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飞秒激光处理对氧化锆表面特性及抗弯强度的影响

[Effects of femtosecond laser treatment on surface characteristics and flexural strength of zirconia].

作者信息

Li W J, Ding Q, Yuan F S, Sun F B, Zheng J Q, Bao R, Zhang L

机构信息

Department of Prosthodontics, Peking University School and Hospital of Stomatology & National Center of Stomatology & National Clinical Research Center for Oral Diseases & National Engineering Laboratory for Digital and Material Technology of Stomatology, Beijing 100081, China.

Center for Digital Dentistry, Peking University School and Hospital of Stomatology & Beijing Key Laboratory of Digital Stomatology & Research Center of Engineering and Technology for Computerized Dentistry Ministry of Health, Beijing 100081, China.

出版信息

Beijing Da Xue Xue Bao Yi Xue Ban. 2021 Aug 18;53(4):770-775. doi: 10.19723/j.issn.1671-167X.2021.04.025.

Abstract

OBJECTIVE

To evaluate the effects of femtosecond laser treated microgrooved surface on microscopic topography, phase transformation, and three-points flexural strength of zirconia, and to provide reference for surface microstructure optimization of zirconia implant.

METHODS

According to different surface treatment methods, 57 computer aided design/computer aided manufacture (CAD/CAM) zirconia bars (20.0 mm×4.0 mm×1.4 mm) were evenly divided into three groups: sintered group, no treatment after sintering, taken as control; sandblasted group, sandblasted with 110 μm aluminium oxide (AlO) after sintering; microgrooved group, femtosecond laser fabricated microgrooves with 50 μm width, 30 μm depth, and 100 μm pitch. Surface microscopic topography was observed with scanning electron microscope (SEM) and 3D laser microscope. Further, surface roughness in each group and microgroove size were measured. Crystal phase was analyzed with X-ray diffraction. Specimens were subjected to three- points flexural strength test, and Weibull distribution was used to analyze their strength characteristics.

RESULTS

SEM showed that sintered surface was flat with clear grain structure; sandblasted surface exihibited bumps and holes with sharp margins and irregular shape; microgrooves were regularly aligned without evident defect, and nano-scale particles were observed on the surface inside of the microgrooves. Ra value of microgrooved group [(9.42±0.28)] μm was significantly higher than that of sandblasted group [(1.04±0.03) μm] and sintered group [(0.60±0.04) μm], and there was statistical difference between sandblasted group and sintered group ( < 0.001). The microgroove size was precise with (49.75±1.24) μm width, (30.85±1.02) μm depth, and (100.58±1.94) μm pitch. Crystal phase analysis showed that monoclinic volume fraction of sandblasted group (18.17%) was much higher than that of sintered group (1.55%), while microgrooved group (2.21%) was similar with sintered group. The flexural strength of sandblasted group (986.22±163.25) MPa had no statistical difference with that of sintered group (946.46±134.15) MPa (=0.847), but the strength in microgrooved group (547.92±30.89) MPa dropped significantly compared with the other two groups ( < 0.001). Weibull modulus of sintered, sandblasted, microgrooved groups were 7.89, 6.98, and 23.46, respectively.

CONCLUSION

Femtosecond laser was able to form micro/nanostructured microgrooves on zirconia surface, which deleteriously affected the flexural strength of zirconia.

摘要

目的

评估飞秒激光处理的微槽表面对氧化锆微观形貌、相变及三点弯曲强度的影响,为氧化锆种植体表面微观结构优化提供参考。

方法

根据不同表面处理方法,将57根计算机辅助设计/计算机辅助制造(CAD/CAM)氧化锆棒(20.0 mm×4.0 mm×1.4 mm)均匀分为三组:烧结组,烧结后不做处理,作为对照组;喷砂组,烧结后用110μm氧化铝(AlO)喷砂;微槽组,用飞秒激光制备宽度50μm、深度30μm、间距100μm的微槽。用扫描电子显微镜(SEM)和3D激光显微镜观察表面微观形貌。此外,测量每组表面粗糙度及微槽尺寸。用X射线衍射分析晶体相。对试件进行三点弯曲强度测试,并用威布尔分布分析其强度特性。

结果

SEM显示,烧结表面平整,晶粒结构清晰;喷砂表面有凸起和孔洞,边缘尖锐,形状不规则;微槽排列规则,无明显缺陷,微槽内部表面观察到纳米级颗粒。微槽组的Ra值[(9.42±0.28)μm]显著高于喷砂组[(1.04±0.03)μm]和烧结组[(0.60±0.04)μm],喷砂组与烧结组之间有统计学差异(<0.001)。微槽尺寸精确,宽度为(49.75±1.24)μm,深度为(30.85±1.02)μm,间距为(100.58±1.94)μm。晶体相分析表明,喷砂组的单斜晶体积分数(18.17%)远高于烧结组(1.55%),而微槽组(2.21%)与烧结组相似。喷砂组的弯曲强度(986.22±163.25)MPa与烧结组(946.46±134.15)MPa无统计学差异(=0.847),但微槽组的强度(547.92±30.89)MPa与其他两组相比显著下降(<0.001)。烧结组、喷砂组、微槽组的威布尔模量分别为7.89、6.98和23.46。

结论

飞秒激光能够在氧化锆表面形成微/纳米结构的微槽,这对氧化锆的弯曲强度产生了有害影响。

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