Department of Biomaterials, School of Dentistry, National and Kapodistrian University of Athens, Greece.
Biomaterials Unit, Dentistry, School of Medical Sciences, University of Manchester, UK.
Dent Mater. 2019 Aug;35(8):1082-1094. doi: 10.1016/j.dental.2019.05.002. Epub 2019 Jun 4.
To evaluate the silane status in commercially available products and their bonding capacity with polished glass-ceramic surfaces before and after hydrofluoric (HF) acid-etching.
The products tested were Calibra Silane Coupling Agent/CS, G-Multi Primer/GM, Kerr Silane Primer/KS, Monobond Plus/MB and Scotchbond Universal Adhesive/SB. The silane status was studied by C nuclear magnetic resonance spectroscopy (C-NMR). The roughness parameters of polished (group A) and HF acid-etched (group B) lithium disilicate glass-ceramic surfaces were measured by optical profilometry (n = 5/group). The interaction of the products with group A and B ceramic surfaces was examined by attenuated total reflection Fourier transform infrared spectroscopy (ATR-FTIR). The shear strength (SBS) of a flowable composite bonded to the ceramic surfaces (groups A, B) was assessed before (NS) and after silane treatment (n = 20/group, product).
The NMR analysis showed the presence of silanol monomers only in CS. Methoxylated-siloxane adducts were found in GM, silanol-siloxane adducts in MB, SB, and siloxane polymers in KS. Acid-etching greatly increased Sa, Sz, Sdr, Sc and Sv parameters (p < 0.001) and ATR-FTIR analysis demonstrated evidence of bonding with the substrate in CS. Weibull analysis of SBS revealed the following rankings in characteristic life (p < 0.05): CS > SB,KS,MB > GM > NS (group A) and CS > GM > SB,KS,MB,NS (group B). The most reliable treatment in both groups was CS. For the same silane treatment, the SBS of group B were significantly higher from group A. Failures were mainly of adhesive type, except of several partial resin cohesive failures found in group B.
The chemical bonding capacity of the silanes was highest in products with silanol monomers. Acid-etching increased bond strength to a level that neutralized the silane contribution in products with silanol-siloxane adducts and siloxane polymers, providing thus bond strength values similar to silane-free treatments.
评估市售产品中的硅烷状态及其在经过氢氟酸（HF）酸蚀前后与抛光玻璃陶瓷表面的结合能力。
测试的产品有 Calibra Silane Coupling Agent/CS、G-Multi Primer/GM、Kerr Silane Primer/KS、Monobond Plus/MB 和 Scotchbond Universal Adhesive/SB。通过 C 核磁共振光谱（C-NMR）研究硅烷状态。通过光学轮廓仪测量抛光（A 组）和 HF 酸蚀（B 组）锂硅玻璃陶瓷表面的粗糙度参数（n=5/组）。通过衰减全反射傅里叶变换红外光谱（ATR-FTIR）检查产品与陶瓷表面（A、B 组）的相互作用。在未处理（NS）和硅烷处理后（n=20/组，产品），评估可流动复合材料与陶瓷表面（A、B 组）的粘结剪切强度（SBS）。
NMR 分析显示 CS 中仅存在硅醇单体。GM 中发现甲氧基硅氧烷加合物，MB、SB 和 KS 中发现硅醇硅氧烷加合物，KS 中发现硅氧烷聚合物。酸蚀极大地增加了 Sa、Sz、Sdr、Sc 和 Sv 参数（p<0.001），ATR-FTIR 分析表明 CS 与基底有粘结证据。SBS 的威布尔分析显示特征寿命的以下等级（p<0.05）：CS>SB、KS、MB>GM>NS（A 组）和 CS>GM>SB、KS、MB、NS（B 组）。在两组中最可靠的处理都是 CS。对于相同的硅烷处理，B 组的 SBS 明显高于 A 组。失效主要是黏附型，除了 B 组中发现的几个部分树脂内聚失效。
具有硅醇单体的产品中的硅烷化学结合能力最高。酸蚀提高了粘结强度，使具有硅醇硅氧烷加合物和硅氧烷聚合物的产品中的硅烷贡献中和，从而提供与无硅烷处理相似的粘结强度值。
