改良热酸蚀处理对氧化铅机械性能及树脂粘接强度的影响

Effect of modified hot-etching treatment on the mechanical properties of zirconia and zirconia/resin bond strength

摘要

目的：探索改良热酸蚀处理对氧化铅弯曲强度、表面晶相及树脂粘接强度的影响。方法：将氧化锆试件根据表面处理方式分为空白组、喷砂组和改良热酸蚀组。使用扫描电子显微镜（scanning electron microscope，SEM）观察各组氧化铅表面形貌，使用 X 射线衍射仪（X-ray diffractometer，XRD）检测各组氧化锆试件表面各晶相比例，使用万能力学试验机测试各组氧化锆试件的挠曲强度。制作平整的牛牙釉质粘接平面，用树脂水门汀完成氧化锆试件粘接，半数粘接试件经过冷热循环疲劳 5000 次，使用万能力学试验机检测各组即刻及温度疲劳后剪切粘接强度（shear bond strengths，SBS）。结果：SEM 结果显示空白组氧化锆表面光滑，喷砂组可见不规则划痕，改良热酸蚀组呈蜂窝状酸蚀形貌。XRD 结果显示单斜相比例，空白组为8.18％，喷砂组为28.34％，改良热酸蚀组为9.69％。挠曲强度喷砂组 $\left[\right(316.40\pm 58.37\left)\mathrm{M}\mathrm{P}\mathrm{a}\right]$ 明显低于空白组 $\left[\right(415.30\pm 47.64\left)\mathrm{M}\mathrm{P}\mathrm{a}\right]$ 和改良热酸蚀组[(398.77±47.94)MPa]，差异具有统计学意义（P<0.01）。即刻 SBS 改良热酸蚀组[(53.77±8.36)MPa]高于空白组[(35.50±4.72)MPa]和喷砂组 $\left[\right(42.97\pm 6.95\left)\mathrm{M}\mathrm{P}\mathrm{a}\right]$ ，差异具有统计学意义 (P<0.01) ；温度疲劳后 SBS 空白组[(21.65±4.01)MPa] 低于改良热酸蚀组 $\left[\right(30.69\pm 7.36\left)\mathrm{M}\mathrm{P}\mathrm{a}\right]$ 和喷砂组 $\left[\right(29.37\pm 5.73\left)\mathrm{M}\mathrm{P}\mathrm{a}\right]$ ，差异具有统计学意义（P<0.01）。结论：改良热酸蚀处理可以提高氧化铅即刻 SBS，具有与喷砂类似抗温度疲劳性能，不会显著降低氧化锆的挠曲强度，未引起明显的表面晶相改变。

Abstract

Objective：To investigate the effect of modified hot-etching treatment on the flexural strength and surface crystalline phase proportions of zirconia and zirconia/resin bond strength. Methods： Zirconia specimens were divided into three groups according to different surface treatments，including blank group，sandblasting treatment group and modified hot-etching treatment group.A scanning electron microscope（SEM）was used to observe the surface morphology of the treated zirconia，an X-ray diffrac- tometer（XRD）was employed to detect the surface crystalline phase proportions，and a universal me- chanical testing machine was utilized to measure the three-point flexural strength of the zirconia specimens of different treatment groups.A bonding surface was prepared with bovine enamel，and the zirconia specimens were bonded using resin cement.Half of the bonded specimens underwent 5000 cycles of thermal cycling fatigue test，and the immediate and fatigued shear bond strengths（SBS）were detected by using a universal mechanical testing machine. Results：SEM observations revealed that the surface of the con- trol group was smooth，the surface of sandblasting treatment group exhibited irregular scratches，and the surface of modified hot-etching treatment group showed a honeycomb-like etched morphology.XRD re- sults indicated that the monoclinic phase proportions were 8.18％for the control group ，28.34％for the sandblasting treatment group，and 9.69％for the modified hot-etching treatment group.The flexural strength of the sandblasting treatment group $\left[\right(316.40\pm 58.37\left)\mathrm{M}\mathrm{P}\mathrm{a}\right]$ was significantly (P<0.01) lower than that of the blank group $\left[\right(415.30\pm 47.64\left)\mathrm{M}\mathrm{P}\mathrm{a}\right]$ and the modified hot-etching treatment group $\left[\right(398.77\pm 47.94\left)\mathrm{M}\mathrm{P}\mathrm{a}\right]$.The immediate SBS of the modified hot-etching treatment group $\left[\right(53.77\pm 8.36\left)\mathrm{M}\mathrm{P}\mathrm{a}\right]$ was higher (P<0.01) than that of blank group $\left[\right(35.50\pm 4.72\left)\mathrm{M}\mathrm{P}\mathrm{a}\right]$ and sandblasting treatment group $\left[\right(42.97\pm 6.95\left)\mathrm{M}\mathrm{P}\mathrm{a}\right]$.After thermal cycling fatigue test，the fatigued SBS of the blank group $\left[\right(21.65\pm 4.01\left)\mathrm{M}\mathrm{P}\mathrm{a}\right]$ was lower (P<0.01) than that of the modified hot- etching treatment group $\left[\right(30.69\pm 7.36\left)\mathrm{M}\mathrm{P}\mathrm{a}\right]$ and the sandblasting treatment group $\left[\right(29.37\pm 5.73)$ MPa]. Conclusion：The modified hot-etching treatment could enhance the immediate zirconia/resin SBS，exhibited similar resistance to thermal fatigue test with sandblasting treatment group，could not sig- nificantly reduce the flexural strength，and did not obviously alter the surface crystalline phase proportions.

关键词

改良热酸蚀 / 氧化锆 / 挠曲强度 / 温度疲劳 / 剪切粘接强度

Key words

Modified hot-etching treatment / Zirconia / Flexural strength / Thermal cycling fatigue / Shear bond strength

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基金资助

北京大学第三医院交叉联合专项基金(BYSYJC2024029)