Yang L L, Zhang X Y, Zheng Y C, Zhou C J, Wu J L
Department of General Dentistry, School and Hospital of Stomatology, Cheeloo College of Medicine, Shandong University & Shandong Key Laboratory of Oral Tissue Regeneration & Shandong Engineering Laboratory for Dental Materials and Oral Tissue Regeneration, Jinan 250012, China.
Liaoning Upcera Digital Dental Technology Co. Ltd, Shenyang 110167, China.
Zhonghua Kou Qiang Yi Xue Za Zhi. 2021 Jan 9;56(1):80-85. doi: 10.3760/cma.j.cn112144-20200217-00061.
To investigate the effects of different surface treatments protocol on the bonding strength between lithium disilicate glass ceramic and resin cements. 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 (=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 (=8). SBS and fracture mode were tested and analyzed. The infrared spectrum analysis was used to characterize the coupled surfaces of the ceramic samples. 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, <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, <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. 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.
为研究不同表面处理方案对二硅酸锂玻璃陶瓷与树脂水门汀之间粘结强度的影响。本研究中，采用尺寸为15 mm×13 mm×3 mm的陶瓷试样来评估氢氟酸蚀刻和硅烷偶联等不同表面处理的效果。首先，将标准锂陶瓷试样分为8组（每组16个），分别用4.5%氢氟酸蚀刻0、10、20、30、40、60、120和180 s。然后，每组试样再进一步分为两个亚组。一个亚组的试样涂覆偶联剂，另一个亚组不涂覆。测试并分析剪切粘结强度（SBS）和失效模式。通过扫描电子显微镜（SEM）观察氢氟酸蚀刻后陶瓷试样的表面形貌。其次，在锂陶瓷试样用4.5%氢氟酸蚀刻30 s后，分别在不同温度下涂覆偶联剂：室温（12℃）下涂覆60 s、60℃热风下涂覆60 s和100℃热风下涂覆60 s（每组8个）。测试并分析SBS和断裂模式。采用红外光谱分析对陶瓷样品的偶联表面进行表征。试样蚀刻30 s后获得最大SBS值。硅烷偶联组的SBS值[（25.91±4.30）MPa，P<0.05]高于未偶联硅烷组[（20.27±4.92）MPa]。蚀刻时间延长（>30 s）时SBS降低，SEM照片显示过度蚀刻的形貌。60℃热风处理产生的SBS值最大[（28.70±5.32）MPa]，高于室温处理组[（20.08±3.64）MPa]或100℃热风处理组[（25.64±4.86）MPa，P<0.05]。并且在60℃热风处理组中发现内聚破坏模式。红外光谱分析显示60℃热风处理组中氧化硅键的含量最高。在本研究中，对于该产品，4.5%氢氟酸的最佳蚀刻时间为30 s。此外，额外应用硅烷偶联剂时可获得理想SBS值。当30 s蚀刻的陶瓷产品在60℃热风下涂覆硅烷偶联剂60 s时，SBS可显著提高。
