釉涂层技术对氧化锆表面特性及粘接强度的影响

Effect of glaze coating technique on surface characteristics and bond strength of zirconia

目的探讨釉涂层技术对氧化锆陶瓷表面特性及粘接强度的影响。方法制作100块完全烧结的氧化锆试件,随机分成5组,每组20块。采用5种方式对各组试件氧化锆表面进行处理,A组为空白对照,B组为氧化铝喷砂,C组为涂釉+1次氢氟酸(HF)蚀刻,D组为涂釉+1次HF蚀刻+硅烷偶联剂,E组为涂釉+2次HF蚀刻+硅烷偶联剂。比较各组氧化锆试件表面微观形貌、化学元素成分、粗糙度及氧化锆与树脂粘接剂之间的粘接强度。结果氧化锆试件表面粗糙度从高至低依次为C组[(0.68±0.05)μm]、D组[(0.57±0.06)μm]、E组[(0.48±0.04)μm]、B组[(0.14±0.04)μm]、A组[(0.06±0.01)μm],各组间两两比较,差异有统计学意义(P<0.05)。扫描电子显微镜观察结果显示,A组氧化锆试件表面可见交错纵横的横线,B组氧化锆试件表面形成不规则的凹坑,C组、D组、E组氧化锆试件表面出现均匀分布的凹坑,且D组、E组凹坑相较于C组更为密集、细小。氧化锆试件表面化学元素成分能谱分析结果显示,A组仅含锆和氧元素,B组含有锆、氧和铝元素,C组、D组、E组均含有锆、氧和硅元素。氧化锆试件剪切粘接强度从高至低依次为E组[(12.71±0.81)MPa]、D组[(10.82±0.75)MPa]、C组[(7.06±0.54)MPa]、B组[(4.98±0.49)MPa]、A组[(3.13±0.47)MPa],各组间两两比较,差异有统计学意义(P<0.05)。结论釉涂层技术提高了氧化锆表面的粗糙度及其粘接强度,适度延长HF酸蚀时间可进一步提升氧化锆表面粘接强度,但酸蚀时间不宜过长,且需注意釉涂层厚度的控制。

Objective To investigate the effect of glaze coating technique on the surface characteristics and bond strength of zirconia ceramics.Methods A total of 100 fully sintered zirconia specimens were prepared and randomly divided into 5 groups,with 20 specimens in each group.The zirconia surfaces of the specimens in each group were treated with five different ways:group A(control group without treatment),group B(alumina sandblasting),group C(glaze coating+etching for one time with hydrofluoric acid[HF]),group D(glaze coating+etching for one time with HF+silane coupling agent),and group E(glaze coating+etchings for two times with HF+silane coupling agent).The surface micromorphology,chemical element composition,roughness,and bond strength between zirconia and resin cement were compared among the groups.Results The surface roughness of zirconia specimens from highest to lowest was as follows:group C[(0.68±0.05)μm],group D[(0.57±0.06)μm],group E[(0.48±0.04)μm],group B[(0.14±0.04)μm],and group A[(0.06±0.01)μm].Pairwise comparisons among the above groups showed statistically significant differences(P<0.05).Scanning electron microscope observation revealed interlaced horizontal lines on the surface of group A zirconia specimens,irregular pits on the surface of group B zirconia specimens,and uniformly distributed pits on the surfaces of zirconia specimens in groups C,D,and E.The pits in groups D and E were denser and finer compared to those in group C.Energy dispersive spectrometry analysis of the chemical element composition on the zirconia specimen surfaces showed that group A contained only zirconium and oxygen,group B contained zirconium,oxygen,and aluminum,and groups C,D,and E contained zirconium,oxygen,and silicon.The shear bond strength of zirconia specimens from highest to lowest was as follows:group E[(12.71±0.81)MPa],group D[(10.82±0.75)MPa],group C[(7.06±0.54)MPa],group B[(4.98±0.49)MPa],and group A[(3.13±0.47)MPa],and between-group differences were observed(P<0.05).Conclusion The glaze coating technique improves the surface roughness and bond strength of zirconia.Appropriately extending the HF etching time can further enhance the bond strength of zirconia surfaces,but the etching time should not be too long,and attention should be paid to the control of glaze coating thickness.