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材料研究学报  2015, Vol. 29 Issue (3): 221-226    DOI: 10.11901/1005.3093.2014.279
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两次氧化条件对阳极氧化铝孔洞的影响
李鑫,李秉羲,骆玉城,李阳平()
凝固技术国家重点实验室 西北工业大学材料学院 西安 710072
Impacts of Processing Parameters on Morphology of Pores for Anodic Oxide Film Prepared on Aluminum Foil by Twice Anodization
Xin LI,Bingxi LI,Yucheng LUO,Yangping LI()
The State Key Laboratory of Solidification Processing, School of Materials Science and Engineering, Northwestern Polytechnical University, Xi’an 710072, China
引用本文:

李鑫,李秉羲,骆玉城,李阳平. 两次氧化条件对阳极氧化铝孔洞的影响[J]. 材料研究学报, 2015, 29(3): 221-226.
Xin LI, Bingxi LI, Yucheng LUO, Yangping LI. Impacts of Processing Parameters on Morphology of Pores for Anodic Oxide Film Prepared on Aluminum Foil by Twice Anodization[J]. Chinese Journal of Materials Research, 2015, 29(3): 221-226.

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摘要: 

采用两次阳极氧化法在草酸溶液中制备多孔氧化铝(AAO), 分别研究了电压、氧化时间及草酸溶液浓度对AAO孔洞特征的影响。结果表明, 在第一次氧化过程中孔间距随氧化电压的提高而增大, 氧化时间和草酸溶液浓度几乎没有影响; 在第二次氧化过程中时间、电压及草酸溶液浓度对孔间距基本无影响, 但是随着氧化电压的增大AAO孔径明显增大, 孔洞呈六方阵列排布。此外, 第二次氧化电压增大时孔洞形状由圆形到长条形、再到六边形变化; 第二次氧化草酸溶液浓度增大至0.4 mol/L时所制备的AAO的相邻孔洞沿特定取向发生贯穿现象, 甚至溶解, 而孔洞整体分布有序性几乎不受影响。

关键词 无机非金属材料, 多孔氧化铝两次氧化法草酸溶液孔洞特征    
Abstract

Aluminum foil was anodic oxidized by a two-step anodization process in oxalic acid solutions. While the influence of processing parameters, such as voltage, time and solution concentration, for the 1st and 2nd steps of anodization process on the characteristics of pores of the anodic aluminum oxides (AAO) films was investigated. Results show that for the 1st anodization, the pores spacing increases with the rising voltage, yet the anodization time and the concentration of oxalic acid solution have almost no influence; for the 2nd anodization process, the pores spacing doesn’t change when varying the voltage, the anodization time and the concentration of solution, but the pore diameter rises greatly with the rise of the voltage. The pores of the AAOs films are well arranged in a form of hexagonal array. Furthermore, the shape of the pores changes slightly when increasing the voltage for the 2nd anodization. High concentration (up to 0.4 mol/L) oxalic acid solution for the 2nd anodization resulted in an oriented piercing of the pore’s wall, even a dissolving of the AAO layer, but the pores arrangement was not affected.

Key wordsinorganic non-metallic materials    AAO    two-step anodization    oxalic acid    characteristics of pore
收稿日期: 2014-06-06     
基金资助:* 陕西省自然科学基础研究计划项目2013JM8033、国家大学生创新创业训练计划项目201210699058和西北工业大学本科毕业论文重点扶持项目(2014年度)资助。
Group t/h U/V CB/mol/L
1# a 2 50 0.3
b 4
c 8
2# a 4 40 0.3
b 50
c 60
3# a 4 50 0.2
b 0.3
c 0.4
表1  电化学阳极氧化法制备AAO的工艺参数
图1  第一次氧化和去除一次氧化层后的AAO的SEM像
图2  第一次氧化时间不同, 其余工艺参数保持不变时AAO的SEM像
图3  第一次氧化电压不同, 其余工艺参数保持不变时AAO的SEM像
图4  第一次氧化草酸浓度不同, 其余工艺参数保持不变时AAO的SEM像
图5  第二次氧化时间不同, 其余工艺参数保持不变时AAO的SEM像
图6  第二次氧化电压不同, 其余工艺参数保持不变时AAO的SEM像
图7  第二次氧化草酸浓度不同, 其余工艺参数保持不变时AAO的SEM像
图8  孔径、孔间距及孔壁厚度随第一次及第二次氧化工艺参数的变化曲线
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