氢氟酸质量分数对二硅酸锂玻璃陶瓷表面形貌及树脂粘接的影响

目的 探讨不同质量分数的氢氟酸对二硅酸锂玻璃陶瓷表面形貌及树脂粘接耐久性的影响。方法 制备大小为11 mm×13 mm×2 mm的二硅酸锂玻璃陶瓷片试件72个,经烧结、研磨、清洗后,随机分为3组,每组24个,分别接受质量分数为32%的磷酸、4%的氢氟酸、9.5%的氢氟酸处理20 s,形成酸蚀后试件。每组随机选出4个陶瓷片,1个使用扫描电子显微镜观察陶瓷表面形态,另外3个用表面粗糙度仪测量陶瓷片表面粗糙度参数（Ra、Rz和Rmax）。陶瓷片表面接受硅烷偶联剂/树脂粘接剂/树脂水门汀处理,并与直径3 mm的复合树脂柱粘接形成粘接试件。将每组20个粘接试件分为两组,10个试件直接进行剪切实验,10个试件经20 000次冷热循环后进行剪切实验。结果 氢氟酸处理组试件表面粗糙度参数值均显著高于磷酸处理组;9.5%氢氟酸组除Ra以外的参数值均高于4%氢氟酸组（P<0.05）。冷热循环明显降低了所有实验组的粘接强度（P<0.05）。冷热循环前后,氢氟酸处理组的粘接强度均高于磷酸处理组;尽管4%氢氟酸组的粘接强度高于9.5%氢氟酸组,但9.5%氢氟酸组在冷热循环过程中的粘接强度降低幅度要明显低于4%氢氟酸组（P<0.05）。结论 氢氟酸的质量分数对陶瓷表面形态及与树脂的粘接耐久性有明显影响,9.5%氢氟酸能更有效地保持二硅酸锂玻璃陶瓷的树脂粘接强度。

Effect of hydrofluoric acid concentration on the surface morphology and bonding effectiveness of lithium disilicate glass ceramics to resin composites

Objective This study aimed at determining the influence of hydrofluoric acid (HF) in varied concentrations on the surface morphology of lithium disilicate glass ceramics and bond durability between resin composites and post-treated lithium disilicate glass ceramics. Methods After being sintered, ground, and washed, 72 as-prepared specimens of lithium disilicate glass ceramics with dimensions of 11 mm×13 mm×2 mm were randomly divided into three groups. Each group was treated with acid solution 32% phosphoric acid (PA) or 4% or 9.5% HF] for 20 s. Then, four acidified specimens from each group were randomly selected. One of the specimens was used to observe the surface morphology using scanning electron microscopy, and the others were used to observe the surface roughness using a surface roughness meter (including Ra, Rz, and Rmax). After treatment with different acid solutions in each group, 20 samples were further treated with silane coupling agent/resin adhesive/resin cement (Monobond S/Multilink Primer A&B/Multilink N), followed by bonding to a composite resin column (Filtek? Z350) with a diameter of 3 mm. A total of 20 specimens in each group were randomly divided into two subgroups, which were used for measuring the microshear bond strength, with one of them subjected to cool-thermal cycle for 20 000 times. Results The surface roughness (Ra, Rz, and Rmax) of lithium disilicate glass ceramics treated with 4% or 9.5% HF was significantly higher than that of the ceramic treated with PA (P<0.05). The lithium disilicate glass ceramics treated with 9.5% HF also demonstrated better surface roughness (Rz and Rmax) than that of the ceramics treated with 4% HF. Cool-thermal cycle treatment reduced the bond strength of lithium disilicate glass ceramics in all groups (P<0.05). After cool-thermal cycle, the lithium disilicate glass ceramics treated with HF had higher bond strength than that of the ceramics treated with PA. The lithium disilicate glass ceramics treated with 4% HF had higher bond strength than that of the ceramics treated with 9.5% HF (P<0.05). During cool-thermal cycle, the lithium disilicate glass ceramics treated with 4% HF demonstrated higher reduction in bond strength than that of the samples treated with 9.5% HF (P<0.05). Conclusion The concentration of HF significantly affected the surface morphology of lithium disilicate glass ceramics and the bond durability between resin composites and post-treated lithium disilicate glass ceramics. The bond strength between resin composites and post-treated lithium disilicate glass ceramic was more efficiently maintained by treatment with 9.5% HF.