杨众,于美,张欣然,代徐勉,刘建华.钛合金前处理后时间对其表面溶胶凝胶成膜行为及膜层性能的影响[J].表面技术,2025,54(10):141-150.
YANG Zhong,YU Mei,ZHANG Xinran,DAI Xumian,LIU Jianhua.Effect of Time after Pretreatment on Sol-gel Film FormationBehaviour and Film Property of Titanium Alloy[J].Surface Technology,2025,54(10):141-150 |
| 钛合金前处理后时间对其表面溶胶凝胶成膜行为及膜层性能的影响 |
| Effect of Time after Pretreatment on Sol-gel Film FormationBehaviour and Film Property of Titanium Alloy |
| 投稿时间：2024-07-11 修订日期：2024-10-18 |
| DOI：10.16490/j.cnki.issn.1001-3660.2025.10.011 |
| 中文关键词: 钛合金 工序转移时间 自然氧化时间 溶胶凝胶 成膜行为 膜层性能 |
| 英文关键词:titanium alloy process transfer time natural oxidation time sol-gel film-forming behavior film properties |
| 基金项目: |
| 作者 | 单位 |
| 杨众 | 北京航空航天大学 材料科学与工程学院，北京 100191 |
| 于美 | 北京航空航天大学 材料科学与工程学院，北京 100191 |
| 张欣然 | 北京航空航天大学 材料科学与工程学院，北京 100191 |
| 代徐勉 | 北京航空航天大学 材料科学与工程学院，北京 100191 |
| 刘建华 | 北京航空航天大学 材料科学与工程学院，北京 100191 |
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| Author | Institution |
| YANG Zhong | School of Materials Science and Engineering, Beihang University, Beijing 100191, China |
| YU Mei | School of Materials Science and Engineering, Beihang University, Beijing 100191, China |
| ZHANG Xinran | School of Materials Science and Engineering, Beihang University, Beijing 100191, China |
| DAI Xumian | School of Materials Science and Engineering, Beihang University, Beijing 100191, China |
| LIU Jianhua | School of Materials Science and Engineering, Beihang University, Beijing 100191, China |
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| 中文摘要: |
| 目的 阐明工序转移时间即前处理后自然氧化时间对钛合金表面溶胶凝胶成膜行为及膜层性能的影响机制。方法 Ti-6Al-4V(TC4)合金表面经活化前处理后自然氧化0~36 h不同时间，模拟前处理后涂装工序前的转移时间。通过研究膜层与TC4基体界面形貌，分析氧化时间对TC4合金表面电化学性质、化学组成以及溶胶凝胶润湿性等的影响规律，采用拉开法测试TC4合金与底漆间的结合强度，采用划格法进一步研究盐雾试验前后的结合强度并进行等级评价，最终提出氧化时间对溶胶凝胶成膜行为及膜层性能的影响机制。结果 在0~36 h自然氧化时间范围内，氧化时间对TC4合金试样表面氧化膜耐蚀性无明显影响;钛合金表面与溶胶凝胶的接触角增大，由前处理后的4.5°上升至自然氧化36 h时的44.3°;溶胶凝胶在TC4合金表面的附着功呈减小趋势，由酸洗活化后的103.94 mJ/m2下降到自然氧化36 h时的89.33 mJ/m2。涂覆成膜后，自然氧化时间对涂敷溶胶凝胶膜层的TC4合金与丙烯酸聚氨酯底漆之间的结合强度影响不大，结合强度等级均评定为0级，但经过240 h中性盐雾试验后，随着自然氧化时间延长，丙烯酸聚氨酯底漆大面积脱落。结论 前处理后自然氧化时间延长，钛合金表面羟基(—OH)极性基团含量降低，而表面氧化物含量增加，阻碍钛合金表面与溶胶凝胶间的缩聚程度，不利于溶胶凝胶的成膜，当侵蚀性离子渗透到溶胶凝胶膜层与TC4合金基体界面孔隙，会破坏溶胶凝胶膜层结构，导致丙烯酸聚氨酯底漆大面积脱落。因此，应严格控制前处理后涂膜的时间，缩短工序间隔时间。 |
| 英文摘要: |
| To clarify the influence mechanism of process transfer time, i.e., natural oxidation time after pretreatment, on the formation behavior and properties of the sol-gel film on the surface of titanium alloy, the Ti-6Al-4V (TC4) alloy surface was naturally oxidized for different times from 0 to 36 h after activation pretreatment to simulate the transfer time before the painting process after the pretreatment. The effect of natural oxidation time on the surface electrochemical properties of TC4 alloy was investigated by open circuit potential (OCP) detection and electrochemical impedance spectroscopy (EIS). A mixed sol-gel of silica sol and zirconium sol was prepared, and the wettability of sol-gel and TC4 samples with different natural oxidation times was measured by optical contact angle measuring instrument. And a sol-gel conversion film was prepared by dip-coating method, and the effect of natural oxidation time on the interface morphologies of the sol-gel film and TC4 matrix was observed by SEM (Scanning Electron Microscope), stereomicroscope, etc. The bonding strength between TC4 alloy coated with a sol-gel film after different natural oxidation times and the acrylic polyurethane primer was tested using the pull-off method. And the bonding strength between TC4 alloy coated with a sol-gel film after different natural oxidation times and the acrylic polyurethane primer before and after the 240 h neutral salt spray test was investigated by scratching method, and photographed under a stereomicroscope, and then the adhesion grade was evaluated. Finally, the influence mechanism of oxidation time on the film formation behavior and the film properties was proposed based on the results of XPS (X-ray Photoelectron Spectroscopy) and other experiments. The results indicated that in the range of 0-36 h, the natural oxidation time had little effect on the corrosion resistance of the oxide film on the surface of TC4 alloy. With the extension of natural oxidation time, the contact angle between the titanium alloy surface and sol-gel increased, and the contact angle increased from 4.5° in the test immediately after activation by acid washing to 44.3° in 36 h of natural oxidation. The adhesion work tended to decrease with the extension of the natural oxidation time, from 103.94 mJ/m2 after the activation to 89.33 mJ/m2 after natural oxidation for 36 h. The natural oxidation time had little effect on the bonding strength between TC4 alloy coated with a sol-gel film after different natural oxidation times and the acrylic polyurethane primer, and the bonding strength grades were all rated as grade 0. However, after the 240 h neutral salt spray test, the detached area of the acrylic polyurethane primer increased significantly. After pretreatment, the natural oxidation time was prolonged, and the hydroxyl (—OH) content on the surface of titanium alloy was reduced while the oxides content increased, which hindered the polycondensation degree between the sol-gel and the TC4 alloy matrix, and was not conducive to sol-gel film formation. When the film is in contact with aggressive media, corrosive ions penetrate into the pores at the interface between the sol-gel film and the TC4 alloy matrix, destroying the structure of the sol-gel film and leading to a large area of acrylic polyurethane primer peeling. |
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