光谱学与光谱分析, 2012, 32 (9): 2515, 网络出版: 2012-09-26  

通孔阳极氧化铝膜的制备及其性能的研究

Preparation and Performance of Through-Hole AAO Film
作者单位
1 上海应用技术学院化学与环境工程学院, 上海 201418
2 瑞吉有限公司, 瑞典 斯德哥尔摩 10691
3 赣南师范学院, 江西 赣州 341000
摘要
在15% H2SO4阳极氧化液中添加硝酸镨制备阳极氧化铝(AAO)膜以提高AAO膜的性能, 采用化学腐蚀和微波处理相结合的方法, 去除AAO膜的阻挡层, 制备通孔的AAO膜。 分别研究镨的添加量、 氧化电压对AAO膜的厚度和硬度的影响及腐蚀时间、 微波处理时间分别对AAO膜的阻挡层的影响, 分别用能谱和扫描电镜等对AAO膜进行了表征。 在15% H2SO4阳极氧化液中添加硝酸镨, 制备出的AAO膜具有更大的厚度和硬度, 当氧化电压为23 V时, 在15% H2SO4+0.14 Pr g·L-1混合液中制备的AAO膜的厚度和硬度分别为162 μm和275.1 HV, 与在阳极氧化液为15% H2SO4溶液中制备的AAO膜的厚度和硬度(150 μm和224.8 HV)相比, 分别提高8.0%和22.4%。 当氧化电压在19~23 V范围时, AAO膜的厚度随着氧化电压的增大而增加; AAO膜的硬度随着氧化电压的增大而减小。 将AAO膜在35 ℃和5% H3PO4溶液中腐蚀13 min, 再用超声波处理10 min, 可得到通孔的AAO膜。 腐蚀后AAO膜表面絮状物为Al2O3。
Abstract
Praseodymium nitrate was used as additives in preparing anodic aluminum oxide (AAO) films to improve its performance. AAO films were prepared by anodization method from a 15 vol.% H2SO4 solution with added praseodymium nitrate. The effects of Pr concentration and anodization voltage on the thickness and microhardness of AAO film were investigated, respectively. The oxide barrier layer of AAO film was removed with the method of combining etching of 5 vol.% H3PO4 solution with ultrasonic wave. treatment The effects of etching time and treating time with ultrasonic wave on the oxide barrier layer of AAO film were investigated respectively. The AAO films were characterized with EDAX and SEM techniques respectively. AAO film prepared in 15 vol.% H2SO4 solution with praseodymium nitrate added showed higher thickness and microhardness. The thickness of AAO films increased with the increase in anodization voltage, while the microhardness of AAO films decreased with the increase in anodization voltage in 19~23 V. When anodization voltage is 23 V, the thickness and microhardness of AAO film prepared in 15 vol.% H2SO4+0.4 Pr g·L-1 mixture solution are as high as 162 μm and 275.1 HV respectively, which are 8.0% and 22.4% higher than that of film prepared in 15 vol.% H2SO4 solution (150 μm and 224.8 HV). The oxide barrier layer of AAO film was removed by combining etching in 5 vol.% H3PO4 solution for 13 min with ultrasonic wave treatment for 10 min, forming through-hole AAO film. The flocks of surface of the etched AAO film are Al2O3.

刘小珍, 刘兆鑫, 陈捷, 王刚, 宋玲玲, 王聪. 通孔阳极氧化铝膜的制备及其性能的研究[J]. 光谱学与光谱分析, 2012, 32(9): 2515. LIU Xiao-zhen, LIU Zhao-xin, CHEN Jie, WANG Gang, SONG Ling-ling, WANG Cong. Preparation and Performance of Through-Hole AAO Film[J]. Spectroscopy and Spectral Analysis, 2012, 32(9): 2515.

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