硅锆浆料涂层对氧化锆陶瓷表面性能的影响

Effect of SiO2-ZrO2 slurry coating on surface performance of zirconia ceramic

目的 探讨硅锆浆料涂层对预烧结氧化锆陶瓷表面性能的影响,以寻求提高氧化锆与树脂粘接剂间粘接强度的新方法.方法 70个预烧结氧化锆试件根据计算机产生的伪随机数字表分为空白对照组（致密烧结）、喷砂组（烧结后喷砂）和5个涂层组（每组10个）,各涂层组分别涂布硅锆摩尔比为2：1、1：1、1：2、1：3和1：4的硅锆浆料涂层后烧结（分别命名为2SiO2-1ZrO2、1SiO2-1ZrO2、1SiO2-2ZrO2、1SiO2-3ZrO2、1SiO2-4ZrO2组）,用粗糙度测量仪、X射线衍射仪、能谱仪以及扫描电镜分析各组表面粗糙度、晶相组成并经氢氟酸酸蚀后行表面形貌观察.结果 空白对照组、喷砂组、2SiO2-1ZrO2、1SiO2-1ZrO2、1SiO2-2ZrO2、1SiO2-3ZrO2、1SiO2-4ZrO2组表面粗糙度分别为（0.33 ±0.03）、（0.86±0.05）、（3.85±0.38）、（3.78±0.56）、（4.06±0.48）、（1.02±0.09）和（1.53±0.23） μm,各涂层组表面粗糙度均显著大于空白对照和喷砂组（P＜0.05）;晶相分析示空白对照组及各涂层组表面均为四方晶相氧化锆,喷砂组出现单斜晶相;能谱仪显示硅锆浆料涂层能增加氧化锆表面硅元素含量;扫描电镜示硅锆涂层表面经氢氟酸酸蚀后形成大小不等的孔隙,并随着涂层浆料中硅含量的减少而变小.结论 硅锆浆料涂层可明显增加氧化锆表面粗糙度,提高氧化锆表面硅元素含量,不引起氧化锆相变,且酸蚀后表面可形成孔隙,能形成可靠的氧化锆粘接面.

Objective To evaluate the effect of SiO2-ZrO2 slurry coating on surface performance of zirconia ceramic.Methods Seventy pre-sintered zirconia discs were randomly divided into seven groups with 10 discs per group.Sample discs in each group received one of the following seven different surface treatments, namely, sintered（group AS）, sand blasting after sintered（group SB）, coated with slurry of mole ratio of SiO2 to ZrO2 2： 1（group 2SiO2-1ZrO2）, coated with slurry of mole ratio of SiO2 to ZrO2 1： 1（group 1SiO2-1ZrO2）, coated with slurry of mole ratio of SiO2 to ZrO2 1 ： 2（group 1SiO2-2ZrO2）, coated with slurry of mole ratio of SiO2 to ZrO2 1 ： 3（group 1SiO2-3ZrO2）, coated with slurry of mole ratio of SiO2 to ZrO2 1：4（group 1 SiO2-4ZrO2）.Profilometer, X-ray diffractometer（XRD）, energy dispersive spectrometer, scanning electron microscopy（SEM） were used to analyze surface performance.Results The surface roughness of the discs in group AS was lower than those in the other groups[（0.33 ± 0.03） μm] （P〈0.05）, there was no statistically significant difference（P〉0.05） among group 2SiO2-1ZrO2[（3.85±0.38） μm], group 1SiO2-1ZrO2[（3.78±0.56） μm] and group 1SiO2-2ZrO2[（4.06 ± 0.48） μtm], and no difference（P〉0.05） was observed between group 1SiO2-3ZrO2 [（1.02±0.09） μm] and group 1SiO2-4ZrO2[（1.53±0.23） μm] either.However, surface roughness in all coating groups was higher than those in group SB[（0.86 ± 0.05） μm] （P〈0.05）.According to the XRD pattern, group AS and all coating groups consisted of 100% tetragonal airconia and monoclinic zirconia was detected at surface of group SB.Contents of surface silicon of coating groups increased significantly,however, no silicon was detected at sample surface of group AS and group SB.SEM showed that zirconia grains of coating exposed since part of silicon was etched by hydrofluoric acid, a three-dimensional network of intergrain nano-spaces was created.Conclusions SiO2-ZrO2 slurry coating could make surface of zirconia rough and increase Si content without creating monoclinic zirconia.