Durability of Siloxane-bond between Ceramic and Resin Cement after Water-storage

目的：分析树脂粘固剂与镜面陶瓷之间的微拉伸粘结强度，探讨酸性磷酸盐单体活化硅烷偶联剂形成的硅氧烷粘结剂的耐久性。方法：以长石瓷为原料制备陶瓷试件(约7×7×10 mm)，抛光得到镜面抛光表面的金刚石化合物。超声波清洗后，表面用硅烷偶联剂(瓷键活化剂，Kuraray)与酸性磷酸盐单体(兆键底漆，Kuraray)活化处理。将两个硅烷化试件用4-META/MMA-TBB树脂粘结剂(超级粘结剂，太阳医疗)在37℃的空气中粘结至少24小时，然后将粘结的试件切片成横梁，平均横截面积为1.070.12mm2。它们浸泡在水中(第1组)或储存在空气中(C…更多控制)在37℃。在0周(基线)、1周、2周、4周和8周后，以1 mm/min的十字头速度进行微拉伸粘结强度测试。用pH=2.4的酸性溶液活化的硅烷偶联剂(组2)代替单独的酸性单体和硅烷偶联剂(组3)也进行了相同的实验。结果：平均基线强度约为26 Mpa，所有空气储存的样品在所有老化时间内具有相似的强度。在水中保存的样品往往强度较低，但由于硅氧烷键在长达8周的时间内被水解，因此没有明显的减弱。多元线性回归分析表明，浸泡在水中的粘结强度显著低于存放在空气中的粘结强度(p&lt；0.05)，而老化过程中粘结强度没有明显下降。此外，组1和组2在所有老化时间上均无显著差异。而组3的粘结强度明显低于组1和组2，P<0.01。结论：在本体外实验范围内，4-META/MMA-TBB树脂粘结剂与长石瓷之间的粘结耐久性来源于硅烷偶联剂的酸化。较少

Objective : To analyze micro-tensile bond strength between resin cement and a ceramic with a mirror finished surface that eliminated the effect of mechanical retention on the bond strength, and to investigate the durability of siloxane-bonds formed by an acidic phosphate monomer activated silane coupling agent.Methods : Ceramic specimen (approximately 7 x 7 x 10mm) was prepared from feldspathic porcelain (Super Porcelain AAA, Noritake), and was polished to obtain a mirror finished surface with diamond compounds. After an ultrasonic cleaning, the surface was treated by a silane coupling agent (PORCELAIN BOND ACTIVATOR, Kuraray) activated with an acidic phosphate monomer (MEGA BOND PRIMER, Kuraray). Two silanated specimens were bonded each other using 4-META/MMA-TBB resin cement (Super-Bond, Sun Medical) at 37℃ in air for at least 24 h. Then the bonded specimen was sliced into beams with a mean cross-sectional area of 1.070.12mm2. They were immersed in water (Group 1) or stored in air (C … More ontrol) at 37℃. After 0 (baseline),1,2,4 and 8 weeks, they were subjected to micro-tensile bond strength tests at a crosshead speed of 1mm/min. The same experiment was also performed using the silane coupling agent activated with an acidic solution of pH=2.4 (Group 2) instead of the acidic monomer and the silane coupling agent alone (Group 3).Results : The average baseline strength was about 26 MPa and all air-stored specimens gave similar strengths for all aging durations. The specimens stored in water tended to give lower strengths but there was no pronounced weakening due to the hydrolysis of siloxane bond up to 8 weeks. Multiple linear regression analysis revealed that the bond strength is significantly lower in specimens immersed in water than those stored in air (p<0.05), while the bond strength was not significantly decreased during aging. Moreover, there was no significant difference between Group 1 and Group 2 for all aging durations. On the other hand, Group 3 gave significantly lower bond strength compared to Groups 1 and 2, with a p-value less than 0.01.Conclusions : Within the limitation of the present in vitro study, it can be concluded that the durability of siloxane-bond between 4-META/MMA-TBB resin cement and feldspathic porcelain is derived from the acidification of the silane coupling agent. Less