不同表面处理对国产口腔二硅酸锂玻璃陶瓷与树脂水门汀粘接强度的影响

目的探讨不同表面处理方式对国产口腔二硅酸锂玻璃陶瓷与树脂水门汀之间粘接强度的影响。方法选择尺寸为15 mm×13 mm×3 mm的二硅酸锂玻璃陶瓷试件,分别进行酸蚀实验和酸蚀后偶联处理实验。酸蚀实验选择128个玻璃陶瓷试件,按照随机数表法随机分为8个处理时间点(每个时间点样本量为16),使用4.5%氢氟酸分别进行0(对照)、10、20、30、40、60、120及180 s的表面酸蚀,再将酸蚀后试件分为偶联处理组(涂布硅烷偶联剂)和无偶联处理组(不涂布硅烷偶联剂)(每组样本量均为8),分别制作粘接试件;测试粘接强度并分析断裂模式。另选8个玻璃陶瓷试件分别行上述时间点酸蚀后进行扫描电镜观察。选择酸蚀实验中的最佳酸蚀时间,进行酸蚀后偶联处理实验。选择玻璃陶瓷试件24个,4.5%氢氟酸酸蚀后涂布偶联剂,分别进行室温放置、60及100℃热风处理60 s(每组样本量为8),之后制作粘接试件;测试粘接强度并分析断裂模式。另选3个试件分别进行酸蚀后偶联处理实验相应处理后再行红外光谱分析。结果无论是否使用偶联剂,试件在氢氟酸酸蚀30 s时均可获得最大粘接强度;酸蚀30 s条件下,偶联处理组粘接强度[(25.91±4.30)MPa]显著大于无偶联处理组[(20.27±4.92)MPa](P<0.05);若酸蚀时间过长(>30 s),则粘接强度下降明显,试件表面显示过酸蚀的微观形貌。酸蚀后偶联处理实验显示,60℃热风组粘接强度最大[(28.70±5.32)MPa],显著大于室温组[(20.08±3.64)MPa]和100℃热风组[(25.64±4.86)MPa](P<0.05),且试件断裂模式均为内聚破坏;红外光谱分析显示,60℃热风组试件表面Si—O—Si键生成量最多,100℃热风组次之,室温组最低。结论4.5%氢氟酸酸蚀二硅酸锂玻璃陶瓷的最佳酸蚀时间为30 s,涂布硅烷偶联剂可获得较理想的粘接效果;60℃热风处理可进一步提高二硅酸锂玻璃陶瓷与树脂水门汀之间的粘接强度。

Effects of different surface treatments on the bonding strength between the lithium disilicate glass ceramic and resin cements

Objective To investigate the effects of different surface treatments protocol on the bonding strength between lithium disilicate glass ceramic and resin cements.Methods Ceramic specimens of 15 mm×13 mm×3 mm were used to evaluate the effects of different surface treatments of hydrofluoric acid etching and silane coupling in current research.Firstly,the standard lithium ceramic specimens were divided into 8 groups(n=16),and were etched by 4.5%hydrofluoric acid for 0,10,20,30,40,60,120 and180 s.Then specimens in each group was further divided into two sub-groups.In one sub-group specimens were coated with coupling agents and in the other were not.Shear bonding strength(SBS)and failure mode were tested and analyzed.The surface morphologies of hydrofluoric acid-etched ceramic specimens were observed by the scanning electron microscopy(SEM).Secondly,after being etched by 4.5%hydrofluoric acid for 30 s,the lithium ceramic specimens were coated with coupling agents at different temperatures:room temperature(12℃)for 60 s,60℃hot air for 60 s and 100℃hot air for 60 s(n=8).SBS and fracture mode were tested and analyzed.The infrared spectrum analysis was used to characterize the coupled surfaces of the ceramic samples.Results The maximum SBS values were obtained after the specimens were etched for 30 s.The silane coupled group showed a higher SBS value[(25.91±4.30)MPa,P<0.05]than the no-silane-coupled group[(20.27±4.92)MPa].SBS decreased with extended etching time(>30 s)and the SEM photos showed over-etching morphologies.The 60℃hot air treatment resulted in the maximum SBS value[(28.70±5.32)MPa]than that of the room temperature[(20.08±3.64)MPa]or 100℃hot air[(25.64±4.86)MPa,P<0.05].And the cohesive failure mode was found in 60℃hot air treatment group.The infrared spectroscopy analysis showed the highest amount of silicon oxide bond in the 60℃hot air treatment group.Conclusions In this study,for this product,the optimum etching time of 4.5%hydrofluoric acid was 30 s.Furthermore,an ideal SBS value could be obtained when the silane coupling agents were applied additionally.SBS could be increased substantially when the 30 s-etched-ceramic product was coated with silane coupling agents at 60℃hot air for 60 s.