, Ytterbium Fiber Lasers, and Hydroxyapatite Nanoparticles on Surface Roughness and Bonding Strength of Resin Cement with Different Viscosities to Lithium Disilicate Glass Ceramic: SEM and EDX Analysis

by
Abdullah Aljamhan
and
Fahad Alkhudhairy
*
Restorative Dental Sciences Department, College of Dentistry, King Saud University, Riyadh 11451, Saudi Arabia
*
Author to whom correspondence should be addressed.
Crystals 2025, 15(7), 661; https://doi.org/10.3390/cryst15070661
Submission received: 14 June 2025 / Revised: 14 July 2025 / Accepted: 16 July 2025 / Published: 20 July 2025
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Abstract

This study looks at the effect of surface conditioners hydrofluoric acid (HFA), Ytterbium fibre laser (YFL), and Hydroxyapatite nanoparticles (HANPs) on the surface roughness (Ra) and shear bond strength (SBS) of different viscosity resin cements to lithium disilicate glass ceramic (LDC). A total of 78 IPS Emax discs were prepared and categorized into groups based on conditioning methods. Group 1 HFA–Silane (S), Group 2: YFL-S, and Group 3: HANPs-S. A scanning electron microscope (n = 1) and profilometer (n = 5) were used on each conditioned group for the assessment of surface topography and Ra. A total of 20 LDC discs for each conditioned group were subsequently categorized into two subgroups based on the application of high- and low-viscosity dual-cured resin cement. SBS and failure mode were assessed. ANOVA and post hoc Tukey tests were employed to identify significant differences in Ra and SBS among different groups. LDC conditioned with HFA-S, HANPs-S, and YFL-S demonstrated comparable Ra scores (p > 0.05). Also, irrespective of the type of conditioning regime, the use of low-viscosity cement improves bond values when bonded to the LDC. LDC treated with YFL-S and HANPs-S can serve as an effective substitute for HFA-S in enhancing the Ra and surface characteristics of LDC. The low-viscosity resin cement demonstrated superior performance by achieving greater bond strength.

1. Introduction

CAD/CAM technology, which is increasingly gaining recognition in the field of dentistry, greatly accelerates the creation of high-quality, aesthetically pleasing, indirect restorations [1]. Lithium disilicate glass ceramic (LDC) stands out in the field of ceramics, particularly in aesthetic dentistry, due to its remarkable optical and mechanical characteristics as well as its impressive longevity [2]. However, it is difficult to achieve satisfactory shear bond strength (SBS) at the LDC–cement interface [3]. An inadequate bond between the substrates can significantly reduce the load-bearing capacity of the indirect prosthesis when exposed to fatigue, eventually leading to fracture [4]. Therefore, the main goal of LDC surface pretreatments is to improve the bonding of hydrophobic resin cement by creating micro-roughness (Ra). The effectiveness of LDC restorations ultimately relies on achieving this ideal surface preparation to form strong resin–ceramic interfaces capable of enduring the challenging conditions of the oral environment.
In the traditional process, glass ceramics are first etched using hydrofluoric acid (HFA) and then treated with a silane (S) coupling agent [5]. The traditional HFA–silane method is considered the benchmark for bonding lithium disilicate as it effectively combines both mechanical and chemical adhesion aspects in a complementary way [6]. Although HFA is effective in strengthening the bond between glass ceramics and luting cement, it poses toxic and hazardous risks, potentially causing both immediate and long-term health issues [7,8]. Consequently, it is advisable to seek safer alternatives to mitigate these risks.
The use of lasers has attracted considerable interest in dentistry [2,9]. Nowadays, a new laser called a pulsed Ytterbium fibre laser (YFL) has attracted scientists and scholars. It functions at a wavelength of 1030–1070 nm, producing pulses that exceed a peak power of 80 W and last for microseconds. It has potential applications across diverse fields, including gynecology, abdominal surgery, cardiovascular procedures, and dental care. Prior research has demonstrated that YFL offers greater benefits compared to other laser technologies when it comes to roughening zirconia [10,11,12]. Similarly, significant advancements in nanotechnology have revealed practical applications for Hydroxyapatite nanoparticles (HANPs) in dentistry [13,14]. These nanoparticles are known for their bioactive and biocompatible properties [15]. Additionally, their morphology closely resembles the apatite crystals present in tooth enamel, sharing similar crystal structure [16]. A study conducted in vitro by Alkhudhairy and colleagues showed that HANPs enhance the surface roughness (Ra) and adhesive strength of zirconia [17]. However, there is a lack of sufficient evidence concerning the impact of YFL and HANPs on the Ra score and the bond strength of LDC when used with luting cement, highlighting the necessity for additional research.
In addition to surface pretreatment, an essential factor in securing the bond of indirect restorations to dentin is selecting cement with appropriate consistency and viscosity, as emphasized by Marshall and his colleagues [18]. It is advised that the luting agent should thoroughly infiltrate the imperfections formed during surface conditioning to effectively seal the microcracks [19]. This action is vital in reinforcing the restorative material and enhancing adhesion strength [20]. Nonetheless, there is a scarcity of information on which viscosity, whether high or low, resin cement is best suited for the SBS of different ceramics, indicating a need for further investigation.
Drawing from the existing indexed literature, this research aims to explore how resin cement with different viscosities affects the SBS of LDC discs that have been conditioned using various techniques (HFA, YFL, and HANPs). The null hypothesis suggests that there will be no significant differences in Ra and surface topography when YFL and HANPs are applied as preconditioning methods compared to HFA (Control). Additionally, it is hypothesized that the SBS of adhesive cement, regardless of whether it is high or low viscosity, will remain consistent across different surface conditioning methods.

2. Materials and Methods

2.1. Sample Preparation and Sample Size Calculation

Using CAD/CAM technology, seventy-eight IPS Emax (Ivoclar Vivadent AG, Schaan, Liechtenstein) discs were manufactured, each measuring 2 mm in height and 5 mm in diameter. This was achieved with a cutting machine (Miter Saw, Atech Solutions, Istanbul, Turkey) that featured a diamond blade and maintained a consistent water-cooling system. The resulting slices underwent polishing through a series of silicon carbide papers (#600, #800, #1200) (Adinath Equipment Private Limited, Ahmedabad, Gujarat, India) (Figure 1A).
Based on the type of conditioning protocols, the samples were categorized into three groups (n = 26) [3]. Samples in each group were calculated by using the WHO sample size calculator. The following were the calculations: confidence level = 95%, absolute precision = 5%, population mean = 1283.618%, population standard deviation (SD) = 0.021, sample size: 26 cases in each group [3,21].

2.1.1. Group 1: HFA-S (Control)

In this cohort, the surface of the specimens was subjected to treatment with a 9.6% concentration of HFA (Pulpdent Corporation, Chicago, IL, USA) for 60 s. The samples were rinsed off, followed by air drying. Silane (Daken Chemical, Hong Kong, China) was applied to the etched surface using an applicator and permitted to dry for 5 min [2].

2.1.2. Group 2: YFL-S

Specimens in this group were prepared using a YFL (Robart Laser, İstanbul, Turkiye). The laser was set to operate at a wavelength of 1070 nm, with an output power of 20 W, a repetition rate of 20 kHz, and a pulse duration consistently maintained at 100 ns. The laser’s lens had a focal length of 160 mm, resulting in a laser beam spot size of 80 μm. The laser beam was applied in a non-contact manner from a distance of 17.8 mm. Subsequently, S was applied on the irradiated surface similar to Group 1 [22,23].

2.1.3. Group 3: HANPs-S

The cohort of LDC in this group underwent a pretreatment process utilizing HANPs through a thermal protocol. A slurry solution was formed by combining 10 g of HANP powder (with a particle size of less than 100 nm) (Merck, Berlin, Germany) and 50 cc of distilled water. Following this, 1g of polyvinyl alcohol (Merck, Germany) was added as a binder for the suspension, and the resulting mixture was heated on a magnetic stirrer at a temperature of 100 °C for 60 min while ensuring a stirring speed of 1000 rpm to achieve uniform consistency [24]. Ultimately, LDC discs were placed into this slurry at a 45° angle for a total time of 1 min. Subsequently, the S agent was brushed identically as it was in Groups 1 and 2.

2.2. Assessment of Ra

Ra analysis was conducted on five LDC discs from each conditioning group using a profilometer (Mitutoyo Corporation, Tokyo, Japan). The analyzer tip was traversed 1.25 mm vertically to the long axis of the discs at intervals of 1 mm in three different locations at a speed of 1 mm/s. The mean Ra was calculated from three Ra values obtained [24,25]

2.3. Topographic Changes in LDC Discs via SEM

The energy dispersive X-ray analysis (EDX) and topography of LDC were examined utilizing a scanning electron microscopy (SEM) (JSM-6 6400, JEOL, Tokyo, Japan). The LDC samples were coated with gold via a sputtering technique (Polaron Range SC 7620, Quorum Technology, Newhaven, UK) and subjected to evaluation under an SEM at different magnifications to ascertain modifications in surface topography (n = 1) [17].

2.4. Resin Cement Bonding

From each conditioning group, twenty discs were categorized into subgroups based on the high-viscosity (HV) (A) and low-viscosity (LV) (B) dual-cure resin cement (Variolink N, Ivoclar, IL, USA). A 2 mm-thick resin cement was built on the LDC via a Tygon tube and cured using a light-emitting diode (LED) (LED Light Curing Device, Coxo Medical, Beijing, China). The exposure to light was systematically administered five times (0°, 90°, 180°, 270°, and vertically positioned on top), with each exposure having a duration of 20 s. All bonded samples were incubated (Incubator, model PL-455G, PecoPooya Electronic Co., Lahore, Pakistan) at a controlled temperature of 37 °C for 24 h [24,26].

2.5. Thermocycling

In order to simulate the oral conditions, the prepared samples were exposed to artificial ageing using a thermocycler (TC-32 Mini Thermal Cycler, Merck, Germany) for a total of 10,000 cycles. Each cycle constitutes a sample’s immersion in two water baths maintained at a temperature between 5 °C and 60 °C. The submergence time in each bath was 30 s, with a transfer time of 5 s [27].

2.6. SBS and Failure Mode Analysis

The SBS was assessed using a universal testing machine (MBIO, BioPDI, Sao Carlos, Brazil) at a cross-head velocity of 1 mm/min until the occurrence of debonding (cement from LDC disc). The maximum load required to fail the bond was recorded in Megapascals (MPa). To determine the failure mode of each specimen, the surfaces of all specimens were subjected to analysis using a stereomicroscope (HIROX, KH-7700, Digital microscope system, Tokyo, Japan) at a magnification of ×50 following debonding. The failure modes were classified as adhesive, cohesive, or combined [28,29]. Failure between the adhesive and substrate was identified as adhesive failure. Failure within the material itself was categorized as cohesive. A blend of both cohesive and adhesive was categorized as a combination failure.

2.7. Statistical Analysis

Data evaluation was conducted utilizing SPSS 21.0 software (IBM Statistics, SPSS, Chicago, IL, USA). One-way analysis of variance (ANOVA) and post hoc Tukey tests were employed to identify significant differences in Ra and SBS (p ≤ 0.05).

3. Results

3.1. SEM and EDS Assessment

Figure 1B illustrates the line EDS of elements within the LDC disc. Figure 2A depicts an LDC disc treated with HFA–Silane, showing an area where the matrix remains intact, alongside a region where the matrix has dissolved, making the glass more visible. Figure 2B presents an LDC disc conditioned with YFL–Silane, where the matrix is uniformly dissolved, highlighting the glass. Cracks are visible on the surface, attributed to the laser’s thermal effect. The LDC treated with HANPs–Silane exhibits a uniform loss of matrix, with the glass structure prominently displayed in Figure 2C.

3.2. Ra Analysis

The Ra scores of the LDC discs following their conditioning process are outlined in Figure 3. The specimens belonging to Group 3 (HANPs–Silane) achieved the most elevated Ra scores (1169.13 ± 0.43 µm). Conversely, the LDC discs in Group 2 (YFL–Silane) displayed the lowest Ra value (1130.11 ± 0.55 µm). The results obtained from the intergroup comparison analysis revealed that the discs treated in Group 1 via HFA–Silane (1152.32 ± 0.46 µm), Group 2, and Group 3 showed no differences in Ra scores (p > 0.05).

3.3. SBS Analysis

The SBS of LDC bonded to different viscosity resin cements after pretreating with different conditioning agents is presented in Figure 4. The samples from Group 3A (HANPs–Silane + LV cement) exhibited the maximum SBS values (11.54 ± 0.22 MPa). Conversely, Group 2B (YFL–Silane + HV cement) demonstrated the lowest bond strength (9.19 ± 0.22 MPa). A comparative analysis of SBS across the various tested groups indicated that Group 1A (HFA–Silane + LV cement) (11.51 ± 0.13 MPa), Group 2A (YFL–Silane + LV cement) (11.46 ± 0.19 MPa), and Group 3A displayed comparable bond strengths, i.e., no significant difference (p > 0.05).
Similarly, Group 1B (HFA+ HV cement) (9.16 ± 0.15 MPa), Group 2B (YFL–Silane + HV cement) (9.19 ± 0.22 MPa), and Group 3B (HANPs–Silane + HV cement) (9.21 ± 0.31 MPa) also demonstrated no statistically significant difference in the bond integrity outcomes (p > 0.05).
Based on the results of the present study, it can be inferred that LDC conditioned with HFA–Silane, HANPs–Silane, and YFL–Silane demonstrated comparable Ra scores (p > 0.05). Also, irrespective of the type of conditioning regime, the use of LV cement improved bond values when bonded to the LDC.

3.4. Fracture Pattern Analysis

Failure mode analysis is presented in Figure 5. All the investigated groups bonded with LV resin cement presented cohesive failures predominantly, whereas the groups with HV resin cement displayed the admixed fractures the most.

4. Discussion

The present analysis was based on the prediction that there would be no notable difference in Ra and surface topography when YFL and HANPs were used as surface conditioners on LDC discs compared to the group treated with HFA. Similarly, it was also anticipated that the SBS of adhesive cement with varying viscosities (high and low) would remain comparable, regardless of the surface conditioning regime used. The results of this investigation suggested that the Ra values of LDC discs pretreated with YFL and HANPs are analogous to those of HFA-conditioned discs, thereby supporting the primary hypothesis. Nonetheless, it is crucial to acknowledge that the secondary stated hypothesis was dismissed as LDC conditioned with YFL, HANPs, and HFA and bonded to lower-viscosity resin cement exhibited superior bond performance compared to its higher-viscosity counterpart.
Attia and their colleagues have determined that the minimum acceptable range for clinical bonding in restorative dentistry is between 10 and 13 MPa [30]. The current research indicated that discs treated with HANPs and YFL exhibited Ra values and adhesion strengths similar to those of the control group. HFA is considered the standard protocol for conditioning various ceramics. Its use results in the breakdown of the matrix network, revealing the underlying crystalline structures and forming a three-dimensional porous interface that enhances the surface area for resin cement retention through micromechanical interlocking [31]. Furthermore, the interaction between the acid and the glass matrix can be explained by the formation of hexafluorosilicates, which sheds light on the bond strength results [32]. In contrast, silane boosts adhesion by enabling interaction between the ceramic’s inorganic components and the organic elements of the bonding agent applied to the ceramic surface, leading to an increase in the cement surface energy and the creation of microscopic connections [33].
Various coating techniques exist to harness the benefits of HANPs [34,35]. However, this study opted for the thermal coating method because it effectively alters the surface properties of zirconia ceramics, as shown in laboratory tests by Alkhudhairy and colleagues [36]. Their findings indicated that HANPs enhance the SBS by increasing Ra, achieved through a thin, uniform coating that is robust enough to facilitate the mechanical interlocking of the cement [36]. The application of HANPs to conditioned LDCs is consistent with the ongoing progress in biomaterials, which aims to achieve improved mechanical properties, biocompatibility, and bioactivity. These improvements can result in more effective and durable outcomes, thereby supporting a wider array of clinical applications [37].
YFL, on the other hand, also exhibited comparable scores of Ra and SBS relative to the control group. This observation aligns with the results from laboratory analyses conducted by Demetoğlu and colleagues [11]. They reported that the bond strength of resin cement to LDC was found to be similar, irrespective of pretreatment with YFL or HFA. This phenomenon can be elucidated by the ability of YFL to enhance the Ra by selectively ablating and removing material from the surface, resulting in micro-irregularities. Conversely, Fornaini et al. articulated in their ex vivo study that zirconia pretreated with YFL displayed comparable outcomes to those of the untreated control [23]. Variations in results can be linked to differing laser settings, such as frequency and power, as well as factors like duration, distance, and power density [38]. The choice between HF and YFL for pretreatment may depend on specific clinical requirements, practitioner preference, and cost considerations. Each method has its distinct advantages in terms of practicality and clinical outcomes. Therefore, whilst HF remains a gold standard due to its established efficacy, lasers present a promising alternative by ensuring safety, reducing handling complexity, and minimizing invasive pretreatment. However, further studies are necessary to confirm the conclusions of this current analysis.
When examining the bond strength concerning the viscosity of resin cement, it was observed that the SBS was consistently lower in high-viscosity resin cement compared to low-viscosity cement across all conditioning groups. This can be attributed to the higher filler content and reduced monomer concentration in these types of cement [24,26], leading to bond swelling and eventual breakdown due to the frequent and sudden temperature changes during the thermal ageing process, which simulates conditions in the oral cavity [39]. The researchers of this study strongly advocate for assessing bond strength values for both low- and high-viscosity cement in real-life in vivo settings.
Regarding the failure pattern, it was observed that the groups that exhibited higher bond integrity scores predominantly revealed a cohesive type of failure mode. The phrase “cohesive failure” refers to the fracture or breakage occurring within a single material rather than at the interface where two distinct materials meet. The emergence of this particular type of debonding could be attributed to inherent deficiencies or limitations present within the material’s composition [40,41].
The current study exhibited certain limitations. Firstly, it was conducted under highly controlled in vitro conditions, which do not accurately represent clinical settings; thus, the findings should be generalized with caution. Additionally, the study did not explore various laser parameters, HF acid concentrations, or application durations. Furthermore, only one sample of LDC was used to assess surface topography after different conditioning methods. To eliminate bias or chance, more samples should have been evaluated using an SEM. The effects of different pretreatment methods on various mechanical tests, such as tensile strength, flexural strength, and colour change, requires further investigation. Employing Atomic Force Microscopy (AFM) could have offered more insight into how different conditioners affect the surface properties of the LDC.

5. Conclusions

Lithium disilicate ceramics treated with Ytterbium fibre laser–Silane and Hydroxynanoparticles–Silane can serve as an effective substitute for hydrofluoric acid in enhancing the surface roughness and topography of Lithium disilicate ceramics. The low-viscosity resin cement demonstrated superior performance by achieving greater bond strength.

Author Contributions

Conceptualization, F.A. and A.A.; methodology, F.A. and A.A.; software, F.A. and A.A.; validation, F.A. and A.A.; formal analysis, F.A. and A.A.; investigation, F.A. and A.A.; resources, F.A. and A.A.; data curation, F.A.; writing—original draft preparation, F.A. and A.A.; writing—review and editing, A.A.; visualization, F.A.; supervision, F.A.; project administration, F.A.; funding acquisition, A.A. and F.A. All authors have read and agreed to the published version of the manuscript.

Funding

Ongoing Research Funding Program (ORF-2025-815) at King Saud University, Riyadh, Saudi Arabia.

Institutional Review Board Statement

The study was approved by the ethical board of King Saud University under IRB # FC-431-25.

Data Availability Statement

The data can be made available on request to the authors.

Acknowledgments

The authors gratefully acknowledge the Ongoing Research Funding Program (ORF-2025-815) at King Saud University, Riyadh, Saudi Arabia, for their financial support.

Conflicts of Interest

The authors declare no conflicts of interest.

References

  1. Ahmed, K.E. We’re Going Digital: The Current State of CAD/CAM Dentistry in Prosthodontics. Prim. Dent. J. 2018, 7, 30–35. [Google Scholar] [CrossRef] [PubMed]
  2. Maawadh, A.M.; Almohareb, T.; Al-Hamdan, R.S.; Al Deeb, M.; Naseem, M.; Alhenaki, A.M.; Vohra, F.; Abduljabbar, T. Repair Strength and Surface Topography of Lithium Disilicate and Hybrid Resin Ceramics with LLLT and Photodynamic Therapy in Comparison to Hydrofluoric Acid. J. Appl. Biomater. Funct. Mater. 2020, 18, 2280800020966938. [Google Scholar] [CrossRef] [PubMed]
  3. Alkhudhairy, F.; Naseem, M.; Ahmad, Z.H.; Alnooh, A.N.; Vohra, F. Efficacy of Phototherapy with Different Conventional Surface Treatments on Adhesive Quality of Lithium Disilicate Ceramics. Photodiagnosis Photodyn. Ther. 2019, 25, 292–295. [Google Scholar] [CrossRef] [PubMed]
  4. Chiapinotto, G.F.; da Rosa, L.S.; Scotti, N.; Kleverlaan, C.J.; Valandro, L.F.; Pereira, G.K.R. Does Adhesive Luting Promote Improved Fatigue Performance of Lithium Disilicate Simplified Crowns? J. Mech. Behav. Biomed. Mater. 2022, 134, 105373. [Google Scholar] [CrossRef] [PubMed]
  5. Albaker, A.M.; Al Deeb, L.; Alhenaki, A.M.; Aldeeb, M.; Al Ahdal, K.; Abduljabbar, T.; Vohra, F. Bonding Integrity and Compressive Strength of Re-Bonded, Surface Conditioned and Er Cr YSGG Laser Treated Lithium Disilicate Ceramics. J. Appl. Biomater. Funct. Mater. 2020, 18, 2280800020910954. [Google Scholar] [CrossRef] [PubMed]
  6. Basunbul, G.I.; Alzahrani, K.M.; Almutairi, B.; Alsunbul, H.; Abduljabbar, T. The Impact of Riboflavin, Nd: YAG Laser, and Ceramic Primer Pretreatment on Surface Roughness, Bond Failure, and Adhesive Strength of Resin Composite to Lithium Disilicate Ceramics: A Scanning Electron Microscopy (SEM) Analysis. J. Biomater. Tissue Eng. 2024, 13, 882–887. [Google Scholar] [CrossRef]
  7. Kim, K.J.; Park, Y.T.; Yoo, J.H.; Park, T.H. Hydrofluoric Acid Burns. Exog. Dermatol. 2004, 3, 12–18. [Google Scholar] [CrossRef]
  8. Özcan, M.; Allahbeickaraghi, A.; Dündar, M. Possible Hazardous Effects of Hydrofluoric Acid and Recommendations for Treatment Approach: A Review. Clin. Oral Investig. 2012, 16, 15–23. [Google Scholar] [CrossRef] [PubMed]
  9. Alkhudhairy, F.; AlKheraif, A.; Bin-Shuwaish, M.; Al-Johany, S.; Naseem, M.; Vohra, F. Effect of Er,Cr:YSGG Laser and Ascorbic Acid on the Bond Strength and Microleakage of Bleached Enamel Surface. Photomed. Laser Surg. 2018, 36, 431–438. [Google Scholar] [CrossRef] [PubMed]
  10. Maziero Volpato, C.A.; Carvalho, O.; Özcan, M.; Fredel, M.C.; Silva, F.S. Effect of Laser Irradiation on the Adhesion of Resin-Based Materials to Zirconia: A Systematic Review and Meta-Analysis. J. Adhes. Sci. Technol. 2021, 35, 1035–1056. [Google Scholar] [CrossRef]
  11. Alkan Demetoğlu, G.; Talay Çevlïk, E. Evaluation of the Effect of Etching with Ytterbium Fiber Laser on the Bond Strength, Color Stability, and Fracture Analysis of Lithium Disilicate Ceramics to Bovine Teeth: An in Vitro Study. BMC Oral Health 2025, 25, 607. [Google Scholar] [CrossRef] [PubMed]
  12. Toyoda, K.; Taniguchi, Y.; Nakamura, K.; Isshi, K.; Kakura, K.; Ikeda, H.; Shimizu, H.; Kido, H.; Kawaguchi, T. Effects of Ytterbium Laser Surface Treatment on the Bonding of Two Resin Cements to Zirconia. Dent. Mater. J. 2022, 41, 45–53. [Google Scholar] [CrossRef] [PubMed]
  13. Al-Hamdan, R.S.; Almutairi, B.; Kattan, H.F.; Alsuwailem, N.A.; Farooq, I.; Vohra, F.; Abduljabbar, T. Influence of Hydroxyapatite Nanospheres in Dentin Adhesive on the Dentin Bond Integrity and Degree of Conversion: A Scanning Electron Microscopy (SEM), Raman, Fourier Transform-Infrared (FTIR), and Microtensile Study. Polymers 2020, 12, 2948. [Google Scholar] [CrossRef] [PubMed]
  14. Yadav, R.; Meena, A.; Patnaik, A. Tribological Behavior of Zinc Oxide-hydroxyapatite Particulates Filled Dental Restorative Composite Materials. Polym. Compos. 2022, 43, 3029–3040. [Google Scholar] [CrossRef]
  15. Huang, S.; Gao, S.; Cheng, L.; Yu, H. Remineralization Potential of Nano-Hydroxyapatite on Initial Enamel Lesions: An in Vitro Study. Caries Res. 2011, 45, 460–468. [Google Scholar] [CrossRef] [PubMed]
  16. Butera, A.; Gallo, S.; Pascadopoli, M.; Montasser, M.A.; Abd El Latief, M.H.; Modica, G.G.; Scribante, A. Home Oral Care with Biomimetic Hydroxyapatite vs. Conventional Fluoridated Toothpaste for the Remineralization and Desensitizing of White Spot Lesions: Randomized Clinical Trial. Int. J. Environ. Res. Public Health 2022, 19, 8676. [Google Scholar] [CrossRef] [PubMed]
  17. Alkhudhairy, F.; Shono, N.N. Surface Roughness and Shear Bond Strength of Y-TZP Treated via Tri-Biochemical Silica Coating, Femtosecond Laser, and Nano-Hydroxyapatite: An SEM Assessment. J. Ceram. Sci. Technol. 2025, 16, 45–50. [Google Scholar] [CrossRef]
  18. Marshall, S.J.; Bayne, S.C.; Baier, R.; Tomsia, A.P.; Marshall, G.W. A Review of Adhesion Science. Dent. Mater. 2010, 26, e11–e16. [Google Scholar] [CrossRef] [PubMed]
  19. Barbon, F.J.; Moraes, R.R.; Isolan, C.P.; Spazzin, A.O.; Boscato, N. Influence of Inorganic Filler Content of Resin Luting Agents and Use of Adhesive on the Performance of Bonded Ceramic. J. Prosthet. Dent. 2019, 122, 566.e1–566.e11. [Google Scholar] [CrossRef] [PubMed]
  20. Beketova, A.; Tzanakakis, E.G.C.; Vouvoudi, E.; Anastasiadis, K.; Rigos, A.E.; Pandoleon, P.; Bikiaris, D.; Tzoutzas, I.G.; Kontonasaki, E. Zirconia Nanoparticles as Reinforcing Agents for Contemporary Dental Luting Cements: Physicochemical Properties and Shear Bond Strength to Monolithic Zirconia. Int. J. Mol. Sci. 2023, 24, 2067. [Google Scholar] [CrossRef] [PubMed]
  21. Alkhudhairy, F.; AlFawaz, Y.F. Pretreatment of Hybrid Ceramics Using Ho: YAG, Low-Level Laser Therapy Activated Malachite Green, and Non-Thermal Plasma on Surface Roughness, Bond Strength, and Color Change, SEM and EDX Analysis. Ceramics 2024, 7, 944–957. [Google Scholar] [CrossRef]
  22. Mutluay Unal, S.; Ozkir, S.E.; Seyfioglu Polat, Z.; Guven, S.; Asutay, H. The Effect of Ytterbium-Doped Fiber Laser with Different Parameters on Physical Properties of Zirconia Surface. Photomed. Laser Surg. 2017, 35, 157–163. [Google Scholar] [CrossRef] [PubMed]
  23. Fornaini, C.; Poli, F.; Merigo, E.; Lutey, A.; Cucinotta, A.; Chevalier, M.; Mckee, S.; Brulat, N.; Rocca, J.P.; Trevisi, G. Nanosecond Pulsed Fiber Laser Irradiation for Enhanced Zirconia Crown Adhesion: Morphological, Chemical, Thermal and Mechanical Analysis. J. Photochem. Photobiol. B Biol. 2021, 219, 112189. [Google Scholar] [CrossRef] [PubMed]
  24. Almohareb, T.; Maawadh, A.; AlDeeb, L.; Alahdal, K.; Alshamrani, A.S.; Alrahlah, A. Influence of High- and Low-Viscosity Resin Cement and Artificial Aging on Bond Integrity and Surface Roughness of Lithium Disilicate Ceramics Pretreated with Ho:YAG Laser and Nano-Hydroxyapatite Coatings. J. Ceram. Sci. Technol. 2025, 16, 29–36. [Google Scholar] [CrossRef]
  25. Cho, J.H.; Kim, S.J.; Shim, J.S.; Lee, K.W. Effect of Zirconia Surface Treatment Using Nitric Acid-Hydrofluoric Acid on the Shear Bond Strengths of Resin Cements. J. Adv. Prosthodont. 2017, 9, 77–84. [Google Scholar] [CrossRef] [PubMed]
  26. Dapieve, K.S.; Pereira, G.K.R.; Venturini, A.B.; Daudt, N.; Valcanaia, A.; Bottino, M.C.; Valandro, L.F. Do Resin Cement Viscosity and Ceramic Surface Etching Influence the Fatigue Performance of Bonded Lithium Disilicate Glass-Ceramic Crowns? Dent. Mater. 2022, 38, e59–e67. [Google Scholar] [CrossRef] [PubMed]
  27. Guarda, G.B.; Correr, A.B.; Gonçalves, L.S.; Costa, A.R.; Borges, G.A.; Sinhoreti, M.A.C.; Correr-Sobrinho, L. Effects of Surface Treatments, Thermocycling, and Cyclic Loading on the Bond Strength of a Resin Cement Bonded to a Lithium Disilicate Glass Ceramic. Oper. Dent. 2013, 38, 208–217. [Google Scholar] [CrossRef] [PubMed]
  28. Alrahlah, A.; Awad, M.M.; Vohra, F.; Al-Mudahi, A.; Al jeaidi, Z.A.; Elsharawy, M. Effect of Self Etching Ceramic Primer and Universal Adhesive on Bond Strength of Lithium Disilicate Ceramic. J. Adhes. Sci. Technol. 2017, 31, 2611–2619. [Google Scholar] [CrossRef]
  29. Vohra, F.; Labban, N.; Al-Hussaini, A.; Al-Jarboua, M.; Zawawi, R.; Alrahlah, A.; Naseem, M. Influence of Er;Cr:YSGG Laser on Shear Bond Strength and Color Stability of Lithium Disilicate Ceramics: An in Vitro Study. Photobiomodulation Photomed. Laser Surg. 2019, 37, 483–488. [Google Scholar] [CrossRef] [PubMed]
  30. Attia, A. Bond Strength of Three Luting Agents to Zirconia Ceramic—Influence of Surface Treatment and Thermocycling. J. Appl. Oral Sci. 2011, 19, 388–395. [Google Scholar] [CrossRef] [PubMed]
  31. Kukiattrakoon, B.; Thammasitboon, K. The Effect of Different Etching Times of Acidulated Phosphate Fluoride Gel on the Shear Bond Strength of High-Leucite Ceramics Bonded to Composite Resin. J. Prosthet. Dent. 2007, 98, 17–23. [Google Scholar] [CrossRef] [PubMed]
  32. Strasser, T.; Preis, V.; Behr, M.; Rosentritt, M. Roughness, Surface Energy, and Superficial Damages of CAD/CAM Materials after Surface Treatment. Clin. Oral Investig. 2018, 22, 2787–2797. [Google Scholar] [CrossRef] [PubMed]
  33. Yavuz, T.; Eraslan, O. The Effect of Silane Applied to Glass Ceramics on Surface Structure and Bonding Strength at Different Temperatures. J. Adv. Prosthodont. 2016, 8, 75–84. [Google Scholar] [CrossRef] [PubMed]
  34. Simões, A.C.; Miranda, J.S.; Souza, R.O.d.A.e.; Kimpara, E.T.; Leite, F.P.P. Bond and Topography Evaluation of a Y-TZP Ceramic with a Superficial Low-Fusing Porcelain Glass Layer After Different Hydrofluoric Acid Etching Protocols. Rev. Odontol. UNESP 2018, 47, 348–353. [Google Scholar] [CrossRef]
  35. Siwen, L.; Shishi, L.; Yanhong, W.; Hongmei, M. Effects of Different Surface Modifications on Micro-Structure and Adhesion of Zirconia Ceramic: An In Vitro Study. Hua Xi Kou Qiang Yi Xue Za Zhi 2017, 35, 43–50. [Google Scholar] [CrossRef] [PubMed]
  36. Alkhudhairy, F.; Shono, N.N. An Investigation of Y-TZP Surface Characteristics and Adhesive Properties Following Treatment with Tri-Biochemical Silica Coating, Femtosecond Laser, and Nano-Hydroxyapatite: A Scanning Electron Microscopy Evaluation. Pakistan J. Med. Sci. 2025, 41, 758–762. [Google Scholar] [CrossRef] [PubMed]
  37. Upadhyay, A.; Pradhan, L.; Yenurkar, D.; Kumar, K.; Mukherjee, S. Advancement in Ceramic Biomaterials for Dental Implants. Int. J. Appl. Ceram. Technol. 2024, 21, 2796–2817. [Google Scholar] [CrossRef]
  38. Aljamhan, A.S.; Alrefeai, M.H.; Alhabdan, A.; Alhusseini, S.A.; Farooq, I.; Vohra, F.; Naseem, M.; Alkhudhairy, F. Influence of ER-CR-YSGG Laser and Photodynamic Therapy on the Dentin Bond Integrity of Nano-Hydroxyapatite Containing Resin Dentin Adhesive: SEM-EDX, Micro-Raman, Micro-Tensile, and FTIR Evaluation. Polymers 2021, 13, 1903. [Google Scholar] [CrossRef] [PubMed]
  39. Dapieve, K.S.; Velho, H.C.; da Rosa, L.S.; Pivetta, J.P.; Maidana, F.C.; Venturini, A.B.; Kleverlaan, C.J.; Pereira, G.K.R.; Valandro, L.F. Ceramic Surface Conditioning, Resin Cement Viscosity, and Aging Relationships Affect the Load-Bearing Capacity Under Fatigue of Bonded Glass-Ceramics. J. Mech. Behav. Biomed. Mater. 2023, 139, 105667. [Google Scholar] [CrossRef] [PubMed]
  40. Alnazeh, A.A. Pretreatment of Enamel with Riboflavin Activated Photodynamic Therapy and Er, Cr: YSGG Laser for Bonding of Orthodontic Bracket with Adhesive Modified with Cerium Oxide Nanoparticles. Photodiagnosis Photodyn. Ther. 2024, 49, 104285. [Google Scholar] [CrossRef] [PubMed]
  41. Erdur, E.A.; Basciftci, F.A. Effect of Ti:Sapphire-Femtosecond Laser on the Surface Roughness of Ceramics. Lasers Surg. Med. 2015, 47, 833–838. [Google Scholar] [CrossRef] [PubMed]
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Figure 1. (A) Prepared LDC disc 2 mm height and 5 mm diameter created using CAD/CAM technology. (B) The line EDS of elements in the LDC disc.
Figure 1. (A) Prepared LDC disc 2 mm height and 5 mm diameter created using CAD/CAM technology. (B) The line EDS of elements in the LDC disc.
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Figure 2. (A) LDC disc conditioned with HFA–Silane. Arrow indicates an area with no loss of matrix. Whereas the area observed is where the matrix is dissolved and the glass is more pronounced. (B) LDC disc conditioned with YFL–Silane. The matrix is dissolved evenly with prominent glass areas. Areas of cracks are seen on the surface due to thermal effect of the laser indicated by arrows. (C) LDC treated with HANPS–Silane. The homogenized loss of the matrix with the prominent structure of glass is shown by the arrows.
Figure 2. (A) LDC disc conditioned with HFA–Silane. Arrow indicates an area with no loss of matrix. Whereas the area observed is where the matrix is dissolved and the glass is more pronounced. (B) LDC disc conditioned with YFL–Silane. The matrix is dissolved evenly with prominent glass areas. Areas of cracks are seen on the surface due to thermal effect of the laser indicated by arrows. (C) LDC treated with HANPS–Silane. The homogenized loss of the matrix with the prominent structure of glass is shown by the arrows.
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Figure 3. Ra of LDC after different surface pretreatments. ANOVA < 0.05; Hydrofluoric acid (HFA), ytterbium fibre lasers (YFLs), Hydroxyapatite nanoparticles (HANPs). Different numbers of asterisks denote statistically significant differences (post hoc Tukey).
Figure 3. Ra of LDC after different surface pretreatments. ANOVA < 0.05; Hydrofluoric acid (HFA), ytterbium fibre lasers (YFLs), Hydroxyapatite nanoparticles (HANPs). Different numbers of asterisks denote statistically significant differences (post hoc Tukey).
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Figure 4. SBS of LDC bonded to different viscosity resin cements after pretreating with different conditioning agents. ANOVA < 0.05. Hydrofluoric acid (HFA), ytterbium fibre lasers (YFLs), Hydroxyapatite nanoparticles (HANPs), Low viscosity (LV), high viscosity (HV). Different superscript small alphabets denote statistically significant differences (post hoc Tukey).
Figure 4. SBS of LDC bonded to different viscosity resin cements after pretreating with different conditioning agents. ANOVA < 0.05. Hydrofluoric acid (HFA), ytterbium fibre lasers (YFLs), Hydroxyapatite nanoparticles (HANPs), Low viscosity (LV), high viscosity (HV). Different superscript small alphabets denote statistically significant differences (post hoc Tukey).
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Figure 5. Fracture distribution among different tested groups.
Figure 5. Fracture distribution among different tested groups.
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MDPI and ACS Style

Aljamhan, A.; Alkhudhairy, F. Impact of Hydrofluoric Acid, Ytterbium Fiber Lasers, and Hydroxyapatite Nanoparticles on Surface Roughness and Bonding Strength of Resin Cement with Different Viscosities to Lithium Disilicate Glass Ceramic: SEM and EDX Analysis. Crystals 2025, 15, 661. https://doi.org/10.3390/cryst15070661

AMA Style

Aljamhan A, Alkhudhairy F. Impact of Hydrofluoric Acid, Ytterbium Fiber Lasers, and Hydroxyapatite Nanoparticles on Surface Roughness and Bonding Strength of Resin Cement with Different Viscosities to Lithium Disilicate Glass Ceramic: SEM and EDX Analysis. Crystals. 2025; 15(7):661. https://doi.org/10.3390/cryst15070661

Chicago/Turabian Style

Aljamhan, Abdullah, and Fahad Alkhudhairy. 2025. "Impact of Hydrofluoric Acid, Ytterbium Fiber Lasers, and Hydroxyapatite Nanoparticles on Surface Roughness and Bonding Strength of Resin Cement with Different Viscosities to Lithium Disilicate Glass Ceramic: SEM and EDX Analysis" Crystals 15, no. 7: 661. https://doi.org/10.3390/cryst15070661

APA Style

Aljamhan, A., & Alkhudhairy, F. (2025). Impact of Hydrofluoric Acid, Ytterbium Fiber Lasers, and Hydroxyapatite Nanoparticles on Surface Roughness and Bonding Strength of Resin Cement with Different Viscosities to Lithium Disilicate Glass Ceramic: SEM and EDX Analysis. Crystals, 15(7), 661. https://doi.org/10.3390/cryst15070661

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