李月月,海几哲,单春龙,李海杰,徐庆宇,雷岳衡.电解液时效对两次阳极氧化法制备TiO2纳米管涂层及性能的影响[J].表面技术,2025,54(6):206-216.
LI Yueyue,HAI Jizhe,SHAN Chunlong,LI Haije,XU Qingyu,LEI Yueheng.Effect of Electrolyte Aging on TiO2 Nanotube Coating and Its Properties Prepared by Double Anodizing Method[J].Surface Technology,2025,54(6):206-216 |
| 电解液时效对两次阳极氧化法制备TiO2纳米管涂层及性能的影响 |
| Effect of Electrolyte Aging on TiO2 Nanotube Coating and Its Properties Prepared by Double Anodizing Method |
| 投稿时间：2024-04-10 修订日期：2024-07-03 |
| DOI：10.16490/j.cnki.issn.1001-3660.2025.06.019 |
| 中文关键词: 钛合金 阳极氧化 TiO2纳米管涂层 电解液时效 微观形貌 |
| 英文关键词:titanium alloy anodizing TiO2 nanotube coating aging electrolyte micro-morphology |
| 基金项目:国家自然科学基金地区科学基金项目(52165026) |
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| Author | Institution |
| LI Yueyue | College of Mechanical Engineering, Xinjiang University, Urumqi 830000, China |
| HAI Jizhe | College of Mechanical Engineering, Xinjiang University, Urumqi 830000, China |
| SHAN Chunlong | Sixth Affiliated Hospital of Xinjiang Medical University, Urumqi 830000, China |
| LI Haije | College of Mechanical Engineering, Xinjiang University, Urumqi 830000, China |
| XU Qingyu | College of Mechanical Engineering, Xinjiang University, Urumqi 830000, China |
| LEI Yueheng | College of Mechanical Engineering, Xinjiang University, Urumqi 830000, China |
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| 中文摘要: |
| 目的 在钛合金表面制备TiO2纳米管涂层，探究电解液重复阳极氧化后成分及数值的变化，以及电解液时效对TiO2纳米管涂层性能的影响。方法 采用乙二醇基电解液，通过两次阳极氧化法，在钛合金表面制备TiO2纳米管涂层，控制电解液时效为0、10和20 h。通过测试，对不同时效的电解液成分及涂层的结构、形态、物相组成、表面润湿性、耐腐蚀性、力学性能、膜结合强度和生物相容性进行综合表征与分析。结果 电解液时效的增加，导致电导率降至491 μs/cm2，pH值升至8.11，氟离子浓度下降而钛离子浓度上升;电流密度降低，纳米管从纳米草状变为开放管顶形态，管壁增厚，管长从7.0 μm缩短至4.4 μm;物相组成保持不变;涂层的耐腐蚀性、硬度、弹性模量均得到增强。在3组样件中，电解液时效为10 h的样件展现出最优的亲水性(15.10°)、结合强度(0.528 N)以及良好的生物相容性。结论 通过调节电解液时效可以提高TiO2纳米管涂层的耐蚀性、硬度和弹性模量，而TiO2纳米管涂层的形貌、亲水性与结合强度在特定的电解液时效范围内展现出优良性，并非随电解液时效的增加而提升。在电解液时效为10 h时，TiO2纳米管涂层的整体性能得到显著提高。 |
| 英文摘要: |
| The work aims to modify the surface of titaium alloy by double anodizing method, prepare a TiO2 nanotube coating on the surface of titanium alloy, analyze the composition and value changes of electrolytes after repeated anodizing, and study the effect of electrolyte aging on the properties of the TiO2 nanotube coating. Glycol based electrolyte was anodized multiple times to obtain different aging electrolytes. A TiO2 nanotube coating was prepared on the surface of the pre-treated titanium alloy by two anodizing methods, and the aging of the electrolyte was controlled for 0 h, 10 h and 20 h. Inductively coupled plasma emission spectrometer, ion chromatograph, pH meter and conductivity instrument were used to study the ion concentration, conductivity and pH value of the electrolyte under different aging conditions. The structure, morphology, phase composition, surface wettability, corrosion resistance, mechanical properties and film bonding strength of the TiO2 nanotube coating were characterized and analyzed by scanning electron microscopy, X-ray diffractometer, contact angle measuring instrument, electrochemical workstation and nanoindentation instrument. The cell compatibility of the TiO2 nanotube coating was tested by cultured rat bone marrow mesenchymal stem cells (BMSCs). The anodic oxidation method was used to prepare the electrolyte with different aging time, and the TiO2 nanotube coating was successfully prepared on the surface of the pre-treated titanium alloy. With the increase of aging, the conductivity of the electrolyte decreased to 491 μs/cm2, the pH increased to 8.11, the concentration of fluoride ion decreased, and the concentration of titanium ion increased. With the decrease of current density, the surface morphology of TiO2 nanotubes changed from nanograss shape to open tube top shape, the tube wall thickness increased, and the tube length shortened from 7.0 μm to 4.4 μm. The phase composition did not change; The corrosion resistance, hardness and elastic modulus were all improved. It was worth noting that although the corrosion resistance of the sample coated with TiO2 nanotube was significantly higher than that of the sample without coatings, the increase of electrolyte aging did not significantly improve the corrosion resistance of the sample. The hydrophilicity and bonding strength did not increase continuously with the increase of electrolyte aging, but reached the best when the electrolyte aging was 10 h, which were 15.10° and 0.528 N, respectively. The biocompatibility of the electrolyte at 10 h and 20 h was better than that of the fresh electrolyte. The aging of the electrolyte improved the hydrophilicity of the sample and was more conducive to cell adhesion and growth. In conclusion, in this paper, the electrolyte of different aging is studied systematically, and the overall performance of TiO2 nanotube coating is tested and analyzed comprehensively. First, the composition and numerical changes of the electrolyte during repeated anodizing are recorded, and then the coating performance is significantly improved by adjusting the aging of the electrolyte, but it is worth noting that not all the properties increase with the increase of the aging of the electrolyte. The hardness and elastic modulus of TiO2 nanotubes increase with the increase of electrolyte aging, and the corrosion resistance is only improved slightly. However, the good morphology, hydrophilicity and bonding strength of the TiO2 nanotube coating only appear in the appropriate range of electrolyte aging, and there is no situation that electrolyte aging is proportional to the improvement of coating performance. Therefore, under the condition of electrolyte aging for 10 h, the TiO2 nanotube coating has been significantly improved, and the overall performance is the best. |
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