Effect of Hydrofluoric Acid Concentration and Etching Time on Bond Strength to Lithium Disilicate Glass Ceramic

2017 ◽  
Vol 42 (6) ◽  
pp. 606-615 ◽  
Author(s):  
J Puppin-Rontani ◽  
D Sundfeld ◽  
AR Costa ◽  
AB Correr ◽  
RM Puppin-Rontani ◽  
...  

SUMMARY The aim of this study was to evaluate the influence of different concentrations of hydrofluoric acid (HF) associated with varied etching times on the microshear bond strength (μSBS) of a resin cement to a lithium disilicate glass ceramic. Two hundred seventy-five ceramic blocks (IPS e.max Press [EMX], Ivoclar Vivadent), measuring 8 mm × 3 mm thickness, were randomly distributed into five groups according to the HF concentrations (n=50): 1%, 2.5%, 5%, 7.5%, and 10%. Further random distribution into subgroups was performed according to the following etching times (n=10): 20, 40, 60, 120, and 20 + 20 seconds. After etching, all blocks were treated with a silane coupling agent followed by a thin layer of an unfilled resin. Three resin cement cylinders (∅︀=1 mm) were made on each EMX surface, which was then stored in deionized water at 37°C for 24 hours before testing. The μSBS was in a universal testing machine at a crosshead speed of 1 mm/min until failure. Data were submitted to two-way analysis of variance, and multiple comparisons were performed using the Tukey post hoc test (α=0.05). One representative EMX sample was etched according to the description of each subgroup and evaluated using scanning electron microscopy for surface characterization. The HF concentrations of 5%, 7.5%, and 10% provided significantly higher μSBS values than 1% and 2.5% (p<0.05), regardless of the etching times. For 1% and 2.5% HF, the etching times from 40 to 120 seconds increased the μSBS values compared with 20 seconds (p<0.05), but etching periods did not differ within the 5%, 7.5%, and 10% HF groups (p>0.05). The effect of re-etching was more evident for 1% and 2.5% HF (p<0.05). Different HF concentrations/etching times directly influenced the bond strength and surface morphology of EMX.

2016 ◽  
Vol 27 (6) ◽  
pp. 727-733 ◽  
Author(s):  
Daniel Sundfeld ◽  
Lourenço Correr-Sobrinho ◽  
Núbia Inocêncya Pavesi Pini ◽  
Ana Rosa Costa ◽  
Renato Herman Sundfeld ◽  
...  

Abstract The aim of this study was to evaluate the effects of hydrofluoric acid (HF) concentration and previous heat treatment (PHT) on the surface morphology and micro-shear bond strength (mSBS) of a lithium disilicate glass ceramic (EMX) to resin cement. One hundred four EMX specimens were randomly assigned to two groups (n=52) according to the HF concentration: 5% and 10%. A new random distribution was made according to the PHTs (n=13): control (no PHT); previously heated HF (70 °C); previously heated EMX surface (85 °C); the combination of heated HF + heated EMX surface. The etching time was set at 20 s. All EMX blocks were silanated and received a thin layer of an unfilled resin. Five resin cement cylinders were made on each EMX surface using Tygon tubes as matrices, and then stored for 24 h at 37 °C. One random etched EMX sample from each group was analyzed using field-emission scanning electron microscopy (FE-SEM). The data were subjected to two-way ANOVA and multiple comparisons were performed using the Tukey post hoc test (a=0.05). For the control groups, 5% HF showed statistically lower mSBS values when compared to 10% HF (p<0.05). PHT increased the mSBS values for 5% HF, yielding statistically similar results to non-PHT 10% HF (p<0.05). FE-SEM images showed increased glassy matrix removal when PHT was applied to HF 5%, but not to the same degree as for 10% HF. PHT has the potential to improve the bond strength of 5% HF concentration on lithium disilicate glass ceramic.


2013 ◽  
Vol 38 (2) ◽  
pp. 208-217 ◽  
Author(s):  
GB Guarda ◽  
AB Correr ◽  
LS Gonçalves ◽  
AR Costa ◽  
GA Borges ◽  
...  

SUMMARY Objectives The aim of this present study was to investigate the effect of two surface treatments, fatigue and thermocycling, on the microtensile bond strength of a newly introduced lithium disilicate glass ceramic (IPS e.max Press, Ivoclar Vivadent) and a dual-cured resin cement. Methods A total of 18 ceramic blocks (10 mm long × 7 mm wide × 3.0 mm thick) were fabricated and divided into six groups (n=3): groups 1, 2, and 3—air particle abraded for five seconds with 50-μm aluminum oxide particles; groups 4, 5, and 6—acid etched with 10% hydrofluoric acid for 20 seconds. A silane coupling agent was applied onto all specimens and allowed to dry for five seconds, and the ceramic blocks were bonded to a block of composite Tetric N-Ceram (Ivoclar Vivadent) with RelyX ARC (3M ESPE) resin cement and placed under a 500-g static load for two minutes. The cement excess was removed with a disposable microbrush, and four periods of light activation for 40 seconds each were performed at right angles using an LED curing unit (UltraLume LED 5, Ultradent) with a final 40 second light exposure from the top surface. All of the specimens were stored in distilled water at 37°C for 24 hours. Groups 2 and 5 were submitted to 3,000 thermal cycles between 5°C and 55°C, and groups 3 and 6 were submitted to a fatigue test of 100,000 cycles at 2 Hz. Specimens were sectioned perpendicular to the bonding area to obtain beams with a cross-sectional area of 1 mm2 (30 beams per group) and submitted to a microtensile bond strength test in a testing machine (EZ Test) at a crosshead speed of 0.5 mm/min. Data were submitted to analysis of variance and Tukey post hoc test (p≤0.05). Results The microtensile bond strength values (MPa) were 26.9 ± 6.9, 22.2 ± 7.8, and 21.2 ± 9.1 for groups 1–3 and 35.0 ± 9.6, 24.3 ± 8.9, and 23.9 ± 6.3 for groups 4–6. For the control group, fatigue testing and thermocycling produced a predominance of adhesive failures. Fatigue and thermocycling significantly decreased the microtensile bond strength for both ceramic surface treatments when compared with the control groups. Etching with 10% hydrofluoric acid significantly increased the microtensile bond strength for the control group.


2018 ◽  
Vol 29 (5) ◽  
pp. 492-499 ◽  
Author(s):  
Catina Prochnow ◽  
Andressa Borin Venturini ◽  
Rafaella Grasel ◽  
André Gundel ◽  
Marco Cícero Bottino ◽  
...  

Abstract This study evaluated the effect of different hydrofluoric acid (HF) concentrations on the bond strength between a lithium disilicate-based glass ceramic and a resin cement. Eighty ceramic-blocks (12×7×2 mm) of IPS e.Max CAD (Ivoclar Vivadent) were produced and randomly assigned to 8 groups, considering 2 study factors: HF concentration in 4 levels, i.e., 1% (HF1), 3% (HF3), 5% (HF5), and 10% (HF10), and storage in 2 levels, i.e., baseline (tests were performed 24 h after cementation), and aged (storage for 150 days + 12,000 thermal-cycles at 5°C and 55°C). Acid etching (20 s) was performed, followed by washing, drying, and silanization. Four resin cement cylinders (ϕ= 0.96 mm) were built-up from starch matrices on each ceramic sample (n= 40). Additional ceramic samples were etched and analyzed for contact angle, micro-morphology, and roughness. In baseline condition (without aging), the HF3, HF5, and HF10 groups showed similar bond strength values (13.9 - 15.9 MPa), and HF1 (11.2 MPa) presented lower values than HF5, being that statistically different (p= 0.012). After aging, all the mean bond strengths statistically decreased, being that HF3, HF5, and HF10 (7.8 - 11 MPa) were similar and higher than HF1 (1.8 MPa) (p= 0.0001). For contact angle, HF3, HF5, and HF10 presented similar values (7.8 - 10.4°), lower than HF1 and CTRL groups. HF5 and HF10 presented rougher surfaces than other conditions. For better bond strength results, the tested ceramic may be etched by HF acid in concentrations of 3%, 5%, and 10%.


2021 ◽  
Vol 2021 ◽  
pp. 1-7
Author(s):  
Amjad Abu Hasna ◽  
Stephanie Semmelmann ◽  
Fernanda Alves Feitosa ◽  
Danilo De Souza Andrade ◽  
Franklin R Tay ◽  
...  

This study evaluated the effect of different surface treatments on the tensile bond strength between lithium disilicate glass-ceramics, resin cement, and dentin. Fifty truncated cone-shape glass-ceramics were divided into five groups (n = 10): G1, control: 10% hydrofluoric acid (HF); G2, Nd:YAG laser + silane; G3, Sil + Nd:YAG laser; G4, graphite + Nd:YAG laser + Sil; and G5, graphite + Sil + Nd:YAG laser. Fifty human third-molars were cut to cylindrical shape and polished to standardize the bonding surfaces. The glass-ceramic specimens were bonded to dentin with a dual-cured resin cement and stored in distilled water for 24 h at 37ºC. Tensile testing was performed on a universal testing machine (10 Kgf load cell at 1 mm/min) until failure. The bond strength values (mean ± SD) in MPa were G1 (9.4 ± 2.3), G2 (9.7 ± 2.0), G3 (6.7 ± 1.9), G4 (4.6 ± 1.1), and G5 (1.2 ± 0.3). Nd:YAG laser and HF improve the bond strength between lithium disilicate glass-ceramics, resin cement, and dentin. The application of a graphite layer prior to Nd:YAG laser irradiation negatively affects this bonding and presented inferior results.


2016 ◽  
Vol 17 (2) ◽  
pp. 149-153 ◽  
Author(s):  
Cristina Parise Gré ◽  
Renan C de Ré Silveira ◽  
Shizuma Shibata ◽  
Carlo TR Lago ◽  
Luiz CC Vieira

ABSTRACT Aim This study evaluated the influence of a silane-coupling agent on the bond strength of a self-adhesive cement and a conventional resin cement to a lithium disilicate glass ceramic. Materials and methods A total of eight ceramic blocks were fabricated and divided into four groups (n = 2). In groups 1 and 3, ceramic surfaces were etched with hydrofluoric acid 10% for 20 seconds, rinsed for 30 seconds, and air-dried. One layer of a silane agent was applied onto all ceramic specimens and air-dried for 30 seconds. In groups 2 and 4, ceramic surfaces were etched with hydrofluoric acid, rinsed, and air-dried without application of the silane-coupling agent. The ceramic blocks were bonded to a block of composite with a self-adhesive resin cement or with a conventional resin cement, according to the manufacturer's instructions. After 24 hours in distilled water at 37°C, the specimens were sectioned perpendicular to the bonding interface area to obtain beams with a bonding area of 0.8 mm2 and submitted to a microtensile bond strength test at a crosshead speed of 0.5 mm/min. Data were statistically analyzed with one-way analysis of variance and the Games–Howell post hoc test (p = 0.05). Fractured specimens were examined under optical microscopy at 40× magnification. Results Silanization resulted in higher microtensile bond strength compared to groups without silane. No significant differences were found between the conventional resin cement and the self-adhesive resin cement with silane agent (p = 0.983), and without silane agent (p = 0.877). Conclusion Silanization appears to be crucial for resin bonding to a lithium disilicate-based ceramic, regardless of the resin cement used. The self-adhesive resin cement performed as well as the conventional resin cement. Clinical significance Applying one layer of a silane-coupling agent after etching the ceramic surface with hydrofluoric acid 10% enhanced the bond strength between resin cements and a glass ceramic. How to cite this article Gré CP, de Ré Silveira RC, Shibata S, Lago CTR, Vieira LCC. Effect of Silanization on Microtensile Bond Strength of Different Resin Cements to a Lithium Disilicate Glass Ceramic. J Contemp Dent Pract 2016;17(2):149-153.


2021 ◽  
Vol 24 (3) ◽  
Author(s):  
Amr El-Etreby ◽  
Osama AlShanti ◽  
Gihan El-Nagar

Objective: The present study aimed to evaluate the effect of repressing and different surface treatment protocols on the shear bond strength of lithium disilicate glass-ceramics. Material and Methods: A total of 52 lithium disilicate glass-ceramic discs (IPS emax Press, Ivoclar Vivadent) were fabricated using the heat-press technique. The discs were divided into two groups; group (P): discs fabricated from new e.max ingots (n=26), group (R): discs fabricated from reused e.max buttons (n=26). Each group was subdivided into subgroup (E): discs were etched with hydrofluoric acid (9.5%) (n=13), subgroup (S): discs were air-abraded with 110 µm alumina particles. All specimens were subjected to X-ray Diffraction analysis, Scanning Electron Microscope, Energy Dispersive X-Ray, Thermo-Cycling, and Shear Bond Strength Testing. Results: Repressed Etched subgroup (RE) recorded the statistically highest shear bond strength value, followed by the Pressed Etched subgroup (PE), while the statistically lowest shear bond strength value was recorded for the Pressed Air-Abraded subgroup (PS) and Repressed Air-Abraded subgroup (RS). Conclusion: Repressing the leftover buttons for the construction of new lithium disilicate glass-ceramic restorations has no adverse effect on the bond strength of the resin cement to the ceramic. Hydrofluoric acid surface treatment improves the shear bond strength and durability of resin cement bond to both pressed and repressed lithium disilicate glass-ceramic. Air-abrasion cannot be considered as a reliable surface treatment when bonding to lithium disilicate glass-ceramics. Keywords Heat pressed; Lithium disilicate glass-ceramics; Repressing; Shear bond strength; Surface treatment.


2015 ◽  
Vol 26 (1) ◽  
pp. 44-49 ◽  
Author(s):  
Rodrigo Furtado de Carvalho ◽  
Caroline Cotes ◽  
Estevão Tomomitsu Kimpara ◽  
Fabíola Pessoa Pereira Leite

This study evaluated the influence of different forms of heat treatment on a pre-hydrolyzed silane to improve the adhesion of phosphate monomer-based (MDP) resin cement to glass ceramic. Resin and feldspathic ceramic blocks (n=48, n=6 for bond test, n=2 for microscopy) were randomly divided into 6 groups and subject to surface treatments: G1: Hydrofluoric acid (HF) 9.6% for 20 s + Silane + MDP resin cement (Panavia F); G2: HF 9.6% for 20 s + Silane + Heat Treatment (oven) + Panavia F; G3: Silane + Heat Treatment (oven) + Panavia F; G4: HF 9.6% for 20 s + Silane + Heat Treatment (hot air) + Panavia F; G5: Silane + Heat Treatment (hot air) + Panavia F; G6: Silane + Panavia F. Microtensile bond strength (MTBS) test was performed using a universal testing machine (1 mm/min). After debonding, the substrate and adherent surfaces were analyzed using stereomicroscope and scanning electron microscope (SEM) to categorize the failure types. Data were analyzed statistically using two-way test ANOVA and Tukey's test (=0.05). Heat treatment of the silane containing MDP, with prior etching with HF (G2: 13.15±0.89a; G4: 12.58±1.03a) presented significantly higher bond strength values than the control group (G1: 9.16±0.64b). The groups without prior etching (G3: 10.47±0.70b; G5: 9.47±0.32b) showed statistically similar bond strength values between them and the control group (G1). The silane application without prior etching and heat treatment resulted in the lowest mean bond strength (G6: 8.05±0.37c). SEM analysis showed predominantly adhesive failures and EDS analysis showed common elements of spectra (Si, Na, Al, K, O, C) characterizing the microstructure of the glass-ceramic studied. Heat treatment of the pre-hydrolyzed silane containing MDP in an oven at 100 °C for 2 min or with hot air application at 50±5 ºC for 1 min, was effective in increasing the bond strength values between the ceramic and resin cement containing MDP.


2015 ◽  
Vol 40 (5) ◽  
pp. 470-479 ◽  
Author(s):  
D Sundfeld Neto ◽  
LZ Naves ◽  
AR Costa ◽  
AB Correr ◽  
S Consani ◽  
...  

SUMMARY The purpose of this study was to evaluate the influence of various concentrations of hydrofluoric acid (HF) on the surface/interface morphology and μ–shear bond strength (μSBS) between IPS Empress Esthetic (EST) (Ivoclar Vivadent) and IPS e.max Press (EMX) (Ivoclar Vivadent) ceramics and resin cement. Ceramic blocks were divided into 12 groups for each kind of ceramic. Six different HF concentrations were evaluated: 1%, 2.5%, 5%, 7.5%, 10%, and 15%. All groups were silanated after etching, and half of the specimens within each group received a thin layer of unfilled resin (UR). Three resin cement cylinders were prepared on each ceramic block for μSBS testing. The specimens were stored in distilled water at 37°C for 24 hours. The μSBS test was carried out in a universal testing machine at a crosshead speed of 0.5 mm/min until fracture. The data were submitted to three-way analysis of variance and multiple comparisons were performed using the Tukey post hoc test (p&lt;0.05). The etched surfaces and bonded interfaces were evaluated using scanning electron microscopy. μSBS means (MPa) for 1%, 2.5%, 5%, 7.5%, 10%, and 15% HF concentrations were, respectively, 25.2, 27.2, 30.1, 31.4, 33.3, and 31.8. μSBS means with or without UR application measured 32.24 and 27.4, respectively; EST and EMX measured 29.8 and 29.9, respectively. For the HF concentrations, 10% and 15% showed higher μSBS means than did 1% and 2.5% (p&lt;0.05); 7.5% was higher than 1% (p&lt;0.05); and no statistical differences were found among the other concentrations (p&gt;0.05). When evaluating UR, μSBS mean was significantly higher and better infiltration was observed on the etched surfaces. No statistical difference was found between the ceramics. The HF concentration and UR influenced the bond strength and surface/interface morphology.


Author(s):  
Siripan Simasetha ◽  
Awiruth Klaisiri ◽  
Tool Sriamporn ◽  
Kraisorn Sappayatosok ◽  
Niyom Thamrongananskul

Abstract Objective The study aimed to evaluate the shear bond strength (SBS) of lithium disilicate glass-ceramic (LDGC) and resin cement (RC) using different surface treatments. Materials and Methods LDGC blocks (Vintage LD Press) were prepared, etched with 4.5% hydrofluoric acid, and randomly divided into seven groups (n = 10), depending on the surface treatments. The groups were divided as follows: 1) no surface treatment (control), 2) Silane Primer (KS), 3) Signum Ceramic Bond I (SGI), 4) Signum Ceramic Bond I/Signum Ceramic Bond II (SGI/SGII), 5) experimental silane (EXP), 6) experimental silane/Signum Ceramic Bond II (EXP/SGII), and 7) Experimental/Adper Scotchbond Multi-purpose Adhesive (EXP/ADP). The specimens were cemented to resin composite blocks with resin cement and stored in water at 37 °C for 24 hours. The specimens underwent 5,000 thermal cycles and were subjected to the SBS test. Mode of failure was evaluated under the stereo microscope. Statistical Analysis Data were analyzed with Welch ANOVA and Games-Howell post hoc tests (α = 0.05). Results The highest mean SBS showed in group EXP/ADP (45.49 ± 3.37 MPa); however, this was not significantly different from group EXP/SGII (41.38 ± 2.17 MPa) (p ≥ 0.05). The lowest SBS was shown in the control group (18.36 ± 0.69 MPa). This was not significantly different from group KS (20.17 ± 1.10 MPa) (p ≥ 0.05). Conclusions The different surface treatments significantly affected the SBS value between LDGC and RC. The application of pure silane coupling agent with or without the application of an adhesive improved the SBS value and bond quality.


2019 ◽  
Vol 44 (5) ◽  
pp. 545-555 ◽  
Author(s):  
EV Maroun ◽  
JGA Guimarães ◽  
WG de Miranda ◽  
LRC Netto ◽  
AB Elias ◽  
...  

SUMMARY The purpose of this study was to evaluate the influence of thermomechanical cycling on the bond strength stability of self-adhesive resin cement to vitrified yttria-stabilized tetragonal zirconia polycrystal (Y-TZP) ceramic. Y-TZP ceramic blocks were divided into four groups according to the surface treatments: AS, as sintered; SB, sandblasted with 50-μm Al2O3 particles; LG, vitrification with a low-fusing glaze and etching with 10% hydrofluoric acid; and HC, vitrification with a ceramic liner and etching with 10% hydrofluoric acid. Lithium disilicate ceramic blocks etched with 10% hydrofluoric acid for 20 seconds (EM) were also tested. Blocks of resin composite were cemented on the ceramic block surfaces using a self-adhesive resin cement. Half of the blocks from each group were cut into beams and submitted to microtensile bond strength (μTBS) testing after immersion in water at 37°C for 24 hours and the other half after mechanical (1,200,000 cycles, 98 N, 2.5 Hz) and thermal (10,000 cycles, 5-55°C, 30-second dwell time) cycling (TMC). Data were analyzed using one-way analysis of variance, Tukey's honest significant difference post hoc test, and Student t-test (α=0.05). After 24 hours, EM and LG presented similar and the highest μTBS, whereas AS showed the lowest μTBS (p&lt;0.05). After TMC, EM presented the highest μTBS, followed by LG (p&lt;0.05). Only EM and LG maintained the stability of μTBS after TMC (p&gt;0.05). The bonding to Y-TZP ceramic vitrified with a low-fusing glaze withstood thermomechanical cycling.


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