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.

Bond Strength to Lithium-Disilicate Ceramic after Different Surface Cleaning Approaches.

PURPOSE: To evaluate the effect of different lithium-disilicate (LiSi) glass-ceramic surface decontamination procedures on the shear bond strength (SBS) to resin cement. MATERIALS AND METHODS: Seventy CAD/CAM LiSi ceramic specimens (IPS e.max CAD, Ivoclar) were cut and sintered. Fifty specimens were treated with 5% hydrofluoric acid (HF) for 20 s, while 20 were left untreated. All 70 specimens were then contaminated with human saliva and try-in silicone paste. The following surface cleaning methods were investigated (n = 10): C: water rinsing (control); PA: 37% H3PO4 etching for 20 s; E: 70% ethanol applied for 20 s; CP: cleaning paste (Ivoclean, Ivoclar) brushed for 20 s; HFSEP: self-etching ceramic primer (Monobond Etch&Prime, Ivoclar) rubbed for 20 s; HF: 5% HF applied for 20 s or no HF etching prior to contamination; SEP: self-etching ceramic primer rubbed for 20 s and no HF etching prior to contamination. Composite cylinders were created and luted with an adhesive resin cement to the decontaminated surfaces. After storage for 24 h at 37°C, the SBS test was conducted. Two fractured specimens per group were observed under SEM to perform fractographic analysis. The data were statistically analyzed with p set at <0.05. RESULTS: The type of surface cleaning approach influenced bond strength (p < 0.001). HFSEP, SEP, and HF attained higher SBS (p < 0.001) compared to other groups. None of the approaches were able to completely remove contaminants from the ceramic surfaces. SEM images showed residual traces of contaminants on CP-treated surfaces. CONCLUSIONS: The self-etching ceramic primer enhanced bond strength to contaminated LiSi ceramic surfaces, irrespective of previous treatment with hydrofluoric acid.

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.

Effect of different surface treatment protocols on the bond strength between lithium disilicate and resin cements.

Because the use of hydrofluoric acid (HF) poses health risks if handled improperly, many clinicians prefer to have the ceramic restorations pre-etched in dental laboratories. However, during the try-in procedure, the pre-etched glass-ceramic restorations may be contaminated with saliva resulting in reduced bond strength. This in-vitro study aimed to investigate the effect of different surface treatments on the bond strength of lithium disilicate (LD) glass-ceramic restorations (IPS e.max Press, Ivoclar Vivadent) to two resin cements. One-hundred eighty blocks (4X4X3mm) of LD glass-ceramic were divided into twelve groups (n = 15), of which six received Variolink Esthetic DC (VE) cement and six received RelyX Ultimate (RU) cement, following the surface treatments: G1) Control: Hydrofluoric Acid + Silane (HF + Sil); G2) Hydrofluoric Acid + Saliva + Silane (HF + S + Sil); G3) Hydrofluoric Acid + Saliva + Ivoclean + Silane (HF + S + IC + Sil); G4) Hydrofluoric Acid + Saliva + Phosphoric Acid + Silane (HF + S + P + Sil); G5) Hydrofluoric Acid + Saliva + Monobond Etch & Prime (HF + S + EP); G6) Monobond Etch & Prime (EP). Following treatment, a resin-cement cylinder (2.3 mm diameter) was built on the glass-ceramic surface, photocured (20 s), stored in distilled water (37 °C, 24 h) and submitted to the shear bond strength test. Bond strength data (MPa) were subjected to two-way ANOVA and Tukey (α = 0.01). Cement type and surface treatment had a significant effect on the bond strength (p < 0.001) (Table 4). Single-step Monobond Etch & Prime (EP) significantly improved the bond strength of resin-cements to glass-ceramic with and without saliva contamination.

Diphoterine, an amphoteric rinsing solution, reduces hydrofluoric acid injuries in an ex vivo pigskin model.

Hydrofluoric acid (HF) is a ubiquitous industrial chemical that is particularly hazardous because of the potential for systemic effects and the induction of severe cutaneous necrosis after contact with the skin. Minimizing skin injury requires decontaminating the affected area promptly with an emergency rinsing solution. Few experimental studies have objectively characterized rinsing solutions such as Diphoterine (DP). Here we develop an ex vivo pigskin model to study and compare the efficacy of rinsing solutions as initial decontaminating agents to stop the progression of skin lesions after HF splashing. The pigskin model shows an immediate local response to HF at varying concentrations and exposure times. We then exposed the pigskin biopsies to 3.75% HF for 1 min and rinsed them with different solutions, including water, 0.9% NaCl solution (saline), 10% calcium gluconate (CaG), Hexafluorine (HXF), and DP. We found DP to be a more effective agent for decontaminating HF lesions than water, saline, and CaG. DP had a similar efficacy as HXF, an emergency rinsing solution used specifically for decontaminating HF-exposed skin. This study shows that skin exposed to HF must be treated quickly from the first minute of exposure.

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.

Ultrathin Feldspathic Ceramic Veneers: A Pilot SEM Evaluation of Etched Intaglio Surfaces.

Ultrathin ceramic veneers are a viable therapeutic option to manage esthetic challenges in the anterior zone. Proper conditioning of the intaglio surface of porcelain veneers is essential to achieve an adequate bonding. In clinical practice, this is typically done with chemical etching using an acid-containing agent, such as hydrofluoric acid. While it is well established that the etching effect is dependent on etching time and the acid concentration, little is known about the impact of etching time and the veneer fabrication method. The purpose of this pilot study was to evaluate, using scanning electron microscopy (SEM), the effect that different etching-time protocols have on the intaglio surface characteristics of ultrathin ceramic veneers fabricated with either the platinum foil technique or the refractory die technique. Several replicas of an ultrathin feldspathic ceramic veneer for a maxillary central incisor were fabricated. Individual specimens were processed according to different intaglio surface-etching protocols: no etching, etching for 90 seconds, etching for 120 seconds, and etching for 150 seconds (9.6% hydrofluoric acid used for all etching groups). It was observed that the 120-second etching protocol resulted in a favorable microroughness surface pattern in the platinum foil group. This pattern was comparable to that obtained by etching for 90 seconds with hydrofluoric acid the intaglio surface of veneers fabricated with the refractory die technique. Increasing the etching time to 150 seconds did not result in a more favorable roughness pattern.

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.

Is dentin analogue material a viable substitute for human dentin in fatigue behavior studies?

This study aimed to compare the fatigue performance of a lithium disilicate ceramic cemented on different substrates (human dentin and glass fiber-reinforced epoxy resin - GFRER), treated with different types of conditioning (CTR - without surface conditioning; HF5 - 5% hydrofluoric acid; HF10 - 10% hydrofluoric acid; H3PO4 - phosphoric acid 37%; SAND - sandblasting with aluminum oxide). The occlusal surface of human molars (DENT group) (n = 15) was ground for dentin exposure and the root portion was cut, then the dentin slice (2.0 mm thick) was conditioned with 37% phosphoric acid and a dual-curing dental adhesive was applied. The GFRER in a round-rod format was cut into discs (Ø = 10 mm, 2.0 mm thick). Lithium disilicate glass ceramic blocks (IPS e.max CAD, Ivoclar, Schaan, Liechtenstein) were shaped into a cylinder format and cut, resulting in 90 discs (Ø = 10 mm, 1.5 mm thick). The substrate materials of each group were etched according to the groups and the ceramic was etched with 5% hydrofluoric acid for 30 s. A silane coupling agent was applied over the cementation surface in ceramic and GFRER surfaces and a dual cement was used for cementation (ceramic/GFRER or dentin). The disc/disc sets were submitted to thermocycling (25,000 cycles + storage for 6 months), and then tested in step-wise accelerated cyclic fatigue test. The failure pattern and topography were analyzed and the roughness and contact angle were measured before and after surface treatment. The DENT group presented the lowest load to failure values and number of cycles to failure in fatigue (637.33 N; 118.333), showing no statistical similarity with any of the other tested groups (p < 0.05). The topographic analysis showed that all proposed surface treatments modified the substrate surface when compared to the CTR group. All of the fractographical inspections demonstrated failure by radial crack. Considering the roughness analysis, the post-etched DENT group showed similar roughness to all groups of GFRER materials with their surface treated, except for SAND, which showed greater roughness and statistically different from the other groups. The DENT group (49.5) showed statistically different post-conditioning contact angle values from the HF10 group (96.5) and similar to the other groups. The glass fiber-reinforced epoxy resin was not able to simulate the results presented by the human dentin substrate when cemented to lithium disilicate regarding fatigue failure load and number of cycles for failure, regardless of the surface treatment. Lithium disilicate cemented on dentin analogue overestimates the load values for fatigue failure.

Characteristic fatigue strength and reliability of dental glass-ceramics: Effect of distinct surface treatments - Hydrofluoric acid etching and silane treatment vs one-step self-etching ceramic primer.

The aim of this study was to mechanically characterize through flexural fatigue test two CAD-CAM glass-ceramics according to distinct surface etching protocols. To do so, feldspathic (FELD) and lithium disilicate (LD) glass ceramics were subjected to different surface treatments: (1) control - no treatment (Ctrl); (2) conventional protocol etching with 5% hydrofluoric acid followed by silane coupling agent application (HF + SIL; Monobond N, Ivoclar); or (3) using a self-etching ceramic primer (E&P; Monobond Etch & Prime, Ivoclar). Ceramic discs (N = 120; Ø = 12 mm; thickness = 1.2 mm) were produced from CAD-CAM blocks, with 60 being from FELD (VITABLOCS Mark II, Vita Zahnfabrik) and 60 from LD (IPS e.max CAD, Ivoclar). Next, 20 disks of each ceramic were allocated into three groups: Ctrl, HF + SIL, or E&P. Surface roughness data were collected on all samples before and after surface treatments (except for Ctrl). Cyclic fatigue (n = 15) biaxial flexural strength tests were performed by the piston-on-three-balls geometry (ISO 6872) considering the test parameters established from a monotonic test (n = 5). The monotonic test was carried out at a 1 mm/min loading rate and 500 kgf loading cell until fracture to obtain the failure data. The cyclic fatigue test was executed underwater at a frequency up to 20 Hz, with the first stress being 25% of the monotonic test for 5000 cycles, followed by increments of 5% of the monotonic test at each step of 10,000 cycles until failure (fracture). Complementary fractography, topography and Atomic Force Microscopy (AFM) analyses were performed. Characteristic Fatigue Strength (CFS) and Weibull modulus were analyzed by Weibull analysis using the fatigue test data. Roughness and complementary analysis data were analyzed by one-way ANOVA. The statistical results exhibited similar CFS among Ctrl, HF + SIL and E&P for both glass-ceramics. The survival analysis corroborates the findings, however the Weibull modulus pointed out superior structural reliability of FELD treated with the E&P group compared to HF + SIL. According to the complementary analyses, HF + SIL exhibited a higher surface area than E&P and Ctrl for FELD (p = 0.001). Roughness showed statistically significant differences among conditions for FELD (E&P < Ctrl = HF + SIL; p < 0.05) and no difference for LD (p > 0.05). Therefore, the CFS were not influenced by any condition evaluated for FELD and LD glass-ceramics; however, superior structural reliability (higher Weibull modulus) for the feldspathic ceramic treated with the E&P was observed.

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.

Open acid dissolution-Ammonia solution extraction-ICP OES rapid determination of 7 trace metal elements in soil.

To overcome the corrosion of hydrofluoric acid on the ICP OES injection system in the acid dissolution system, this paper makes some improvements based on the traditional open digestion. The improved method does not require the complete removal of hydrofluoric acid. After appropriate digestion of the sample with a mixed acid, the solution can be transferred to a colorimetric tube containing ammonium hydroxide solution to give the final volume for analysis. In this paper, two-point standard curves are plotted using soil standards and process blanks, which is not only convenient but also overcomes the interference of the matrix effect. Through continuous experiments, the preferred ratio of mixed acid is 3 mL nitric acid + 5 mL hydrofluoric acid, and the concentration of ammonia solution is 0.5%. The spectral lines of the measured elements V (292.4), Cr (283.5), Co (228.6), Ni (231.6), Cu (324.7), Zn (213.8) and Pb (220.3) were determined. The method quantification limits of the seven measured elements V, Cr, Co, Ni, Cu, Zn and Pb were 0.909, 4.32, 0.269, 0.261, 0.968, 3.69 and 2.64 µg g-1, respectively, and the precision was 3.5%, 5.2%, 4.8%, 2.4%, 6.1% and 4.5%, respectively. After processing six national standard materials according to the experimental method, the measured values of each measured element were basically in agreement with the certified values, indicating that this method is fully feasible for the measurement of V, Cr, Co, Ni, Cu, Zn and Pb in soil. This method greatly improves the efficiency of pretreatment and is particularly suitable for analysing large batches of samples.

Changes in mineral fraction and pore morphology of coal with acidification treatment: contribution of clay minerals to methane adsorption.

The accurate calculation of the contribution which provided by clay minerals in coal on methane adsorption not only bares a significant importance for evaluating the effectiveness of acid stimulation in improving permeability and estimating the coalbed methane reserves but also serves a guide for the governance and utilization of methane resources. In this study, hydrochloric acid (HCl) and hydrofluoric acid (HF) were used to remove specific minerals in Qingdong coal samples. We firstly analyzed the mineral compositions of coal samples with different acidification treatments based on the X-ray diffraction (XRD) experiments, together with analysis of the changes in pore morphology and adsorption capacity. The results showed that acidification did not significantly change the shape of the pores, which remained slit-/plate-like pore. However, the altered adsorption capacity of the coal samples was attributed to changes in pore structure and mineral distribution. Acid erosion of mesopores promoted the transition from mesopores to macropores, contributing to an increase of 8.4% and 24.36% in the percentage of macropores in coal samples treated with HCl and HF, respectively. Fractal dimension D1 grew from 2.2193 to 2.3888 and 2.2572, respectively, but D2 decreased from 2.6146 to 2.5814 and 2.5433, indicating an increment in pore surface roughness and a simplification of the pore structure. The mineral richness of the coal seams should be taken into consideration when applying acid stimulation to increase permeability due to that the acidification products may block the passage of gas migration when the mineral content is slight, which can hinder gas extraction. The aim of this study is to quantitatively determine the contribution rate of clay minerals in coal to methane adsorption with a calculation method is provided by combining pore parameters and limit adsorption capacity, resulting in a contribution rate of 15%.

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.

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.

Interfacial fracture toughness of different surface treatments on zirconia-reinforced lithium silicate glass-ceramics.

This study investigated the influence of different surface treatments on unfiring or firing zirconia-reinforced lithium silicate (ZLS) glass-ceramics. Celtra Duo and IPS e.max CAD blocks were cut and process following manufacturer protocols. The specimen surface was treated with seven different protocols. Two ceramic blocks with the same surface treatment were bonded with luting agent and prepared for mini-interfacial fracture toughness tests (mini-iFT). The specimens were tested after 1-week storage. The data was statistically analyzed using two-way ANOVA and Dunnett's T3 comparison (α=0.05). The highest mini-iFT of both Celtra Duo unfired and fired was shown in the HF+S group, which was not significantly different from HF+S+UA. For IPS e.max CAD, the mini-iFT was higher in the groups treated with hydrofluoric acid. Additional adhesive after silane application did not significantly improve bonding effectiveness. Therefore, surface treatment with hydrofluoric acid and silane is recommended for both unfiring and firing ZLS glass ceramics.

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.

Theoretical study on efficient HF gas sensing by functionalized, decorated, and doped nanocone strategy.

Hydrogen fluoride (HF) is a highly dangerous and corrosive gas that can cause severe burns and respiratory damage. The density functional theory method (DFT) used to study the interaction between the HF gas and the surface of a carbon nanocone (CNC) doped with gallium atom as a chemical sensor. The results showed that CNC wasn't a good candidate to sense the HF gas and consequently its electrical properties are changed insignificant. To improve the properties of the CNC, several strategies were tried: functionalizing by pyridinol (Pyr) and pyridinol oxide (PyrO), decorated with metals (M = B, Al, and Ga), and doped with element of third group (M = B, Al, and Ga). The obtained data demonstrated that the promising results were obtained by doping the CNC with Ga atom. After full optimization, we achieved one stable configuration between the HF gas and CNC-Ga structure (S15 configuration) with Eads = -19.86 kcal/mol. The electronic properties of the CNC-Ga structure is sensible changed after the HF molecule is adsorbed. According to calculated the energy gap between HOMO and LUMO orbitals of S15 configuration are increased which could be applied a chemical signal. Eventually, one could propose that the CNC-Ga has the ability to act as a Φ-type sensor based on its physical adsorption energy and quick recovery time and doped with gallium atom is a promising strategy.