剧烈-温和阳极氧化结合法快速制备有序阳极氧化铝膜的研究

doi:10.3724/SP.J.1077.2014.13525

无机材料学报 ›› 2014, Vol. 29 ›› Issue (6): 645-649.DOI: 10.3724/SP.J.1077.2014.13525 CSTR: 32189.14.SP.J.1077.2014.13525

剧烈-温和阳极氧化结合法快速制备有序阳极氧化铝膜的研究

郝爱文^{1, 2}, 黄丽清¹, 程龙¹, 李新¹, 张薇薇¹, 单冬至¹, 冯雪红¹

(1. 西安交通大学理学院, 物质非平衡合成与调控教育部重点实验室, 西安 710049; 2. 中国洛阳电子装备试验中心, 洛阳 471000)

收稿日期:2013-10-12 修回日期:2013-12-20 出版日期:2014-06-20 网络出版日期:2014-05-27
作者简介:郝爱文(1987-), 男, 硕士研究生. E-mail: lqhuangxjtu@126.com
基金资助:
陕西省科学技术研究发展计划项目(2012K07-19);Scientific and Technological R & D Project in Shaanxi Province of China (2012K07-19)

Fast Fabrication of Highly Ordered Porous Anodic Alumina Membranes by Hard-mild Anodization

HAO Ai-Wen^{1, 2}, HUANG Li-Qing¹, CHENG Long¹, Li Xin¹, ZHANG Wei-Wei¹, SHAN Dong-Zhi¹, FENG Xue-Hong¹

(1. Non-equilibrium Condensed Matter and Quantum Engineering Laboratory, School of Science, Xi’an Jiaotong University, Xi’an 710049, China; 2. Luoyang Electronic Equipment Test Center of China, Luoyang 471000, China)

Received:2013-10-12 Revised:2013-12-20 Published:2014-06-20 Online:2014-05-27
About author:HAO Ai-Wen. E-mail: lqhuangxjtu@126.com

摘要/Abstract

摘要：

本研究采用剧烈-温和阳极氧化(hard anodization-mild anodization, HA-MA)结合快速制备高度有序多孔阳极氧化铝(porous anodic alumina, PAA)膜的方法, 即先利用HA在铝表面快速形成有序凹坑阵列, 然后再对表面留有有序凹坑的铝基进行温和阳极氧化, 制备出有序PAA膜。研究了剧烈阳极氧化时氧化电压、氧化时间对所制备PAA膜有序度的影响。研究结果表明, HA-MA结合法制备PAA膜的优化HA参数为: 0.3 mol/L硫酸、80 V、10 min。HA-MA结合法所制备PAA膜的有序性和机械稳定性与二步温和阳极氧化法的相近, 但形成有序PAA膜所需的时间为4.5 h, 约为温和阳极氧化法的1/4, 极大地提高了高度有序PAA膜的制备效率。

关键词: 多孔阳极氧化铝, 温和阳极氧化法, 剧烈阳极氧化法, 剧烈-温和阳极氧化结合法

Abstract:

A hard-mild anodization combined method (HA-MA) for rapidly fabricating highly ordered porous anodic alumina (PAA) membranes is presented in this paper. Firstly, by using hard-anodization (HA), the ordered pit arrays on aluminum surface were rapidly prepared and then, by using mild anodization (MA), ordered PAA membranes were fabricated on the ordered pit arrays aluminum surface. The effect of HA parameters, such as anodization voltage and duration, on the order degree of as-fabricated PAA membranes were investigated. The results showed that the optimum HA voltage and duration in 0.3 mol/L sulfuric acid at -1.5℃ were 80 V and 10 min, respectively. The order degree and mechanical stability of as-fabricated PAA membranes were similar to that of PAA membranes fabricated by two-step MA method, but its total process duration was within 4.5 h, which cost only about 1/4 time as that of by two-step MA method, The HA-MA method greatly improved the fabrication efficiency of ordered PAA.

Key words: porous anodic alumina, mild anodization, hard anodization, hard-mild combined method

中图分类号:

O611

郝爱文, 黄丽清, 程龙, 李新, 张薇薇, 单冬至, 冯雪红. 剧烈-温和阳极氧化结合法快速制备有序阳极氧化铝膜的研究[J]. 无机材料学报, 2014, 29(6): 645-649.

HAO Ai-Wen, HUANG Li-Qing, CHENG Long, Li Xin, ZHANG Wei-Wei, SHAN Dong-Zhi, FENG Xue-Hong. Fast Fabrication of Highly Ordered Porous Anodic Alumina Membranes by Hard-mild Anodization[J]. Journal of Inorganic Materials, 2014, 29(6): 645-649.

图/表 5

图1 不同UH下阳极氧化电流IA随时间t的变化曲线

Fig. 1 Current-time transients during HA of aluminium substrates in 0.3 mol/L H2SO4 (-1.5?C) at UH=60, 70 and 80 V, respectively

图2 tH为30 min时不同UH下所制备PAA膜下表面的SEM照片(插图为FFT图)和孔间距Dint随UH变化关系图

Fig. 2 SEM images of bottom surface and dependence of Dint on the anodization voltage UH for PAA which was fabricated by HA for 30 min in 0.3 mol/L H2SO4 (-1.5℃) at various anodization voltage UH (Insets show the FFT image of corresponding membrane) (a) SEM image of PAA fabricated at UH=60 V; (b) SEM image of PAA fabricated at UH=70 V; (c) SEM image of PAA fabricated at UH=80 V; (d) Dependence of Dint on the anodization voltage UH for fabricated PAA

图3 UHO为80 V时不同氧化时间所制备硫酸HA膜下表面的SEM照片(插图为FFT图)

Fig. 3 SEM images of PAA bottom surface fabricated by HA in 0.3 mol/L H2SO4 (-1.5℃) at UH= 80 VI (Inset shows the FFT image of corresponding membrane) (a) SEM image of PAA fabricated at tH = 25 min; (b) SEM image of PAA fabricated at tH = 20 min; (c) SEM image of PAA fabricated at tH =15 min; (d) SEM image of PAA fabricated at tH=10 min

图4 UH为80 V时阳极氧化电流密度和孔间距随时间变化的关系

Fig. 4 Dependence of current density IA and Dint of fabricated PAA on anodization time tH for HA in 0.3 mol/L H2SO4 (-1.5℃) at UH= 80 V

图5 HA-MA结合法、MA法所制备PAA膜上、下表面的SEM照片. 插图为相应的FFT照片

Fig. 5 SEM images of top and bottom surfaces of PAA fabricated by HA-MA and MA, respectively. The inset shows the FFT image of corresponding SEM image (a) Top and (b) bottom surfaces of PAA fabricated by HA-MA with optimum HA parameters; (c) Top and (d) bottom surfaces of PAA fabricated by HA-MA with non-optimum HA parameters; (e) Top and (f) bottom surfaces of PAA fabricated by two step MA

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剧烈-温和阳极氧化结合法快速制备有序阳极氧化铝膜的研究

Fast Fabrication of Highly Ordered Porous Anodic Alumina Membranes by Hard-mild Anodization

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