飞秒激光诱导氧化锆陶瓷微结构及对其粘结性能的影响  

Femtosecond Laser-induced Microstructure on Dental Zirconia Ceramics and Its Effect on Bonding Properties

作　　者：宋逸婷 朱莉[1] 徐一迪 刘思文 林婷婷[2] 黄盛斌[1,2] 林继兴 麻健丰[1,2] SONG Yiting;ZHU Li;XU Yidi;LIU Siwen;LIN Tingting;HUANG Shengbin;LIN Jixing;Ma Jianfeng(Institute of Stomatology, Wenzhou Medical University, Wenzhou 325027, China;School and Hospital of Stomatology, Wenzhou Medical University, Wenzhou 325007, China)

机构地区：[1]温州医科大学口腔医学研究所,浙江温州325027 [2]温州医科大学口腔医学院附属口腔医院,浙江温州325007

出　　处：《口腔医学研究》2022年第3期261-267,共7页Journal of Oral Science Research

基　　金：国家自然科学基金(编号:81870813);温州市科技计划项目(编号:H20190002);温州市重大科技专项(编号:2018ZY012)。

摘　　要：目的:研究飞秒激光加工对氧化钇稳定四方氧化锆多晶陶瓷(Y-TZP)表面微结构及其与自粘型树脂水门汀粘接性能的影响。方法:选取120例烧结氧化锆陶瓷试件随机分为6个研究组,分别对其进行如下处理。A组:对照组,不做处理;B组:氧化铝喷砂;C~F组:表面飞秒激光线性沟槽加工,加工重复次数分别为2、4、6和10次;激光共焦显微镜(CLSM)观察3D形貌及测量沟槽深度,原子力显微镜(AFM)测量表面粗糙度Ra,X射线衍射仪(XRD)分析表面晶相组成,扫描电镜(SEM)观察微观组织,电子万能试验机测试老化(5±1)℃和(55±1)℃的水中交替浸泡5000次,每次30 s前后氧化锆陶瓷与自粘型树脂水门汀的剪切强度,体式显微镜下观察断裂模式;采用SPSS 19.0对所得结果进行单因素方差分析及多重检验。结果:飞秒激光在氧化锆表面扫描2、4、6和10次后,可以得到~30μm、~50μm、~60μm、~70μm深的规则V型沟槽,其表面粗糙度随激光扫描次数的增加而增加;激光表面处理不会导致表面晶相转变;微观组织显示,激光处理后,氧化锆陶瓷基体无陨石坑、孔洞、嵴状突起等缺陷,但过多的扫描次数(10次)可见熔铸层堆积;陶瓷表面V型沟槽增加了表面积的同时,与树脂形成互锁结构,其剪切强度从A组(对照组)与B组(喷砂组)的3.68 Mpa和4.87 MPa,提高至17.78 MPa(C组),22.5 MPa(D组),27.4 MPa(E组)和27.54 MPa(F组),且老化后的剪切强度仍为对照组5倍以上;其断裂模式由对照组与喷砂组的完全粘结破坏转变为内聚破坏和混合破坏;激光处理后的氧化锆陶瓷抗弯强度为457.73 MPa(E组),满足临床应用要求。结论:飞秒激光加工是氧化锆陶瓷表面改性的理想方法之一,合理的微结构设计可以显著提高与自粘型树脂水门汀结合强度,同时具备较好的抗老化性,可替代喷砂等传统的表面处理方法,以延长牙列缺损修复使用寿命。Objective:To study the influence of femtosecond laser processing on the topographies of yttria-stabilised tetragonal zirconia polycrystal(Y-TZP)and its bonding strength with self-adhesive resin cement.Methods:One hundred and twenty cases of sintered zirconia ceramic specimens were randomly divided into six research groups and treated as follows.Group A:Control group with no treatment;group B:alumina sandblasting;C-F group:surface femtosecond laser linear groove processing,processing repetitions were 2,4,6,and 10 times,respectively.Topographic surface analysis and groove depth were performed by laser confocal microscope(CLSM).Surface roughness Ra was measured by atomic force microscope(AFM).Crystal phase was evaluated by X-ray diffraction(XRD).Surface morphology was observed by scanning electron microscopy(SEM).The specimens were then subjected to shear bond strength testing of zirconia ceramic and self-adhesive resin cement before and after aging(5000 cycles with temperature range from(5±1)℃to(55±1)℃for 30s each).Further,stereomicroscope was used to observe the fracture modes.Results:In this study,regular V-shaped grooves with depths of about 30μm,50μm,60μm,and 70μm were obtained after 2,4,6,and 10 times of laser pulses scanning on the surface of zirconia.The surface roughness increased with the increase of laser scanning times.Laser surface treatment does not lead to surface crystal phase transformation.The microstructure showed that after laser ablation by laser,the zirconia ceramic substrate had no craters,holes,ridges,and other defects,but too many scanning times(10 times)could be seen in the casting layer accumulation.The V-shaped grooves on the ceramic surface increased the surface area and formed an interlocking structure with the resin.The shear strength increased from 3.68 MPa and 4.87 MPa in group A(control group)and group B(sandblasting group)to 17.78 MPa(group C),22.5 MPa(group D),27.4 MPa(group E),and 27.54 MPa(group F),and the shear strength after aging was still more than 5 times that of

关 键 词：微结构 飞秒激光 激光加工 表面纹理 粘接强度 

分 类 号：R78[医药卫生—口腔医学]