de Carvalho Rodrigo Furtado, Cotes Caroline, Kimpara Estevão Tomomitsu, Leite Fabíola Pessoa Pereira, Özcan Mutlu
Department of Dentistry, Dental School, UFJF - Federal University of Juiz de Fora, Governador Valadares, MG, Brazil.
Department of Dental Materials and Prosthodontics, São José dos Campos Dental School, UNESP - Univ Estadual Paulista, São José dos Campos, SP, Brazil.
Braz Dent J. 2015 Jan-Feb;26(1):44-9. doi: 10.1590/0103-6440201300212.
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.
本研究评估了不同形式的热处理对预水解硅烷的影响，以改善基于磷酸盐单体（MDP）的树脂水门汀与玻璃陶瓷的粘结。将树脂块和长石质陶瓷块（n = 48，粘结测试n = 6，显微镜观察n = 2）随机分为6组并进行表面处理：G1：9.6%氢氟酸（HF）处理20 s + 硅烷 + MDP树脂水门汀（Panavia F）；G2：9.6% HF处理20 s + 硅烷 + 热处理（烘箱） + Panavia F；G3：硅烷 + 热处理（烘箱） + Panavia F；G4：9.6% HF处理20 s + 硅烷 + 热处理（热风） + Panavia F；G5：硅烷 + 热处理（热风） + Panavia F；G6：硅烷 + Panavia F。使用万能试验机（1 mm/min）进行微拉伸粘结强度（MTBS）测试。脱粘后，使用体视显微镜和扫描电子显微镜（SEM）分析基底和粘结表面，以对失效类型进行分类。数据采用双向方差分析和Tukey检验进行统计学分析（α = 0.05）。含MDP的硅烷在100℃烘箱中热处理2分钟或在50±5℃下热风处理1分钟后，再用HF预蚀刻（G2：13.15±0.89a；G4：12.58±1.03a），其粘结强度值显著高于对照组（G1：9.16±0.64b）。未进行预蚀刻的组（G3：10.47±0.70b；G5：9.47±0.32b）与对照组（G1）之间的粘结强度值在统计学上相似。未进行预蚀刻和热处理直接应用硅烷导致最低的平均粘结强度（G6：8.05±0.37c）。SEM分析显示主要为粘结失效，EDS分析显示了表征所研究玻璃陶瓷微观结构的常见光谱元素（Si、Na、Al、K、O、C）。含MDP的预水解硅烷在100℃烘箱中热处理2分钟或在50±5℃下热风处理1分钟，可有效提高陶瓷与含MDP的树脂水门汀之间的粘结强度值。
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