OBJECTIVES: The aims of the study were to develop and test multi-phase glaze coatings for zirconia restorations, so that the surface could be etched and adhesively bonded. METHODS: Zirconia disc specimens (n=125, 16 mm x 1 mm) were cut from cylinders of Y-TZP (yttria-stabilized tetragonal zirconia polycrystals) ZS-Blanks (Kavo, Everest) and sintered overnight. Specimens were subjected to the recommended firing cycles, and next sandblasted. The specimens were divided into 5 groups of 25, with Group 1 as the sandblasted control. Groups 2-5 were coated with overglaze materials (P25 and IPS e.max Ceram glazes) containing secondary phases. Group 2 was (wt%): 10% hydroxyapatite (HA)/P25 glaze, Group 3: 20% IPS Empress 2 glass-ceramic/glaze, Group 4: 20% IPS Empress 2 glass/glaze and Group 5: 30% IPS Empress 2 glass/glaze. After sintering and etching, Monobond-S and composite resin cylinders (Variolink II, Ivoclar-Vivadent) were applied and light cured on the test surfaces. Specimens were water stored for 7 days. Groups were tested using the shear bond strength (SBS) test at a crosshead speed of 0.5 mm/min. Overglazed and the fractured specimen surfaces were viewed using secondary electron microscopy. Room and high temperature XRD and DSC were carried out to characterize the materials. RESULTS: The mean (SD) SBS (MPa) of the test groups were: Group 1: 7.7 (3.2); Group 2: 5.6 (1.7); Group 3: 11.0 (3.0); Group 4: 8.8 (2.6) and Group 5: 9.1 (2.6). Group 3 was significantly different to the control Group 1 (p<0.05). There was no significant difference in the mean SBS values between Group 1 and Groups 2, 4 and 5 (p>0.05). Group 2 showed statistically lower SBS than Groups 3-5 (p<0.05). Lithium disilicate fibres were present in Groups 3-5 and fine scale fibres were grown in the glaze following a porcelain firing cycle (Groups 4 and 5). XRD indicated a lithium disilicate/minor lithium orthophosphate phase (Group 3), and a tetragonal zirconia phase for the sintered Y-TZP ZS-Blanks. DSC and high temperature XRD confirmed the crystallization temperatures and phases for the IPS Empress 2 glass. CONCLUSIONS: The application of a novel glass-ceramic/glaze material containing a major lithium disilicate phase might be a step in improving the bond strength of a zirconia substrate to a resin cement.
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机译：目的：本研究的目的是开发和测试用于氧化锆修复体的多相釉料涂层，以便可以对表面进行蚀刻和粘合。方法：从Y-TZP（氧化钇稳定的四方氧化锆多晶）ZS-Blanks（Kavo，Everest）的圆柱体上切出氧化锆圆盘标本（n = 125，16 mm x 1 mm），并烧结过夜。对样品进行建议的烧成周期，然后进行喷砂处理。将标本分为5组，每组25个，其中第1组为喷砂对照。第2-5组使用含有第二相的上釉材料（P25和IPS e.max Ceram釉）涂覆。第2组是（wt％）：10％羟基磷灰石（HA）/ P25釉料，第3组：20％IPS Empress 2玻璃陶瓷/釉料，第4组：20％IPS Empress 2玻璃/釉料和第5组：30％IPS皇后2玻璃/釉。烧结和蚀刻后，施加Monobond-S和复合树脂圆柱体（Variolink II，Ivoclar-Vivadent）并将其光固化在测试表面上。将标本储水7天。使用剪切粘结强度（SBS）测试以0.5 mm / min的十字头速度测试组。使用二次电子显微镜观察上釉和破裂的样品表面。进行了室温和高温XRD和DSC表征材料。结果：测试组的平均（SD）SBS（MPa）为：组1：7.7（3.2）;第2组：5.6（1.7）;第3组：11.0（3.0）;第4组：8.8（2.6）和第5组：9.1（2.6）。第3组与对照组1有显着差异（p <0.05）。第1组与第2、4和5组之间的平均SBS值无显着差异（p> 0.05）。第2组的SBS在统计上低于第3-5组（p <0.05）。在组3-5中存在二硅酸锂纤维，并且在瓷烧制循环之后（组4和5），在釉料中生长了细规模的纤维。 XRD表示烧结的Y-TZP ZS-Blanks的二硅酸锂/次磷酸正磷酸锂相（第3族）和四方氧化锆相。 DSC和高温XRD证实了IPS Empress 2玻璃的结晶温度和晶相。结论：包含主要的二硅酸锂相的新型玻璃陶瓷/釉料的应用可能是提高氧化锆基体与树脂胶粘剂结合强度的一个步骤。
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