Abstract The objective of this study was to evaluate the influence of hydrofluoric acid (HF) concentration, etching time, and application of phosphoric acid (PA) followed by neutralization with sodium bicarbonate on the bond strength between a feldspar ceramic and resin cement. Thus, 80 blocks (10 x 12 x 2 mm) of glass ceramic (VM - Vita Mark II - Vita Zahnfabrik) were made and randomly assigned to eight groups (n = 10) according to the factors: HF concentration (5 and 10%), etching time (60 and 120 s), and use of phosphoric acid (PA) (with and without). According to the experimental group, 37% PA (Condac, FGM) was applied after HF etching for 60s. Afterwards, samples were immersed in sodium bicarbonate for 1 min then in an ultrasonic bath in distilled water (5 min) for cleaning. After surface bonding treatment, cylinders (Ø = 2 mm; h = 2 mm) of dual resin cement (AllCem / FGM) were made in the center of each block. The samples were then stored in water (37ºC) for 90 days and submitted to the shear bond test (50 KgF, 1 mm/min). Failure analysis was performed by stereomicroscope and scanning electron microscopy. Data (MPa) were analyzed with 3-way ANOVA and Tukey’s test. Only the factor “HF concentration” was significant (p = 0.02). Most failures were of cohesive in ceramic (40%) and mixed types (42.5%). The 10% HF resulted in higher shear bond strength value than the 5% HF. Surface cleaning with phosphoric acid followed by sodium bicarbonate and HF time (60 or 120 seconds) did not influence the resin bond strength to feldspar ceramic.

Abstract: The objective of this study was to evaluate the effect of the hydrofluoridric acid (HF) concentration and time of acid conditioning on bond strength of three glass ceramics to a resin cement. Thus, fifty blocks (10 mm x 5 mm x 2 mm) of each ceramic (LDCAD: IPS e.max CAD; LCAD: IPS Empress CAD and LDHP: IPS e.max Press) were made and embedded in acrylic resin. The surfaces were polished with sandpaper (#600, 800, 1000, and 1200 grits) and blocks were randomly divided into 15 groups (n = 10) according to the following factors: Concentration of HF (10% and 5%), conditioning time (20 s and 60 s) and ceramic (LDCAD, LDHP, and L). After conditioning, silane (Prosil / FGM) was applied and after 2 min, cylinders (Ø = 2 mm; h = 2 mm) of dual resin cement (AllCem / FGM) were made in the center of each block using a Teflon strip as matrix and light cured for 40 s (1,200 mW/cm2). Then, the samples were thermocycled (10,000 cycles, 5/55°C, 30s) and submitted to the shear bond test (50 KgF, 0.5 mm/min). The data (MPa) were analyzed with 3-way ANOVA and Tukey's test (5%). Failure analysis was performed using a stereomicroscope (20x) and a scanning electron microscope (SEM). ANOVA revealed that the “concentration” factor (p = 0.01) and the interaction “acid concentration X ceramic” (p = 0.009) had a significant effect, however, the “ceramic” (p = 0.897) and “conditioning time” (p = 0.260) factors did not influence the results. The LDHP10%60s (10.98 MPa)aA* group presented significantly higher bond strength than LDHP10%20s (6.57 MPa)bA, LCAD5%20s (6,90 ±3,5)aB and LDHP5%60s (5.66 ± 2,9MPa)aA* groups (Tukey). Failure analysis revealed that 100% of specimens had mixed failure. In conclusion, etching with 5% HF for 20 seconds is recommended for lithium disilicate and leucite-reinforced CAD/CAM ceramics. However, for pressed lithium disilicate ceramic, 10% HF for 60 s showed significantly higher bond strength to resin cement.

Resumo Este estudo avaliou a efetividade de um adesivo “multi-mode” (Single Bond Universal/3M) como um substituto para a silicatização e aplicação do silano na resistência de união das cerâmicas de zircônia e um cimento resinoso. Para isso, 120 blocos cerâmicos sinterizados de zircônia nas dimensões de (5 x 5 x 5 mm) foram obtidos, lixados com lixas de granulação decrescente (#600, #800, #1000 e #1200) e divididos aleatoriamente em 12 grupos (n = 10), de acordo com os fatores “tratamento de superfície” (ScSi - silicatização + silanização; ScSBU - silicatização + Single Bond; SBU - SBU sem fotoativação e SBUp - SBU com fotoativação) e “cerâmica” (Lava/3M ESPE, Ceramill Zircônia/ Amann Girrbach e Zirkonzahn/Zirkonzahn). Posteriormente, cilindros de cimento resinoso dual (RelyX Ultimate/3M ESPE) foram confeccionados no centro de cada bloco com auxílio de uma matriz de silicone (Ø=2 mm; h=5 mm) e fotopolimerizados por 40 s (1200 mW/ cm²). Em seguida, as amostras foram armazenadas durante trinta dias em água destilada (37 °C) e submetidas ao ensaio de resistência de união ao cisalhamento (1 mm/min, 100 kgF). Os dados (MPa) foram analisados sob ANOVA (2 fatores) e teste de Tukey (5%). Análises complementares também foram realizadas. ANOVA revelou que apenas o fator “tratamento de superfície” foi significativo (p=0,0001). O tratamento ScSi (14.28A) promoveu valores de adesão estatisticamente superiores aos demais ScSBU (9.03B), SBU (8.47B) e SBUp (7.82B), os quais foram semelhantes entre si (Tukey). A Análise de falhas revelou que 100% da falhas que ocorreram foram mistas. A silicatização seguida da silanização promoveu a melhor resistência de união entre cimento resinoso e a cerâmica, independentemente do tipo da cerâmica ou do SBU.

Abstract This study evaluated the effectiveness of a multi-mode adhesive (SBU-Scotch Bond Universal/3M) as a substitute for silica coating and silane application on the bonding of zirconia ceramics to resin cement. One-hundred and twenty sintered zirconia ceramic blocks (5 x 5 x 5 mm) were obtained, finished by grounding with silicon carbide paper (#600, #800, #1000 and #1200) and randomly divided into 12 groups (n=10) in accordance with the factors “surface treatment” (ScSi - silicatization + silanization; ScSBU - silicatization + SBU; SBU - SBU without photoactivation and SBUp - SBU photoactivated) and “ceramic” (Lava / 3M ESPE, Ceramill Zirconia / Amann Girrbach and Zirkonzahn / Zirkonzahn). Dual resin cement cylinders (RelyX Ultimate/3M ESPE) were subsequently produced in the center of each block using a silicon matrix (Ø=2 mm, h=5 mm) and photoactivated for 40 s (1200 mW/cm2). The samples were stored for 30 days in distilled water (37ºC) and submitted to shear bond strength test (1 mm/min, 100 KgF). Data (MPa) were analyzed under ANOVA (2 levels) and Tukey test (5%). Complementary analyzes were also performed. ANOVA revealed that only the factor “surface treatment” was significant (p=0.0001). The ScSi treatment (14.28A) promoted statistically higher bond strength values than the other ScSBU (9.03B), SBU (8.47B) and SBUp (7.82B), which were similar to each other (Tukey). Failure analysis revealed that 100% of the failures were mixed. The silica coating followed by the silanization promoted higher bond strength values of resin cement and ceramic, regardless of the zirconia ceramic or SBU.