Effect of composite surface treatment and aging on the bond strength between a core build-up composite and a luting agent

Objective The purpose of this study was to assess the influence of conditioning methods and thermocycling on the bond strength between composite core and resin cement. Material and Methods Eighty blocks (8×8×4 mm) were prepared with core build-up composite. The cementation surface was roughened with 120-grit carbide paper and the blocks were thermocycled (5,000 cycles, between 5°C and 55°C, with a 30 s dwell time in each bath). A layer of temporary luting agent was applied. After 24 h, the layer was removed, and the blocks were divided into five groups, according to surface treatment: (NT) No treatment (control); (SP) Grinding with 120-grit carbide paper; (AC) Etching with 37% phosphoric acid; (SC) Sandblasting with 30 mm SiO2 particles, silane application; (AO) Sandblasting with 50 mm Al2O3 particles, silane application. Two composite blocks were cemented to each other (n=8) and sectioned into sticks. Half of the specimens from each block were immediately tested for microtensile bond strength (µTBS), while the other half was subjected to storage for 6 months, thermocycling (12,000 cycles, between 5°C and 55°C, with a dwell time of 30 s in each bath) and µTBS test in a mechanical testing machine. Bond strength data were analyzed by repeated measures two-way ANOVA and Tukey test (α=0.05). Results The µTBS was significantly affected by surface treatment (p=0.007) and thermocycling (p=0.000). Before aging, the SP group presented higher bond strength when compared to NT and AC groups, whereas all the other groups were statistically similar. After aging, all the groups were statistically similar. SP submitted to thermocycling showed lower bond strength than SP without thermocycling. Conclusion Core composites should be roughened with a diamond bur before the luting process. Thermocycling tends to reduce the bond strength between composite and resin cement. .

Heat Treatment of Pre-hydrolyzed Silane Increases Adhesion of Phosphate Monomer-based Resin Cement to Glass Ceramic

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.

Este estudo avaliou o efeito de diferentes formas de tratamento térmico de um silano pré-hidrolisado na adesão de um cimento resinoso à base de monómeros fosfatados (MDP) à uma cerâmica vítrea. Blocos em resina e cerâmica feldspática (n=48, n=6 para teste de união, n=2 para microscopia) foram divididos aleatoriamente em 4 grupos e submetidos a tratamentos de superfície: G1-ácido fluorídrico (HF) 9,6% por 20 s + Silano + cimento resinoso com MDP (Panavia F) ; G2-HF 9,6% por 20 s + Silano + Tratamento Térmico (forno) + Panavia F; G3-Silano + Tratamento Térmico (forno) + Panavia F; G4-HF 9,6% por 20 s + Silano + Tratamento Térmico (ar quente) + Panavia F; G5-Silano + Tratamento Térmico (ar quente) + Panavia F; G6-Silano + Panavia F. Teste de microtração (MTBS) foi realizado utilizando máquina de ensaios universal (1 mm/min). Após o descolamento, substrato e superfícies aderentes foram analisadas utilizando estereoscópico e microscópio eletrônica de varredura (MEV) para classificação dos tipos de falha. Os dados foram analisados estatisticamente utilizando o teste ANOVA dois fatores e o teste de Tukey (=0,05). O tratamento térmico do silano contendo MDP, com condicionamento prévio com HF (G2:13,15±0,89a e G4:12,58±1,03a) resultou em valores de resistência de união significativamente superiores aos do grupo controle (G1:9,16±0,64b). Os grupos sem condicionamento prévio (G3:10,47±0,70b e G5:9,47±0,32b), apresentaram valores de resistência de união estatisticamente semelhantes entre eles e ao controle (G1). O silano utilizado sem condicionamento prévio e tratamento térmico apresentou os menores valores de resistência de união (G6:8,05±0,37c). As análises em MEV mostraram predominância de falhas adesivas e as análises em EDS demonstraram espectros com elementos semelhantes (Si, Na, Al, K, O, C) caracterizando a microsestrutura da vitro-cerâmica estudada. O tratamento térmico do silano pré-hidrolisado contendo MDP, realizado em forno a 100 °C durante 2 min ou com ar quente a 50±5 °C durante 1 min, foi eficaz no aumento dos valores de união entre cimento resinoso contendo MDP e cerâmica.

May the flexural strength of ceramics be influenced by salivary pH? / A resistência à flexão de cerâmicas pode ser influenciada pelo pH salivar?

Objective: This study purpose was to compare the three-point flexural strength of feldspathic ceramic after storage in artificial saliva for 30 days with different pH regimens, as acidic pH (3.5), neutral pH (7.0), basic pH (10) and alternating between acid/ basic pH, for 15 days each. Material and Methods: The bars were luted with resin cement and subjected to storage in artificial saliva of different pH values. Results: The values of flexural strength were significantly higher for bars stored in distilled water, at neutral and basic pH, when compared with the results for bars stored in acidic pH and in acid/basic pH. Conclusions: Storage for 30 days in artificial saliva at acidic pH, or alternating between acidic and basic pH, can reduce the mechanical properties of ceramics.

Objetivo: O objetivo do estudo foi comparar a resistência à flexão três pontos de uma cerâmica feldspática após armazenagem em saliva artificial, durante 30 dias com diferentes regimes de pH: pH ácido (3,5), pH neutro (7,0), pH básico (10) e alternando entre pH ácido/básico durante 15 dias cada. Material e Métodos: As barras foram cimentados com cimento resinoso e submetidas a armazenagem em saliva artificial com os diferentes valores de pH. Resultados: Os valores de resistência à flexão foram significativamente maiores para as barras armazenadas em água destilada, em pH neutro e em básico, quando comparadas com os resultados para as barras armazenadas em pH ácido e em meio ácido/básico. Conclusões: A armazenamento durante 30 dias em saliva artificial, com pH ácido, ou alternando entre pH ácido e basico, pode reduzir as propriedades mecânicas das cerâmicas