Effect of Various Surface Treatments of Zirconia on its Adhesive Properties to Dentin: An In Vitro Study.

AIM: To assess the effectiveness of various surface treatments and adhesives on the bond strength of zirconia-based ceramic to dentin. MATERIALS AND METHODS: Eighty samples of zirconia were subjected to the four-surface treatment protocols (sandblasting, 48% hydrofluoric acid (HF), 48% hydrofluoric acid + 70% nitric acid (HNO3) and no treatment (control) following which the samples from each group were subdivided into two subgroups (n = 10) based on the resin cement employed for cementation (RelyX U200 and G-Cem Linkforce). The bonded specimens were subjected to shear stress to measure the bond strength using Universal testing machine. To test the difference in bond strength among the eight study groups, the Kruskal-Wallis ANOVA test was applied and for comparison between cements in each group, Mann-Whitney U test was applied. RESULTS: The highest bond strength values were observed for 48% HF group cemented with G-Cem Linkforce resin cement (16.220 ± 1.574) and lowest for control group-RelyX (4.954 ± 0.972). G-Cem cement showed higher bond strength than RelyX for all surface treatments except 48% HF + 70% nitric acid. CONCLUSION: It can be inferred that 48% HF can etch zirconia and generate a porous structure that proves to be beneficial for bonding. CLINICAL SIGNIFICANCE: The increasing demand for esthetics has led to the replacement of metal-ceramic materials with zirconia-based ceramics. However, the chemical inertness of zirconia to various conventional surface treating agents has continuously challenged researchers to discover a new surface treatment protocol that could enhance the bond strength of zirconia. How to cite this article: Yenamandra MS, Joseph A, Singh P, et al. Effect of Various Surface Treatments of Zirconia on its Adhesive Properties to Dentin: An In Vitro Study. J Contemp Dent Pract 2024;25(3):226-230.

Preheated acid associated with silane and electric current in the adhesion of the resin cement to ceramic.

This study verified the effect of the combination of preheated hydrofluoric acid/silane/electric current in the adhesion of the resin cement to ceramic. IPS E.max Press ceramic discs embedded in PVC rigid tubes were divided into four groups associating preheated hydrofluoric acid and silane applied with electrical current (n=10): Ha+S (Heated acid + silane); Ha+S+Ec (Heated acid + silane + electrical current); A+S (Acid + silane) and A+S+Ec (Acid + silano + electrical current). Resin cement/ceramic samples were stored in water at 37°C for 24h. After storage, they were submitted to the microshear test, fracture analysis, and contact angle at 24h or after thermocycling (10,000 cycles/5-55ºC). Bond strength data were evaluated by two-way ANOVA. For comparison between evaluation times (24h or thermocycling) was applied unpaired t-test. A significance post-hoc test of p=0.05 was assumed for analyses and graphs (GraphPad Prism 9.0 software). At 24h, the microshear strength showed similar values between Ha+S, Ha+S+Ec, and A+S+Ec groups, while A+S showed the lowest value with a statistical difference. After thermocycling, Ha+S and Ha+S+Ec were similar, as well as A+S and A+S+Ec. There was a significant difference in all groups comparing 24h (highest value) with after thermocycling (lowest value). Adhesive fracture was predominant in all groups and evaluation times. Ha+S and A+S groups showed higher contact angle values compared to the Ha+S+Ec and A+S+Ec with lower values. In conclusion, the association of preheated hydrofluoric acid/silane applied or not with electric current promoted different microshear strength values, fracture types, and contact angles in the resin cement/ceramic bond.

Dental silicate ceramics surface modification by nonthermal plasma: A systematic review.

OBJECTIVES: Nonthermal atmospheric or low-pressure plasma (NTP) can improve the surface characteristics of dental materials without affecting their bulk properties. This study aimed to systematically review the available scientific evidence on the effectiveness of using NTP for the surface treatment of etchable, silica-based dental ceramics before cementation, and elucidate its potential to replace the hazardous and technically demanding protocol of hydrofluoric acid (HF) etching. METHODS: A valid search query was developed with the help of PubMed's Medical Subject Headings (MeSH) vocabulary thesaurus and translated to three electronic databases: PubMed, Web of Science, and Scopus. The methodological quality of the studies was assessed according to an adapted version of the Methodological Index for Non-Randomized Studies (MINORS). RESULTS: Thirteen in vitro study reports published between 2008 and 2023 were selected for the qualitative and quantitative data synthesis. The implemented methodologies were diverse, comprising 19 different plasma treatment protocols with various device settings. Argon, helium, oxygen, or atmospheric air plasma may significantly increase the wettability and roughness of silicate ceramics by plasma cleaning, etching, and activation, but the treatment generally results in inferior bond strength values after cementation compared to those achieved with HF etching. The technically demanding protocol of plasma-enhanced chemical vapor deposition was employed more commonly, in which the surface deposition of hexamethyl disiloxane with subsequent oxygen plasma activation proved the most promising, yielding bond strengths comparable to those of the positive control. Lack of power analysis, missing adequate control, absence of examiner blinding, and non-performance of specimen aging were common methodological frailties that contributed most to the increase in bias risk (mean MINORS score 15.3 ± 1.1). SIGNIFICANCE: NTP can potentially improve the adhesive surface characteristics of dental silicate ceramics in laboratory conditions, but the conventional protocol of HF etching still performs better in terms of the resin-ceramic bond strength and longevity. More preclinical research is needed to determine the optimal NTP treatment settings and assess the aging of plasma-treated ceramic surfaces in atmospheric conditions.

Surface property changes observed in zirconia during etching with high-concentration hydrofluoric acid over various immersion times.

This study investigated the degree of phase transformation, surface roughness, and bond strength of zirconia immersed for various times in a 40% hydrofluoric acid (HF) solution. Non-etched sintered zirconia specimens were used as the control, while experimental groups were etched with a 40% HF solution for 5, 10, 20, 40, 80, 160 and 320 min. In each of the control and experimental groups, five specimens for X-ray diffraction analysis, four for surface morphology and surface roughness analysis, and ten for bonding strength measurement were used. As a result, the surface roughness of zirconia increased as the application time increased during the 40% HF etching, but the bond strength between zirconia and resin cement did not increase proportionally. The phase transformation from tetragonal to monoclinic also gradually increased with application time.

Hydrofluoric acid concentration and etching time affect differently the microstructure and surface properties of pressed lithium disilicate glass ceramics.

OBJECTIVE: To evaluate the effect of different hydrofluoric acid concentrations and etching times on the surface, chemical composition and microstructure of lithium disilicate. MATERIAL AND METHODS: Ninety specimens of pressed lithium disilicate (LDS) were obtained (IPS e.max Press, Rosetta SP and LiSi Press). The specimens of each material were divided in two groups according to the hydrofluoric acid concentration: 5% and 10% (n = 15/group), and subdivided according to the etching time: 20, 40 and 60 s (n = 5/group). Crystalline evaluations and chemical composition were performed through x-ray diffraction (XRD) and energy-dispersive x-ray spectroscopy (EDS), respectively. Microstructural analyses were performed by scanning electron microscope (SEM), surface roughness (Ra), and material thickness removal evaluation. Thickness removal and Ra data were analyzed by ANOVA and Tukey test (p < 0.05). RESULTS: XRD demonstrated characteristic peaks of lithium disilicate crystals, lithium phosphate and of a vitreous phase for all materials. EDS identified different compositions and SEM confirmed different surface responses to acid etching protocols. Material and etching time influenced Ra and material thickness removal (p < 0.05). CONCLUSION: Hydrofluoric acid concentration and etching time affect the surface characteristics of LDS differently. LiSi Press presented higher resistance to hydrofluoric acid etching compared to e.max Press and Rosetta SP. CLINICAL SIGNIFICANCE: Applying the appropriate etching protocol is pivotal to avoid excessive material removal and to prevent jeopardize the mechanical and optical properties of the material.

Effect of Hydrofluoric Acid Concentration on Bond Strength to Glass-Ceramics: A Systematic Review and Meta-Analysis of In-Vitro Studies.

PURPOSE: To conduct a systematic review and meta-analysis of in-vitro bond strength to glass-ceramics using hydrofluoric acid (HF) at lower (<5%) and higher (>5%) concentrations ([HF]) to treat ceramic surfaces. METHODS: Systematic searches were carried out in PubMed, Scopus, LILACS, and Web of Science for articles published through July 2021, and a meta-analysis was performed to estimate the combined effect by comparing the differences between the standardized means of the bond strengths of the evaluated materials. RESULTS: In total, 943 articles were found, of which 17 studies were selected for qualitative analysis and 12 for quantitative analysis. The bond strength to glass-ceramics using 4% to 5% HF did not differ from that using 7% to 10% HF for the following HF etching times and glass-ceramic materials: 20 s for lithium-disilicate (Z = 0.65, p = 0.51), 60 s for feldspathic (Z = 0.53, p = 0.60), and 60 s for leucite (Z = 0.72, p = 0.35). CONCLUSION: The lower concentration HF (<5%) etchant is a reliable surface treatment for adhesive bonding to glass-ceramics with satisfactory bond strength in short-term evaluations.

Effects of Hydrofluoric Acid Concentrations, Commercial Brands, and Adhesive Application on the Bond Strength of a Resin Luting Agent to Lithium Disilicate Glass Ceramic.

OBJECTIVES: To evaluate the surface topography/roughness and bond strength of a resin luting agent to a lithium disilicate glass ceramic after etching with different concentrations of hydrofluoric acid (HF) and commercial brands. METHODS: For bond strength evaluation, 260 lithium disilicate glass ceramic (EMX) discs were randomly distributed into 13 groups based on concentrations of HF and commercial brands (n=20): 5% and 10%, Lysanda (LY5 and LY10); 5% and 10%, Maquira (MA5 and MA10); 5% and 10%, FGM (FG5 and FG10); 4.8%, Ivoclar Vivadent (IV5); 5% and 10%, PHS do Brasil (PH5 and PH10); 5% and 10%, BM4 (BM5 and BM10); 9%, Ultradent Inc (UL10); and Dentsply (DE10). A further random distribution (n=10) was made based on the application (+) or absence (-) of an adhesive layer. Resin luting agent cylinders (1 mm in diameter) were added on EMX surfaces, light-cured, and stored for 24 hours in deionized water at 37°C. On a universal testing machine (DL 500, EMIC), specimens were submitted to a microshear bond strength test at a crosshead speed of 1 mm/min until failure. A representative etched EMX disc from each group underwent surface topography analysis using field-emission scanning electron microscopy (n=1), and five (n=5) etched EMX discs from each group were tested for surface roughness. Data were statistically analyzed using analysis of variance and Tukey test (α=0.05). RESULTS: A less conditioned and smoother surface was observed for 5% HF compared to 10%. Additionally, commercial brands of HF were shown to affect bond strength. When the adhesive layer was not used (-), a 10% concentration promoted higher bond strengths to EMX. However, when adhesive was applied (+), the concentrations of HF and commercial brands had no effect on bond strength results. CONCLUSIONS: A 10% concentration of HF results in higher bond strength than a 5% concentration. If an adhesive layer is applied, neither this distinction nor the influence of commercial brands is observed.

The loss of resin cement adhesion to ceramic influences the fatigue behavior of bonded lithium disilicate restorations.

When partial and/or non-retentive preparation, such as those for occlusal veneers, is indicated, a proper and stable adhesion is essential. Therefore, the aim of this in vitro study was to evaluate the effect of loss of adhesion in different regions of the bonding interface on the fatigue behavior of simplified lithium disilicate restorations. For this, lithium disilicate (IPS e.max CAD) discs (1 mm thick and Ø = 10 mm) were fabricated, polished with #400-, #600-, #1200-grit silicon carbide (SiC) papers, and crystallized. As substrate, fiber-reinforced resin epoxy discs (2.5 mm thick and Ø = 10 mm) were fabricated and polished with #600-grit SiC paper. The ceramic bonding surface was treated with 5% hydrofluoric acid and a silane-containing primer (Monobond N), while the substrate was etched with 10% hydrofluoric acid followed by the application of the bonding system primers (Primer A + B). A lacquer (nail polish) was used to simulate the loss of adhesion in specific areas according to the study design to compose the testing groups: bonded (control; did not received nail polish application); - non-bonded (loss of adhesion in the whole specimen area); - margin (loss of adhesion in the ceramic margin); - center (loss of adhesion in the ceramic central area). The adhesive area of partially bonded groups was 50% of the adhesive surface. Then, the discs (n = 12) were bonded to the respective substrate using a resin cement (Multilink N), light-cured, water-stored for 90 days, and subjected to thermocycling (25,000 cycles, 5° to 55 °C) before testing. A cyclic fatigue test was run (20 Hz, initial load of 200 N for 5000 cycles, 50 N step size for 10,000 cycles each until specimen failure), and the fatigue failure load and number of cycles for failure were recorded. As complementary analysis, finite element analysis (FEA) and scanning electron microscopy analysis were performed. Kaplan-Meier log-rank (Mantel-Cox) was conducted for survival analysis. The results showed that as the loss of adhesion reaches the central area, the worse is the fatigue behavior and the higher is the stress peak concentration in the ceramic bonding surface. The bonded specimens presented better fatigue behavior and stress distribution compared to the others. In conclusion in a non-retentive preparation situation, proper adhesion is a must for the restoration fatigue behavior even after aging; while the loss of adhesion reaches central areas the mechanical functioning is compromised.

Influence of surface treatments and adhesive protocols on repair bond strength of glass-matrix and resin-matrix CAD/CAM ceramics.

OBJECTIVE: To specify the effects of self-etching ceramic primer, Monobond Etch and Prime (MEP), and universal adhesive (UA) on repair bond strength between CAD/CAM blocks and resin composite. MATERIALS AND METHODS: Vita Mark II (VM), IPS e.max CAD (EMAX), Shofu Block HC (SHC), and Tetric CAD (TET) blocks were sliced and thermocycled. They were divided into four groups according to surface treatments (n = 24): control, sandblasting (AL), hydrofluoric acid etching (HF), and MEP application. SEM analysis assessed surface topography. Subdivided, specimens followed distinct adhesive protocols (n = 12): control (silane + adhesive [SA] or adhesive [A] only for MEP group) and UA. Microshear bond strength (µSBS) was measured following resin composite repair. Data were analyzed using two-way ANOVA and Tukey tests (p < 0.05). RESULTS: The µSBS of CAD/CAM blocks was significantly influenced by surface treatment type and adhesive protocol. The highest µSBS values for each block, considering surface treatment + adhesive protocol, were VM, HF + SA, or HF + UA; EMAX, MEP + A; and SHC and TET, AL + SA, or AL + UA. CONCLUSIONS: Except for EMAX, it was not the adhesive protocol that made the significant difference in bond strength for each CAD/CAM block, but the surface treatment. MEP + UA application on glass ceramics lowered µSBS values significantly, so it is not recommended in clinical conditions. CLINICAL SIGNIFICANCE: Repair is an essential therapeutic option, particularly in esthetic restorations, to swiftly repair the impaired esthetics caused by fracture. Repair protocol is dependent on the restorative material, and to have a reliable repair bond strength, the following surface treatment and adhesive protocol combinations are recommended for each CAD/CAM block: VM, HF + SA, or HF + UA; EMAX, MEP + A; and SHC and TET, AL + SA, or AL + UA.

Preheated Composite as an Alternative for Bonding Feldspathic and Hybrid Ceramics: A Microshear Bond Strength Study.

PURPOSE: To evaluate the bond strength between alternative or conventional luting agents and indirect restorative materials. MATERIALS AND METHODS: Blocks of a polymer-infiltrated ceramic network (PICN, Vita Enamic) and a feldspathic ceramic (FEL, Vita Mark II) were sliced and divided according to the luting agent: resin cement (PICN-RC, FEL-RC), flowable composite (PICN-FC, FEL-FC), or preheated composite (PICN-PH, FEL-PH). The ceramic surfaces were polished, etched with 5% hydrofluoric acid for 60 s, and then a silane layer was applied. Cylinders of the luting agents were built up on the ceramic surfaces. In half the samples, the microshear bond strength (µSBS) was tested after 24 h (baseline). The other half was tested after 5000 thermocycles (5°C-55°C) (aging). The failure modes were determined using a stereomicroscope, and the ceramic surfaces were analyzed using a scanning electron microscope. Data were statistically analyzed with two-way ANOVA. RESULTS: Thermocycling reduced the bond strength values of all experimental groups. Regarding FEL, the preheated composite obtained the highest results. Resin cement showed results similar to the flowable composite at baseline and after aging. The highest results of PICN were obtained from the preheated composite followed by resin cement and flowable composite. Significant differences among the three luting agents were observed before and after aging. The most frequent failures among the experimental groups were adhesive and cohesive in the ceramic. CONCLUSION: Bond strength results indicate that the preheated composite can be an alternative for adhesive cementation when applied on the tested feldspathic ceramic or PICN.

Fracture load of ultrathin occlusal veneers: Effect of thickness and surface conditioning.

OBJECTIVE: This in-vitro study is planned to analyze the effect of different thicknesses of ceramic occlusal veneers and different surface treatments on fracture resistance. MATERIALS AND METHODS: A total of 48 sound mandibular molars are anatomically prepared from the occlusal surface with two different thicknesses (1.0 and 0.5 mm). CAD/CAM zirconia-reinforced glass ceramic blocks (Vita Suprinity) are used for fabricating occlusal veneers. The teeth are randomly divided into two primary groups A and B (n=24) according to occlusal veneer thickness. Each group is subdivided according to surface conditioning into three equal subgroups (n=8)-subgroup HF: etching with hydrofluoric acid and ceramic primer application; subgroup APF: etching with acidulated phosphate fluoride and ceramic primer application; subgroup EP: conditioning with etch and prime only. Dual-cure adhesive resin cement (Multilink Automix) is utilized to adhesively bond the veneers. All specimens are subjected to 240,000 cycles of dynamic load aging prior to the fracture resistance test. The fracture resistance is measured in Newton (N). The Failure mode patterns are analyzed and categorized using a scanning electron microscope (SEM). The results are analyzed using a two-way ANOVA with Bonferroni's Post-Hoc test, followed by a one-way ANOVA for each factor. That is in addition to one-way ANOVA for surface treatment under each thickness, each followed by Bonferroni's Post-Hoc test. Then, a T-test is used to compare the two thicknesses under each surface treatment. All tests are set at 0.05 significance level. RESULTS: The two-way ANOVA test revealed that restoration thickness and surface treatment both significantly affect the fracture resistance values (p<0.05). The highest fracture resistance mean (2672±216N) is obtained from HF at 1.0 mm thickness, while the lowest mean (2104±299N) is obtained from APF at 0.5 mm thickness. CONCLUSION: All test groups, regardless of thickness, demonstrated fracture resistance values that exceeded both normal and parafunctional bite forces. The veneers that bonded after hydrofluoric acid etching followed by ceramic primer application showed more favourable fracture patterns.

Hybrid ceramic repair strength, surface roughness, and bond failure, using methylene blue-activated low-level laser therapy, Carbon dioxide, and Ti: Al2O3 laser.

AIMS: To evaluate the impact of various pretreatment regimes (LLLT, Ti-sapphire laser, CO2, and HFA-S) on hybrid ceramics, specifically focusing on their ability to enhance repair strength and minimize surface roughness (Ra). MATERIAL AND METHODS: Discs were made from hybrid ceramics and after disinfection were randomly divided into four groups based on different surface conditioning techniques. Each group consisted of 15 discs, resulting in a total sample size of 60. dics in group 1 was surface treated with Low-level laser therapy (LLLT) using methylene blue (MB), Discs in group 2 with Ti-sapphire laser, Discs in group 3 with CO2 laser, and discs in group 4 with HFA-S. Five samples from each group were assessed for Ra. The remaining 10 samples from each group underwent repair using a porcelain repair kit in adherence to the planned instructions. The bond strength of each sample in all groups was measured using a universal testing machine. Following the bond strength testing, the specimens from all study groups were analyzed to determine the mode of failure. To evaluate the data, a two-way analysis of variance (ANOVA) was used, followed by post hoc multiple comparisons. RESULTS: The highest repair bond strength was observed in group 4 hybrid ceramics pretreated with HFA-S (19.05±0.79 MPa). The lowest repair bond scores were observed in group 1 hybrid ceramics preconditioned with LLLT in the presence of Photosensitizer (13.41±0.36 MPa). The highest Ra scores were exhibited in group 2 surface treated with Ti-sapphire laser (0.0515±0.16 µm) and the lowest Ra scores were observed in Group 4 HFA-S (0.0311±0.79 µm). Predominant bond failure among different investigated groups was cohesive. CONCLUSION: The current gold standard for hybrid ceramic conditioning is the use of hydrofluoric acid (HFA) combined with a silane coupling agent. Low-level laser therapy with methylene blue photosensitizer is not recommended for the treatment of hybrid ceramics.

Decontamination of lithium disilicate ceramics using various photosensitizers, herbal and chemical disinfectants, and the effect of surface conditioners on bond strength values.

AIM: To assess and compare the antimicrobial efficacy of disinfectants on lithium disilicate ceramic (LDC) used in dental applications and shear bond strength (SBS) of LDC after using different conditioners hydrofluoric acid (HF), self-etching ceramic primers (SECP) and Neodymium-doped yttrium orthovanadate (Nd: YVO4). MATERIALS AND METHODS: One hundred and twenty LDC discs were fabricated by auto-polymerizing acrylic resin using the lost wax technique. S. aureus, S. mutans, and C. albican were inoculated on thirty discs (n = 30 each). Each group was further divided into three subgroups based on different disinfecting agents used (n = 30) Group 1: Garlic extract, Group 2: Rose Bengal (RB) activated by PDT, and Group 3: Sodium hypochlorite (NaOCl). An assessment of the survival rate of microorganisms was performed. The remaining thirty samples were surface treated using three different LDC surface conditioners (n = 10) Group 1: HF + Silane (S), group 2: SECP, and Group 3: Nd: YVO4 laser+S. SBS and failure mode analysis were performed using a universal testing machine and stereomicroscope at 40x magnification, The statistical analysis was conducted using one-way ANOVA and Post Hoc Tukey test. RESULTS: Garlic extract, RB, and 2% NaOCl sample displayed comparable outcomes of antimicrobial potency against C. albicans, S aureus, and S. mutans (p > 0.05). Furthermore, SBS analysis showed HF+S, SECP, and Nd: YVO4+S exhibited comparable outcomes of bond strength (p > 0.05). CONCLUSION: Garlic extract and Rose bengal activated by PDT can be contemplated as alternatives to the chemical agent NaOCl used for LDC disinfection. Similarly, SECP and Nd: YVO4 possess the potential to be used for the surface conditioning of LDC to improve the bond integrity with resin cement.

Repair Bond Strength to Hybrid CAD/CAM Materials after Silane Heat Treatment with Laser.

PURPOSE: This study investigated the effect of different surface treatments and the effect of silane heat treatment with laser on the shear bond strength (SBS) of a nanoceramic composite to repaired hybrid CAD/CAM blocks. MATERIALS AND METHODS: 60 hybrid CAD/CAM specimens (Cerasmart, GC) were prepared and randomly divided into six groups according to the different surface treatments (n = 10): group ER: Er:YAG laser+silane (Monobond Plus, Ivoclar Vivadent); group ER+SHT: Er:YAG laser+silane heat treatment; group B: bur+silane; group B+SHT: bur+silane heat treatment; group HF: hydrofluoric acid+silane; group HF+SHT: hydrofluoric acid+silane heat treatment. Afterwards, a universal adhesive (Universal Bond Quick, Kuraray) was applied, and nanoceramic resin composite (Zenit, President) cylinders were bonded to the Cerasmart specimens. They were thermocycled for 10,000 cycles (5-55°C) and subjected to SBS testing using a universal testing machine. Failure modes were examined with a stereomicroscope (15X). Scanning electron microscopy (SEM) was used to evaluate the surface topography (n = 2). The data were statistically analyzed using the Mann-Whitney U-test and the Kruskal-Wallis test (p < 0.05). RESULTS: Regarding the surface treatments, group ER showed significantly lower SBS than groups B and HF (p < 0.05). Regarding the presence of silane heat treatment by laser, groups ER+SHT and B+SHT showed significantly lower SBS than group HF+SHT(p < 0.05). In addition, group B+SHT showed significantly lower SBS than did group B (p < 0.05). CONCLUSION: Er:YAG laser treatment for repairing hybrid CAD/CAM blocks was not as effective as bur roughening or hydrofluoric acid etching. Silane heated by Er:YAG laser was incapable of significantly increasing the bond strength to repaired hybrid CAD/CAM blocks.

The Impact of Different Surface Treatments on Topography and Bond Strength of Resin Cement to Lithium Disilicate Glass Ceramic.

OBJECTIVE: To evaluate the influence of different surface treatments on topography, surface roughness, surface energy, and microtensile bond strength stability of resin cement to lithium disilicate glass ceramic. METHODS AND MATERIALS: Seventy disc-shaped specimens of IPS e.max Press were divided into seven groups according to the surface treatment: NT - non-treated (control); FSil - hydrofluoric acid (HF) + silane; FPSil - HF + phosphoric acid (HP) + silane; FUSil - HF + ultrasonic bath (U) + silane; FPUSil - HF + HP + U + silane; MEP - Monobond Etch and Prime (MEP); and MEPH - MEP + heating. Topography and surface roughness were evaluated using a 3D laser confocal microscope (3DLCM) and scanning electron microscopy (SEM) and surface energy with a goniometer. The microtensile bond strength (µTBS) was evaluated after storage in distilled water at 37°C for 24 hours and after thermocycling (5,000 cycles, 5°-55° C, 30-second dwell time). Data were analyzed using one-way ANOVA (surface roughness and surface energy), two-way ANOVA (µTBS), Tukey's HSD post-hoc test, and Student t-test (α=0.05). RESULTS: FUSil, FPSil, and FSil presented similar and highest surface roughness, whereas NT, FPUSil, MEP, and MEPH showed similar, and lowest, roughness values (p<0.05). FPUSil, FPSil, FUSil, and FSil presented a similar and highest surface energy. NT, MEP, and MEPH showed similar and lowest surface energy. CONCLUSION: Only FSil, FPSil, and MEPH maintained bond strength stability after thermocycling, with FPSil leading to less bond strength reduction, suggesting this protocol is more reliable for bonding resin cements to lithium disilicate glass ceramics.

Effect of resin cement elastic modulus on the biaxial flexural strength and structural reliability of an ultra-thin lithium disilicate glass-ceramic material.

OBJECTIVES: Photo- and dual-polymerized resin-based luting agent was evaluated for elastic moduli effects on ultra-thin lithium disilicate (LD) glass-ceramic strengthening, structural reliability, and stress distribution. MATERIALS AND METHODS: One hundred-sixty LD discs (IPS e.max CAD, Ivoclar/Vivadent) were produced in ultra-thin thicknesses (half with 0.3 mm and the other half with 0.5 mm). The ultra-thin ceramic disks were coated with two different cement types (Variolink Veneer - V and Panavia F 2.0 - P). Two positive control groups were tested following hydrofluoric (HF) acid etching (LDt3, LDt5) and two negative control groups were tested for untreated ceramic (LD 3, LD 5). Biaxial flexural strength (BFS), characteristic strength (σ0) and Weibull modulus (m) were the response variables (n = 20) at the ceramic/resin cement interface (z = 0). Finite element analysis (FEA) was used to calculate maximum principal stress. Data were analyzed using two-way ANOVA, and Tukey's test. Scanning electron microscopy (SEM) was used to analyze the failed specimens using fractography and surface morphology. RESULTS: The BFS of LD at either thickness was not affected by cement types, as also demonstrated by FEA. Structural reliability significantly improved in the positive control group (LDt5). CONCLUSION: The cementation of ultra-thin LD with a resin-cement of varying elastic moduli did not influence BFS. LD surface modification by HF acid-etching increased the reliability. CLINICAL RELEVANCE: Ultra-thin anterior veneer designs made from lithium disilicate have been widely proposed and the apparent success of LD ultra-thin veneers was not influenced by the cement choice in the current studies albeit the elastic moduli luting agents used were of similar values.

Effect of different surface treatments on resin-matrix CAD/CAM ceramics bonding to dentin: in vitro study.

BACKGROUND: Evaluating the effect of different surface treatment methods on the micro-tensile bond strength (µTBS) of two different resin-matrix computer-aided design/computer-aided manufacturing (CAD/CAM) ceramics (RMCs). METHODS: A standardized inlay preparations were performed on 100 intact maxillary premolars. According to the type of the restorative material, the teeth were randomly divided into two equally sized groups (n = 50): (polymer-infiltrated ceramic (Vita Enamic) and resin-based composites (Lava Ultimate)). The inlays were fabricated using CAD/CAM technology. In each group, the specimens were randomly assigned to five subgroups (n = 10) according to the surface treatment method: group 1 used was the control group (no surface treatment); group 2, was treated with air abrasion with 50 µm Al2O3 (A) and universal adhesive (UA); group 3, was treated with air abrasion with 50 µm Al2O3 (A) and silane coupling agent (S); group 4, was treated with hydrofluoric acid (HF) and universal adhesive (UA) and group 5, was treated with Hydrofluoric acid (HF) + silane coupling agent (S). The inlays were then cemented to their respective preparations using dual-cure self-adhesive resin cement (RelyX U200, 3 M ESPE) according to the manufacturer's instructions. The µTBS test was conducted in all groups, and stereomicroscope and scanning electron microscope were used to inspect the failure mode. The data were statistically analyzed using a two-way analysis of variance (ANOVA) and Tukey's post-hoc multiple comparison tests at a significance level of p < 0.05. RESULTS: Surface treatments significantly increased the µTBS of the materials compared to the control group (p < 0.05). For CAD/CAM RBCs, the µTBS value highest in group 2 whereas, for PICN, the µTBS value was highest in group 3. Cohesive failure of CAD/CAM restorative material was the most predominant mode of failure in all treated groups, whereas adhesive failure at restoration-cement interface was the most predominant failure mode in the control group. CONCLUSION: Surface treatments increase the µTBS of resin-matrix CAD/CAM ceramics to tooth structure. Air abrasion followed by universal adhesive and hydrofluoric acid followed by silane application appears to be the best strategies for optimizing the bond strength of CAD/CAM RBCs and PICN respectively.

Innovation Glass-Ceramic Spray Deposition Technology Improving the Adhesive Performance for Zirconium-Based Dental Restorations.

Glass-ceramic spray deposition (GCSD) is a novel technique for coating lithium disilicate (LD) glass-ceramics onto zirconia through simple tempering steps. GCSD has been proven to improve the bonding of zirconia to resin cement, but the effect of etching time on GCSD and the long-term durability of the bond achieved remain unknown. The effects of air abrasion with aluminum particles (ABB) and air abrasion (GAB) or etching with 5.0% hydrogen fluoride (HF) for 20, 60, 90, and 120 s (G20, G60, G90, and G120) on the resin cement−zirconia bond were studied. LD was included as a control (LDG). The microstructure, sub-micron roughness, wettability, and phase changes of samples were analyzed. After resin cement was bonded to zirconia, half of the samples were subjected to thermocycling (5000 cycles at 5−55 °C). The bond strengths of the samples were determined in shear bond strength (SBS) tests (n = 10 per group). An LD structure can be formed on zirconia after GCSD and proper etching processes, which result in high roughness and a hydrophilic nature. GCSD and HF etching significantly improved SBS, with G90 and G120 samples with pre- or post-thermocycling exhibiting SBS values comparable to those of LDG (p > 0.760). The surface characteristics of the LD layer are influenced by the etching time and affect the SBS of the bond of zirconia to resin cement. HF etching for 90−120 s after GCSD results in zirconia with SBS and bond durability comparable to LD.

Influence of Fit-checking Material and Cleaning Protocols on the Bond Strength of Lithium Disilicate Glass-ceramics.

OBJECTIVES: To evaluate the bond strength of a resin luting agent to a lithium disilicate glass-ceramic after the use of different fit-checking materials and cleaning protocols. METHODS AND MATERIALS: Two hundred and forty-two (242) ceramic specimens were etched with 5% hydrofluoric acid for 20 seconds and distributed into 22 groups (n=10), in total. Four (4) groups were created based on fit-checking material and that had no following cleaning protocol: no fit-checking material used (control group); articulating paper; articulating spray; and fit-checker liquid. For each fit-checking material (3), 6 cleaning protocols were tested creating an additional 18 groups (n=10): air/water spray; 70% alcohol (ethanol); acetone; 35% phosphoric acid; 5% hydrofluoric acid; and a commercially available cleaning paste (Ivoclean, Ivoclar Vivadent). Silane and bonding resin were applied to all ceramic surfaces. Resin luting agent cylinders (1 mm in diameter) were created using silicone matrices, light-cured, and specimens were stored in deionized water at 37°C for 24 hours. Microshear bond strength test (µSBS) was performed on a universal testing machine (DL 500, EMIC) at a crosshead speed of 1 mm/min until failure. Results were statistically analyzed using ANOVA and Tukey's test (α=0.05). RESULTS: Articulating paper and fit-checker liquid, when not properly removed, negatively affected the bond strength (p<0.05). None of the tested cleaning protocols were effective for articulating paper (p<0.05). There was no significant difference in bond strength after the cleaning protocols between articulating spray and fit-checker liquid when compared to the control group (no contamination) (p>0.05). CONCLUSION: The cleaning protocols tested can effectively restore the bond strength of resin luting agents to lithium disilicate ceramics that were exposed to articulating spray or fit-checker liquid. The use of articulating paper is not recommended for fit-checking indirect lithium disilicate restorations.

Low-cost fabrication and characterization process for development of a sensitive optical fiber structure.

The structure of silica single-mode fiber (SMF) must be modified in order to develop optical fiber-based biosensors. To reduce the diameter of the optical fiber, a low-cost chemical etching method is very popular. The proposed chemical etching method is a simple, rapid, and cost-effective technique for removing the silica cladding up to a desired diameter. In the laboratory, hydrofluoric acid (HF acid, 40% concentration) is used for etching. A variation on etching is also proposed and tested with 40% HF as well as with magnetic stirring at the different speeds. The etching experiments are also carried out at different temperatures. The etching results of silica fiber are presented through a step-by-step procedure using a rapid and resource-efficient method for the fabrication of optical fiber-based biosensors. The etched diameter characterization is done using a calibrated compound microscope. The sensing experiment with unetched and etched optical fiber is also performed for the detection of different concentrations of glucose biomolecules.