大气压冷等离子体处理提高氧化锆粘接性能

Effects of different atmospheric pressure cold gas plasmas on bonding of zirconia

目的:研究大气压冷等离子体处理对氧化锆粘接性能的影响。方法:将60个氧化锆试件磨光后随机分为6组(n=10)对照组(C),无表面处理;预处理剂组(P),预处理剂均匀涂布氧化锆表面并吹干;喷砂组(SB),氧化铝颗粒均匀喷砂20sec;喷砂+预处理剂组(SBP),氧化锆表面经氧化铝颗粒均匀喷砂后涂布预处理剂并吹干;氦气大气压冷等离子处理组(HP),氦气(He)作为发生气体的大气压冷离子处理90sec;氩气大气压冷等离子处理组(AP),氩气(Ar)作为发生气体的大气压冷离子处理90sec。各组观察氧化锆表面形貌,测量粗糙度和接触角,进行X射线光电子能谱(XPS)分析,测量剪切粘接强度,并对测量结果进行统计学分析。结果:喷砂组表面形貌显著改变,氦气和氩气大气压冷等离子处理组表面形貌与对照组相似。氦气和氩气大气压冷等离子处理组表面粗糙度为(0. 03±0. 01)μm,小于对照组(0. 04±0. 01)μm,差异无统计学意义(P> 0. 05)。喷砂、氦气和氩气大气压冷等离子处理组表面接触角分别为52. 48°±2. 76°、32. 51°±3. 36°、25. 98°±3. 16°,均较对照组(72. 16°±4. 88°)明显减小,差异有统计学意义(P<0. 05)。氦气大气压冷等离子处理组和氩气大气压冷等离子处理组的剪切粘接强度分别为(16. 02±1. 95)MPa和(16. 06±1. 78)MPa,明显大于对照组(9. 06±0. 94)MPa、喷砂组(14. 72±1. 88)MPa和预处理剂组(12. 40±1. 32)MPa,差异有统计学意义(P<0. 05),但小于喷砂+预处理剂组(17. 25±1. 77)MPa,差异无统计学意义(P> 0. 05)。而氦气冷离子处理组和氩气冷等离子处理组间剪切粘接强度差异无统计学意义(P> 0. 05)。XPS结果显示,喷砂、氦气和氩气大气压冷等离子处理后表面碳元素减少,氧元素增加,碳/氧比值减小。结论:大气压冷等离子体处理几乎不会改变氧化锆表面形貌和粗糙度;大气压冷等离子体处理可提高氧化锆表面亲水性,增加表面氧含量,改善氧化锆粘接强度;氦气和氩气作为发生气体进行大气压冷等离子体处理对氧化锆表面性能和粘接强度的影响相似。

Objective: To evaluate the effects of atmospheric pressure cold plasma on bonding of zirconia. Methods: Sixty zirconia disks were polished and randomly assigned into six groups(n=10): control(C), no treatment. primer(P), applied primer to discs and dried. sand-blasting(SB), alumina sandblast treatment. sand-blasting+primer(SBP), applied air abrasion with aluminum oxide and primer. helium atmospheric pressure cold plasma(HP), applied cold plasma generated from helium gas for 90 s. argon atmospheric pressure cold plasma(AP), applied cold plasma generated from argon gas for 90 s. Surface modifications were assessed by observing surface topography and measuring the surface roughness and contact angle. X-ray photoelectron spectroscopy(XPS) analysis characterized the surface chemical compositions. Shear bond strength(SBS)tests examined the adhesion between resin cement and zirconia. Results: Surface morphology of two plasma treatment groups were similar to the control group. Sandblasted zirconia showed different uneven surface morphology. The surface roughness(Ra) of helium gas plasma group(0.03±0.01)μm and argon gas plasma group(0.03±0.01)μm were lower than the control group(0.04 ±0.01)μm without statistically significance(P >0.05). The contact angle of sand-blasting group(52.48°±2.76°), helium gas plasma group(32.51°±3.36°) and argon gas plasma group(25.98°±3.16°) were lower than the control group(72.16°±4.88°) with statistically significance(P<0.05). The values of shear bond strength of helium gas plasma group and argon gas plasma group were(16.02±1.95)MPa and(16.06±1.78)MPa, which were higher than values of the control group(9.06±0.94)MPa, sand-blasting group(14.72±1.88)MPa and primer group(12.40±1.32) MPa with statistically significance(P <0.05) while which were lower than sand-blasting+primer group(17.25 ±1.77)MPa without statistically significance(P>0.05). XPS showed increase in O and decrease in C elements after sand-blasting and plasma treatments.Conclusion: The atmospheric pressure cold plasma hardly affected the surface morphology and roughness of zirconia. The atmospheric pressure cold plasma improved hydrophilicity and increased oxygen content of zirconia surfaces. The shear bond strength of two plasma groups improved evidently. The effects on surface morphology and bonding of zirconia showed no difference between helium gas plasma group and argon gas plasma group.