郑俊杰,刘向锋,刘超,付佳俊,王青华.激光-化学制备超疏水氧化锆陶瓷工艺及修复性能研究[J].表面技术,2024,53(24):165-177.
ZHENG Junjie,LIU Xiangfeng,LIU Chao,FU Jiajun,WANG Qinghua.Fabrication and Repairing Performance of Superhydrophobic Zirconia Ceramic by Laser-chemical Treatment[J].Surface Technology,2024,53(24):165-177 |
| 激光-化学制备超疏水氧化锆陶瓷工艺及修复性能研究 |
| Fabrication and Repairing Performance of Superhydrophobic Zirconia Ceramic by Laser-chemical Treatment |
| 投稿时间：2024-01-22 修订日期：2024-07-09 |
| DOI：10.16490/j.cnki.issn.1001-3660.2024.24.015 |
| 中文关键词: 氧化锆陶瓷 超疏水表面 激光加工 机械稳定性 修复性能 |
| 英文关键词:zirconia ceramic superhydrophobic surface laser processing mechanical stability repairing performance |
| 基金项目:国家自然科学基金(52105175);江苏省自然科学基金(BK20210235);江苏省双创博士资助项目(JSSCBS20210121);南京市留学人员科技创新择优资助项目(1102002310);东南大学至善青年学者项目(2242024RCB0035) |
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| Author | Institution |
| ZHENG Junjie | School of Mechanical Engineering, Southeast University, Nanjing 211189, China |
| LIU Xiangfeng | School of Mechanical Engineering, Southeast University, Nanjing 211189, China |
| LIU Chao | School of Mechanical Engineering, Southeast University, Nanjing 211189, China |
| FU Jiajun | School of Mechanical Engineering, Southeast University, Nanjing 211189, China |
| WANG Qinghua | School of Mechanical Engineering, Southeast University, Nanjing 211189, China |
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| 中文摘要: |
| 目的 通过超疏水化改变氧化锆陶瓷表面的功能特性，使其具备抵抗环境变化的性质。方法 开发了一种结合纳秒激光织构和硅烷化学修饰、热处理方法的超疏水氧化锆陶瓷表面制备工艺，得到了超疏水氧化锆表面，同时对激光加工前后的氧化锆陶瓷表面形貌、化学组成、润湿性进行了表征。结果 利用激光表面微织构方法在氧化锆陶瓷材料表面诱导出了多级微纳结构，并进行硅烷化学修饰和热处理，获得了接触角159.6°的超疏水氧化锆陶瓷表面。研究了激光扫描速度与间距对表面超疏水性能的影响。发现当扫描速度为20~200 mm/s时，随扫描速度的减小，表面的亚微米和纳米颗粒变小，表面微纳结构更明显，进一步使水滴接触角增大;当扫描间距为50~200 μm时，随扫描间距的增大，受到热影响的区域面积相对比例减小，微纳结构减少，进一步使水滴接触角减小。摩擦磨损实验证明，超疏水氧化锆陶瓷表面的机械稳定性高，可抵抗外界摩擦的影响。此外，还测试了使用硅油-热处理方法快速修复受到摩擦后的氧化锆陶瓷表面接触角，证明修复后的氧化锆陶瓷表面仍然保持超疏水特性。结论 研发的可修复超疏水氧化锆陶瓷具有稳定良好的超疏水特性，有望拓展氧化锆陶瓷在相关领域的应用。 |
| 英文摘要: |
| Zirconia ceramic shows potential application value with high-performance in the fields of structural ceramics, functional ceramics, biomaterials, and catalyst carriers. However, the inherent hydrophilicity of zirconia limits its application in some situations. Therefore, the fabrication of superhydrophobic zirconia ceramic surface through surface modification technology has important research value. Current research indicates that laser texturing can be effectively applied to prepare superhydrophobic zirconia ceramic surfaces. Nerveless, the existing femtosecond and picosecond laser processes have high costs and require long-term air post-treatment, resulting in low preparation efficiency. In addition, due to the fact that superhydrophobic surfaces are prone to fail in some harsh environments, the self-healing function of superhydrophobic surface is also limited. It is very necessary to design an efficient and low-cost laser preparation technology to achieve rapid preparation of self-healing superhydrophobic zirconia ceramic surfaces. At the stage of sample preparation, the zirconia ceramic samples were ultrasonically treated for 5 min to remove surface impurities. A laser marking machine with 355 nm ultraviolet laser light source was used to perform laser surface texture treatment (Fig.1). The laser textured sample was soaked in the mixture of 0.5 mL of silane solution for 3 h and then dried at 200 ℃ for 30 min to obtain superhydrophobic zirconia ceramic. At the stage of performance evaluation, a contact angle measurement device was used to measure the water contact angle of the surface of the laser textured zirconia ceramic. Then, the morphological characteristics and composition of the surface were analyzed by confocal laser scanning microscope, SEM, and XPS. Moreover, the mechanical stability of the superhydrophobic zirconia ceramic surface was explored through a load sandpaper friction experiment. Meanwhile, the superhydrophobic zirconia ceramic surface was repaired by silicone oil-heat method, thereby achieving the reuse of materials. The test results indicated that the laser scanning speed and spacing had obvious effect on wettability of the zirconia ceramic surface. Under the condition that the scanning speed was 20 mm/s and the scanning spacing was 100 μm, the superhydrophobic zirconia ceramic surface exhibited superior water contact angle of 159.6°. The surface had a neatly arranged and dense micro/nanostructure, which could intercept more air layers. Moreover, the composition of the superhydrophobic zirconia ceramic surface underwent significant changes during the preparation process. The surface exhibited oxidized reaction by laser ablation, resulting in the decrease of the hydrophobic groups (C—C (H)) and the increase of the hydrophilic groups (O—C==O). The surface exhibited excellent hydrophilicity with high surface energy. After silanization and heat treatment, non-polar C-F bonds in silane solution and groups such as alkyl were deposited on the surface. The superhydrophobic zirconia ceramic surface was obtained under the combined effects of relevant micro/nanostructures and low surface energy. The friction experiment results suggested the microstructure of the sample surface was destroyed under friction, and the surface wettability was also changed. Through the repair process, the surface superhydrophobicity could be restored. This was caused by the further deposition of hydrophobic groups in the silicone oil during the silicone oil-heat treatment repair process. After heat treatment, silicon atoms were deposited to form a thin film. Thus, the recovery of superhydrophobicity on the sample surface after friction was achieved. In summary, the sample surface prepared by the laser-chemical process shows excellent superhydrophobicity and self-healing properties. This provides a support for the applications of zirconia in the fields of structural ceramics, functional ceramics, biomaterials, and catalyst carriers. |
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