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目的:研究热处理温度对TiO2纳米管膜层表面特性的影响。方法:利用阳极氧化法在纯钛表面制备TiO2纳米管膜层。以TiO2纳米管膜层为对照组,通过扫描电镜、能谱分析仪、X射线分析仪,激光共聚焦显微镜及接触角分析仪检测450℃、500℃、550℃及600℃热处理后的TiO2纳米管膜层表征。结果:利用阳极氧化法可获得管径规整均一,高度有序的TiO2纳米管膜层。450℃、500℃及550℃处理后膜层表面形貌及纳米管管径相近;仅550℃组纳米管壁厚度增加;600℃处理后膜层形貌破坏,纳米管结构坍塌。各组均由钛、氧元素组成;仅对照组含有少量氟元素。对照组TiO2纳米管为非晶态结构;450℃处理后,锐钛矿相出现;500℃处理后,锐钛矿衍射峰强度增加;550℃处理后,锐钛矿衍射峰减弱,且金红石相出现;600℃处理后,金红石相衍射峰显著升高。对照组TiO2纳米管膜层及450℃处组膜层具有较高的亲水性及表面能,其余各组的亲水性及表面能随热处理温度的升高呈逐渐下降的趋势。结论:不同温度的热处理可改变TiO2纳米管膜层的表面特性,且晶相结构是引起膜层表面特性改变的主要原因。550℃及以下温度处理不会破坏TiO2纳米管结构,并可获得不同晶相的TiO2纳米管膜层。
Objective: To study the effect of heat treatment temperature on the surface properties of TiO2 nanotube films. Methods: The TiO2 nanotube film was prepared on pure titanium by anodic oxidation. TiO2 nanotubes were used as the control group. The nanostructured TiO2 nanostructures were characterized by scanning electron microscopy, energy dispersive spectroscopy, X-ray analyzer, confocal laser scanning microscopy and contact angle analyzer. Tube film characterization. Results: The uniform and highly ordered TiO2 nanotube films were obtained by anodic oxidation. After 450 ℃, 500 ℃ and 550 ℃, the surface morphology and nanotube diameter are similar. The thickness of the nanotube increases only at 550 ℃. The morphology of the film is destroyed after 600 ℃, and the nanotube structure collapses. Each group is composed of titanium, oxygen; only the control group contains a small amount of fluorine. TiO2 nanotubes were amorphous in the control group. The anatase phase appeared after 450 ℃ treatment, and the intensity of the anatase diffraction peak increased after 500 ℃ treatment. The diffraction peak of anatase was weakened after 550 ℃ treatment, and the rutile phase Appeared; after 600 ℃ treatment, the diffraction peak of rutile phase increased significantly. The control group TiO2 nanotube film and the film layer at 450 ℃ have higher hydrophilicity and surface energy. The hydrophilicity and surface energy of the other groups decrease gradually with the increase of heat treatment temperature. Conclusion: The heat treatment at different temperatures can change the surface properties of the TiO2 nanotube film. The crystal structure is the main reason for the change of surface properties. The temperature of 550 ℃ and below will not destroy the structure of TiO2 nanotubes, and get TiO2 nanotubes with different crystal phases.