硅锆浆料涂层对氧化锆陶瓷与树脂水门汀粘接强度的影响

Effect of SiO_(2)-ZrO_(2) slurry coating on shear bond strength of zirconia to resin cement

目的探讨不同配比硅锆涂层对氧化锆陶瓷与树脂水门汀粘接强度的影响,以期为氧化锆的临床应用提供参考。方法将140个预烧结氧化锆瓷片根据伪随机数字表随机分为空白组、喷砂组和5个涂层组(每组20个),并进行相应处理。空白组无涂层直接烧结,喷砂组无涂层烧结后喷砂,涂层2∶1组、1∶1组、1∶2组、1∶3组和1∶4组分别按硅锆摩尔比为2∶1、1∶1、1∶2、1∶3和1∶4涂布涂层后烧结。氧化锆瓷片表面经氢氟酸酸蚀和硅烷偶联剂处理后,使用树脂水门汀粘接瓷片与预成复合树脂柱,制作粘接试件。粘接试件分为两个亚组,一亚组试件置于37℃水浴24 h(冷热循环前),另一亚组试件经5和55℃冷热循环5000次;测试各组试件剪切强度,即粘接强度,观察并记录各组试件破坏模式,另按上述方法各涂层组制作1个瓷片用于扫描电镜观察酸蚀后表面形貌并测量涂层厚度。结果冷热循环前,涂层1∶1组粘接强度最大[(41.69±6.28)MPa],显著大于其余各组(P<0.05);涂层1∶2组粘接强度其次,除与涂层2∶1组差异无统计学意义外(P>0.05),与其他组差异均有统计学意义(P<0.05);喷砂组、涂层2∶1组和1∶3组粘接强度差异均无统计学意义(P>0.05),均显著大于空白组和涂层1∶4组(P<0.05);空白组粘接强度显著大于涂层1∶4组(P<0.05)。冷热循环后,涂层2∶1组、1∶1组、1∶2组粘接强度[分别为(24.13±5.50)、(22.28±4.40)和(23.11±4.80)MPa]差异均无统计学意义(P>0.05),均显著大于其余各组(P<0.05);喷砂组和涂层1∶3组粘接强度差异无统计学意义(P>0.05),均显著大于空白组和涂层1∶4组(P<0.05);空白组与涂层1∶4组粘接强度下降至几乎为0 MPa,两组差异无统计学意义(P>0.05)。扫描电镜示各涂层组表面酸蚀后形成程度不一的粗糙表面,涂层厚度在30μm以内。结论硅锆浆料涂层可影响氧化锆与树脂水门汀的粘接强度,其中硅锆配比为1∶1的浆料可使氧化锆获得较高且稳定的粘接强度。

Objective To evaluate the effect of shear bond strength between resin cement and zirconia using SiO_(2)-ZrO_(2) slurry coating.Methods One hundred and forty pre-sintered zirconia discs were randomly divided into seven groups(n=20)according to the surface treatments:AS(as-sintered),SB(sand blasting with Al2O3),2SiO_(2)-1ZrO_(2)(2∶1 mole ratio SiO_(2)-ZrO_(2) coating),1SiO_(2)-1ZrO_(2)(mole ratio 1∶1 SiO_(2)-ZrO_(2) coating),1SiO_(2)-2ZrO_(2)(mole ratio 1∶2 SiO_(2)-ZrO_(2) coating),1SiO_(2)-3ZrO_(2)(mole ratio 1∶3 SiO_(2)-ZrO_(2) coating),1SiO_(2)-4ZrO_(2)(mole ratio 1∶4 SiO_(2)-ZrO_(2) coating).Each zirconia disc was bonded to composite resin cylinder using resin cement.All specimens were stored in distilled water(37℃,24 h).Each group was divided into two subgroups in which half specimens were tested using universal testing machine and another half specimens accepted artificial aging of 5000 times thermocycling then tested.Scaning electron microscopy(SEM)was used to observe the micro-morphology of coating surface etched by hydrofluoric acid,then the coating thickness was measured.Results Before artificial aging,1SiO_(2)-1ZrO_(2) showed a higher shear bond strength[(41.69±6.28)MPa]than all the other group(P<0.05).1SiO_(2)-2ZrO_(2) gained a higher strength than AS,SB,1SiO_(2)-3ZrO_(2) and 1SiO_(2)-4ZrO_(2)(P<0.05).However,1SiO_(2)-2ZrO_(2) did not get a significant higher shear bond strength than 2SiO_(2)-1ZrO_(2)(P>0.05).No significant differences were found among SB,2SiO_(2)-1ZrO_(2) and 1SiO_(2)-3ZrO_(2)(P>0.05).After artificial aging,shear bond strength of all groups were decreased significantly besides 2SiO_(2)-1ZrO_(2).2SiO_(2)-1ZrO_(2),1SiO_(2)-1ZrO_(2) and 1SiO_(2)-2ZrO_(2)[(24.13±5.50),(22.28±4.40),(23.11±4.80)MPa]showed higher shear bond strength than SB and 1SiO_(2)-3ZrO_(2)(P<0.05),no intergroup differences were observed(P>0.05).Shear bond strength of AS and 1SiO_(2)-4ZrO_(2) fell to 0 MPa approximately.The SEM images of etched coating surface showed contraction fissure due to different thermal expansion coefficient between SiO_(2) and ZrO_(2) and intercrystal pores of zirconia.The thickness of coating was measured to be less than 30μm.Conclusions Mole ratio 1∶1 SiO_(2)-1ZrO_(2) slurry coating showed the highest shear bond strength of resin cement to zirconia.