São Paulo State University, Department of Prosthodontics and Dental Materials, São José dos Campos, Brazil.
Dent Mater. 2012 Feb;28(2):189-96. doi: 10.1016/j.dental.2011.10.009. Epub 2011 Oct 27.
This study characterized the feldspathic ceramic surfaces after various silanization protocols.
Ceramic bars (2 mm × 4 mm × 10 mm) (N = 18) of feldpathic ceramic (VM7, VITA Zahnfabrik) were manufactured and finished. Before silane application, the specimens were ultrasonically cleaned in distilled water for 10 min. The ceramic specimens were randomly divided into nine groups (N = 2 per group) and were treated with different silane protocols. MPS silane (ESPE-Sil, 3M ESPE) was applied to all specimens and left to react at 20°C for 2 min (G20). After drying, the specimens were subjected to heat treatment in an oven at 38°C (G38), 79°C (G79) or 100°C (G100) for 1 min. Half of the specimens of each group were rinsed with water at 80°C for 15s (G20B, G38B, G79B, G100B). The control group (GC) received no silane. Attenuated total reflection infrared Fourier transform analysis (ATR FT-IR) was performed using a spectrometer. Thickness of silane layer was measured using a spectroscopic ellipsometer working in the λ = 632.8 nm (He-Ne laser) at 70° incidence angle. Surface roughness was evaluated using an optical profilometer. Specimens were further analyzed under the Scanning Electron Microscopy (SEM) to observe the topographic patterns.
ATR FT-IR analysis showed changes in Si-O peaks with enlarged bands around 940 cm(-1). Ellipsometry measurements showed that all post-heat treatment actions reduced the silane film thickness (30.8-33.5 nm) compared to G20 (40 nm). The groups submitted to rinsing in hot water (B groups) showed thinner silane films (9.8-14.4 nm) than those of their corresponding groups (without washing) (30.8-40 nm). Profilometer analysis showed that heat treatments (Ra ≈ 0.10-0.19 μm; Rq ≈ 0.15-0.26 μm) provided a smoother surface than the control group (Ra ≈ 0.48 μm; Rq ≈ 0.65 μm). Similar patterns were also observed in SEM images.
Heat treatment after MPS silane application improved the silane layer network. Rinsing with boiling water eliminated the outmost unreacted regions of the silane yielding to thinner film thicknesses.
本研究对不同硅烷化方案处理后的长石陶瓷表面进行了表征。
制备并加工长石陶瓷（VM7，VITA Zahnfabrik）的陶瓷棒（2mm×4mm×10mm）（N=18）。在进行硅烷处理之前，将样品在去离子水中用超声清洗 10 分钟。将陶瓷样品随机分为 9 组（每组 2 个样品），并采用不同的硅烷处理方案进行处理。所有样品均应用 MPS 硅烷（ESPE-Sil，3M ESPE），在 20°C 下反应 2 分钟（G20）。干燥后，将样品在 38°C（G38）、79°C（G79）或 100°C（G100）的烘箱中加热处理 1 分钟。每组的一半样品在 80°C 的水中冲洗 15 秒（G20B、G38B、G79B、G100B）。对照组（GC）未进行硅烷处理。使用光谱仪进行衰减全反射红外傅里叶变换分析（ATR FT-IR）。使用λ=632.8nm（氦氖激光）、70°入射角的光谱椭圆偏振仪测量硅烷层的厚度。使用光学轮廓仪评估表面粗糙度。使用扫描电子显微镜（SEM）进一步分析样品，观察形貌图案。
ATR FT-IR 分析表明 Si-O 峰发生变化，940cm(-1)左右的峰带增大。椭圆光度测量表明，所有后热处理操作都降低了硅烷膜厚度（30.8-33.5nm），而 G20 组为 40nm。在热水中冲洗的（B）组显示出比相应组（未冲洗）更薄的硅烷膜（9.8-14.4nm）（30.8-40nm）。轮廓仪分析表明，热处理（Ra≈0.10-0.19μm；Rq≈0.15-0.26μm）提供的表面比对照组（Ra≈0.48μm；Rq≈0.65μm）更光滑。SEM 图像也显示出类似的模式。
MPS 硅烷处理后进行热处理可改善硅烷层网络。用沸水冲洗可去除硅烷的最外层未反应区，从而获得更薄的膜厚。
