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采用新的二次阳极氧化工艺,制备了多孔纳米阳极氧化铝(anodized Al2O3,AAO)膜。对铝在草酸溶液中的二次阳极氧化过程进行了研究。利用扫描电镜、原子力显微镜、透射电镜等对其形貌进行了表征和分析。结果表明:用高纯铝所制备的纳米AAO膜孔大小一致,有序性强;膜的孔径随扩孔时间的增加而增大,随草酸浓度的增加而减少。进一步延长扩孔时间至1.5h,其孔径生长规律仍符合AAO膜孔径可控性动力学模型方程,使原模型的扩孔时间范围由1.0h拓展到1.5h。AAO膜的最佳制备工艺为:采用0.3mol/L草酸溶液,电压为40V,在40℃氧化9h和扩孔1h。在最佳制备工艺条件下,制备的AAO膜厚为112.7μm,孔径为70nm左右。
A new anodized Al2O3 (AAO) film was prepared by a new secondary anodic oxidation process. The secondary anodization of aluminum in oxalic acid solution was studied. Morphology was characterized by scanning electron microscopy, atomic force microscopy and transmission electron microscopy. The results show that the pore size of AAO membrane prepared by high purity aluminum is uniform and orderly. The membrane pore size increases with the increase of reaming time and decreases with the increase of oxalic acid concentration. Further expanding the reaming time to 1.5h, its aperture growth law is still in line with AAO membrane pore size controllable kinetic model equation, the original model reaming time range expanded from 1.0h to 1.5h. The optimal preparation process of AAO membrane was as follows: 0.3mol / L oxalic acid solution was used, the voltage was 40V, oxidation was carried out at 40 ℃ for 9h and reaming for 1h. Under the optimal preparation conditions, the prepared AAO film has a thickness of 112.7μm and a pore size of about 70nm.